# Electronic Supplementary Material (ESI) for Polymer Chemistry.
# This journal is © The Royal Society of Chemistry 2017

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

data_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1544968'
_audit_update_record             
;
2017-04-20 deposited with the CCDC.
2017-06-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H26 N2 O2 S2'
_chemical_formula_sum            'C27 H26 N2 O2 S2'
_chemical_formula_weight         474.62

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'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   P212121

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

_cell_length_a                   5.7227(18)
_cell_length_b                   12.3378(37)
_cell_length_c                   33.1425(107)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2340.2
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7745
_cell_measurement_theta_min      1.7612
_cell_measurement_theta_max      27.4546

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1000
_exptl_absorpt_coefficient_mu    0.256
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.9459
_exptl_absorpt_correction_T_max  0.9823
_exptl_absorpt_process_details   'The Rigaku Corporation, Tokyo, Japan'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(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  
;
Mercury2 (2x2 bin mode)
;
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            23427
_diffrn_reflns_av_R_equivalents  0.0948
_diffrn_reflns_av_sigmaI/netI    0.0800
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_theta_min         1.76
_diffrn_reflns_theta_max         27.46
_reflns_number_total             5305
_reflns_number_gt                4601
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_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)+(0.1008P)²+1.2065P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.05(12)
_refine_ls_number_reflns         5305
_refine_ls_number_parameters     336
_refine_ls_number_restraints     177
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0645
_refine_ls_wR_factor_ref         0.1703
_refine_ls_wR_factor_gt          0.1613
_refine_ls_goodness_of_fit_ref   0.920
_refine_ls_restrained_S_all      0.905
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.002

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
O2 O 1.0970(5) -0.15495(19) 0.30331(6) 0.0304(6) Uani 1 1 d . . .
H2 H 0.9928 -0.1962 0.2960 0.046 Uiso 1 1 calc R . .
O1 O 0.2803(4) -0.32602(19) 0.15817(7) 0.0308(6) Uani 1 1 d . . .
H1 H 0.3747 -0.3480 0.1749 0.046 Uiso 1 1 calc R . .
N2 N 0.7034(5) -0.2549(2) 0.30603(8) 0.0264(6) Uani 1 1 d . . .
C12 C 0.8099(6) -0.3773(3) 0.23065(9) 0.0241(7) Uani 1 1 d . . .
H12A H 0.9212 -0.3245 0.2407 0.029 Uiso 1 1 calc R . .
H12B H 0.8969 -0.4353 0.2178 0.029 Uiso 1 1 calc R . .
C13 C 0.6678(6) -0.4238(3) 0.26638(9) 0.0221(7) Uani 1 1 d . . .
C8 C 0.3611(6) -0.2331(3) 0.14124(9) 0.0240(7) Uani 1 1 d . . .
C14 C 0.4855(6) -0.5052(3) 0.25122(10) 0.0263(7) Uani 1 1 d . . .
H14A H 0.3996 -0.5336 0.2737 0.039 Uiso 1 1 calc R . .
H14B H 0.5628 -0.5634 0.2374 0.039 Uiso 1 1 calc R . .
H14C H 0.3801 -0.4695 0.2330 0.039 Uiso 1 1 calc R . .
C11 C 0.7246(6) -0.2386(3) 0.18361(9) 0.0239(7) Uani 1 1 d . . .
H11 H 0.8676 -0.2079 0.1905 0.029 Uiso 1 1 calc R . .
C18 C 0.8262(6) -0.1355(3) 0.35865(9) 0.0235(7) Uani 1 1 d . . .
C21 C 1.1940(6) -0.0372(3) 0.35726(10) 0.0263(7) Uani 1 1 d . . .
H21 H 1.3365 -0.0221 0.3450 0.032 Uiso 1 1 calc R . .
C15 C 0.8404(6) -0.4820(3) 0.29470(9) 0.0287(7) Uani 1 1 d . . .
H15A H 0.7567 -0.5123 0.3171 0.043 Uiso 1 1 calc R . .
H15B H 0.9541 -0.4311 0.3044 0.043 Uiso 1 1 calc R . .
H15C H 0.9180 -0.5390 0.2802 0.043 Uiso 1 1 calc R . .
C10 C 0.5757(6) -0.1868(3) 0.15274(9) 0.0225(7) Uani 1 1 d . . .
C9 C 0.6466(6) -0.0891(3) 0.13466(9) 0.0244(7) Uani 1 1 d . . .
H9 H 0.7890 -0.0588 0.1421 0.029 Uiso 1 1 calc R . .
C16 C 0.5388(6) -0.3332(3) 0.28904(10) 0.0265(7) Uani 1 1 d . . .
H16A H 0.4334 -0.2964 0.2707 0.032 Uiso 1 1 calc R . .
H16B H 0.4461 -0.3646 0.3106 0.032 Uiso 1 1 calc R . .
C22 C 1.1374(6) 0.0118(3) 0.39322(10) 0.0271(7) Uani 1 1 d . . .
H22 H 1.2412 0.0611 0.4046 0.033 Uiso 1 1 calc R . .
C6 C 0.2979(6) -0.0851(3) 0.09526(10) 0.0272(7) Uani 1 1 d . . .
H6 H 0.2039 -0.0512 0.0761 0.033 Uiso 1 1 calc R . .
C7 C 0.2244(6) -0.1814(3) 0.11212(10) 0.0293(8) Uani 1 1 d . . .
H7 H 0.0834 -0.2120 0.1041 0.035 Uiso 1 1 calc R . .
C19 C 0.7765(6) -0.0854(3) 0.39565(9) 0.0246(7) Uani 1 1 d . . .
H19 H 0.6380 -0.1026 0.4089 0.030 Uiso 1 1 calc R . .
C17 C 0.6644(6) -0.2136(3) 0.34090(10) 0.0250(7) Uani 1 1 d . . .
H17 H 0.5310 -0.2336 0.3551 0.030 Uiso 1 1 calc R . .
C20 C 1.0384(6) -0.1098(3) 0.33900(9) 0.0247(7) Uani 1 1 d . . .
N1 N 0.6571(5) -0.3257(2) 0.20091(8) 0.0230(6) Uani 1 1 d . . .
C27 C 0.6901(8) 0.1072(3) 0.51494(11) 0.0373(10) Uani 0.965(4) 1 d P . .
H27 H 0.5940 0.1218 0.5369 0.045 Uiso 0.965(4) 1 calc PR . .
C26 C 0.8961(8) 0.1534(3) 0.50932(11) 0.0324(9) Uani 0.965(4) 1 d P . .
H26 H 0.9588 0.2041 0.5271 0.039 Uiso 0.965(4) 1 calc PR . .
C25 C 1.0138(5) 0.1187(2) 0.47364(8) 0.0159(6) Uani 0.965(4) 1 d P . .
H25 H 1.1614 0.1419 0.4657 0.019 Uiso 0.965(4) 1 calc PR . .
S2 S 0.6197(2) 0.01813(9) 0.47766(3) 0.0390(3) Uani 0.965(4) 1 d P . .
C1 C 0.793(3) 0.2302(12) 0.0634(5) 0.028(2) Uani 0.677(4) 1 d PDU A 1
H1A H 0.8953 0.2874 0.0588 0.033 Uiso 0.677(4) 1 calc PR A 1
C2 C 0.591(3) 0.2140(11) 0.0426(5) 0.0302(19) Uani 0.677(4) 1 d PDU A 1
H2A H 0.5406 0.2596 0.0220 0.036 Uiso 0.677(4) 1 calc PR A 1
C3 C 0.461(3) 0.1171(16) 0.0558(5) 0.032(3) Uani 0.677(4) 1 d PDU A 1
H3 H 0.3188 0.0940 0.0452 0.038 Uiso 0.677(4) 1 calc PR A 1
S1 S 0.8335(6) 0.1317(3) 0.09924(11) 0.0277(5) Uani 0.677(4) 1 d PDU A 1
C2A C 0.810(6) 0.220(2) 0.0715(10) 0.031(5) Uani 0.323(4) 1 d PDU A 2
H2A1 H 0.9326 0.2689 0.0737 0.037 Uiso 0.323(4) 1 calc PR A 2
C1A C 0.634(6) 0.231(2) 0.0450(10) 0.038(5) Uani 0.323(4) 1 d PDU A 2
H1A1 H 0.6215 0.2883 0.0268 0.045 Uiso 0.323(4) 1 calc PR A 2
C3A C 0.789(5) 0.121(3) 0.0969(10) 0.038(5) Uani 0.323(4) 1 d PDU A 2
H3A H 0.8952 0.0991 0.1165 0.046 Uiso 0.323(4) 1 calc PR A 2
S1A S 0.4370(18) 0.1274(10) 0.0487(3) 0.0314(14) Uani 0.323(4) 1 d PDU A 2
C4 C 0.5839(6) 0.0654(3) 0.08658(9) 0.0262(7) Uani 1 1 d DU . .
C5 C 0.5104(6) -0.0367(3) 0.10613(9) 0.0237(7) Uani 1 1 d . A .
C23 C 0.9273(6) -0.0108(3) 0.41322(9) 0.0250(7) Uani 1 1 d . . .
C24 C 0.8727(7) 0.0428(3) 0.45169(9) 0.0239(7) Uani 0.965(4) 1 d P . .


_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
O2 C20 1.350(4) . ?
O2 H2 0.8200 . ?
O1 C8 1.358(4) . ?
O1 H1 0.8200 . ?
N2 C17 1.283(4) . ?
N2 C16 1.462(4) . ?
C12 N1 1.463(4) . ?
C12 C13 1.547(4) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C14 1.533(5) . ?
C13 C16 1.535(4) . ?
C13 C15 1.540(4) . ?
C8 C7 1.396(5) . ?
C8 C10 1.407(5) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C11 N1 1.278(4) . ?
C11 C10 1.477(4) . ?
C11 H11 0.9300 . ?
C18 C19 1.403(4) . ?
C18 C20 1.414(5) . ?
C18 C17 1.459(5) . ?
C21 C22 1.375(5) . ?
C21 C20 1.400(5) . ?
C21 H21 0.9300 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C10 C9 1.406(4) . ?
C9 C5 1.385(4) . ?
C9 H9 0.9300 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C22 C23 1.401(5) . ?
C22 H22 0.9300 . ?
C6 C7 1.379(5) . ?
C6 C5 1.402(5) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C19 C23 1.389(5) . ?
C19 H19 0.9300 . ?
C17 H17 0.9300 . ?
C27 C26 1.323(6) . ?
C27 S2 1.702(4) . ?
C27 H27 0.9300 . ?
C26 C25 1.427(5) . ?
C26 H26 0.9300 . ?
C25 C24 1.434(4) . ?
C25 H25 0.9300 . ?
S2 C24 1.711(4) . ?
C1 C2 1.357(9) . ?
C1 S1 1.715(10) . ?
C1 H1A 0.9300 . ?
C2 C3 1.48(2) . ?
C2 H2A 0.9300 . ?
C3 C4 1.395(13) . ?
C3 H3 0.9300 . ?
S1 C4 1.699(4) . ?
C2A C1A 1.341(15) . ?
C2A C3A 1.49(3) . ?
C2A H2A1 0.9300 . ?
C1A S1A 1.711(18) . ?
C1A H1A1 0.9300 . ?
C3A C4 1.399(18) . ?
C3A H3A 0.9300 . ?
S1A C4 1.695(8) . ?
C4 C5 1.478(5) . ?
C23 C24 1.470(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
C20 O2 H2 109.5 . . ?
C8 O1 H1 109.5 . . ?
C17 N2 C16 119.8(3) . . ?
N1 C12 C13 111.3(3) . . ?
N1 C12 H12A 109.4 . . ?
C13 C12 H12A 109.4 . . ?
N1 C12 H12B 109.4 . . ?
C13 C12 H12B 109.4 . . ?
H12A C12 H12B 108.0 . . ?
C14 C13 C16 108.0(3) . . ?
C14 C13 C15 109.3(3) . . ?
C16 C13 C15 110.5(3) . . ?
C14 C13 C12 110.5(2) . . ?
C16 C13 C12 110.9(3) . . ?
C15 C13 C12 107.6(3) . . ?
O1 C8 C7 118.7(3) . . ?
O1 C8 C10 121.9(3) . . ?
C7 C8 C10 119.4(3) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N1 C11 C10 120.0(3) . . ?
N1 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
C19 C18 C20 118.5(3) . . ?
C19 C18 C17 121.0(3) . . ?
C20 C18 C17 120.5(3) . . ?
C22 C21 C20 120.4(3) . . ?
C22 C21 H21 119.8 . . ?
C20 C21 H21 119.8 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C9 C10 C8 119.0(3) . . ?
C9 C10 C11 120.0(3) . . ?
C8 C10 C11 121.0(3) . . ?
C5 C9 C10 121.9(3) . . ?
C5 C9 H9 119.0 . . ?
C10 C9 H9 119.0 . . ?
N2 C16 C13 111.1(3) . . ?
N2 C16 H16A 109.4 . . ?
C13 C16 H16A 109.4 . . ?
N2 C16 H16B 109.4 . . ?
C13 C16 H16B 109.4 . . ?
H16A C16 H16B 108.0 . . ?
C21 C22 C23 121.6(3) . . ?
C21 C22 H22 119.2 . . ?
C23 C22 H22 119.2 . . ?
C7 C6 C5 121.8(3) . . ?
C7 C6 H6 119.1 . . ?
C5 C6 H6 119.1 . . ?
C6 C7 C8 120.2(3) . . ?
C6 C7 H7 119.9 . . ?
C8 C7 H7 119.9 . . ?
C23 C19 C18 122.2(3) . . ?
C23 C19 H19 118.9 . . ?
C18 C19 H19 118.9 . . ?
N2 C17 C18 121.0(3) . . ?
N2 C17 H17 119.5 . . ?
C18 C17 H17 119.5 . . ?
O2 C20 C21 119.0(3) . . ?
O2 C20 C18 121.6(3) . . ?
C21 C20 C18 119.4(3) . . ?
C11 N1 C12 119.1(3) . . ?
C26 C27 S2 112.8(3) . . ?
C26 C27 H27 123.6 . . ?
S2 C27 H27 123.6 . . ?
C27 C26 C25 114.1(3) . . ?
C27 C26 H26 123.0 . . ?
C25 C26 H26 123.0 . . ?
C26 C25 C24 110.5(3) . . ?
C26 C25 H25 124.7 . . ?
C24 C25 H25 124.7 . . ?
C27 S2 C24 92.87(19) . . ?
C2 C1 S1 111.3(9) . . ?
C2 C1 H1A 124.4 . . ?
S1 C1 H1A 124.4 . . ?
C1 C2 C3 113.5(10) . . ?
C1 C2 H2A 123.3 . . ?
C3 C2 H2A 123.3 . . ?
C4 C3 C2 109.3(13) . . ?
C4 C3 H3 125.3 . . ?
C2 C3 H3 125.3 . . ?
C4 S1 C1 93.2(4) . . ?
C1A C2A C3A 113.2(17) . . ?
C1A C2A H2A1 123.4 . . ?
C3A C2A H2A1 123.4 . . ?
C2A C1A S1A 111.7(16) . . ?
C2A C1A H1A1 124.1 . . ?
S1A C1A H1A1 124.1 . . ?
C4 C3A C2A 109.3(15) . . ?
C4 C3A H3A 125.3 . . ?
C2A C3A H3A 125.3 . . ?
C4 S1A C1A 93.6(8) . . ?
C3 C4 C3A 112.2(19) . . ?
C3 C4 C5 124.5(9) . . ?
C3A C4 C5 123.2(12) . . ?
C3 C4 S1A 0.8(13) . . ?
C3A C4 S1A 112.1(9) . . ?
C5 C4 S1A 124.7(5) . . ?
C3 C4 S1 112.7(9) . . ?
C3A C4 S1 0.4(14) . . ?
C5 C4 S1 122.8(3) . . ?
S1A C4 S1 112.5(5) . . ?
C9 C5 C6 117.7(3) . . ?
C9 C5 C4 122.5(3) . . ?
C6 C5 C4 119.8(3) . . ?
C19 C23 C22 117.8(3) . . ?
C19 C23 C24 122.0(3) . . ?
C22 C23 C24 120.2(3) . . ?
C25 C24 C23 127.9(3) . . ?
C25 C24 S2 109.7(2) . . ?
C23 C24 S2 122.4(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C12 C13 C14 57.4(3) . . . . ?
N1 C12 C13 C16 -62.4(3) . . . . ?
N1 C12 C13 C15 176.7(3) . . . . ?
O1 C8 C10 C9 -178.6(3) . . . . ?
C7 C8 C10 C9 0.3(5) . . . . ?
O1 C8 C10 C11 0.8(5) . . . . ?
C7 C8 C10 C11 179.6(3) . . . . ?
N1 C11 C10 C9 177.9(3) . . . . ?
N1 C11 C10 C8 -1.4(5) . . . . ?
C8 C10 C9 C5 0.5(5) . . . . ?
C11 C10 C9 C5 -178.8(3) . . . . ?
C17 N2 C16 C13 -141.7(3) . . . . ?
C14 C13 C16 N2 177.4(3) . . . . ?
C15 C13 C16 N2 57.9(4) . . . . ?
C12 C13 C16 N2 -61.4(4) . . . . ?
C20 C21 C22 C23 1.6(5) . . . . ?
C5 C6 C7 C8 0.8(5) . . . . ?
O1 C8 C7 C6 177.9(3) . . . . ?
C10 C8 C7 C6 -0.9(5) . . . . ?
C20 C18 C19 C23 0.7(5) . . . . ?
C17 C18 C19 C23 -180.0(3) . . . . ?
C16 N2 C17 C18 179.7(3) . . . . ?
C19 C18 C17 N2 176.1(3) . . . . ?
C20 C18 C17 N2 -4.6(5) . . . . ?
C22 C21 C20 O2 178.7(3) . . . . ?
C22 C21 C20 C18 -2.5(5) . . . . ?
C19 C18 C20 O2 -179.9(3) . . . . ?
C17 C18 C20 O2 0.8(5) . . . . ?
C19 C18 C20 C21 1.3(5) . . . . ?
C17 C18 C20 C21 -178.0(3) . . . . ?
C10 C11 N1 C12 178.4(3) . . . . ?
C13 C12 N1 C11 141.6(3) . . . . ?
S2 C27 C26 C25 -0.2(4) . . . . ?
C27 C26 C25 C24 1.7(4) . . . . ?
C26 C27 S2 C24 -1.1(3) . . . . ?
S1 C1 C2 C3 -0.2(10) . . . . ?
C1 C2 C3 C4 -0.8(15) . . . . ?
C2 C1 S1 C4 0.9(8) . . . . ?
C3A C2A C1A S1A 0.3(18) . . . . ?
C1A C2A C3A C4 -1(3) . . . . ?
C2A C1A S1A C4 0.5(18) . . . . ?
C2 C3 C4 C3A 2(3) . . . . ?
C2 C3 C4 C5 -177.6(9) . . . . ?
C2 C3 C4 S1A -79(94) . . . . ?
C2 C3 C4 S1 1.5(15) . . . . ?
C2A C3A C4 C3 1(3) . . . . ?
C2A C3A C4 C5 179.9(19) . . . . ?
C2A C3A C4 S1A 1(3) . . . . ?
C2A C3A C4 S1 162(100) . . . . ?
C1A S1A C4 C3 99(95) . . . . ?
C1A S1A C4 C3A -1(3) . . . . ?
C1A S1A C4 C5 -179.6(16) . . . . ?
C1A S1A C4 S1 -1.3(15) . . . . ?
C1 S1 C4 C3 -1.5(12) . . . . ?
C1 S1 C4 C3A -20(100) . . . . ?
C1 S1 C4 C5 177.7(7) . . . . ?
C1 S1 C4 S1A -0.6(8) . . . . ?
C10 C9 C5 C6 -0.7(5) . . . . ?
C10 C9 C5 C4 -179.3(3) . . . . ?
C7 C6 C5 C9 0.0(5) . . . . ?
C7 C6 C5 C4 178.7(3) . . . . ?
C3 C4 C5 C9 175.3(11) . . . . ?
C3A C4 C5 C9 -4(2) . . . . ?
S1A C4 C5 C9 174.4(6) . . . . ?
S1 C4 C5 C9 -3.7(5) . . . . ?
C3 C4 C5 C6 -3.3(12) . . . . ?
C3A C4 C5 C6 177(2) . . . . ?
S1A C4 C5 C6 -4.3(7) . . . . ?
S1 C4 C5 C6 177.6(3) . . . . ?
C18 C19 C23 C22 -1.5(5) . . . . ?
C18 C19 C23 C24 179.0(3) . . . . ?
C21 C22 C23 C19 0.4(5) . . . . ?
C21 C22 C23 C24 179.8(3) . . . . ?
C26 C25 C24 C23 179.0(3) . . . . ?
C26 C25 C24 S2 -2.4(3) . . . . ?
C19 C23 C24 C25 178.2(3) . . . . ?
C22 C23 C24 C25 -1.2(5) . . . . ?
C19 C23 C24 S2 -0.2(5) . . . . ?
C22 C23 C24 S2 -179.7(2) . . . . ?
C27 S2 C24 C25 2.0(3) . . . . ?
C27 S2 C24 C23 -179.3(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.46
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.423
_refine_diff_density_min         -0.354
_refine_diff_density_rms         0.062
####################################################################### 
# 
# 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_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1544970'
_audit_update_record             
;
2017-04-20 deposited with the CCDC.
2017-06-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C35 H28 N2 Ni O2 S4'
_chemical_formula_weight         695.54

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'
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   P21/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                   7.5151(37)
_cell_length_b                   35.3340(164)
_cell_length_c                   11.4224(55)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.44
_cell_angle_gamma                90.00
_cell_volume                     3032.9966(2000)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4607
_cell_measurement_theta_max      25.2014
_cell_measurement_theta_min      1.7290

_exptl_crystal_description       needle
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1440
_exptl_absorpt_coefficient_mu    0.953
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8703
_exptl_absorpt_correction_T_max  0.9720
_exptl_absorpt_process_details   'The Rigaku Corporation, Tokyo, Japan'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(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  
;
Mercury2 (2x2 bin mode)
;
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            20776
_diffrn_reflns_av_R_equivalents  0.1090
_diffrn_reflns_av_sigmaI/netI    0.0941
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.22
_diffrn_reflns_theta_max         25.03
_reflns_number_total             5274
_reflns_number_gt                3926
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_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)+(0.0524P)²+0.2608P] 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         5274
_refine_ls_number_parameters     474
_refine_ls_number_restraints     322
_refine_ls_R_factor_all          0.0852
_refine_ls_R_factor_gt           0.0570
_refine_ls_wR_factor_ref         0.1331
_refine_ls_wR_factor_gt          0.1216
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.025
_refine_ls_shift/su_max          0.035
_refine_ls_shift/su_mean         0.004

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 0.73802(7) 0.005241(13) -0.00049(4) 0.02462(18) Uani 1 1 d . . .
S2 S 0.67676(13) -0.20885(3) 0.17244(9) 0.0245(3) Uani 1 1 d . . .
S3 S 0.70503(13) 0.23701(3) 0.06419(9) 0.0253(3) Uani 1 1 d . B .
O2 O 0.7434(4) 0.04801(7) 0.0928(2) 0.0281(7) Uani 1 1 d . . .
O1 O 0.6881(4) -0.01818(7) 0.1414(2) 0.0298(7) Uani 1 1 d . . .
C26 C 0.7635(5) 0.16184(10) -0.0029(3) 0.0204(9) Uani 1 1 d . B .
C22 C 0.7939(5) 0.09495(10) -0.0556(3) 0.0211(9) Uani 1 1 d . . .
C23 C 0.7478(5) 0.08351(11) 0.0593(3) 0.0251(9) Uani 1 1 d . . .
N2 N 0.8273(4) 0.03092(9) -0.1316(3) 0.0245(8) Uani 1 1 d . . .
N1 N 0.6962(4) -0.03919(8) -0.0872(3) 0.0232(7) Uani 1 1 d . . .
C27 C 0.8033(5) 0.13380(10) -0.0830(3) 0.0220(9) Uani 1 1 d . . .
H27 H 0.8383 0.1410 -0.1595 0.026 Uiso 1 1 calc R . .
C12 C 0.7024(5) -0.05442(11) 0.1644(3) 0.0237(9) Uani 1 1 d . . .
C32 C 0.7560(5) 0.31272(10) 0.0067(3) 0.0235(9) Uani 1 1 d U . .
C9 C 0.7352(5) -0.13224(10) 0.2260(3) 0.0214(9) Uani 1 1 d . . .
C5 C 0.7387(5) -0.24305(10) 0.2753(3) 0.0238(9) Uani 1 1 d . . .
C24 C 0.7099(5) 0.11236(11) 0.1411(3) 0.0273(10) Uani 1 1 d . B .
H24 H 0.6803 0.1056 0.2190 0.033 Uiso 1 1 calc R . .
C14 C 0.7174(5) -0.12124(11) 0.1102(3) 0.0231(9) Uani 1 1 d . . .
H14 H 0.7133 -0.1400 0.0507 0.028 Uiso 1 1 calc R . .
C13 C 0.7054(5) -0.08302(11) 0.0787(3) 0.0233(9) Uani 1 1 d . . .
C8 C 0.7516(5) -0.17213(10) 0.2616(3) 0.0226(9) Uani 1 1 d . . .
C20 C 0.9140(5) 0.00701(11) -0.2220(3) 0.0292(10) Uani 1 1 d . . .
H20A H 1.0049 -0.0091 -0.1833 0.035 Uiso 1 1 calc R . .
H20B H 0.9763 0.0237 -0.2779 0.035 Uiso 1 1 calc R . .
C31 C 0.7767(5) 0.27351(10) -0.0258(3) 0.0211(9) Uani 1 1 d . B .
C7 C 0.8187(5) -0.18624(11) 0.3653(3) 0.0262(10) Uani 1 1 d . . .
H7 H 0.8648 -0.1706 0.4261 0.031 Uiso 1 1 calc R . .
C21 C 0.8436(5) 0.06744(11) -0.1418(3) 0.0241(9) Uani 1 1 d . . .
H21 H 0.8927 0.0767 -0.2126 0.029 Uiso 1 1 calc R . .
C16 C 0.6396(5) -0.03418(11) -0.2113(3) 0.0281(10) Uani 1 1 d . . .
H16A H 0.5365 -0.0168 -0.2140 0.034 Uiso 1 1 calc R . .
H16B H 0.5997 -0.0589 -0.2425 0.034 Uiso 1 1 calc R . .
C29 C 0.8544(5) 0.21893(11) -0.1282(3) 0.0243(9) Uani 1 1 d . B .
H29 H 0.9024 0.2048 -0.1913 0.029 Uiso 1 1 calc R . .
C6 C 0.8124(5) -0.22634(11) 0.3726(3) 0.0247(9) Uani 1 1 d . . .
H6 H 0.8550 -0.2402 0.4383 0.030 Uiso 1 1 calc R . .
C10 C 0.7344(5) -0.10384(11) 0.3121(3) 0.0253(9) Uani 1 1 d . . .
H10 H 0.7464 -0.1108 0.3922 0.030 Uiso 1 1 calc R . .
C30 C 0.8526(5) 0.25875(10) -0.1257(3) 0.0224(9) Uani 1 1 d . . .
H30 H 0.8990 0.2740 -0.1868 0.027 Uiso 1 1 calc R B .
C28 C 0.7806(5) 0.20228(10) -0.0313(3) 0.0209(9) Uani 1 1 d . . .
C25 C 0.7148(5) 0.14996(11) 0.1106(3) 0.0249(9) Uani 1 1 d . . .
H25 H 0.6845 0.1685 0.1673 0.030 Uiso 1 1 calc R B .
C15 C 0.6832(5) -0.07301(11) -0.0440(3) 0.0259(9) Uani 1 1 d . . .
H15 H 0.6570 -0.0930 -0.0971 0.031 Uiso 1 1 calc R . .
C11 C 0.7165(5) -0.06616(11) 0.2830(3) 0.0261(9) Uani 1 1 d . . .
H11 H 0.7136 -0.0477 0.3435 0.031 Uiso 1 1 calc R . .
C17 C 0.7856(5) -0.01857(11) -0.2908(3) 0.0281(10) Uani 1 1 d . . .
C1 C 0.7544(9) -0.35246(18) 0.2380(6) 0.0314(17) Uani 0.82 1 d PU A 1
H1 H 0.7824 -0.3785 0.2486 0.038 Uiso 0.82 1 calc PR A 1
C2 C 0.6510(10) -0.3391(2) 0.1496(6) 0.0323(18) Uani 0.82 1 d PU A 1
H2 H 0.5976 -0.3552 0.0927 0.039 Uiso 0.82 1 calc PR A 1
C3 C 0.628(3) -0.2985(5) 0.1485(17) 0.028(3) Uani 0.82 1 d PU A 1
H3 H 0.5625 -0.2845 0.0919 0.033 Uiso 0.82 1 calc PR A 1
S1 S 0.8296(3) -0.31661(5) 0.3295(2) 0.0306(5) Uani 0.82 1 d PU A 1
C1A C 0.675(5) -0.3466(11) 0.187(3) 0.020(5) Uani 0.18 1 d PU A 2
H1A H 0.6376 -0.3683 0.1442 0.025 Uiso 0.18 1 calc PR A 2
C2A C 0.797(4) -0.3465(9) 0.281(2) 0.023(5) Uani 0.18 1 d PU A 2
H2A H 0.8508 -0.3679 0.3175 0.027 Uiso 0.18 1 calc PR A 2
C3A C 0.824(6) -0.3067(11) 0.312(4) 0.028(6) Uani 0.18 1 d PU A 2
H3A H 0.9053 -0.2984 0.3704 0.033 Uiso 0.18 1 calc PR A 2
S1A S 0.610(3) -0.3038(6) 0.164(2) 0.028(3) Uani 0.18 1 d PU A 2
C4 C 0.7216(5) -0.28304(11) 0.2475(4) 0.0267(9) Uani 1 1 d U . .
C18 C 0.8994(6) -0.05010(12) -0.3429(4) 0.0424(12) Uani 1 1 d . . .
H18A H 0.9934 -0.0390 -0.3909 0.064 Uiso 1 1 calc R . .
H18B H 0.8245 -0.0666 -0.3917 0.064 Uiso 1 1 calc R . .
H18C H 0.9532 -0.0650 -0.2795 0.064 Uiso 1 1 calc R . .
C19 C 0.6945(6) 0.00378(12) -0.3889(4) 0.0422(12) Uani 1 1 d . . .
H19A H 0.6322 0.0256 -0.3555 0.063 Uiso 1 1 calc R . .
H19B H 0.6087 -0.0125 -0.4297 0.063 Uiso 1 1 calc R . .
H19C H 0.7841 0.0127 -0.4444 0.063 Uiso 1 1 calc R . .
S4 S 0.8374(6) 0.34857(8) -0.0785(4) 0.0286(6) Uani 0.78 1 d PU B 1
C33 C 0.675(3) 0.3284(6) 0.1044(16) 0.032(4) Uani 0.78 1 d PU B 1
H33 H 0.6191 0.3134 0.1627 0.038 Uiso 0.78 1 calc PR B 1
C34 C 0.6801(17) 0.3680(3) 0.1103(8) 0.029(2) Uani 0.78 1 d PU B 1
H34 H 0.6323 0.3826 0.1725 0.035 Uiso 0.78 1 calc PR B 1
C35 C 0.7626(15) 0.3829(3) 0.0158(8) 0.031(2) Uani 0.78 1 d PU B 1
H35 H 0.7774 0.4093 0.0031 0.037 Uiso 0.78 1 calc PR B 1
S4A S 0.652(3) 0.3281(5) 0.1166(15) 0.025(3) Uani 0.22 1 d PU B 2
C33A C 0.836(8) 0.3414(13) -0.067(5) 0.022(6) Uani 0.22 1 d PU B 2
H33A H 0.9044 0.3374 -0.1357 0.026 Uiso 0.22 1 calc PR B 2
C34A C 0.788(6) 0.3784(11) -0.013(3) 0.028(5) Uani 0.22 1 d PU B 2
H34A H 0.8281 0.4022 -0.0413 0.033 Uiso 0.22 1 calc PR B 2
C35A C 0.681(7) 0.3744(11) 0.082(3) 0.026(5) Uani 0.22 1 d PU B 2
H35A H 0.6289 0.3949 0.1234 0.032 Uiso 0.22 1 calc PR B 2


_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 O2 1.849(3) . ?
Ni1 O1 1.861(3) . ?
Ni1 N2 1.879(3) . ?
Ni1 N1 1.881(3) . ?
S2 C8 1.740(4) . ?
S2 C5 1.746(4) . ?
S3 C28 1.740(4) . ?
S3 C31 1.738(4) . ?
O2 C23 1.312(4) . ?
O1 C12 1.311(4) . ?
C26 C27 1.382(5) . ?
C26 C25 1.414(5) . ?
C26 C28 1.471(5) . ?
C22 C27 1.410(5) . ?
C22 C23 1.419(5) . ?
C22 C21 1.435(5) . ?
C23 C24 1.413(5) . ?
N2 C21 1.302(5) . ?
N2 C20 1.489(5) . ?
N1 C15 1.297(5) . ?
N1 C16 1.488(5) . ?
C27 H27 0.9500 . ?
C12 C13 1.407(5) . ?
C12 C11 1.421(5) . ?
C32 C33 1.392(17) . ?
C32 C31 1.443(5) . ?
C32 C33A 1.45(4) . ?
C32 S4A 1.581(16) . ?
C32 S4 1.714(5) . ?
C9 C14 1.384(5) . ?
C9 C10 1.405(5) . ?
C9 C8 1.472(5) . ?
C5 C6 1.371(5) . ?
C5 C4 1.454(5) . ?
C24 C25 1.374(5) . ?
C24 H24 0.9500 . ?
C14 C13 1.400(5) . ?
C14 H14 0.9500 . ?
C13 C15 1.453(5) . ?
C8 C7 1.377(5) . ?
C20 C17 1.534(5) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C31 C30 1.382(5) . ?
C7 C6 1.420(5) . ?
C7 H7 0.9500 . ?
C21 H21 0.9500 . ?
C16 C17 1.532(5) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C29 C28 1.374(5) . ?
C29 C30 1.407(5) . ?
C29 H29 0.9500 . ?
C6 H6 0.9500 . ?
C10 C11 1.379(5) . ?
C10 H10 0.9500 . ?
C30 H30 0.9500 . ?
C25 H25 0.9500 . ?
C15 H15 0.9500 . ?
C11 H11 0.9500 . ?
C17 C19 1.528(5) . ?
C17 C18 1.528(5) . ?
C1 C2 1.354(9) . ?
C1 S1 1.734(7) . ?
C1 H1 0.9500 . ?
C2 C3 1.443(17) . ?
C2 H2 0.9500 . ?
C3 C4 1.435(19) . ?
C3 H3 0.9500 . ?
S1 C4 1.712(4) . ?
C1A C2A 1.41(4) . ?
C1A S1A 1.61(4) . ?
C1A H1A 0.9500 . ?
C2A C3A 1.46(5) . ?
C2A H2A 0.9500 . ?
C3A C4 1.35(4) . ?
C3A H3A 0.9500 . ?
S1A C4 1.46(2) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
S4 C35 1.720(8) . ?
C33 C34 1.40(2) . ?
C33 H33 0.9500 . ?
C34 C35 1.355(12) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
S4A C35A 1.70(5) . ?
C33A C34A 1.49(6) . ?
C33A H33A 0.9500 . ?
C34A C35A 1.36(5) . ?
C34A H34A 0.9500 . ?
C35A H35A 0.9500 . ?

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 Ni1 O1 82.26(11) . . ?
O2 Ni1 N2 93.33(12) . . ?
O1 Ni1 N2 169.91(12) . . ?
O2 Ni1 N1 171.12(12) . . ?
O1 Ni1 N1 93.07(12) . . ?
N2 Ni1 N1 92.44(13) . . ?
C8 S2 C5 92.23(18) . . ?
C28 S3 C31 92.76(18) . . ?
C23 O2 Ni1 127.9(2) . . ?
C12 O1 Ni1 126.3(2) . . ?
C27 C26 C25 116.9(3) . . ?
C27 C26 C28 122.0(3) . . ?
C25 C26 C28 121.0(3) . . ?
C27 C22 C23 119.7(3) . . ?
C27 C22 C21 119.6(3) . . ?
C23 C22 C21 120.5(3) . . ?
O2 C23 C24 119.4(4) . . ?
O2 C23 C22 123.3(4) . . ?
C24 C23 C22 117.2(3) . . ?
C21 N2 C20 117.3(3) . . ?
C21 N2 Ni1 125.8(3) . . ?
C20 N2 Ni1 116.1(2) . . ?
C15 N1 C16 116.8(3) . . ?
C15 N1 Ni1 125.5(3) . . ?
C16 N1 Ni1 116.6(2) . . ?
C26 C27 C22 122.7(3) . . ?
C26 C27 H27 118.7 . . ?
C22 C27 H27 118.7 . . ?
O1 C12 C13 124.3(3) . . ?
O1 C12 C11 118.8(3) . . ?
C13 C12 C11 116.9(3) . . ?
C33 C32 C31 129.7(9) . . ?
C33 C32 C33A 112(2) . . ?
C31 C32 C33A 118(2) . . ?
C33 C32 S4A 4.6(15) . . ?
C31 C32 S4A 126.1(7) . . ?
C33A C32 S4A 116(2) . . ?
C33 C32 S4 108.8(9) . . ?
C31 C32 S4 121.6(3) . . ?
C33A C32 S4 4(2) . . ?
S4A C32 S4 112.3(7) . . ?
C14 C9 C10 117.9(3) . . ?
C14 C9 C8 122.7(3) . . ?
C10 C9 C8 119.4(3) . . ?
C6 C5 C4 129.0(4) . . ?
C6 C5 S2 110.6(3) . . ?
C4 C5 S2 120.2(3) . . ?
C25 C24 C23 121.6(4) . . ?
C25 C24 H24 119.2 . . ?
C23 C24 H24 119.2 . . ?
C9 C14 C13 121.4(4) . . ?
C9 C14 H14 119.3 . . ?
C13 C14 H14 119.3 . . ?
C14 C13 C12 121.0(4) . . ?
C14 C13 C15 119.3(3) . . ?
C12 C13 C15 119.6(3) . . ?
C7 C8 C9 127.8(3) . . ?
C7 C8 S2 110.4(3) . . ?
C9 C8 S2 121.7(3) . . ?
N2 C20 C17 114.4(3) . . ?
N2 C20 H20A 108.7 . . ?
C17 C20 H20A 108.7 . . ?
N2 C20 H20B 108.7 . . ?
C17 C20 H20B 108.7 . . ?
H20A C20 H20B 107.6 . . ?
C30 C31 C32 128.4(3) . . ?
C30 C31 S3 109.9(3) . . ?
C32 C31 S3 121.7(3) . . ?
C8 C7 C6 113.5(4) . . ?
C8 C7 H7 123.2 . . ?
C6 C7 H7 123.2 . . ?
N2 C21 C22 125.8(4) . . ?
N2 C21 H21 117.1 . . ?
C22 C21 H21 117.1 . . ?
N1 C16 C17 114.0(3) . . ?
N1 C16 H16A 108.7 . . ?
C17 C16 H16A 108.7 . . ?
N1 C16 H16B 108.7 . . ?
C17 C16 H16B 108.7 . . ?
H16A C16 H16B 107.6 . . ?
C28 C29 C30 114.1(3) . . ?
C28 C29 H29 123.0 . . ?
C30 C29 H29 123.0 . . ?
C5 C6 C7 113.3(4) . . ?
C5 C6 H6 123.3 . . ?
C7 C6 H6 123.3 . . ?
C11 C10 C9 121.5(4) . . ?
C11 C10 H10 119.3 . . ?
C9 C10 H10 119.3 . . ?
C31 C30 C29 113.4(3) . . ?
C31 C30 H30 123.3 . . ?
C29 C30 H30 123.3 . . ?
C29 C28 C26 129.1(3) . . ?
C29 C28 S3 109.8(3) . . ?
C26 C28 S3 121.1(3) . . ?
C24 C25 C26 121.8(4) . . ?
C24 C25 H25 119.1 . . ?
C26 C25 H25 119.1 . . ?
N1 C15 C13 125.7(4) . . ?
N1 C15 H15 117.2 . . ?
C13 C15 H15 117.2 . . ?
C10 C11 C12 121.2(4) . . ?
C10 C11 H11 119.4 . . ?
C12 C11 H11 119.4 . . ?
C19 C17 C18 109.9(3) . . ?
C19 C17 C20 110.4(3) . . ?
C18 C17 C20 106.1(3) . . ?
C19 C17 C16 107.6(3) . . ?
C18 C17 C16 111.9(3) . . ?
C20 C17 C16 111.0(3) . . ?
C2 C1 S1 112.1(5) . . ?
C2 C1 H1 123.9 . . ?
S1 C1 H1 123.9 . . ?
C1 C2 C3 114.9(10) . . ?
C1 C2 H2 122.5 . . ?
C3 C2 H2 122.6 . . ?
C2 C3 C4 108.3(13) . . ?
C2 C3 H3 125.9 . . ?
C4 C3 H3 125.9 . . ?
C4 S1 C1 91.5(3) . . ?
C2A C1A S1A 109(3) . . ?
C2A C1A H1A 125.7 . . ?
S1A C1A H1A 125.7 . . ?
C1A C2A C3A 106(3) . . ?
C1A C2A H2A 127.1 . . ?
C3A C2A H2A 127.1 . . ?
C4 C3A C2A 113(3) . . ?
C4 C3A H3A 123.5 . . ?
C2A C3A H3A 123.5 . . ?
C4 S1A C1A 101.0(19) . . ?
C3A C4 C3 118(2) . . ?
C3A C4 C5 115.8(19) . . ?
C3 C4 C5 125.8(8) . . ?
C3A C4 S1A 111(2) . . ?
C3 C4 S1A 11.3(16) . . ?
C5 C4 S1A 132.7(9) . . ?
C3A C4 S1 6.9(19) . . ?
C3 C4 S1 113.2(8) . . ?
C5 C4 S1 120.9(3) . . ?
S1A C4 S1 106.1(8) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C32 S4 C35 92.6(4) . . ?
C34 C33 C32 115.1(14) . . ?
C34 C33 H33 122.5 . . ?
C32 C33 H33 122.5 . . ?
C35 C34 C33 111.3(11) . . ?
C35 C34 H34 124.4 . . ?
C33 C34 H34 124.4 . . ?
C34 C35 S4 112.3(8) . . ?
C34 C35 H35 123.9 . . ?
S4 C35 H35 123.9 . . ?
C32 S4A C35A 94.6(18) . . ?
C32 C33A C34A 106(4) . . ?
C32 C33A H33A 127.2 . . ?
C34A C33A H33A 127.2 . . ?
C35A C34A C33A 113(4) . . ?
C35A C34A H34A 123.7 . . ?
C33A C34A H34A 123.7 . . ?
C34A C35A S4A 111(3) . . ?
C34A C35A H35A 124.3 . . ?
S4A C35A H35A 124.3 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 Ni1 O2 C23 -168.9(3) . . . . ?
N2 Ni1 O2 C23 20.2(3) . . . . ?
N1 Ni1 O2 C23 -110.3(8) . . . . ?
O2 Ni1 O1 C12 -162.3(3) . . . . ?
N2 Ni1 O1 C12 -97.7(7) . . . . ?
N1 Ni1 O1 C12 25.3(3) . . . . ?
Ni1 O2 C23 C24 165.3(3) . . . . ?
Ni1 O2 C23 C22 -16.5(5) . . . . ?
C27 C22 C23 O2 -177.1(3) . . . . ?
C21 C22 C23 O2 -1.6(6) . . . . ?
C27 C22 C23 C24 1.1(5) . . . . ?
C21 C22 C23 C24 176.6(3) . . . . ?
O2 Ni1 N2 C21 -11.3(3) . . . . ?
O1 Ni1 N2 C21 -75.0(8) . . . . ?
N1 Ni1 N2 C21 161.9(3) . . . . ?
O2 Ni1 N2 C20 157.8(3) . . . . ?
O1 Ni1 N2 C20 94.1(7) . . . . ?
N1 Ni1 N2 C20 -28.9(3) . . . . ?
O2 Ni1 N1 C15 -71.9(9) . . . . ?
O1 Ni1 N1 C15 -13.9(3) . . . . ?
N2 Ni1 N1 C15 157.6(3) . . . . ?
O2 Ni1 N1 C16 95.8(8) . . . . ?
O1 Ni1 N1 C16 153.8(3) . . . . ?
N2 Ni1 N1 C16 -34.6(3) . . . . ?
C25 C26 C27 C22 1.0(5) . . . . ?
C28 C26 C27 C22 177.6(3) . . . . ?
C23 C22 C27 C26 -2.1(6) . . . . ?
C21 C22 C27 C26 -177.7(3) . . . . ?
Ni1 O1 C12 C13 -20.2(5) . . . . ?
Ni1 O1 C12 C11 159.6(3) . . . . ?
C8 S2 C5 C6 0.2(3) . . . . ?
C8 S2 C5 C4 -175.3(3) . . . . ?
O2 C23 C24 C25 179.2(3) . . . . ?
C22 C23 C24 C25 0.9(6) . . . . ?
C10 C9 C14 C13 2.3(5) . . . . ?
C8 C9 C14 C13 -178.8(3) . . . . ?
C9 C14 C13 C12 -3.1(6) . . . . ?
C9 C14 C13 C15 -178.7(3) . . . . ?
O1 C12 C13 C14 -178.7(3) . . . . ?
C11 C12 C13 C14 1.5(5) . . . . ?
O1 C12 C13 C15 -3.0(6) . . . . ?
C11 C12 C13 C15 177.2(3) . . . . ?
C14 C9 C8 C7 159.9(4) . . . . ?
C10 C9 C8 C7 -21.2(6) . . . . ?
C14 C9 C8 S2 -22.2(5) . . . . ?
C10 C9 C8 S2 156.8(3) . . . . ?
C5 S2 C8 C7 -0.6(3) . . . . ?
C5 S2 C8 C9 -178.8(3) . . . . ?
C21 N2 C20 C17 -120.3(4) . . . . ?
Ni1 N2 C20 C17 69.6(4) . . . . ?
C33 C32 C31 C30 177.3(12) . . . . ?
C33A C32 C31 C30 -6(3) . . . . ?
S4A C32 C31 C30 173.7(10) . . . . ?
S4 C32 C31 C30 -2.9(6) . . . . ?
C33 C32 C31 S3 -3.3(13) . . . . ?
C33A C32 C31 S3 174(3) . . . . ?
S4A C32 C31 S3 -6.9(11) . . . . ?
S4 C32 C31 S3 176.4(3) . . . . ?
C28 S3 C31 C30 1.0(3) . . . . ?
C28 S3 C31 C32 -178.5(3) . . . . ?
C9 C8 C7 C6 178.9(3) . . . . ?
S2 C8 C7 C6 0.8(4) . . . . ?
C20 N2 C21 C22 -170.0(3) . . . . ?
Ni1 N2 C21 C22 -1.0(5) . . . . ?
C27 C22 C21 N2 -173.9(4) . . . . ?
C23 C22 C21 N2 10.6(6) . . . . ?
C15 N1 C16 C17 -121.8(4) . . . . ?
Ni1 N1 C16 C17 69.3(4) . . . . ?
C4 C5 C6 C7 175.2(4) . . . . ?
S2 C5 C6 C7 0.2(4) . . . . ?
C8 C7 C6 C5 -0.7(5) . . . . ?
C14 C9 C10 C11 0.0(5) . . . . ?
C8 C9 C10 C11 -179.0(3) . . . . ?
C32 C31 C30 C29 178.6(4) . . . . ?
S3 C31 C30 C29 -0.8(4) . . . . ?
C28 C29 C30 C31 0.1(5) . . . . ?
C30 C29 C28 C26 -178.4(3) . . . . ?
C30 C29 C28 S3 0.7(4) . . . . ?
C27 C26 C28 C29 -8.7(6) . . . . ?
C25 C26 C28 C29 167.7(4) . . . . ?
C27 C26 C28 S3 172.3(3) . . . . ?
C25 C26 C28 S3 -11.3(5) . . . . ?
C31 S3 C28 C29 -0.9(3) . . . . ?
C31 S3 C28 C26 178.3(3) . . . . ?
C23 C24 C25 C26 -2.1(6) . . . . ?
C27 C26 C25 C24 1.1(5) . . . . ?
C28 C26 C25 C24 -175.5(3) . . . . ?
C16 N1 C15 C13 -170.2(3) . . . . ?
Ni1 N1 C15 C13 -2.5(5) . . . . ?
C14 C13 C15 N1 -169.3(4) . . . . ?
C12 C13 C15 N1 15.0(6) . . . . ?
C9 C10 C11 C12 -1.5(6) . . . . ?
O1 C12 C11 C10 -179.1(3) . . . . ?
C13 C12 C11 C10 0.7(5) . . . . ?
N2 C20 C17 C19 81.6(4) . . . . ?
N2 C20 C17 C18 -159.4(3) . . . . ?
N2 C20 C17 C16 -37.5(4) . . . . ?
N1 C16 C17 C19 -150.8(3) . . . . ?
N1 C16 C17 C18 88.3(4) . . . . ?
N1 C16 C17 C20 -30.0(4) . . . . ?
S1 C1 C2 C3 1.1(11) . . . . ?
C1 C2 C3 C4 -1.6(16) . . . . ?
C2 C1 S1 C4 -0.3(5) . . . . ?
S1A C1A C2A C3A -5(4) . . . . ?
C1A C2A C3A C4 3(5) . . . . ?
C2A C1A S1A C4 4(3) . . . . ?
C2A C3A C4 C3 -11(4) . . . . ?
C2A C3A C4 C5 179(2) . . . . ?
C2A C3A C4 S1A 0(4) . . . . ?
C2A C3A C4 S1 40(15) . . . . ?
C2 C3 C4 C3A 7(3) . . . . ?
C2 C3 C4 C5 177.0(7) . . . . ?
C2 C3 C4 S1A -52(8) . . . . ?
C2 C3 C4 S1 1.3(15) . . . . ?
C6 C5 C4 C3A -16(2) . . . . ?
S2 C5 C4 C3A 158(2) . . . . ?
C6 C5 C4 C3 173.9(10) . . . . ?
S2 C5 C4 C3 -11.6(11) . . . . ?
C6 C5 C4 S1A 162.4(15) . . . . ?
S2 C5 C4 S1A -23.1(15) . . . . ?
C6 C5 C4 S1 -10.7(6) . . . . ?
S2 C5 C4 S1 163.8(2) . . . . ?
C1A S1A C4 C3A -3(3) . . . . ?
C1A S1A C4 C3 123(9) . . . . ?
C1A S1A C4 C5 179.0(15) . . . . ?
C1A S1A C4 S1 -7(2) . . . . ?
C1 S1 C4 C3A -132(17) . . . . ?
C1 S1 C4 C3 -0.6(9) . . . . ?
C1 S1 C4 C5 -176.5(4) . . . . ?
C1 S1 C4 S1A 8.8(11) . . . . ?
C33 C32 S4 C35 0.0(10) . . . . ?
C31 C32 S4 C35 -179.8(5) . . . . ?
C33A C32 S4 C35 -142(35) . . . . ?
S4A C32 S4 C35 3.1(10) . . . . ?
C31 C32 C33 C34 179.1(9) . . . . ?
C33A C32 C33 C34 2(3) . . . . ?
S4A C32 C33 C34 -141(22) . . . . ?
S4 C32 C33 C34 -0.7(18) . . . . ?
C32 C33 C34 C35 1(2) . . . . ?
C33 C34 C35 S4 -1.3(16) . . . . ?
C32 S4 C35 C34 0.8(9) . . . . ?
C33 C32 S4A C35A 41(21) . . . . ?
C31 C32 S4A C35A -176.0(17) . . . . ?
C33A C32 S4A C35A 3(3) . . . . ?
S4 C32 S4A C35A 0.9(19) . . . . ?
C33 C32 C33A C34A -4(5) . . . . ?
C31 C32 C33A C34A 179(3) . . . . ?
S4A C32 C33A C34A -1(5) . . . . ?
S4 C32 C33A C34A 35(32) . . . . ?
C32 C33A C34A C35A -3(6) . . . . ?
C33A C34A C35A S4A 6(5) . . . . ?
C32 S4A C35A C34A -5(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.508
_refine_diff_density_rms         0.109
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1545045'
_audit_update_record             
;
2017-04-20 deposited with the CCDC.
2017-06-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H38 N4 O4 S4 V'
_chemical_formula_weight         817.92

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'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P21/n

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

_cell_length_a                   19.124
_cell_length_b                   7.767
_cell_length_c                   25.554
_cell_angle_alpha                90.00
_cell_angle_beta                 98.99
_cell_angle_gamma                90.00
_cell_volume                     3749.0
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    4827
_cell_measurement_theta_max      25.6014
_cell_measurement_theta_min      1.4490

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1700
_exptl_absorpt_coefficient_mu    0.536
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9051
_exptl_absorpt_correction_T_max  0.9686
_exptl_absorpt_process_details   'The Rigaku Corporation, Tokyo, Japan'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(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  
;
Mercury2 (2x2 bin mode)
;
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            29463
_diffrn_reflns_av_R_equivalents  0.1364
_diffrn_reflns_av_sigmaI/netI    0.1840
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         2.84
_diffrn_reflns_theta_max         25.00
_reflns_number_total             6608
_reflns_number_gt                3274
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_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)+(0.0983P)²+0.1916P] 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         6608
_refine_ls_number_parameters     517
_refine_ls_number_restraints     183
_refine_ls_R_factor_all          0.1870
_refine_ls_R_factor_gt           0.0900
_refine_ls_wR_factor_ref         0.2472
_refine_ls_wR_factor_gt          0.1927
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.018
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.42486(7) 0.10038(16) 0.29709(5) 0.0311(4) Uani 1 1 d . . .
S3 S 0.29505(10) -0.2283(2) 0.55729(7) 0.0335(5) Uani 1 1 d . . .
S2 S 0.45756(11) -0.2063(3) 0.00469(8) 0.0386(5) Uani 1 1 d . . .
S4 S 0.18427(12) -0.3752(3) 0.68640(9) 0.0538(7) Uani 1 1 d . . .
O1 O 0.3646(3) 0.1282(6) 0.22815(19) 0.0342(13) Uani 1 1 d . . .
N2 N 0.4693(3) -0.0067(7) 0.3699(2) 0.0277(14) Uani 1 1 d . . .
O3 O 0.4691(3) 0.2772(6) 0.30544(19) 0.0376(13) Uani 1 1 d . . .
O2 O 0.3382(2) 0.1450(6) 0.32782(18) 0.0298(12) Uani 1 1 d . . .
C33 C 0.3166(4) -0.3678(8) 0.6785(3) 0.0309(18) Uani 1 1 d . . .
H33 H 0.3604 -0.3431 0.6670 0.037 Uiso 1 1 calc R . .
N1 N 0.4976(3) -0.0334(7) 0.2592(2) 0.0290(14) Uani 1 1 d . . .
N3 N 0.3670(3) -0.1941(8) 0.2864(2) 0.0354(16) Uani 1 1 d . . .
C21 C 0.4355(4) -0.0433(8) 0.4080(3) 0.0256(17) Uani 1 1 d . . .
H21 H 0.4623 -0.0945 0.4385 0.031 Uiso 1 1 calc R . .
C5 C 0.4206(4) -0.2197(9) -0.0618(3) 0.0346(19) Uani 1 1 d . . .
C27 C 0.2676(4) -0.0394(9) 0.4643(3) 0.0341(19) Uani 1 1 d . . .
C14 C 0.4293(4) -0.1004(9) 0.1186(3) 0.0300(18) Uani 1 1 d . . .
H14 H 0.4674 -0.1723 0.1126 0.036 Uiso 1 1 calc R . .
N4 N 0.4182(4) -0.6032(8) 0.4455(3) 0.0449(18) Uani 1 1 d . . .
C25 C 0.2477(4) 0.1191(9) 0.3806(3) 0.0322(19) Uani 1 1 d . . .
H25 H 0.2169 0.1864 0.3559 0.039 Uiso 1 1 calc R . .
C13 C 0.4261(4) -0.0422(9) 0.1708(3) 0.0350(19) Uani 1 1 d . . .
C36 C 0.3014(4) -0.4839(9) 0.2586(3) 0.042(2) Uani 1 1 d . . .
H36A H 0.3269 -0.5479 0.2345 0.062 Uiso 1 1 calc R . .
H36B H 0.2533 -0.4589 0.2409 0.062 Uiso 1 1 calc R . .
H36C H 0.2993 -0.5532 0.2904 0.062 Uiso 1 1 calc R . .
C22 C 0.3355(4) -0.0727(8) 0.4543(3) 0.0282(17) Uani 1 1 d . . .
H22 H 0.3663 -0.1386 0.4794 0.034 Uiso 1 1 calc R . .
C23 C 0.3608(4) -0.0150(8) 0.4097(3) 0.0285(17) Uani 1 1 d . . .
C8 C 0.3825(4) -0.1112(9) 0.0222(3) 0.0338(19) Uani 1 1 d . . .
C4 C 0.4598(4) -0.2928(10) -0.1017(3) 0.0366(18) Uani 1 1 d DU . .
C1 C 0.4968(5) -0.3898(15) -0.1845(4) 0.041(3) Uani 0.88 1 d PDU A 1
H1 H 0.5016 -0.4173 -0.2200 0.033(14) Uiso 0.88 1 calc PR A 1
C2 C 0.5467(6) -0.4195(17) -0.1431(5) 0.048(3) Uani 0.88 1 d PDU A 1
H2 H 0.5914 -0.4704 -0.1451 0.033(14) Uiso 0.88 1 calc PR A 1
C3 C 0.5237(8) -0.364(3) -0.0954(7) 0.050(4) Uani 0.88 1 d PDU A 1
H3 H 0.5520 -0.3772 -0.0616 0.033(14) Uiso 0.88 1 calc PR A 1
S1 S 0.42297(17) -0.2962(4) -0.16661(10) 0.0489(9) Uani 0.88 1 d PDU A 1
C1A C 0.538(3) -0.444(14) -0.154(2) 0.048(9) Uani 0.12 1 d PDU A 2
H1A H 0.5760 -0.4984 -0.1669 0.058 Uiso 0.12 1 calc PR A 2
C2A C 0.475(3) -0.414(12) -0.1825(15) 0.045(9) Uani 0.12 1 d PDU A 2
H2A H 0.4620 -0.4438 -0.2188 0.054 Uiso 0.12 1 calc PR A 2
C3A C 0.429(3) -0.330(11) -0.1512(15) 0.038(10) Uani 0.12 1 d PDU A 2
H3A H 0.3815 -0.3027 -0.1644 0.045 Uiso 0.12 1 calc PR A 2
S1A S 0.5417(14) -0.374(6) -0.0895(13) 0.043(6) Uani 0.12 1 d PDU A 2
C18 C 0.6573(4) -0.1696(10) 0.3617(3) 0.039(2) Uani 1 1 d . . .
H18A H 0.6779 -0.2463 0.3377 0.058 Uiso 1 1 calc R . .
H18B H 0.6645 -0.2188 0.3974 0.058 Uiso 1 1 calc R . .
H18C H 0.6803 -0.0567 0.3624 0.058 Uiso 1 1 calc R . .
C15 C 0.4879(4) -0.0793(9) 0.2100(3) 0.0344(19) Uani 1 1 d . . .
H15 H 0.5248 -0.1438 0.1984 0.041 Uiso 1 1 calc R . .
C19 C 0.5407(4) -0.3259(9) 0.3396(3) 0.038(2) Uani 1 1 d . . .
H19A H 0.5606 -0.4009 0.3149 0.057 Uiso 1 1 calc R . .
H19B H 0.4899 -0.3111 0.3276 0.057 Uiso 1 1 calc R . .
H19C H 0.5482 -0.3781 0.3750 0.057 Uiso 1 1 calc R . .
C37 C 0.3385(4) -0.3225(11) 0.2737(3) 0.0350(19) Uani 1 1 d . . .
C11 C 0.3167(4) 0.1070(9) 0.1371(3) 0.0360(19) Uani 1 1 d . . .
H11 H 0.2773 0.1753 0.1428 0.043 Uiso 1 1 calc R . .
C9 C 0.3781(4) -0.0551(9) 0.0763(3) 0.0333(19) Uani 1 1 d . . .
C24 C 0.3171(4) 0.0845(9) 0.3704(3) 0.0298(18) Uani 1 1 d . . .
C40 C 0.3807(5) -0.6254(11) 0.4911(3) 0.057(3) Uani 1 1 d . . .
H40A H 0.3334 -0.5743 0.4831 0.085 Uiso 1 1 calc R . .
H40B H 0.4074 -0.5683 0.5222 0.085 Uiso 1 1 calc R . .
H40C H 0.3764 -0.7484 0.4986 0.085 Uiso 1 1 calc R . .
C39 C 0.3809(5) -0.5119(10) 0.4016(3) 0.049(2) Uani 1 1 d . . .
H39A H 0.3337 -0.4815 0.4089 0.074 Uiso 1 1 calc R . .
H39B H 0.3765 -0.5845 0.3699 0.074 Uiso 1 1 calc R . .
H39C H 0.4069 -0.4067 0.3957 0.074 Uiso 1 1 calc R . .
C20 C 0.5471(3) -0.0290(9) 0.3812(3) 0.0282(17) Uani 1 1 d . . .
H20A H 0.5600 -0.0760 0.4175 0.034 Uiso 1 1 calc R . .
H20B H 0.5698 0.0854 0.3805 0.034 Uiso 1 1 calc R . .
C32 C 0.2509(4) -0.3203(10) 0.6513(3) 0.037(2) Uani 1 1 d . . .
C31 C 0.2333(4) -0.2280(10) 0.6006(3) 0.040(2) Uani 1 1 d . . .
C17 C 0.5775(4) -0.1493(9) 0.3419(3) 0.0308(18) Uani 1 1 d . . .
C7 C 0.3319(5) -0.0969(11) -0.0226(3) 0.051(2) Uani 1 1 d . A .
H7 H 0.2863 -0.0498 -0.0218 0.061 Uiso 1 1 calc R . .
C28 C 0.2417(4) -0.1004(9) 0.5114(3) 0.0322(18) Uani 1 1 d . . .
C6 C 0.3531(5) -0.1569(10) -0.0690(3) 0.044(2) Uani 1 1 d . . .
H6 H 0.3235 -0.1544 -0.1025 0.052 Uiso 1 1 calc R A .
C29 C 0.1787(4) -0.0659(9) 0.5301(3) 0.038(2) Uani 1 1 d . . .
H29 H 0.1418 0.0016 0.5110 0.046 Uiso 1 1 calc R . .
C35 C 0.2434(5) -0.4678(10) 0.7352(3) 0.048(2) Uani 1 1 d . . .
H35 H 0.2303 -0.5206 0.7658 0.057 Uiso 1 1 calc R . .
C26 C 0.2233(4) 0.0589(9) 0.4249(3) 0.0334(19) Uani 1 1 d . . .
H26 H 0.1760 0.0831 0.4295 0.040 Uiso 1 1 calc R . .
C12 C 0.3699(4) 0.0655(9) 0.1812(3) 0.0338(19) Uani 1 1 d . . .
C10 C 0.3212(4) 0.0504(9) 0.0868(3) 0.0338(19) Uani 1 1 d . . .
H10 H 0.2855 0.0825 0.0584 0.041 Uiso 1 1 calc R . .
C34 C 0.3099(5) -0.4582(10) 0.7258(3) 0.048(2) Uani 1 1 d . . .
H34 H 0.3489 -0.5071 0.7484 0.057 Uiso 1 1 calc R . .
C16 C 0.5708(4) -0.0625(10) 0.2869(3) 0.0333(19) Uani 1 1 d . . .
H16A H 0.5953 0.0501 0.2912 0.040 Uiso 1 1 calc R . .
H16B H 0.5960 -0.1346 0.2639 0.040 Uiso 1 1 calc R . .
C30 C 0.1740(4) -0.1389(10) 0.5795(3) 0.044(2) Uani 1 1 d . . .
H30 H 0.1336 -0.1277 0.5967 0.053 Uiso 1 1 calc R . .
C38 C 0.4822(5) -0.6635(10) 0.4464(3) 0.042(2) Uani 1 1 d . . .
H38 H 0.5031 -0.6449 0.4155 0.051 Uiso 1 1 calc R . .
O4 O 0.5178(3) -0.7401(7) 0.4822(2) 0.0513(16) 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
V1 O3 1.610(5) . ?
V1 O1 1.960(5) . ?
V1 O2 1.972(5) . ?
V1 N1 2.091(6) . ?
V1 N2 2.093(6) . ?
S3 C28 1.740(7) . ?
S3 C31 1.740(8) . ?
S2 C8 1.735(7) . ?
S2 C5 1.739(7) . ?
S4 C35 1.706(8) . ?
S4 C32 1.722(8) . ?
O1 C12 1.313(8) . ?
N2 C21 1.280(8) . ?
N2 C20 1.482(8) . ?
O2 C24 1.306(8) . ?
C33 C32 1.387(10) . ?
C33 C34 1.421(10) . ?
C33 H33 0.9500 . ?
N1 C15 1.291(8) . ?
N1 C16 1.484(8) . ?
N3 C37 1.159(9) . ?
C21 C23 1.454(9) . ?
C21 H21 0.9500 . ?
C5 C6 1.365(10) . ?
C5 C4 1.470(11) . ?
C27 C22 1.387(10) . ?
C27 C26 1.430(10) . ?
C27 C28 1.452(10) . ?
C14 C9 1.386(10) . ?
C14 C13 1.418(10) . ?
C14 H14 0.9500 . ?
N4 C38 1.309(10) . ?
N4 C39 1.420(9) . ?
N4 C40 1.471(10) . ?
C25 C26 1.371(10) . ?
C25 C24 1.419(10) . ?
C25 H25 0.9500 . ?
C13 C12 1.421(10) . ?
C13 C15 1.453(10) . ?
C36 C37 1.462(11) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C22 C23 1.381(9) . ?
C22 H22 0.9500 . ?
C23 C24 1.427(10) . ?
C8 C7 1.384(10) . ?
C8 C9 1.463(10) . ?
C4 C3 1.327(16) . ?
C4 C3A 1.34(2) . ?
C4 S1A 1.671(17) . ?
C4 S1 1.699(7) . ?
C1 C2 1.329(11) . ?
C1 S1 1.713(10) . ?
C1 H1 0.9500 . ?
C2 C3 1.43(2) . ?
C2 H2 0.9500 . ?
C3 H3 0.9500 . ?
C1A C2A 1.33(2) . ?
C1A S1A 1.72(2) . ?
C1A H1A 0.9500 . ?
C2A C3A 1.43(3) . ?
C2A H2A 0.9500 . ?
C3A H3A 0.9500 . ?
C18 C17 1.538(9) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C15 H15 0.9500 . ?
C19 C17 1.538(10) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C11 C10 1.374(10) . ?
C11 C12 1.432(10) . ?
C11 H11 0.9500 . ?
C9 C10 1.421(10) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C20 C17 1.549(9) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C32 C31 1.473(11) . ?
C31 C30 1.365(10) . ?
C17 C16 1.547(10) . ?
C7 C6 1.392(10) . ?
C7 H7 0.9500 . ?
C28 C29 1.391(10) . ?
C6 H6 0.9500 . ?
C29 C30 1.399(10) . ?
C29 H29 0.9500 . ?
C35 C34 1.332(11) . ?
C35 H35 0.9500 . ?
C26 H26 0.9500 . ?
C10 H10 0.9500 . ?
C34 H34 0.9500 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C30 H30 0.9500 . ?
C38 O4 1.209(9) . ?
C38 H38 0.9500 . ?

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
O3 V1 O1 104.3(2) . . ?
O3 V1 O2 104.7(2) . . ?
O1 V1 O2 85.8(2) . . ?
O3 V1 N1 96.4(2) . . ?
O1 V1 N1 88.8(2) . . ?
O2 V1 N1 158.9(2) . . ?
O3 V1 N2 95.1(2) . . ?
O1 V1 N2 160.5(2) . . ?
O2 V1 N2 88.0(2) . . ?
N1 V1 N2 90.4(2) . . ?
C28 S3 C31 92.5(4) . . ?
C8 S2 C5 93.0(4) . . ?
C35 S4 C32 91.4(4) . . ?
C12 O1 V1 131.5(5) . . ?
C21 N2 C20 115.8(6) . . ?
C21 N2 V1 125.6(5) . . ?
C20 N2 V1 118.4(4) . . ?
C24 O2 V1 131.0(5) . . ?
C32 C33 C34 111.2(7) . . ?
C32 C33 H33 124.4 . . ?
C34 C33 H33 124.4 . . ?
C15 N1 C16 113.8(6) . . ?
C15 N1 V1 125.7(5) . . ?
C16 N1 V1 120.0(4) . . ?
N2 C21 C23 127.1(7) . . ?
N2 C21 H21 116.5 . . ?
C23 C21 H21 116.5 . . ?
C6 C5 C4 128.2(7) . . ?
C6 C5 S2 110.0(6) . . ?
C4 C5 S2 121.8(6) . . ?
C22 C27 C26 116.0(7) . . ?
C22 C27 C28 122.9(7) . . ?
C26 C27 C28 121.2(7) . . ?
C9 C14 C13 121.7(7) . . ?
C9 C14 H14 119.2 . . ?
C13 C14 H14 119.2 . . ?
C38 N4 C39 123.0(7) . . ?
C38 N4 C40 121.0(7) . . ?
C39 N4 C40 116.0(7) . . ?
C26 C25 C24 122.3(7) . . ?
C26 C25 H25 118.8 . . ?
C24 C25 H25 118.8 . . ?
C14 C13 C12 120.5(7) . . ?
C14 C13 C15 115.9(7) . . ?
C12 C13 C15 123.0(7) . . ?
C37 C36 H36A 109.5 . . ?
C37 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C37 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C23 C22 C27 123.4(7) . . ?
C23 C22 H22 118.3 . . ?
C27 C22 H22 118.3 . . ?
C22 C23 C24 120.9(7) . . ?
C22 C23 C21 116.6(6) . . ?
C24 C23 C21 122.1(7) . . ?
C7 C8 C9 128.5(7) . . ?
C7 C8 S2 108.6(6) . . ?
C9 C8 S2 122.9(6) . . ?
C3 C4 C3A 106(3) . . ?
C3 C4 C5 129.6(10) . . ?
C3A C4 C5 123(2) . . ?
C3 C4 S1A 4(2) . . ?
C3A C4 S1A 110.5(13) . . ?
C5 C4 S1A 125.5(13) . . ?
C3 C4 S1 110.1(9) . . ?
C3A C4 S1 12(4) . . ?
C5 C4 S1 120.3(6) . . ?
S1A C4 S1 114.2(13) . . ?
C2 C1 S1 112.4(8) . . ?
C2 C1 H1 123.8 . . ?
S1 C1 H1 123.8 . . ?
C1 C2 C3 110.4(11) . . ?
C1 C2 H2 124.8 . . ?
C3 C2 H2 124.8 . . ?
C4 C3 C2 115.1(12) . . ?
C4 C3 H3 122.4 . . ?
C2 C3 H3 122.4 . . ?
C4 S1 C1 91.9(5) . . ?
C2A C1A S1A 111.9(14) . . ?
C2A C1A H1A 124.1 . . ?
S1A C1A H1A 124.1 . . ?
C1A C2A C3A 110.3(16) . . ?
C1A C2A H2A 124.8 . . ?
C3A C2A H2A 124.8 . . ?
C4 C3A C2A 114.6(17) . . ?
C4 C3A H3A 122.7 . . ?
C2A C3A H3A 122.7 . . ?
C4 S1A C1A 92.5(9) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N1 C15 C13 126.4(7) . . ?
N1 C15 H15 116.8 . . ?
C13 C15 H15 116.8 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N3 C37 C36 178.8(9) . . ?
C10 C11 C12 121.5(7) . . ?
C10 C11 H11 119.3 . . ?
C12 C11 H11 119.3 . . ?
C14 C9 C10 117.8(7) . . ?
C14 C9 C8 121.6(7) . . ?
C10 C9 C8 120.6(7) . . ?
O2 C24 C25 120.3(7) . . ?
O2 C24 C23 123.9(7) . . ?
C25 C24 C23 115.8(7) . . ?
N4 C40 H40A 109.5 . . ?
N4 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
N4 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
N4 C39 H39A 109.5 . . ?
N4 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
N4 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
N2 C20 C17 114.3(5) . . ?
N2 C20 H20A 108.7 . . ?
C17 C20 H20A 108.7 . . ?
N2 C20 H20B 108.7 . . ?
C17 C20 H20B 108.7 . . ?
H20A C20 H20B 107.6 . . ?
C33 C32 C31 129.3(7) . . ?
C33 C32 S4 111.1(6) . . ?
C31 C32 S4 119.5(6) . . ?
C30 C31 C32 130.9(7) . . ?
C30 C31 S3 110.7(6) . . ?
C32 C31 S3 118.3(6) . . ?
C19 C17 C18 110.2(6) . . ?
C19 C17 C16 112.4(6) . . ?
C18 C17 C16 106.3(6) . . ?
C19 C17 C20 110.3(6) . . ?
C18 C17 C20 107.6(6) . . ?
C16 C17 C20 109.8(6) . . ?
C8 C7 C6 114.8(8) . . ?
C8 C7 H7 122.6 . . ?
C6 C7 H7 122.6 . . ?
C29 C28 C27 130.5(7) . . ?
C29 C28 S3 109.1(6) . . ?
C27 C28 S3 120.4(6) . . ?
C5 C6 C7 113.6(7) . . ?
C5 C6 H6 123.2 . . ?
C7 C6 H6 123.2 . . ?
C28 C29 C30 114.4(7) . . ?
C28 C29 H29 122.8 . . ?
C30 C29 H29 122.8 . . ?
C34 C35 S4 112.7(7) . . ?
C34 C35 H35 123.6 . . ?
S4 C35 H35 123.6 . . ?
C25 C26 C27 121.5(7) . . ?
C25 C26 H26 119.2 . . ?
C27 C26 H26 119.2 . . ?
O1 C12 C13 123.9(7) . . ?
O1 C12 C11 119.3(7) . . ?
C13 C12 C11 116.8(7) . . ?
C11 C10 C9 121.7(7) . . ?
C11 C10 H10 119.2 . . ?
C9 C10 H10 119.2 . . ?
C35 C34 C33 113.4(8) . . ?
C35 C34 H34 123.3 . . ?
C33 C34 H34 123.3 . . ?
N1 C16 C17 116.0(5) . . ?
N1 C16 H16A 108.3 . . ?
C17 C16 H16A 108.3 . . ?
N1 C16 H16B 108.3 . . ?
C17 C16 H16B 108.3 . . ?
H16A C16 H16B 107.4 . . ?
C31 C30 C29 113.3(7) . . ?
C31 C30 H30 123.3 . . ?
C29 C30 H30 123.3 . . ?
O4 C38 N4 127.2(9) . . ?
O4 C38 H38 116.4 . . ?
N4 C38 H38 116.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 V1 O1 C12 102.7(6) . . . . ?
O2 V1 O1 C12 -153.2(6) . . . . ?
N1 V1 O1 C12 6.4(6) . . . . ?
N2 V1 O1 C12 -81.4(9) . . . . ?
O3 V1 N2 C21 115.9(6) . . . . ?
O1 V1 N2 C21 -60.1(9) . . . . ?
O2 V1 N2 C21 11.3(5) . . . . ?
N1 V1 N2 C21 -147.7(6) . . . . ?
O3 V1 N2 C20 -58.4(5) . . . . ?
O1 V1 N2 C20 125.7(7) . . . . ?
O2 V1 N2 C20 -163.0(5) . . . . ?
N1 V1 N2 C20 38.1(5) . . . . ?
O3 V1 O2 C24 -110.3(6) . . . . ?
O1 V1 O2 C24 145.9(6) . . . . ?
N1 V1 O2 C24 70.5(8) . . . . ?
N2 V1 O2 C24 -15.6(6) . . . . ?
O3 V1 N1 C15 -111.2(6) . . . . ?
O1 V1 N1 C15 -6.9(6) . . . . ?
O2 V1 N1 C15 68.0(9) . . . . ?
N2 V1 N1 C15 153.6(6) . . . . ?
O3 V1 N1 C16 60.3(5) . . . . ?
O1 V1 N1 C16 164.6(5) . . . . ?
O2 V1 N1 C16 -120.5(6) . . . . ?
N2 V1 N1 C16 -34.9(5) . . . . ?
C20 N2 C21 C23 172.6(6) . . . . ?
V1 N2 C21 C23 -1.7(10) . . . . ?
C8 S2 C5 C6 -1.4(6) . . . . ?
C8 S2 C5 C4 179.6(6) . . . . ?
C9 C14 C13 C12 -0.1(11) . . . . ?
C9 C14 C13 C15 -171.8(7) . . . . ?
C26 C27 C22 C23 0.5(10) . . . . ?
C28 C27 C22 C23 -179.8(6) . . . . ?
C27 C22 C23 C24 0.0(10) . . . . ?
C27 C22 C23 C21 173.0(6) . . . . ?
N2 C21 C23 C22 177.1(6) . . . . ?
N2 C21 C23 C24 -10.0(11) . . . . ?
C5 S2 C8 C7 1.4(6) . . . . ?
C5 S2 C8 C9 -177.3(6) . . . . ?
C6 C5 C4 C3 -175.5(15) . . . . ?
S2 C5 C4 C3 3.3(17) . . . . ?
C6 C5 C4 C3A -10(5) . . . . ?
S2 C5 C4 C3A 169(5) . . . . ?
C6 C5 C4 S1A -178(2) . . . . ?
S2 C5 C4 S1A 1(3) . . . . ?
C6 C5 C4 S1 3.6(11) . . . . ?
S2 C5 C4 S1 -177.6(4) . . . . ?
S1 C1 C2 C3 0.1(11) . . . . ?
C3A C4 C3 C2 14(5) . . . . ?
C5 C4 C3 C2 -178.8(10) . . . . ?
S1A C4 C3 C2 -155(37) . . . . ?
S1 C4 C3 C2 2.0(18) . . . . ?
C1 C2 C3 C4 -1.4(18) . . . . ?
C3 C4 S1 C1 -1.7(12) . . . . ?
C3A C4 S1 C1 -74(11) . . . . ?
C5 C4 S1 C1 179.1(7) . . . . ?
S1A C4 S1 C1 0(2) . . . . ?
C2 C1 S1 C4 0.9(8) . . . . ?
S1A C1A C2A C3A 0(2) . . . . ?
C3 C4 C3A C2A -6(8) . . . . ?
C5 C4 C3A C2A -175(5) . . . . ?
S1A C4 C3A C2A -5(8) . . . . ?
S1 C4 C3A C2A 105(16) . . . . ?
C1A C2A C3A C4 3(6) . . . . ?
C3 C4 S1A C1A 17(36) . . . . ?
C3A C4 S1A C1A 5(7) . . . . ?
C5 C4 S1A C1A 174(4) . . . . ?
S1 C4 S1A C1A -7(4) . . . . ?
C2A C1A S1A C4 -3(4) . . . . ?
C16 N1 C15 C13 -169.5(7) . . . . ?
V1 N1 C15 C13 2.5(10) . . . . ?
C14 C13 C15 N1 177.4(7) . . . . ?
C12 C13 C15 N1 5.9(12) . . . . ?
C13 C14 C9 C10 -1.0(11) . . . . ?
C13 C14 C9 C8 178.2(7) . . . . ?
C7 C8 C9 C14 170.5(8) . . . . ?
S2 C8 C9 C14 -11.1(10) . . . . ?
C7 C8 C9 C10 -10.3(12) . . . . ?
S2 C8 C9 C10 168.1(6) . . . . ?
V1 O2 C24 C25 -171.6(5) . . . . ?
V1 O2 C24 C23 9.7(10) . . . . ?
C26 C25 C24 O2 -179.8(6) . . . . ?
C26 C25 C24 C23 -1.0(10) . . . . ?
C22 C23 C24 O2 178.9(6) . . . . ?
C21 C23 C24 O2 6.3(10) . . . . ?
C22 C23 C24 C25 0.2(10) . . . . ?
C21 C23 C24 C25 -172.5(6) . . . . ?
C21 N2 C20 C17 124.4(7) . . . . ?
V1 N2 C20 C17 -60.8(7) . . . . ?
C34 C33 C32 C31 -179.0(7) . . . . ?
C34 C33 C32 S4 3.9(8) . . . . ?
C35 S4 C32 C33 -2.3(6) . . . . ?
C35 S4 C32 C31 -179.8(6) . . . . ?
C33 C32 C31 C30 -159.9(9) . . . . ?
S4 C32 C31 C30 17.1(12) . . . . ?
C33 C32 C31 S3 21.2(11) . . . . ?
S4 C32 C31 S3 -161.8(4) . . . . ?
C28 S3 C31 C30 2.1(6) . . . . ?
C28 S3 C31 C32 -178.8(6) . . . . ?
N2 C20 C17 C19 -55.4(8) . . . . ?
N2 C20 C17 C18 -175.7(6) . . . . ?
N2 C20 C17 C16 69.1(7) . . . . ?
C9 C8 C7 C6 177.5(7) . . . . ?
S2 C8 C7 C6 -1.0(9) . . . . ?
C22 C27 C28 C29 173.0(7) . . . . ?
C26 C27 C28 C29 -7.4(12) . . . . ?
C22 C27 C28 S3 -2.6(10) . . . . ?
C26 C27 C28 S3 177.0(5) . . . . ?
C31 S3 C28 C29 -1.4(6) . . . . ?
C31 S3 C28 C27 175.1(6) . . . . ?
C4 C5 C6 C7 179.9(7) . . . . ?
S2 C5 C6 C7 1.0(9) . . . . ?
C8 C7 C6 C5 0.0(11) . . . . ?
C27 C28 C29 C30 -175.7(7) . . . . ?
S3 C28 C29 C30 0.4(8) . . . . ?
C32 S4 C35 C34 0.0(7) . . . . ?
C24 C25 C26 C27 1.6(11) . . . . ?
C22 C27 C26 C25 -1.3(10) . . . . ?
C28 C27 C26 C25 179.0(6) . . . . ?
V1 O1 C12 C13 -1.0(10) . . . . ?
V1 O1 C12 C11 179.3(5) . . . . ?
C14 C13 C12 O1 -178.0(6) . . . . ?
C15 C13 C12 O1 -6.8(11) . . . . ?
C14 C13 C12 C11 1.7(10) . . . . ?
C15 C13 C12 C11 172.8(7) . . . . ?
C10 C11 C12 O1 177.3(7) . . . . ?
C10 C11 C12 C13 -2.3(11) . . . . ?
C12 C11 C10 C9 1.4(11) . . . . ?
C14 C9 C10 C11 0.3(11) . . . . ?
C8 C9 C10 C11 -178.9(7) . . . . ?
S4 C35 C34 C33 2.2(9) . . . . ?
C32 C33 C34 C35 -4.0(10) . . . . ?
C15 N1 C16 C17 -133.5(7) . . . . ?
V1 N1 C16 C17 54.0(7) . . . . ?
C19 C17 C16 N1 57.9(8) . . . . ?
C18 C17 C16 N1 178.5(6) . . . . ?
C20 C17 C16 N1 -65.3(8) . . . . ?
C32 C31 C30 C29 178.8(8) . . . . ?
S3 C31 C30 C29 -2.3(9) . . . . ?
C28 C29 C30 C31 1.3(10) . . . . ?
C39 N4 C38 O4 178.9(8) . . . . ?
C40 N4 C38 O4 -0.3(13) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.522
_refine_diff_density_min         -0.562
_refine_diff_density_rms         0.111
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1544969'
_audit_update_record             
;
2017-04-20 deposited with the CCDC.
2017-06-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C74 H62 Co2 N6 O6 S8'
_chemical_formula_weight         1505.64

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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P21/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                   8.9360(18)
_cell_length_b                   11.6472(25)
_cell_length_c                   31.5458(69)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.75
_cell_angle_gamma                90.00
_cell_volume                     3276.2263(1000)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9415
_cell_measurement_theta_min      1.7485
_cell_measurement_theta_max      27.5126

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1560
_exptl_absorpt_coefficient_mu    0.823
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8383
_exptl_absorpt_process_details   'The Rigaku Corporation, Tokyo, Japan'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(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  
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            58109
_diffrn_reflns_av_R_equivalents  0.0741
_diffrn_reflns_av_sigmaI/netI    0.0367
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         2.18
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5778
_reflns_number_gt                5691
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_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)+(0.0464P)²+7.5581P] 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         5778
_refine_ls_number_parameters     474
_refine_ls_number_restraints     176
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0628
_refine_ls_wR_factor_ref         0.1448
_refine_ls_wR_factor_gt          0.1438
_refine_ls_goodness_of_fit_ref   1.226
_refine_ls_restrained_S_all      1.209
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.15841(5) 0.00154(4) 0.492455(16) 0.02183(16) Uani 1 1 d . . .
S3 S 0.57811(12) -0.17078(9) 0.70866(3) 0.0309(3) Uani 1 1 d . . .
S2 S -0.11418(12) 0.04650(9) 0.26318(3) 0.0306(2) Uani 1 1 d . . .
S1 S -0.28911(14) -0.07297(11) 0.13829(4) 0.0422(3) Uani 1 1 d . . .
O3 O 0.0289(3) 0.0552(2) 0.53413(8) 0.0239(6) Uani 1 1 d . . .
O2 O 0.1741(3) -0.1430(2) 0.51960(8) 0.0265(6) Uani 1 1 d . . .
O1 O 0.2740(3) -0.0571(2) 0.44898(8) 0.0261(6) Uani 1 1 d . . .
N1 N 0.1413(3) 0.1437(3) 0.46202(10) 0.0232(7) Uani 1 1 d . . .
N2 N 0.3321(3) 0.0592(3) 0.52389(10) 0.0217(7) Uani 1 1 d . . .
C28 C 0.4351(4) -0.2492(3) 0.68231(12) 0.0274(9) Uani 1 1 d . . .
C4 C -0.2605(5) 0.0071(3) 0.18399(12) 0.0280(9) Uani 1 1 d . . .
C22 C 0.3972(4) -0.1122(3) 0.62103(12) 0.0254(8) Uani 1 1 d . . .
H22 H 0.4616 -0.0602 0.6352 0.030 Uiso 1 1 calc R . .
C21 C 0.3824(4) 0.0198(3) 0.56032(12) 0.0222(8) Uani 1 1 d . . .
H21 H 0.4578 0.0618 0.5749 0.027 Uiso 1 1 calc R . .
C24 C 0.2359(4) -0.1622(3) 0.55766(13) 0.0262(8) Uani 1 1 d . . .
C23 C 0.3327(4) -0.0828(3) 0.58037(12) 0.0226(8) Uani 1 1 d . . .
C5 C -0.1403(5) -0.0246(3) 0.21503(12) 0.0269(9) Uani 1 1 d . . .
C6 C -0.0395(5) -0.1123(4) 0.21292(14) 0.0346(10) Uani 1 1 d . . .
H6 H -0.0351 -0.1603 0.1895 0.041 Uiso 1 1 calc R . .
C8 C 0.0324(4) -0.0434(4) 0.28049(12) 0.0273(9) Uani 1 1 d . . .
C9 C 0.1058(4) -0.0342(3) 0.32311(12) 0.0259(8) Uani 1 1 d . . .
C13 C 0.1375(4) 0.0514(3) 0.39359(12) 0.0252(8) Uani 1 1 d . . .
C17 C 0.3266(4) 0.2681(3) 0.50153(12) 0.0233(8) Uani 1 1 d . . .
C27 C 0.3680(4) -0.2160(3) 0.64054(13) 0.0279(9) Uani 1 1 d . . .
C18 C 0.4015(5) 0.3412(3) 0.46870(13) 0.0292(9) Uani 1 1 d . . .
H18A H 0.3585 0.4168 0.4680 0.044 Uiso 1 1 calc R . .
H18B H 0.3860 0.3064 0.4412 0.044 Uiso 1 1 calc R . .
H18C H 0.5071 0.3464 0.4763 0.044 Uiso 1 1 calc R . .
C30 C 0.4923(5) -0.3531(4) 0.74443(13) 0.0341(10) Uani 1 1 d . . .
H30 H 0.4832 -0.4132 0.7635 0.041 Uiso 1 1 calc R . .
C25 C 0.2093(4) -0.2674(3) 0.57757(14) 0.0299(9) Uani 1 1 d . . .
H25 H 0.1475 -0.3212 0.5634 0.036 Uiso 1 1 calc R . .
C14 C 0.0802(4) 0.0536(4) 0.35108(12) 0.0275(9) Uani 1 1 d . . .
H14 H 0.0232 0.1163 0.3415 0.033 Uiso 1 1 calc R . .
C31 C 0.5919(5) -0.2664(4) 0.75106(13) 0.0296(9) Uani 1 1 d . A .
C29 C 0.4038(5) -0.3439(4) 0.70601(13) 0.0325(9) Uani 1 1 d . . .
H29 H 0.3305 -0.3973 0.6974 0.039 Uiso 1 1 calc R . .
C15 C 0.1249(4) 0.1497(3) 0.42125(12) 0.0248(8) Uani 1 1 d . . .
H15 H 0.1038 0.2208 0.4089 0.030 Uiso 1 1 calc R . .
C1 C -0.4399(5) 0.0070(4) 0.12169(14) 0.0364(10) Uani 1 1 d . . .
H1 H -0.4959 -0.0058 0.0962 0.044 Uiso 1 1 calc R . .
C3 C -0.3707(4) 0.0966(3) 0.18729(12) 0.0260(9) Uani 1 1 d . . .
H3 H -0.3770 0.1481 0.2096 0.031 Uiso 1 1 calc R . .
C32 C 0.6991(5) -0.2484(3) 0.78729(13) 0.0297(9) Uani 1 1 d DU . .
C19 C 0.3367(5) 0.3286(4) 0.54462(13) 0.0314(9) Uani 1 1 d . . .
H19A H 0.4392 0.3482 0.5523 0.047 Uiso 1 1 calc R . .
H19B H 0.3001 0.2783 0.5657 0.047 Uiso 1 1 calc R . .
H19C H 0.2770 0.3972 0.5429 0.047 Uiso 1 1 calc R . .
C11 C 0.2613(5) -0.1274(4) 0.37927(13) 0.0331(10) Uani 1 1 d . . .
H11 H 0.3270 -0.1863 0.3877 0.040 Uiso 1 1 calc R . .
C20 C 0.4125(4) 0.1536(3) 0.50421(12) 0.0232(8) Uani 1 1 d . . .
H20A H 0.4346 0.1306 0.4757 0.028 Uiso 1 1 calc R . .
H20B H 0.5073 0.1656 0.5204 0.028 Uiso 1 1 calc R . .
C12 C 0.2240(4) -0.0449(4) 0.40888(13) 0.0271(9) Uani 1 1 d . . .
C2 C -0.4701(5) 0.0908(4) 0.14906(13) 0.0344(10) Uani 1 1 d . . .
H2 H -0.5493 0.1418 0.1439 0.041 Uiso 1 1 calc R . .
C26 C 0.2722(4) -0.2933(4) 0.61747(14) 0.0309(9) Uani 1 1 d . . .
H26 H 0.2508 -0.3637 0.6296 0.037 Uiso 1 1 calc R . .
C16 C 0.1585(4) 0.2477(3) 0.48779(12) 0.0246(8) Uani 1 1 d . . .
H16A H 0.1016 0.2402 0.5128 0.030 Uiso 1 1 calc R . .
H16B H 0.1194 0.3131 0.4715 0.030 Uiso 1 1 calc R . .
C10 C 0.2025(5) -0.1232(4) 0.33786(13) 0.0329(10) Uani 1 1 d . . .
H10 H 0.2274 -0.1806 0.3191 0.040 Uiso 1 1 calc R . .
C7 C 0.0564(5) -0.1225(4) 0.24969(13) 0.0336(10) Uani 1 1 d . . .
H7 H 0.1304 -0.1786 0.2529 0.040 Uiso 1 1 calc R . .
C37 C 0.9266(6) 0.4259(5) 0.5535(3) 0.074(2) Uani 1 1 d . . .
C36 C 0.8232(7) 0.3448(6) 0.5494(3) 0.089(3) Uani 1 1 d . . .
H36A H 0.7574 0.3508 0.5722 0.133 Uiso 1 1 calc R . .
H36B H 0.8706 0.2708 0.5504 0.133 Uiso 1 1 calc R . .
H36C H 0.7663 0.3538 0.5228 0.133 Uiso 1 1 calc R . .
N3 N 1.0114(9) 0.4927(6) 0.5565(6) 0.286(10) Uani 1 1 d . . .
C33 C 0.7971(16) -0.1607(10) 0.7947(5) 0.040(3) Uani 0.83 1 d PDU A 1
H33 H 0.8062 -0.1007 0.7756 0.048 Uiso 0.83 1 calc PR A 1
C34 C 0.8854(10) -0.1673(7) 0.8340(2) 0.0380(15) Uani 0.83 1 d PDU A 1
H34 H 0.9568 -0.1132 0.8434 0.046 Uiso 0.83 1 calc PR A 1
C35 C 0.8512(8) -0.2630(6) 0.8560(2) 0.0360(15) Uani 0.83 1 d PDU A 1
H35 H 0.8971 -0.2831 0.8823 0.043 Uiso 0.83 1 calc PR A 1
S4 S 0.7126(2) -0.34268(15) 0.82937(5) 0.0368(4) Uani 0.83 1 d PDU A 1
S4A S 0.808(2) -0.1344(12) 0.7932(6) 0.035(3) Uani 0.17 1 d PDU A 2
C33A C 0.709(3) -0.326(2) 0.8189(8) 0.031(6) Uani 0.17 1 d PDU A 2
H33A H 0.6543 -0.3934 0.8194 0.037 Uiso 0.17 1 calc PR A 2
C34A C 0.816(4) -0.289(3) 0.8514(9) 0.037(6) Uani 0.17 1 d PDU A 2
H34A H 0.8401 -0.3300 0.8763 0.044 Uiso 0.17 1 calc PR A 2
C35A C 0.878(5) -0.187(3) 0.8414(10) 0.037(6) Uani 0.17 1 d PDU A 2
H35A H 0.9499 -0.1494 0.8588 0.044 Uiso 0.17 1 calc PR A 2


_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
Co1 O2 1.889(3) . ?
Co1 O1 1.897(3) . ?
Co1 N2 1.909(3) . ?
Co1 O3 1.912(3) . ?
Co1 N1 1.915(3) . ?
Co1 O3 1.939(3) 3_556 ?
Co1 Co1 2.9016(10) 3_556 ?
S3 C28 1.737(4) . ?
S3 C31 1.739(4) . ?
S2 C5 1.732(4) . ?
S2 C8 1.736(4) . ?
S1 C1 1.693(5) . ?
S1 C4 1.722(4) . ?
O3 Co1 1.939(2) 3_556 ?
O2 C24 1.308(5) . ?
O1 C12 1.321(5) . ?
N1 C15 1.287(5) . ?
N1 C16 1.462(5) . ?
N2 C21 1.290(5) . ?
N2 C20 1.472(5) . ?
C28 C29 1.372(6) . ?
C28 C27 1.464(5) . ?
C4 C3 1.442(6) . ?
C4 C5 1.453(6) . ?
C22 C27 1.389(6) . ?
C22 C23 1.414(5) . ?
C22 H22 0.9300 . ?
C21 C23 1.437(5) . ?
C21 H21 0.9300 . ?
C24 C25 1.404(6) . ?
C24 C23 1.426(5) . ?
C5 C6 1.366(6) . ?
C6 C7 1.402(6) . ?
C6 H6 0.9300 . ?
C8 C7 1.366(6) . ?
C8 C9 1.461(5) . ?
C9 C14 1.380(6) . ?
C9 C10 1.408(6) . ?
C13 C14 1.404(5) . ?
C13 C12 1.428(6) . ?
C13 C15 1.448(5) . ?
C17 C19 1.528(5) . ?
C17 C18 1.529(5) . ?
C17 C20 1.539(5) . ?
C17 C16 1.554(5) . ?
C27 C26 1.411(6) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C30 C31 1.353(6) . ?
C30 C29 1.407(6) . ?
C30 H30 0.9300 . ?
C25 C26 1.378(6) . ?
C25 H25 0.9300 . ?
C14 H14 0.9300 . ?
C31 C32 1.458(6) . ?
C29 H29 0.9300 . ?
C15 H15 0.9300 . ?
C1 C2 1.342(6) . ?
C1 H1 0.9300 . ?
C3 C2 1.451(6) . ?
C3 H3 0.9300 . ?
C32 C33A 1.341(19) . ?
C32 C33 1.356(12) . ?
C32 S4A 1.650(13) . ?
C32 S4 1.721(4) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C11 C10 1.377(6) . ?
C11 C12 1.396(6) . ?
C11 H11 0.9300 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C2 H2 0.9300 . ?
C26 H26 0.9300 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C10 H10 0.9300 . ?
C7 H7 0.9300 . ?
C37 N3 1.085(9) . ?
C37 C36 1.322(8) . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C33 C34 1.428(15) . ?
C33 H33 0.9300 . ?
C34 C35 1.358(8) . ?
C34 H34 0.9300 . ?
C35 S4 1.722(7) . ?
C35 H35 0.9300 . ?
S4A C35A 1.72(2) . ?
C33A C34A 1.42(2) . ?
C33A H33A 0.9300 . ?
C34A C35A 1.359(17) . ?
C34A H34A 0.9300 . ?
C35A H35A 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Co1 O1 88.82(12) . . ?
O2 Co1 N2 92.55(12) . . ?
O1 Co1 N2 92.26(12) . . ?
O2 Co1 O3 90.58(12) . . ?
O1 Co1 O3 175.67(11) . . ?
N2 Co1 O3 92.05(12) . . ?
O2 Co1 N1 176.86(12) . . ?
O1 Co1 N1 88.73(13) . . ?
N2 Co1 N1 89.51(13) . . ?
O3 Co1 N1 91.72(12) . . ?
O2 Co1 O3 85.91(11) . 3_556 ?
O1 Co1 O3 93.45(11) . 3_556 ?
N2 Co1 O3 174.05(12) . 3_556 ?
O3 Co1 O3 82.23(11) . 3_556 ?
N1 Co1 O3 92.28(12) . 3_556 ?
O2 Co1 Co1 87.65(8) . 3_556 ?
O1 Co1 Co1 134.22(8) . 3_556 ?
N2 Co1 Co1 133.49(9) . 3_556 ?
O3 Co1 Co1 41.46(7) . 3_556 ?
N1 Co1 Co1 92.66(9) . 3_556 ?
O3 Co1 Co1 40.77(8) 3_556 3_556 ?
C28 S3 C31 92.5(2) . . ?
C5 S2 C8 92.5(2) . . ?
C1 S1 C4 91.9(2) . . ?
Co1 O3 Co1 97.77(11) . 3_556 ?
C24 O2 Co1 125.7(2) . . ?
C12 O1 Co1 119.2(2) . . ?
C15 N1 C16 120.8(3) . . ?
C15 N1 Co1 123.3(3) . . ?
C16 N1 Co1 115.9(2) . . ?
C21 N2 C20 119.3(3) . . ?
C21 N2 Co1 124.1(3) . . ?
C20 N2 Co1 116.5(2) . . ?
C29 C28 C27 128.0(4) . . ?
C29 C28 S3 109.4(3) . . ?
C27 C28 S3 122.5(3) . . ?
C3 C4 C5 127.8(4) . . ?
C3 C4 S1 112.8(3) . . ?
C5 C4 S1 119.3(3) . . ?
C27 C22 C23 122.4(4) . . ?
C27 C22 H22 118.8 . . ?
C23 C22 H22 118.8 . . ?
N2 C21 C23 126.1(3) . . ?
N2 C21 H21 117.0 . . ?
C23 C21 H21 117.0 . . ?
O2 C24 C25 119.1(4) . . ?
O2 C24 C23 123.7(4) . . ?
C25 C24 C23 117.1(4) . . ?
C22 C23 C24 119.8(4) . . ?
C22 C23 C21 118.8(3) . . ?
C24 C23 C21 120.9(3) . . ?
C6 C5 C4 128.1(4) . . ?
C6 C5 S2 110.4(3) . . ?
C4 C5 S2 121.4(3) . . ?
C5 C6 C7 113.1(4) . . ?
C5 C6 H6 123.4 . . ?
C7 C6 H6 123.4 . . ?
C7 C8 C9 128.4(4) . . ?
C7 C8 S2 109.5(3) . . ?
C9 C8 S2 122.0(3) . . ?
C14 C9 C10 117.2(4) . . ?
C14 C9 C8 124.0(4) . . ?
C10 C9 C8 118.7(4) . . ?
C14 C13 C12 119.5(4) . . ?
C14 C13 C15 121.6(4) . . ?
C12 C13 C15 118.6(3) . . ?
C19 C17 C18 110.1(3) . . ?
C19 C17 C20 110.5(3) . . ?
C18 C17 C20 106.3(3) . . ?
C19 C17 C16 108.6(3) . . ?
C18 C17 C16 110.8(3) . . ?
C20 C17 C16 110.6(3) . . ?
C22 C27 C26 116.9(4) . . ?
C22 C27 C28 123.4(4) . . ?
C26 C27 C28 119.7(4) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C31 C30 C29 113.8(4) . . ?
C31 C30 H30 123.1 . . ?
C29 C30 H30 123.1 . . ?
C26 C25 C24 121.9(4) . . ?
C26 C25 H25 119.0 . . ?
C24 C25 H25 119.0 . . ?
C9 C14 C13 122.2(4) . . ?
C9 C14 H14 118.9 . . ?
C13 C14 H14 118.9 . . ?
C30 C31 C32 128.3(4) . . ?
C30 C31 S3 110.3(3) . . ?
C32 C31 S3 121.4(3) . . ?
C28 C29 C30 114.0(4) . . ?
C28 C29 H29 123.0 . . ?
C30 C29 H29 123.0 . . ?
N1 C15 C13 123.4(4) . . ?
N1 C15 H15 118.3 . . ?
C13 C15 H15 118.3 . . ?
C2 C1 S1 113.0(4) . . ?
C2 C1 H1 123.5 . . ?
S1 C1 H1 123.5 . . ?
C4 C3 C2 106.9(4) . . ?
C4 C3 H3 126.6 . . ?
C2 C3 H3 126.6 . . ?
C33A C32 C33 111.4(17) . . ?
C33A C32 C31 119.7(13) . . ?
C33 C32 C31 128.9(7) . . ?
C33A C32 S4A 116.5(12) . . ?
C33 C32 S4A 5.5(12) . . ?
C31 C32 S4A 123.8(7) . . ?
C33A C32 S4 2.5(13) . . ?
C33 C32 S4 109.6(7) . . ?
C31 C32 S4 121.5(3) . . ?
S4A C32 S4 114.6(7) . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C10 C11 C12 121.2(4) . . ?
C10 C11 H11 119.4 . . ?
C12 C11 H11 119.4 . . ?
N2 C20 C17 114.5(3) . . ?
N2 C20 H20A 108.6 . . ?
C17 C20 H20A 108.6 . . ?
N2 C20 H20B 108.6 . . ?
C17 C20 H20B 108.6 . . ?
H20A C20 H20B 107.6 . . ?
O1 C12 C11 119.1(4) . . ?
O1 C12 C13 123.3(4) . . ?
C11 C12 C13 117.5(4) . . ?
C1 C2 C3 115.5(4) . . ?
C1 C2 H2 122.3 . . ?
C3 C2 H2 122.3 . . ?
C25 C26 C27 121.9(4) . . ?
C25 C26 H26 119.0 . . ?
C27 C26 H26 119.0 . . ?
N1 C16 C17 110.2(3) . . ?
N1 C16 H16A 109.6 . . ?
C17 C16 H16A 109.6 . . ?
N1 C16 H16B 109.6 . . ?
C17 C16 H16B 109.6 . . ?
H16A C16 H16B 108.1 . . ?
C11 C10 C9 121.9(4) . . ?
C11 C10 H10 119.1 . . ?
C9 C10 H10 119.1 . . ?
C8 C7 C6 114.5(4) . . ?
C8 C7 H7 122.7 . . ?
C6 C7 H7 122.7 . . ?
N3 C37 C36 179.4(14) . . ?
C37 C36 H36A 109.5 . . ?
C37 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C37 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C32 C33 C34 115.1(10) . . ?
C32 C33 H33 122.5 . . ?
C34 C33 H33 122.5 . . ?
C35 C34 C33 110.9(7) . . ?
C35 C34 H34 124.5 . . ?
C33 C34 H34 124.5 . . ?
C34 C35 S4 111.9(5) . . ?
C34 C35 H35 124.1 . . ?
S4 C35 H35 124.1 . . ?
C32 S4 C35 92.5(3) . . ?
C32 S4A C35A 89.4(10) . . ?
C32 C33A C34A 110.3(15) . . ?
C32 C33A H33A 124.9 . . ?
C34A C33A H33A 124.9 . . ?
C35A C34A C33A 111.0(16) . . ?
C35A C34A H34A 124.5 . . ?
C33A C34A H34A 124.5 . . ?
C34A C35A S4A 112.9(16) . . ?
C34A C35A H35A 123.5 . . ?
S4A C35A H35A 123.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 Co1 O3 Co1 -85.79(12) . . . 3_556 ?
N2 Co1 O3 Co1 -178.36(13) . . . 3_556 ?
N1 Co1 O3 Co1 92.07(13) . . . 3_556 ?
O3 Co1 O3 Co1 0.0 3_556 . . 3_556 ?
O1 Co1 O2 C24 119.2(3) . . . . ?
N2 Co1 O2 C24 27.0(3) . . . . ?
O3 Co1 O2 C24 -65.1(3) . . . . ?
O3 Co1 O2 C24 -147.2(3) 3_556 . . . ?
Co1 Co1 O2 C24 -106.4(3) 3_556 . . . ?
O2 Co1 O1 C12 129.1(3) . . . . ?
N2 Co1 O1 C12 -138.4(3) . . . . ?
N1 Co1 O1 C12 -49.0(3) . . . . ?
O3 Co1 O1 C12 43.2(3) 3_556 . . . ?
Co1 Co1 O1 C12 43.5(3) 3_556 . . . ?
O1 Co1 N1 C15 38.0(3) . . . . ?
N2 Co1 N1 C15 130.3(3) . . . . ?
O3 Co1 N1 C15 -137.7(3) . . . . ?
O3 Co1 N1 C15 -55.4(3) 3_556 . . . ?
Co1 Co1 N1 C15 -96.2(3) 3_556 . . . ?
O1 Co1 N1 C16 -137.9(3) . . . . ?
N2 Co1 N1 C16 -45.6(3) . . . . ?
O3 Co1 N1 C16 46.4(3) . . . . ?
O3 Co1 N1 C16 128.7(2) 3_556 . . . ?
Co1 Co1 N1 C16 87.9(2) 3_556 . . . ?
O2 Co1 N2 C21 -23.8(3) . . . . ?
O1 Co1 N2 C21 -112.7(3) . . . . ?
O3 Co1 N2 C21 66.9(3) . . . . ?
N1 Co1 N2 C21 158.6(3) . . . . ?
Co1 Co1 N2 C21 65.4(3) 3_556 . . . ?
O2 Co1 N2 C20 155.3(3) . . . . ?
O1 Co1 N2 C20 66.4(3) . . . . ?
O3 Co1 N2 C20 -114.0(3) . . . . ?
N1 Co1 N2 C20 -22.3(3) . . . . ?
Co1 Co1 N2 C20 -115.5(2) 3_556 . . . ?
C31 S3 C28 C29 -0.3(3) . . . . ?
C31 S3 C28 C27 -178.3(3) . . . . ?
C1 S1 C4 C3 1.1(3) . . . . ?
C1 S1 C4 C5 177.4(3) . . . . ?
C20 N2 C21 C23 -169.1(3) . . . . ?
Co1 N2 C21 C23 10.1(5) . . . . ?
Co1 O2 C24 C25 165.3(3) . . . . ?
Co1 O2 C24 C23 -15.9(5) . . . . ?
C27 C22 C23 C24 -1.2(6) . . . . ?
C27 C22 C23 C21 -172.7(3) . . . . ?
O2 C24 C23 C22 -178.5(3) . . . . ?
C25 C24 C23 C22 0.2(5) . . . . ?
O2 C24 C23 C21 -7.3(6) . . . . ?
C25 C24 C23 C21 171.5(3) . . . . ?
N2 C21 C23 C22 -178.4(4) . . . . ?
N2 C21 C23 C24 10.3(6) . . . . ?
C3 C4 C5 C6 176.9(4) . . . . ?
S1 C4 C5 C6 1.2(6) . . . . ?
C3 C4 C5 S2 0.2(6) . . . . ?
S1 C4 C5 S2 -175.5(2) . . . . ?
C8 S2 C5 C6 -0.4(3) . . . . ?
C8 S2 C5 C4 176.9(3) . . . . ?
C4 C5 C6 C7 -176.6(4) . . . . ?
S2 C5 C6 C7 0.5(5) . . . . ?
C5 S2 C8 C7 0.2(3) . . . . ?
C5 S2 C8 C9 -176.2(3) . . . . ?
C7 C8 C9 C14 175.7(4) . . . . ?
S2 C8 C9 C14 -8.6(6) . . . . ?
C7 C8 C9 C10 -8.0(6) . . . . ?
S2 C8 C9 C10 167.6(3) . . . . ?
C23 C22 C27 C26 1.3(6) . . . . ?
C23 C22 C27 C28 179.0(4) . . . . ?
C29 C28 C27 C22 173.5(4) . . . . ?
S3 C28 C27 C22 -9.0(6) . . . . ?
C29 C28 C27 C26 -8.9(6) . . . . ?
S3 C28 C27 C26 168.6(3) . . . . ?
O2 C24 C25 C26 179.5(4) . . . . ?
C23 C24 C25 C26 0.6(6) . . . . ?
C10 C9 C14 C13 -5.0(6) . . . . ?
C8 C9 C14 C13 171.3(4) . . . . ?
C12 C13 C14 C9 -0.6(6) . . . . ?
C15 C13 C14 C9 172.7(4) . . . . ?
C29 C30 C31 C32 179.5(4) . . . . ?
C29 C30 C31 S3 -0.5(5) . . . . ?
C28 S3 C31 C30 0.5(3) . . . . ?
C28 S3 C31 C32 -179.5(3) . . . . ?
C27 C28 C29 C30 177.9(4) . . . . ?
S3 C28 C29 C30 0.1(5) . . . . ?
C31 C30 C29 C28 0.3(6) . . . . ?
C16 N1 C15 C13 167.1(3) . . . . ?
Co1 N1 C15 C13 -8.6(5) . . . . ?
C14 C13 C15 N1 162.4(4) . . . . ?
C12 C13 C15 N1 -24.2(6) . . . . ?
C4 S1 C1 C2 -0.3(4) . . . . ?
C5 C4 C3 C2 -177.5(4) . . . . ?
S1 C4 C3 C2 -1.5(4) . . . . ?
C30 C31 C32 C33A 1.8(17) . . . . ?
S3 C31 C32 C33A -178.2(16) . . . . ?
C30 C31 C32 C33 -178.5(9) . . . . ?
S3 C31 C32 C33 1.5(10) . . . . ?
C30 C31 C32 S4A -176.0(9) . . . . ?
S3 C31 C32 S4A 4.0(10) . . . . ?
C30 C31 C32 S4 -0.2(6) . . . . ?
S3 C31 C32 S4 179.8(2) . . . . ?
C21 N2 C20 C17 -112.0(4) . . . . ?
Co1 N2 C20 C17 68.8(4) . . . . ?
C19 C17 C20 N2 78.2(4) . . . . ?
C18 C17 C20 N2 -162.4(3) . . . . ?
C16 C17 C20 N2 -42.1(4) . . . . ?
Co1 O1 C12 C11 -149.8(3) . . . . ?
Co1 O1 C12 C13 32.6(5) . . . . ?
C10 C11 C12 O1 174.9(4) . . . . ?
C10 C11 C12 C13 -7.4(6) . . . . ?
C14 C13 C12 O1 -175.6(4) . . . . ?
C15 C13 C12 O1 10.9(6) . . . . ?
C14 C13 C12 C11 6.8(6) . . . . ?
C15 C13 C12 C11 -166.7(4) . . . . ?
S1 C1 C2 C3 -0.6(5) . . . . ?
C4 C3 C2 C1 1.3(5) . . . . ?
C24 C25 C26 C27 -0.6(6) . . . . ?
C22 C27 C26 C25 -0.4(6) . . . . ?
C28 C27 C26 C25 -178.2(4) . . . . ?
C15 N1 C16 C17 -99.9(4) . . . . ?
Co1 N1 C16 C17 76.1(3) . . . . ?
C19 C17 C16 N1 -149.2(3) . . . . ?
C18 C17 C16 N1 89.8(4) . . . . ?
C20 C17 C16 N1 -27.8(4) . . . . ?
C12 C11 C10 C9 1.8(7) . . . . ?
C14 C9 C10 C11 4.5(6) . . . . ?
C8 C9 C10 C11 -172.0(4) . . . . ?
C9 C8 C7 C6 176.1(4) . . . . ?
S2 C8 C7 C6 0.0(5) . . . . ?
C5 C6 C7 C8 -0.3(6) . . . . ?
C33A C32 C33 C34 -2(2) . . . . ?
C31 C32 C33 C34 178.7(6) . . . . ?
S4A C32 C33 C34 156(15) . . . . ?
S4 C32 C33 C34 0.3(11) . . . . ?
C32 C33 C34 C35 0.2(12) . . . . ?
C33 C34 C35 S4 -0.6(9) . . . . ?
C33A C32 S4 C35 137(32) . . . . ?
C33 C32 S4 C35 -0.5(7) . . . . ?
C31 C32 S4 C35 -179.1(4) . . . . ?
S4A C32 S4 C35 -2.9(9) . . . . ?
C34 C35 S4 C32 0.6(6) . . . . ?
C33A C32 S4A C35A 0(2) . . . . ?
C33 C32 S4A C35A -23(14) . . . . ?
C31 C32 S4A C35A 177.8(18) . . . . ?
S4 C32 S4A C35A 1.7(18) . . . . ?
C33 C32 C33A C34A 2(2) . . . . ?
C31 C32 C33A C34A -177.8(14) . . . . ?
S4A C32 C33A C34A 0.1(18) . . . . ?
S4 C32 C33A C34A -40(31) . . . . ?
C32 C33A C34A C35A 0(2) . . . . ?
C33A C34A C35A S4A 0(3) . . . . ?
C32 S4A C35A C34A 0(3) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.766
_refine_diff_density_min         -0.868
_refine_diff_density_rms         0.079
####################################################################### 
# 
# 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_cul3c4
_database_code_depnum_ccdc_archive 'CCDC 1544972'
_audit_update_record             
;
2017-04-20 deposited with the CCDC.
2017-06-20 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT341_cul3c4              
;
PROBLEM: Low Bond Precision on  C-C Bonds
RESPONSE: This result is to be expected given the disorder of the n-butyl groups.
;
# end Validation Reply Form
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C59 H64 Cl0 Cu N2 O2 S6'
_chemical_formula_weight         1089.02

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c n'

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

_cell_length_a                   29.325(16)
_cell_length_b                   20.484(11)
_cell_length_c                   9.653(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5798(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    12855
_cell_measurement_theta_min      1.3888
_cell_measurement_theta_max      25.0313

_exptl_crystal_description       needle
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2292
_exptl_absorpt_coefficient_mu    0.634
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8836
_exptl_absorpt_correction_T_max  0.9751
_exptl_absorpt_process_details   'The Rigaku Corporation, Tokyo, Japan'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(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  
;
Mercury2 (2x2 bin mode)
;
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            81863
_diffrn_reflns_av_R_equivalents  0.1058
_diffrn_reflns_av_sigmaI/netI    0.0403
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.31
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5103
_reflns_number_gt                5023
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_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)+(0.0413P)²+58.3792P] 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         5103
_refine_ls_number_parameters     417
_refine_ls_number_restraints     413
_refine_ls_R_factor_all          0.1139
_refine_ls_R_factor_gt           0.1134
_refine_ls_wR_factor_ref         0.3267
_refine_ls_wR_factor_gt          0.3260
_refine_ls_goodness_of_fit_ref   1.365
_refine_ls_restrained_S_all      1.317
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.002

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
Cu1 Cu 0.0000 0.99878(9) 0.7500 0.0560(5) Uani 1 2 d S . .
S2 S 0.26472(10) 1.10586(14) 0.0390(4) 0.0685(9) Uani 1 1 d . A .
S3 S 0.21005(10) 1.01910(12) 0.2587(4) 0.0617(8) Uani 1 1 d . A .
O1 O 0.0414(2) 0.9333(3) 0.6903(8) 0.0535(18) Uani 1 1 d . . .
N1 N 0.0239(3) 1.0650(4) 0.6249(8) 0.0453(19) Uani 1 1 d . . .
C4 C 0.324(3) 1.1890(11) -0.084(7) 0.096(6) Uani 0.61 1 d PDU A 1
S1 S 0.2848(4) 1.2321(5) -0.1689(15) 0.116(3) Uani 0.61 1 d PDU A 1
C1 C 0.3196(10) 1.2981(14) -0.176(4) 0.112(6) Uani 0.61 1 d PDU A 1
H1 H 0.3110 1.3372 -0.2218 0.134 Uiso 0.61 1 calc PR A 1
C2 C 0.3587(12) 1.2919(17) -0.114(4) 0.125(7) Uani 0.61 1 d PDU A 1
H2 H 0.3823 1.3237 -0.1114 0.150 Uiso 0.61 1 calc PR A 1
C3 C 0.3600(14) 1.231(2) -0.051(5) 0.121(8) Uani 0.61 1 d PDU A 1
H3 H 0.3839 1.2180 0.0098 0.145 Uiso 0.61 1 calc PR A 1
C4A C 0.324(3) 1.1892(15) -0.081(10) 0.102(7) Uani 0.39 1 d PDU A 2
C3A C 0.2906(19) 1.232(3) -0.126(8) 0.112(8) Uani 0.39 1 d PDU A 2
H3A H 0.2593 1.2198 -0.1247 0.135 Uiso 0.39 1 calc PR A 2
C2A C 0.3054(14) 1.293(2) -0.172(6) 0.120(8) Uani 0.39 1 d PDU A 2
H2A H 0.2866 1.3260 -0.2090 0.145 Uiso 0.39 1 calc PR A 2
C1A C 0.3493(13) 1.296(2) -0.155(7) 0.125(8) Uani 0.39 1 d PDU A 2
H1A H 0.3663 1.3336 -0.1780 0.150 Uiso 0.39 1 calc PR A 2
S1A S 0.3744(6) 1.2275(10) -0.090(2) 0.120(5) Uani 0.39 1 d PDU A 2
C5 C 0.3165(4) 1.1215(6) -0.0367(15) 0.077(4) Uani 1 1 d D . .
C6 C 0.3435(4) 1.0684(7) -0.0389(14) 0.072(4) Uani 1 1 d . A .
C7 C 0.3917(5) 1.0663(7) -0.0980(17) 0.096(5) Uani 1 1 d D . .
H7A H 0.3939 1.0981 -0.1749 0.115 Uiso 1 1 calc R A 1
H7B H 0.3974 1.0223 -0.1368 0.115 Uiso 1 1 calc R A 1
C8 C 0.4293(13) 1.082(6) 0.011(4) 0.124(12) Uani 0.60 1 d PDU A 1
H8A H 0.4322 1.0467 0.0804 0.149 Uiso 0.60 1 calc PR A 1
H8B H 0.4233 1.1238 0.0588 0.149 Uiso 0.60 1 calc PR A 1
C9 C 0.4727(11) 1.086(2) -0.084(4) 0.138(11) Uani 0.60 1 d PDU A 1
H9A H 0.4683 1.1202 -0.1561 0.165 Uiso 0.60 1 calc PR A 1
H9B H 0.4780 1.0439 -0.1308 0.165 Uiso 0.60 1 calc PR A 1
C10 C 0.5145(10) 1.104(2) 0.010(4) 0.152(13) Uani 0.60 1 d PDU A 1
H10A H 0.5387 1.1234 -0.0464 0.229 Uiso 0.60 1 calc PR A 1
H10B H 0.5259 1.0646 0.0555 0.229 Uiso 0.60 1 calc PR A 1
H10C H 0.5048 1.1356 0.0811 0.229 Uiso 0.60 1 calc PR A 1
C8A C 0.4267(18) 1.074(10) 0.023(5) 0.124(14) Uani 0.40 1 d PDU A 2
H8A1 H 0.4229 1.0352 0.0837 0.149 Uiso 0.40 1 calc PR A 2
H8A2 H 0.4171 1.1123 0.0777 0.149 Uiso 0.40 1 calc PR A 2
C9A C 0.4791(18) 1.081(4) -0.004(6) 0.134(12) Uani 0.40 1 d PDU A 2
H9A1 H 0.4836 1.1190 -0.0674 0.161 Uiso 0.40 1 calc PR A 2
H9A2 H 0.4899 1.0419 -0.0532 0.161 Uiso 0.40 1 calc PR A 2
C10A C 0.5099(19) 1.092(4) 0.127(5) 0.163(19) Uani 0.40 1 d PDU A 2
H10D H 0.4930 1.1171 0.1962 0.245 Uiso 0.40 1 calc PR A 2
H10E H 0.5375 1.1158 0.1002 0.245 Uiso 0.40 1 calc PR A 2
H10F H 0.5184 1.0494 0.1656 0.245 Uiso 0.40 1 calc PR A 2
C13 C 0.3355(5) 0.9039(6) -0.1016(16) 0.086(4) Uani 1 1 d D . .
H13A H 0.3533 0.9223 -0.1796 0.103 Uiso 1 1 calc R B 1
H13B H 0.3028 0.9046 -0.1273 0.103 Uiso 1 1 calc R B 1
C14 C 0.3431(4) 0.9442(6) 0.0273(17) 0.087(4) Uani 1 1 d . A .
H14A H 0.3299 0.9208 0.1077 0.104 Uiso 1 1 calc R . .
H14B H 0.3763 0.9486 0.0434 0.104 Uiso 1 1 calc R . .
C15 C 0.3223(4) 1.0107(5) 0.0186(12) 0.061(3) Uani 1 1 d . . .
C16 C 0.2793(4) 1.0240(5) 0.0667(12) 0.059(3) Uani 1 1 d . A .
C17 C 0.2462(3) 0.9836(5) 0.1372(11) 0.053(3) Uani 1 1 d . . .
C18 C 0.2346(4) 0.9189(6) 0.1274(15) 0.077(4) Uani 1 1 d . A .
H18 H 0.2497 0.8897 0.0664 0.092 Uiso 1 1 calc R . .
C19 C 0.1989(4) 0.8992(6) 0.2141(13) 0.071(4) Uani 1 1 d . . .
H19 H 0.1878 0.8557 0.2172 0.085 Uiso 1 1 calc R A .
C20 C 0.1816(4) 0.9478(5) 0.2929(13) 0.068(3) Uani 1 1 d . A .
C21 C 0.1457(3) 0.9463(5) 0.3969(12) 0.053(3) Uani 1 1 d . . .
C22 C 0.1390(3) 0.8902(5) 0.4767(11) 0.055(3) Uani 1 1 d . A .
H22 H 0.1583 0.8536 0.4631 0.066 Uiso 1 1 calc R . .
C23 C 0.1049(4) 0.8868(5) 0.5746(12) 0.055(3) Uani 1 1 d . . .
H23 H 0.1010 0.8475 0.6255 0.066 Uiso 1 1 calc R A .
C24 C 0.0751(3) 0.9408(5) 0.6021(11) 0.048(2) Uani 1 1 d . A .
C25 C 0.0831(3) 0.9991(5) 0.5238(10) 0.047(2) Uani 1 1 d . . .
C26 C 0.1179(3) 0.9996(5) 0.4247(12) 0.057(3) Uani 1 1 d . A .
H26 H 0.1228 1.0386 0.3736 0.069 Uiso 1 1 calc R . .
C27 C 0.0551(3) 1.0568(4) 0.5399(9) 0.044(2) Uani 1 1 d . A .
H27 H 0.0614 1.0922 0.4791 0.052 Uiso 1 1 calc R . .
C28 C -0.0041(4) 1.1263(4) 0.6197(12) 0.061(3) Uani 1 1 d . . .
H28A H -0.0365 1.1143 0.6064 0.073 Uiso 1 1 calc R . .
H28B H 0.0055 1.1523 0.5383 0.073 Uiso 1 1 calc R . .
C29 C 0.0000 1.1691(7) 0.7500 0.058(4) Uani 1 2 d S . .
C30 C 0.0430(4) 1.2115(5) 0.7420(15) 0.071(3) Uani 1 1 d . . .
H30A H 0.0398 1.2430 0.6662 0.106 Uiso 1 1 calc R . .
H30B H 0.0696 1.1837 0.7251 0.106 Uiso 1 1 calc R . .
H30C H 0.0470 1.2349 0.8297 0.106 Uiso 1 1 calc R . .
C11 C 0.3452(9) 0.7937(11) -0.201(3) 0.097(8) Uani 0.60 1 d PDU C 1
H11A H 0.3126 0.7897 -0.2225 0.146 Uiso 0.60 1 calc PR C 1
H11B H 0.3585 0.7502 -0.1898 0.146 Uiso 0.60 1 calc PR C 1
H11C H 0.3606 0.8163 -0.2779 0.146 Uiso 0.60 1 calc PR C 1
C12 C 0.3512(9) 0.8317(9) -0.072(3) 0.076(7) Uani 0.60 1 d PDU C 1
H12A H 0.3835 0.8309 -0.0429 0.091 Uiso 0.60 1 calc PR C 1
H12B H 0.3325 0.8125 0.0031 0.091 Uiso 0.60 1 calc PR C 1
C11A C 0.3519(18) 0.798(2) -0.010(5) 0.124(15) Uani 0.40 1 d PDU C 2
H11D H 0.3589 0.8202 0.0775 0.186 Uiso 0.40 1 calc PR C 2
H11E H 0.3686 0.7570 -0.0154 0.186 Uiso 0.40 1 calc PR C 2
H11F H 0.3190 0.7898 -0.0155 0.186 Uiso 0.40 1 calc PR C 2
C12A C 0.3657(12) 0.8411(13) -0.128(4) 0.080(10) Uani 0.40 1 d PDU C 2
H12C H 0.3585 0.8207 -0.2184 0.095 Uiso 0.40 1 calc PR C 2
H12D H 0.3986 0.8515 -0.1245 0.095 Uiso 0.40 1 calc PR C 2


_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
Cu1 O1 1.900(7) 4_556 ?
Cu1 O1 1.900(7) . ?
Cu1 N1 1.946(8) 4_556 ?
Cu1 N1 1.946(8) . ?
S2 C5 1.715(13) . ?
S2 C16 1.752(11) . ?
S3 C20 1.714(12) . ?
S3 C17 1.740(10) . ?
O1 C24 1.312(12) . ?
N1 C27 1.240(11) . ?
N1 C28 1.501(12) . ?
C4 C3 1.39(8) . ?
C4 C5 1.474(18) . ?
C4 S1 1.67(7) . ?
S1 C1 1.70(3) . ?
C1 C2 1.30(3) . ?
C1 H1 0.9500 . ?
C2 C3 1.40(5) . ?
C2 H2 0.9500 . ?
C3 H3 0.9500 . ?
C4A C3A 1.39(8) . ?
C4A C5 1.47(2) . ?
C4A S1A 1.66(8) . ?
C3A C2A 1.40(5) . ?
C3A H3A 0.9500 . ?
C2A C1A 1.30(3) . ?
C2A H2A 0.9500 . ?
C1A S1A 1.70(3) . ?
C1A H1A 0.9500 . ?
C5 C6 1.347(17) . ?
C6 C15 1.445(16) . ?
C6 C7 1.523(17) . ?
C7 C8 1.56(2) . ?
C7 C8A 1.56(2) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.571(19) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.57(2) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C8A C9A 1.57(2) . ?
C8A H8A1 0.9900 . ?
C8A H8A2 0.9900 . ?
C9A C10A 1.57(2) . ?
C9A H9A1 0.9900 . ?
C9A H9A2 0.9900 . ?
C10A H10D 0.9800 . ?
C10A H10E 0.9800 . ?
C10A H10F 0.9800 . ?
C13 C14 1.509(18) . ?
C13 C12 1.58(2) . ?
C13 C12A 1.58(2) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.496(16) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.372(14) . ?
C16 C17 1.445(14) . ?
C17 C18 1.371(15) . ?
C18 C19 1.402(16) . ?
C18 H18 0.9500 . ?
C19 C20 1.351(16) . ?
C19 H19 0.9500 . ?
C20 C21 1.455(16) . ?
C21 C26 1.389(14) . ?
C21 C22 1.397(14) . ?
C22 C23 1.376(14) . ?
C22 H22 0.9500 . ?
C23 C24 1.436(14) . ?
C23 H23 0.9500 . ?
C24 C25 1.431(13) . ?
C25 C26 1.399(14) . ?
C25 C27 1.447(13) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C28 C29 1.537(13) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.533(12) . ?
C29 C30 1.533(12) 4_556 ?
C29 C28 1.537(13) 4_556 ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C11 C12 1.48(3) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C11A C12A 1.49(3) . ?
C11A H11D 0.9800 . ?
C11A H11E 0.9800 . ?
C11A H11F 0.9800 . ?
C12A H12C 0.9900 . ?
C12A H12D 0.9900 . ?

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 Cu1 O1 90.1(4) 4_556 . ?
O1 Cu1 N1 94.2(3) 4_556 4_556 ?
O1 Cu1 N1 155.6(3) . 4_556 ?
O1 Cu1 N1 155.6(3) 4_556 . ?
O1 Cu1 N1 94.2(3) . . ?
N1 Cu1 N1 91.7(5) 4_556 . ?
C5 S2 C16 91.6(5) . . ?
C20 S3 C17 94.1(5) . . ?
C24 O1 Cu1 126.4(6) . . ?
C27 N1 C28 119.6(9) . . ?
C27 N1 Cu1 125.6(7) . . ?
C28 N1 Cu1 114.0(6) . . ?
C3 C4 C5 128(6) . . ?
C3 C4 S1 108(2) . . ?
C5 C4 S1 123(5) . . ?
C4 S1 C1 91(2) . . ?
C2 C1 S1 116(3) . . ?
C2 C1 H1 122.1 . . ?
S1 C1 H1 122.1 . . ?
C1 C2 C3 108(4) . . ?
C1 C2 H2 125.9 . . ?
C3 C2 H2 125.9 . . ?
C4 C3 C2 116(4) . . ?
C4 C3 H3 122.2 . . ?
C2 C3 H3 122.2 . . ?
C3A C4A C5 125(7) . . ?
C3A C4A S1A 108(2) . . ?
C5 C4A S1A 127(6) . . ?
C4A C3A C2A 116(5) . . ?
C4A C3A H3A 122.0 . . ?
C2A C3A H3A 122.1 . . ?
C1A C2A C3A 108(4) . . ?
C1A C2A H2A 125.9 . . ?
C3A C2A H2A 125.9 . . ?
C2A C1A S1A 116(4) . . ?
C2A C1A H1A 122.1 . . ?
S1A C1A H1A 122.1 . . ?
C4A S1A C1A 92(2) . . ?
C6 C5 C4A 132(3) . . ?
C6 C5 C4 132(3) . . ?
C4A C5 C4 1(7) . . ?
C6 C5 S2 112.2(9) . . ?
C4A C5 S2 116(3) . . ?
C4 C5 S2 116(2) . . ?
C5 C6 C15 113.6(10) . . ?
C5 C6 C7 125.1(12) . . ?
C15 C6 C7 121.3(12) . . ?
C6 C7 C8 113(2) . . ?
C6 C7 C8A 109(3) . . ?
C8 C7 C8A 8(9) . . ?
C6 C7 H7A 108.9 . . ?
C8 C7 H7A 108.9 . . ?
C8A C7 H7A 116.9 . . ?
C6 C7 H7B 108.9 . . ?
C8 C7 H7B 108.9 . . ?
C8A C7 H7B 105.2 . . ?
H7A C7 H7B 107.7 . . ?
C7 C8 C9 101(2) . . ?
C7 C8 H8A 111.6 . . ?
C9 C8 H8A 111.6 . . ?
C7 C8 H8B 111.6 . . ?
C9 C8 H8B 111.6 . . ?
H8A C8 H8B 109.4 . . ?
C8 C9 C10 108(3) . . ?
C8 C9 H9A 110.2 . . ?
C10 C9 H9A 110.2 . . ?
C8 C9 H9B 110.2 . . ?
C10 C9 H9B 110.2 . . ?
H9A C9 H9B 108.5 . . ?
C7 C8A C9A 122(4) . . ?
C7 C8A H8A1 106.8 . . ?
C9A C8A H8A1 106.8 . . ?
C7 C8A H8A2 106.8 . . ?
C9A C8A H8A2 106.8 . . ?
H8A1 C8A H8A2 106.7 . . ?
C8A C9A C10A 116(4) . . ?
C8A C9A H9A1 108.2 . . ?
C10A C9A H9A1 108.2 . . ?
C8A C9A H9A2 108.2 . . ?
C10A C9A H9A2 108.2 . . ?
H9A1 C9A H9A2 107.4 . . ?
C9A C10A H10D 109.5 . . ?
C9A C10A H10E 109.5 . . ?
H10D C10A H10E 109.5 . . ?
C9A C10A H10F 109.5 . . ?
H10D C10A H10F 109.5 . . ?
H10E C10A H10F 109.5 . . ?
C14 C13 C12 108.7(14) . . ?
C14 C13 C12A 119.7(19) . . ?
C12 C13 C12A 26.2(12) . . ?
C14 C13 H13A 109.9 . . ?
C12 C13 H13A 109.9 . . ?
C12A C13 H13A 83.8 . . ?
C14 C13 H13B 109.9 . . ?
C12 C13 H13B 109.9 . . ?
C12A C13 H13B 120.9 . . ?
H13A C13 H13B 108.3 . . ?
C15 C14 C13 113.1(12) . . ?
C15 C14 H14A 109.0 . . ?
C13 C14 H14A 109.0 . . ?
C15 C14 H14B 109.0 . . ?
C13 C14 H14B 109.0 . . ?
H14A C14 H14B 107.8 . . ?
C16 C15 C6 111.4(10) . . ?
C16 C15 C14 122.4(11) . . ?
C6 C15 C14 126.2(10) . . ?
C15 C16 C17 131.6(10) . . ?
C15 C16 S2 111.2(8) . . ?
C17 C16 S2 117.1(8) . . ?
C18 C17 C16 133.4(10) . . ?
C18 C17 S3 107.4(8) . . ?
C16 C17 S3 119.2(8) . . ?
C17 C18 C19 115.0(11) . . ?
C17 C18 H18 122.5 . . ?
C19 C18 H18 122.5 . . ?
C20 C19 C18 113.9(11) . . ?
C20 C19 H19 123.1 . . ?
C18 C19 H19 123.1 . . ?
C19 C20 C21 130.0(11) . . ?
C19 C20 S3 109.7(10) . . ?
C21 C20 S3 120.3(8) . . ?
C26 C21 C22 117.2(10) . . ?
C26 C21 C20 122.7(10) . . ?
C22 C21 C20 120.1(10) . . ?
C23 C22 C21 121.5(10) . . ?
C23 C22 H22 119.2 . . ?
C21 C22 H22 119.2 . . ?
C22 C23 C24 122.0(9) . . ?
C22 C23 H23 119.0 . . ?
C24 C23 H23 119.0 . . ?
O1 C24 C25 124.4(9) . . ?
O1 C24 C23 119.1(9) . . ?
C25 C24 C23 116.4(9) . . ?
C26 C25 C24 119.1(10) . . ?
C26 C25 C27 118.7(9) . . ?
C24 C25 C27 122.1(9) . . ?
C21 C26 C25 123.7(10) . . ?
C21 C26 H26 118.1 . . ?
C25 C26 H26 118.1 . . ?
N1 C27 C25 126.8(9) . . ?
N1 C27 H27 116.6 . . ?
C25 C27 H27 116.6 . . ?
N1 C28 C29 114.0(9) . . ?
N1 C28 H28A 108.7 . . ?
C29 C28 H28A 108.7 . . ?
N1 C28 H28B 108.7 . . ?
C29 C28 H28B 108.7 . . ?
H28A C28 H28B 107.6 . . ?
C30 C29 C30 110.9(12) . 4_556 ?
C30 C29 C28 110.2(7) . . ?
C30 C29 C28 107.5(7) 4_556 . ?
C30 C29 C28 107.5(7) . 4_556 ?
C30 C29 C28 110.2(7) 4_556 4_556 ?
C28 C29 C28 110.5(11) . 4_556 ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C11 C12 C13 107.8(18) . . ?
C11 C12 H12A 110.2 . . ?
C13 C12 H12A 110.2 . . ?
C11 C12 H12B 110.2 . . ?
C13 C12 H12B 110.2 . . ?
H12A C12 H12B 108.5 . . ?
C12A C11A H11D 109.5 . . ?
C12A C11A H11E 109.5 . . ?
H11D C11A H11E 109.5 . . ?
C12A C11A H11F 109.4 . . ?
H11D C11A H11F 109.5 . . ?
H11E C11A H11F 109.5 . . ?
C11A C12A C13 102(2) . . ?
C11A C12A H12C 111.5 . . ?
C13 C12A H12C 111.4 . . ?
C11A C12A H12D 111.4 . . ?
C13 C12A H12D 111.4 . . ?
H12C C12A H12D 109.3 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 Cu1 O1 C24 160.9(9) 4_556 . . . ?
N1 Cu1 O1 C24 -98.7(11) 4_556 . . . ?
N1 Cu1 O1 C24 4.9(8) . . . . ?
O1 Cu1 N1 C27 -98.1(11) 4_556 . . . ?
O1 Cu1 N1 C27 1.6(9) . . . . ?
N1 Cu1 N1 C27 157.9(10) 4_556 . . . ?
O1 Cu1 N1 C28 71.7(11) 4_556 . . . ?
O1 Cu1 N1 C28 171.3(7) . . . . ?
N1 Cu1 N1 C28 -32.4(6) 4_556 . . . ?
C3 C4 S1 C1 7(2) . . . . ?
C5 C4 S1 C1 178(4) . . . . ?
C4 S1 C1 C2 -2.6(15) . . . . ?
S1 C1 C2 C3 -2.7(18) . . . . ?
C5 C4 C3 C2 179(4) . . . . ?
S1 C4 C3 C2 -10(4) . . . . ?
C1 C2 C3 C4 8(3) . . . . ?
C5 C4A C3A C2A -176(8) . . . . ?
S1A C4A C3A C2A 3(3) . . . . ?
C4A C3A C2A C1A -3(3) . . . . ?
C3A C2A C1A S1A 1.6(19) . . . . ?
C3A C4A S1A C1A -1(2) . . . . ?
C5 C4A S1A C1A 177(8) . . . . ?
C2A C1A S1A C4A -0.2(17) . . . . ?
C3A C4A C5 C6 152(3) . . . . ?
S1A C4A C5 C6 -26(10) . . . . ?
C3A C4A C5 C4 67(100) . . . . ?
S1A C4A C5 C4 -111(100) . . . . ?
C3A C4A C5 S2 -31(6) . . . . ?
S1A C4A C5 S2 151(5) . . . . ?
C3 C4 C5 C6 -52(6) . . . . ?
S1 C4 C5 C6 138(3) . . . . ?
C3 C4 C5 C4A 43(100) . . . . ?
S1 C4 C5 C4A -126(100) . . . . ?
C3 C4 C5 S2 126(4) . . . . ?
S1 C4 C5 S2 -44(4) . . . . ?
C16 S2 C5 C6 -1.0(12) . . . . ?
C16 S2 C5 C4A -178(5) . . . . ?
C16 S2 C5 C4 -180(4) . . . . ?
C4A C5 C6 C15 179(6) . . . . ?
C4 C5 C6 C15 180(4) . . . . ?
S2 C5 C6 C15 1.8(16) . . . . ?
C4A C5 C6 C7 -3(6) . . . . ?
C4 C5 C6 C7 -1(5) . . . . ?
S2 C5 C6 C7 -179.5(11) . . . . ?
C5 C6 C7 C8 91(5) . . . . ?
C15 C6 C7 C8 -91(5) . . . . ?
C5 C6 C7 C8A 98(8) . . . . ?
C15 C6 C7 C8A -83(8) . . . . ?
C6 C7 C8 C9 -172(4) . . . . ?
C8A C7 C8 C9 130(67) . . . . ?
C7 C8 C9 C10 178(5) . . . . ?
C6 C7 C8A C9A -173(10) . . . . ?
C8 C7 C8A C9A -49(51) . . . . ?
C7 C8A C9A C10A 177(11) . . . . ?
C12 C13 C14 C15 -170.4(14) . . . . ?
C12A C13 C14 C15 163.4(18) . . . . ?
C5 C6 C15 C16 -1.8(17) . . . . ?
C7 C6 C15 C16 179.5(12) . . . . ?
C5 C6 C15 C14 178.3(13) . . . . ?
C7 C6 C15 C14 0(2) . . . . ?
C13 C14 C15 C16 93.0(15) . . . . ?
C13 C14 C15 C6 -87.0(15) . . . . ?
C6 C15 C16 C17 -176.8(12) . . . . ?
C14 C15 C16 C17 3(2) . . . . ?
C6 C15 C16 S2 0.9(13) . . . . ?
C14 C15 C16 S2 -179.1(10) . . . . ?
C5 S2 C16 C15 0.0(10) . . . . ?
C5 S2 C16 C17 178.1(10) . . . . ?
C15 C16 C17 C18 -36(2) . . . . ?
S2 C16 C17 C18 146.8(12) . . . . ?
C15 C16 C17 S3 147.0(11) . . . . ?
S2 C16 C17 S3 -30.6(13) . . . . ?
C20 S3 C17 C18 0.5(10) . . . . ?
C20 S3 C17 C16 178.5(9) . . . . ?
C16 C17 C18 C19 -178.2(12) . . . . ?
S3 C17 C18 C19 -0.5(14) . . . . ?
C17 C18 C19 C20 0.3(17) . . . . ?
C18 C19 C20 C21 -178.0(12) . . . . ?
C18 C19 C20 S3 0.1(14) . . . . ?
C17 S3 C20 C19 -0.4(10) . . . . ?
C17 S3 C20 C21 178.0(10) . . . . ?
C19 C20 C21 C26 -150.4(13) . . . . ?
S3 C20 C21 C26 31.6(16) . . . . ?
C19 C20 C21 C22 31.6(19) . . . . ?
S3 C20 C21 C22 -146.4(9) . . . . ?
C26 C21 C22 C23 2.8(16) . . . . ?
C20 C21 C22 C23 -179.1(10) . . . . ?
C21 C22 C23 C24 -1.3(16) . . . . ?
Cu1 O1 C24 C25 -7.3(14) . . . . ?
Cu1 O1 C24 C23 176.3(7) . . . . ?
C22 C23 C24 O1 175.7(9) . . . . ?
C22 C23 C24 C25 -1.0(15) . . . . ?
O1 C24 C25 C26 -174.9(9) . . . . ?
C23 C24 C25 C26 1.6(14) . . . . ?
O1 C24 C25 C27 2.7(16) . . . . ?
C23 C24 C25 C27 179.2(9) . . . . ?
C22 C21 C26 C25 -2.2(17) . . . . ?
C20 C21 C26 C25 179.7(10) . . . . ?
C24 C25 C26 C21 0.0(16) . . . . ?
C27 C25 C26 C21 -177.6(10) . . . . ?
C28 N1 C27 C25 -175.2(9) . . . . ?
Cu1 N1 C27 C25 -6.0(15) . . . . ?
C26 C25 C27 N1 -177.9(10) . . . . ?
C24 C25 C27 N1 4.5(16) . . . . ?
C27 N1 C28 C29 -116.9(10) . . . . ?
Cu1 N1 C28 C29 72.7(9) . . . . ?
N1 C28 C29 C30 82.4(11) . . . . ?
N1 C28 C29 C30 -156.6(9) . . . 4_556 ?
N1 C28 C29 C28 -36.3(6) . . . 4_556 ?
C14 C13 C12 C11 -177.7(18) . . . . ?
C12A C13 C12 C11 -58(4) . . . . ?
C14 C13 C12A C11A 64(4) . . . . ?
C12 C13 C12A C11A -7(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.657
_refine_diff_density_min         -0.485
_refine_diff_density_rms         0.093
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1544971'
_audit_update_record             
;
2017-04-20 deposited with the CCDC.
2017-06-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C60 H58 Cl2 N2 Ni O2 S6'
_chemical_formula_weight         1161.05

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P21/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                   8.868(2)
_cell_length_b                   19.809(5)
_cell_length_c                   33.077(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.154(7)
_cell_angle_gamma                90.00
_cell_volume                     5680(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    19045
_cell_measurement_theta_max      27.4855
_cell_measurement_theta_min      1.6281

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2424
_exptl_absorpt_coefficient_mu    0.701
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8611
_exptl_absorpt_correction_T_max  0.8902
_exptl_absorpt_process_details   'The Rigaku Corporation, Tokyo, Japan'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(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  
;
Mercury2 (2x2 bin mode)
;
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            101640
_diffrn_reflns_av_R_equivalents  0.0842
_diffrn_reflns_av_sigmaI/netI    0.0466
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_theta_min         1.63
_diffrn_reflns_theta_max         25.00
_reflns_number_total             10011
_reflns_number_gt                9901
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_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)+(0.1000P)²+17.8250P] 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         10011
_refine_ls_number_parameters     759
_refine_ls_number_restraints     393
_refine_ls_R_factor_all          0.0958
_refine_ls_R_factor_gt           0.0945
_refine_ls_wR_factor_ref         0.2444
_refine_ls_wR_factor_gt          0.2432
_refine_ls_goodness_of_fit_ref   1.216
_refine_ls_restrained_S_all      1.202
_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 0.81814(7) -0.46510(3) -0.004524(19) 0.0298(2) Uani 1 1 d . . .
S2 S 0.2250(2) -0.99730(7) 0.04001(5) 0.0469(4) Uani 1 1 d . A .
S3 S 0.43449(19) -0.79949(7) 0.04325(5) 0.0444(4) Uani 1 1 d . A .
S4 S 1.12922(18) -0.15171(7) -0.12793(4) 0.0400(3) Uani 1 1 d . A .
S5 S 1.33893(18) 0.04800(7) -0.11836(4) 0.0406(3) Uani 1 1 d . A .
S6 S 1.3205(2) 0.22243(9) -0.19556(6) 0.0606(5) Uani 1 1 d . A .
O1 O 0.7441(5) -0.53643(17) -0.03957(11) 0.0369(8) Uani 1 1 d . A .
O2 O 0.8951(5) -0.43508(18) -0.04913(12) 0.0437(10) Uani 1 1 d . A .
N1 N 0.7093(5) -0.4916(2) 0.03579(14) 0.0373(10) Uani 1 1 d . A .
N2 N 0.9174(5) -0.3971(2) 0.03054(14) 0.0366(10) Uani 1 1 d . A .
S1 S 0.0643(4) -1.11605(17) 0.13361(9) 0.0483(8) Uani 0.64 1 d PDU A 1
C1 C -0.0591(15) -1.1768(6) 0.1069(4) 0.047(3) Uani 0.64 1 d PDU A 1
H1 H -0.1000 -1.2135 0.1196 0.057 Uiso 0.64 1 calc PR A 1
C2 C -0.0888(14) -1.1652(6) 0.0662(4) 0.046(3) Uani 0.64 1 d PDU A 1
H2 H -0.1602 -1.1912 0.0470 0.056 Uiso 0.64 1 calc PR A 1
C3 C -0.0037(19) -1.1101(9) 0.0544(4) 0.051(4) Uani 0.64 1 d PDU A 1
H3 H -0.0068 -1.0969 0.0266 0.061 Uiso 0.64 1 calc PR A 1
C3A C 0.090(2) -1.1243(11) 0.1227(5) 0.054(6) Uani 0.36 1 d PDU A 2
H3A H 0.1673 -1.1243 0.1474 0.065 Uiso 0.36 1 calc PR A 2
C2A C -0.038(3) -1.1702(11) 0.1140(6) 0.048(5) Uani 0.36 1 d PDU A 2
H2A H -0.0729 -1.1956 0.1346 0.057 Uiso 0.36 1 calc PR A 2
C1A C -0.102(3) -1.1735(11) 0.0735(6) 0.049(5) Uani 0.36 1 d PDU A 2
H1A H -0.1715 -1.2080 0.0612 0.059 Uiso 0.36 1 calc PR A 2
S1A S -0.0447(10) -1.1077(4) 0.0468(2) 0.0485(16) Uani 0.36 1 d PDU A 2
C4 C 0.0847(7) -1.0783(3) 0.08897(17) 0.0417(12) Uani 1 1 d DU . .
C5 C 0.1822(7) -1.0190(3) 0.08703(18) 0.0402(12) Uani 1 1 d . A .
C6 C 0.2501(7) -0.9739(3) 0.11770(18) 0.0419(13) Uani 1 1 d . . .
C7 C 0.2356(8) -0.9754(4) 0.1627(2) 0.0543(16) Uani 1 1 d . A .
H7A H 0.1389 -0.9992 0.1644 0.065 Uiso 1 1 calc R . .
H7B H 0.2264 -0.9284 0.1720 0.065 Uiso 1 1 calc R . .
C8 C 0.3693(9) -1.0094(4) 0.1923(2) 0.0652(19) Uani 1 1 d . . .
H8A H 0.3710 -1.0577 0.1849 0.078 Uiso 1 1 calc R A .
H8B H 0.4670 -0.9890 0.1883 0.078 Uiso 1 1 calc R . .
C10 C 0.3700(9) -0.9290(4) 0.2530(2) 0.067(2) Uani 1 1 d . . .
H10A H 0.4737 -0.9107 0.2545 0.101 Uiso 1 1 calc R A .
H10B H 0.3449 -0.9271 0.2804 0.101 Uiso 1 1 calc R . .
H10C H 0.2949 -0.9021 0.2335 0.101 Uiso 1 1 calc R . .
C14 C 0.4211(8) -0.8684(3) 0.1312(2) 0.0518(15) Uani 1 1 d D . .
H14A H 0.5023 -0.8494 0.1181 0.062 Uiso 1 1 calc R A 1
H14B H 0.4736 -0.8910 0.1571 0.062 Uiso 1 1 calc R A 1
C15 C 0.3350(7) -0.9218(3) 0.10254(18) 0.0401(12) Uani 1 1 d . A .
C16 C 0.3315(7) -0.9273(3) 0.06088(18) 0.0414(13) Uani 1 1 d . . .
C17 C 0.3987(7) -0.8844(3) 0.03345(17) 0.0406(13) Uani 1 1 d . A .
C18 C 0.4436(8) -0.9019(3) -0.00261(18) 0.0462(14) Uani 1 1 d . . .
H18 H 0.4349 -0.9465 -0.0134 0.055 Uiso 1 1 calc R A .
C19 C 0.5037(8) -0.8478(3) -0.02205(19) 0.0467(14) Uani 1 1 d . A .
H19 H 0.5371 -0.8519 -0.0474 0.056 Uiso 1 1 calc R . .
C20 C 0.5087(7) -0.7883(3) -0.00027(17) 0.0369(12) Uani 1 1 d . . .
C21 C 0.5694(6) -0.7216(3) -0.00947(16) 0.0354(11) Uani 1 1 d . A .
C22 C 0.6070(7) -0.7089(3) -0.04846(17) 0.0386(12) Uani 1 1 d . . .
H22 H 0.5913 -0.7438 -0.0686 0.046 Uiso 1 1 calc R A .
C23 C 0.6652(6) -0.6482(3) -0.05797(16) 0.0347(11) Uani 1 1 d . A .
H23 H 0.6890 -0.6421 -0.0844 0.042 Uiso 1 1 calc R . .
C24 C 0.6905(6) -0.5940(3) -0.02901(17) 0.0350(11) Uani 1 1 d . . .
C25 C 0.6493(6) -0.6057(3) 0.00951(16) 0.0348(11) Uani 1 1 d . A .
C26 C 0.5905(7) -0.6687(3) 0.01850(16) 0.0382(12) Uani 1 1 d . . .
H26 H 0.5644 -0.6752 0.0447 0.046 Uiso 1 1 calc R A .
C27 C 0.6469(6) -0.5510(3) 0.03813(18) 0.0372(12) Uani 1 1 d . . .
H27 H 0.5962 -0.5587 0.0603 0.045 Uiso 1 1 calc R A .
C28 C 0.6754(6) -0.4385(3) 0.06384(18) 0.0404(13) Uani 1 1 d . . .
H28 H 0.5756 -0.4199 0.0621 0.048 Uiso 1 1 calc R A .
C29 C 0.8187(6) -0.4161(3) 0.09626(16) 0.0345(11) Uani 1 1 d . A .
C30 C 0.8521(8) -0.4655(3) 0.13251(19) 0.0490(15) Uani 1 1 d . . .
H30A H 0.8604 -0.5113 0.1221 0.074 Uiso 1 1 calc R A .
H30B H 0.7680 -0.4637 0.1476 0.074 Uiso 1 1 calc R . .
H30C H 0.9493 -0.4530 0.1512 0.074 Uiso 1 1 calc R . .
C31 C 0.7852(8) -0.3461(3) 0.1115(2) 0.0496(15) Uani 1 1 d . . .
H31A H 0.8725 -0.3312 0.1330 0.074 Uiso 1 1 calc R A .
H31B H 0.6918 -0.3479 0.1229 0.074 Uiso 1 1 calc R . .
H31C H 0.7697 -0.3142 0.0883 0.074 Uiso 1 1 calc R . .
C32 C 0.9571(7) -0.4142(3) 0.07562(17) 0.0388(12) Uani 1 1 d . . .
H32 H 1.0595 -0.4231 0.0901 0.047 Uiso 1 1 calc R A .
C33 C 0.9704(7) -0.3410(3) 0.01896(17) 0.0380(12) Uani 1 1 d . . .
H33 H 1.0105 -0.3090 0.0398 0.046 Uiso 1 1 calc R A .
C34 C 1.0268(6) -0.2592(3) -0.03176(16) 0.0337(11) Uani 1 1 d . . .
H34 H 1.0454 -0.2263 -0.0104 0.040 Uiso 1 1 calc R A .
C35 C 0.9732(6) -0.3234(2) -0.02331(16) 0.0344(11) Uani 1 1 d . A .
C36 C 0.9458(7) -0.3737(3) -0.05460(17) 0.0378(12) Uani 1 1 d . . .
C37 C 0.9788(8) -0.3563(3) -0.09354(18) 0.0456(14) Uani 1 1 d . A .
H37 H 0.9647 -0.3891 -0.1149 0.055 Uiso 1 1 calc R . .
C38 C 1.0306(7) -0.2933(3) -0.10095(17) 0.0424(13) Uani 1 1 d . . .
H38 H 1.0516 -0.2836 -0.1273 0.051 Uiso 1 1 calc R A .
C39 C 1.0535(6) -0.2422(2) -0.07033(16) 0.0331(11) Uani 1 1 d . A .
C40 C 1.1099(6) -0.1739(3) -0.07866(16) 0.0353(11) Uani 1 1 d . . .
C41 C 1.1457(8) -0.1210(3) -0.05274(18) 0.0469(15) Uani 1 1 d . A .
H41 H 1.1410 -0.1229 -0.0243 0.056 Uiso 1 1 calc R . .
C42 C 1.1908(8) -0.0627(3) -0.07155(18) 0.0465(14) Uani 1 1 d . . .
H42 H 1.2213 -0.0220 -0.0569 0.056 Uiso 1 1 calc R A .
C43 C 1.1866(6) -0.0700(2) -0.11232(16) 0.0339(11) Uani 1 1 d . A .
C44 C 1.2237(6) -0.0183(3) -0.14073(17) 0.0372(12) Uani 1 1 d . . .
C45 C 1.1728(7) -0.0093(3) -0.18273(18) 0.0393(12) Uani 1 1 d . A .
C46 C 1.0750(7) -0.0577(3) -0.21184(19) 0.0472(14) Uani 1 1 d . . .
H46 H 0.9655 -0.0571 -0.2169 0.057 Uiso 1 1 calc R A .
C47 C 1.1646(8) -0.1086(3) -0.2330(2) 0.0525(15) Uani 1 1 d . A .
H47 H 1.2738 -0.1094 -0.2292 0.063 Uiso 1 1 calc R . .
C48 C 1.0565(9) -0.1578(4) -0.2608(2) 0.0610(18) Uani 1 1 d . . .
H48 H 0.9484 -0.1602 -0.2625 0.073 Uiso 1 1 calc R A .
C49 C 1.1451(11) -0.2032(4) -0.2859(3) 0.076(2) Uani 1 1 d . A .
H49A H 1.1943 -0.1749 -0.3038 0.114 Uiso 1 1 calc R . .
H49B H 1.0730 -0.2345 -0.3030 0.114 Uiso 1 1 calc R . .
H49C H 1.2242 -0.2288 -0.2669 0.114 Uiso 1 1 calc R . .
C50 C 0.8102(9) 0.1612(5) -0.3057(3) 0.082(3) Uani 1 1 d . . .
H50A H 0.7356 0.1392 -0.2920 0.123 Uiso 1 1 calc R . .
H50B H 0.7700 0.1615 -0.3357 0.123 Uiso 1 1 calc R . .
H50C H 0.8273 0.2077 -0.2957 0.123 Uiso 1 1 calc R . .
C51 C 0.9599(9) 0.1232(4) -0.2962(2) 0.069(2) Uani 1 1 d . . .
H51 H 1.0090 0.1062 -0.3170 0.083 Uiso 1 1 calc R . .
C52 C 1.0252(8) 0.1143(4) -0.2506(2) 0.0571(17) Uani 1 1 d . . .
H52 H 0.9752 0.1305 -0.2298 0.069 Uiso 1 1 calc R . .
C53 C 1.1803(8) 0.0767(3) -0.24091(19) 0.0518(15) Uani 1 1 d . A .
H53 H 1.2411 0.0684 -0.2608 0.062 Uiso 1 1 calc R . .
C54 C 1.2255(7) 0.0545(3) -0.19651(18) 0.0405(13) Uani 1 1 d . . .
C55 C 1.3161(7) 0.0902(3) -0.16503(17) 0.0408(13) Uani 1 1 d . A .
C56 C 1.3989(8) 0.1545(3) -0.16550(19) 0.0458(14) Uani 1 1 d . . .
C57 C 1.5406(9) 0.1709(3) -0.1430(2) 0.0547(17) Uani 1 1 d . A .
H57 H 1.6006 0.1411 -0.1235 0.066 Uiso 1 1 calc R . .
C58 C 1.5912(9) 0.2367(3) -0.1513(2) 0.0575(17) Uani 1 1 d . . .
H58 H 1.6894 0.2548 -0.1390 0.069 Uiso 1 1 calc R A .
C59 C 1.4821(9) 0.2704(3) -0.1789(2) 0.0634(19) Uani 1 1 d . A .
H59 H 1.4941 0.3153 -0.1879 0.076 Uiso 1 1 calc R . .
C9 C 0.3642(10) -1.0042(5) 0.2378(2) 0.075(2) Uani 1 1 d . A .
H9A H 0.4527 -1.0292 0.2544 0.090 Uiso 1 1 calc R . .
H9B H 0.2683 -1.0256 0.2424 0.090 Uiso 1 1 calc R . .
C11 C 0.3430(19) -0.7111(8) 0.1882(5) 0.073(4) Uani 0.55 1 d PDU A 1
H11A H 0.3040 -0.6797 0.1655 0.110 Uiso 0.55 1 calc PR A 1
H11B H 0.4082 -0.6866 0.2111 0.110 Uiso 0.55 1 calc PR A 1
H11C H 0.2559 -0.7315 0.1977 0.110 Uiso 0.55 1 calc PR A 1
C12 C 0.4359(15) -0.7654(7) 0.1733(5) 0.059(3) Uani 0.55 1 d PDU A 1
H12A H 0.4901 -0.7928 0.1970 0.071 Uiso 0.55 1 calc PR A 1
H12B H 0.5141 -0.7450 0.1597 0.071 Uiso 0.55 1 calc PR A 1
C13 C 0.327(2) -0.8096(8) 0.1430(6) 0.066(5) Uani 0.55 1 d PDU A 1
H13A H 0.2806 -0.7833 0.1181 0.079 Uiso 0.55 1 calc PR A 1
H13B H 0.2437 -0.8267 0.1558 0.079 Uiso 0.55 1 calc PR A 1
C11A C 0.423(2) -0.7500(11) 0.1999(5) 0.079(5) Uani 0.45 1 d PDU A 2
H11D H 0.3277 -0.7582 0.2097 0.118 Uiso 0.45 1 calc PR A 2
H11E H 0.4740 -0.7096 0.2134 0.118 Uiso 0.45 1 calc PR A 2
H11F H 0.4918 -0.7890 0.2067 0.118 Uiso 0.45 1 calc PR A 2
C12A C 0.385(2) -0.7399(7) 0.1543(5) 0.061(4) Uani 0.45 1 d PDU A 2
H12C H 0.4800 -0.7270 0.1448 0.074 Uiso 0.45 1 calc PR A 2
H12D H 0.3099 -0.7026 0.1474 0.074 Uiso 0.45 1 calc PR A 2
C13A C 0.317(3) -0.8050(10) 0.1318(8) 0.053(5) Uani 0.45 1 d PDU A 2
H13C H 0.2741 -0.7927 0.1026 0.064 Uiso 0.45 1 calc PR A 2
H13D H 0.2295 -0.8190 0.1440 0.064 Uiso 0.45 1 calc PR A 2
Cl1 Cl 0.6939(5) -0.5538(2) -0.16243(10) 0.1211(12) Uani 0.89 1 d PDU B 1
Cl2 Cl 0.5055(4) -0.44185(18) -0.14296(10) 0.1030(9) Uani 0.89 1 d PDU B 1
C60 C 0.6821(12) -0.4806(5) -0.1348(4) 0.095(3) Uani 0.89 1 d PDU B 1
H60A H 0.7139 -0.4913 -0.1050 0.114 Uiso 0.89 1 calc PR B 1
H60B H 0.7577 -0.4480 -0.1415 0.114 Uiso 0.89 1 calc PR B 1
Cl2A Cl 0.579(4) -0.4380(17) -0.1071(10) 0.119(7) Uani 0.11 1 d PDU C 2
Cl1A Cl 0.727(3) -0.4887(15) -0.1663(9) 0.108(7) Uani 0.11 1 d PDU C 2
C60A C 0.617(12) -0.512(2) -0.131(3) 0.112(10) Uani 0.11 1 d PDU C 2
H60C H 0.5195 -0.5333 -0.1455 0.134 Uiso 0.11 1 calc PR C 2
H60D H 0.6740 -0.5440 -0.1106 0.134 Uiso 0.11 1 calc PR C 2


_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 O2 1.849(4) . ?
Ni1 O1 1.858(3) . ?
Ni1 N2 1.872(4) . ?
Ni1 N1 1.878(5) . ?
S2 C5 1.731(6) . ?
S2 C16 1.737(6) . ?
S3 C20 1.718(6) . ?
S3 C17 1.730(5) . ?
S4 C40 1.731(5) . ?
S4 C43 1.742(5) . ?
S5 C55 1.730(6) . ?
S5 C44 1.732(6) . ?
S6 C59 1.711(8) . ?
S6 C56 1.730(6) . ?
O1 C24 1.310(6) . ?
O2 C36 1.322(6) . ?
N1 C27 1.310(7) . ?
N1 C28 1.476(7) . ?
N2 C33 1.295(7) . ?
N2 C32 1.497(7) . ?
S1 C4 1.699(6) . ?
S1 C1 1.737(11) . ?
C1 C2 1.336(12) . ?
C1 H1 0.9500 . ?
C2 C3 1.428(14) . ?
C2 H2 0.9500 . ?
C3 C4 1.393(13) . ?
C3 H3 0.9500 . ?
C3A C4 1.434(15) . ?
C3A C2A 1.435(16) . ?
C3A H3A 0.9500 . ?
C2A C1A 1.342(16) . ?
C2A H2A 0.9500 . ?
C1A S1A 1.712(16) . ?
C1A H1A 0.9500 . ?
S1A C4 1.710(8) . ?
C4 C5 1.469(7) . ?
C5 C6 1.389(8) . ?
C6 C15 1.429(8) . ?
C6 C7 1.520(9) . ?
C7 C8 1.528(10) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.518(11) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C10 C9 1.569(11) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C14 C15 1.517(8) . ?
C14 C13 1.527(14) . ?
C14 C13A 1.558(15) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.376(8) . ?
C16 C17 1.458(8) . ?
C17 C18 1.379(8) . ?
C18 C19 1.411(8) . ?
C18 H18 0.9500 . ?
C19 C20 1.376(8) . ?
C19 H19 0.9500 . ?
C20 C21 1.484(7) . ?
C21 C26 1.384(7) . ?
C21 C22 1.420(8) . ?
C22 C23 1.372(7) . ?
C22 H22 0.9500 . ?
C23 C24 1.425(7) . ?
C23 H23 0.9500 . ?
C24 C25 1.417(7) . ?
C25 C26 1.410(7) . ?
C25 C27 1.441(7) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C28 C29 1.545(8) . ?
C28 H28 0.9500 . ?
C29 C32 1.525(7) . ?
C29 C30 1.527(8) . ?
C29 C31 1.527(7) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32 0.9500 . ?
C33 C35 1.446(7) . ?
C33 H33 0.9500 . ?
C34 C39 1.387(7) . ?
C34 C35 1.407(7) . ?
C34 H34 0.9500 . ?
C35 C36 1.420(7) . ?
C36 C37 1.422(8) . ?
C37 C38 1.369(8) . ?
C37 H37 0.9500 . ?
C38 C39 1.415(7) . ?
C38 H38 0.9500 . ?
C39 C40 1.488(7) . ?
C40 C41 1.349(8) . ?
C41 C42 1.409(8) . ?
C41 H41 0.9500 . ?
C42 C43 1.349(8) . ?
C42 H42 0.9500 . ?
C43 C44 1.472(7) . ?
C44 C45 1.379(8) . ?
C45 C54 1.454(7) . ?
C45 C46 1.499(8) . ?
C46 C47 1.540(9) . ?
C46 H46 0.9500 . ?
C47 C48 1.532(9) . ?
C47 H47 0.9500 . ?
C48 C49 1.545(10) . ?
C48 H48 0.9500 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C50 C51 1.500(11) . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C51 C52 1.507(10) . ?
C51 H51 0.9500 . ?
C52 C53 1.538(10) . ?
C52 H52 0.9500 . ?
C53 C54 1.505(8) . ?
C53 H53 0.9500 . ?
C54 C55 1.371(8) . ?
C55 C56 1.471(8) . ?
C56 C57 1.358(9) . ?
C57 C58 1.424(9) . ?
C57 H57 0.9500 . ?
C58 C59 1.357(11) . ?
C58 H58 0.9500 . ?
C59 H59 0.9500 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C11 C12 1.501(14) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.513(17) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C11A C12A 1.487(16) . ?
C11A H11D 0.9800 . ?
C11A H11E 0.9800 . ?
C11A H11F 0.9800 . ?
C12A C13A 1.55(3) . ?
C12A H12C 0.9900 . ?
C12A H12D 0.9900 . ?
C13A H13C 0.9900 . ?
C13A H13D 0.9900 . ?
Cl1 C60 1.728(10) . ?
Cl2 C60 1.714(10) . ?
C60 H60A 0.9900 . ?
C60 H60B 0.9900 . ?
Cl2A C60A 1.729(18) . ?
Cl1A C60A 1.734(18) . ?
C60A H60C 0.9900 . ?
C60A H60D 0.9900 . ?

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 Ni1 O1 83.57(16) . . ?
O2 Ni1 N2 93.37(17) . . ?
O1 Ni1 N2 172.86(19) . . ?
O2 Ni1 N1 170.9(2) . . ?
O1 Ni1 N1 93.62(17) . . ?
N2 Ni1 N1 90.36(19) . . ?
C5 S2 C16 92.6(3) . . ?
C20 S3 C17 93.2(3) . . ?
C40 S4 C43 92.2(3) . . ?
C55 S5 C44 92.2(3) . . ?
C59 S6 C56 92.2(3) . . ?
C24 O1 Ni1 126.6(3) . . ?
C36 O2 Ni1 126.7(3) . . ?
C27 N1 C28 117.3(5) . . ?
C27 N1 Ni1 125.5(4) . . ?
C28 N1 Ni1 116.7(3) . . ?
C33 N2 C32 117.7(5) . . ?
C33 N2 Ni1 125.9(4) . . ?
C32 N2 Ni1 115.8(3) . . ?
C4 S1 C1 92.0(4) . . ?
C2 C1 S1 111.2(7) . . ?
C2 C1 H1 124.4 . . ?
S1 C1 H1 124.4 . . ?
C1 C2 C3 113.9(9) . . ?
C1 C2 H2 123.1 . . ?
C3 C2 H2 123.1 . . ?
C4 C3 C2 111.0(9) . . ?
C4 C3 H3 124.5 . . ?
C2 C3 H3 124.5 . . ?
C4 C3A C2A 110.6(11) . . ?
C4 C3A H3A 124.7 . . ?
C2A C3A H3A 124.7 . . ?
C1A C2A C3A 112.6(12) . . ?
C1A C2A H2A 123.7 . . ?
C3A C2A H2A 123.7 . . ?
C2A C1A S1A 111.5(11) . . ?
C2A C1A H1A 124.3 . . ?
S1A C1A H1A 124.3 . . ?
C4 S1A C1A 93.5(7) . . ?
C3 C4 C3A 105.8(10) . . ?
C3 C4 C5 124.1(7) . . ?
C3A C4 C5 128.3(9) . . ?
C3 C4 S1 111.7(7) . . ?
C3A C4 S1 15.3(11) . . ?
C5 C4 S1 124.2(4) . . ?
C3 C4 S1A 9.0(10) . . ?
C3A C4 S1A 108.9(8) . . ?
C5 C4 S1A 122.5(5) . . ?
S1 C4 S1A 112.5(4) . . ?
C6 C5 C4 130.6(5) . . ?
C6 C5 S2 110.7(4) . . ?
C4 C5 S2 118.7(4) . . ?
C5 C6 C15 112.7(5) . . ?
C5 C6 C7 126.1(5) . . ?
C15 C6 C7 121.1(5) . . ?
C6 C7 C8 115.0(6) . . ?
C6 C7 H7A 108.5 . . ?
C8 C7 H7A 108.5 . . ?
C6 C7 H7B 108.5 . . ?
C8 C7 H7B 108.5 . . ?
H7A C7 H7B 107.5 . . ?
C9 C8 C7 115.2(7) . . ?
C9 C8 H8A 108.5 . . ?
C7 C8 H8A 108.5 . . ?
C9 C8 H8B 108.5 . . ?
C7 C8 H8B 108.5 . . ?
H8A C8 H8B 107.5 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C15 C14 C13 117.6(9) . . ?
C15 C14 C13A 110.4(10) . . ?
C13 C14 C13A 13.9(14) . . ?
C15 C14 H14A 107.9 . . ?
C13 C14 H14A 107.9 . . ?
C13A C14 H14A 100.7 . . ?
C15 C14 H14B 107.9 . . ?
C13 C14 H14B 107.9 . . ?
C13A C14 H14B 121.8 . . ?
H14A C14 H14B 107.2 . . ?
C16 C15 C6 113.1(5) . . ?
C16 C15 C14 125.7(5) . . ?
C6 C15 C14 121.2(5) . . ?
C15 C16 C17 130.7(5) . . ?
C15 C16 S2 110.8(4) . . ?
C17 C16 S2 118.5(4) . . ?
C18 C17 C16 128.4(5) . . ?
C18 C17 S3 109.4(4) . . ?
C16 C17 S3 122.2(4) . . ?
C17 C18 C19 114.1(5) . . ?
C17 C18 H18 123.0 . . ?
C19 C18 H18 123.0 . . ?
C20 C19 C18 112.7(5) . . ?
C20 C19 H19 123.7 . . ?
C18 C19 H19 123.7 . . ?
C19 C20 C21 128.9(5) . . ?
C19 C20 S3 110.7(4) . . ?
C21 C20 S3 120.4(4) . . ?
C26 C21 C22 116.7(5) . . ?
C26 C21 C20 122.8(5) . . ?
C22 C21 C20 120.5(5) . . ?
C23 C22 C21 122.3(5) . . ?
C23 C22 H22 118.9 . . ?
C21 C22 H22 118.9 . . ?
C22 C23 C24 121.4(5) . . ?
C22 C23 H23 119.3 . . ?
C24 C23 H23 119.3 . . ?
O1 C24 C25 124.0(5) . . ?
O1 C24 C23 119.4(5) . . ?
C25 C24 C23 116.6(5) . . ?
C26 C25 C24 120.8(5) . . ?
C26 C25 C27 118.0(5) . . ?
C24 C25 C27 120.7(5) . . ?
C21 C26 C25 122.2(5) . . ?
C21 C26 H26 118.9 . . ?
C25 C26 H26 118.9 . . ?
N1 C27 C25 124.8(5) . . ?
N1 C27 H27 117.6 . . ?
C25 C27 H27 117.6 . . ?
N1 C28 C29 113.2(4) . . ?
N1 C28 H28 123.4 . . ?
C29 C28 H28 123.4 . . ?
C32 C29 C30 109.0(5) . . ?
C32 C29 C31 110.8(5) . . ?
C30 C29 C31 110.0(5) . . ?
C32 C29 C28 108.5(4) . . ?
C30 C29 C28 110.9(5) . . ?
C31 C29 C28 107.5(5) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N2 C32 C29 114.1(5) . . ?
N2 C32 H32 122.9 . . ?
C29 C32 H32 122.9 . . ?
N2 C33 C35 125.1(5) . . ?
N2 C33 H33 117.5 . . ?
C35 C33 H33 117.5 . . ?
C39 C34 C35 122.1(5) . . ?
C39 C34 H34 118.9 . . ?
C35 C34 H34 118.9 . . ?
C34 C35 C36 120.2(5) . . ?
C34 C35 C33 119.1(5) . . ?
C36 C35 C33 120.0(5) . . ?
O2 C36 C35 123.8(5) . . ?
O2 C36 C37 119.2(5) . . ?
C35 C36 C37 117.0(5) . . ?
C38 C37 C36 121.6(5) . . ?
C38 C37 H37 119.2 . . ?
C36 C37 H37 119.2 . . ?
C37 C38 C39 121.8(5) . . ?
C37 C38 H38 119.1 . . ?
C39 C38 H38 119.1 . . ?
C34 C39 C38 117.3(4) . . ?
C34 C39 C40 121.3(4) . . ?
C38 C39 C40 121.4(5) . . ?
C41 C40 C39 129.2(5) . . ?
C41 C40 S4 110.1(4) . . ?
C39 C40 S4 120.6(4) . . ?
C40 C41 C42 114.0(5) . . ?
C40 C41 H41 123.0 . . ?
C42 C41 H41 123.0 . . ?
C43 C42 C41 113.7(5) . . ?
C43 C42 H42 123.1 . . ?
C41 C42 H42 123.1 . . ?
C42 C43 C44 126.9(5) . . ?
C42 C43 S4 109.9(4) . . ?
C44 C43 S4 123.2(4) . . ?
C45 C44 C43 131.5(5) . . ?
C45 C44 S5 111.8(4) . . ?
C43 C44 S5 116.5(4) . . ?
C44 C45 C54 111.7(5) . . ?
C44 C45 C46 125.9(5) . . ?
C54 C45 C46 122.4(5) . . ?
C45 C46 C47 115.2(5) . . ?
C45 C46 H46 122.4 . . ?
C47 C46 H46 122.4 . . ?
C48 C47 C46 111.8(6) . . ?
C48 C47 H47 124.1 . . ?
C46 C47 H47 124.1 . . ?
C47 C48 C49 111.6(6) . . ?
C47 C48 H48 124.2 . . ?
C49 C48 H48 124.2 . . ?
C48 C49 H49A 109.5 . . ?
C48 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C48 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C51 C50 H50A 109.5 . . ?
C51 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C51 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C50 C51 C52 114.0(7) . . ?
C50 C51 H51 123.0 . . ?
C52 C51 H51 123.0 . . ?
C51 C52 C53 113.8(6) . . ?
C51 C52 H52 123.1 . . ?
C53 C52 H52 123.1 . . ?
C54 C53 C52 112.8(5) . . ?
C54 C53 H53 123.6 . . ?
C52 C53 H53 123.6 . . ?
C55 C54 C45 112.8(5) . . ?
C55 C54 C53 125.7(5) . . ?
C45 C54 C53 121.5(5) . . ?
C54 C55 C56 130.8(5) . . ?
C54 C55 S5 111.6(4) . . ?
C56 C55 S5 117.6(4) . . ?
C57 C56 C55 127.4(6) . . ?
C57 C56 S6 110.0(5) . . ?
C55 C56 S6 122.6(5) . . ?
C56 C57 C58 113.9(7) . . ?
C56 C57 H57 123.0 . . ?
C58 C57 H57 123.0 . . ?
C59 C58 C57 111.8(7) . . ?
C59 C58 H58 124.1 . . ?
C57 C58 H58 124.1 . . ?
C58 C59 S6 111.9(5) . . ?
C58 C59 H59 124.1 . . ?
S6 C59 H59 124.1 . . ?
C8 C9 C10 112.0(7) . . ?
C8 C9 H9A 109.2 . . ?
C10 C9 H9A 109.2 . . ?
C8 C9 H9B 109.2 . . ?
C10 C9 H9B 109.2 . . ?
H9A C9 H9B 107.9 . . ?
C11 C12 C13 108.4(12) . . ?
C11 C12 H12A 110.0 . . ?
C13 C12 H12A 110.0 . . ?
C11 C12 H12B 110.0 . . ?
C13 C12 H12B 110.0 . . ?
H12A C12 H12B 108.4 . . ?
C12 C13 C14 107.8(13) . . ?
C12 C13 H13A 110.1 . . ?
C14 C13 H13A 110.1 . . ?
C12 C13 H13B 110.1 . . ?
C14 C13 H13B 110.1 . . ?
H13A C13 H13B 108.5 . . ?
C12A C11A H11D 109.5 . . ?
C12A C11A H11E 109.5 . . ?
H11D C11A H11E 109.5 . . ?
C12A C11A H11F 109.5 . . ?
H11D C11A H11F 109.5 . . ?
H11E C11A H11F 109.5 . . ?
C11A C12A C13A 111.0(16) . . ?
C11A C12A H12C 109.4 . . ?
C13A C12A H12C 109.4 . . ?
C11A C12A H12D 109.4 . . ?
C13A C12A H12D 109.4 . . ?
H12C C12A H12D 108.0 . . ?
C12A C13A C14 120.4(16) . . ?
C12A C13A H13C 107.2 . . ?
C14 C13A H13C 107.2 . . ?
C12A C13A H13D 107.2 . . ?
C14 C13A H13D 107.2 . . ?
H13C C13A H13D 106.9 . . ?
Cl2 C60 Cl1 116.6(7) . . ?
Cl2 C60 H60A 108.1 . . ?
Cl1 C60 H60A 108.1 . . ?
Cl2 C60 H60B 108.1 . . ?
Cl1 C60 H60B 108.1 . . ?
H60A C60 H60B 107.3 . . ?
Cl2A C60A Cl1A 106(3) . . ?
Cl2A C60A H60C 110.5 . . ?
Cl1A C60A H60C 110.5 . . ?
Cl2A C60A H60D 110.5 . . ?
Cl1A C60A H60D 110.5 . . ?
H60C C60A H60D 108.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 Ni1 O1 C24 166.0(5) . . . . ?
N2 Ni1 O1 C24 101.0(14) . . . . ?
N1 Ni1 O1 C24 -22.7(5) . . . . ?
O1 Ni1 O2 C36 164.4(5) . . . . ?
N2 Ni1 O2 C36 -22.1(5) . . . . ?
N1 Ni1 O2 C36 92.0(12) . . . . ?
O2 Ni1 N1 C27 87.6(12) . . . . ?
O1 Ni1 N1 C27 15.9(5) . . . . ?
N2 Ni1 N1 C27 -158.1(5) . . . . ?
O2 Ni1 N1 C28 -84.4(12) . . . . ?
O1 Ni1 N1 C28 -156.1(4) . . . . ?
N2 Ni1 N1 C28 29.9(4) . . . . ?
O2 Ni1 N2 C33 19.1(5) . . . . ?
O1 Ni1 N2 C33 83.5(15) . . . . ?
N1 Ni1 N2 C33 -152.6(5) . . . . ?
O2 Ni1 N2 C32 -151.9(4) . . . . ?
O1 Ni1 N2 C32 -87.5(14) . . . . ?
N1 Ni1 N2 C32 36.3(4) . . . . ?
C4 S1 C1 C2 -3.7(10) . . . . ?
S1 C1 C2 C3 4.9(11) . . . . ?
C1 C2 C3 C4 -3.8(14) . . . . ?
C4 C3A C2A C1A 19(3) . . . . ?
C3A C2A C1A S1A -15(3) . . . . ?
C2A C1A S1A C4 6(2) . . . . ?
C2 C3 C4 C3A 15.8(18) . . . . ?
C2 C3 C4 C5 -178.5(8) . . . . ?
C2 C3 C4 S1 0.9(14) . . . . ?
C2 C3 C4 S1A -96(5) . . . . ?
C2A C3A C4 C3 -23(2) . . . . ?
C2A C3A C4 C5 172.5(15) . . . . ?
C2A C3A C4 S1 92(4) . . . . ?
C2A C3A C4 S1A -14(2) . . . . ?
C1 S1 C4 C3 1.5(11) . . . . ?
C1 S1 C4 C3A -68(3) . . . . ?
C1 S1 C4 C5 -179.0(7) . . . . ?
C1 S1 C4 S1A 11.2(7) . . . . ?
C1A S1A C4 C3 76(5) . . . . ?
C1A S1A C4 C3A 4.9(15) . . . . ?
C1A S1A C4 C5 179.0(11) . . . . ?
C1A S1A C4 S1 -11.0(11) . . . . ?
C3 C4 C5 C6 165.0(11) . . . . ?
C3A C4 C5 C6 -32.7(17) . . . . ?
S1 C4 C5 C6 -14.4(10) . . . . ?
S1A C4 C5 C6 154.4(7) . . . . ?
C3 C4 C5 S2 -14.6(12) . . . . ?
C3A C4 C5 S2 147.7(14) . . . . ?
S1 C4 C5 S2 166.0(4) . . . . ?
S1A C4 C5 S2 -25.2(8) . . . . ?
C16 S2 C5 C6 -0.8(5) . . . . ?
C16 S2 C5 C4 178.8(5) . . . . ?
C4 C5 C6 C15 -179.0(6) . . . . ?
S2 C5 C6 C15 0.6(7) . . . . ?
C4 C5 C6 C7 -1.2(11) . . . . ?
S2 C5 C6 C7 178.4(5) . . . . ?
C5 C6 C7 C8 97.5(8) . . . . ?
C15 C6 C7 C8 -84.9(8) . . . . ?
C6 C7 C8 C9 173.6(6) . . . . ?
C5 C6 C15 C16 0.0(8) . . . . ?
C7 C6 C15 C16 -177.9(6) . . . . ?
C5 C6 C15 C14 -178.6(5) . . . . ?
C7 C6 C15 C14 3.5(9) . . . . ?
C13 C14 C15 C16 101.7(12) . . . . ?
C13A C14 C15 C16 88.6(13) . . . . ?
C13 C14 C15 C6 -79.9(12) . . . . ?
C13A C14 C15 C6 -93.0(12) . . . . ?
C6 C15 C16 C17 178.3(6) . . . . ?
C14 C15 C16 C17 -3.1(11) . . . . ?
C6 C15 C16 S2 -0.6(7) . . . . ?
C14 C15 C16 S2 177.9(5) . . . . ?
C5 S2 C16 C15 0.8(5) . . . . ?
C5 S2 C16 C17 -178.3(5) . . . . ?
C15 C16 C17 C18 153.4(7) . . . . ?
S2 C16 C17 C18 -27.7(9) . . . . ?
C15 C16 C17 S3 -26.4(10) . . . . ?
S2 C16 C17 S3 152.5(4) . . . . ?
C20 S3 C17 C18 -0.1(5) . . . . ?
C20 S3 C17 C16 179.6(5) . . . . ?
C16 C17 C18 C19 179.5(6) . . . . ?
S3 C17 C18 C19 -0.7(7) . . . . ?
C17 C18 C19 C20 1.5(9) . . . . ?
C18 C19 C20 C21 177.2(6) . . . . ?
C18 C19 C20 S3 -1.5(7) . . . . ?
C17 S3 C20 C19 1.0(5) . . . . ?
C17 S3 C20 C21 -177.9(5) . . . . ?
C19 C20 C21 C26 -169.1(6) . . . . ?
S3 C20 C21 C26 9.6(8) . . . . ?
C19 C20 C21 C22 11.8(10) . . . . ?
S3 C20 C21 C22 -169.5(4) . . . . ?
C26 C21 C22 C23 1.7(8) . . . . ?
C20 C21 C22 C23 -179.2(5) . . . . ?
C21 C22 C23 C24 -0.3(9) . . . . ?
Ni1 O1 C24 C25 14.3(8) . . . . ?
Ni1 O1 C24 C23 -168.3(4) . . . . ?
C22 C23 C24 O1 -179.0(5) . . . . ?
C22 C23 C24 C25 -1.4(8) . . . . ?
O1 C24 C25 C26 179.2(5) . . . . ?
C23 C24 C25 C26 1.7(8) . . . . ?
O1 C24 C25 C27 7.5(9) . . . . ?
C23 C24 C25 C27 -169.9(5) . . . . ?
C22 C21 C26 C25 -1.3(9) . . . . ?
C20 C21 C26 C25 179.6(5) . . . . ?
C24 C25 C26 C21 -0.4(9) . . . . ?
C27 C25 C26 C21 171.5(5) . . . . ?
C28 N1 C27 C25 170.8(5) . . . . ?
Ni1 N1 C27 C25 -1.1(8) . . . . ?
C26 C25 C27 N1 173.8(5) . . . . ?
C24 C25 C27 N1 -14.4(9) . . . . ?
C27 N1 C28 C29 114.0(5) . . . . ?
Ni1 N1 C28 C29 -73.4(5) . . . . ?
N1 C28 C29 C32 38.9(6) . . . . ?
N1 C28 C29 C30 -80.9(6) . . . . ?
N1 C28 C29 C31 158.8(5) . . . . ?
C33 N2 C32 C29 114.9(5) . . . . ?
Ni1 N2 C32 C29 -73.3(5) . . . . ?
C30 C29 C32 N2 151.7(4) . . . . ?
C31 C29 C32 N2 -87.1(6) . . . . ?
C28 C29 C32 N2 30.8(6) . . . . ?
C32 N2 C33 C35 165.6(5) . . . . ?
Ni1 N2 C33 C35 -5.3(8) . . . . ?
C39 C34 C35 C36 0.6(9) . . . . ?
C39 C34 C35 C33 170.6(5) . . . . ?
N2 C33 C35 C34 176.7(5) . . . . ?
N2 C33 C35 C36 -13.2(9) . . . . ?
Ni1 O2 C36 C35 11.1(8) . . . . ?
Ni1 O2 C36 C37 -170.4(4) . . . . ?
C34 C35 C36 O2 -179.8(5) . . . . ?
C33 C35 C36 O2 10.2(9) . . . . ?
C34 C35 C36 C37 1.6(8) . . . . ?
C33 C35 C36 C37 -168.4(6) . . . . ?
O2 C36 C37 C38 179.5(6) . . . . ?
C35 C36 C37 C38 -1.8(9) . . . . ?
C36 C37 C38 C39 -0.1(10) . . . . ?
C35 C34 C39 C38 -2.5(8) . . . . ?
C35 C34 C39 C40 179.8(5) . . . . ?
C37 C38 C39 C34 2.3(9) . . . . ?
C37 C38 C39 C40 179.9(6) . . . . ?
C34 C39 C40 C41 1.5(9) . . . . ?
C38 C39 C40 C41 -176.1(6) . . . . ?
C34 C39 C40 S4 -175.3(4) . . . . ?
C38 C39 C40 S4 7.1(8) . . . . ?
C43 S4 C40 C41 0.1(5) . . . . ?
C43 S4 C40 C39 177.4(5) . . . . ?
C39 C40 C41 C42 -177.9(6) . . . . ?
S4 C40 C41 C42 -0.8(7) . . . . ?
C40 C41 C42 C43 1.4(9) . . . . ?
C41 C42 C43 C44 178.7(6) . . . . ?
C41 C42 C43 S4 -1.3(7) . . . . ?
C40 S4 C43 C42 0.7(5) . . . . ?
C40 S4 C43 C44 -179.3(5) . . . . ?
C42 C43 C44 C45 -152.2(7) . . . . ?
S4 C43 C44 C45 27.8(9) . . . . ?
C42 C43 C44 S5 21.6(8) . . . . ?
S4 C43 C44 S5 -158.4(3) . . . . ?
C55 S5 C44 C45 1.6(5) . . . . ?
C55 S5 C44 C43 -173.4(4) . . . . ?
C43 C44 C45 C54 172.1(6) . . . . ?
S5 C44 C45 C54 -1.9(6) . . . . ?
C43 C44 C45 C46 -7.9(10) . . . . ?
S5 C44 C45 C46 178.1(5) . . . . ?
C44 C45 C46 C47 -92.5(7) . . . . ?
C54 C45 C46 C47 87.5(7) . . . . ?
C45 C46 C47 C48 177.8(5) . . . . ?
C46 C47 C48 C49 173.2(6) . . . . ?
C50 C51 C52 C53 -178.8(7) . . . . ?
C51 C52 C53 C54 -166.9(6) . . . . ?
C44 C45 C54 C55 1.3(7) . . . . ?
C46 C45 C54 C55 -178.7(6) . . . . ?
C44 C45 C54 C53 -178.0(5) . . . . ?
C46 C45 C54 C53 2.0(9) . . . . ?
C52 C53 C54 C55 -92.8(7) . . . . ?
C52 C53 C54 C45 86.4(7) . . . . ?
C45 C54 C55 C56 176.5(6) . . . . ?
C53 C54 C55 C56 -4.3(11) . . . . ?
C45 C54 C55 S5 -0.1(7) . . . . ?
C53 C54 C55 S5 179.1(5) . . . . ?
C44 S5 C55 C54 -0.8(5) . . . . ?
C44 S5 C55 C56 -177.9(5) . . . . ?
C54 C55 C56 C57 -141.3(7) . . . . ?
S5 C55 C56 C57 35.2(9) . . . . ?
C54 C55 C56 S6 40.4(9) . . . . ?
S5 C55 C56 S6 -143.1(4) . . . . ?
C59 S6 C56 C57 2.1(5) . . . . ?
C59 S6 C56 C55 -179.3(5) . . . . ?
C55 C56 C57 C58 178.3(6) . . . . ?
S6 C56 C57 C58 -3.2(7) . . . . ?
C56 C57 C58 C59 2.9(9) . . . . ?
C57 C58 C59 S6 -1.2(8) . . . . ?
C56 S6 C59 C58 -0.5(6) . . . . ?
C7 C8 C9 C10 -61.2(9) . . . . ?
C11 C12 C13 C14 -174.8(14) . . . . ?
C15 C14 C13 C12 177.0(11) . . . . ?
C13A C14 C13 C12 -121(8) . . . . ?
C11A C12A C13A C14 -69(2) . . . . ?
C15 C14 C13A C12A -172.3(16) . . . . ?
C13 C14 C13A C12A 64(6) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.254
_refine_diff_density_min         -1.056
_refine_diff_density_rms         0.103
