# 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_1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C27 H23 Cu N3 O4 S'
_chemical_formula_weight         549.08

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2/c

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                   26.919(5)
_cell_length_b                   8.7230(17)
_cell_length_c                   22.424(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.99(3)
_cell_angle_gamma                90.00
_cell_volume                     5008.2(17)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5898
_cell_measurement_theta_min      1.9097
_cell_measurement_theta_max      27.9064

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2264
_exptl_absorpt_coefficient_mu    0.994
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5334
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   CrystalClear


_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16212
_diffrn_reflns_av_R_equivalents  0.0919
_diffrn_reflns_av_unetI/netI     0.1007
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.91
_diffrn_reflns_theta_max         25.01
_reflns_number_total             4419
_reflns_number_gt                2681
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0495P)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       0.00060(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4419
_refine_ls_number_parameters     326
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_gt           0.0567
_refine_ls_wR_factor_ref         0.1274
_refine_ls_wR_factor_gt          0.1150
_refine_ls_goodness_of_fit_ref   0.922
_refine_ls_restrained_S_all      0.922
_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
Cu1 Cu 0.857641(17) 0.21839(6) 0.87079(2) 0.0414(2) Uani 1 1 d . . .
N1 N 0.82178(12) 0.1373(4) 0.94343(17) 0.0442(10) Uani 1 1 d . . .
N2 N 0.82831(12) 0.0143(4) 0.83436(15) 0.0417(9) Uani 1 1 d . . .
N3 N 0.92850(12) 0.1115(4) 0.89534(14) 0.0370(9) Uani 1 1 d . . .
C1 C 0.78114(16) -0.0195(5) 0.8538(2) 0.0555(13) Uani 1 1 d . . .
H1A H 0.7516 0.0371 0.8271 0.067 Uiso 1 1 calc R . .
H1B H 0.7731 -0.1280 0.8481 0.067 Uiso 1 1 calc R . .
C2 C 0.78904(16) 0.0223(6) 0.9203(2) 0.0493(12) Uani 1 1 d . . .
C3 C 0.76061(17) -0.0540(6) 0.9555(3) 0.0638(15) Uani 1 1 d . . .
H3 H 0.7391 -0.1368 0.9384 0.077 Uiso 1 1 calc R . .
C4 C 0.76536(18) -0.0041(7) 1.0145(3) 0.0662(16) Uani 1 1 d . . .
H4 H 0.7470 -0.0530 1.0379 0.079 Uiso 1 1 calc R . .
C5 C 0.79821(17) 0.1222(6) 1.0405(2) 0.0536(13) Uani 1 1 d . . .
C6 C 0.80408(19) 0.1852(7) 1.1001(2) 0.0667(16) Uani 1 1 d . . .
H6 H 0.7853 0.1445 1.1249 0.080 Uiso 1 1 calc R . .
C7 C 0.8366(2) 0.3032(7) 1.1213(2) 0.0681(16) Uani 1 1 d . . .
H7 H 0.8404 0.3426 1.1610 0.082 Uiso 1 1 calc R . .
C8 C 0.86478(17) 0.3682(6) 1.0851(2) 0.0615(14) Uani 1 1 d . . .
H8 H 0.8873 0.4496 1.1010 0.074 Uiso 1 1 calc R . .
C9 C 0.85962(16) 0.3134(6) 1.0262(2) 0.0515(13) Uani 1 1 d . . .
H9 H 0.8781 0.3586 1.0020 0.062 Uiso 1 1 calc R . .
C10 C 0.82688(15) 0.1904(5) 1.0030(2) 0.0456(12) Uani 1 1 d . . .
C11 C 0.86857(15) -0.1034(5) 0.86317(19) 0.0482(12) Uani 1 1 d . . .
H11A H 0.8671 -0.1836 0.8327 0.058 Uiso 1 1 calc R . .
H11B H 0.8606 -0.1494 0.8985 0.058 Uiso 1 1 calc R . .
C12 C 0.92299(16) -0.0388(5) 0.88515(18) 0.0410(11) Uani 1 1 d . . .
C13 C 0.96596(17) -0.1409(5) 0.8974(2) 0.0511(12) Uani 1 1 d . . .
H13 H 0.9606 -0.2447 0.8881 0.061 Uiso 1 1 calc R . .
C14 C 1.01468(17) -0.0855(6) 0.9228(2) 0.0549(13) Uani 1 1 d . . .
H14 H 1.0430 -0.1519 0.9318 0.066 Uiso 1 1 calc R . .
C15 C 1.02312(16) 0.0716(6) 0.93592(19) 0.0444(12) Uani 1 1 d . . .
C16 C 1.07304(16) 0.1342(6) 0.9628(2) 0.0550(14) Uani 1 1 d . . .
H16 H 1.1022 0.0707 0.9723 0.066 Uiso 1 1 calc R . .
C17 C 1.07914(18) 0.2875(7) 0.9751(2) 0.0595(14) Uani 1 1 d . . .
H17 H 1.1123 0.3279 0.9938 0.071 Uiso 1 1 calc R . .
C18 C 1.03538(17) 0.3834(6) 0.9592(2) 0.0597(14) Uani 1 1 d . . .
H18 H 1.0398 0.4881 0.9668 0.072 Uiso 1 1 calc R . .
C19 C 0.98600(16) 0.3259(5) 0.9327(2) 0.0477(12) Uani 1 1 d . . .
H19 H 0.9573 0.3911 0.9225 0.057 Uiso 1 1 calc R . .
C20 C 0.97920(15) 0.1691(5) 0.92124(18) 0.0386(11) Uani 1 1 d . . .
C21 C 0.81343(17) 0.0122(6) 0.76377(19) 0.0607(14) Uani 1 1 d . . .
H21A H 0.8050 -0.0921 0.7491 0.073 Uiso 1 1 calc R . .
H21B H 0.7823 0.0740 0.7467 0.073 Uiso 1 1 calc R . .
C22 C 0.85600(19) 0.0719(6) 0.7393(2) 0.0542(13) Uani 1 1 d . . .
C23 C 0.8940(2) -0.0240(7) 0.7296(2) 0.0681(16) Uani 1 1 d . . .
H23 H 0.8935 -0.1283 0.7381 0.082 Uiso 1 1 calc R . .
C24 C 0.9326(2) 0.0344(9) 0.7076(3) 0.089(2) Uani 1 1 d . . .
H24 H 0.9581 -0.0310 0.7021 0.106 Uiso 1 1 calc R . .
C25 C 0.9340(3) 0.1836(11) 0.6939(3) 0.109(3) Uani 1 1 d . . .
H25 H 0.9600 0.2208 0.6784 0.131 Uiso 1 1 calc R . .
C26 C 0.8972(3) 0.2805(9) 0.7027(3) 0.101(2) Uani 1 1 d . . .
H26 H 0.8985 0.3844 0.6939 0.121 Uiso 1 1 calc R . .
C27 C 0.8579(2) 0.2247(7) 0.7248(2) 0.0732(17) Uani 1 1 d . . .
H27 H 0.8325 0.2913 0.7299 0.088 Uiso 1 1 calc R . .
S1 S 0.82262(4) 0.49385(14) 0.84289(5) 0.0462(3) Uani 1 1 d . . .
O1 O 0.87504(10) 0.4384(3) 0.88510(13) 0.0519(8) Uani 1 1 d . . .
O2 O 0.79475(10) 0.3420(3) 0.82425(13) 0.0508(8) Uani 1 1 d . . .
O3 O 0.82887(12) 0.5710(4) 0.78863(14) 0.0661(10) Uani 1 1 d . . .
O4 O 0.79691(11) 0.5873(4) 0.87784(15) 0.0633(9) 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 O1 1.978(3) . ?
Cu1 O2 2.007(3) . ?
Cu1 N2 2.015(3) . ?
Cu1 N3 2.040(3) . ?
Cu1 N1 2.249(4) . ?
N1 C2 1.330(5) . ?
N1 C10 1.381(5) . ?
N2 C11 1.488(5) . ?
N2 C1 1.493(5) . ?
N2 C21 1.508(5) . ?
N3 C12 1.331(5) . ?
N3 C20 1.401(5) . ?
C1 C2 1.485(6) . ?
C2 C3 1.423(6) . ?
C3 C4 1.362(6) . ?
C4 C5 1.420(7) . ?
C5 C6 1.408(7) . ?
C5 C10 1.433(6) . ?
C6 C7 1.340(7) . ?
C7 C8 1.392(6) . ?
C8 C9 1.370(6) . ?
C9 C10 1.384(6) . ?
C11 C12 1.503(5) . ?
C12 C13 1.418(5) . ?
C13 C14 1.348(6) . ?
C14 C15 1.405(6) . ?
C15 C16 1.402(6) . ?
C15 C20 1.410(5) . ?
C16 C17 1.365(6) . ?
C17 C18 1.399(6) . ?
C18 C19 1.373(5) . ?
C19 C20 1.393(6) . ?
C21 C22 1.508(6) . ?
C22 C27 1.376(7) . ?
C22 C23 1.390(6) . ?
C23 C24 1.377(7) . ?
C24 C25 1.341(9) . ?
C25 C26 1.361(9) . ?
C26 C27 1.390(7) . ?
S1 O3 1.445(3) . ?
S1 O4 1.447(3) . ?
S1 O1 1.515(3) . ?
S1 O2 1.516(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
O1 Cu1 O2 71.48(11) . . ?
O1 Cu1 N2 165.08(12) . . ?
O2 Cu1 N2 95.85(12) . . ?
O1 Cu1 N3 104.17(13) . . ?
O2 Cu1 N3 162.60(13) . . ?
N2 Cu1 N3 85.54(13) . . ?
O1 Cu1 N1 108.72(13) . . ?
O2 Cu1 N1 93.67(12) . . ?
N2 Cu1 N1 79.25(14) . . ?
N3 Cu1 N1 103.62(13) . . ?
C2 N1 C10 119.1(4) . . ?
C2 N1 Cu1 109.6(3) . . ?
C10 N1 Cu1 131.2(3) . . ?
C11 N2 C1 107.9(3) . . ?
C11 N2 C21 111.7(3) . . ?
C1 N2 C21 109.2(3) . . ?
C11 N2 Cu1 107.0(2) . . ?
C1 N2 Cu1 108.6(3) . . ?
C21 N2 Cu1 112.3(3) . . ?
C12 N3 C20 117.9(3) . . ?
C12 N3 Cu1 111.0(3) . . ?
C20 N3 Cu1 131.1(3) . . ?
C2 C1 N2 111.9(3) . . ?
N1 C2 C3 122.8(5) . . ?
N1 C2 C1 116.7(4) . . ?
C3 C2 C1 120.5(5) . . ?
C4 C3 C2 118.9(5) . . ?
C3 C4 C5 120.5(5) . . ?
C6 C5 C4 124.4(5) . . ?
C6 C5 C10 118.1(5) . . ?
C4 C5 C10 117.4(5) . . ?
C7 C6 C5 120.4(5) . . ?
C6 C7 C8 121.3(5) . . ?
C9 C8 C7 120.5(5) . . ?
C8 C9 C10 119.8(5) . . ?
N1 C10 C9 119.0(4) . . ?
N1 C10 C5 121.2(4) . . ?
C9 C10 C5 119.8(5) . . ?
N2 C11 C12 112.9(4) . . ?
N3 C12 C13 123.0(4) . . ?
N3 C12 C11 118.1(4) . . ?
C13 C12 C11 118.8(4) . . ?
C14 C13 C12 119.0(4) . . ?
C13 C14 C15 120.8(4) . . ?
C16 C15 C14 122.8(4) . . ?
C16 C15 C20 119.2(5) . . ?
C14 C15 C20 118.0(4) . . ?
C17 C16 C15 120.5(4) . . ?
C16 C17 C18 119.7(4) . . ?
C19 C18 C17 121.2(5) . . ?
C18 C19 C20 119.6(4) . . ?
C19 C20 N3 119.0(4) . . ?
C19 C20 C15 119.7(4) . . ?
N3 C20 C15 121.3(4) . . ?
C22 C21 N2 113.1(3) . . ?
C27 C22 C23 117.6(5) . . ?
C27 C22 C21 120.5(5) . . ?
C23 C22 C21 121.9(5) . . ?
C24 C23 C22 120.4(6) . . ?
C25 C24 C23 121.3(7) . . ?
C24 C25 C26 119.8(7) . . ?
C25 C26 C27 120.1(7) . . ?
C22 C27 C26 120.8(6) . . ?
O3 S1 O4 113.2(2) . . ?
O3 S1 O1 110.27(19) . . ?
O4 S1 O1 110.53(18) . . ?
O3 S1 O2 110.55(19) . . ?
O4 S1 O2 111.28(18) . . ?
O1 S1 O2 100.34(16) . . ?
S1 O1 Cu1 94.61(14) . . ?
S1 O2 Cu1 93.43(13) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.561
_refine_diff_density_min         -0.718
_refine_diff_density_rms         0.079
_database_code_depnum_ccdc_archive 'CCDC 1028398'
#######################################################################
#
#                 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_2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C29 H33 N3 Ni O7 S'
_chemical_formula_weight         626.35

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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   14.759(3)
_cell_length_b                   13.805(3)
_cell_length_c                   14.772(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.14(3)
_cell_angle_gamma                90.00
_cell_volume                     2992.4(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    113(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      6.169141
_cell_measurement_theta_max      54.96809

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1312
_exptl_absorpt_coefficient_mu    0.768
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3251
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   CrystalClear

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      113(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'fine-focus sealed tube'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            29820
_diffrn_reflns_av_R_equivalents  0.0728
_diffrn_reflns_av_unetI/netI     0.0384
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.03
_diffrn_reflns_theta_max         25.01
_reflns_number_total             5253
_reflns_number_gt                4685
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0592P)²+2.3124P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5253
_refine_ls_number_parameters     381
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0448
_refine_ls_wR_factor_ref         0.1066
_refine_ls_wR_factor_gt          0.1036
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.039
_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
C28 C 0.5563(6) 0.6949(7) 0.3429(5) 0.201(5) Uani 1 1 d . . .
H28A H 0.5182 0.7187 0.2909 0.301 Uiso 1 1 calc R . .
H28B H 0.5939 0.7465 0.3692 0.301 Uiso 1 1 calc R . .
H28C H 0.5188 0.6707 0.3872 0.301 Uiso 1 1 calc R . .
Ni1 Ni 0.70689(2) 0.58024(2) 0.033010(19) 0.02064(11) Uani 1 1 d . . .
N1 N 0.81344(14) 0.51761(15) -0.03291(13) 0.0247(5) Uani 1 1 d . . .
N2 N 0.75689(13) 0.70887(14) -0.02143(14) 0.0230(4) Uani 1 1 d . . .
N3 N 0.79262(13) 0.63397(14) 0.14461(13) 0.0212(4) Uani 1 1 d . . .
O1 O 0.61853(12) 0.54424(14) -0.07946(12) 0.0261(4) Uani 1 1 d . . .
H1 H 0.5695 0.5714 -0.0766 0.039 Uiso 1 1 calc R . .
O2 O 0.65688(13) 0.46913(13) 0.10706(13) 0.0284(4) Uani 1 1 d . . .
H2 H 0.6169 0.4401 0.0751 0.043 Uiso 1 1 calc R . .
C1 C 0.85100(17) 0.68886(18) -0.04273(18) 0.0277(6) Uani 1 1 d . . .
H1A H 0.8935 0.7079 0.0089 0.033 Uiso 1 1 calc R . .
H1B H 0.8635 0.7281 -0.0944 0.033 Uiso 1 1 calc R . .
C2 C 0.86679(17) 0.58381(18) -0.06430(18) 0.0278(6) Uani 1 1 d . . .
C3 C 0.9399(2) 0.5604(2) -0.1138(3) 0.0487(8) Uani 1 1 d . . .
H3 H 0.9766 0.6091 -0.1336 0.058 Uiso 1 1 calc R . .
C4 C 0.9565(2) 0.4669(3) -0.1326(3) 0.0600(10) Uani 1 1 d . . .
H4 H 1.0043 0.4510 -0.1661 0.072 Uiso 1 1 calc R . .
C5 C 0.90212(18) 0.3937(2) -0.1019(2) 0.0393(7) Uani 1 1 d . . .
C6 C 0.9156(2) 0.2944(2) -0.1199(3) 0.0516(9) Uani 1 1 d . . .
H6 H 0.9637 0.2758 -0.1520 0.062 Uiso 1 1 calc R . .
C7 C 0.8592(2) 0.2257(2) -0.0908(3) 0.0535(9) Uani 1 1 d . . .
H7 H 0.8690 0.1605 -0.1024 0.064 Uiso 1 1 calc R . .
C8 C 0.7864(2) 0.2537(2) -0.0433(2) 0.0518(9) Uani 1 1 d . . .
H8 H 0.7473 0.2067 -0.0246 0.062 Uiso 1 1 calc R . .
C9 C 0.7717(2) 0.3489(2) -0.0238(2) 0.0401(7) Uani 1 1 d . . .
H9 H 0.7231 0.3658 0.0081 0.048 Uiso 1 1 calc R . .
C10 C 0.82948(17) 0.42099(18) -0.05177(18) 0.0279(6) Uani 1 1 d . . .
C11 C 0.75933(17) 0.77871(17) 0.05479(17) 0.0252(5) Uani 1 1 d . . .
H11A H 0.6983 0.8026 0.0603 0.030 Uiso 1 1 calc R . .
H11B H 0.7975 0.8335 0.0429 0.030 Uiso 1 1 calc R . .
C12 C 0.79664(16) 0.72992(17) 0.14214(17) 0.0239(5) Uani 1 1 d . . .
C13 C 0.83427(18) 0.78578(19) 0.21672(18) 0.0322(6) Uani 1 1 d . . .
H13 H 0.8357 0.8530 0.2127 0.039 Uiso 1 1 calc R . .
C14 C 0.86836(19) 0.7405(2) 0.29430(19) 0.0352(6) Uani 1 1 d . . .
H14 H 0.8915 0.7767 0.3446 0.042 Uiso 1 1 calc R . .
C15 C 0.86885(17) 0.63839(19) 0.29884(17) 0.0287(6) Uani 1 1 d . . .
C16 C 0.90921(19) 0.5871(2) 0.37564(19) 0.0354(6) Uani 1 1 d . . .
H16 H 0.9324 0.6208 0.4275 0.042 Uiso 1 1 calc R . .
C17 C 0.91428(19) 0.4885(2) 0.37405(19) 0.0371(6) Uani 1 1 d . . .
H17 H 0.9421 0.4554 0.4244 0.045 Uiso 1 1 calc R . .
C18 C 0.87771(17) 0.43657(19) 0.29666(18) 0.0302(6) Uani 1 1 d . . .
H18 H 0.8818 0.3694 0.2962 0.036 Uiso 1 1 calc R . .
C19 C 0.83623(16) 0.48409(18) 0.22209(17) 0.0254(5) Uani 1 1 d . . .
H19 H 0.8114 0.4490 0.1717 0.030 Uiso 1 1 calc R . .
C20 C 0.83100(15) 0.58593(17) 0.22133(16) 0.0220(5) Uani 1 1 d . . .
C21 C 0.69599(17) 0.74164(19) -0.10362(17) 0.0279(6) Uani 1 1 d . . .
H21A H 0.6333 0.7363 -0.0901 0.033 Uiso 1 1 calc R . .
H21B H 0.7037 0.6974 -0.1532 0.033 Uiso 1 1 calc R . .
C22 C 0.71109(17) 0.84352(19) -0.13615(17) 0.0283(6) Uani 1 1 d . . .
C23 C 0.7713(2) 0.8646(2) -0.19972(19) 0.0416(7) Uani 1 1 d . . .
H23 H 0.8047 0.8152 -0.2232 0.050 Uiso 1 1 calc R . .
C24 C 0.7816(2) 0.9602(3) -0.2284(2) 0.0563(10) Uani 1 1 d . . .
H24 H 0.8231 0.9744 -0.2697 0.068 Uiso 1 1 calc R . .
C25 C 0.7306(3) 1.0334(3) -0.1958(2) 0.0593(10) Uani 1 1 d . . .
H25 H 0.7374 1.0966 -0.2157 0.071 Uiso 1 1 calc R . .
C26 C 0.6699(3) 1.0133(2) -0.1342(2) 0.0544(9) Uani 1 1 d . . .
H26 H 0.6355 1.0627 -0.1121 0.065 Uiso 1 1 calc R . .
C27 C 0.6603(2) 0.9190(2) -0.1053(2) 0.0387(7) Uani 1 1 d . . .
H27 H 0.6186 0.9057 -0.0639 0.046 Uiso 1 1 calc R . .
S1 S 0.50504(4) 0.68337(4) 0.06030(4) 0.02196(15) Uani 1 1 d . . .
O3 O 0.60371(11) 0.66486(13) 0.08207(11) 0.0269(4) Uani 1 1 d . . .
O4 O 0.47644(11) 0.64426(12) -0.03247(11) 0.0266(4) Uani 1 1 d . . .
O5 O 0.45535(12) 0.62971(13) 0.12660(12) 0.0305(4) Uani 1 1 d . . .
O6 O 0.48678(14) 0.78632(13) 0.06358(14) 0.0398(5) Uani 1 1 d . . .
H31 H 0.638(2) 0.492(2) 0.149(2) 0.039(10) Uiso 1 1 d . . .
H30 H 0.608(2) 0.486(3) -0.090(2) 0.043(9) Uiso 1 1 d . . .
O7 O 0.57554(17) 0.53786(19) 0.25475(15) 0.0590(7) Uani 1 1 d . . .
H7A H 0.5520 0.5625 0.2075 0.088 Uiso 1 1 calc R . .
C29 C 0.6176(3) 0.6118(6) 0.3129(4) 0.142(3) Uani 1 1 d . . .
H29A H 0.6657 0.6409 0.2822 0.170 Uiso 1 1 calc R . .
H29B H 0.6463 0.5807 0.3675 0.170 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
C28 C29 1.555(8) . ?
Ni1 O1 2.0603(18) . ?
Ni1 O2 2.0656(18) . ?
Ni1 N3 2.103(2) . ?
Ni1 O3 2.1082(18) . ?
Ni1 N2 2.115(2) . ?
Ni1 N1 2.121(2) . ?
N1 C2 1.322(3) . ?
N1 C10 1.388(3) . ?
N2 C11 1.480(3) . ?
N2 C1 1.483(3) . ?
N2 C21 1.501(3) . ?
N3 C12 1.327(3) . ?
N3 C20 1.381(3) . ?
C1 C2 1.508(4) . ?
C2 C3 1.404(4) . ?
C3 C4 1.349(5) . ?
C4 C5 1.395(5) . ?
C5 C6 1.415(4) . ?
C5 C10 1.417(4) . ?
C6 C7 1.363(5) . ?
C7 C8 1.399(5) . ?
C8 C9 1.367(4) . ?
C9 C10 1.402(4) . ?
C11 C12 1.507(3) . ?
C12 C13 1.409(4) . ?
C13 C14 1.354(4) . ?
C14 C15 1.411(4) . ?
C15 C16 1.414(4) . ?
C15 C20 1.418(3) . ?
C16 C17 1.363(4) . ?
C17 C18 1.408(4) . ?
C18 C19 1.369(4) . ?
C19 C20 1.408(3) . ?
C21 C22 1.510(3) . ?
C22 C27 1.389(4) . ?
C22 C23 1.391(4) . ?
C23 C24 1.400(5) . ?
C24 C25 1.376(5) . ?
C25 C26 1.372(5) . ?
C26 C27 1.382(4) . ?
S1 O6 1.4483(19) . ?
S1 O3 1.4796(18) . ?
S1 O5 1.4830(18) . ?
S1 O4 1.4914(17) . ?
O7 C29 1.433(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
O1 Ni1 O2 90.96(7) . . ?
O1 Ni1 N3 173.27(8) . . ?
O2 Ni1 N3 93.78(7) . . ?
O1 Ni1 O3 89.58(7) . . ?
O2 Ni1 O3 85.26(8) . . ?
N3 Ni1 O3 86.06(7) . . ?
O1 Ni1 N2 96.45(8) . . ?
O2 Ni1 N2 169.73(8) . . ?
N3 Ni1 N2 78.27(8) . . ?
O3 Ni1 N2 87.69(8) . . ?
O1 Ni1 N1 88.16(8) . . ?
O2 Ni1 N1 105.36(8) . . ?
N3 Ni1 N1 95.18(8) . . ?
O3 Ni1 N1 169.17(7) . . ?
N2 Ni1 N1 82.05(8) . . ?
C2 N1 C10 118.2(2) . . ?
C2 N1 Ni1 112.19(17) . . ?
C10 N1 Ni1 129.40(17) . . ?
C11 N2 C1 109.61(19) . . ?
C11 N2 C21 112.51(19) . . ?
C1 N2 C21 112.21(19) . . ?
C11 N2 Ni1 103.82(14) . . ?
C1 N2 Ni1 107.29(14) . . ?
C21 N2 Ni1 110.95(14) . . ?
C12 N3 C20 119.1(2) . . ?
C12 N3 Ni1 110.82(15) . . ?
C20 N3 Ni1 129.30(15) . . ?
N2 C1 C2 113.16(19) . . ?
N1 C2 C3 122.9(2) . . ?
N1 C2 C1 118.6(2) . . ?
C3 C2 C1 118.4(2) . . ?
C4 C3 C2 119.6(3) . . ?
C3 C4 C5 120.2(3) . . ?
C4 C5 C6 122.8(3) . . ?
C4 C5 C10 118.1(3) . . ?
C6 C5 C10 119.0(3) . . ?
C7 C6 C5 120.8(3) . . ?
C6 C7 C8 119.6(3) . . ?
C9 C8 C7 121.2(3) . . ?
C8 C9 C10 120.4(3) . . ?
N1 C10 C9 120.1(2) . . ?
N1 C10 C5 121.0(2) . . ?
C9 C10 C5 118.9(2) . . ?
N2 C11 C12 109.72(19) . . ?
N3 C12 C13 122.7(2) . . ?
N3 C12 C11 117.2(2) . . ?
C13 C12 C11 120.2(2) . . ?
C14 C13 C12 119.2(2) . . ?
C13 C14 C15 120.1(2) . . ?
C14 C15 C16 122.5(2) . . ?
C14 C15 C20 118.2(2) . . ?
C16 C15 C20 119.2(2) . . ?
C17 C16 C15 120.3(3) . . ?
C16 C17 C18 120.4(2) . . ?
C19 C18 C17 120.6(2) . . ?
C18 C19 C20 120.3(2) . . ?
N3 C20 C19 120.2(2) . . ?
N3 C20 C15 120.6(2) . . ?
C19 C20 C15 119.1(2) . . ?
N2 C21 C22 116.2(2) . . ?
C27 C22 C23 118.1(3) . . ?
C27 C22 C21 119.4(2) . . ?
C23 C22 C21 122.4(3) . . ?
C22 C23 C24 120.0(3) . . ?
C25 C24 C23 120.4(3) . . ?
C26 C25 C24 120.2(3) . . ?
C25 C26 C27 119.5(3) . . ?
C26 C27 C22 121.9(3) . . ?
O6 S1 O3 110.15(11) . . ?
O6 S1 O5 111.18(12) . . ?
O3 S1 O5 108.35(11) . . ?
O6 S1 O4 110.53(11) . . ?
O3 S1 O4 108.21(10) . . ?
O5 S1 O4 108.34(10) . . ?
S1 O3 Ni1 138.70(10) . . ?
O7 C29 C28 117.9(4) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.592
_refine_diff_density_min         -0.661
_refine_diff_density_rms         0.067
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 85 2 ' '
2 0.951 0.146 0.729 8 0 ' '
3 0.569 0.208 0.764 7 3 ' '
4 0.069 0.292 0.264 7 3 ' '
5 0.451 0.354 0.229 8 0 ' '
6 0.500 0.500 0.500 85 2 ' '
7 0.549 0.646 0.771 8 0 ' '
8 0.931 0.708 0.736 7 3 ' '
9 0.431 0.792 0.236 7 3 ' '
10 0.049 0.854 0.271 8 0 ' '
_platon_squeeze_details          
;
;
_database_code_depnum_ccdc_archive 'CCDC 1028399'
