# Electronic Supplementary Material (ESI) for RSC Advances.
# 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_FO4332
_database_code_depnum_ccdc_archive 'CCDC 1043774'
_audit_update_record             
;
2016-06-30 deposited with the CCDC.
2016-08-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H31 N7 O5 S Zn2, C2 H3 N, H2 O'
_chemical_formula_sum            'C30 H36 N8 O6 S Zn2'
_chemical_formula_weight         767.47

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n '
_symmetry_space_group_name_Hall  '-P 2yn'

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

_cell_length_a                   13.4746(8)
_cell_length_b                   15.0226(11)
_cell_length_c                   16.6745(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.667(4)
_cell_angle_gamma                90.00
_cell_volume                     3368.4(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.046
_exptl_crystal_size_mid          0.046
_exptl_crystal_size_min          0.034
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1584
_exptl_absorpt_coefficient_mu    1.540
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6133
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2002'

_exptl_special_details           ?

_diffrn_ambient_temperature      133(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  Kappa_CCD
_diffrn_measurement_method       'phi- + omega-scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15345
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_sigmaI/netI    0.0471
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.42
_diffrn_reflns_theta_max         27.49
_reflns_number_total             6769
_reflns_number_gt                5432
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       COLLECT
_computing_cell_refinement       DENZO
_computing_data_reduction        DENZO
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXL-97

_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)+(0.0138P)²+11.0751P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6769
_refine_ls_number_parameters     457
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0565
_refine_ls_wR_factor_ref         0.1176
_refine_ls_wR_factor_gt          0.1062
_refine_ls_goodness_of_fit_ref   1.177
_refine_ls_restrained_S_all      1.177
_refine_ls_shift/su_max          0.007
_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
Zn1 Zn 0.21546(3) 0.17775(3) 0.90193(3) 0.02475(13) Uani 1 1 d . . .
Zn2 Zn 0.07524(3) 0.22045(3) 0.73512(3) 0.02708(13) Uani 1 1 d . . .
S1 S 0.21409(7) 0.06215(8) 0.99691(7) 0.0294(2) Uani 1 1 d . . .
O1 O 0.22577(19) 0.2208(2) 0.78147(17) 0.0270(6) Uani 1 1 d . . .
O2 O 0.2257(2) 0.2990(2) 0.9476(2) 0.0375(8) Uani 1 1 d . . .
O3 O 0.1854(4) 0.4242(3) 1.0085(3) 0.0705(13) Uani 1 1 d . . .
O4 O 0.07089(19) 0.1701(2) 0.85264(18) 0.0295(7) Uani 1 1 d . . .
O5 O -0.0885(2) 0.1477(2) 0.82061(19) 0.0378(8) Uani 1 1 d . . .
N1 N 0.3798(3) -0.0156(3) 1.0538(2) 0.0285(8) Uani 1 1 d . . .
N2 N 0.4035(2) 0.0726(2) 0.9467(2) 0.0253(8) Uani 1 1 d . . .
N3 N 0.3622(2) 0.1340(2) 0.8924(2) 0.0242(7) Uani 1 1 d . . .
N4 N 0.1246(3) 0.3038(3) 0.6450(2) 0.0311(8) Uani 1 1 d . . .
N5 N -0.0622(3) 0.2182(3) 0.6483(2) 0.0307(8) Uani 1 1 d . . .
N6 N -0.0087(3) 0.3318(3) 0.7735(2) 0.0334(9) Uani 1 1 d . A .
N7 N 0.0783(3) 0.0931(3) 0.6826(2) 0.0322(8) Uani 1 1 d . . .
C1 C 0.3415(3) 0.0402(3) 0.9970(2) 0.0236(9) Uani 1 1 d . . .
C2 C 0.4249(3) 0.1702(3) 0.8467(3) 0.0289(10) Uani 1 1 d . . .
H2A H 0.4920 0.1509 0.8540 0.035 Uiso 1 1 calc R . .
C3 C 0.4031(3) 0.2368(3) 0.7858(3) 0.0295(10) Uani 1 1 d . . .
C4 C 0.4851(3) 0.2826(3) 0.7589(3) 0.0330(10) Uani 1 1 d . . .
H4A H 0.5495 0.2662 0.7805 0.040 Uiso 1 1 calc R . .
C5 C 0.4781(3) 0.3502(3) 0.7029(3) 0.0322(10) Uani 1 1 d . . .
C6 C 0.3848(3) 0.3659(3) 0.6671(3) 0.0317(10) Uani 1 1 d . . .
H6A H 0.3779 0.4096 0.6260 0.038 Uiso 1 1 calc R . .
C7 C 0.2998(3) 0.3206(3) 0.6884(3) 0.0274(9) Uani 1 1 d . . .
C8 C 0.3052(3) 0.2586(3) 0.7530(3) 0.0274(9) Uani 1 1 d . . .
C9 C 0.5673(3) 0.4040(4) 0.6833(3) 0.0408(12) Uani 1 1 d . . .
H9A H 0.5543 0.4332 0.6311 0.061 Uiso 1 1 calc R . .
H9B H 0.6252 0.3647 0.6811 0.061 Uiso 1 1 calc R . .
H9C H 0.5808 0.4492 0.7249 0.061 Uiso 1 1 calc R . .
C10 C 0.2096(3) 0.3397(3) 0.6393(3) 0.0325(10) Uani 1 1 d . . .
H10A H 0.2144 0.3834 0.5985 0.039 Uiso 1 1 calc R . .
C11 C 0.0439(3) 0.3303(3) 0.5863(3) 0.0367(11) Uani 1 1 d . . .
H11A H 0.0717 0.3487 0.5353 0.044 Uiso 1 1 calc R . .
H11B H 0.0066 0.3811 0.6073 0.044 Uiso 1 1 calc R . .
C12 C -0.0245(3) 0.2514(3) 0.5718(3) 0.0346(11) Uani 1 1 d . . .
H12A H -0.0814 0.2689 0.5346 0.042 Uiso 1 1 calc R . .
H12B H 0.0118 0.2030 0.5460 0.042 Uiso 1 1 calc R . .
C13 C -0.1390(3) 0.2772(3) 0.6785(3) 0.0379(11) Uani 1 1 d . A .
H13A H -0.1878 0.2405 0.7057 0.045 Uiso 1 1 calc R . .
H13B H -0.1748 0.3070 0.6323 0.045 Uiso 1 1 calc R . .
C14 C -0.0980(3) 0.3472(3) 0.7362(3) 0.0401(12) Uani 1 1 d . . .
C15 C -0.1543(8) 0.4219(7) 0.7549(8) 0.062(3) Uani 0.86(2) 1 d P A 1
H15 H -0.2161 0.4333 0.7260 0.074 Uiso 0.86(2) 1 calc PR A 1
C16 C -0.1211(7) 0.4771(7) 0.8135(8) 0.080(4) Uani 0.86(2) 1 d P A 1
H16 H -0.1601 0.5267 0.8277 0.096 Uiso 0.86(2) 1 calc PR A 1
C17 C -0.0291(6) 0.4615(6) 0.8534(7) 0.064(3) Uani 0.86(2) 1 d P A 1
H17 H -0.0048 0.4993 0.8960 0.076 Uiso 0.86(2) 1 calc PR A 1
C15A C -0.142(5) 0.424(4) 0.728(3) 0.029(12) Uiso 0.14(2) 1 d P A 2
H15A H -0.2010 0.4319 0.6947 0.035 Uiso 0.14(2) 1 calc PR A 2
C16A C -0.087(4) 0.507(4) 0.780(3) 0.054(14) Uiso 0.14(2) 1 d P A 2
H16A H -0.1171 0.5643 0.7841 0.065 Uiso 0.14(2) 1 calc PR A 2
C17A C 0.007(4) 0.488(3) 0.818(3) 0.042(12) Uiso 0.14(2) 1 d P A 2
H17A H 0.0539 0.5323 0.8340 0.050 Uiso 0.14(2) 1 calc PR A 2
C18 C 0.0262(4) 0.3899(4) 0.8299(3) 0.0489(14) Uani 1 1 d . . .
H18A H 0.0911 0.3812 0.8544 0.059 Uiso 0.86(2) 1 calc PR A 1
H18B H 0.0626 0.3693 0.8769 0.059 Uiso 0.14(2) 1 calc PR A 2
C19 C -0.0933(3) 0.1253(3) 0.6396(3) 0.0368(11) Uani 1 1 d . . .
H19A H -0.1337 0.1177 0.5884 0.044 Uiso 1 1 calc R . .
H19B H -0.1351 0.1090 0.6841 0.044 Uiso 1 1 calc R . .
C20 C -0.0041(3) 0.0644(3) 0.6406(3) 0.0347(11) Uani 1 1 d . . .
C21 C -0.0062(4) -0.0166(3) 0.6012(3) 0.0432(12) Uani 1 1 d . . .
H21A H -0.0653 -0.0363 0.5724 0.052 Uiso 1 1 calc R . .
C22 C 0.0780(4) -0.0683(4) 0.6040(3) 0.0483(14) Uani 1 1 d . . .
H22A H 0.0777 -0.1237 0.5764 0.058 Uiso 1 1 calc R . .
C23 C 0.1632(4) -0.0395(4) 0.6470(3) 0.0441(13) Uani 1 1 d . . .
H23A H 0.2224 -0.0739 0.6493 0.053 Uiso 1 1 calc R . .
C24 C 0.1588(4) 0.0405(3) 0.6861(3) 0.0372(11) Uani 1 1 d . . .
H24A H 0.2161 0.0597 0.7175 0.045 Uiso 1 1 calc R . .
C25 C 0.1820(4) 0.3414(4) 1.0005(3) 0.0400(12) Uani 1 1 d . . .
C26 C 0.1260(5) 0.2908(4) 1.0589(4) 0.0664(19) Uani 1 1 d . . .
H26A H 0.1345 0.3192 1.1118 0.100 Uiso 1 1 calc R . .
H26B H 0.1511 0.2296 1.0625 0.100 Uiso 1 1 calc R . .
H26C H 0.0553 0.2900 1.0411 0.100 Uiso 1 1 calc R . .
C27 C -0.0176(3) 0.1481(3) 0.8714(3) 0.0280(9) Uani 1 1 d . . .
C28 C -0.0335(3) 0.1229(4) 0.9567(3) 0.0406(12) Uani 1 1 d . . .
H28A H -0.0955 0.0891 0.9584 0.061 Uiso 1 1 calc R . .
H28B H -0.0377 0.1769 0.9893 0.061 Uiso 1 1 calc R . .
H28C H 0.0223 0.0863 0.9780 0.061 Uiso 1 1 calc R . .
O1W O -0.2898(3) 0.1457(3) 0.8393(3) 0.0553(12) Uani 1 1 d . . .
C2AN C -0.1705(6) 0.3704(5) 1.0373(6) 0.097(3) Uani 1 1 d . . .
H2A1 H -0.1747 0.3503 1.0928 0.145 Uiso 1 1 calc R . .
H2A2 H -0.1751 0.4355 1.0352 0.145 Uiso 1 1 calc R . .
H2A3 H -0.1068 0.3515 1.0175 0.145 Uiso 1 1 calc R . .
N1AN N -0.3145(6) 0.2988(5) 0.9503(5) 0.098(2) Uani 1 1 d . . .
C1AN C -0.2523(6) 0.3315(6) 0.9867(6) 0.080(2) Uani 1 1 d . . .
H1N1 H 0.344(4) -0.045(3) 1.082(3) 0.037(15) Uiso 1 1 d . . .
H2N1 H 0.442(4) -0.033(3) 1.053(3) 0.034(13) Uiso 1 1 d . . .
H1W1 H -0.240(4) 0.143(4) 0.837(4) 0.05(2) Uiso 1 1 d . . .
H2W1 H -0.290(4) 0.208(4) 0.880(3) 0.050(16) 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
Zn1 O2 1.976(3) . ?
Zn1 O4 2.068(3) . ?
Zn1 N3 2.099(3) . ?
Zn1 O1 2.123(3) . ?
Zn1 S1 2.3511(12) . ?
Zn2 N4 2.096(4) . ?
Zn2 O4 2.105(3) . ?
Zn2 N7 2.106(4) . ?
Zn2 O1 2.124(3) . ?
Zn2 N6 2.140(4) . ?
Zn2 N5 2.277(3) . ?
S1 C1 1.749(4) . ?
O1 C8 1.326(5) . ?
O2 C25 1.264(6) . ?
O3 C25 1.252(6) . ?
O4 C27 1.294(5) . ?
O5 C27 1.236(5) . ?
N1 C1 1.342(5) . ?
N1 H1N1 0.82(5) . ?
N1 H2N1 0.88(5) . ?
N2 C1 1.315(5) . ?
N2 N3 1.384(5) . ?
N3 C2 1.293(5) . ?
N4 C10 1.275(6) . ?
N4 C11 1.472(5) . ?
N5 C19 1.463(6) . ?
N5 C13 1.475(6) . ?
N5 C12 1.490(6) . ?
N6 C14 1.339(6) . ?
N6 C18 1.345(6) . ?
N7 C24 1.340(6) . ?
N7 C20 1.345(6) . ?
C2 C3 1.443(6) . ?
C2 H2A 0.9500 . ?
C3 C4 1.400(6) . ?
C3 C8 1.434(6) . ?
C4 C5 1.378(6) . ?
C4 H4A 0.9500 . ?
C5 C6 1.377(6) . ?
C5 C9 1.503(6) . ?
C6 C7 1.397(6) . ?
C6 H6A 0.9500 . ?
C7 C8 1.422(6) . ?
C7 C10 1.450(6) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9500 . ?
C11 C12 1.511(6) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.505(7) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15A 1.30(6) . ?
C14 C15 1.401(11) . ?
C15 C16 1.336(13) . ?
C15 H15 0.9500 . ?
C16 C17 1.389(10) . ?
C16 H16 0.9500 . ?
C17 C18 1.380(9) . ?
C17 H17 0.9500 . ?
C15A C16A 1.67(9) . ?
C15A H15A 0.9500 . ?
C16A C17A 1.41(6) . ?
C16A H16A 0.9500 . ?
C17A C18 1.50(5) . ?
C17A H17A 0.9500 . ?
C18 H18A 0.9500 . ?
C18 H18B 0.9500 . ?
C19 C20 1.508(7) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.384(7) . ?
C21 C22 1.373(7) . ?
C21 H21A 0.9500 . ?
C22 C23 1.383(7) . ?
C22 H22A 0.9500 . ?
C23 C24 1.371(7) . ?
C23 H23A 0.9500 . ?
C24 H24A 0.9500 . ?
C25 C26 1.479(8) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28 1.501(6) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
O1W H1W1 0.67(6) . ?
O1W H2W1 1.16(6) . ?
C2AN C1AN 1.466(11) . ?
C2AN H2A1 0.9800 . ?
C2AN H2A2 0.9800 . ?
C2AN H2A3 0.9800 . ?
N1AN C1AN 1.116(10) . ?

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
O2 Zn1 O4 104.21(13) . . ?
O2 Zn1 N3 105.96(13) . . ?
O4 Zn1 N3 145.09(13) . . ?
O2 Zn1 O1 94.40(13) . . ?
O4 Zn1 O1 76.00(11) . . ?
N3 Zn1 O1 84.53(12) . . ?
O2 Zn1 S1 115.13(10) . . ?
O4 Zn1 S1 100.29(9) . . ?
N3 Zn1 S1 82.40(10) . . ?
O1 Zn1 S1 150.00(9) . . ?
N4 Zn2 O4 155.62(13) . . ?
N4 Zn2 N7 103.22(15) . . ?
O4 Zn2 N7 93.62(13) . . ?
N4 Zn2 O1 85.40(12) . . ?
O4 Zn2 O1 75.22(11) . . ?
N7 Zn2 O1 96.30(13) . . ?
N4 Zn2 N6 86.87(15) . . ?
O4 Zn2 N6 87.48(13) . . ?
N7 Zn2 N6 149.27(14) . . ?
O1 Zn2 N6 113.57(13) . . ?
N4 Zn2 N5 80.55(13) . . ?
O4 Zn2 N5 121.10(12) . . ?
N7 Zn2 N5 76.06(14) . . ?
O1 Zn2 N5 161.90(12) . . ?
N6 Zn2 N5 77.15(14) . . ?
C1 S1 Zn1 95.16(14) . . ?
C8 O1 Zn1 124.9(3) . . ?
C8 O1 Zn2 130.1(3) . . ?
Zn1 O1 Zn2 102.99(11) . . ?
C25 O2 Zn1 135.1(3) . . ?
C27 O4 Zn1 141.0(3) . . ?
C27 O4 Zn2 113.4(3) . . ?
Zn1 O4 Zn2 105.56(12) . . ?
C1 N1 H1N1 122(3) . . ?
C1 N1 H2N1 120(3) . . ?
H1N1 N1 H2N1 116(5) . . ?
C1 N2 N3 114.7(3) . . ?
C2 N3 N2 114.5(3) . . ?
C2 N3 Zn1 124.5(3) . . ?
N2 N3 Zn1 120.0(2) . . ?
C10 N4 C11 117.7(4) . . ?
C10 N4 Zn2 129.4(3) . . ?
C11 N4 Zn2 112.5(3) . . ?
C19 N5 C13 113.9(4) . . ?
C19 N5 C12 110.2(4) . . ?
C13 N5 C12 112.1(4) . . ?
C19 N5 Zn2 107.0(3) . . ?
C13 N5 Zn2 109.5(3) . . ?
C12 N5 Zn2 103.4(2) . . ?
C14 N6 C18 118.4(4) . . ?
C14 N6 Zn2 118.2(3) . . ?
C18 N6 Zn2 123.3(3) . . ?
C24 N7 C20 118.3(4) . . ?
C24 N7 Zn2 123.7(3) . . ?
C20 N7 Zn2 118.0(3) . . ?
N2 C1 N1 116.8(4) . . ?
N2 C1 S1 126.4(3) . . ?
N1 C1 S1 116.8(3) . . ?
N3 C2 C3 126.5(4) . . ?
N3 C2 H2A 116.7 . . ?
C3 C2 H2A 116.7 . . ?
C4 C3 C8 119.5(4) . . ?
C4 C3 C2 115.9(4) . . ?
C8 C3 C2 124.6(4) . . ?
C5 C4 C3 123.9(4) . . ?
C5 C4 H4A 118.1 . . ?
C3 C4 H4A 118.1 . . ?
C6 C5 C4 116.2(4) . . ?
C6 C5 C9 122.3(4) . . ?
C4 C5 C9 121.5(4) . . ?
C5 C6 C7 123.2(4) . . ?
C5 C6 H6A 118.4 . . ?
C7 C6 H6A 118.4 . . ?
C6 C7 C8 120.5(4) . . ?
C6 C7 C10 115.5(4) . . ?
C8 C7 C10 123.9(4) . . ?
O1 C8 C7 123.2(4) . . ?
O1 C8 C3 120.6(4) . . ?
C7 C8 C3 116.1(4) . . ?
C5 C9 H9A 109.5 . . ?
C5 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C5 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N4 C10 C7 126.7(4) . . ?
N4 C10 H10A 116.6 . . ?
C7 C10 H10A 116.6 . . ?
N4 C11 C12 108.2(4) . . ?
N4 C11 H11A 110.1 . . ?
C12 C11 H11A 110.1 . . ?
N4 C11 H11B 110.1 . . ?
C12 C11 H11B 110.1 . . ?
H11A C11 H11B 108.4 . . ?
N5 C12 C11 111.3(4) . . ?
N5 C12 H12A 109.4 . . ?
C11 C12 H12A 109.4 . . ?
N5 C12 H12B 109.4 . . ?
C11 C12 H12B 109.4 . . ?
H12A C12 H12B 108.0 . . ?
N5 C13 C14 113.7(4) . . ?
N5 C13 H13A 108.8 . . ?
C14 C13 H13A 108.8 . . ?
N5 C13 H13B 108.8 . . ?
C14 C13 H13B 108.8 . . ?
H13A C13 H13B 107.7 . . ?
C15A C14 N6 126(3) . . ?
C15A C14 C15 20(2) . . ?
N6 C14 C15 121.2(6) . . ?
C15A C14 C13 114(3) . . ?
N6 C14 C13 117.3(4) . . ?
C15 C14 C13 121.3(6) . . ?
C16 C15 C14 119.9(8) . . ?
C16 C15 H15 120.0 . . ?
C14 C15 H15 120.0 . . ?
C15 C16 C17 119.6(8) . . ?
C15 C16 H16 120.2 . . ?
C17 C16 H16 120.2 . . ?
C18 C17 C16 118.4(7) . . ?
C18 C17 H17 120.8 . . ?
C16 C17 H17 120.8 . . ?
C14 C15A C16A 115(5) . . ?
C14 C15A H15A 122.3 . . ?
C16A C15A H15A 122.3 . . ?
C17A C16A C15A 115(5) . . ?
C17A C16A H16A 122.3 . . ?
C15A C16A H16A 122.3 . . ?
C16A C17A C18 114(4) . . ?
C16A C17A H17A 122.9 . . ?
C18 C17A H17A 122.9 . . ?
N6 C18 C17 122.3(5) . . ?
N6 C18 C17A 119.3(17) . . ?
C17 C18 C17A 35.3(18) . . ?
N6 C18 H18A 118.9 . . ?
C17 C18 H18A 118.9 . . ?
C17A C18 H18A 109.8 . . ?
N6 C18 H18B 120.4 . . ?
C17 C18 H18B 106.2 . . ?
C17A C18 H18B 120.4 . . ?
H18A C18 H18B 35.7 . . ?
N5 C19 C20 110.8(4) . . ?
N5 C19 H19A 109.5 . . ?
C20 C19 H19A 109.5 . . ?
N5 C19 H19B 109.5 . . ?
C20 C19 H19B 109.5 . . ?
H19A C19 H19B 108.1 . . ?
N7 C20 C21 121.3(5) . . ?
N7 C20 C19 116.3(4) . . ?
C21 C20 C19 122.4(4) . . ?
C22 C21 C20 119.3(5) . . ?
C22 C21 H21A 120.3 . . ?
C20 C21 H21A 120.3 . . ?
C21 C22 C23 119.8(5) . . ?
C21 C22 H22A 120.1 . . ?
C23 C22 H22A 120.1 . . ?
C24 C23 C22 117.5(5) . . ?
C24 C23 H23A 121.2 . . ?
C22 C23 H23A 121.2 . . ?
N7 C24 C23 123.7(5) . . ?
N7 C24 H24A 118.1 . . ?
C23 C24 H24A 118.1 . . ?
O3 C25 O2 124.0(5) . . ?
O3 C25 C26 117.2(5) . . ?
O2 C25 C26 118.8(5) . . ?
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 . . ?
O5 C27 O4 121.4(4) . . ?
O5 C27 C28 119.8(4) . . ?
O4 C27 C28 118.9(4) . . ?
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 . . ?
H1W1 O1W H2W1 97(6) . . ?
C1AN C2AN H2A1 109.5 . . ?
C1AN C2AN H2A2 109.5 . . ?
H2A1 C2AN H2A2 109.5 . . ?
C1AN C2AN H2A3 109.5 . . ?
H2A1 C2AN H2A3 109.5 . . ?
H2A2 C2AN H2A3 109.5 . . ?
N1AN C1AN C2AN 177.1(10) . . ?

_diffrn_measured_fraction_theta_max 0.874
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.913
_refine_diff_density_max         0.538
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.092


















































































































































































































































































































































































































































































































































































































































































































































































































































































































































































































































































































































































































































































































































####################################################################### 
# 
# 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_FO5645
_database_code_depnum_ccdc_archive 'CCDC 1048856'
_audit_update_record             
;
2016-06-30 deposited with the CCDC.
2016-08-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H24 N3 Ni O2 P S, 2(C H4 O)'
_chemical_formula_sum            'C30 H32 N3 Ni O4 P S'
_chemical_formula_weight         620.33

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   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'

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

_cell_length_a                   14.8310(6)
_cell_length_b                   7.6772(3)
_cell_length_c                   25.8278(9)
_cell_angle_alpha                90
_cell_angle_beta                 93.346(1)
_cell_angle_gamma                90
_cell_volume                     2935.75(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.045
_exptl_crystal_size_mid          0.034
_exptl_crystal_size_min          0.032
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1296
_exptl_absorpt_coefficient_mu    0.826
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6305
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2002'

_exptl_special_details           ?

_diffrn_ambient_temperature      133(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi- + omega-scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16312
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_sigmaI/netI    0.0339
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         2.67
_diffrn_reflns_theta_max         27.45
_reflns_number_total             6439
_reflns_number_gt                5537
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       COLLECT
_computing_cell_refinement       DENZO
_computing_data_reduction        DENZO
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXL-97

_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)+(0.0432P)²+5.2222P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6439
_refine_ls_number_parameters     450
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0478
_refine_ls_wR_factor_ref         0.1226
_refine_ls_wR_factor_gt          0.1153
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_restrained_S_all      1.124
_refine_ls_shift/su_max          0.010
_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 0.60612(2) 0.19025(5) 0.693797(14) 0.02057(11) Uani 1 1 d . . .
S1 S 0.54141(5) 0.17680(9) 0.76510(3) 0.02355(16) Uani 1 1 d . . .
P1 P 0.50058(5) 0.36389(9) 0.66009(3) 0.02021(16) Uani 1 1 d . . .
O1 O 0.65287(13) 0.1898(3) 0.62860(8) 0.0254(4) Uani 1 1 d . . .
O2 O 0.72368(15) 0.3462(3) 0.48923(8) 0.0324(5) Uani 1 1 d . . .
N1 N 0.6058(2) -0.0099(4) 0.84578(11) 0.0357(7) Uani 1 1 d . . .
H1N1 H 0.552(3) -0.007(5) 0.8543(14) 0.034(10) Uiso 1 1 d . . .
H2N1 H 0.636(3) -0.097(5) 0.8593(15) 0.039(10) Uiso 1 1 d . . .
N2 N 0.69386(17) -0.0151(3) 0.77546(10) 0.0285(5) Uani 1 1 d . . .
N3 N 0.69934(16) 0.0529(3) 0.72550(9) 0.0235(5) Uani 1 1 d . . .
C1 C 0.6207(2) 0.0375(4) 0.79645(11) 0.0261(6) Uani 1 1 d . . .
C2 C 0.7753(2) 0.0175(4) 0.70489(12) 0.0255(6) Uani 1 1 d . . .
H2 H 0.819(2) -0.043(5) 0.7236(13) 0.031(9) Uiso 1 1 d . . .
C3 C 0.79879(19) 0.0705(4) 0.65388(12) 0.0252(6) Uani 1 1 d . . .
C4 C 0.8866(2) 0.0365(4) 0.63962(12) 0.0295(6) Uani 1 1 d . . .
H4 H 0.926(2) -0.016(4) 0.6650(13) 0.026(8) Uiso 1 1 d . . .
C5 C 0.9171(2) 0.0827(4) 0.59139(12) 0.0298(6) Uani 1 1 d . . .
C6 C 0.8561(2) 0.1637(4) 0.55634(12) 0.0275(6) Uani 1 1 d . . .
H6 H 0.873(2) 0.196(4) 0.5273(14) 0.025(9) Uiso 1 1 d . . .
C7 C 0.7670(2) 0.2001(4) 0.56879(11) 0.0251(6) Uani 1 1 d . . .
C8 C 0.73601(19) 0.1537(4) 0.61804(11) 0.0229(6) Uani 1 1 d . . .
C9 C 1.0142(2) 0.0484(5) 0.57900(14) 0.0423(9) Uani 1 1 d . . .
H9B H 1.0246 0.0936 0.5444 0.063 Uiso 1 1 calc R . .
H9A H 1.0257 -0.0773 0.5799 0.063 Uiso 1 1 calc R . .
H9C H 1.0549 0.1066 0.6047 0.063 Uiso 1 1 calc R . .
C10 C 0.7043(2) 0.2890(4) 0.53151(12) 0.0283(6) Uani 1 1 d . . .
H10 H 0.640(2) 0.301(4) 0.5415(14) 0.032(9) Uiso 1 1 d . . .
C11 C 0.54886(19) 0.5227(4) 0.61719(11) 0.0220(6) Uani 1 1 d . . .
C12 C 0.5047(2) 0.5802(4) 0.57099(12) 0.0274(6) Uani 1 1 d . . .
H12 H 0.448(2) 0.533(4) 0.5608(13) 0.025(8) Uiso 1 1 d . . .
C13 C 0.5466(2) 0.7008(4) 0.54009(13) 0.0332(7) Uani 1 1 d . . .
H13 H 0.519(3) 0.735(5) 0.5103(15) 0.038(10) Uiso 1 1 d . . .
C14 C 0.6312(2) 0.7647(4) 0.55464(13) 0.0356(7) Uani 1 1 d . . .
H14 H 0.657(3) 0.840(5) 0.5341(14) 0.036(10) Uiso 1 1 d . . .
C15 C 0.6756(2) 0.7079(4) 0.60018(13) 0.0328(7) Uani 1 1 d . . .
H15 H 0.733(2) 0.750(5) 0.6103(13) 0.029(9) Uiso 1 1 d . . .
C16 C 0.6351(2) 0.5876(4) 0.63149(12) 0.0268(6) Uani 1 1 d . . .
H16 H 0.666(2) 0.546(4) 0.6606(12) 0.018(8) Uiso 1 1 d . . .
C17 C 0.43749(19) 0.4912(4) 0.70558(11) 0.0225(6) Uani 1 1 d . . .
C18 C 0.3656(2) 0.4134(4) 0.72991(12) 0.0278(6) Uani 1 1 d . . .
H18 H 0.347(2) 0.292(4) 0.7207(12) 0.024(8) Uiso 1 1 d . . .
C19 C 0.3225(2) 0.5022(4) 0.76824(13) 0.0311(7) Uani 1 1 d . . .
H19 H 0.277(2) 0.453(4) 0.7833(13) 0.028(9) Uiso 1 1 d . . .
C20 C 0.3504(2) 0.6680(4) 0.78306(13) 0.0331(7) Uani 1 1 d . . .
H20 H 0.325(2) 0.724(5) 0.8089(14) 0.033(9) Uiso 1 1 d . . .
C21 C 0.4207(2) 0.7463(5) 0.75890(14) 0.0362(7) Uani 1 1 d . . .
H21 H 0.437(3) 0.861(6) 0.7663(16) 0.052(12) Uiso 1 1 d . . .
C22 C 0.4645(2) 0.6588(4) 0.72028(13) 0.0300(7) Uani 1 1 d . . .
H22 H 0.516(3) 0.710(5) 0.7059(14) 0.039(10) Uiso 1 1 d . . .
C23 C 0.41422(19) 0.2409(4) 0.62319(11) 0.0224(5) Uani 1 1 d . . .
C24 C 0.4286(2) 0.0659(4) 0.61306(13) 0.0306(7) Uani 1 1 d . . .
H24 H 0.484(2) 0.012(5) 0.6235(14) 0.037(10) Uiso 1 1 d . . .
C25 C 0.3610(2) -0.0336(4) 0.58799(14) 0.0365(8) Uani 1 1 d . . .
H25 H 0.366(2) -0.150(5) 0.5821(14) 0.038(10) Uiso 1 1 d . . .
C26 C 0.2785(2) 0.0403(5) 0.57342(13) 0.0321(7) Uani 1 1 d . . .
H26 H 0.236(3) -0.022(5) 0.5611(15) 0.043(11) Uiso 1 1 d . . .
C27 C 0.2637(2) 0.2152(4) 0.58250(12) 0.0308(7) Uani 1 1 d . . .
H27 H 0.206(3) 0.272(5) 0.5750(14) 0.039(10) Uiso 1 1 d . . .
C28 C 0.3309(2) 0.3153(4) 0.60720(12) 0.0281(6) Uani 1 1 d . . .
H28 H 0.317(2) 0.437(5) 0.6152(13) 0.028(9) Uiso 1 1 d . . .
O1M O 0.9208(2) 0.4922(5) 0.37803(13) 0.0682(9) Uani 1 1 d . . .
H1M H 0.9290 0.4779 0.4102 0.102 Uiso 1 1 calc R . .
C1M C 0.8560(3) 0.3696(6) 0.35774(18) 0.0526(10) Uani 1 1 d . . .
H1M1 H 0.8251 0.3165 0.3863 0.079 Uiso 1 1 calc R . .
H1M2 H 0.8866 0.2788 0.3387 0.079 Uiso 1 1 calc R . .
H1M3 H 0.8117 0.4291 0.3343 0.079 Uiso 1 1 calc R . .
O2M O 0.8825(2) 0.5135(5) 0.47866(13) 0.0687(9) Uani 1 1 d . . .
H2M H 0.8306 0.4698 0.4787 0.103 Uiso 1 1 calc R . .
C2M C 0.8959(3) 0.6371(7) 0.52302(17) 0.0621(12) Uani 1 1 d . . .
H2M1 H 0.9606 0.6577 0.5302 0.093 Uiso 1 1 calc R . .
H2M2 H 0.8701 0.5872 0.5538 0.093 Uiso 1 1 calc R . .
H2M3 H 0.8657 0.7477 0.5142 0.093 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1 1.858(2) . ?
Ni1 N3 1.887(2) . ?
Ni1 S1 2.1282(8) . ?
Ni1 P1 2.1968(8) . ?
S1 C1 1.752(3) . ?
P1 C23 1.816(3) . ?
P1 C11 1.822(3) . ?
P1 C17 1.828(3) . ?
O1 C8 1.308(3) . ?
O2 C10 1.227(4) . ?
N1 C1 1.356(4) . ?
N1 H1N1 0.85(4) . ?
N1 H2N1 0.87(4) . ?
N2 C1 1.305(4) . ?
N2 N3 1.399(3) . ?
N3 C2 1.303(4) . ?
C2 C3 1.441(4) . ?
C2 H2 0.91(4) . ?
C3 C4 1.398(4) . ?
C3 C8 1.425(4) . ?
C4 C5 1.396(4) . ?
C4 H4 0.95(3) . ?
C5 C6 1.389(4) . ?
C5 C9 1.516(4) . ?
C6 C7 1.406(4) . ?
C6 H6 0.84(3) . ?
C7 C8 1.423(4) . ?
C7 C10 1.467(4) . ?
C9 H9B 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10 1.00(4) . ?
C11 C12 1.399(4) . ?
C11 C16 1.402(4) . ?
C12 C13 1.392(4) . ?
C12 H12 0.94(3) . ?
C13 C14 1.379(5) . ?
C13 H13 0.89(4) . ?
C14 C15 1.384(5) . ?
C14 H14 0.89(4) . ?
C15 C16 1.388(4) . ?
C15 H15 0.93(4) . ?
C16 H16 0.91(3) . ?
C17 C22 1.394(4) . ?
C17 C18 1.403(4) . ?
C18 C19 1.388(4) . ?
C18 H18 0.99(3) . ?
C19 C20 1.385(5) . ?
C19 H19 0.89(3) . ?
C20 C21 1.384(5) . ?
C20 H20 0.90(4) . ?
C21 C22 1.394(5) . ?
C21 H21 0.93(4) . ?
C22 H22 0.95(4) . ?
C23 C24 1.388(4) . ?
C23 C28 1.401(4) . ?
C24 C25 1.390(4) . ?
C24 H24 0.94(4) . ?
C25 C26 1.381(5) . ?
C25 H25 0.91(4) . ?
C26 C27 1.382(5) . ?
C26 H26 0.84(4) . ?
C27 C28 1.385(4) . ?
C27 H27 0.96(4) . ?
C28 H28 0.98(3) . ?
O1M C1M 1.423(5) . ?
O1M H1M 0.8400 . ?
C1M H1M1 0.9800 . ?
C1M H1M2 0.9800 . ?
C1M H1M3 0.9800 . ?
O2M C2M 1.492(6) . ?
O2M H2M 0.8400 . ?
C2M H2M1 0.9800 . ?
C2M H2M2 0.9800 . ?
C2M H2M3 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni1 N3 95.13(10) . . ?
O1 Ni1 S1 174.29(7) . . ?
N3 Ni1 S1 87.33(8) . . ?
O1 Ni1 P1 86.39(6) . . ?
N3 Ni1 P1 176.35(8) . . ?
S1 Ni1 P1 91.46(3) . . ?
C1 S1 Ni1 96.04(10) . . ?
C23 P1 C11 108.60(13) . . ?
C23 P1 C17 104.09(13) . . ?
C11 P1 C17 105.50(13) . . ?
C23 P1 Ni1 110.91(10) . . ?
C11 P1 Ni1 110.54(9) . . ?
C17 P1 Ni1 116.72(9) . . ?
C8 O1 Ni1 126.54(18) . . ?
C1 N1 H1N1 116(3) . . ?
C1 N1 H2N1 119(3) . . ?
H1N1 N1 H2N1 113(4) . . ?
C1 N2 N3 111.2(2) . . ?
C2 N3 N2 113.4(2) . . ?
C2 N3 Ni1 124.7(2) . . ?
N2 N3 Ni1 121.89(19) . . ?
N2 C1 N1 119.5(3) . . ?
N2 C1 S1 123.3(2) . . ?
N1 C1 S1 117.2(2) . . ?
N3 C2 C3 125.1(3) . . ?
N3 C2 H2 119(2) . . ?
C3 C2 H2 115(2) . . ?
C4 C3 C8 119.7(3) . . ?
C4 C3 C2 117.8(3) . . ?
C8 C3 C2 122.5(3) . . ?
C5 C4 C3 122.9(3) . . ?
C5 C4 H4 121(2) . . ?
C3 C4 H4 117(2) . . ?
C6 C5 C4 117.6(3) . . ?
C6 C5 C9 122.1(3) . . ?
C4 C5 C9 120.4(3) . . ?
C5 C6 C7 121.7(3) . . ?
C5 C6 H6 119(2) . . ?
C7 C6 H6 119(2) . . ?
C6 C7 C8 120.8(3) . . ?
C6 C7 C10 120.7(3) . . ?
C8 C7 C10 118.5(3) . . ?
O1 C8 C7 119.4(2) . . ?
O1 C8 C3 123.2(3) . . ?
C7 C8 C3 117.4(3) . . ?
C5 C9 H9B 109.5 . . ?
C5 C9 H9A 109.5 . . ?
H9B C9 H9A 109.5 . . ?
C5 C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
O2 C10 C7 125.3(3) . . ?
O2 C10 H10 118(2) . . ?
C7 C10 H10 117(2) . . ?
C12 C11 C16 119.1(3) . . ?
C12 C11 P1 123.3(2) . . ?
C16 C11 P1 117.5(2) . . ?
C13 C12 C11 119.8(3) . . ?
C13 C12 H12 121(2) . . ?
C11 C12 H12 119(2) . . ?
C14 C13 C12 120.7(3) . . ?
C14 C13 H13 120(3) . . ?
C12 C13 H13 119(3) . . ?
C13 C14 C15 120.0(3) . . ?
C13 C14 H14 119(2) . . ?
C15 C14 H14 121(2) . . ?
C14 C15 C16 120.3(3) . . ?
C14 C15 H15 121(2) . . ?
C16 C15 H15 119(2) . . ?
C15 C16 C11 120.2(3) . . ?
C15 C16 H16 120(2) . . ?
C11 C16 H16 120(2) . . ?
C22 C17 C18 119.0(3) . . ?
C22 C17 P1 121.3(2) . . ?
C18 C17 P1 119.4(2) . . ?
C19 C18 C17 120.3(3) . . ?
C19 C18 H18 120.1(19) . . ?
C17 C18 H18 119.6(19) . . ?
C20 C19 C18 120.4(3) . . ?
C20 C19 H19 120(2) . . ?
C18 C19 H19 120(2) . . ?
C21 C20 C19 119.7(3) . . ?
C21 C20 H20 119(2) . . ?
C19 C20 H20 121(2) . . ?
C20 C21 C22 120.5(3) . . ?
C20 C21 H21 121(3) . . ?
C22 C21 H21 119(3) . . ?
C17 C22 C21 120.1(3) . . ?
C17 C22 H22 120(2) . . ?
C21 C22 H22 120(2) . . ?
C24 C23 C28 118.8(3) . . ?
C24 C23 P1 119.4(2) . . ?
C28 C23 P1 121.7(2) . . ?
C23 C24 C25 120.4(3) . . ?
C23 C24 H24 121(2) . . ?
C25 C24 H24 119(2) . . ?
C26 C25 C24 120.3(3) . . ?
C26 C25 H25 116(2) . . ?
C24 C25 H25 123(2) . . ?
C25 C26 C27 120.0(3) . . ?
C25 C26 H26 120(3) . . ?
C27 C26 H26 119(3) . . ?
C26 C27 C28 120.0(3) . . ?
C26 C27 H27 123(2) . . ?
C28 C27 H27 116(2) . . ?
C27 C28 C23 120.6(3) . . ?
C27 C28 H28 118(2) . . ?
C23 C28 H28 121(2) . . ?
C1M O1M H1M 109.5 . . ?
O1M C1M H1M1 109.5 . . ?
O1M C1M H1M2 109.5 . . ?
H1M1 C1M H1M2 109.5 . . ?
O1M C1M H1M3 109.5 . . ?
H1M1 C1M H1M3 109.5 . . ?
H1M2 C1M H1M3 109.5 . . ?
C2M O2M H2M 109.5 . . ?
O2M C2M H2M1 109.5 . . ?
O2M C2M H2M2 109.5 . . ?
H2M1 C2M H2M2 109.5 . . ?
O2M C2M H2M3 109.5 . . ?
H2M1 C2M H2M3 109.5 . . ?
H2M2 C2M H2M3 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.961
_diffrn_reflns_theta_full        27.45
_diffrn_measured_fraction_theta_full 0.961
_refine_diff_density_max         0.845
_refine_diff_density_min         -0.709
_refine_diff_density_rms         0.075


































































































































































































































































































































































































































































































































































































































































































































































































































































































































































































































































































































