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

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

data_aja0907
_database_code_depnum_ccdc_archive 'CCDC 1470090'
_audit_update_record             
;
2016-03-22 deposited with the CCDC.
2016-05-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H36 Mn N10 O3 S3, 2(Cl O4), C2 H3 N'
_chemical_formula_sum            'C44 H39 Cl2 Mn N11 O11 S3'
_chemical_formula_weight         1119.88

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'
S S 0.1246 0.1234 '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'
Mn Mn 0.3368 0.7283 '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'

_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3 :H'
_space_group_name_Hall           '-R 3'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   13.7370(4)
_cell_length_b                   13.7370(13)
_cell_length_c                   44.1110(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     7208.8(5)
_cell_formula_units_Z            6
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1324
_cell_measurement_theta_min      2.518
_cell_measurement_theta_max      25

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_F_000             3450
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    0.589
_shelx_estimated_absorpt_T_min   0.891
_shelx_estimated_absorpt_T_max   0.988
_exptl_absorpt_correction_type   Empirical
_exptl_absorpt_correction_T_min  0.8913
_exptl_absorpt_correction_T_max  0.9883
_exptl_absorpt_process_details   Denzo/Scalepack

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8291
_diffrn_reflns_av_unetI/netI     0.2751
_diffrn_reflns_av_R_equivalents  0.1933
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_theta_min         2.518
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             2831
_reflns_number_gt                1324
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0576P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2831
_refine_ls_number_parameters     229
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.1343
_refine_ls_R_factor_gt           0.0739
_refine_ls_wR_factor_ref         0.1632
_refine_ls_wR_factor_gt          0.1455
_refine_ls_goodness_of_fit_ref   0.939
_refine_ls_restrained_S_all      0.937
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6260(4) 0.4080(4) 0.06721(12) 0.0371(12) Uani 1 1 d . . . . .
H1A H 0.6086 0.3933 0.0458 0.045 Uiso 1 1 calc R U . . .
H1B H 0.6852 0.4857 0.0694 0.045 Uiso 1 1 calc R U . . .
C2 C 0.5228(4) 0.3906(4) 0.08399(13) 0.0337(11) Uani 1 1 d . . . . .
C3 C 0.4396(5) 0.4002(4) 0.06890(13) 0.0422(14) Uani 1 1 d . . . . .
H3 H 0.4425 0.4110 0.0480 0.051 Uiso 1 1 calc R U . . .
C4 C 0.3511(4) 0.3930(5) 0.08628(15) 0.0431(14) Uani 1 1 d . . . . .
H4 H 0.2937 0.3989 0.0769 0.052 Uiso 1 1 calc R U . . .
C5 C 0.3482(4) 0.3776(4) 0.11670(15) 0.0431(14) Uani 1 1 d . . . . .
H5 H 0.2896 0.3729 0.1283 0.052 Uiso 1 1 calc R U . . .
C6 C 0.4347(4) 0.3690(4) 0.12993(12) 0.0283(11) Uani 1 1 d . . . . .
C7 C 0.4536(3) 0.2911(4) 0.17870(13) 0.0297(11) Uani 1 1 d . . . . .
C8 C 0.3930(4) 0.3483(4) 0.22532(15) 0.0405(14) Uani 1 1 d . . . . .
C9 C 0.3722(4) 0.3229(4) 0.25805(15) 0.0398(13) Uani 1 1 d . . . . .
C10 C 0.3439(4) 0.3906(4) 0.27496(15) 0.0431(14) Uani 1 1 d . . . . .
H10 H 0.3421 0.4506 0.2658 0.052 Uiso 1 1 calc R U . . .
C11 C 0.3191(5) 0.3692(5) 0.30476(14) 0.0473(14) Uani 1 1 d . . . . .
H11 H 0.3015 0.4155 0.3160 0.057 Uiso 1 1 calc R U . . .
C12 C 0.3196(5) 0.2789(5) 0.31868(15) 0.0525(16) Uani 1 1 d . . . . .
H12 H 0.3008 0.2635 0.3391 0.063 Uiso 1 1 calc R U . . .
C13 C 0.3482(5) 0.2125(5) 0.30204(16) 0.0468(14) Uani 1 1 d . . . . .
H13 H 0.3510 0.1533 0.3114 0.056 Uiso 1 1 calc R U . . .
C14 C 0.3728(4) 0.2330(4) 0.27164(14) 0.0419(14) Uani 1 1 d . . . . .
H14 H 0.3897 0.1863 0.2603 0.050 Uiso 1 1 calc R U . . .
N1 N 0.6667 0.3333 0.07878(19) 0.0310(17) Uani 1 3 d S T P . .
N2 N 0.5211(3) 0.3734(3) 0.11396(11) 0.0322(10) Uani 1 1 d . . . . .
N3 N 0.4346(3) 0.3591(3) 0.16132(11) 0.0340(10) Uani 1 1 d . . . . .
H3A H 0.4198 0.4043 0.1711 0.041 Uiso 1 1 calc R U . . .
N4 N 0.4375(3) 0.2917(3) 0.20912(11) 0.0367(10) Uani 1 1 d . . . . .
H4A H 0.4572 0.2521 0.2198 0.044 Uiso 1 1 calc R U . . .
S1 S 0.49653(10) 0.20274(10) 0.16514(4) 0.0355(4) Uani 1 1 d . . . . .
O1 O 0.3722(4) 0.4144(3) 0.21189(10) 0.0542(12) Uani 1 1 d . . . . .
O2 O 0.6469(3) 0.4210(3) 0.24492(11) 0.0499(11) Uani 1 1 d . . . . .
O3 O 0.6667 0.3333 0.2882(2) 0.075(3) Uani 1 3 d S T P . .
O4 O 0.3333 0.6667 -0.0001(3) 0.155(6) Uani 1 3 d S T P . .
O5 O 0.2331(4) 0.6619(4) 0.03988(17) 0.097(2) Uani 1 1 d . . . . .
Mn1 Mn 0.6667 0.3333 0.13040(3) 0.0291(4) Uani 1 3 d S T P . .
Cl1 Cl 0.6667 0.3333 0.25665(7) 0.0481(7) Uani 1 3 d S T P . .
Cl2 Cl 0.3333 0.6667 0.0302 0.0412(6) Uani 1 3 d S T P . .
C15 C 0.365(4) 0.739(2) 0.1285(5) 0.164(14) Uani 0.3333 1 d D U P . .
C16 C 0.3981(18) 0.8118(15) 0.1564(4) 0.065(6) Uani 0.3333 1 d D U P . .
H16A H 0.4310 0.7849 0.1710 0.097 Uiso 0.3333 1 calc R U P . .
H16B H 0.3325 0.8089 0.1650 0.097 Uiso 0.3333 1 calc R U P . .
H16C H 0.4515 0.8880 0.1511 0.097 Uiso 0.3333 1 calc R U P . .
N5 N 0.3333 0.6667 0.1159(4) 0.1502(13) Uani 1 3 d DS TU 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
C1 N1 1.483(6) . ?
C1 C2 1.510(7) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N2 1.341(7) . ?
C2 C3 1.384(7) . ?
C3 C4 1.398(8) . ?
C3 H3 0.9300 . ?
C4 C5 1.356(9) . ?
C4 H4 0.9300 . ?
C5 C6 1.380(7) . ?
C5 H5 0.9300 . ?
C6 N2 1.355(6) . ?
C6 N3 1.391(6) . ?
C7 N3 1.331(6) . ?
C7 N4 1.360(7) . ?
C7 S1 1.702(5) . ?
C8 O1 1.231(6) . ?
C8 N4 1.401(7) . ?
C8 C9 1.479(8) . ?
C9 C14 1.376(7) . ?
C9 C10 1.390(7) . ?
C10 C11 1.353(8) . ?
C10 H10 0.9300 . ?
C11 C12 1.388(8) . ?
C11 H11 0.9300 . ?
C12 C13 1.371(8) . ?
C12 H12 0.9300 . ?
C13 C14 1.377(8) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
N1 C1 1.482(6) 3_665 ?
N1 C1 1.482(6) 2_655 ?
N1 Mn1 2.277(8) . ?
N2 Mn1 2.436(4) . ?
N3 H3A 0.8600 . ?
N4 H4A 0.8600 . ?
S1 Mn1 2.6148(16) . ?
O2 Cl1 1.456(4) . ?
O3 Cl1 1.390(9) . ?
O4 Cl2 1.335(14) . ?
O5 Cl2 1.411(5) . ?
Mn1 N2 2.435(4) 2_655 ?
Mn1 N2 2.435(4) 3_665 ?
Mn1 S1 2.6139(16) 2_655 ?
Mn1 S1 2.6151(16) 3_665 ?
Cl1 O2 1.455(4) 3_665 ?
Cl1 O2 1.455(4) 2_655 ?
Cl2 O5 1.411(5) 3_565 ?
Cl2 O5 1.411(5) 2_665 ?
C15 N5 1.030(9) . ?
C15 C15 1.50(4) 3_565 ?
C15 C15 1.50(4) 2_665 ?
C15 C16 1.503(9) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
N5 C15 1.030(9) 2_665 ?
N5 C15 1.030(9) 3_565 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 111.8(4) . . ?
N1 C1 H1A 109.3 . . ?
C2 C1 H1A 109.3 . . ?
N1 C1 H1B 109.3 . . ?
C2 C1 H1B 109.3 . . ?
H1A C1 H1B 107.9 . . ?
N2 C2 C3 123.2(5) . . ?
N2 C2 C1 116.3(4) . . ?
C3 C2 C1 120.3(5) . . ?
C2 C3 C4 117.3(5) . . ?
C2 C3 H3 121.3 . . ?
C4 C3 H3 121.3 . . ?
C5 C4 C3 120.7(5) . . ?
C5 C4 H4 119.7 . . ?
C3 C4 H4 119.7 . . ?
C4 C5 C6 118.2(5) . . ?
C4 C5 H5 120.9 . . ?
C6 C5 H5 120.9 . . ?
N2 C6 C5 123.2(5) . . ?
N2 C6 N3 118.7(4) . . ?
C5 C6 N3 118.1(5) . . ?
N3 C7 N4 118.3(4) . . ?
N3 C7 S1 123.9(4) . . ?
N4 C7 S1 117.8(4) . . ?
O1 C8 N4 119.3(6) . . ?
O1 C8 C9 123.7(5) . . ?
N4 C8 C9 117.0(5) . . ?
C14 C9 C10 119.7(6) . . ?
C14 C9 C8 123.3(5) . . ?
C10 C9 C8 116.8(5) . . ?
C11 C10 C9 120.0(6) . . ?
C11 C10 H10 120.0 . . ?
C9 C10 H10 120.0 . . ?
C10 C11 C12 120.7(6) . . ?
C10 C11 H11 119.6 . . ?
C12 C11 H11 119.6 . . ?
C13 C12 C11 119.2(6) . . ?
C13 C12 H12 120.4 . . ?
C11 C12 H12 120.4 . . ?
C12 C13 C14 120.5(6) . . ?
C12 C13 H13 119.7 . . ?
C14 C13 H13 119.7 . . ?
C9 C14 C13 119.8(6) . . ?
C9 C14 H14 120.1 . . ?
C13 C14 H14 120.1 . . ?
C1 N1 C1 108.8(4) 3_665 2_655 ?
C1 N1 C1 108.8(4) 3_665 . ?
C1 N1 C1 108.8(4) 2_655 . ?
C1 N1 Mn1 110.2(4) 3_665 . ?
C1 N1 Mn1 110.2(4) 2_655 . ?
C1 N1 Mn1 110.1(4) . . ?
C2 N2 C6 117.3(4) . . ?
C2 N2 Mn1 112.9(3) . . ?
C6 N2 Mn1 129.4(3) . . ?
C7 N3 C6 130.6(4) . . ?
C7 N3 H3A 114.7 . . ?
C6 N3 H3A 114.7 . . ?
C7 N4 C8 128.6(5) . . ?
C7 N4 H4A 115.7 . . ?
C8 N4 H4A 115.7 . . ?
C7 S1 Mn1 103.09(17) . . ?
N1 Mn1 N2 72.67(11) . 2_655 ?
N1 Mn1 N2 72.68(11) . 3_665 ?
N2 Mn1 N2 111.56(10) 2_655 3_665 ?
N1 Mn1 N2 72.68(11) . . ?
N2 Mn1 N2 111.53(10) 2_655 . ?
N2 Mn1 N2 111.51(10) 3_665 . ?
N1 Mn1 S1 125.89(4) . 2_655 ?
N2 Mn1 S1 77.09(10) 2_655 2_655 ?
N2 Mn1 S1 78.44(10) 3_665 2_655 ?
N2 Mn1 S1 161.41(13) . 2_655 ?
N1 Mn1 S1 125.88(4) . . ?
N2 Mn1 S1 78.43(10) 2_655 . ?
N2 Mn1 S1 161.42(13) 3_665 . ?
N2 Mn1 S1 77.06(10) . . ?
S1 Mn1 S1 89.13(6) 2_655 . ?
N1 Mn1 S1 125.87(4) . 3_665 ?
N2 Mn1 S1 161.43(13) 2_655 3_665 ?
N2 Mn1 S1 77.07(10) 3_665 3_665 ?
N2 Mn1 S1 78.40(10) . 3_665 ?
S1 Mn1 S1 89.13(6) 2_655 3_665 ?
S1 Mn1 S1 89.11(6) . 3_665 ?
O3 Cl1 O2 110.8(2) . 3_665 ?
O3 Cl1 O2 110.8(2) . 2_655 ?
O2 Cl1 O2 108.1(2) 3_665 2_655 ?
O3 Cl1 O2 110.8(2) . . ?
O2 Cl1 O2 108.1(2) 3_665 . ?
O2 Cl1 O2 108.1(2) 2_655 . ?
O4 Cl2 O5 107.6(3) . . ?
O4 Cl2 O5 107.6(3) . 3_565 ?
O5 Cl2 O5 111.3(3) . 3_565 ?
O4 Cl2 O5 107.6(3) . 2_665 ?
O5 Cl2 O5 111.3(3) . 2_665 ?
O5 Cl2 O5 111.3(3) 3_565 2_665 ?
N5 C15 C15 43.3(14) . 3_565 ?
N5 C15 C15 43.3(14) . 2_665 ?
C15 C15 C15 60.001(7) 3_565 2_665 ?
N5 C15 C16 158(3) . . ?
C15 C15 C16 120(3) 3_565 . ?
C15 C15 C16 120(3) 2_665 . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 N5 C15 93(3) . 2_665 ?
C15 N5 C15 93(3) . 3_565 ?
C15 N5 C15 93(3) 2_665 3_565 ?

_refine_diff_density_max         0.713
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.078

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_aja0838
_database_code_depnum_ccdc_archive 'CCDC 1470091'
_audit_update_record             
;
2016-03-22 deposited with the CCDC.
2016-05-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H36.50 Cd Cl2 N10 O11.25 S3'
_chemical_formula_weight         1140.79

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3 :H'
_space_group_name_Hall           '-R 3'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   13.8780(17)
_cell_length_b                   13.8780(17)
_cell_length_c                   43.257(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     7215(2)
_cell_formula_units_Z            6
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    1023
_cell_measurement_theta_min      2.825
_cell_measurement_theta_max      25.242

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_F_000             3471
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    0.765
_shelx_estimated_absorpt_T_min   0.862
_shelx_estimated_absorpt_T_max   0.985
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.862
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7891
_diffrn_reflns_av_unetI/netI     0.2631
_diffrn_reflns_av_R_equivalents  0.1115
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_theta_min         2.825
_diffrn_reflns_theta_max         27.523
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.806
_diffrn_measured_fraction_theta_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.806
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.806
_diffrn_reflns_point_group_measured_fraction_full 0.981
_reflns_number_total             2976
_reflns_number_gt                1099
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1069P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2976
_refine_ls_number_parameters     210
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.0925
_refine_ls_R_factor_gt           0.0844
_refine_ls_wR_factor_ref         0.2295
_refine_ls_wR_factor_gt          0.2064
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.020
_refine_ls_shift/su_max          0.008
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.0726(4) 0.1126(4) 0.27414(16) 0.0452(14) Uani 1 1 d . U . . .
H1A H 0.1507 0.1310 0.2712 0.054 Uiso 1 1 calc R U . . .
H1B H 0.0607 0.1159 0.2966 0.054 Uiso 1 1 calc R U . . .
C2 C 0.0564(5) 0.1988(5) 0.25829(19) 0.0499(15) Uani 1 1 d . U . . .
C3 C 0.0712(5) 0.2945(5) 0.27278(18) 0.0507(16) Uani 1 1 d . . . . .
H3 H 0.0831 0.3029 0.2945 0.061 Uiso 1 1 calc R U . . .
C4 C 0.0689(6) 0.3763(5) 0.2561(2) 0.062(2) Uani 1 1 d . . . . .
H4 H 0.0826 0.4430 0.2660 0.074 Uiso 1 1 calc R U . . .
C5 C 0.0464(6) 0.3627(5) 0.22450(18) 0.0524(17) Uani 1 1 d . . . . .
H5 H 0.0399 0.4174 0.2129 0.063 Uiso 1 1 calc R U . . .
C6 C 0.0338(4) 0.2673(5) 0.21037(15) 0.0408(13) Uani 1 1 d . . . . .
C7 C -0.0450(5) 0.1679(5) 0.16089(19) 0.0489(16) Uani 1 1 d . . . . .
C8 C 0.0142(5) 0.2846(5) 0.11379(18) 0.0462(14) Uani 1 1 d . U . . .
C9 C -0.0068(5) 0.2834(4) 0.08014(17) 0.0427(14) Uani 1 1 d . U . . .
C10 C -0.0983(5) 0.1945(6) 0.06603(17) 0.0548(17) Uani 1 1 d . . . . .
H10 H -0.1498 0.1328 0.0781 0.066 Uiso 1 1 calc R U . . .
C11 C -0.1142(6) 0.1959(6) 0.03472(18) 0.0612(19) Uani 1 1 d . . . . .
H11 H -0.1754 0.1340 0.0251 0.073 Uiso 1 1 calc R U . . .
C12 C -0.0422(7) 0.2862(7) 0.0172(2) 0.075(2) Uani 1 1 d . . . . .
H12 H -0.0545 0.2873 -0.0043 0.089 Uiso 1 1 calc R U . . .
C13 C 0.0494(5) 0.3768(6) 0.0313(2) 0.0599(19) Uani 1 1 d . . . . .
H13 H 0.0992 0.4398 0.0194 0.072 Uiso 1 1 calc R U . . .
C14 C 0.0663(6) 0.3734(6) 0.06272(19) 0.0561(17) Uani 1 1 d . . . . .
H14 H 0.1290 0.4338 0.0723 0.067 Uiso 1 1 calc R U . . .
N1 N 0.0000 0.0000 0.26353(18) 0.0380(19) Uani 1 3 d S T P . .
N2 N 0.0386(3) 0.1866(4) 0.22666(13) 0.0404(11) Uani 1 1 d . U . . .
N3 N 0.0233(4) 0.2547(4) 0.17747(12) 0.0401(11) Uani 1 1 d . . . . .
H3A H 0.0696 0.3139 0.1668 0.048 Uiso 1 1 calc R U . . .
N4 N -0.0403(4) 0.1875(4) 0.12919(14) 0.0482(14) Uani 1 1 d . . . . .
H4A H -0.0783 0.1280 0.1176 0.058 Uiso 1 1 calc R U . . .
O1 O 0.0804(4) 0.3734(4) 0.12745(12) 0.0720(15) Uani 1 1 d . . . . .
O2 O 0.2370(5) 0.6669(5) 0.02275(16) 0.0850(18) Uani 1 1 d . . . . .
O3 O 0.3333 0.6667 0.0663(3) 0.118(4) Uani 1 3 d S T P . .
O4 O 0.0000 0.0000 0.0454(3) 0.126(5) Uani 1 3 d S T P . .
O5 O -0.1029(4) -0.0154(4) 0.09211(15) 0.0765(17) Uani 1 1 d . . . . .
O6 O 0.3333 0.6667 0.1667 0.102(11) Uani 0.5 6 d S T P . .
S1 S -0.13369(11) 0.04177(12) 0.17356(4) 0.0417(5) Uani 1 1 d . . . . .
Cl1 Cl 0.3333 0.6667 0.03322(8) 0.0525(8) Uani 1 3 d S T P . .
Cl2 Cl 0.0000 0.0000 0.08153(11) 0.0767(11) Uani 1 3 d S T P . .
Cd1 Cd 0.0000 0.0000 0.20809(2) 0.0340(4) Uani 1 3 d S T 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
C1 N1 1.447(6) . ?
C1 C2 1.490(8) . ?
C2 N2 1.386(9) . ?
C2 C3 1.388(9) . ?
C3 C4 1.359(9) . ?
C4 C5 1.393(10) . ?
C5 C6 1.388(8) . ?
C6 N2 1.353(7) . ?
C6 N3 1.433(8) . ?
C7 N3 1.312(7) . ?
C7 N4 1.393(9) . ?
C7 S1 1.651(7) . ?
C8 O1 1.257(7) . ?
C8 N4 1.347(8) . ?
C8 C9 1.483(10) . ?
C9 C14 1.375(9) . ?
C9 C10 1.393(9) . ?
C10 C11 1.374(10) . ?
C11 C12 1.374(10) . ?
C12 C13 1.404(10) . ?
C13 C14 1.383(10) . ?
N1 C1 1.447(6) 3 ?
N1 C1 1.447(6) 2 ?
N1 Cd1 2.398(8) . ?
N2 Cd1 2.500(5) . ?
O2 Cl1 1.413(5) . ?
O3 Cl1 1.433(13) . ?
O4 Cl2 1.564(15) . ?
O5 Cl2 1.411(5) . ?
S1 Cd1 2.6617(16) . ?
Cl1 O2 1.413(5) 2_665 ?
Cl1 O2 1.413(6) 3_565 ?
Cl2 O5 1.411(5) 3 ?
Cl2 O5 1.411(5) 2 ?
Cd1 N2 2.500(5) 2 ?
Cd1 N2 2.500(5) 3 ?
Cd1 S1 2.6617(16) 2 ?
Cd1 S1 2.6617(16) 3 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 114.7(5) . . ?
N2 C2 C3 119.7(6) . . ?
N2 C2 C1 116.4(6) . . ?
C3 C2 C1 123.4(7) . . ?
C4 C3 C2 120.4(7) . . ?
C3 C4 C5 120.4(6) . . ?
C6 C5 C4 118.3(6) . . ?
N2 C6 C5 121.7(6) . . ?
N2 C6 N3 117.4(5) . . ?
C5 C6 N3 120.7(5) . . ?
N3 C7 N4 114.7(6) . . ?
N3 C7 S1 127.2(6) . . ?
N4 C7 S1 118.1(4) . . ?
O1 C8 N4 121.2(7) . . ?
O1 C8 C9 121.1(6) . . ?
N4 C8 C9 117.7(5) . . ?
C14 C9 C10 119.8(7) . . ?
C14 C9 C8 118.4(6) . . ?
C10 C9 C8 121.8(6) . . ?
C11 C10 C9 120.1(6) . . ?
C10 C11 C12 120.4(7) . . ?
C11 C12 C13 119.9(8) . . ?
C14 C13 C12 119.3(7) . . ?
C9 C14 C13 120.6(7) . . ?
C1 N1 C1 110.4(4) 3 . ?
C1 N1 C1 110.4(4) 3 2 ?
C1 N1 C1 110.4(4) . 2 ?
C1 N1 Cd1 108.5(4) 3 . ?
C1 N1 Cd1 108.5(4) . . ?
C1 N1 Cd1 108.5(4) 2 . ?
C6 N2 C2 119.5(5) . . ?
C6 N2 Cd1 128.1(4) . . ?
C2 N2 Cd1 112.1(4) . . ?
C7 N3 C6 129.6(6) . . ?
C8 N4 C7 129.0(6) . . ?
C7 S1 Cd1 100.7(2) . . ?
O2 Cl1 O2 110.2(3) . 2_665 ?
O2 Cl1 O2 110.2(3) . 3_565 ?
O2 Cl1 O2 110.2(3) 2_665 3_565 ?
O2 Cl1 O3 108.7(3) . . ?
O2 Cl1 O3 108.7(3) 2_665 . ?
O2 Cl1 O3 108.7(3) 3_565 . ?
O5 Cl2 O5 110.0(3) 3 2 ?
O5 Cl2 O5 110.0(3) 3 . ?
O5 Cl2 O5 110.0(3) 2 . ?
O5 Cl2 O4 108.9(3) 3 . ?
O5 Cl2 O4 108.9(3) 2 . ?
O5 Cl2 O4 108.9(3) . . ?
N1 Cd1 N2 71.26(13) . 2 ?
N1 Cd1 N2 71.26(13) . 3 ?
N2 Cd1 N2 110.19(13) 2 3 ?
N1 Cd1 N2 71.26(13) . . ?
N2 Cd1 N2 110.19(13) 2 . ?
N2 Cd1 N2 110.19(13) 3 . ?
N1 Cd1 S1 124.13(4) . . ?
N2 Cd1 S1 79.08(11) 2 . ?
N2 Cd1 S1 164.52(14) 3 . ?
N2 Cd1 S1 76.50(12) . . ?
N1 Cd1 S1 124.13(4) . 2 ?
N2 Cd1 S1 76.50(12) 2 2 ?
N2 Cd1 S1 79.08(11) 3 2 ?
N2 Cd1 S1 164.52(14) . 2 ?
S1 Cd1 S1 91.59(5) . 2 ?
N1 Cd1 S1 124.13(4) . 3 ?
N2 Cd1 S1 164.52(14) 2 3 ?
N2 Cd1 S1 76.50(12) 3 3 ?
N2 Cd1 S1 79.08(11) . 3 ?
S1 Cd1 S1 91.59(5) . 3 ?
S1 Cd1 S1 91.59(5) 2 3 ?

_refine_diff_density_max         0.792
_refine_diff_density_min         -0.934
_refine_diff_density_rms         0.159

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_aja0821
_database_code_depnum_ccdc_archive 'CCDC 1470093'
_audit_update_record             
;
2016-03-22 deposited with the CCDC.
2016-05-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C51.20 H50.60 Cl2 N14.60 Ni O11.40 S3'
_chemical_formula_weight         1278.65

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.8450(5)
_cell_length_b                   14.6430(5)
_cell_length_c                   15.8030(6)
_cell_angle_alpha                107.831(2)
_cell_angle_beta                 97.828(2)
_cell_angle_gamma                94.342(2)
_cell_volume                     2997.95(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6566
_cell_measurement_theta_min      2.92
_cell_measurement_theta_max      27.57

_exptl_crystal_description       needle
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_F_000             1322
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.587
_shelx_estimated_absorpt_T_min   0.867
_shelx_estimated_absorpt_T_max   0.944
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.8671
_exptl_absorpt_correction_T_max  0.9436
_exptl_absorpt_process_details   Denzo/Scalepack

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            25225
_diffrn_reflns_av_unetI/netI     0.1650
_diffrn_reflns_av_R_equivalents  0.1043
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.921
_diffrn_reflns_theta_max         27.570
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             13501
_reflns_number_gt                6559
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1189P)²+0.6118P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         13501
_refine_ls_number_parameters     838
_refine_ls_number_restraints     272
_refine_ls_R_factor_all          0.1942
_refine_ls_R_factor_gt           0.0931
_refine_ls_wR_factor_ref         0.2617
_refine_ls_wR_factor_gt          0.2129
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.051
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.1362(5) 0.0453(4) 0.6047(4) 0.0478(15) Uani 1 1 d . . . A 1
H1A H 0.1168 -0.0072 0.5484 0.057 Uiso 1 1 calc R U . A 1
H1B H 0.1237 0.1050 0.5932 0.057 Uiso 1 1 calc R U . A 1
C2 C 0.0754(5) 0.0305(4) 0.6715(4) 0.0419(14) Uani 1 1 d . . . A 1
C3 C -0.0191(5) -0.0169(4) 0.6450(4) 0.0528(16) Uani 1 1 d . . . A 1
H3 H -0.0451 -0.0448 0.5841 0.063 Uiso 1 1 calc R U . A 1
C4 C -0.0748(5) -0.0224(4) 0.7102(4) 0.0519(16) Uani 1 1 d . . . A 1
H4 H -0.1391 -0.0529 0.6933 0.062 Uiso 1 1 calc R U . A 1
C5 C -0.0351(4) 0.0170(4) 0.7985(4) 0.0423(13) Uani 1 1 d . . . A 1
H5 H -0.0714 0.0137 0.8430 0.051 Uiso 1 1 calc R U . A 1
C6 C 0.0625(4) 0.0632(4) 0.8217(3) 0.0351(12) Uani 1 1 d . . . A 1
C7 C 0.1758(4) 0.1619(4) 0.9624(3) 0.0347(12) Uani 1 1 d . . . A 1
C8 C 0.1033(4) 0.1725(4) 1.1013(4) 0.0387(13) Uani 1 1 d . . . A 1
C9 C 0.1240(5) 0.2177(4) 1.2011(4) 0.0442(14) Uani 1 1 d . . . A 1
C10 C 0.0432(5) 0.2289(4) 1.2458(4) 0.0472(15) Uani 1 1 d . . . A 1
H10 H -0.0201 0.2119 1.2129 0.057 Uiso 1 1 calc R U . A 1
C11 C 0.0570(5) 0.2648(5) 1.3379(4) 0.0555(17) Uani 1 1 d . . . A 1
H11 H 0.0030 0.2742 1.3674 0.067 Uiso 1 1 calc R U . A 1
C12 C 0.1503(6) 0.2870(5) 1.3870(4) 0.0600(18) Uani 1 1 d . . . A 1
H12 H 0.1591 0.3103 1.4496 0.072 Uiso 1 1 calc R U . A 1
C13 C 0.2312(5) 0.2749(5) 1.3442(4) 0.0609(18) Uani 1 1 d . . . A 1
H13 H 0.2942 0.2900 1.3777 0.073 Uiso 1 1 calc R U . A 1
C14 C 0.2178(5) 0.2405(4) 1.2517(4) 0.0495(15) Uani 1 1 d . . . A 1
H14 H 0.2722 0.2323 1.2227 0.059 Uiso 1 1 calc R U . A 1
C15 C 0.3032(5) 0.1102(4) 0.5991(4) 0.0582(17) Uani 1 1 d . . . A 1
H15A H 0.2842 0.0904 0.5341 0.070 Uiso 1 1 calc R U . A 1
H15B H 0.3720 0.1026 0.6127 0.070 Uiso 1 1 calc R U . A 1
C16 C 0.2882(5) 0.2157(4) 0.6405(4) 0.0495(15) Uani 1 1 d . . . A 1
C17 C 0.3091(5) 0.2825(5) 0.5989(4) 0.0600(18) Uani 1 1 d . . . A 1
H17 H 0.3331 0.2640 0.5447 0.072 Uiso 1 1 calc R U . A 1
C18 C 0.2945(5) 0.3761(5) 0.6373(5) 0.0622(18) Uani 1 1 d . . . A 1
H18 H 0.3094 0.4226 0.6104 0.075 Uiso 1 1 calc R U . A 1
C19 C 0.2574(5) 0.4007(4) 0.7166(4) 0.0526(16) Uani 1 1 d . . . A 1
H19 H 0.2456 0.4640 0.7435 0.063 Uiso 1 1 calc R U . A 1
C20 C 0.2379(4) 0.3314(4) 0.7555(4) 0.0434(14) Uani 1 1 d . . . A 1
C21 C 0.2227(4) 0.4214(4) 0.9102(4) 0.0462(14) Uani 1 1 d . . . A 1
C22 C 0.0784(5) 0.3694(4) 0.9704(4) 0.0447(15) Uani 1 1 d . . . A 1
C23 C 0.0304(4) 0.3951(4) 1.0528(5) 0.0530(16) Uani 1 1 d D U . A 1
C24 C 0.0697(8) 0.4570(7) 1.1326(7) 0.109(3) Uani 1 1 d . U . A 1
H24 H 0.1326 0.4885 1.1395 0.130 Uiso 1 1 calc R U . A 1
C25 C 0.0216(9) 0.4775(7) 1.2067(7) 0.124(3) Uani 1 1 d . U . A 1
H25 H 0.0525 0.5211 1.2618 0.148 Uiso 1 1 calc R U . A 1
C26 C -0.0659(8) 0.4356(7) 1.1985(7) 0.096(2) Uani 1 1 d . U . A 1
H26 H -0.0982 0.4496 1.2480 0.115 Uiso 1 1 calc R U . A 1
C27 C -0.1105(7) 0.3731(7) 1.1211(7) 0.092(2) Uani 1 1 d . U . A 1
H27 H -0.1745 0.3455 1.1164 0.110 Uiso 1 1 calc R U . A 1
C28 C -0.0626(5) 0.3471(6) 1.0449(6) 0.079(2) Uani 1 1 d D . . A 1
H28 H -0.0923 0.2998 0.9915 0.095 Uiso 1 1 calc R U . A 1
C29 C 0.2742(5) -0.0487(4) 0.6144(4) 0.0550(17) Uani 1 1 d . . . A 1
H29A H 0.2390 -0.0888 0.5558 0.066 Uiso 1 1 calc R U . A 1
H29B H 0.3439 -0.0445 0.6115 0.066 Uiso 1 1 calc R U . A 1
C30 C 0.2546(5) -0.0939(4) 0.6834(4) 0.0478(15) Uani 1 1 d . . . A 1
C31 C 0.2206(5) -0.1907(4) 0.6619(5) 0.0545(16) Uani 1 1 d . . . A 1
H31 H 0.2014 -0.2294 0.6021 0.065 Uiso 1 1 calc R U . A 1
C32 C 0.2158(6) -0.2282(5) 0.7309(5) 0.068(2) Uani 1 1 d . . . A 1
H32 H 0.1904 -0.2925 0.7180 0.081 Uiso 1 1 calc R U . A 1
C33 C 0.2480(5) -0.1722(4) 0.8185(5) 0.0613(18) Uani 1 1 d . . . A 1
H33 H 0.2475 -0.1980 0.8655 0.074 Uiso 1 1 calc R U . A 1
C34 C 0.2812(4) -0.0760(4) 0.8349(4) 0.0438(14) Uani 1 1 d . . . A 1
C35 C 0.3098(4) -0.0100(4) 1.0028(4) 0.0422(14) Uani 1 1 d . . . A 1
C36 C 0.4526(4) 0.1214(4) 1.0683(5) 0.0464(15) Uani 1 1 d . . . A 1
C37 C 0.4978(4) 0.1983(4) 1.1528(4) 0.0499(15) Uani 1 1 d . . . A 1
C38 C 0.4918(5) 0.1932(6) 1.2371(5) 0.072(2) Uani 1 1 d . . . A 1
H38 H 0.4598 0.1380 1.2432 0.087 Uiso 1 1 calc R U . A 1
C39 C 0.5331(6) 0.2697(6) 1.3133(5) 0.090(3) Uani 1 1 d . . . A 1
H39 H 0.5279 0.2666 1.3704 0.108 Uiso 1 1 calc R U . A 1
C40 C 0.5819(6) 0.3505(6) 1.3036(6) 0.094(3) Uani 1 1 d . . . A 1
H40 H 0.6109 0.4017 1.3543 0.112 Uiso 1 1 calc R U . A 1
C41 C 0.5875(6) 0.3552(6) 1.2198(7) 0.082(2) Uani 1 1 d . . . A 1
H41 H 0.6194 0.4105 1.2138 0.099 Uiso 1 1 calc R U . A 1
C42 C 0.5473(5) 0.2806(5) 1.1446(5) 0.0648(19) Uani 1 1 d . . . A 1
H42 H 0.5529 0.2846 1.0878 0.078 Uiso 1 1 calc R U . A 1
C43 C 0.4943(6) 0.1692(4) 0.8245(4) 0.0495(16) Uani 1 1 d . . . A 1
C44 C 0.5985(5) 0.1950(6) 0.8627(5) 0.072(2) Uani 1 1 d . . . A 1
H44A H 0.6089 0.1917 0.9230 0.108 Uiso 1 1 calc R U . A 1
H44B H 0.6192 0.2595 0.8640 0.108 Uiso 1 1 calc R U . A 1
H44C H 0.6358 0.1507 0.8264 0.108 Uiso 1 1 calc R U . A 1
N1 N 0.2430(4) 0.0496(3) 0.6362(3) 0.0451(12) Uani 1 1 d . . . A 1
N2 N 0.1162(3) 0.0718(3) 0.7606(3) 0.0373(11) Uani 1 1 d . . . A 1
N3 N 0.0979(3) 0.1007(3) 0.9135(3) 0.0369(10) Uani 1 1 d . . . A 1
H3A H 0.0618 0.0798 0.9455 0.044 Uiso 1 1 calc R U . A 1
N4 N 0.1745(3) 0.1969(3) 1.0551(3) 0.0381(11) Uani 1 1 d . . . A 1
H4A H 0.2235 0.2382 1.0873 0.046 Uiso 1 1 calc R U . A 1
N5 N 0.2556(4) 0.2392(3) 0.7200(3) 0.0434(12) Uani 1 1 d . . . A 1
N6 N 0.1917(3) 0.3506(3) 0.8324(3) 0.0415(11) Uani 1 1 d . . . A 1
H6 H 0.1390 0.3135 0.8287 0.050 Uiso 1 1 calc R U . A 1
N7 N 0.1628(4) 0.4298(3) 0.9753(3) 0.0445(12) Uani 1 1 d . . . A 1
H7 H 0.1799 0.4778 1.0242 0.053 Uiso 1 1 calc R U . A 1
N8 N 0.2826(4) -0.0363(3) 0.7708(3) 0.0423(11) Uani 1 1 d . . . A 1
N9 N 0.3286(3) -0.0148(3) 0.9209(3) 0.0442(12) Uani 1 1 d . . . A 1
H9 H 0.3769 0.0255 0.9205 0.053 Uiso 1 1 calc R U . A 1
N10 N 0.3741(3) 0.0592(3) 1.0738(3) 0.0403(11) Uani 1 1 d . . . A 1
H10A H 0.3637 0.0638 1.1273 0.048 Uiso 1 1 calc R U . A 1
N11 N 0.4133(4) 0.1497(3) 0.7954(3) 0.0464(12) Uani 1 1 d . . . A 1
O1 O 0.0447(3) 0.3003(3) 0.9029(3) 0.0521(10) Uani 1 1 d . . . A 1
O2 O 0.0298(3) 0.1158(3) 1.0623(3) 0.0468(10) Uani 1 1 d . . . A 1
O3 O 0.4806(3) 0.1155(3) 0.9967(3) 0.0529(11) Uani 1 1 d . . . A 1
S1 S 0.32512(14) 0.49794(13) 0.93574(12) 0.0647(5) Uani 1 1 d . . . A 1
S2 S 0.27454(11) 0.20250(10) 0.92832(9) 0.0382(3) Uani 1 1 d . . . A 1
S3 S 0.21784(12) -0.07158(12) 1.02610(11) 0.0554(4) Uani 1 1 d . . . A 1
Ni1 Ni 0.26349(5) 0.11688(5) 0.77470(4) 0.0387(2) Uani 1 1 d . . . A 1
C45 C 0.3683(5) 0.4408(5) 0.1565(4) 0.0563(17) Uani 1 1 d . . . B 1
C46 C 0.4376(6) 0.5284(6) 0.1742(7) 0.087(2) Uani 1 1 d . . . B 1
H46A H 0.4042 0.5757 0.1551 0.130 Uiso 1 1 calc R U . B 1
H46B H 0.4908 0.5125 0.1414 0.130 Uiso 1 1 calc R U . B 1
H46C H 0.4630 0.5543 0.2375 0.130 Uiso 1 1 calc R U . B 1
N12 N 0.3156(4) 0.3757(4) 0.1437(4) 0.0642(15) Uani 1 1 d . . . B 1
C47 C 0.8014(6) 0.2945(6) 0.8105(7) 0.084(3) Uani 1 1 d . . . C 1
C48 C 0.8339(5) 0.2009(5) 0.7736(5) 0.074(2) Uani 1 1 d . . . C 1
H48A H 0.9027 0.2092 0.7708 0.111 Uiso 1 1 calc R U . C 1
H48B H 0.7976 0.1691 0.7141 0.111 Uiso 1 1 calc R U . C 1
H48C H 0.8229 0.1622 0.8115 0.111 Uiso 1 1 calc R U . C 1
N13 N 0.7764(7) 0.3663(6) 0.8411(8) 0.140(4) Uani 1 1 d . . . C 1
C49 C 0.4313(11) 0.7658(10) 0.3722(11) 0.133(10) Uani 0.601(12) 1 d D . P D 1
C50 C 0.3852(12) 0.7939(12) 0.4507(10) 0.102(6) Uani 0.601(12) 1 d D . P D 1
H50A H 0.3463 0.7386 0.4546 0.153 Uiso 0.601(12) 1 calc R U P D 1
H50B H 0.3437 0.8425 0.4465 0.153 Uiso 0.601(12) 1 calc R U P D 1
H50C H 0.4347 0.8194 0.5036 0.153 Uiso 0.601(12) 1 calc R U P D 1
N14 N 0.461(3) 0.728(2) 0.3095(17) 0.284(19) Uani 0.601(12) 1 d D . P D 1
C51 C 0.1013(11) 0.5258(10) 0.5444(9) 0.063(4) Uani 0.502(8) 1 d D . P E 1
C52 C -0.0068(13) 0.501(4) 0.519(2) 0.105(10) Uani 0.502(8) 1 d D U P E 1
H52A H -0.0378 0.5386 0.5668 0.157 Uiso 0.502(8) 1 calc R U P E 1
H52B H -0.0241 0.4337 0.5092 0.157 Uiso 0.502(8) 1 calc R U P E 1
H52C H -0.0286 0.5157 0.4648 0.157 Uiso 0.502(8) 1 calc R U P E 1
N15 N 0.1723(11) 0.5446(9) 0.5922(10) 0.089(4) Uani 0.502(8) 1 d D U P E 1
C53 C 0.2296(15) 0.5463(13) 0.4546(11) 0.098(5) Uani 0.498(8) 1 d D U P E 2
C54 C 0.2344(17) 0.5305(13) 0.3601(11) 0.114(6) Uani 0.498(8) 1 d D U P E 2
H54A H 0.3006 0.5232 0.3502 0.171 Uiso 0.498(8) 1 calc R U P E 2
H54B H 0.2138 0.5849 0.3438 0.171 Uiso 0.498(8) 1 calc R U P E 2
H54C H 0.1918 0.4731 0.3239 0.171 Uiso 0.498(8) 1 calc R U P E 2
N16 N 0.2323(13) 0.5568(10) 0.5270(10) 0.102(5) Uani 0.498(8) 1 d D U P E 2
Cl1 Cl 0.37621(13) 0.03250(12) 0.35132(11) 0.0601(5) Uani 1 1 d . . . F 1
O4 O 0.3322(4) 0.0244(4) 0.2610(3) 0.0829(16) Uani 1 1 d . . . F 1
O5 O 0.4663(5) -0.0038(5) 0.3491(4) 0.114(2) Uani 1 1 d . . . F 1
O6 O 0.3925(5) 0.1328(4) 0.4064(4) 0.0940(18) Uani 1 1 d . . . F 1
O7 O 0.3099(4) -0.0165(4) 0.3887(3) 0.0889(17) Uani 1 1 d . . . F 1
Cl2 Cl 0.97041(13) 0.25374(11) 0.59124(10) 0.0532(4) Uani 0.524(8) 1 d . . P G
1
O8 O 1.0106(13) 0.2821(12) 0.6835(9) 0.088(5) Uani 0.524(8) 1 d . U P G 1
O9 O 0.9148(9) 0.1601(7) 0.5632(8) 0.095(3) Uani 0.524(8) 1 d . U P G 1
O11 O 1.0484(10) 0.2458(10) 0.5400(8) 0.104(4) Uani 0.524(8) 1 d . U P G 1
O10 O 0.9026(12) 0.3175(10) 0.5850(10) 0.120(4) Uani 0.524(8) 1 d . U P G 1
Cl2A Cl 0.97041(13) 0.25374(11) 0.59124(10) 0.0532(4) Uani 0.476(8) 1 d D U P G
2
O8A O 1.0175(10) 0.2455(9) 0.6742(6) 0.054(3) Uani 0.476(8) 1 d D U P G 2
O9A O 0.9941(9) 0.1797(7) 0.5183(6) 0.089(4) Uani 0.476(8) 1 d D U P G 2
O11A O 1.0010(9) 0.3452(6) 0.5834(8) 0.104(4) Uani 0.476(8) 1 d D U P G 2
O10A O 0.8659(5) 0.2429(10) 0.5880(7) 0.094(4) Uani 0.476(8) 1 d D U P G 2
O12 O 0.4389(16) 0.6386(17) 0.4268(11) 0.171(10) Uani 0.399(12) 1 d . U P D 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
C1 N1 1.484(8) . ?
C1 C2 1.491(8) . ?
C2 N2 1.371(7) . ?
C2 C3 1.379(8) . ?
C3 C4 1.386(8) . ?
C4 C5 1.354(8) . ?
C5 C6 1.411(8) . ?
C6 N2 1.325(6) . ?
C6 N3 1.387(7) . ?
C7 N3 1.329(7) . ?
C7 N4 1.399(6) . ?
C7 S2 1.669(5) . ?
C8 O2 1.222(6) . ?
C8 N4 1.391(7) . ?
C8 C9 1.489(8) . ?
C9 C14 1.388(9) . ?
C9 C10 1.396(8) . ?
C10 C11 1.369(8) . ?
C11 C12 1.373(9) . ?
C12 C13 1.380(9) . ?
C13 C14 1.373(8) . ?
C15 N1 1.472(7) . ?
C15 C16 1.525(8) . ?
C16 N5 1.347(7) . ?
C16 C17 1.369(8) . ?
C17 C18 1.362(9) . ?
C18 C19 1.377(8) . ?
C19 C20 1.366(8) . ?
C20 N5 1.350(7) . ?
C20 N6 1.412(7) . ?
C21 N6 1.334(7) . ?
C21 N7 1.390(7) . ?
C21 S1 1.659(6) . ?
C22 O1 1.229(7) . ?
C22 N7 1.389(7) . ?
C22 C23 1.501(8) . ?
C23 C24 1.323(11) . ?
C23 C28 1.389(5) . ?
C24 C25 1.389(11) . ?
C25 C26 1.287(13) . ?
C26 C27 1.317(13) . ?
C27 C28 1.419(11) . ?
C29 C30 1.482(8) . ?
C29 N1 1.487(7) . ?
C30 N8 1.364(7) . ?
C30 C31 1.380(8) . ?
C31 C32 1.370(9) . ?
C32 C33 1.367(10) . ?
C33 C34 1.383(8) . ?
C34 N8 1.314(7) . ?
C34 N9 1.416(7) . ?
C35 N9 1.336(7) . ?
C35 N10 1.405(7) . ?
C35 S3 1.651(6) . ?
C36 O3 1.226(7) . ?
C36 N10 1.394(7) . ?
C36 C37 1.479(9) . ?
C37 C38 1.371(9) . ?
C37 C42 1.390(8) . ?
C38 C39 1.386(10) . ?
C39 C40 1.377(11) . ?
C40 C41 1.359(11) . ?
C41 C42 1.359(10) . ?
C43 N11 1.131(8) . ?
C43 C44 1.459(10) . ?
N1 Ni1 2.076(4) . ?
N2 Ni1 2.056(5) . ?
N5 Ni1 2.218(4) . ?
N8 Ni1 2.261(4) . ?
N11 Ni1 2.051(6) . ?
S2 Ni1 2.3440(15) . ?
C45 N12 1.104(7) . ?
C45 C46 1.471(10) . ?
C47 N13 1.117(10) . ?
C47 C48 1.448(11) . ?
C49 N14 1.123(8) . ?
C49 C50 1.436(8) . ?
C51 N15 1.115(8) . ?
C51 C52 1.48(3) 2_566 ?
C51 C52 1.482(9) . ?
C53 N16 1.102(8) . ?
C53 C54 1.450(8) . ?
Cl1 O5 1.393(6) . ?
Cl1 O7 1.419(5) . ?
Cl1 O4 1.440(5) . ?
Cl1 O6 1.443(5) . ?
Cl2 O10 1.389(12) . ?
Cl2 O8 1.407(14) . ?
Cl2 O11 1.426(10) . ?
Cl2 O9 1.430(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 112.6(5) . . ?
N2 C2 C3 121.8(5) . . ?
N2 C2 C1 116.3(5) . . ?
C3 C2 C1 121.7(5) . . ?
C2 C3 C4 119.3(6) . . ?
C5 C4 C3 119.5(6) . . ?
C4 C5 C6 118.8(5) . . ?
N2 C6 N3 122.2(5) . . ?
N2 C6 C5 122.7(5) . . ?
N3 C6 C5 115.1(5) . . ?
N3 C7 N4 115.3(4) . . ?
N3 C7 S2 128.8(4) . . ?
N4 C7 S2 115.8(4) . . ?
O2 C8 N4 121.8(5) . . ?
O2 C8 C9 122.5(5) . . ?
N4 C8 C9 115.7(5) . . ?
C14 C9 C10 118.9(5) . . ?
C14 C9 C8 123.8(5) . . ?
C10 C9 C8 117.0(6) . . ?
C11 C10 C9 120.2(6) . . ?
C10 C11 C12 120.1(6) . . ?
C11 C12 C13 120.6(6) . . ?
C14 C13 C12 119.5(7) . . ?
C13 C14 C9 120.7(6) . . ?
N1 C15 C16 109.3(5) . . ?
N5 C16 C17 122.6(6) . . ?
N5 C16 C15 116.5(5) . . ?
C17 C16 C15 120.9(5) . . ?
C18 C17 C16 119.6(6) . . ?
C17 C18 C19 118.7(6) . . ?
C20 C19 C18 119.4(6) . . ?
N5 C20 C19 122.5(5) . . ?
N5 C20 N6 115.7(4) . . ?
C19 C20 N6 121.7(5) . . ?
N6 C21 N7 115.6(5) . . ?
N6 C21 S1 126.2(5) . . ?
N7 C21 S1 118.1(5) . . ?
O1 C22 N7 122.4(5) . . ?
O1 C22 C23 122.2(5) . . ?
N7 C22 C23 115.4(5) . . ?
C24 C23 C28 117.2(7) . . ?
C24 C23 C22 125.9(6) . . ?
C28 C23 C22 116.9(6) . . ?
C23 C24 C25 123.2(9) . . ?
C26 C25 C24 119.5(11) . . ?
C25 C26 C27 121.1(9) . . ?
C26 C27 C28 121.2(8) . . ?
C23 C28 C27 117.5(8) . . ?
C30 C29 N1 110.9(4) . . ?
N8 C30 C31 121.5(5) . . ?
N8 C30 C29 115.5(5) . . ?
C31 C30 C29 122.6(5) . . ?
C32 C31 C30 118.2(6) . . ?
C33 C32 C31 120.8(6) . . ?
C32 C33 C34 117.6(6) . . ?
N8 C34 C33 123.3(6) . . ?
N8 C34 N9 113.8(5) . . ?
C33 C34 N9 122.4(5) . . ?
N9 C35 N10 114.0(5) . . ?
N9 C35 S3 126.8(5) . . ?
N10 C35 S3 119.2(4) . . ?
O3 C36 N10 122.1(6) . . ?
O3 C36 C37 121.3(6) . . ?
N10 C36 C37 116.5(5) . . ?
C38 C37 C42 119.2(7) . . ?
C38 C37 C36 123.7(6) . . ?
C42 C37 C36 117.1(6) . . ?
C37 C38 C39 120.4(7) . . ?
C40 C39 C38 119.4(8) . . ?
C41 C40 C39 119.8(8) . . ?
C40 C41 C42 121.3(7) . . ?
C41 C42 C37 119.8(7) . . ?
N11 C43 C44 179.5(8) . . ?
C15 N1 C1 112.4(5) . . ?
C15 N1 C29 109.9(4) . . ?
C1 N1 C29 111.3(5) . . ?
C15 N1 Ni1 107.1(3) . . ?
C1 N1 Ni1 105.2(3) . . ?
C29 N1 Ni1 110.8(3) . . ?
C6 N2 C2 117.8(5) . . ?
C6 N2 Ni1 130.2(4) . . ?
C2 N2 Ni1 111.0(3) . . ?
C7 N3 C6 133.6(5) . . ?
C8 N4 C7 127.6(5) . . ?
C16 N5 C20 117.1(4) . . ?
C16 N5 Ni1 109.4(4) . . ?
C20 N5 Ni1 132.8(3) . . ?
C21 N6 C20 125.6(5) . . ?
C22 N7 C21 127.4(5) . . ?
C34 N8 C30 118.4(5) . . ?
C34 N8 Ni1 129.5(4) . . ?
C30 N8 Ni1 107.1(3) . . ?
C35 N9 C34 129.9(5) . . ?
C36 N10 C35 128.0(5) . . ?
C43 N11 Ni1 165.9(5) . . ?
C7 S2 Ni1 107.35(19) . . ?
N11 Ni1 N2 173.41(17) . . ?
N11 Ni1 N1 97.57(19) . . ?
N2 Ni1 N1 84.30(18) . . ?
N11 Ni1 N5 86.58(18) . . ?
N2 Ni1 N5 100.01(17) . . ?
N1 Ni1 N5 76.64(17) . . ?
N11 Ni1 N8 89.60(18) . . ?
N2 Ni1 N8 84.47(17) . . ?
N1 Ni1 N8 80.25(17) . . ?
N5 Ni1 N8 155.85(17) . . ?
N11 Ni1 S2 85.98(14) . . ?
N2 Ni1 S2 92.67(12) . . ?
N1 Ni1 S2 174.25(14) . . ?
N5 Ni1 S2 99.15(12) . . ?
N8 Ni1 S2 104.37(12) . . ?
N12 C45 C46 179.2(8) . . ?
N13 C47 C48 178.1(10) . . ?
N14 C49 C50 168(2) . . ?
N15 C51 C52 179(2) . 2_566 ?
N15 C51 C52 154.5(17) . . ?
C52 C51 C52 25(2) 2_566 . ?
N16 C53 C54 175(2) . . ?
O5 Cl1 O7 112.9(4) . . ?
O5 Cl1 O4 109.0(4) . . ?
O7 Cl1 O4 108.9(3) . . ?
O5 Cl1 O6 108.8(4) . . ?
O7 Cl1 O6 107.5(3) . . ?
O4 Cl1 O6 109.6(3) . . ?
O10 Cl2 O8 104.8(9) . . ?
O10 Cl2 O11 120.0(9) . . ?
O8 Cl2 O11 109.0(10) . . ?
O10 Cl2 O9 105.8(9) . . ?
O8 Cl2 O9 110.6(8) . . ?
O11 Cl2 O9 106.6(8) . . ?

_refine_diff_density_max         0.785
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.096

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_aja0909
_database_code_depnum_ccdc_archive 'CCDC 1470094'
_audit_update_record             
;
2016-03-22 deposited with the CCDC.
2016-05-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C45 H40 Cl5 N11 O11 S3 Zn'
_chemical_formula_weight         1249.68

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'
S S 0.1246 0.1234 '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'
Zn Zn 0.2839 1.4301 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_H-M_alt        'P c c n'
_space_group_name_Hall           '-P 2ab 2ac'

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

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

_cell_length_a                   30.5910(3)
_cell_length_b                   19.7950(3)
_cell_length_c                   17.5370(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10619.5(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5486
_cell_measurement_theta_min      2.451
_cell_measurement_theta_max      25.050

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_F_000             5104
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    0.901
_shelx_estimated_absorpt_T_min   0.661
_shelx_estimated_absorpt_T_max   0.982
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.661
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_process_details   Denzo/Scalepack

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Seales tube'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            36743
_diffrn_reflns_av_unetI/netI     0.0817
_diffrn_reflns_av_R_equivalents  0.0869
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.451
_diffrn_reflns_theta_max         25.050
_diffrn_reflns_theta_full        24.500
_diffrn_measured_fraction_theta_max 0.891
_diffrn_measured_fraction_theta_full 0.884
_diffrn_reflns_Laue_measured_fraction_max 0.891
_diffrn_reflns_Laue_measured_fraction_full 0.884
_diffrn_reflns_point_group_measured_fraction_max 0.891
_diffrn_reflns_point_group_measured_fraction_full 0.884
_reflns_number_total             8397
_reflns_number_gt                5486
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0979P)²+64.6242P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8397
_refine_ls_number_parameters     719
_refine_ls_number_restraints     120
_refine_ls_R_factor_all          0.1310
_refine_ls_R_factor_gt           0.0853
_refine_ls_wR_factor_ref         0.2283
_refine_ls_wR_factor_gt          0.2035
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.034
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.9040(2) 0.1029(4) 0.0900(4) 0.0392(18) Uani 1 1 d . . . . .
H1A H 0.9001 0.1375 0.0498 0.047 Uiso 1 1 calc R U . . .
H1B H 0.9345 0.1053 0.1084 0.047 Uiso 1 1 calc R U . . .
C2 C 0.8734(2) 0.1176(3) 0.1549(4) 0.0352(16) Uani 1 1 d . . . . .
C3 C 0.8842(3) 0.1638(4) 0.2104(4) 0.0439(19) Uani 1 1 d . . . . .
H3 H 0.9120 0.1851 0.2102 0.053 Uiso 1 1 calc R U . . .
C4 C 0.8542(3) 0.1787(4) 0.2661(5) 0.048(2) Uani 1 1 d . . . . .
H4 H 0.8606 0.2118 0.3036 0.058 Uiso 1 1 calc R U . . .
C5 C 0.8151(3) 0.1453(4) 0.2671(5) 0.046(2) Uani 1 1 d . . . . .
H5 H 0.7940 0.1542 0.3057 0.055 Uiso 1 1 calc R U . . .
C6 C 0.8069(2) 0.0987(4) 0.2109(4) 0.0346(16) Uani 1 1 d . . . . .
C7 C 0.7625(3) -0.0005(4) 0.2295(5) 0.047(2) Uani 1 1 d . . . . .
C8 C 0.6840(2) 0.0004(4) 0.1941(4) 0.0392(18) Uani 1 1 d . . . . .
C9 C 0.6435(3) -0.0407(4) 0.1937(5) 0.0455(19) Uani 1 1 d . . . . .
C10 C 0.6421(3) -0.1093(4) 0.2139(4) 0.0436(19) Uani 1 1 d . . . . .
H10 H 0.6682 -0.1326 0.2266 0.052 Uiso 1 1 calc R U . . .
C11 C 0.6022(3) -0.1427(4) 0.2153(5) 0.057(2) Uani 1 1 d . . . . .
H11 H 0.6011 -0.1890 0.2296 0.068 Uiso 1 1 calc R U . . .
C12 C 0.5646(4) -0.1099(6) 0.1963(8) 0.097(4) Uani 1 1 d . . . . .
H12 H 0.5375 -0.1334 0.1973 0.116 Uiso 1 1 calc R U . . .
C13 C 0.5656(4) -0.0418(6) 0.1754(11) 0.123(6) Uani 1 1 d . . . . .
H13 H 0.5395 -0.0186 0.1625 0.147 Uiso 1 1 calc R U . . .
C14 C 0.6059(3) -0.0085(5) 0.1737(8) 0.087(4) Uani 1 1 d . . . . .
H14 H 0.6071 0.0375 0.1584 0.104 Uiso 1 1 calc R U . . .
C15 C 0.9141(3) -0.0179(4) 0.1056(5) 0.0406(18) Uani 1 1 d . . . . .
H15A H 0.9123 -0.0040 0.1597 0.049 Uiso 1 1 calc R U . . .
H15B H 0.9453 -0.0246 0.0927 0.049 Uiso 1 1 calc R U . . .
C16 C 0.8895(3) -0.0835(4) 0.0943(4) 0.0394(18) Uani 1 1 d . . . . .
C17 C 0.9092(3) -0.1443(4) 0.1089(4) 0.0411(18) Uani 1 1 d . . . . .
H17 H 0.9390 -0.1460 0.1240 0.049 Uiso 1 1 calc R U . . .
C18 C 0.8856(3) -0.2025(4) 0.1016(5) 0.053(2) Uani 1 1 d . . . . .
H18 H 0.8987 -0.2450 0.1123 0.063 Uiso 1 1 calc R U . . .
C19 C 0.8425(3) -0.1991(4) 0.0784(4) 0.044(2) Uani 1 1 d . . . . .
H19 H 0.8252 -0.2389 0.0739 0.053 Uiso 1 1 calc R U . . .
C20 C 0.8251(3) -0.1364(4) 0.0620(4) 0.0446(19) Uani 1 1 d . . . . .
C21 C 0.7741(3) -0.1239(4) -0.0412(4) 0.0386(18) Uani 1 1 d . . . . .
C22 C 0.6945(3) -0.1403(4) -0.0201(5) 0.0437(19) Uani 1 1 d . . . . .
C23 C 0.6514(3) -0.1448(4) -0.0593(5) 0.046(2) Uani 1 1 d . . . . .
C24 C 0.6473(3) -0.1639(4) -0.1346(5) 0.051(2) Uani 1 1 d . U . . .
H24 H 0.6723 -0.1768 -0.1631 0.061 Uiso 1 1 calc R U . . .
C25 C 0.6061(3) -0.1640(5) -0.1687(6) 0.067(3) Uani 1 1 d . U . . .
H25 H 0.6029 -0.1755 -0.2210 0.080 Uiso 1 1 calc R U . . .
C26 C 0.5702(4) -0.1472(6) -0.1257(7) 0.081(3) Uani 1 1 d . . . . .
H26 H 0.5421 -0.1474 -0.1488 0.098 Uiso 1 1 calc R U . . .
C27 C 0.5738(3) -0.1302(5) -0.0499(7) 0.075(3) Uani 1 1 d . . . . .
H27 H 0.5486 -0.1193 -0.0208 0.090 Uiso 1 1 calc R U . . .
C28 C 0.6146(3) -0.1291(5) -0.0171(5) 0.058(2) Uani 1 1 d . . . . .
H28 H 0.6175 -0.1175 0.0352 0.070 Uiso 1 1 calc R U . . .
C29 C 0.9079(2) 0.0301(4) -0.0229(4) 0.0367(17) Uani 1 1 d . . . . .
H29A H 0.9073 -0.0179 -0.0388 0.044 Uiso 1 1 calc R U . . .
H29B H 0.9381 0.0472 -0.0298 0.044 Uiso 1 1 calc R U . . .
C30 C 0.8770(2) 0.0704(3) -0.0722(4) 0.0326(16) Uani 1 1 d . . . . .
C31 C 0.8888(2) 0.0960(4) -0.1420(4) 0.0394(18) Uani 1 1 d . . . . .
H31 H 0.9173 0.0884 -0.1616 0.047 Uiso 1 1 calc R U . . .
C32 C 0.8588(2) 0.1324(4) -0.1831(4) 0.0391(18) Uani 1 1 d . . . . .
H32 H 0.8662 0.1499 -0.2319 0.047 Uiso 1 1 calc R U . . .
C33 C 0.8171(2) 0.1437(3) -0.1522(4) 0.0325(16) Uani 1 1 d . . . . .
H33 H 0.7958 0.1693 -0.1790 0.039 Uiso 1 1 calc R U . . .
C34 C 0.8083(2) 0.1165(3) -0.0822(4) 0.0302(15) Uani 1 1 d . . . . .
C35 C 0.7423(2) 0.0977(3) -0.0024(4) 0.0266(14) Uani 1 1 d . . . . .
C36 C 0.6829(2) 0.1844(3) -0.0106(4) 0.0301(15) Uani 1 1 d . . . . .
C37 C 0.6390(2) 0.1989(3) 0.0200(4) 0.0274(14) Uani 1 1 d . . . . .
C38 C 0.6098(2) 0.2341(3) -0.0271(4) 0.0371(17) Uani 1 1 d . . . . .
H38 H 0.6193 0.2503 -0.0754 0.045 Uiso 1 1 calc R U . . .
C39 C 0.5674(2) 0.2453(4) -0.0034(4) 0.0420(18) Uani 1 1 d . . . . .
H39 H 0.5476 0.2689 -0.0355 0.050 Uiso 1 1 calc R U . . .
C40 C 0.5537(2) 0.2222(4) 0.0673(5) 0.0438(19) Uani 1 1 d . . . . .
H40 H 0.5244 0.2294 0.0834 0.053 Uiso 1 1 calc R U . . .
C41 C 0.5828(2) 0.1887(4) 0.1142(5) 0.0441(19) Uani 1 1 d . . . . .
H41 H 0.5737 0.1734 0.1630 0.053 Uiso 1 1 calc R U . . .
C42 C 0.6251(2) 0.1773(4) 0.0903(4) 0.0388(18) Uani 1 1 d . . . . .
H42 H 0.6449 0.1542 0.1229 0.047 Uiso 1 1 calc R U . . .
N1 N 0.89574(19) 0.0352(3) 0.0574(3) 0.0335(13) Uani 1 1 d . . . . .
N2 N 0.83492(18) 0.0853(3) 0.1541(3) 0.0320(13) Uani 1 1 d . . . . .
N3 N 0.7660(2) 0.0639(3) 0.2090(3) 0.0359(14) Uani 1 1 d . . . . .
H3A H 0.7425 0.0857 0.1938 0.043 Uiso 1 1 calc R U . . .
N4 N 0.7207(2) -0.0287(3) 0.2215(4) 0.055(2) Uani 1 1 d . . . . .
H4A H 0.7181 -0.0710 0.2363 0.066 Uiso 1 1 calc R U . . .
N5 N 0.8475(2) -0.0788(3) 0.0725(3) 0.0368(14) Uani 1 1 d . . . . .
N6 N 0.7815(2) -0.1317(3) 0.0338(4) 0.0387(15) Uani 1 1 d . . . . .
H6 H 0.7593 -0.1339 0.0657 0.046 Uiso 1 1 calc R U . . .
N7 N 0.7312(2) -0.1298(3) -0.0650(4) 0.0443(16) Uani 1 1 d . . . . .
H7 H 0.7266 -0.1263 -0.1144 0.053 Uiso 1 1 calc R U . . .
N8 N 0.83690(18) 0.0800(3) -0.0421(3) 0.0312(13) Uani 1 1 d . . . . .
N9 N 0.76728(17) 0.1333(3) -0.0488(3) 0.0272(12) Uani 1 1 d . . . . .
H9 H 0.7571 0.1735 -0.0609 0.033 Uiso 1 1 calc R U . . .
N10 N 0.70332(18) 0.1276(3) 0.0192(3) 0.0306(13) Uani 1 1 d . . . . .
H10A H 0.6895 0.1078 0.0571 0.037 Uiso 1 1 calc R U . . .
S1 S 0.80338(8) -0.04685(14) 0.26131(19) 0.0781(9) Uani 1 1 d . . . . .
S2 S 0.81229(7) -0.10504(12) -0.10537(12) 0.0545(6) Uani 1 1 d . . . . .
S3 S 0.75067(6) 0.01839(8) 0.03044(11) 0.0331(4) Uani 1 1 d . . . . .
O1 O 0.68342(16) 0.0592(3) 0.1715(3) 0.0421(12) Uani 1 1 d . . . . .
O2 O 0.69703(19) -0.1439(3) 0.0503(3) 0.0541(15) Uani 1 1 d . . . . .
O3 O 0.70098(15) 0.2174(2) -0.0616(3) 0.0317(11) Uani 1 1 d . . . . .
Zn1 Zn 0.82552(3) 0.02160(4) 0.05935(5) 0.0305(3) Uani 1 1 d . . . . .
O4 O 0.9970(2) 0.2374(4) 0.2272(3) 0.0687(19) Uani 1 1 d . . . . .
O5 O 0.94023(16) 0.2636(3) 0.3116(3) 0.0594(17) Uani 1 1 d . . . . .
O6 O 0.9913(2) 0.3454(3) 0.2814(4) 0.077(2) Uani 1 1 d . . . . .
O7 O 1.01230(17) 0.2527(3) 0.3572(3) 0.0533(15) Uani 1 1 d . . . . .
Cl1 Cl 0.98540(6) 0.27477(11) 0.29459(11) 0.0455(5) Uani 1 1 d . . . . .
O8 O 0.77991(16) 0.2127(2) 0.0990(3) 0.0397(12) Uani 1 1 d . . . . .
O9 O 0.72573(17) 0.2038(3) 0.1935(3) 0.0473(14) Uani 1 1 d . . . . .
Cl2 Cl 0.7500 0.2500 0.14603(13) 0.0327(5) Uani 1 2 d S T P . .
C43 C 0.9300(4) 0.0758(8) 0.3872(8) 0.109(4) Uani 1 1 d . U . . .
H43 H 0.9285 0.1259 0.3802 0.130 Uiso 1 1 calc R U . . .
Cl3 Cl 0.94863(15) 0.0397(3) 0.3040(3) 0.1438(17) Uani 1 1 d . . . . .
Cl4 Cl 0.96075(14) 0.0590(2) 0.4653(2) 0.1245(14) Uani 1 1 d . . . . .
Cl5 Cl 0.87538(12) 0.04429(18) 0.4035(3) 0.1168(13) Uani 1 1 d . . . . .
O10 O 0.7459(3) 0.8087(5) 0.1877(6) 0.163(5) Uani 1 1 d D . . . .
O11 O 0.7500 0.7500 0.3036(4) 0.181(8) Uani 1 2 d DS T P . .
O12 O 0.8089(2) 0.7530(6) 0.2260(6) 0.077(4) Uani 0.5 1 d D . P . .
Cl6 Cl 0.76056(12) 0.7477(4) 0.2247(2) 0.0445(14) Uani 0.5 1 d D U P . .
C44 C 1.0349(3) 0.1323(5) 0.0608(7) 0.0667(11) Uani 0.788(9) 1 d D U P A 1
C45 C 1.0653(3) 0.1806(5) 0.0883(7) 0.0664(15) Uani 0.788(9) 1 d D U P A 1
H45A H 1.0933 0.1584 0.0986 0.100 Uiso 0.788(9) 1 calc R U P A 1
H45B H 1.0541 0.2008 0.1355 0.100 Uiso 0.788(9) 1 calc R U P A 1
H45C H 1.0695 0.2161 0.0500 0.100 Uiso 0.788(9) 1 calc R U P A 1
N11 N 1.0117(3) 0.0964(5) 0.0348(6) 0.0676(12) Uani 0.788(9) 1 d D U P A 1
C44A C 1.0190(15) 0.1014(12) 0.0763(12) 0.0668(10) Uani 0.212(9) 1 d D U P A 2
C45A C 1.0226(14) 0.0579(14) 0.1404(13) 0.0668(10) Uani 0.212(9) 1 d D U P A 2
H45D H 1.0178 0.0111 0.1243 0.100 Uiso 0.212(9) 1 calc R U P A 2
H45E H 1.0007 0.0704 0.1786 0.100 Uiso 0.212(9) 1 calc R U P A 2
H45F H 1.0519 0.0621 0.1626 0.100 Uiso 0.212(9) 1 calc R U P A 2
N11A N 1.0168(13) 0.1373(12) 0.0286(12) 0.0670(13) Uani 0.212(9) 1 d D U P 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
C1 N1 1.477(9) . ?
C1 C2 1.500(10) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 N2 1.341(9) . ?
C2 C3 1.376(10) . ?
C3 C4 1.371(11) . ?
C3 H3 0.9500 . ?
C4 C5 1.367(11) . ?
C4 H4 0.9500 . ?
C5 C6 1.373(10) . ?
C5 H5 0.9500 . ?
C6 N2 1.339(9) . ?
C6 N3 1.430(9) . ?
C7 N3 1.328(9) . ?
C7 N4 1.401(10) . ?
C7 S1 1.649(8) . ?
C8 O1 1.230(9) . ?
C8 N4 1.352(10) . ?
C8 C9 1.481(11) . ?
C9 C14 1.361(12) . ?
C9 C10 1.403(11) . ?
C10 C11 1.388(11) . ?
C10 H10 0.9500 . ?
C11 C12 1.363(14) . ?
C11 H11 0.9500 . ?
C12 C13 1.397(15) . ?
C12 H12 0.9500 . ?
C13 C14 1.398(14) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 N1 1.461(9) . ?
C15 C16 1.514(10) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 N5 1.344(9) . ?
C16 C17 1.372(10) . ?
C17 C18 1.367(11) . ?
C17 H17 0.9500 . ?
C18 C19 1.382(12) . ?
C18 H18 0.9500 . ?
C19 C20 1.381(11) . ?
C19 H19 0.9500 . ?
C20 N5 1.342(10) . ?
C20 N6 1.427(10) . ?
C21 N6 1.344(9) . ?
C21 N7 1.383(10) . ?
C21 S2 1.664(8) . ?
C22 O2 1.240(9) . ?
C22 N7 1.386(10) . ?
C22 C23 1.489(11) . ?
C23 C24 1.380(11) . ?
C23 C28 1.384(12) . ?
C24 C25 1.394(12) . ?
C24 H24 0.9500 . ?
C25 C26 1.373(15) . ?
C25 H25 0.9500 . ?
C26 C27 1.376(15) . ?
C26 H26 0.9500 . ?
C27 C28 1.372(13) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 N1 1.459(9) . ?
C29 C30 1.511(10) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 N8 1.348(9) . ?
C30 C31 1.373(10) . ?
C31 C32 1.371(10) . ?
C31 H31 0.9500 . ?
C32 C33 1.405(10) . ?
C32 H32 0.9500 . ?
C33 C34 1.368(9) . ?
C33 H33 0.9500 . ?
C34 N8 1.335(9) . ?
C34 N9 1.424(9) . ?
C35 N9 1.320(8) . ?
C35 N10 1.383(8) . ?
C35 S3 1.693(7) . ?
C36 O3 1.239(8) . ?
C36 N10 1.388(8) . ?
C36 C37 1.476(9) . ?
C37 C42 1.372(10) . ?
C37 C38 1.401(9) . ?
C38 C39 1.381(10) . ?
C38 H38 0.9500 . ?
C39 C40 1.387(11) . ?
C39 H39 0.9500 . ?
C40 C41 1.383(11) . ?
C40 H40 0.9500 . ?
C41 C42 1.378(10) . ?
C41 H41 0.9500 . ?
C42 H42 0.9500 . ?
N1 Zn1 2.165(6) . ?
N2 Zn1 2.106(6) . ?
N3 H3A 0.8800 . ?
N4 H4A 0.8800 . ?
N5 Zn1 2.111(6) . ?
N6 H6 0.8800 . ?
N7 H7 0.8800 . ?
N8 Zn1 2.150(6) . ?
N9 H9 0.8800 . ?
N10 H10A 0.8800 . ?
S3 Zn1 2.3461(19) . ?
O4 Cl1 1.438(6) . ?
O5 Cl1 1.430(5) . ?
O6 Cl1 1.428(7) . ?
O7 Cl1 1.440(5) . ?
O8 Cl2 1.437(5) . ?
O9 Cl2 1.443(5) . ?
Cl2 O8 1.437(5) 2_655 ?
Cl2 O9 1.443(5) 2_655 ?
C43 Cl4 1.694(13) . ?
C43 Cl3 1.722(13) . ?
C43 Cl5 1.805(15) . ?
C43 H43 1.0000 . ?
O10 Cl6 1.307(11) 2_665 ?
O10 Cl6 1.443(7) . ?
O11 Cl6 1.422(7) 2_665 ?
O11 Cl6 1.422(7) . ?
O12 Cl6 1.482(7) . ?
O12 Cl6 2.125(8) 2_665 ?
Cl6 Cl6 0.652(7) 2_665 ?
Cl6 O10 1.307(11) 2_665 ?
Cl6 O12 2.125(8) 2_665 ?
C44 N11 1.1011(9) . ?
C44 C45 1.4205(9) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C44A N11A 1.1004(10) . ?
C44A C45A 1.4203(10) . ?
C45A H45D 0.9800 . ?
C45A H45E 0.9800 . ?
C45A H45F 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 111.4(6) . . ?
N1 C1 H1A 109.4 . . ?
C2 C1 H1A 109.4 . . ?
N1 C1 H1B 109.4 . . ?
C2 C1 H1B 109.4 . . ?
H1A C1 H1B 108.0 . . ?
N2 C2 C3 122.2(7) . . ?
N2 C2 C1 116.5(6) . . ?
C3 C2 C1 121.2(7) . . ?
C4 C3 C2 119.1(7) . . ?
C4 C3 H3 120.4 . . ?
C2 C3 H3 120.4 . . ?
C5 C4 C3 119.5(7) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
C4 C5 C6 118.3(8) . . ?
C4 C5 H5 120.9 . . ?
C6 C5 H5 120.9 . . ?
N2 C6 C5 123.4(7) . . ?
N2 C6 N3 116.5(6) . . ?
C5 C6 N3 120.0(7) . . ?
N3 C7 N4 115.5(7) . . ?
N3 C7 S1 124.3(6) . . ?
N4 C7 S1 120.2(6) . . ?
O1 C8 N4 121.9(7) . . ?
O1 C8 C9 120.5(7) . . ?
N4 C8 C9 117.6(7) . . ?
C14 C9 C10 119.5(8) . . ?
C14 C9 C8 116.7(7) . . ?
C10 C9 C8 123.8(8) . . ?
C11 C10 C9 119.5(8) . . ?
C11 C10 H10 120.2 . . ?
C9 C10 H10 120.2 . . ?
C12 C11 C10 120.7(9) . . ?
C12 C11 H11 119.6 . . ?
C10 C11 H11 119.6 . . ?
C11 C12 C13 120.3(10) . . ?
C11 C12 H12 119.9 . . ?
C13 C12 H12 119.9 . . ?
C12 C13 C14 118.7(11) . . ?
C12 C13 H13 120.6 . . ?
C14 C13 H13 120.6 . . ?
C9 C14 C13 121.2(9) . . ?
C9 C14 H14 119.4 . . ?
C13 C14 H14 119.4 . . ?
N1 C15 C16 110.5(6) . . ?
N1 C15 H15A 109.5 . . ?
C16 C15 H15A 109.5 . . ?
N1 C15 H15B 109.5 . . ?
C16 C15 H15B 109.5 . . ?
H15A C15 H15B 108.1 . . ?
N5 C16 C17 122.3(7) . . ?
N5 C16 C15 117.0(6) . . ?
C17 C16 C15 120.6(7) . . ?
C18 C17 C16 119.3(7) . . ?
C18 C17 H17 120.4 . . ?
C16 C17 H17 120.4 . . ?
C17 C18 C19 119.5(7) . . ?
C17 C18 H18 120.2 . . ?
C19 C18 H18 120.2 . . ?
C20 C19 C18 118.2(8) . . ?
C20 C19 H19 120.9 . . ?
C18 C19 H19 120.9 . . ?
N5 C20 C19 122.6(8) . . ?
N5 C20 N6 118.0(7) . . ?
C19 C20 N6 119.4(7) . . ?
N6 C21 N7 116.4(7) . . ?
N6 C21 S2 124.7(6) . . ?
N7 C21 S2 118.8(6) . . ?
O2 C22 N7 121.6(8) . . ?
O2 C22 C23 120.7(8) . . ?
N7 C22 C23 117.6(7) . . ?
C24 C23 C28 119.8(8) . . ?
C24 C23 C22 122.7(8) . . ?
C28 C23 C22 117.5(8) . . ?
C23 C24 C25 119.6(9) . . ?
C23 C24 H24 120.2 . . ?
C25 C24 H24 120.2 . . ?
C26 C25 C24 119.1(10) . . ?
C26 C25 H25 120.4 . . ?
C24 C25 H25 120.4 . . ?
C25 C26 C27 121.8(10) . . ?
C25 C26 H26 119.1 . . ?
C27 C26 H26 119.1 . . ?
C28 C27 C26 118.7(10) . . ?
C28 C27 H27 120.6 . . ?
C26 C27 H27 120.6 . . ?
C27 C28 C23 120.9(9) . . ?
C27 C28 H28 119.6 . . ?
C23 C28 H28 119.6 . . ?
N1 C29 C30 110.8(6) . . ?
N1 C29 H29A 109.5 . . ?
C30 C29 H29A 109.5 . . ?
N1 C29 H29B 109.5 . . ?
C30 C29 H29B 109.5 . . ?
H29A C29 H29B 108.1 . . ?
N8 C30 C31 122.5(7) . . ?
N8 C30 C29 114.8(6) . . ?
C31 C30 C29 122.7(6) . . ?
C32 C31 C30 119.1(7) . . ?
C32 C31 H31 120.5 . . ?
C30 C31 H31 120.5 . . ?
C31 C32 C33 119.3(7) . . ?
C31 C32 H32 120.4 . . ?
C33 C32 H32 120.4 . . ?
C34 C33 C32 117.5(7) . . ?
C34 C33 H33 121.2 . . ?
C32 C33 H33 121.2 . . ?
N8 C34 C33 123.8(6) . . ?
N8 C34 N9 119.2(6) . . ?
C33 C34 N9 116.8(6) . . ?
N9 C35 N10 116.1(6) . . ?
N9 C35 S3 128.1(5) . . ?
N10 C35 S3 115.7(5) . . ?
O3 C36 N10 120.0(6) . . ?
O3 C36 C37 124.5(6) . . ?
N10 C36 C37 115.5(6) . . ?
C42 C37 C38 119.2(6) . . ?
C42 C37 C36 123.2(6) . . ?
C38 C37 C36 117.5(6) . . ?
C39 C38 C37 120.0(7) . . ?
C39 C38 H38 120.0 . . ?
C37 C38 H38 120.0 . . ?
C38 C39 C40 120.1(7) . . ?
C38 C39 H39 119.9 . . ?
C40 C39 H39 119.9 . . ?
C41 C40 C39 119.6(7) . . ?
C41 C40 H40 120.2 . . ?
C39 C40 H40 120.2 . . ?
C42 C41 C40 120.1(7) . . ?
C42 C41 H41 119.9 . . ?
C40 C41 H41 119.9 . . ?
C37 C42 C41 120.9(7) . . ?
C37 C42 H42 119.5 . . ?
C41 C42 H42 119.5 . . ?
C29 N1 C15 114.2(6) . . ?
C29 N1 C1 113.1(6) . . ?
C15 N1 C1 111.3(6) . . ?
C29 N1 Zn1 105.1(4) . . ?
C15 N1 Zn1 106.4(4) . . ?
C1 N1 Zn1 106.0(4) . . ?
C6 N2 C2 117.4(6) . . ?
C6 N2 Zn1 128.2(5) . . ?
C2 N2 Zn1 114.4(5) . . ?
C7 N3 C6 121.9(6) . . ?
C7 N3 H3A 119.1 . . ?
C6 N3 H3A 119.1 . . ?
C8 N4 C7 128.6(7) . . ?
C8 N4 H4A 115.7 . . ?
C7 N4 H4A 115.7 . . ?
C20 N5 C16 117.9(6) . . ?
C20 N5 Zn1 128.5(5) . . ?
C16 N5 Zn1 113.6(5) . . ?
C21 N6 C20 120.2(7) . . ?
C21 N6 H6 119.9 . . ?
C20 N6 H6 119.9 . . ?
C21 N7 C22 127.6(7) . . ?
C21 N7 H7 116.2 . . ?
C22 N7 H7 116.2 . . ?
C34 N8 C30 117.8(6) . . ?
C34 N8 Zn1 128.3(5) . . ?
C30 N8 Zn1 113.3(4) . . ?
C35 N9 C34 129.7(5) . . ?
C35 N9 H9 115.2 . . ?
C34 N9 H9 115.2 . . ?
C35 N10 C36 129.1(6) . . ?
C35 N10 H10A 115.5 . . ?
C36 N10 H10A 115.5 . . ?
C35 S3 Zn1 101.3(2) . . ?
N2 Zn1 N5 115.7(2) . . ?
N2 Zn1 N8 108.0(2) . . ?
N5 Zn1 N8 123.0(2) . . ?
N2 Zn1 N1 78.6(2) . . ?
N5 Zn1 N1 78.7(2) . . ?
N8 Zn1 N1 76.1(2) . . ?
N2 Zn1 S3 108.67(16) . . ?
N5 Zn1 S3 107.96(17) . . ?
N8 Zn1 S3 89.64(16) . . ?
N1 Zn1 S3 165.51(17) . . ?
O6 Cl1 O5 107.9(4) . . ?
O6 Cl1 O4 109.8(4) . . ?
O5 Cl1 O4 109.2(4) . . ?
O6 Cl1 O7 110.3(4) . . ?
O5 Cl1 O7 110.3(4) . . ?
O4 Cl1 O7 109.3(4) . . ?
O8 Cl2 O8 109.9(4) 2_655 . ?
O8 Cl2 O9 109.2(3) 2_655 . ?
O8 Cl2 O9 109.4(3) . . ?
O8 Cl2 O9 109.4(3) 2_655 2_655 ?
O8 Cl2 O9 109.2(3) . 2_655 ?
O9 Cl2 O9 109.6(5) . 2_655 ?
Cl4 C43 Cl3 114.7(7) . . ?
Cl4 C43 Cl5 108.6(8) . . ?
Cl3 C43 Cl5 107.3(8) . . ?
Cl4 C43 H43 108.7 . . ?
Cl3 C43 H43 108.7 . . ?
Cl5 C43 H43 108.7 . . ?
Cl6 O10 Cl6 26.9(3) 2_665 . ?
Cl6 O11 Cl6 26.5(3) 2_665 . ?
Cl6 O12 Cl6 3.7(5) . 2_665 ?
Cl6 Cl6 O10 88.3(12) 2_665 2_665 ?
Cl6 Cl6 O11 76.73(16) 2_665 . ?
O10 Cl6 O11 118.5(8) 2_665 . ?
Cl6 Cl6 O10 64.9(11) 2_665 . ?
O10 Cl6 O10 116.4(11) 2_665 . ?
O11 Cl6 O10 109.9(6) . . ?
Cl6 Cl6 O12 167.9(16) 2_665 . ?
O10 Cl6 O12 102.6(6) 2_665 . ?
O11 Cl6 O12 102.1(5) . . ?
O10 Cl6 O12 105.0(6) . . ?
Cl6 Cl6 O12 8.4(11) 2_665 2_665 ?
O10 Cl6 O12 81.3(5) 2_665 2_665 ?
O11 Cl6 O12 76.3(3) . 2_665 ?
O10 Cl6 O12 72.5(5) . 2_665 ?
O12 Cl6 O12 176.0(6) . 2_665 ?
N11 C44 C45 175.4(13) . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C44 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
N11A C44A C45A 177(3) . . ?
C44A C45A H45D 109.5 . . ?
C44A C45A H45E 109.5 . . ?
H45D C45A H45E 109.5 . . ?
C44A C45A H45F 109.5 . . ?
H45D C45A H45F 109.5 . . ?
H45E C45A H45F 109.5 . . ?

_refine_diff_density_max         1.649
_refine_diff_density_min         -1.089
_refine_diff_density_rms         0.126

_shelxl_version_number           2013-4

