# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_19ap21n

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'Co 2+, (Cl -1)2, (C14 H13 N3 S)'
_chemical_formula_sum            'C14 H13 Cl2 Co N3 S'
_chemical_melting_point          ?

_exptl_crystal_description       'big block'
_exptl_crystal_colour            'dark green'

_diffrn_ambient_temperature      293(2)
_chemical_formula_weight         385.16

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'
Cl Cl 0.1484 0.1585 '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   'P 21/n'
_symmetry_int_tables_number      14
_chemical_absolute_configuration ?

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                   8.9069(4)
_cell_length_b                   14.7753(6)
_cell_length_c                   12.3744(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.793(4)
_cell_angle_gamma                90.00
_cell_volume                     1588.07(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5674
_cell_measurement_theta_min      2.18
_cell_measurement_theta_max      26.37
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             780
_exptl_absorpt_coefficient_mu    1.543
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.4841
_exptl_absorpt_correction_T_max  0.7686
_exptl_absorpt_process_details   'CrysAlis CCD, Oxford 2001'

_exptl_special_details           
; 
 ? 
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Sapphire CCD diffractometer'
_diffrn_measurement_method       'omega - 2theta'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5674
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.18
_diffrn_reflns_theta_max         26.37
_reflns_number_total             3246
_reflns_number_gt                2636
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlis CCD'
_computing_cell_refinement       ?
_computing_data_reduction        'CrysAlis RED 171'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'WinGX v1.80.05'
_computing_publication_material  CIFTAB

_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)+(0.0706P)²+0.5575P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3246
_refine_ls_number_parameters     192
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0320
_refine_ls_wR_factor_ref         0.0963
_refine_ls_wR_factor_gt          0.0920
_refine_ls_goodness_of_fit_ref   0.873
_refine_ls_restrained_S_all      0.873
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.001

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 0.36560(3) 0.123128(19) 0.73073(2) 0.03096(12) Uani 1 1 d . . .
Cl2 Cl 0.22799(7) -0.00186(4) 0.72259(6) 0.04887(18) Uani 1 1 d . . .
Cl3 Cl 0.23481(7) 0.24814(4) 0.74393(5) 0.04694(17) Uani 1 1 d . . .
N1 N 0.5576(2) 0.11857(12) 0.85161(15) 0.0334(4) Uani 1 1 d . . .
C2 C 0.6015(3) 0.11677(15) 0.96054(19) 0.0384(5) Uani 1 1 d . . .
C21 C 0.4857(3) 0.12082(18) 1.0303(2) 0.0508(7) Uani 1 1 d . . .
H21A H 0.3848 0.1111 0.9847 0.076 Uiso 1 1 calc R . .
H21B H 0.4897 0.1792 1.0649 0.076 Uiso 1 1 calc R . .
H21C H 0.5078 0.0748 1.0863 0.076 Uiso 1 1 calc R . .
C3 C 0.7620(3) 0.11237(18) 0.9924(2) 0.0452(6) Uani 1 1 d . . .
H3 H 0.8204 0.1100 1.0647 0.054 Uiso 1 1 calc R . .
C4 C 0.8168(3) 0.11221(15) 0.8985(2) 0.0386(5) Uani 1 1 d . . .
C41 C 0.9773(3) 0.1101(2) 0.8820(3) 0.0610(8) Uani 1 1 d . . .
H41A H 1.0481 0.1067 0.9527 0.092 Uiso 1 1 calc R . .
H41C H 0.9970 0.1641 0.8443 0.092 Uiso 1 1 calc R . .
H41B H 0.9904 0.0582 0.8384 0.092 Uiso 1 1 calc R . .
N5 N 0.6901(2) 0.11628(12) 0.81221(15) 0.0331(4) Uani 1 1 d . . .
C6 C 0.6710(2) 0.11985(14) 0.69783(19) 0.0330(5) Uani 1 1 d . . .
S7 S 0.81525(7) 0.11826(5) 0.62786(6) 0.0527(2) Uani 1 1 d . . .
C8 C 0.6798(3) 0.12465(18) 0.5062(2) 0.0497(7) Uani 1 1 d . . .
H8 H 0.7028 0.1261 0.4365 0.060 Uiso 1 1 calc R . .
C9 C 0.5348(3) 0.12725(14) 0.52371(18) 0.0338(5) Uani 1 1 d . . .
N10 N 0.5305(2) 0.12470(11) 0.63531(15) 0.0298(4) Uani 1 1 d . . .
C91 C 0.3921(3) 0.13129(14) 0.43665(18) 0.0329(5) Uani 1 1 d . . .
C92 C 0.2501(3) 0.1461(2) 0.4603(2) 0.0568(7) Uani 1 1 d . . .
H92 H 0.2430 0.1532 0.5337 0.068 Uiso 1 1 calc R . .
C93 C 0.1182(3) 0.1508(2) 0.3774(2) 0.0584(7) Uani 1 1 d . . .
H93 H 0.0234 0.1604 0.3953 0.070 Uiso 1 1 calc R . .
C94 C 0.1266(3) 0.1413(2) 0.2702(2) 0.0509(7) Uani 1 1 d . . .
H94 H 0.0376 0.1443 0.2144 0.061 Uiso 1 1 calc R . .
C95 C 0.2658(3) 0.1273(2) 0.2439(2) 0.0649(10) Uani 1 1 d . . .
H95 H 0.2716 0.1213 0.1702 0.078 Uiso 1 1 calc R . .
C96 C 0.3993(3) 0.12189(19) 0.3273(2) 0.0532(7) Uani 1 1 d . . .
H96 H 0.4937 0.1119 0.3090 0.064 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 N1 2.0087(19) . ?
Co1 N10 2.0782(18) . ?
Co1 Cl2 2.2064(6) . ?
Co1 Cl3 2.2090(6) . ?
N1 C2 1.318(3) . ?
N1 N5 1.373(2) . ?
C2 C3 1.398(3) . ?
C2 C21 1.485(3) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C3 C4 1.357(4) . ?
C3 H3 0.9300 . ?
C4 N5 1.372(3) . ?
C4 C41 1.488(3) . ?
C41 H41A 0.9600 . ?
C41 H41C 0.9600 . ?
C41 H41B 0.9600 . ?
N5 C6 1.389(3) . ?
C6 N10 1.320(3) . ?
C6 S7 1.701(2) . ?
S7 C8 1.710(3) . ?
C8 C9 1.356(3) . ?
C8 H8 0.9300 . ?
C9 N10 1.391(3) . ?
C9 C91 1.474(3) . ?
C91 C96 1.376(3) . ?
C91 C92 1.377(3) . ?
C92 C93 1.380(4) . ?
C92 H92 0.9300 . ?
C93 C94 1.352(4) . ?
C93 H93 0.9300 . ?
C94 C95 1.365(4) . ?
C94 H94 0.9300 . ?
C95 C96 1.393(4) . ?
C95 H95 0.9300 . ?
C96 H96 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
N1 Co1 N10 80.28(7) . . ?
N1 Co1 Cl2 112.26(5) . . ?
N10 Co1 Cl2 116.02(5) . . ?
N1 Co1 Cl3 110.43(5) . . ?
N10 Co1 Cl3 118.90(5) . . ?
Cl2 Co1 Cl3 113.98(3) . . ?
C2 N1 N5 106.21(18) . . ?
C2 N1 Co1 140.63(16) . . ?
N5 N1 Co1 113.16(13) . . ?
N1 C2 C3 110.0(2) . . ?
N1 C2 C21 120.4(2) . . ?
C3 C2 C21 129.5(2) . . ?
C2 C21 H21A 109.5 . . ?
C2 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C2 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C4 C3 C2 107.3(2) . . ?
C4 C3 H3 126.3 . . ?
C2 C3 H3 126.3 . . ?
C3 C4 N5 106.0(2) . . ?
C3 C4 C41 131.0(2) . . ?
N5 C4 C41 123.0(2) . . ?
C4 C41 H41A 109.5 . . ?
C4 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
C4 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41C C41 H41B 109.5 . . ?
N1 N5 C4 110.38(18) . . ?
N1 N5 C6 116.11(17) . . ?
C4 N5 C6 133.50(19) . . ?
N10 C6 N5 119.06(19) . . ?
N10 C6 S7 115.32(17) . . ?
N5 C6 S7 125.62(16) . . ?
C6 S7 C8 88.98(11) . . ?
C9 C8 S7 111.84(19) . . ?
C9 C8 H8 124.1 . . ?
S7 C8 H8 124.1 . . ?
C8 C9 N10 113.2(2) . . ?
C8 C9 C91 125.6(2) . . ?
N10 C9 C91 121.16(19) . . ?
C6 N10 C9 110.62(18) . . ?
C6 N10 Co1 111.36(14) . . ?
C9 N10 Co1 138.00(14) . . ?
C96 C91 C92 118.0(2) . . ?
C96 C91 C9 119.6(2) . . ?
C92 C91 C9 122.3(2) . . ?
C93 C92 C91 121.4(2) . . ?
C93 C92 H92 119.3 . . ?
C91 C92 H92 119.3 . . ?
C94 C93 C92 120.0(2) . . ?
C94 C93 H93 120.0 . . ?
C92 C93 H93 120.0 . . ?
C93 C94 C95 120.0(2) . . ?
C93 C94 H94 120.0 . . ?
C95 C94 H94 120.0 . . ?
C94 C95 C96 120.2(2) . . ?
C94 C95 H95 119.9 . . ?
C96 C95 H95 119.9 . . ?
C91 C96 C95 120.3(2) . . ?
C91 C96 H96 119.8 . . ?
C95 C96 H96 119.8 . . ?

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
N10 Co1 N1 C2 178.5(2) . . . . ?
Cl2 Co1 N1 C2 -67.2(2) . . . . ?
Cl3 Co1 N1 C2 61.2(2) . . . . ?
N10 Co1 N1 N5 -1.69(13) . . . . ?
Cl2 Co1 N1 N5 112.56(12) . . . . ?
Cl3 Co1 N1 N5 -119.04(12) . . . . ?
N5 N1 C2 C3 -0.6(2) . . . . ?
Co1 N1 C2 C3 179.20(18) . . . . ?
N5 N1 C2 C21 178.4(2) . . . . ?
Co1 N1 C2 C21 -1.7(4) . . . . ?
N1 C2 C3 C4 0.5(3) . . . . ?
C21 C2 C3 C4 -178.5(2) . . . . ?
C2 C3 C4 N5 -0.1(3) . . . . ?
C2 C3 C4 C41 178.7(3) . . . . ?
C2 N1 N5 C4 0.5(2) . . . . ?
Co1 N1 N5 C4 -179.33(14) . . . . ?
C2 N1 N5 C6 -178.50(18) . . . . ?
Co1 N1 N5 C6 1.6(2) . . . . ?
C3 C4 N5 N1 -0.2(2) . . . . ?
C41 C4 N5 N1 -179.2(2) . . . . ?
C3 C4 N5 C6 178.6(2) . . . . ?
C41 C4 N5 C6 -0.4(4) . . . . ?
N1 N5 C6 N10 -0.3(3) . . . . ?
C4 N5 C6 N10 -179.0(2) . . . . ?
N1 N5 C6 S7 179.89(14) . . . . ?
C4 N5 C6 S7 1.1(3) . . . . ?
N10 C6 S7 C8 0.08(18) . . . . ?
N5 C6 S7 C8 179.9(2) . . . . ?
C6 S7 C8 C9 -0.2(2) . . . . ?
S7 C8 C9 N10 0.4(3) . . . . ?
S7 C8 C9 C91 -178.93(17) . . . . ?
N5 C6 N10 C9 -179.73(18) . . . . ?
S7 C6 N10 C9 0.1(2) . . . . ?
N5 C6 N10 Co1 -1.1(2) . . . . ?
S7 C6 N10 Co1 178.70(10) . . . . ?
C8 C9 N10 C6 -0.3(3) . . . . ?
C91 C9 N10 C6 179.03(18) . . . . ?
C8 C9 N10 Co1 -178.33(17) . . . . ?
C91 C9 N10 Co1 1.0(3) . . . . ?
N1 Co1 N10 C6 1.53(13) . . . . ?
Cl2 Co1 N10 C6 -108.59(13) . . . . ?
Cl3 Co1 N10 C6 109.59(13) . . . . ?
N1 Co1 N10 C9 179.6(2) . . . . ?
Cl2 Co1 N10 C9 69.4(2) . . . . ?
Cl3 Co1 N10 C9 -72.4(2) . . . . ?
C8 C9 C91 C96 7.7(3) . . . . ?
N10 C9 C91 C96 -171.6(2) . . . . ?
C8 C9 C91 C92 -171.0(3) . . . . ?
N10 C9 C91 C92 9.8(3) . . . . ?
C96 C91 C92 C93 0.5(4) . . . . ?
C9 C91 C92 C93 179.2(3) . . . . ?
C91 C92 C93 C94 -0.4(5) . . . . ?
C92 C93 C94 C95 -0.1(5) . . . . ?
C93 C94 C95 C96 0.6(5) . . . . ?
C92 C91 C96 C95 -0.1(4) . . . . ?
C9 C91 C96 C95 -178.8(2) . . . . ?
C94 C95 C96 C91 -0.5(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.327
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.070

_database_code_depnum_ccdc_archive 'CCDC 988739'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_mr35-sch_shape

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         
'(Ni 2+), 2(C14 H13 N3 S1), 2(H2 O), 2(Cl O4 1-)'
_chemical_formula_sum            'C28 H30 Cl2 N6 Ni O10 S2'
_chemical_melting_point          ?

_exptl_crystal_description       column
_exptl_crystal_colour            blue-green

_diffrn_ambient_temperature      293(2)
_chemical_formula_weight         804.31

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_int_tables_number      15
_chemical_absolute_configuration ?

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

_cell_length_a                   24.0372(10)
_cell_length_b                   9.6174(3)
_cell_length_c                   16.0976(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 113.255(5)
_cell_angle_gamma                90.00
_cell_volume                     3419.0(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5751
_cell_measurement_theta_min      2.31
_cell_measurement_theta_max      26.37
_exptl_crystal_size_max          0.98
_exptl_crystal_size_mid          0.58
_exptl_crystal_size_min          0.27
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1656
_exptl_absorpt_coefficient_mu    0.909
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.4694
_exptl_absorpt_correction_T_max  0.7913
_exptl_absorpt_process_details   'CrysAlis CCD, Oxford 2001'

_exptl_special_details           
; 
 ? 
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Sapphire CCD diffractometer'
_diffrn_measurement_method       'omega - 2theta'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5751
_diffrn_reflns_av_R_equivalents  0.0849
_diffrn_reflns_av_sigmaI/netI    0.0625
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.31
_diffrn_reflns_theta_max         26.37
_reflns_number_total             3494
_reflns_number_gt                2954
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlis CCD'
_computing_cell_refinement       ?
_computing_data_reduction        'CrysAlis RED 171'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'WinGX v1.80.05'
_computing_publication_material  CIFTAB

_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)+(0.0886P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0008(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3494
_refine_ls_number_parameters     231
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0458
_refine_ls_wR_factor_ref         0.1320
_refine_ls_wR_factor_gt          0.1279
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.068
_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 0.5000 0.24640(3) 0.2500 0.02854(17) Uani 1 2 d S . .
N1 N 0.59103(9) 0.23978(17) 0.26816(12) 0.0326(4) Uani 1 1 d . . .
C2 C 0.64115(10) 0.1651(2) 0.30771(15) 0.0392(5) Uani 1 1 d . . .
C21 C 0.64599(13) 0.0508(3) 0.37206(19) 0.0552(7) Uani 1 1 d . . .
H21A H 0.6478 0.0891 0.4281 0.083 Uiso 1 1 calc R . .
H21B H 0.6820 -0.0021 0.3826 0.083 Uiso 1 1 calc R . .
H21C H 0.6112 -0.0087 0.3470 0.083 Uiso 1 1 calc R . .
C3 C 0.68609(12) 0.2126(3) 0.27983(19) 0.0517(6) Uani 1 1 d . . .
H3 H 0.7253 0.1779 0.2986 0.062 Uiso 1 1 calc R . .
C4 C 0.66240(12) 0.3175(3) 0.2210(2) 0.0516(6) Uani 1 1 d . . .
C41 C 0.69033(16) 0.4029(4) 0.1704(3) 0.0912(13) Uani 1 1 d . . .
H41A H 0.7305 0.3696 0.1830 0.137 Uiso 1 1 calc R . .
H41B H 0.6922 0.4983 0.1888 0.137 Uiso 1 1 calc R . .
H41C H 0.6663 0.3958 0.1067 0.137 Uiso 1 1 calc R . .
N5 N 0.60442(9) 0.3334(2) 0.21413(13) 0.0390(4) Uani 1 1 d . . .
C6 C 0.55936(11) 0.4272(2) 0.16651(15) 0.0378(5) Uani 1 1 d . . .
S7 S 0.57205(3) 0.57699(7) 0.11931(5) 0.0561(2) Uani 1 1 d . . .
C8 C 0.49834(13) 0.6227(3) 0.09324(19) 0.0531(7) Uani 1 1 d . . .
H8 H 0.4807 0.7046 0.0639 0.064 Uiso 1 1 calc R . .
C9 C 0.46873(11) 0.5245(2) 0.12081(16) 0.0406(5) Uani 1 1 d . . .
N10 N 0.50422(9) 0.41054(19) 0.16276(12) 0.0349(4) Uani 1 1 d . . .
C92 C 0.36346(13) 0.4325(3) 0.06424(18) 0.0489(6) Uani 1 1 d . . .
H92 H 0.3758 0.3543 0.0421 0.059 Uiso 1 1 calc R . .
C91 C 0.40498(12) 0.5351(2) 0.10931(17) 0.0430(5) Uani 1 1 d . . .
C93 C 0.30347(14) 0.4473(3) 0.0525(2) 0.0659(9) Uani 1 1 d . . .
H93 H 0.2756 0.3785 0.0224 0.079 Uiso 1 1 calc R . .
C94 C 0.28485(16) 0.5628(4) 0.0849(3) 0.0825(12) Uani 1 1 d . . .
H94 H 0.2445 0.5721 0.0767 0.099 Uiso 1 1 calc R . .
C95 C 0.32587(19) 0.6637(4) 0.1292(3) 0.0948(14) Uani 1 1 d . . .
H95 H 0.3130 0.7418 0.1508 0.114 Uiso 1 1 calc R . .
C96 C 0.38578(16) 0.6521(3) 0.1424(3) 0.0704(9) Uani 1 1 d . . .
H96 H 0.4133 0.7212 0.1730 0.084 Uiso 1 1 calc R . .
O4 O 0.48795(9) 0.0900(2) 0.15618(12) 0.0452(4) Uani 1 1 d . . .
H4A H 0.4706(18) 0.104(3) 0.107(2) 0.068 Uiso 1 1 d . . .
H4B H 0.5148(19) 0.049(3) 0.158(2) 0.068 Uiso 1 1 d . . .
Cl2 Cl 0.60877(3) 0.93590(7) 0.09411(4) 0.0519(2) Uani 1 1 d . . .
O20 O 0.5999(2) 1.0718(2) 0.0595(2) 0.1207(15) Uani 1 1 d . . .
O21 O 0.58781(14) 0.9232(2) 0.16527(16) 0.0786(7) Uani 1 1 d . . .
O22 O 0.66949(14) 0.8964(5) 0.1260(3) 0.1393(14) Uani 1 1 d . . .
O23 O 0.57483(12) 0.8412(2) 0.02388(13) 0.0699(6) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O4 2.0692(17) . ?
Ni1 O4 2.0692(17) 2_655 ?
Ni1 N1 2.091(2) 2_655 ?
Ni1 N1 2.091(2) . ?
Ni1 N10 2.1417(18) 2_655 ?
Ni1 N10 2.1417(18) . ?
N1 C2 1.329(3) . ?
N1 N5 1.375(3) . ?
C2 C3 1.400(4) . ?
C2 C21 1.484(4) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C3 C4 1.347(4) . ?
C3 H3 0.9300 . ?
C4 N5 1.363(3) . ?
C4 C41 1.490(4) . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
N5 C6 1.385(3) . ?
C6 N10 1.313(3) . ?
C6 S7 1.712(2) . ?
S7 C8 1.709(3) . ?
C8 C9 1.359(3) . ?
C8 H8 0.9300 . ?
C9 N10 1.389(3) . ?
C9 C91 1.473(3) . ?
C92 C93 1.386(4) . ?
C92 C91 1.387(4) . ?
C92 H92 0.9300 . ?
C91 C96 1.398(4) . ?
C93 C94 1.374(5) . ?
C93 H93 0.9300 . ?
C94 C95 1.367(5) . ?
C94 H94 0.9300 . ?
C95 C96 1.375(5) . ?
C95 H95 0.9300 . ?
C96 H96 0.9300 . ?
O4 H4A 0.75(3) . ?
O4 H4B 0.75(4) . ?
Cl2 O22 1.395(3) . ?
Cl2 O20 1.404(2) . ?
Cl2 O21 1.427(2) . ?
Cl2 O23 1.430(2) . ?

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
O4 Ni1 O4 86.75(11) . 2_655 ?
O4 Ni1 N1 92.21(7) . 2_655 ?
O4 Ni1 N1 85.25(7) 2_655 2_655 ?
O4 Ni1 N1 85.25(7) . . ?
O4 Ni1 N1 92.21(7) 2_655 . ?
N1 Ni1 N1 176.51(9) 2_655 . ?
O4 Ni1 N10 170.11(7) . 2_655 ?
O4 Ni1 N10 94.96(8) 2_655 2_655 ?
N1 Ni1 N10 78.25(7) 2_655 2_655 ?
N1 Ni1 N10 104.39(7) . 2_655 ?
O4 Ni1 N10 94.96(8) . . ?
O4 Ni1 N10 170.11(7) 2_655 . ?
N1 Ni1 N10 104.39(7) 2_655 . ?
N1 Ni1 N10 78.25(7) . . ?
N10 Ni1 N10 85.03(10) 2_655 . ?
C2 N1 N5 105.20(19) . . ?
C2 N1 Ni1 141.63(16) . . ?
N5 N1 Ni1 112.64(14) . . ?
N1 C2 C3 109.8(2) . . ?
N1 C2 C21 122.8(2) . . ?
C3 C2 C21 127.4(2) . . ?
C2 C21 H21A 109.5 . . ?
C2 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C2 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C4 C3 C2 107.7(2) . . ?
C4 C3 H3 126.1 . . ?
C2 C3 H3 126.1 . . ?
C3 C4 N5 106.0(2) . . ?
C3 C4 C41 129.9(3) . . ?
N5 C4 C41 124.1(3) . . ?
C4 C41 H41A 109.5 . . ?
C4 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C4 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C4 N5 N1 111.3(2) . . ?
C4 N5 C6 132.0(2) . . ?
N1 N5 C6 116.68(18) . . ?
N10 C6 N5 120.07(19) . . ?
N10 C6 S7 115.83(18) . . ?
N5 C6 S7 123.80(17) . . ?
C8 S7 C6 88.66(12) . . ?
C9 C8 S7 111.53(19) . . ?
C9 C8 H8 124.2 . . ?
S7 C8 H8 124.2 . . ?
C8 C9 N10 114.0(2) . . ?
C8 C9 C91 124.3(2) . . ?
N10 C9 C91 121.6(2) . . ?
C6 N10 C9 109.96(19) . . ?
C6 N10 Ni1 111.59(15) . . ?
C9 N10 Ni1 136.16(15) . . ?
C93 C92 C91 119.5(3) . . ?
C93 C92 H92 120.2 . . ?
C91 C92 H92 120.2 . . ?
C92 C91 C96 119.6(3) . . ?
C92 C91 C9 120.9(2) . . ?
C96 C91 C9 119.4(3) . . ?
C94 C93 C92 120.6(3) . . ?
C94 C93 H93 119.7 . . ?
C92 C93 H93 119.7 . . ?
C95 C94 C93 119.7(3) . . ?
C95 C94 H94 120.1 . . ?
C93 C94 H94 120.1 . . ?
C94 C95 C96 121.2(3) . . ?
C94 C95 H95 119.4 . . ?
C96 C95 H95 119.4 . . ?
C95 C96 C91 119.3(3) . . ?
C95 C96 H96 120.3 . . ?
C91 C96 H96 120.3 . . ?
Ni1 O4 H4A 120(3) . . ?
Ni1 O4 H4B 119(3) . . ?
H4A O4 H4B 104(4) . . ?
O22 Cl2 O20 111.8(3) . . ?
O22 Cl2 O21 109.3(2) . . ?
O20 Cl2 O21 110.64(18) . . ?
O22 Cl2 O23 107.8(2) . . ?
O20 Cl2 O23 109.22(16) . . ?
O21 Cl2 O23 107.93(16) . . ?

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
O4 Ni1 N1 C2 -77.0(2) . . . . ?
O4 Ni1 N1 C2 9.5(2) 2_655 . . . ?
N1 Ni1 N1 C2 -33.7(2) 2_655 . . . ?
N10 Ni1 N1 C2 105.2(2) 2_655 . . . ?
N10 Ni1 N1 C2 -173.1(2) . . . . ?
O4 Ni1 N1 N5 92.88(14) . . . . ?
O4 Ni1 N1 N5 179.44(14) 2_655 . . . ?
N1 Ni1 N1 N5 136.22(13) 2_655 . . . ?
N10 Ni1 N1 N5 -84.87(14) 2_655 . . . ?
N10 Ni1 N1 N5 -3.19(13) . . . . ?
N5 N1 C2 C3 0.8(3) . . . . ?
Ni1 N1 C2 C3 171.18(19) . . . . ?
N5 N1 C2 C21 -179.8(2) . . . . ?
Ni1 N1 C2 C21 -9.4(4) . . . . ?
N1 C2 C3 C4 -0.8(3) . . . . ?
C21 C2 C3 C4 179.8(3) . . . . ?
C2 C3 C4 N5 0.4(3) . . . . ?
C2 C3 C4 C41 -179.1(3) . . . . ?
C3 C4 N5 N1 0.1(3) . . . . ?
C41 C4 N5 N1 179.7(3) . . . . ?
C3 C4 N5 C6 177.5(2) . . . . ?
C41 C4 N5 C6 -3.0(5) . . . . ?
C2 N1 N5 C4 -0.6(3) . . . . ?
Ni1 N1 N5 C4 -174.12(17) . . . . ?
C2 N1 N5 C6 -178.41(19) . . . . ?
Ni1 N1 N5 C6 8.1(2) . . . . ?
C4 N5 C6 N10 172.0(3) . . . . ?
N1 N5 C6 N10 -10.7(3) . . . . ?
C4 N5 C6 S7 -14.5(4) . . . . ?
N1 N5 C6 S7 162.77(16) . . . . ?
N10 C6 S7 C8 0.6(2) . . . . ?
N5 C6 S7 C8 -173.1(2) . . . . ?
C6 S7 C8 C9 -0.1(2) . . . . ?
S7 C8 C9 N10 -0.4(3) . . . . ?
S7 C8 C9 C91 179.0(2) . . . . ?
N5 C6 N10 C9 173.10(19) . . . . ?
S7 C6 N10 C9 -0.9(3) . . . . ?
N5 C6 N10 Ni1 7.4(3) . . . . ?
S7 C6 N10 Ni1 -166.60(11) . . . . ?
C8 C9 N10 C6 0.8(3) . . . . ?
C91 C9 N10 C6 -178.6(2) . . . . ?
C8 C9 N10 Ni1 161.4(2) . . . . ?
C91 C9 N10 Ni1 -17.9(4) . . . . ?
O4 Ni1 N10 C6 -86.16(17) . . . . ?
O4 Ni1 N10 C6 13.4(5) 2_655 . . . ?
N1 Ni1 N10 C6 -179.74(15) 2_655 . . . ?
N1 Ni1 N10 C6 -2.08(15) . . . . ?
N10 Ni1 N10 C6 103.76(17) 2_655 . . . ?
O4 Ni1 N10 C9 113.4(2) . . . . ?
O4 Ni1 N10 C9 -147.0(4) 2_655 . . . ?
N1 Ni1 N10 C9 19.8(2) 2_655 . . . ?
N1 Ni1 N10 C9 -162.5(2) . . . . ?
N10 Ni1 N10 C9 -56.7(2) 2_655 . . . ?
C93 C92 C91 C96 0.1(4) . . . . ?
C93 C92 C91 C9 -178.3(2) . . . . ?
C8 C9 C91 C92 123.9(3) . . . . ?
N10 C9 C91 C92 -56.8(3) . . . . ?
C8 C9 C91 C96 -54.5(4) . . . . ?
N10 C9 C91 C96 124.8(3) . . . . ?
C91 C92 C93 C94 0.2(4) . . . . ?
C92 C93 C94 C95 -0.1(5) . . . . ?
C93 C94 C95 C96 -0.2(6) . . . . ?
C94 C95 C96 C91 0.4(6) . . . . ?
C92 C91 C96 C95 -0.4(5) . . . . ?
C9 C91 C96 C95 178.1(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.706
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.085

_database_code_depnum_ccdc_archive 'CCDC 988743'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_mr43-sch_shape

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         
'(Cu 2+)2, (N O3 -1)2, 4(C14 H13 N3 S ), (Cu 2+), (N O3 1-)4'
_chemical_formula_sum            'C56 H52 Cu3 N18 O18 S4'
_chemical_melting_point          ?

_exptl_crystal_description       'triangular block'
_exptl_crystal_colour            'dark green'

_diffrn_ambient_temperature      293(2)
_chemical_formula_weight         1584.02

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'
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'
Cu Cu 0.3201 1.2651 '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'
_symmetry_int_tables_number      60
_chemical_absolute_configuration ?

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

_cell_length_a                   19.8159(6)
_cell_length_b                   13.1908(6)
_cell_length_c                   25.0863(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6557.2(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    16524
_cell_measurement_theta_min      2.02
_cell_measurement_theta_max      26.37
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3236
_exptl_absorpt_coefficient_mu    1.176
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.7496
_exptl_absorpt_correction_T_max  0.8433
_exptl_absorpt_process_details   'CrysAlis CCD, Oxford 2001'

_exptl_special_details           
; 
 ? 
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Sapphire CCD diffractometer'
_diffrn_measurement_method       'omega - 2theta'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16524
_diffrn_reflns_av_R_equivalents  0.0534
_diffrn_reflns_av_sigmaI/netI    0.0812
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         2.02
_diffrn_reflns_theta_max         26.37
_reflns_number_total             6694
_reflns_number_gt                3896
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlis CCD'
_computing_cell_refinement       ?
_computing_data_reduction        'CrysAlis RED 171'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'WinGX v1.80.05'
_computing_publication_material  CIFTAB

_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)+(0.0654P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6694
_refine_ls_number_parameters     450
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1010
_refine_ls_R_factor_gt           0.0459
_refine_ls_wR_factor_ref         0.1230
_refine_ls_wR_factor_gt          0.1021
_refine_ls_goodness_of_fit_ref   0.943
_refine_ls_restrained_S_all      0.943
_refine_ls_shift/su_max          0.012
_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
Cu1 Cu 0.18416(2) 0.58216(4) 0.051881(16) 0.02784(13) Uani 1 1 d . . .
N1 N 0.12542(14) 0.5648(2) 0.11525(11) 0.0286(7) Uani 1 1 d . . .
C2 C 0.12176(19) 0.6032(3) 0.16412(14) 0.0336(9) Uani 1 1 d . . .
C21 C 0.1696(2) 0.6822(4) 0.18213(15) 0.0467(11) Uani 1 1 d . . .
H21A H 0.1957 0.7055 0.1523 0.070 Uiso 1 1 calc R . .
H21B H 0.1991 0.6543 0.2087 0.070 Uiso 1 1 calc R . .
H21C H 0.1449 0.7380 0.1971 0.070 Uiso 1 1 calc R . .
C3 C 0.0689(2) 0.5559(3) 0.19153(15) 0.0408(10) Uani 1 1 d . . .
H3 H 0.0560 0.5692 0.2265 0.049 Uiso 1 1 calc R . .
C4 C 0.03954(19) 0.4870(3) 0.15835(15) 0.0380(10) Uani 1 1 d . . .
C41 C -0.0167(2) 0.4148(4) 0.16750(17) 0.0546(12) Uani 1 1 d . . .
H41A H -0.0311 0.4189 0.2040 0.082 Uiso 1 1 calc R . .
H41B H -0.0017 0.3471 0.1600 0.082 Uiso 1 1 calc R . .
H41C H -0.0538 0.4315 0.1445 0.082 Uiso 1 1 calc R . .
N5 N 0.07441(14) 0.4946(2) 0.11117(11) 0.0296(7) Uani 1 1 d . . .
C6 C 0.06957(18) 0.4411(3) 0.06355(14) 0.0317(9) Uani 1 1 d . . .
S7 S 0.00065(5) 0.37131(9) 0.04444(4) 0.0464(3) Uani 1 1 d . . .
C8 C 0.0402(2) 0.3479(3) -0.01495(15) 0.0428(10) Uani 1 1 d . . .
H8 H 0.0218 0.3091 -0.0422 0.051 Uiso 1 1 calc R . .
C9 C 0.10126(19) 0.3929(3) -0.01734(14) 0.0335(9) Uani 1 1 d . . .
C9A C 0.1497(2) 0.3887(3) -0.06220(14) 0.0369(9) Uani 1 1 d . . .
C9B C 0.2189(2) 0.3923(3) -0.05328(16) 0.0415(10) Uani 1 1 d . . .
H9B H 0.2355 0.3966 -0.0187 0.050 Uiso 1 1 calc R . .
C9C C 0.2632(2) 0.3894(3) -0.0960(2) 0.0560(13) Uani 1 1 d . . .
H9C H 0.3095 0.3928 -0.0899 0.067 Uiso 1 1 calc R . .
C9D C 0.2396(3) 0.3817(4) -0.1469(2) 0.0698(16) Uani 1 1 d . . .
H9D H 0.2695 0.3806 -0.1754 0.084 Uiso 1 1 calc R . .
C9E C 0.1714(3) 0.3755(4) -0.15590(18) 0.0673(15) Uani 1 1 d . . .
H9E H 0.1555 0.3689 -0.1906 0.081 Uiso 1 1 calc R . .
C9F C 0.1261(2) 0.3790(3) -0.11427(16) 0.0521(12) Uani 1 1 d . . .
H9F H 0.0800 0.3749 -0.1209 0.062 Uiso 1 1 calc R . .
N10 N 0.11804(14) 0.4487(2) 0.02802(11) 0.0284(7) Uani 1 1 d . . .
N11 N 0.24857(15) 0.6095(2) -0.00685(11) 0.0339(8) Uani 1 1 d . . .
C12 C 0.2503(2) 0.6329(3) -0.05865(15) 0.0393(10) Uani 1 1 d . . .
C22 C 0.1875(2) 0.6491(4) -0.08957(15) 0.0486(11) Uani 1 1 d . . .
H22A H 0.1690 0.5848 -0.0999 0.073 Uiso 1 1 calc R . .
H22B H 0.1974 0.6884 -0.1208 0.073 Uiso 1 1 calc R . .
H22C H 0.1553 0.6848 -0.0680 0.073 Uiso 1 1 calc R . .
C13 C 0.3174(2) 0.6307(3) -0.07642(17) 0.0490(11) Uani 1 1 d . . .
H13 H 0.3319 0.6448 -0.1109 0.059 Uiso 1 1 calc R . .
C14 C 0.3577(2) 0.6044(3) -0.03454(18) 0.0485(12) Uani 1 1 d . . .
C42 C 0.4316(2) 0.5827(4) -0.0312(2) 0.0691(15) Uani 1 1 d . . .
H42A H 0.4515 0.6241 -0.0040 0.104 Uiso 1 1 calc R . .
H42B H 0.4524 0.5976 -0.0649 0.104 Uiso 1 1 calc R . .
H42C H 0.4383 0.5125 -0.0227 0.104 Uiso 1 1 calc R . .
N15 N 0.31450(15) 0.5930(2) 0.00803(12) 0.0376(8) Uani 1 1 d . . .
C16 C 0.32337(18) 0.5545(3) 0.05944(16) 0.0368(10) Uani 1 1 d . . .
S17 S 0.39806(5) 0.54890(11) 0.09283(5) 0.0594(4) Uani 1 1 d . . .
C18 C 0.3557(2) 0.4958(4) 0.14500(18) 0.0599(13) Uani 1 1 d . . .
H18 H 0.3761 0.4765 0.1768 0.072 Uiso 1 1 calc R . .
C19 C 0.2889(2) 0.4849(3) 0.13476(15) 0.0382(10) Uani 1 1 d . . .
N20 N 0.26986(15) 0.5231(2) 0.08502(11) 0.0314(7) Uani 1 1 d . . .
C9G C 0.2418(2) 0.4276(4) 0.16890(15) 0.0463(11) Uani 1 1 d . . .
C9H C 0.1970(2) 0.3590(3) 0.14725(17) 0.0466(11) Uani 1 1 d . . .
H9H H 0.1936 0.3527 0.1104 0.056 Uiso 1 1 calc R . .
C9I C 0.1568(3) 0.2987(4) 0.1803(2) 0.0697(15) Uani 1 1 d . . .
H9I H 0.1261 0.2533 0.1655 0.084 Uiso 1 1 calc R . .
C9J C 0.1626(4) 0.3067(6) 0.2341(3) 0.100(2) Uani 1 1 d . . .
H9J H 0.1362 0.2665 0.2563 0.119 Uiso 1 1 calc R . .
C9K C 0.2070(4) 0.3736(7) 0.2553(2) 0.107(3) Uani 1 1 d . . .
H9K H 0.2109 0.3780 0.2922 0.129 Uiso 1 1 calc R . .
C9L C 0.2466(3) 0.4351(4) 0.22410(18) 0.0744(17) Uani 1 1 d . . .
H9L H 0.2763 0.4811 0.2396 0.089 Uiso 1 1 calc R . .
N31 N 0.1362(2) 0.7729(3) 0.03024(13) 0.0459(9) Uani 1 1 d . . .
O3 O 0.11764(12) 0.6801(2) 0.02242(9) 0.0358(6) Uani 1 1 d . . .
O8 O 0.1033(2) 0.8399(3) 0.00971(15) 0.0871(13) Uani 1 1 d . . .
O9 O 0.18678(18) 0.7877(3) 0.05772(12) 0.0621(9) Uani 1 1 d . . .
Cu2 Cu 0.0000 0.95522(7) 0.2500 0.0594(3) Uani 1 2 d S . .
N32 N -0.0032(2) 0.8191(4) 0.16686(18) 0.0678(12) Uani 1 1 d . . .
O31 O 0.03824(19) 0.8520(3) 0.20161(14) 0.0794(11) Uani 1 1 d . . .
O32 O 0.0194(2) 0.7715(3) 0.12884(16) 0.0981(14) Uani 1 1 d . . .
O33 O -0.0611(2) 0.8407(4) 0.1728(2) 0.1258(18) Uani 1 1 d . . .
N33 N 0.0578(3) 1.0945(4) 0.3125(2) 0.0812(14) Uani 1 1 d . . .
O34 O -0.00250(18) 1.0597(3) 0.30689(14) 0.0811(11) Uani 1 1 d . . .
O35 O 0.1019(2) 1.0582(3) 0.28409(18) 0.0951(13) Uani 1 1 d . . .
O36 O 0.0680(3) 1.1596(4) 0.3453(2) 0.1275(19) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N11 1.982(3) . ?
Cu1 N1 1.984(3) . ?
Cu1 O3 1.988(3) . ?
Cu1 N20 2.045(3) . ?
Cu1 N10 2.275(3) . ?
N1 C2 1.329(4) . ?
N1 N5 1.375(4) . ?
C2 C3 1.400(5) . ?
C2 C21 1.478(5) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C3 C4 1.363(5) . ?
C3 H3 0.9300 . ?
C4 N5 1.374(4) . ?
C4 C41 1.484(6) . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
N5 C6 1.391(4) . ?
C6 N10 1.314(4) . ?
C6 S7 1.715(4) . ?
S7 C8 1.711(4) . ?
C8 C9 1.349(5) . ?
C8 H8 0.9300 . ?
C9 N10 1.396(4) . ?
C9 C9A 1.480(5) . ?
C9A C9F 1.393(5) . ?
C9A C9B 1.391(5) . ?
C9B C9C 1.386(6) . ?
C9B H9B 0.9300 . ?
C9C C9D 1.363(7) . ?
C9C H9C 0.9300 . ?
C9D C9E 1.371(7) . ?
C9D H9D 0.9300 . ?
C9E C9F 1.378(6) . ?
C9E H9E 0.9300 . ?
C9F H9F 0.9300 . ?
N11 C12 1.336(4) . ?
N11 N15 1.376(4) . ?
C12 C13 1.401(6) . ?
C12 C22 1.483(6) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C13 C14 1.365(6) . ?
C13 H13 0.9300 . ?
C14 N15 1.376(5) . ?
C14 C42 1.495(6) . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
N15 C16 1.397(5) . ?
C16 N20 1.307(5) . ?
C16 S17 1.702(4) . ?
S17 C18 1.705(5) . ?
C18 C19 1.357(6) . ?
C18 H18 0.9300 . ?
C19 N20 1.397(4) . ?
C19 C9G 1.475(6) . ?
C9G C9H 1.379(6) . ?
C9G C9L 1.392(6) . ?
C9H C9I 1.398(6) . ?
C9H H9H 0.9300 . ?
C9I C9J 1.361(8) . ?
C9I H9I 0.9300 . ?
C9J C9K 1.355(10) . ?
C9J H9J 0.9300 . ?
C9K C9L 1.373(9) . ?
C9K H9K 0.9300 . ?
C9L H9L 0.9300 . ?
N31 O8 1.214(4) . ?
N31 O9 1.231(4) . ?
N31 O3 1.293(4) . ?
Cu2 O31 1.975(4) . ?
Cu2 O31 1.975(4) 3 ?
Cu2 O34 1.984(4) . ?
Cu2 O34 1.984(4) 3 ?
N32 O33 1.191(5) . ?
N32 O32 1.226(5) . ?
N32 O31 1.274(5) . ?
N33 O36 1.205(6) . ?
N33 O35 1.226(6) . ?
N33 O34 1.288(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N11 Cu1 N1 173.98(12) . . ?
N11 Cu1 O3 91.86(12) . . ?
N1 Cu1 O3 89.08(11) . . ?
N11 Cu1 N20 80.61(12) . . ?
N1 Cu1 N20 96.74(12) . . ?
O3 Cu1 N20 161.67(12) . . ?
N11 Cu1 N10 108.42(12) . . ?
N1 Cu1 N10 77.50(11) . . ?
O3 Cu1 N10 91.34(11) . . ?
N20 Cu1 N10 106.88(11) . . ?
C2 N1 N5 106.6(3) . . ?
C2 N1 Cu1 136.7(3) . . ?
N5 N1 Cu1 116.7(2) . . ?
N1 C2 C3 108.9(3) . . ?
N1 C2 C21 121.1(3) . . ?
C3 C2 C21 130.1(3) . . ?
C2 C21 H21A 109.5 . . ?
C2 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C2 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C4 C3 C2 108.5(3) . . ?
C4 C3 H3 125.8 . . ?
C2 C3 H3 125.8 . . ?
C3 C4 N5 105.2(3) . . ?
C3 C4 C41 130.9(4) . . ?
N5 C4 C41 123.9(4) . . ?
C4 C41 H41A 109.5 . . ?
C4 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C4 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
N1 N5 C4 110.8(3) . . ?
N1 N5 C6 117.2(3) . . ?
C4 N5 C6 131.9(3) . . ?
N10 C6 N5 119.5(3) . . ?
N10 C6 S7 115.7(3) . . ?
N5 C6 S7 124.6(3) . . ?
C8 S7 C6 88.61(19) . . ?
C9 C8 S7 111.7(3) . . ?
C9 C8 H8 124.1 . . ?
S7 C8 H8 124.1 . . ?
C8 C9 N10 114.2(3) . . ?
C8 C9 C9A 126.8(4) . . ?
N10 C9 C9A 119.0(3) . . ?
C9F C9A C9B 119.0(4) . . ?
C9F C9A C9 119.9(4) . . ?
C9B C9A C9 121.1(3) . . ?
C9C C9B C9A 119.9(4) . . ?
C9C C9B H9B 120.0 . . ?
C9A C9B H9B 120.0 . . ?
C9D C9C C9B 120.6(5) . . ?
C9D C9C H9C 119.7 . . ?
C9B C9C H9C 119.7 . . ?
C9C C9D C9E 119.8(5) . . ?
C9C C9D H9D 120.1 . . ?
C9E C9D H9D 120.1 . . ?
C9D C9E C9F 121.0(5) . . ?
C9D C9E H9E 119.5 . . ?
C9F C9E H9E 119.5 . . ?
C9E C9F C9A 119.7(5) . . ?
C9E C9F H9F 120.2 . . ?
C9A C9F H9F 120.2 . . ?
C6 N10 C9 109.8(3) . . ?
C6 N10 Cu1 107.6(2) . . ?
C9 N10 Cu1 139.5(2) . . ?
C12 N11 N15 106.0(3) . . ?
C12 N11 Cu1 141.4(3) . . ?
N15 N11 Cu1 112.4(2) . . ?
N11 C12 C13 109.2(4) . . ?
N11 C12 C22 121.3(3) . . ?
C13 C12 C22 129.2(4) . . ?
C12 C22 H22A 109.5 . . ?
C12 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C12 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C14 C13 C12 108.3(4) . . ?
C14 C13 H13 125.8 . . ?
C12 C13 H13 125.8 . . ?
C13 C14 N15 105.2(4) . . ?
C13 C14 C42 131.7(4) . . ?
N15 C14 C42 123.0(4) . . ?
C14 C42 H42A 109.5 . . ?
C14 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C14 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
N11 N15 C14 111.2(3) . . ?
N11 N15 C16 115.3(3) . . ?
C14 N15 C16 132.7(3) . . ?
N20 C16 N15 117.8(3) . . ?
N20 C16 S17 116.7(3) . . ?
N15 C16 S17 125.4(3) . . ?
C16 S17 C18 88.2(2) . . ?
C19 C18 S17 112.2(3) . . ?
C19 C18 H18 123.9 . . ?
S17 C18 H18 123.9 . . ?
C18 C19 N20 113.2(4) . . ?
C18 C19 C9G 124.2(4) . . ?
N20 C19 C9G 122.2(3) . . ?
C16 N20 C19 109.5(3) . . ?
C16 N20 Cu1 110.7(2) . . ?
C19 N20 Cu1 136.4(2) . . ?
C9H C9G C9L 118.9(5) . . ?
C9H C9G C19 121.0(3) . . ?
C9L C9G C19 119.8(5) . . ?
C9G C9H C9I 120.5(4) . . ?
C9G C9H H9H 119.8 . . ?
C9I C9H H9H 119.8 . . ?
C9J C9I C9H 119.7(6) . . ?
C9J C9I H9I 120.1 . . ?
C9H C9I H9I 120.1 . . ?
C9K C9J C9I 119.6(6) . . ?
C9K C9J H9J 120.2 . . ?
C9I C9J H9J 120.2 . . ?
C9J C9K C9L 122.2(6) . . ?
C9J C9K H9K 118.9 . . ?
C9L C9K H9K 118.9 . . ?
C9K C9L C9G 119.0(6) . . ?
C9K C9L H9L 120.5 . . ?
C9G C9L H9L 120.5 . . ?
O8 N31 O9 124.0(4) . . ?
O8 N31 O3 118.1(4) . . ?
O9 N31 O3 117.9(4) . . ?
N31 O3 Cu1 111.7(2) . . ?
O31 Cu2 O31 92.9(2) . 3 ?
O31 Cu2 O34 158.46(15) . . ?
O31 Cu2 O34 91.53(16) 3 . ?
O31 Cu2 O34 91.53(16) . 3 ?
O31 Cu2 O34 158.47(15) 3 3 ?
O34 Cu2 O34 92.1(2) . 3 ?
O33 N32 O32 124.8(5) . . ?
O33 N32 O31 117.0(5) . . ?
O32 N32 O31 118.2(5) . . ?
N32 O31 Cu2 114.1(3) . . ?
O36 N33 O35 123.7(6) . . ?
O36 N33 O34 119.0(6) . . ?
O35 N33 O34 117.3(5) . . ?
N33 O34 Cu2 107.7(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
N11 Cu1 N1 C2 3.1(14) . . . . ?
O3 Cu1 N1 C2 -95.9(4) . . . . ?
N20 Cu1 N1 C2 66.7(4) . . . . ?
N10 Cu1 N1 C2 172.5(4) . . . . ?
N11 Cu1 N1 N5 -175.5(11) . . . . ?
O3 Cu1 N1 N5 85.5(2) . . . . ?
N20 Cu1 N1 N5 -111.9(2) . . . . ?
N10 Cu1 N1 N5 -6.1(2) . . . . ?
N5 N1 C2 C3 1.1(4) . . . . ?
Cu1 N1 C2 C3 -177.7(3) . . . . ?
N5 N1 C2 C21 -179.8(3) . . . . ?
Cu1 N1 C2 C21 1.5(6) . . . . ?
N1 C2 C3 C4 -0.2(5) . . . . ?
C21 C2 C3 C4 -179.2(4) . . . . ?
C2 C3 C4 N5 -0.8(5) . . . . ?
C2 C3 C4 C41 178.0(4) . . . . ?
C2 N1 N5 C4 -1.6(4) . . . . ?
Cu1 N1 N5 C4 177.4(2) . . . . ?
C2 N1 N5 C6 -177.8(3) . . . . ?
Cu1 N1 N5 C6 1.2(4) . . . . ?
C3 C4 N5 N1 1.5(4) . . . . ?
C41 C4 N5 N1 -177.4(4) . . . . ?
C3 C4 N5 C6 176.9(4) . . . . ?
C41 C4 N5 C6 -2.0(7) . . . . ?
N1 N5 C6 N10 9.3(5) . . . . ?
C4 N5 C6 N10 -165.9(4) . . . . ?
N1 N5 C6 S7 -165.3(3) . . . . ?
C4 N5 C6 S7 19.5(6) . . . . ?
N10 C6 S7 C8 1.4(3) . . . . ?
N5 C6 S7 C8 176.2(3) . . . . ?
C6 S7 C8 C9 -0.2(3) . . . . ?
S7 C8 C9 N10 -0.9(5) . . . . ?
S7 C8 C9 C9A 179.6(3) . . . . ?
C8 C9 C9A C9F 30.4(6) . . . . ?
N10 C9 C9A C9F -149.2(4) . . . . ?
C8 C9 C9A C9B -148.4(4) . . . . ?
N10 C9 C9A C9B 32.1(6) . . . . ?
C9F C9A C9B C9C 2.0(6) . . . . ?
C9 C9A C9B C9C -179.3(4) . . . . ?
C9A C9B C9C C9D -0.9(7) . . . . ?
C9B C9C C9D C9E -0.7(8) . . . . ?
C9C C9D C9E C9F 1.3(8) . . . . ?
C9D C9E C9F C9A -0.1(8) . . . . ?
C9B C9A C9F C9E -1.5(7) . . . . ?
C9 C9A C9F C9E 179.8(4) . . . . ?
N5 C6 N10 C9 -177.2(3) . . . . ?
S7 C6 N10 C9 -2.1(4) . . . . ?
N5 C6 N10 Cu1 -13.2(4) . . . . ?
S7 C6 N10 Cu1 161.89(19) . . . . ?
C8 C9 N10 C6 1.9(5) . . . . ?
C9A C9 N10 C6 -178.5(3) . . . . ?
C8 C9 N10 Cu1 -154.2(3) . . . . ?
C9A C9 N10 Cu1 25.4(5) . . . . ?
N11 Cu1 N10 C6 -170.9(2) . . . . ?
N1 Cu1 N10 C6 10.2(2) . . . . ?
O3 Cu1 N10 C6 -78.5(2) . . . . ?
N20 Cu1 N10 C6 103.6(2) . . . . ?
N11 Cu1 N10 C9 -14.5(4) . . . . ?
N1 Cu1 N10 C9 166.7(4) . . . . ?
O3 Cu1 N10 C9 77.9(4) . . . . ?
N20 Cu1 N10 C9 -100.0(4) . . . . ?
N1 Cu1 N11 C12 -132.4(11) . . . . ?
O3 Cu1 N11 C12 -33.5(4) . . . . ?
N20 Cu1 N11 C12 163.3(4) . . . . ?
N10 Cu1 N11 C12 58.5(4) . . . . ?
N1 Cu1 N11 N15 53.7(13) . . . . ?
O3 Cu1 N11 N15 152.6(3) . . . . ?
N20 Cu1 N11 N15 -10.6(2) . . . . ?
N10 Cu1 N11 N15 -115.4(2) . . . . ?
N15 N11 C12 C13 0.3(4) . . . . ?
Cu1 N11 C12 C13 -173.9(3) . . . . ?
N15 N11 C12 C22 175.9(4) . . . . ?
Cu1 N11 C12 C22 1.7(7) . . . . ?
N11 C12 C13 C14 0.6(5) . . . . ?
C22 C12 C13 C14 -174.6(4) . . . . ?
C12 C13 C14 N15 -1.1(5) . . . . ?
C12 C13 C14 C42 174.6(5) . . . . ?
C12 N11 N15 C14 -1.0(4) . . . . ?
Cu1 N11 N15 C14 175.0(3) . . . . ?
C12 N11 N15 C16 -172.0(3) . . . . ?
Cu1 N11 N15 C16 4.0(4) . . . . ?
C13 C14 N15 N11 1.4(5) . . . . ?
C42 C14 N15 N11 -174.8(4) . . . . ?
C13 C14 N15 C16 170.3(4) . . . . ?
C42 C14 N15 C16 -5.9(7) . . . . ?
N11 N15 C16 N20 10.5(5) . . . . ?
C14 N15 C16 N20 -158.1(4) . . . . ?
N11 N15 C16 S17 -167.1(3) . . . . ?
C14 N15 C16 S17 24.3(6) . . . . ?
N20 C16 S17 C18 2.2(3) . . . . ?
N15 C16 S17 C18 179.8(4) . . . . ?
C16 S17 C18 C19 0.2(4) . . . . ?
S17 C18 C19 N20 -2.3(5) . . . . ?
S17 C18 C19 C9G 170.3(3) . . . . ?
N15 C16 N20 C19 178.4(3) . . . . ?
S17 C16 N20 C19 -3.8(4) . . . . ?
N15 C16 N20 Cu1 -18.9(4) . . . . ?
S17 C16 N20 Cu1 158.9(2) . . . . ?
C18 C19 N20 C16 3.9(5) . . . . ?
C9G C19 N20 C16 -169.0(4) . . . . ?
C18 C19 N20 Cu1 -152.4(3) . . . . ?
C9G C19 N20 Cu1 34.7(6) . . . . ?
N11 Cu1 N20 C16 16.0(3) . . . . ?
N1 Cu1 N20 C16 -158.5(3) . . . . ?
O3 Cu1 N20 C16 -50.8(5) . . . . ?
N10 Cu1 N20 C16 122.5(3) . . . . ?
N11 Cu1 N20 C19 172.1(4) . . . . ?
N1 Cu1 N20 C19 -2.4(4) . . . . ?
O3 Cu1 N20 C19 105.3(5) . . . . ?
N10 Cu1 N20 C19 -81.4(4) . . . . ?
C18 C19 C9G C9H -132.9(5) . . . . ?
N20 C19 C9G C9H 39.2(6) . . . . ?
C18 C19 C9G C9L 40.8(6) . . . . ?
N20 C19 C9G C9L -147.1(4) . . . . ?
C9L C9G C9H C9I 0.6(6) . . . . ?
C19 C9G C9H C9I 174.4(4) . . . . ?
C9G C9H C9I C9J -1.0(7) . . . . ?
C9H C9I C9J C9K 0.4(10) . . . . ?
C9I C9J C9K C9L 0.6(12) . . . . ?
C9J C9K C9L C9G -1.0(10) . . . . ?
C9H C9G C9L C9K 0.4(7) . . . . ?
C19 C9G C9L C9K -173.5(5) . . . . ?
O8 N31 O3 Cu1 173.1(3) . . . . ?
O9 N31 O3 Cu1 -6.3(4) . . . . ?
N11 Cu1 O3 N31 -74.1(2) . . . . ?
N1 Cu1 O3 N31 100.0(2) . . . . ?
N20 Cu1 O3 N31 -9.0(5) . . . . ?
N10 Cu1 O3 N31 177.5(2) . . . . ?
O33 N32 O31 Cu2 -11.8(6) . . . . ?
O32 N32 O31 Cu2 165.2(4) . . . . ?
O31 Cu2 O31 N32 84.8(3) 3 . . . ?
O34 Cu2 O31 N32 -173.6(4) . . . . ?
O34 Cu2 O31 N32 -74.1(3) 3 . . . ?
O36 N33 O34 Cu2 179.9(5) . . . . ?
O35 N33 O34 Cu2 -0.7(6) . . . . ?
O31 Cu2 O34 N33 21.8(7) . . . . ?
O31 Cu2 O34 N33 123.5(3) 3 . . . ?
O34 Cu2 O34 N33 -77.7(3) 3 . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.810
_refine_diff_density_min         -0.893
_refine_diff_density_rms         0.091

_database_code_depnum_ccdc_archive 'CCDC 989127'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_mr49-1-auto-sch_shape

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         
'(Ni 2+), 2(C6 H9 N3 S), (N O3 1-), (N O3 1-), 0.9(C4 H10 O), 0.4(H2 O)'
_chemical_formula_sum            'C15.60 H27.80 N8 Ni O7.30 S2'
_chemical_melting_point          ?

_exptl_crystal_description       tabular
_exptl_crystal_colour            'dark green'

_diffrn_ambient_temperature      293(2)
_chemical_formula_weight         567.09

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   'P 21/n'
_symmetry_int_tables_number      14
_chemical_absolute_configuration ?

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                   16.6552(6)
_cell_length_b                   14.1497(5)
_cell_length_c                   23.1221(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.258(4)
_cell_angle_gamma                90.00
_cell_volume                     5281.2(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    17920
_cell_measurement_theta_min      2.32
_cell_measurement_theta_max      25.03
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2366
_exptl_absorpt_coefficient_mu    0.943
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.7399
_exptl_absorpt_correction_T_max  0.8872
_exptl_absorpt_process_details   'CrysAlis CCD, Oxford 2001'

_exptl_special_details           
; 
 ? 
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Sapphire CCD diffractometer'
_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            17920
_diffrn_reflns_av_R_equivalents  0.0792
_diffrn_reflns_av_sigmaI/netI    0.1087
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.32
_diffrn_reflns_theta_max         25.03
_reflns_number_total             9376
_reflns_number_gt                4786
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       CrysAlisCCD
_computing_cell_refinement       ?
_computing_data_reduction        'CrysAlis 171'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'WinGX v1.80.05'
_computing_publication_material  CIFTAB

_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)+(0.1202P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9376
_refine_ls_number_parameters     635
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1445
_refine_ls_R_factor_gt           0.0720
_refine_ls_wR_factor_ref         0.2381
_refine_ls_wR_factor_gt          0.2057
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.047
_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
Ni1 Ni 0.35322(5) 0.06095(7) 0.25251(4) 0.0491(3) Uani 1 1 d . . .
N1 N 0.4683(3) -0.0015(4) 0.2630(3) 0.0506(15) Uani 1 1 d . . .
C2 C 0.4972(5) -0.0704(6) 0.2354(4) 0.056(2) Uani 1 1 d . . .
C21 C 0.4601(6) -0.0954(7) 0.1730(4) 0.081(3) Uani 1 1 d . . .
H21A H 0.4186 -0.1431 0.1713 0.121 Uiso 1 1 calc R . .
H21B H 0.5023 -0.1192 0.1550 0.121 Uiso 1 1 calc R . .
H21C H 0.4351 -0.0404 0.1516 0.121 Uiso 1 1 calc R . .
C3 C 0.5674(5) -0.1107(6) 0.2740(4) 0.059(2) Uani 1 1 d . . .
H3 H 0.5984 -0.1610 0.2653 0.071 Uiso 1 1 calc R . .
C4 C 0.5817(4) -0.0628(6) 0.3263(4) 0.056(2) Uani 1 1 d . . .
C41 C 0.6470(6) -0.0807(7) 0.3831(4) 0.087(3) Uani 1 1 d . . .
H41A H 0.6705 -0.1423 0.3815 0.130 Uiso 1 1 calc R . .
H41B H 0.6223 -0.0776 0.4165 0.130 Uiso 1 1 calc R . .
H41C H 0.6897 -0.0338 0.3876 0.130 Uiso 1 1 calc R . .
N5 N 0.5220(4) 0.0060(4) 0.3193(3) 0.0504(15) Uani 1 1 d . . .
C6 C 0.5090(5) 0.0791(6) 0.3558(4) 0.057(2) Uani 1 1 d . . .
S7 S 0.42058(13) 0.14294(18) 0.33832(11) 0.0737(7) Uani 1 1 d . . .
N10 N 0.5694(4) 0.1013(5) 0.4031(3) 0.0680(19) Uani 1 1 d . . .
H10A H 0.5771 0.0539 0.4293 0.102 Uiso 0.66 1 calc PR . .
H10B H 0.5557 0.1533 0.4201 0.102 Uiso 0.67 1 calc PR . .
H10C H 0.6160 0.1114 0.3918 0.102 Uiso 0.67 1 calc PR . .
N11 N 0.2402(3) 0.1212(4) 0.2441(3) 0.0429(14) Uani 1 1 d . . .
C12 C 0.1826(5) 0.1193(6) 0.2749(3) 0.053(2) Uani 1 1 d . . .
C27 C 0.1970(5) 0.0748(7) 0.3339(4) 0.073(3) Uani 1 1 d . . .
H27A H 0.1961 0.0073 0.3295 0.109 Uiso 1 1 calc R . .
H27B H 0.1544 0.0939 0.3528 0.109 Uiso 1 1 calc R . .
H27C H 0.2500 0.0942 0.3579 0.109 Uiso 1 1 calc R . .
C13 C 0.1097(4) 0.1634(6) 0.2418(4) 0.062(2) Uani 1 1 d . . .
H13 H 0.0601 0.1689 0.2531 0.074 Uiso 1 1 calc R . .
C14 C 0.1249(4) 0.1962(5) 0.1906(4) 0.053(2) Uani 1 1 d . . .
C42 C 0.0671(5) 0.2509(8) 0.1425(4) 0.080(3) Uani 1 1 d . . .
H42A H 0.0176 0.2657 0.1549 0.119 Uiso 1 1 calc R . .
H42B H 0.0531 0.2138 0.1067 0.119 Uiso 1 1 calc R . .
H42C H 0.0935 0.3084 0.1351 0.119 Uiso 1 1 calc R . .
N15 N 0.2054(3) 0.1692(4) 0.1922(3) 0.0451(14) Uani 1 1 d . . .
C16 C 0.2589(4) 0.1958(5) 0.1565(4) 0.0496(19) Uani 1 1 d . . .
S17 S 0.35916(12) 0.16723(15) 0.17636(10) 0.0601(6) Uani 1 1 d . . .
N20 N 0.2278(4) 0.2404(6) 0.1081(4) 0.085(2) Uani 1 1 d . . .
H20A H 0.1750 0.2238 0.0943 0.127 Uiso 0.66 1 calc PR . .
H20B H 0.2558 0.2262 0.0811 0.127 Uiso 0.67 1 calc PR . .
H20C H 0.2309 0.3023 0.1151 0.127 Uiso 0.67 1 calc PR . .
N41 N 0.2812(4) -0.0995(5) 0.2338(4) 0.064(2) Uani 1 1 d . . .
O42 O 0.3116(4) -0.0714(5) 0.2869(3) 0.0734(17) Uani 1 1 d . . .
O43 O 0.2920(3) -0.0435(4) 0.1933(3) 0.0590(14) Uani 1 1 d . . .
O44 O 0.2445(4) -0.1743(4) 0.2228(4) 0.093(2) Uani 1 1 d . . .
Ni2 Ni 0.64895(5) 0.55040(6) 0.24132(4) 0.0478(3) Uani 1 1 d . . .
N21 N 0.5531(4) 0.4767(4) 0.2618(3) 0.0521(16) Uani 1 1 d . . .
C22 C 0.4910(5) 0.4236(6) 0.2324(4) 0.055(2) Uani 1 1 d . . .
C28 C 0.4853(5) 0.3912(7) 0.1694(4) 0.078(3) Uani 1 1 d . . .
H28A H 0.5107 0.4373 0.1492 0.117 Uiso 1 1 calc R . .
H28B H 0.4281 0.3838 0.1488 0.117 Uiso 1 1 calc R . .
H28C H 0.5133 0.3317 0.1702 0.117 Uiso 1 1 calc R . .
C23 C 0.4365(5) 0.4039(5) 0.2676(4) 0.055(2) Uani 1 1 d . . .
H23 H 0.3893 0.3665 0.2569 0.066 Uiso 1 1 calc R . .
C24 C 0.4640(4) 0.4482(5) 0.3195(4) 0.0501(19) Uani 1 1 d . . .
C43 C 0.4221(5) 0.4612(7) 0.3704(4) 0.071(2) Uani 1 1 d . . .
H43A H 0.3633 0.4529 0.3557 0.106 Uiso 1 1 calc R . .
H43B H 0.4333 0.5235 0.3868 0.106 Uiso 1 1 calc R . .
H43C H 0.4431 0.4152 0.4009 0.106 Uiso 1 1 calc R . .
N25 N 0.5382(3) 0.4915(4) 0.3174(3) 0.0481(15) Uani 1 1 d . . .
C26 C 0.5938(4) 0.5472(5) 0.3589(4) 0.0513(19) Uani 1 1 d . . .
S27 S 0.65747(13) 0.62267(16) 0.33528(10) 0.0626(6) Uani 1 1 d . . .
N30 N 0.5919(4) 0.5384(5) 0.4146(3) 0.0678(19) Uani 1 1 d . . .
H30A H 0.5462 0.5657 0.4203 0.102 Uiso 0.66 1 calc PR . .
H30B H 0.6362 0.5661 0.4377 0.102 Uiso 0.67 1 calc PR . .
H30C H 0.5918 0.4773 0.4239 0.102 Uiso 0.67 1 calc PR . .
N31 N 0.7382(3) 0.6302(4) 0.2183(3) 0.0515(16) Uani 1 1 d . . .
C32 C 0.8155(5) 0.6506(6) 0.2383(4) 0.062(2) Uani 1 1 d . . .
C29 C 0.8647(5) 0.6062(7) 0.2959(4) 0.084(3) Uani 1 1 d . . .
H29A H 0.8426 0.6268 0.3284 0.126 Uiso 1 1 calc R . .
H29B H 0.9217 0.6249 0.3030 0.126 Uiso 1 1 calc R . .
H29C H 0.8608 0.5386 0.2927 0.126 Uiso 1 1 calc R . .
C33 C 0.8415(6) 0.7176(7) 0.2017(5) 0.074(3) Uani 1 1 d . . .
H33 H 0.8946 0.7423 0.2075 0.089 Uiso 1 1 calc R . .
C34 C 0.7763(6) 0.7392(6) 0.1573(4) 0.067(2) Uani 1 1 d . . .
C44 C 0.7669(7) 0.8148(8) 0.1108(5) 0.101(4) Uani 1 1 d . . .
H44A H 0.8128 0.8578 0.1214 0.152 Uiso 1 1 calc R . .
H44B H 0.7162 0.8486 0.1083 0.152 Uiso 1 1 calc R . .
H44C H 0.7658 0.7865 0.0729 0.152 Uiso 1 1 calc R . .
N35 N 0.7121(4) 0.6859(4) 0.1673(3) 0.0545(17) Uani 1 1 d . . .
C36 C 0.6280(5) 0.6827(5) 0.1354(4) 0.056(2) Uani 1 1 d . . .
S37 S 0.55726(12) 0.64724(16) 0.17107(10) 0.0615(6) Uani 1 1 d . . .
N40 N 0.6106(4) 0.7080(6) 0.0801(4) 0.077(2) Uani 1 1 d . . .
H40A H 0.6377 0.6712 0.0601 0.116 Uiso 0.66 1 calc PR . .
H40B H 0.6256 0.7679 0.0775 0.116 Uiso 0.67 1 calc PR . .
H40C H 0.5563 0.7023 0.0646 0.116 Uiso 0.67 1 calc PR . .
N45 N 0.7151(4) 0.3999(5) 0.2173(4) 0.0586(18) Uani 1 1 d . . .
O46 O 0.6658(3) 0.4471(4) 0.1780(3) 0.0619(15) Uani 1 1 d . . .
O47 O 0.7326(3) 0.4337(4) 0.2692(3) 0.0635(15) Uani 1 1 d . . .
O48 O 0.7427(4) 0.3251(4) 0.2055(3) 0.088(2) Uani 1 1 d . . .
N2 N 0.7372(5) 0.6184(6) 0.9971(4) 0.075(2) Uani 1 1 d . . .
O2 O 0.7656(6) 0.5728(6) 0.9623(4) 0.127(3) Uani 1 1 d . . .
O3 O 0.6900(4) 0.6891(6) 0.9781(3) 0.097(2) Uani 1 1 d . . .
O4 O 0.7505(4) 0.6002(5) 1.0498(3) 0.087(2) Uani 1 1 d . . .
N6 N 0.9260(5) 0.8146(6) 0.0198(4) 0.075(2) Uani 1 1 d . . .
O6 O 0.9368(5) 0.8203(6) 0.0742(4) 0.105(2) Uani 1 1 d . . .
O7 O 0.9269(6) 0.8858(5) -0.0093(4) 0.118(3) Uani 1 1 d . . .
O8 O 0.9106(5) 0.7346(5) -0.0040(3) 0.101(2) Uani 1 1 d . . .
C81 C 0.6319(17) 0.7657(17) 0.5082(9) 0.232(12) Uani 1 1 d D . .
H81A H 0.6277 0.8205 0.5318 0.347 Uiso 1 1 calc R . .
H81B H 0.5803 0.7319 0.4996 0.347 Uiso 1 1 calc R . .
H81C H 0.6442 0.7851 0.4715 0.347 Uiso 1 1 calc R . .
C82 C 0.6969(13) 0.7055(17) 0.5406(10) 0.199(10) Uani 1 1 d D . .
H82A H 0.6845 0.6871 0.5779 0.238 Uiso 1 1 calc R . .
H82B H 0.7484 0.7407 0.5501 0.238 Uiso 1 1 calc R . .
O83 O 0.7071(5) 0.6253(8) 0.5094(4) 0.121(3) Uani 1 1 d . . .
C84 C 0.7702(13) 0.5635(18) 0.5436(8) 0.211(10) Uani 1 1 d D . .
H84A H 0.8223 0.5976 0.5539 0.253 Uiso 1 1 calc R . .
H84B H 0.7558 0.5473 0.5805 0.253 Uiso 1 1 calc R . .
C85 C 0.7818(12) 0.4778(16) 0.5135(10) 0.216(11) Uani 1 1 d D . .
H85A H 0.8234 0.4398 0.5393 0.324 Uiso 1 1 calc R . .
H85B H 0.7992 0.4928 0.4779 0.324 Uiso 1 1 calc R . .
H85C H 0.7306 0.4434 0.5030 0.324 Uiso 1 1 calc R . .
C71 C 0.4917(19) 0.8627(19) 0.9674(12) 0.232(15) Uani 0.80 1 d PD A 1
H71A H 0.4841 0.9017 0.9326 0.349 Uiso 0.80 1 calc PR A 1
H71B H 0.5489 0.8447 0.9805 0.349 Uiso 0.80 1 calc PR A 1
H71C H 0.4759 0.8972 0.9986 0.349 Uiso 0.80 1 calc PR A 1
C72 C 0.4409(18) 0.7788(18) 0.9533(10) 0.222(15) Uani 0.80 1 d PD A 1
H72A H 0.4547 0.7460 0.9202 0.266 Uiso 0.80 1 calc PR A 1
H72B H 0.3831 0.7970 0.9411 0.266 Uiso 0.80 1 calc PR A 1
O73 O 0.4522(6) 0.7209(11) 0.9997(5) 0.113(4) Uani 0.80 1 d PD A 1
C74 C 0.4042(18) 0.6483(18) 0.9758(10) 0.244(18) Uani 0.80 1 d PD A 1
H74A H 0.4242 0.6219 0.9432 0.293 Uiso 0.80 1 calc PR A 1
H74B H 0.3480 0.6704 0.9597 0.293 Uiso 0.80 1 calc PR A 1
C75 C 0.4043(19) 0.576(2) 1.0199(11) 0.29(2) Uani 0.80 1 d PD A 1
H75A H 0.3671 0.5259 1.0023 0.432 Uiso 0.80 1 calc PR A 1
H75B H 0.3865 0.6024 1.0528 0.432 Uiso 0.80 1 calc PR A 1
H75C H 0.4592 0.5507 1.0338 0.432 Uiso 0.80 1 calc PR A 1
O51 O 0.9419(18) 0.5525(16) -0.0544(10) 0.310(13) Uani 0.80 1 d P B 1


_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 N11 2.033(5) . ?
Ni1 N1 2.070(6) . ?
Ni1 O43 2.100(5) . ?
Ni1 O42 2.212(6) . ?
Ni1 S7 2.333(3) . ?
Ni1 S17 2.336(2) . ?
N1 C2 1.320(9) . ?
N1 N5 1.390(8) . ?
C2 C3 1.406(11) . ?
C2 C21 1.466(11) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C3 C4 1.355(11) . ?
C3 H3 0.9300 . ?
C4 N5 1.372(9) . ?
C4 C41 1.506(11) . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
N5 C6 1.385(10) . ?
C6 N10 1.330(10) . ?
C6 S7 1.690(8) . ?
N10 H10A 0.8900 . ?
N10 H10B 0.8900 . ?
N10 H10C 0.8900 . ?
N11 C12 1.327(8) . ?
N11 N15 1.377(8) . ?
C12 C13 1.410(11) . ?
C12 C27 1.467(11) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C13 C14 1.352(11) . ?
C13 H13 0.9300 . ?
C14 N15 1.385(9) . ?
C14 C42 1.495(11) . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
N15 C16 1.407(9) . ?
C16 N20 1.278(10) . ?
C16 S17 1.670(7) . ?
N20 H20A 0.8900 . ?
N20 H20B 0.8900 . ?
N20 H20C 0.8900 . ?
N41 O44 1.217(9) . ?
N41 O42 1.271(9) . ?
N41 O43 1.272(8) . ?
Ni2 N31 2.039(6) . ?
Ni2 N21 2.058(6) . ?
Ni2 O46 2.136(5) . ?
Ni2 O47 2.153(5) . ?
Ni2 S37 2.372(2) . ?
Ni2 S27 2.374(2) . ?
N21 C22 1.322(9) . ?
N21 N25 1.383(8) . ?
C22 C23 1.389(11) . ?
C22 C28 1.507(11) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C23 C24 1.330(11) . ?
C23 H23 0.9300 . ?
C24 N25 1.391(9) . ?
C24 C43 1.520(10) . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
N25 C26 1.400(9) . ?
C26 N30 1.302(9) . ?
C26 S27 1.688(8) . ?
N30 H30A 0.8900 . ?
N30 H30B 0.8900 . ?
N30 H30C 0.8900 . ?
N31 C32 1.288(9) . ?
N31 N35 1.396(8) . ?
C32 C33 1.407(12) . ?
C32 C29 1.518(13) . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C33 C34 1.333(13) . ?
C33 H33 0.9300 . ?
C34 N35 1.374(9) . ?
C34 C44 1.498(13) . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
N35 C36 1.414(10) . ?
C36 N40 1.290(10) . ?
C36 S37 1.672(8) . ?
N40 H40A 0.8900 . ?
N40 H40B 0.8900 . ?
N40 H40C 0.8900 . ?
N45 O48 1.211(8) . ?
N45 O46 1.255(9) . ?
N45 O47 1.258(9) . ?
N2 O2 1.214(10) . ?
N2 O4 1.211(9) . ?
N2 O3 1.282(10) . ?
N6 O7 1.212(9) . ?
N6 O6 1.229(10) . ?
N6 O8 1.257(9) . ?
C81 C82 1.435(17) . ?
C81 H81A 0.9600 . ?
C81 H81B 0.9600 . ?
C81 H81C 0.9600 . ?
C82 O83 1.38(2) . ?
C82 H82A 0.9700 . ?
C82 H82B 0.9700 . ?
O83 C84 1.444(19) . ?
C84 C85 1.435(16) . ?
C84 H84A 0.9700 . ?
C84 H84B 0.9700 . ?
C85 H85A 0.9600 . ?
C85 H85B 0.9600 . ?
C85 H85C 0.9600 . ?
C71 C72 1.448(18) . ?
C71 H71A 0.9600 . ?
C71 H71B 0.9600 . ?
C71 H71C 0.9600 . ?
C72 O73 1.326(17) . ?
C72 H72A 0.9700 . ?
C72 H72B 0.9700 . ?
O73 C74 1.336(18) . ?
C74 C75 1.446(17) . ?
C74 H74A 0.9700 . ?
C74 H74B 0.9700 . ?
C75 H75A 0.9600 . ?
C75 H75B 0.9600 . ?
C75 H75C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N11 Ni1 N1 178.7(2) . . ?
N11 Ni1 O43 86.7(2) . . ?
N1 Ni1 O43 93.6(2) . . ?
N11 Ni1 O42 91.4(2) . . ?
N1 Ni1 O42 87.7(2) . . ?
O43 Ni1 O42 59.6(2) . . ?
N11 Ni1 S7 96.46(17) . . ?
N1 Ni1 S7 82.83(18) . . ?
O43 Ni1 S7 163.48(18) . . ?
O42 Ni1 S7 104.1(2) . . ?
N11 Ni1 S17 82.44(17) . . ?
N1 Ni1 S17 98.81(19) . . ?
O43 Ni1 S17 93.76(17) . . ?
O42 Ni1 S17 153.0(2) . . ?
S7 Ni1 S17 102.71(10) . . ?
C2 N1 N5 106.4(6) . . ?
C2 N1 Ni1 134.1(5) . . ?
N5 N1 Ni1 116.1(4) . . ?
N1 C2 C3 109.7(7) . . ?
N1 C2 C21 122.6(7) . . ?
C3 C2 C21 127.6(7) . . ?
C2 C21 H21A 109.5 . . ?
C2 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C2 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C4 C3 C2 107.4(7) . . ?
C4 C3 H3 126.3 . . ?
C2 C3 H3 126.3 . . ?
C3 C4 N5 106.7(7) . . ?
C3 C4 C41 128.6(8) . . ?
N5 C4 C41 124.7(8) . . ?
C4 C41 H41A 109.5 . . ?
C4 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C4 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C4 N5 N1 109.7(6) . . ?
C4 N5 C6 132.4(7) . . ?
N1 N5 C6 117.8(6) . . ?
N10 C6 N5 118.5(7) . . ?
N10 C6 S7 120.6(6) . . ?
N5 C6 S7 120.7(6) . . ?
C6 S7 Ni1 98.4(3) . . ?
C6 N10 H10A 109.5 . . ?
C6 N10 H10B 109.5 . . ?
H10A N10 H10B 109.5 . . ?
C6 N10 H10C 109.5 . . ?
H10A N10 H10C 109.5 . . ?
H10B N10 H10C 109.5 . . ?
C12 N11 N15 105.9(6) . . ?
C12 N11 Ni1 135.7(6) . . ?
N15 N11 Ni1 118.1(4) . . ?
N11 C12 C13 109.8(7) . . ?
N11 C12 C27 122.2(7) . . ?
C13 C12 C27 128.0(7) . . ?
C12 C27 H27A 109.5 . . ?
C12 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C12 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C14 C13 C12 107.8(6) . . ?
C14 C13 H13 126.1 . . ?
C12 C13 H13 126.1 . . ?
C13 C14 N15 105.7(7) . . ?
C13 C14 C42 127.1(7) . . ?
N15 C14 C42 127.2(7) . . ?
C14 C42 H42A 109.5 . . ?
C14 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C14 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
N11 N15 C14 110.8(6) . . ?
N11 N15 C16 116.9(5) . . ?
C14 N15 C16 131.2(7) . . ?
N20 C16 N15 117.9(7) . . ?
N20 C16 S17 121.5(6) . . ?
N15 C16 S17 120.6(6) . . ?
C16 S17 Ni1 97.9(3) . . ?
C16 N20 H20A 109.5 . . ?
C16 N20 H20B 109.5 . . ?
H20A N20 H20B 109.5 . . ?
C16 N20 H20C 109.5 . . ?
H20A N20 H20C 109.5 . . ?
H20B N20 H20C 109.5 . . ?
O44 N41 O42 122.2(8) . . ?
O44 N41 O43 122.9(9) . . ?
O42 N41 O43 114.9(7) . . ?
N41 O42 Ni1 90.1(5) . . ?
N41 O43 Ni1 95.3(5) . . ?
N31 Ni2 N21 176.1(3) . . ?
N31 Ni2 O46 88.4(2) . . ?
N21 Ni2 O46 92.9(2) . . ?
N31 Ni2 O47 92.5(2) . . ?
N21 Ni2 O47 91.4(2) . . ?
O46 Ni2 O47 59.7(2) . . ?
N31 Ni2 S37 83.64(19) . . ?
N21 Ni2 S37 92.58(19) . . ?
O46 Ni2 S37 95.59(19) . . ?
O47 Ni2 S37 155.2(2) . . ?
N31 Ni2 S27 96.77(18) . . ?
N21 Ni2 S27 83.26(18) . . ?
O46 Ni2 S27 159.04(19) . . ?
O47 Ni2 S27 99.7(2) . . ?
S37 Ni2 S27 105.14(9) . . ?
C22 N21 N25 105.5(6) . . ?
C22 N21 Ni2 136.3(5) . . ?
N25 N21 Ni2 117.6(4) . . ?
N21 C22 C23 110.7(7) . . ?
N21 C22 C28 121.7(7) . . ?
C23 C22 C28 127.7(7) . . ?
C22 C28 H28A 109.5 . . ?
C22 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C22 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C24 C23 C22 107.8(7) . . ?
C24 C23 H23 126.1 . . ?
C22 C23 H23 126.1 . . ?
C23 C24 N25 106.6(6) . . ?
C23 C24 C43 129.3(7) . . ?
N25 C24 C43 123.8(7) . . ?
C24 C43 H43A 109.5 . . ?
C24 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C24 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C24 N25 N21 109.3(6) . . ?
C24 N25 C26 131.8(6) . . ?
N21 N25 C26 118.9(6) . . ?
N30 C26 N25 116.8(7) . . ?
N30 C26 S27 123.4(6) . . ?
N25 C26 S27 119.8(6) . . ?
C26 S27 Ni2 97.1(3) . . ?
C26 N30 H30A 109.5 . . ?
C26 N30 H30B 109.5 . . ?
H30A N30 H30B 109.5 . . ?
C26 N30 H30C 109.5 . . ?
H30A N30 H30C 109.5 . . ?
H30B N30 H30C 109.5 . . ?
C32 N31 N35 104.6(6) . . ?
C32 N31 Ni2 139.3(6) . . ?
N35 N31 Ni2 116.0(4) . . ?
N31 C32 C33 111.3(9) . . ?
N31 C32 C29 119.8(8) . . ?
C33 C32 C29 128.8(8) . . ?
C32 C29 H29A 109.5 . . ?
C32 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C32 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C34 C33 C32 107.7(8) . . ?
C34 C33 H33 126.1 . . ?
C32 C33 H33 126.1 . . ?
C33 C34 N35 105.4(8) . . ?
C33 C34 C44 129.7(9) . . ?
N35 C34 C44 124.4(9) . . ?
C34 C44 H44A 109.5 . . ?
C34 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C34 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C34 N35 N31 111.0(7) . . ?
C34 N35 C36 130.0(7) . . ?
N31 N35 C36 119.0(6) . . ?
N40 C36 N35 117.3(7) . . ?
N40 C36 S37 123.9(7) . . ?
N35 C36 S37 118.7(6) . . ?
C36 S37 Ni2 95.6(3) . . ?
C36 N40 H40A 109.5 . . ?
C36 N40 H40B 109.5 . . ?
H40A N40 H40B 109.5 . . ?
C36 N40 H40C 109.5 . . ?
H40A N40 H40C 109.5 . . ?
H40B N40 H40C 109.5 . . ?
O48 N45 O46 121.2(9) . . ?
O48 N45 O47 122.4(9) . . ?
O46 N45 O47 116.3(6) . . ?
N45 O46 Ni2 92.4(5) . . ?
N45 O47 Ni2 91.5(4) . . ?
O2 N2 O4 123.4(10) . . ?
O2 N2 O3 119.5(10) . . ?
O4 N2 O3 117.1(9) . . ?
O7 N6 O6 119.6(9) . . ?
O7 N6 O8 122.4(9) . . ?
O6 N6 O8 117.9(9) . . ?
C82 C81 H81A 109.5 . . ?
C82 C81 H81B 109.5 . . ?
H81A C81 H81B 109.5 . . ?
C82 C81 H81C 109.5 . . ?
H81A C81 H81C 109.5 . . ?
H81B C81 H81C 109.5 . . ?
C81 C82 O83 113(2) . . ?
C81 C82 H82A 109.0 . . ?
O83 C82 H82A 109.0 . . ?
C81 C82 H82B 109.0 . . ?
O83 C82 H82B 109.0 . . ?
H82A C82 H82B 107.8 . . ?
C84 O83 C82 112.3(14) . . ?
C85 C84 O83 114.4(16) . . ?
C85 C84 H84A 108.7 . . ?
O83 C84 H84A 108.7 . . ?
C85 C84 H84B 108.7 . . ?
O83 C84 H84B 108.7 . . ?
H84A C84 H84B 107.6 . . ?
C84 C85 H85A 109.5 . . ?
C84 C85 H85B 109.5 . . ?
H85A C85 H85B 109.5 . . ?
C84 C85 H85C 109.5 . . ?
H85A C85 H85C 109.5 . . ?
H85B C85 H85C 109.5 . . ?
C72 C71 H71A 109.5 . . ?
C72 C71 H71B 109.5 . . ?
H71A C71 H71B 109.5 . . ?
C72 C71 H71C 109.5 . . ?
H71A C71 H71C 109.5 . . ?
H71B C71 H71C 109.5 . . ?
C71 C72 O73 111(2) . . ?
C71 C72 H72A 109.3 . . ?
O73 C72 H72A 109.3 . . ?
C71 C72 H72B 109.3 . . ?
O73 C72 H72B 109.3 . . ?
H72A C72 H72B 108.0 . . ?
C74 O73 C72 100.9(17) . . ?
O73 C74 C75 110.9(19) . . ?
O73 C74 H74A 109.5 . . ?
C75 C74 H74A 109.5 . . ?
O73 C74 H74B 109.5 . . ?
C75 C74 H74B 109.5 . . ?
H74A C74 H74B 108.0 . . ?
C74 C75 H75A 109.5 . . ?
C74 C75 H75B 109.5 . . ?
H75A C75 H75B 109.5 . . ?
C74 C75 H75C 109.5 . . ?
H75A C75 H75C 109.5 . . ?
H75B C75 H75C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N11 Ni1 N1 C2 117(10) . . . . ?
O43 Ni1 N1 C2 11.2(8) . . . . ?
O42 Ni1 N1 C2 70.5(8) . . . . ?
S7 Ni1 N1 C2 175.0(8) . . . . ?
S17 Ni1 N1 C2 -83.2(8) . . . . ?
N11 Ni1 N1 N5 -39(11) . . . . ?
O43 Ni1 N1 N5 -144.9(5) . . . . ?
O42 Ni1 N1 N5 -85.6(5) . . . . ?
S7 Ni1 N1 N5 18.9(5) . . . . ?
S17 Ni1 N1 N5 120.7(5) . . . . ?
N5 N1 C2 C3 2.4(9) . . . . ?
Ni1 N1 C2 C3 -155.3(6) . . . . ?
N5 N1 C2 C21 -175.8(8) . . . . ?
Ni1 N1 C2 C21 26.4(13) . . . . ?
N1 C2 C3 C4 -1.1(9) . . . . ?
C21 C2 C3 C4 177.0(8) . . . . ?
C2 C3 C4 N5 -0.7(9) . . . . ?
C2 C3 C4 C41 177.0(8) . . . . ?
C3 C4 N5 N1 2.2(8) . . . . ?
C41 C4 N5 N1 -175.6(7) . . . . ?
C3 C4 N5 C6 -175.0(7) . . . . ?
C41 C4 N5 C6 7.1(13) . . . . ?
C2 N1 N5 C4 -2.9(8) . . . . ?
Ni1 N1 N5 C4 159.5(5) . . . . ?
C2 N1 N5 C6 174.8(6) . . . . ?
Ni1 N1 N5 C6 -22.8(8) . . . . ?
C4 N5 C6 N10 12.8(12) . . . . ?
N1 N5 C6 N10 -164.3(7) . . . . ?
C4 N5 C6 S7 -170.8(6) . . . . ?
N1 N5 C6 S7 12.1(9) . . . . ?
N10 C6 S7 Ni1 179.1(6) . . . . ?
N5 C6 S7 Ni1 2.8(7) . . . . ?
N11 Ni1 S7 C6 168.4(3) . . . . ?
N1 Ni1 S7 C6 -10.4(3) . . . . ?
O43 Ni1 S7 C6 68.0(6) . . . . ?
O42 Ni1 S7 C6 75.4(3) . . . . ?
S17 Ni1 S7 C6 -107.9(3) . . . . ?
N1 Ni1 N11 C12 -10(11) . . . . ?
O43 Ni1 N11 C12 96.3(7) . . . . ?
O42 Ni1 N11 C12 36.8(7) . . . . ?
S7 Ni1 N11 C12 -67.5(7) . . . . ?
S17 Ni1 N11 C12 -169.5(7) . . . . ?
N1 Ni1 N11 N15 179(100) . . . . ?
O43 Ni1 N11 N15 -75.0(5) . . . . ?
O42 Ni1 N11 N15 -134.4(5) . . . . ?
S7 Ni1 N11 N15 121.3(4) . . . . ?
S17 Ni1 N11 N15 19.2(4) . . . . ?
N15 N11 C12 C13 1.9(8) . . . . ?
Ni1 N11 C12 C13 -170.1(6) . . . . ?
N15 N11 C12 C27 -179.2(7) . . . . ?
Ni1 N11 C12 C27 8.8(12) . . . . ?
N11 C12 C13 C14 -2.5(9) . . . . ?
C27 C12 C13 C14 178.6(8) . . . . ?
C12 C13 C14 N15 1.9(9) . . . . ?
C12 C13 C14 C42 -177.7(8) . . . . ?
C12 N11 N15 C14 -0.7(7) . . . . ?
Ni1 N11 N15 C14 173.0(5) . . . . ?
C12 N11 N15 C16 168.8(6) . . . . ?
Ni1 N11 N15 C16 -17.5(7) . . . . ?
C13 C14 N15 N11 -0.8(8) . . . . ?
C42 C14 N15 N11 178.8(8) . . . . ?
C13 C14 N15 C16 -168.4(7) . . . . ?
C42 C14 N15 C16 11.2(13) . . . . ?
N11 N15 C16 N20 -180.0(7) . . . . ?
C14 N15 C16 N20 -13.0(12) . . . . ?
N11 N15 C16 S17 1.6(9) . . . . ?
C14 N15 C16 S17 168.5(6) . . . . ?
N20 C16 S17 Ni1 -166.9(7) . . . . ?
N15 C16 S17 Ni1 11.5(6) . . . . ?
N11 Ni1 S17 C16 -14.5(3) . . . . ?
N1 Ni1 S17 C16 165.9(3) . . . . ?
O43 Ni1 S17 C16 71.7(3) . . . . ?
O42 Ni1 S17 C16 63.5(5) . . . . ?
S7 Ni1 S17 C16 -109.5(3) . . . . ?
O44 N41 O42 Ni1 -178.1(6) . . . . ?
O43 N41 O42 Ni1 1.8(6) . . . . ?
N11 Ni1 O42 N41 84.3(4) . . . . ?
N1 Ni1 O42 N41 -96.7(4) . . . . ?
O43 Ni1 O42 N41 -1.2(4) . . . . ?
S7 Ni1 O42 N41 -178.7(4) . . . . ?
S17 Ni1 O42 N41 8.3(6) . . . . ?
O44 N41 O43 Ni1 178.0(6) . . . . ?
O42 N41 O43 Ni1 -1.9(6) . . . . ?
N11 Ni1 O43 N41 -92.4(4) . . . . ?
N1 Ni1 O43 N41 86.3(4) . . . . ?
O42 Ni1 O43 N41 1.2(4) . . . . ?
S7 Ni1 O43 N41 9.4(8) . . . . ?
S17 Ni1 O43 N41 -174.6(4) . . . . ?
N31 Ni2 N21 C22 74(4) . . . . ?
O46 Ni2 N21 C22 -35.8(8) . . . . ?
O47 Ni2 N21 C22 -95.5(8) . . . . ?
S37 Ni2 N21 C22 59.9(8) . . . . ?
S27 Ni2 N21 C22 164.9(8) . . . . ?
N31 Ni2 N21 N25 -95(4) . . . . ?
O46 Ni2 N21 N25 154.8(5) . . . . ?
O47 Ni2 N21 N25 95.1(5) . . . . ?
S37 Ni2 N21 N25 -109.5(5) . . . . ?
S27 Ni2 N21 N25 -4.5(5) . . . . ?
N25 N21 C22 C23 0.1(9) . . . . ?
Ni2 N21 C22 C23 -170.2(6) . . . . ?
N25 N21 C22 C28 -179.5(7) . . . . ?
Ni2 N21 C22 C28 10.2(13) . . . . ?
N21 C22 C23 C24 1.9(9) . . . . ?
C28 C22 C23 C24 -178.6(8) . . . . ?
C22 C23 C24 N25 -3.0(8) . . . . ?
C22 C23 C24 C43 170.9(8) . . . . ?
C23 C24 N25 N21 3.1(8) . . . . ?
C43 C24 N25 N21 -171.2(7) . . . . ?
C23 C24 N25 C26 179.9(7) . . . . ?
C43 C24 N25 C26 5.6(12) . . . . ?
C22 N21 N25 C24 -1.9(8) . . . . ?
Ni2 N21 N25 C24 170.5(5) . . . . ?
C22 N21 N25 C26 -179.2(6) . . . . ?
Ni2 N21 N25 C26 -6.8(8) . . . . ?
C24 N25 C26 N30 22.2(11) . . . . ?
N21 N25 C26 N30 -161.3(6) . . . . ?
C24 N25 C26 S27 -156.6(6) . . . . ?
N21 N25 C26 S27 20.0(9) . . . . ?
N30 C26 S27 Ni2 161.6(6) . . . . ?
N25 C26 S27 Ni2 -19.7(6) . . . . ?
N31 Ni2 S27 C26 -172.4(3) . . . . ?
N21 Ni2 S27 C26 11.5(3) . . . . ?
O46 Ni2 S27 C26 -69.0(5) . . . . ?
O47 Ni2 S27 C26 -78.8(3) . . . . ?
S37 Ni2 S27 C26 102.3(3) . . . . ?
N21 Ni2 N31 C32 148(3) . . . . ?
O46 Ni2 N31 C32 -101.8(8) . . . . ?
O47 Ni2 N31 C32 -42.2(8) . . . . ?
S37 Ni2 N31 C32 162.4(8) . . . . ?
S27 Ni2 N31 C32 57.9(8) . . . . ?
N21 Ni2 N31 N35 -27(4) . . . . ?
O46 Ni2 N31 N35 82.8(5) . . . . ?
O47 Ni2 N31 N35 142.3(5) . . . . ?
S37 Ni2 N31 N35 -13.0(4) . . . . ?
S27 Ni2 N31 N35 -117.6(4) . . . . ?
N35 N31 C32 C33 -0.6(8) . . . . ?
Ni2 N31 C32 C33 -176.4(6) . . . . ?
N35 N31 C32 C29 177.2(7) . . . . ?
Ni2 N31 C32 C29 1.4(13) . . . . ?
N31 C32 C33 C34 0.4(10) . . . . ?
C29 C32 C33 C34 -177.2(8) . . . . ?
C32 C33 C34 N35 0.1(10) . . . . ?
C32 C33 C34 C44 171.3(9) . . . . ?
C33 C34 N35 N31 -0.5(9) . . . . ?
C44 C34 N35 N31 -172.3(8) . . . . ?
C33 C34 N35 C36 177.7(8) . . . . ?
C44 C34 N35 C36 5.8(13) . . . . ?
C32 N31 N35 C34 0.7(8) . . . . ?
Ni2 N31 N35 C34 177.6(5) . . . . ?
C32 N31 N35 C36 -177.7(7) . . . . ?
Ni2 N31 N35 C36 -0.8(8) . . . . ?
C34 N35 C36 N40 24.4(12) . . . . ?
N31 N35 C36 N40 -157.6(7) . . . . ?
C34 N35 C36 S37 -155.3(7) . . . . ?
N31 N35 C36 S37 22.7(9) . . . . ?
N40 C36 S37 Ni2 152.7(7) . . . . ?
N35 C36 S37 Ni2 -27.6(6) . . . . ?
N31 Ni2 S37 C36 19.7(3) . . . . ?
N21 Ni2 S37 C36 -161.3(3) . . . . ?
O46 Ni2 S37 C36 -68.1(3) . . . . ?
O47 Ni2 S37 C36 -62.4(5) . . . . ?
S27 Ni2 S37 C36 115.0(3) . . . . ?
O48 N45 O46 Ni2 175.9(6) . . . . ?
O47 N45 O46 Ni2 -2.8(6) . . . . ?
N31 Ni2 O46 N45 95.5(4) . . . . ?
N21 Ni2 O46 N45 -88.2(4) . . . . ?
O47 Ni2 O46 N45 1.7(4) . . . . ?
S37 Ni2 O46 N45 178.9(4) . . . . ?
S27 Ni2 O46 N45 -9.5(7) . . . . ?
O48 N45 O47 Ni2 -175.9(6) . . . . ?
O46 N45 O47 Ni2 2.8(6) . . . . ?
N31 Ni2 O47 N45 -88.4(4) . . . . ?
N21 Ni2 O47 N45 90.9(4) . . . . ?
O46 Ni2 O47 N45 -1.7(4) . . . . ?
S37 Ni2 O47 N45 -8.2(6) . . . . ?
S27 Ni2 O47 N45 174.3(4) . . . . ?
C81 C82 O83 C84 -177.5(19) . . . . ?
C82 O83 C84 C85 179(2) . . . . ?
C71 C72 O73 C74 -177(3) . . . . ?
C72 O73 C74 C75 -178(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.460
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.107

_database_code_depnum_ccdc_archive 'CCDC 988741'
