Supplementary Material (ESI) for Dalton Transactions
This journal is © The Royal Society of Chemistry 2010

data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Jie Dai'
_publ_contact_author_email       DAIJIE@SUDA.EDU.CN

_publ_section_title              
;
Cu(II) and Ni(II) dioxotetraamine complexes
integrated with tetrathiafulvalene moiety, structures and
solution chemistry
;
loop_
_publ_author_name
'Jie Dai'
'Li-Bin Huo'
'Zhe-Jun Lu'
'Yu-Rong Qin'
'Jin-Po Wang'
;
Qin-Yu Zhu
;

# Attachment 'CIF1-4.CIF'

data_l
_database_code_depnum_ccdc_archive 'CCDC 750340'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C17 H25 Cu N5 O3 S6'
_chemical_formula_weight         603.32

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'
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'
O O 0.0106 0.0060 '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/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   8.6930(10)
_cell_length_b                   20.337(2)
_cell_length_c                   14.2013(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.016(3)
_cell_angle_gamma                90.00
_cell_volume                     2509.1(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1244
_exptl_absorpt_coefficient_mu    1.399
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4873
_exptl_absorpt_correction_T_max  0.8500
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      223(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean 14.63
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15276
_diffrn_reflns_av_R_equivalents  0.0665
_diffrn_reflns_av_sigmaI/netI    0.0657
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.04
_diffrn_reflns_theta_max         25.50
_reflns_number_total             4651
_reflns_number_gt                3876
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0485P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/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         4651
_refine_ls_number_parameters     297
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0484
_refine_ls_wR_factor_ref         0.1151
_refine_ls_wR_factor_gt          0.1071
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.034
_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 0.36846(6) 0.66027(2) 0.50070(3) 0.02859(15) Uani 1 1 d . . .
S1 S 0.56249(12) 0.51180(4) 0.23697(6) 0.0314(2) Uani 1 1 d . . .
S2 S 0.37375(13) 0.61310(4) 0.14472(6) 0.0310(2) Uani 1 1 d . . .
S3 S 0.45001(13) 0.40393(5) 0.08922(6) 0.0345(3) Uani 1 1 d . . .
S4 S 0.24130(12) 0.49661(4) -0.00878(6) 0.0324(2) Uani 1 1 d . . .
S5 S 0.29822(15) 0.28393(5) 0.00619(7) 0.0410(3) Uani 1 1 d . . .
S6 S 0.04993(13) 0.39462(5) -0.10529(7) 0.0394(3) Uani 1 1 d . . .
O1 O 0.6969(4) 0.52870(14) 0.40363(17) 0.0408(7) Uani 1 1 d . . .
O2 O 0.3620(4) 0.73383(12) 0.22429(17) 0.0412(7) Uani 1 1 d . . .
O3 O 0.1908(4) 0.57265(16) 0.4934(2) 0.0525(9) Uani 1 1 d . . .
H3A H 0.228(7) 0.542(2) 0.520(4) 0.066(18) Uiso 1 1 d . . .
N2 N 0.4278(4) 0.63966(15) 0.6364(2) 0.0359(8) Uani 1 1 d . . .
H2B H 0.3948 0.6719 0.6753 0.043 Uiso 1 1 calc R . .
H2A H 0.3861 0.6007 0.6541 0.043 Uiso 1 1 calc R . .
N4 N 0.2064(4) 0.72383(16) 0.5462(2) 0.0379(8) Uani 1 1 d . . .
H4B H 0.1338 0.7015 0.5780 0.046 Uiso 1 1 calc R . .
H4A H 0.2509 0.7540 0.5859 0.046 Uiso 1 1 calc R . .
N1 N 0.5559(4) 0.60856(14) 0.47491(19) 0.0285(7) Uani 1 1 d . . .
N3 N 0.3305(4) 0.70424(15) 0.3788(2) 0.0310(7) Uani 1 1 d . . .
N5 N 0.0120(8) 0.3418(4) 0.3121(4) 0.118(3) Uani 1 1 d . . .
C11 C 0.5973(5) 0.6359(2) 0.6401(2) 0.0380(10) Uani 1 1 d . . .
H11B H 0.6340 0.6181 0.7009 0.046 Uiso 1 1 calc R . .
H11A H 0.6415 0.6798 0.6325 0.046 Uiso 1 1 calc R . .
C10 C 0.6447(5) 0.59175(19) 0.5616(2) 0.0340(9) Uani 1 1 d . . .
H10B H 0.7550 0.5971 0.5515 0.041 Uiso 1 1 calc R . .
H10A H 0.6261 0.5458 0.5784 0.041 Uiso 1 1 calc R . .
C14 C 0.1347(6) 0.7572(2) 0.4640(3) 0.0454(11) Uani 1 1 d . . .
H14B H 0.0907 0.7993 0.4829 0.055 Uiso 1 1 calc R . .
H14A H 0.0518 0.7299 0.4362 0.055 Uiso 1 1 calc R . .
C13 C 0.2563(6) 0.7681(2) 0.3940(3) 0.0452(12) Uani 1 1 d . . .
H13B H 0.2104 0.7848 0.3347 0.054 Uiso 1 1 calc R . .
H13A H 0.3319 0.8002 0.4182 0.054 Uiso 1 1 calc R . .
C9 C 0.5938(4) 0.57256(18) 0.4027(2) 0.0271(8) Uani 1 1 d . . .
C1 C 0.5117(4) 0.57971(17) 0.3075(2) 0.0262(8) Uani 1 1 d . . .
C2 C 0.4258(4) 0.62675(16) 0.2647(2) 0.0245(8) Uani 1 1 d . . .
C12 C 0.3725(5) 0.69357(17) 0.2924(2) 0.0280(9) Uani 1 1 d . . .
C3 C 0.4250(5) 0.52969(17) 0.1473(2) 0.0296(9) Uani 1 1 d . . .
C4 C 0.3743(5) 0.48420(17) 0.0858(2) 0.0285(8) Uani 1 1 d . . .
C5 C 0.3001(5) 0.36999(18) 0.0185(2) 0.0326(9) Uani 1 1 d . . .
C6 C 0.2069(5) 0.41202(18) -0.0276(2) 0.0303(9) Uani 1 1 d . . .
C7 C 0.2809(6) 0.2580(2) 0.1270(3) 0.0443(11) Uani 1 1 d . . .
H7C H 0.3660 0.2756 0.1651 0.066 Uiso 1 1 calc R . .
H7B H 0.2827 0.2103 0.1301 0.066 Uiso 1 1 calc R . .
H7A H 0.1845 0.2740 0.1507 0.066 Uiso 1 1 calc R . .
C8 C 0.1370(7) 0.3479(2) -0.1985(3) 0.0572(14) Uani 1 1 d . . .
H8C H 0.2188 0.3735 -0.2252 0.086 Uiso 1 1 calc R . .
H8B H 0.0596 0.3378 -0.2472 0.086 Uiso 1 1 calc R . .
H8A H 0.1791 0.3072 -0.1727 0.086 Uiso 1 1 calc R . .
C15 C 0.0968(7) 0.5591(2) 0.4139(4) 0.0684(17) Uani 1 1 d . . .
H15A H 0.0154 0.5917 0.4085 0.103 Uiso 1 1 calc R . .
H15B H 0.0518 0.5157 0.4200 0.103 Uiso 1 1 calc R . .
H15C H 0.1578 0.5605 0.3581 0.103 Uiso 1 1 calc R . .
C16 C 0.0019(12) 0.4440(4) 0.2101(6) 0.125(3) Uani 1 1 d . . .
C17 C 0.0030(8) 0.3871(3) 0.2666(4) 0.0758(18) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0367(3) 0.0282(3) 0.0209(2) -0.00141(17) 0.00158(19) 0.0021(2)
S1 0.0413(6) 0.0294(5) 0.0231(4) -0.0023(3) -0.0024(4) 0.0071(4)
S2 0.0451(7) 0.0269(5) 0.0204(4) -0.0020(3) -0.0058(4) 0.0034(4)
S3 0.0441(7) 0.0273(5) 0.0316(5) -0.0043(4) -0.0049(4) 0.0024(5)
S4 0.0404(6) 0.0283(5) 0.0281(5) -0.0034(4) -0.0033(4) 0.0001(4)
S5 0.0600(8) 0.0264(5) 0.0367(5) -0.0049(4) 0.0039(5) -0.0037(5)
S6 0.0390(7) 0.0417(6) 0.0371(6) -0.0055(4) -0.0031(5) -0.0058(5)
O1 0.0466(19) 0.0484(17) 0.0270(13) -0.0008(12) -0.0036(12) 0.0204(15)
O2 0.068(2) 0.0277(14) 0.0278(13) 0.0038(11) 0.0022(13) 0.0047(14)
O3 0.058(2) 0.0370(18) 0.061(2) 0.0051(15) -0.0187(18) -0.0018(17)
N2 0.051(2) 0.0326(18) 0.0241(15) 0.0013(13) 0.0045(14) 0.0056(17)
N4 0.043(2) 0.0400(19) 0.0311(17) -0.0048(14) 0.0100(15) 0.0016(16)
N1 0.035(2) 0.0303(16) 0.0197(14) -0.0006(12) -0.0011(13) 0.0039(14)
N3 0.040(2) 0.0281(16) 0.0250(16) -0.0012(12) 0.0024(14) 0.0072(15)
N5 0.103(6) 0.156(6) 0.093(4) 0.042(4) -0.007(4) -0.050(5)
C11 0.053(3) 0.041(2) 0.0196(18) 0.0003(16) -0.0043(17) -0.004(2)
C10 0.036(2) 0.041(2) 0.0247(19) 0.0032(16) -0.0039(16) 0.0030(19)
C14 0.051(3) 0.053(3) 0.032(2) -0.0064(19) -0.0026(19) 0.022(2)
C13 0.068(3) 0.036(2) 0.032(2) 0.0003(17) 0.002(2) 0.023(2)
C9 0.028(2) 0.031(2) 0.0229(18) 0.0040(14) -0.0003(15) -0.0023(18)
C1 0.031(2) 0.0265(19) 0.0217(17) -0.0048(14) 0.0035(15) -0.0016(16)
C2 0.033(2) 0.0219(18) 0.0189(16) 0.0002(13) 0.0014(15) -0.0047(16)
C12 0.035(2) 0.0263(19) 0.0226(18) -0.0007(14) -0.0035(16) -0.0021(17)
C3 0.039(2) 0.028(2) 0.0221(17) -0.0010(14) -0.0013(16) -0.0020(17)
C4 0.035(2) 0.0269(19) 0.0232(17) -0.0007(14) 0.0006(15) -0.0001(17)
C5 0.040(3) 0.033(2) 0.0249(18) -0.0054(15) 0.0040(17) -0.0034(19)
C6 0.037(2) 0.032(2) 0.0214(17) -0.0037(15) 0.0026(16) -0.0040(18)
C7 0.055(3) 0.033(2) 0.044(2) 0.0058(18) 0.003(2) 0.006(2)
C8 0.071(4) 0.062(3) 0.039(2) -0.018(2) -0.002(2) -0.002(3)
C15 0.070(4) 0.058(3) 0.075(4) 0.018(3) -0.024(3) -0.013(3)
C16 0.159(9) 0.111(6) 0.105(6) 0.036(5) -0.023(6) 0.027(6)
C17 0.062(4) 0.107(5) 0.058(4) -0.001(3) -0.001(3) -0.022(4)

_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 N3 1.966(3) . ?
Cu1 N1 1.984(3) . ?
Cu1 N2 2.022(3) . ?
Cu1 N4 2.034(3) . ?
Cu1 O3 2.358(3) . ?
S1 C3 1.754(4) . ?
S1 C1 1.771(3) . ?
S2 C3 1.754(4) . ?
S2 C2 1.770(3) . ?
S3 C5 1.759(4) . ?
S3 C4 1.760(4) . ?
S4 C4 1.759(3) . ?
S4 C6 1.765(4) . ?
S5 C5 1.759(4) . ?
S5 C7 1.807(4) . ?
S6 C6 1.760(4) . ?
S6 C8 1.816(5) . ?
O1 C9 1.264(5) . ?
O2 C12 1.268(4) . ?
O3 C15 1.398(5) . ?
O3 H3A 0.79(5) . ?
N2 C11 1.474(6) . ?
N2 H2B 0.9100 . ?
N2 H2A 0.9100 . ?
N4 C14 1.470(5) . ?
N4 H4B 0.9100 . ?
N4 H4A 0.9100 . ?
N1 C9 1.311(5) . ?
N1 C10 1.471(4) . ?
N3 C12 1.310(5) . ?
N3 C13 1.469(5) . ?
N5 C17 1.126(8) . ?
C11 C10 1.500(5) . ?
C11 H11B 0.9800 . ?
C11 H11A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10A 0.9800 . ?
C14 C13 1.493(7) . ?
C14 H14B 0.9800 . ?
C14 H14A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13A 0.9800 . ?
C9 C1 1.514(4) . ?
C1 C2 1.345(5) . ?
C2 C12 1.493(5) . ?
C3 C4 1.337(5) . ?
C5 C6 1.333(5) . ?
C7 H7C 0.9700 . ?
C7 H7B 0.9700 . ?
C7 H7A 0.9700 . ?
C8 H8C 0.9700 . ?
C8 H8B 0.9700 . ?
C8 H8A 0.9700 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 H15C 0.9700 . ?
C16 C17 1.408(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Cu1 N1 101.06(13) . . ?
N3 Cu1 N2 164.39(13) . . ?
N1 Cu1 N2 83.24(13) . . ?
N3 Cu1 N4 83.92(13) . . ?
N1 Cu1 N4 167.93(13) . . ?
N2 Cu1 N4 89.16(13) . . ?
N3 Cu1 O3 102.46(12) . . ?
N1 Cu1 O3 97.59(13) . . ?
N2 Cu1 O3 91.72(13) . . ?
N4 Cu1 O3 91.97(14) . . ?
C3 S1 C1 94.11(17) . . ?
C3 S2 C2 94.33(16) . . ?
C5 S3 C4 94.54(18) . . ?
C4 S4 C6 94.53(16) . . ?
C5 S5 C7 101.39(18) . . ?
C6 S6 C8 103.2(2) . . ?
C15 O3 Cu1 123.2(3) . . ?
C15 O3 H3A 117(4) . . ?
Cu1 O3 H3A 108(4) . . ?
C11 N2 Cu1 105.4(2) . . ?
C11 N2 H2B 110.7 . . ?
Cu1 N2 H2B 110.7 . . ?
C11 N2 H2A 110.7 . . ?
Cu1 N2 H2A 110.7 . . ?
H2B N2 H2A 108.8 . . ?
C14 N4 Cu1 108.7(2) . . ?
C14 N4 H4B 110.0 . . ?
Cu1 N4 H4B 110.0 . . ?
C14 N4 H4A 110.0 . . ?
Cu1 N4 H4A 110.0 . . ?
H4B N4 H4A 108.3 . . ?
C9 N1 C10 112.7(3) . . ?
C9 N1 Cu1 132.1(2) . . ?
C10 N1 Cu1 112.3(2) . . ?
C12 N3 C13 115.0(3) . . ?
C12 N3 Cu1 134.9(3) . . ?
C13 N3 Cu1 109.5(2) . . ?
N2 C11 C10 107.8(3) . . ?
N2 C11 H11B 110.1 . . ?
C10 C11 H11B 110.1 . . ?
N2 C11 H11A 110.1 . . ?
C10 C11 H11A 110.1 . . ?
H11B C11 H11A 108.5 . . ?
N1 C10 C11 109.4(3) . . ?
N1 C10 H10B 109.8 . . ?
C11 C10 H10B 109.8 . . ?
N1 C10 H10A 109.8 . . ?
C11 C10 H10A 109.8 . . ?
H10B C10 H10A 108.2 . . ?
N4 C14 C13 107.9(4) . . ?
N4 C14 H14B 110.1 . . ?
C13 C14 H14B 110.1 . . ?
N4 C14 H14A 110.1 . . ?
C13 C14 H14A 110.1 . . ?
H14B C14 H14A 108.4 . . ?
N3 C13 C14 106.9(3) . . ?
N3 C13 H13B 110.3 . . ?
C14 C13 H13B 110.3 . . ?
N3 C13 H13A 110.3 . . ?
C14 C13 H13A 110.3 . . ?
H13B C13 H13A 108.6 . . ?
O1 C9 N1 125.7(3) . . ?
O1 C9 C1 112.9(3) . . ?
N1 C9 C1 121.4(3) . . ?
C2 C1 C9 135.1(3) . . ?
C2 C1 S1 116.4(2) . . ?
C9 C1 S1 108.1(3) . . ?
C1 C2 C12 134.5(3) . . ?
C1 C2 S2 116.2(3) . . ?
C12 C2 S2 109.0(2) . . ?
O2 C12 N3 126.3(3) . . ?
O2 C12 C2 113.7(3) . . ?
N3 C12 C2 119.8(3) . . ?
C4 C3 S2 125.3(3) . . ?
C4 C3 S1 122.1(3) . . ?
S2 C3 S1 112.45(19) . . ?
C3 C4 S4 126.3(3) . . ?
C3 C4 S3 120.6(3) . . ?
S4 C4 S3 112.91(18) . . ?
C6 C5 S3 117.0(3) . . ?
C6 C5 S5 125.9(3) . . ?
S3 C5 S5 116.8(2) . . ?
C5 C6 S6 128.5(3) . . ?
C5 C6 S4 117.0(3) . . ?
S6 C6 S4 114.5(2) . . ?
S5 C7 H7C 109.5 . . ?
S5 C7 H7B 109.5 . . ?
H7C C7 H7B 109.5 . . ?
S5 C7 H7A 109.5 . . ?
H7C C7 H7A 109.5 . . ?
H7B C7 H7A 109.5 . . ?
S6 C8 H8C 109.5 . . ?
S6 C8 H8B 109.5 . . ?
H8C C8 H8B 109.5 . . ?
S6 C8 H8A 109.5 . . ?
H8C C8 H8A 109.5 . . ?
H8B C8 H8A 109.5 . . ?
O3 C15 H15A 109.5 . . ?
O3 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O3 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N5 C17 C16 176.4(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
N3 Cu1 O3 C15 3.8(4) . . . . ?
N1 Cu1 O3 C15 -99.4(4) . . . . ?
N2 Cu1 O3 C15 177.2(4) . . . . ?
N4 Cu1 O3 C15 88.0(4) . . . . ?
N3 Cu1 N2 C11 -75.5(6) . . . . ?
N1 Cu1 N2 C11 31.6(2) . . . . ?
N4 Cu1 N2 C11 -139.0(2) . . . . ?
O3 Cu1 N2 C11 129.0(2) . . . . ?
N3 Cu1 N4 C14 9.7(3) . . . . ?
N1 Cu1 N4 C14 124.8(6) . . . . ?
N2 Cu1 N4 C14 175.7(3) . . . . ?
O3 Cu1 N4 C14 -92.6(3) . . . . ?
N3 Cu1 N1 C9 -43.9(4) . . . . ?
N2 Cu1 N1 C9 151.3(4) . . . . ?
N4 Cu1 N1 C9 -157.4(5) . . . . ?
O3 Cu1 N1 C9 60.4(4) . . . . ?
N3 Cu1 N1 C10 157.2(2) . . . . ?
N2 Cu1 N1 C10 -7.6(3) . . . . ?
N4 Cu1 N1 C10 43.7(7) . . . . ?
O3 Cu1 N1 C10 -98.5(3) . . . . ?
N1 Cu1 N3 C12 20.0(4) . . . . ?
N2 Cu1 N3 C12 124.7(5) . . . . ?
N4 Cu1 N3 C12 -171.1(4) . . . . ?
O3 Cu1 N3 C12 -80.4(4) . . . . ?
N1 Cu1 N3 C13 -149.8(3) . . . . ?
N2 Cu1 N3 C13 -45.0(7) . . . . ?
N4 Cu1 N3 C13 19.1(3) . . . . ?
O3 Cu1 N3 C13 109.8(3) . . . . ?
Cu1 N2 C11 C10 -49.4(3) . . . . ?
C9 N1 C10 C11 178.8(3) . . . . ?
Cu1 N1 C10 C11 -18.1(4) . . . . ?
N2 C11 C10 N1 44.7(4) . . . . ?
Cu1 N4 C14 C13 -36.0(4) . . . . ?
C12 N3 C13 C14 144.1(4) . . . . ?
Cu1 N3 C13 C14 -43.9(4) . . . . ?
N4 C14 C13 N3 52.3(4) . . . . ?
C10 N1 C9 O1 -1.5(6) . . . . ?
Cu1 N1 C9 O1 -160.3(3) . . . . ?
C10 N1 C9 C1 177.3(3) . . . . ?
Cu1 N1 C9 C1 18.5(6) . . . . ?
O1 C9 C1 C2 -160.5(4) . . . . ?
N1 C9 C1 C2 20.5(7) . . . . ?
O1 C9 C1 S1 12.1(4) . . . . ?
N1 C9 C1 S1 -166.9(3) . . . . ?
C3 S1 C1 C2 -15.6(3) . . . . ?
C3 S1 C1 C9 170.2(3) . . . . ?
C9 C1 C2 C12 0.0(8) . . . . ?
S1 C1 C2 C12 -172.2(4) . . . . ?
C9 C1 C2 S2 173.1(4) . . . . ?
S1 C1 C2 S2 1.0(4) . . . . ?
C3 S2 C2 C1 14.2(3) . . . . ?
C3 S2 C2 C12 -171.0(3) . . . . ?
C13 N3 C12 O2 3.9(6) . . . . ?
Cu1 N3 C12 O2 -165.5(3) . . . . ?
C13 N3 C12 C2 -170.3(4) . . . . ?
Cu1 N3 C12 C2 20.4(6) . . . . ?
C1 C2 C12 O2 146.7(4) . . . . ?
S2 C2 C12 O2 -26.8(4) . . . . ?
C1 C2 C12 N3 -38.5(7) . . . . ?
S2 C2 C12 N3 148.0(3) . . . . ?
C2 S2 C3 C4 159.5(4) . . . . ?
C2 S2 C3 S1 -24.3(3) . . . . ?
C1 S1 C3 C4 -159.0(4) . . . . ?
C1 S1 C3 S2 24.6(3) . . . . ?
S2 C3 C4 S4 -2.2(6) . . . . ?
S1 C3 C4 S4 -178.1(2) . . . . ?
S2 C3 C4 S3 173.4(2) . . . . ?
S1 C3 C4 S3 -2.5(5) . . . . ?
C6 S4 C4 C3 -165.3(4) . . . . ?
C6 S4 C4 S3 18.8(3) . . . . ?
C5 S3 C4 C3 164.2(4) . . . . ?
C5 S3 C4 S4 -19.6(2) . . . . ?
C4 S3 C5 C6 13.3(4) . . . . ?
C4 S3 C5 S5 -172.6(2) . . . . ?
C7 S5 C5 C6 -126.1(4) . . . . ?
C7 S5 C5 S3 60.4(3) . . . . ?
S3 C5 C6 S6 178.6(2) . . . . ?
S5 C5 C6 S6 5.0(6) . . . . ?
S3 C5 C6 S4 -2.1(5) . . . . ?
S5 C5 C6 S4 -175.6(2) . . . . ?
C8 S6 C6 C5 -59.9(4) . . . . ?
C8 S6 C6 S4 120.8(3) . . . . ?
C4 S4 C6 C5 -10.3(4) . . . . ?
C4 S4 C6 S6 169.2(2) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H2A S1 0.91 2.79 3.566(3) 144.0 3_666
N2 H2B O2 0.91 2.06 2.925(4) 157.6 4_576
O3 H3A O1 0.79(5) 1.91(5) 2.691(4) 173(6) 3_666
N4 H4A O2 0.91 2.17 2.954(4) 143.5 4_576
N4 H4B N5 0.91 2.23 3.115(7) 165.2 3_566

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.510
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.079

####################END

data_2
_database_code_depnum_ccdc_archive 'CCDC 750341'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H22 Cu N4 O3 S6, 0.5(H2 O)'
_chemical_formula_sum            'C15 H23 Cu N4 O3.50 S6'
_chemical_formula_weight         571.27

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_Int_Tables_number      15

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                   17.545(3)
_cell_length_b                   19.829(3)
_cell_length_c                   15.151(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 121.226(2)
_cell_angle_gamma                90.00
_cell_volume                     4507.5(11)
_cell_formula_units_Z            8
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    8437
_cell_measurement_theta_min      3.1
_cell_measurement_theta_max      25.3

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.40
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.684
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2352
_exptl_absorpt_coefficient_mu    1.553
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.390
_exptl_absorpt_correction_T_max  0.537
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      153(2)
_diffrn_radiation_wavelength     0.71070
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean 7.31
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21588
_diffrn_reflns_av_R_equivalents  0.0229
_diffrn_reflns_av_sigmaI/netI    0.0171
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.10
_diffrn_reflns_theta_max         25.35
_reflns_number_total             4119
_reflns_number_gt                3933
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       CrystalClear
_computing_cell_refinement       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0361P)^2^+8.7413P] where P=(Fo^2^+2Fc^2^)/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         4119
_refine_ls_number_parameters     279
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0314
_refine_ls_wR_factor_ref         0.0774
_refine_ls_wR_factor_gt          0.0761
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_restrained_S_all      1.114
_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 0.646289(18) 0.077560(14) 0.46062(2) 0.01863(9) Uani 1 1 d . . .
S1 S 0.64091(5) 0.14169(3) 0.78341(5) 0.02667(15) Uani 1 1 d . . .
S2 S 0.75495(4) 0.24008(3) 0.76308(5) 0.02692(15) Uani 1 1 d . . .
S3 S 0.58450(5) 0.26163(3) 0.89432(5) 0.03058(16) Uani 1 1 d . . .
S4 S 0.69762(5) 0.35499(3) 0.86241(6) 0.03627(18) Uani 1 1 d . . .
S5 S 0.48738(4) 0.37130(4) 0.93253(5) 0.03289(16) Uani 1 1 d . . .
S6 S 0.62239(5) 0.47835(3) 0.90338(5) 0.03462(17) Uani 1 1 d . . .
O1 O 0.62348(11) 0.01589(8) 0.71094(12) 0.0215(3) Uani 1 1 d . . .
O2 O 0.84311(12) 0.20924(11) 0.67018(15) 0.0407(5) Uani 1 1 d . . .
O3 O 0.52216(12) 0.14813(9) 0.40086(14) 0.0286(4) Uani 1 1 d D . .
H3 H 0.5149(19) 0.1716(12) 0.3530(15) 0.028(8) Uiso 1 1 d D . .
O4 O 0.5000 0.23384(13) 0.2500 0.0290(6) Uani 1 2 d SD . .
H4 H 0.4560(16) 0.2592(15) 0.226(3) 0.065(12) Uiso 1 1 d D . .
N1 N 0.64066(12) 0.03004(9) 0.57257(14) 0.0173(4) Uani 1 1 d . . .
N2 N 0.57665(13) -0.00362(10) 0.37755(14) 0.0212(4) Uani 1 1 d . . .
H2A H 0.5166 0.0025 0.3507 0.025 Uiso 1 1 calc R . .
H2B H 0.5862 -0.0114 0.3242 0.025 Uiso 1 1 calc R . .
N3 N 0.74964(13) 0.13574(9) 0.54442(15) 0.0200(4) Uani 1 1 d . . .
N4 N 0.66560(13) 0.11078(11) 0.34455(16) 0.0262(4) Uani 1 1 d . . .
H4A H 0.6394 0.0823 0.2885 0.031 Uiso 1 1 calc R . .
H4B H 0.6438 0.1537 0.3236 0.031 Uiso 1 1 calc R . .
C1 C 0.67629(15) 0.12091(11) 0.69703(17) 0.0189(5) Uani 1 1 d . . .
C2 C 0.72809(15) 0.16666(12) 0.68661(17) 0.0198(5) Uani 1 1 d . . .
C3 C 0.67697(17) 0.22519(12) 0.80018(19) 0.0254(5) Uani 1 1 d . . .
C4 C 0.65411(17) 0.27308(12) 0.84416(19) 0.0267(5) Uani 1 1 d . . .
C5 C 0.56692(17) 0.34845(13) 0.90090(19) 0.0264(5) Uani 1 1 d . . .
C6 C 0.61851(17) 0.39109(13) 0.88571(19) 0.0274(5) Uani 1 1 d . . .
C7 C 0.5583(2) 0.39608(18) 1.0661(2) 0.0476(8) Uani 1 1 d . . .
H7A H 0.5943 0.3574 1.1065 0.071 Uiso 1 1 calc R . .
H7B H 0.5214 0.4115 1.0933 0.071 Uiso 1 1 calc R . .
H7C H 0.5977 0.4328 1.0708 0.071 Uiso 1 1 calc R . .
C8 C 0.6218(2) 0.50882(15) 0.7908(2) 0.0405(7) Uani 1 1 d . . .
H8A H 0.6795 0.4993 0.7979 0.061 Uiso 1 1 calc R . .
H8B H 0.6112 0.5576 0.7843 0.061 Uiso 1 1 calc R . .
H8C H 0.5744 0.4861 0.7292 0.061 Uiso 1 1 calc R . .
C9 C 0.64574(14) 0.05098(11) 0.65791(17) 0.0178(4) Uani 1 1 d . . .
C10 C 0.60780(15) -0.03966(11) 0.54577(17) 0.0198(5) Uani 1 1 d . . .
H10A H 0.5460 -0.0425 0.5312 0.024 Uiso 1 1 calc R . .
H10B H 0.6457 -0.0702 0.6040 0.024 Uiso 1 1 calc R . .
C11 C 0.61056(16) -0.06005(12) 0.45152(18) 0.0222(5) Uani 1 1 d . . .
H11A H 0.6725 -0.0709 0.4712 0.027 Uiso 1 1 calc R . .
H11B H 0.5733 -0.1006 0.4197 0.027 Uiso 1 1 calc R . .
C12 C 0.77749(15) 0.16911(12) 0.63009(18) 0.0232(5) Uani 1 1 d . . .
C13 C 0.80123(17) 0.15018(13) 0.4947(2) 0.0276(5) Uani 1 1 d . . .
H13A H 0.8647 0.1385 0.5423 0.033 Uiso 1 1 calc R . .
H13B H 0.7975 0.1988 0.4783 0.033 Uiso 1 1 calc R . .
C14 C 0.76393(17) 0.10916(13) 0.39673(19) 0.0279(5) Uani 1 1 d . . .
H14A H 0.7832 0.1285 0.3512 0.033 Uiso 1 1 calc R . .
H14B H 0.7856 0.0621 0.4133 0.033 Uiso 1 1 calc R . .
C15 C 0.5064(2) 0.19039(15) 0.4657(2) 0.0387(7) Uani 1 1 d . . .
H15A H 0.5134 0.1641 0.5242 0.058 Uiso 1 1 calc R . .
H15B H 0.4457 0.2085 0.4263 0.058 Uiso 1 1 calc R . .
H15C H 0.5493 0.2277 0.4913 0.058 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.02085(16) 0.02242(17) 0.01724(16) 0.00083(10) 0.01313(13) -0.00098(11)
S1 0.0437(4) 0.0211(3) 0.0312(3) -0.0067(2) 0.0307(3) -0.0084(3)
S2 0.0310(3) 0.0262(3) 0.0324(3) -0.0101(3) 0.0226(3) -0.0107(3)
S3 0.0444(4) 0.0252(3) 0.0386(4) -0.0078(3) 0.0331(3) -0.0081(3)
S4 0.0448(4) 0.0277(3) 0.0552(5) -0.0196(3) 0.0392(4) -0.0169(3)
S5 0.0307(3) 0.0399(4) 0.0343(4) 0.0016(3) 0.0212(3) 0.0053(3)
S6 0.0445(4) 0.0239(3) 0.0368(4) -0.0056(3) 0.0220(3) -0.0024(3)
O1 0.0316(9) 0.0205(8) 0.0212(8) 0.0001(6) 0.0199(7) -0.0027(7)
O2 0.0290(10) 0.0554(13) 0.0470(12) -0.0215(10) 0.0262(9) -0.0225(9)
O3 0.0314(10) 0.0276(9) 0.0327(10) 0.0067(8) 0.0208(9) 0.0071(8)
O4 0.0229(13) 0.0249(13) 0.0365(15) 0.000 0.0135(12) 0.000
N1 0.0183(9) 0.0197(10) 0.0177(9) -0.0001(7) 0.0119(8) -0.0009(7)
N2 0.0228(10) 0.0283(11) 0.0169(10) -0.0024(8) 0.0133(8) -0.0005(8)
N3 0.0205(9) 0.0233(10) 0.0239(10) 0.0002(8) 0.0169(9) -0.0018(8)
N4 0.0293(11) 0.0319(11) 0.0237(11) 0.0053(9) 0.0183(9) 0.0027(9)
C1 0.0204(11) 0.0227(12) 0.0164(11) -0.0015(9) 0.0115(9) 0.0008(9)
C2 0.0192(11) 0.0224(12) 0.0186(11) -0.0037(9) 0.0104(9) -0.0007(9)
C3 0.0337(13) 0.0227(12) 0.0285(13) -0.0056(10) 0.0222(11) -0.0090(10)
C4 0.0348(14) 0.0236(12) 0.0312(13) -0.0099(10) 0.0238(12) -0.0106(10)
C5 0.0292(13) 0.0279(13) 0.0251(13) -0.0051(10) 0.0163(11) -0.0015(10)
C6 0.0304(13) 0.0270(13) 0.0276(13) -0.0078(10) 0.0171(11) -0.0045(10)
C7 0.0511(19) 0.063(2) 0.0361(16) -0.0106(15) 0.0281(15) 0.0038(16)
C8 0.0418(16) 0.0344(15) 0.0356(16) 0.0009(12) 0.0134(13) -0.0117(13)
C9 0.0161(10) 0.0199(11) 0.0194(11) 0.0016(9) 0.0106(9) 0.0019(9)
C10 0.0237(11) 0.0200(11) 0.0203(11) -0.0005(9) 0.0146(10) -0.0003(9)
C11 0.0282(12) 0.0214(12) 0.0213(12) -0.0029(9) 0.0159(10) -0.0015(10)
C12 0.0191(11) 0.0281(13) 0.0266(13) -0.0004(10) 0.0148(10) -0.0015(10)
C13 0.0276(13) 0.0335(14) 0.0339(14) -0.0005(11) 0.0246(12) -0.0038(11)
C14 0.0325(13) 0.0326(14) 0.0305(13) 0.0038(11) 0.0248(12) 0.0035(11)
C15 0.0410(16) 0.0384(16) 0.0410(16) -0.0019(13) 0.0244(14) 0.0085(13)

_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 N3 1.9606(19) . ?
Cu1 N1 1.9870(18) . ?
Cu1 N2 2.0183(19) . ?
Cu1 N4 2.0637(19) . ?
Cu1 O3 2.3402(17) . ?
S1 C3 1.743(2) . ?
S1 C1 1.764(2) . ?
S2 C3 1.753(2) . ?
S2 C2 1.766(2) . ?
S3 C4 1.756(2) . ?
S3 C5 1.761(3) . ?
S4 C6 1.753(3) . ?
S4 C4 1.754(2) . ?
S5 C5 1.754(3) . ?
S5 C7 1.809(3) . ?
S6 C6 1.747(3) . ?
S6 C8 1.804(3) . ?
O1 C9 1.268(3) . ?
O2 C12 1.266(3) . ?
O3 C15 1.423(3) . ?
O3 H3 0.814(10) . ?
O4 H4 0.831(10) . ?
N1 C9 1.316(3) . ?
N1 C10 1.471(3) . ?
N2 C11 1.473(3) . ?
N2 H2A 0.9200 . ?
N2 H2B 0.9200 . ?
N3 C12 1.305(3) . ?
N3 C13 1.475(3) . ?
N4 C14 1.479(3) . ?
N4 H4A 0.9200 . ?
N4 H4B 0.9200 . ?
C1 C2 1.350(3) . ?
C1 C9 1.494(3) . ?
C2 C12 1.502(3) . ?
C3 C4 1.336(3) . ?
C5 C6 1.343(4) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C10 C11 1.509(3) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C13 C14 1.512(4) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Cu1 N1 99.49(8) . . ?
N3 Cu1 N2 158.56(8) . . ?
N1 Cu1 N2 82.65(8) . . ?
N3 Cu1 N4 81.88(8) . . ?
N1 Cu1 N4 168.96(8) . . ?
N2 Cu1 N4 92.12(8) . . ?
N3 Cu1 O3 105.16(7) . . ?
N1 Cu1 O3 99.54(7) . . ?
N2 Cu1 O3 95.43(7) . . ?
N4 Cu1 O3 90.60(7) . . ?
C3 S1 C1 95.12(11) . . ?
C3 S2 C2 94.84(11) . . ?
C4 S3 C5 94.57(12) . . ?
C6 S4 C4 94.85(12) . . ?
C5 S5 C7 101.09(13) . . ?
C6 S6 C8 101.90(13) . . ?
C15 O3 Cu1 124.04(16) . . ?
C15 O3 H3 106(2) . . ?
Cu1 O3 H3 112(2) . . ?
C9 N1 C10 112.62(18) . . ?
C9 N1 Cu1 132.91(16) . . ?
C10 N1 Cu1 113.31(13) . . ?
C11 N2 Cu1 104.85(14) . . ?
C11 N2 H2A 110.8 . . ?
Cu1 N2 H2A 110.8 . . ?
C11 N2 H2B 110.8 . . ?
Cu1 N2 H2B 110.8 . . ?
H2A N2 H2B 108.9 . . ?
C12 N3 C13 113.38(19) . . ?
C12 N3 Cu1 133.32(16) . . ?
C13 N3 Cu1 112.96(15) . . ?
C14 N4 Cu1 101.47(14) . . ?
C14 N4 H4A 111.5 . . ?
Cu1 N4 H4A 111.5 . . ?
C14 N4 H4B 111.5 . . ?
Cu1 N4 H4B 111.5 . . ?
H4A N4 H4B 109.3 . . ?
C2 C1 C9 134.6(2) . . ?
C2 C1 S1 116.55(17) . . ?
C9 C1 S1 108.63(15) . . ?
C1 C2 C12 135.3(2) . . ?
C1 C2 S2 116.37(17) . . ?
C12 C2 S2 108.11(16) . . ?
C4 C3 S1 124.60(19) . . ?
C4 C3 S2 121.76(19) . . ?
S1 C3 S2 113.45(14) . . ?
C3 C4 S4 121.22(19) . . ?
C3 C4 S3 125.46(19) . . ?
S4 C4 S3 113.26(13) . . ?
C6 C5 S5 125.9(2) . . ?
C6 C5 S3 116.91(19) . . ?
S5 C5 S3 117.11(14) . . ?
C5 C6 S6 125.0(2) . . ?
C5 C6 S4 116.9(2) . . ?
S6 C6 S4 117.61(14) . . ?
S5 C7 H7A 109.5 . . ?
S5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
S5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
S6 C8 H8A 109.5 . . ?
S6 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
S6 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O1 C9 N1 124.3(2) . . ?
O1 C9 C1 115.03(19) . . ?
N1 C9 C1 120.67(19) . . ?
N1 C10 C11 108.21(18) . . ?
N1 C10 H10A 110.1 . . ?
C11 C10 H10A 110.1 . . ?
N1 C10 H10B 110.1 . . ?
C11 C10 H10B 110.1 . . ?
H10A C10 H10B 108.4 . . ?
N2 C11 C10 108.54(18) . . ?
N2 C11 H11A 110.0 . . ?
C10 C11 H11A 110.0 . . ?
N2 C11 H11B 110.0 . . ?
C10 C11 H11B 110.0 . . ?
H11A C11 H11B 108.4 . . ?
O2 C12 N3 125.0(2) . . ?
O2 C12 C2 113.4(2) . . ?
N3 C12 C2 121.4(2) . . ?
N3 C13 C14 109.2(2) . . ?
N3 C13 H13A 109.8 . . ?
C14 C13 H13A 109.8 . . ?
N3 C13 H13B 109.8 . . ?
C14 C13 H13B 109.8 . . ?
H13A C13 H13B 108.3 . . ?
N4 C14 C13 107.71(19) . . ?
N4 C14 H14A 110.2 . . ?
C13 C14 H14A 110.2 . . ?
N4 C14 H14B 110.2 . . ?
C13 C14 H14B 110.2 . . ?
H14A C14 H14B 108.5 . . ?
O3 C15 H15A 109.5 . . ?
O3 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O3 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 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
N3 Cu1 O3 C15 -51.8(2) . . . . ?
N1 Cu1 O3 C15 50.8(2) . . . . ?
N2 Cu1 O3 C15 134.3(2) . . . . ?
N4 Cu1 O3 C15 -133.6(2) . . . . ?
N3 Cu1 N1 C9 45.9(2) . . . . ?
N2 Cu1 N1 C9 -155.7(2) . . . . ?
N4 Cu1 N1 C9 142.1(4) . . . . ?
O3 Cu1 N1 C9 -61.4(2) . . . . ?
N3 Cu1 N1 C10 -147.60(15) . . . . ?
N2 Cu1 N1 C10 10.83(15) . . . . ?
N4 Cu1 N1 C10 -51.4(5) . . . . ?
O3 Cu1 N1 C10 105.13(15) . . . . ?
N3 Cu1 N2 C11 63.6(3) . . . . ?
N1 Cu1 N2 C11 -33.70(14) . . . . ?
N4 Cu1 N2 C11 136.54(14) . . . . ?
O3 Cu1 N2 C11 -132.66(14) . . . . ?
N1 Cu1 N3 C12 -38.3(2) . . . . ?
N2 Cu1 N3 C12 -132.4(2) . . . . ?
N4 Cu1 N3 C12 152.7(2) . . . . ?
O3 Cu1 N3 C12 64.3(2) . . . . ?
N1 Cu1 N3 C13 149.05(16) . . . . ?
N2 Cu1 N3 C13 55.0(3) . . . . ?
N4 Cu1 N3 C13 -19.87(16) . . . . ?
O3 Cu1 N3 C13 -108.28(16) . . . . ?
N3 Cu1 N4 C14 40.65(15) . . . . ?
N1 Cu1 N4 C14 -57.3(5) . . . . ?
N2 Cu1 N4 C14 -118.67(15) . . . . ?
O3 Cu1 N4 C14 145.87(15) . . . . ?
C3 S1 C1 C2 10.3(2) . . . . ?
C3 S1 C1 C9 -174.31(16) . . . . ?
C9 C1 C2 C12 1.2(5) . . . . ?
S1 C1 C2 C12 175.0(2) . . . . ?
C9 C1 C2 S2 -172.5(2) . . . . ?
S1 C1 C2 S2 1.3(3) . . . . ?
C3 S2 C2 C1 -12.1(2) . . . . ?
C3 S2 C2 C12 172.52(17) . . . . ?
C1 S1 C3 C4 166.7(2) . . . . ?
C1 S1 C3 S2 -18.27(16) . . . . ?
C2 S2 C3 C4 -166.0(2) . . . . ?
C2 S2 C3 S1 18.79(16) . . . . ?
S1 C3 C4 S4 177.32(15) . . . . ?
S2 C3 C4 S4 2.7(3) . . . . ?
S1 C3 C4 S3 0.5(4) . . . . ?
S2 C3 C4 S3 -174.12(15) . . . . ?
C6 S4 C4 C3 164.5(2) . . . . ?
C6 S4 C4 S3 -18.34(17) . . . . ?
C5 S3 C4 C3 -164.9(3) . . . . ?
C5 S3 C4 S4 18.05(17) . . . . ?
C7 S5 C5 C6 -73.5(3) . . . . ?
C7 S5 C5 S3 103.37(18) . . . . ?
C4 S3 C5 C6 -10.7(2) . . . . ?
C4 S3 C5 S5 172.19(15) . . . . ?
S5 C5 C6 S6 4.8(4) . . . . ?
S3 C5 C6 S6 -172.07(15) . . . . ?
S5 C5 C6 S4 176.27(15) . . . . ?
S3 C5 C6 S4 -0.6(3) . . . . ?
C8 S6 C6 C5 -136.4(2) . . . . ?
C8 S6 C6 S4 52.14(18) . . . . ?
C4 S4 C6 C5 11.5(2) . . . . ?
C4 S4 C6 S6 -176.33(16) . . . . ?
C10 N1 C9 O1 -1.2(3) . . . . ?
Cu1 N1 C9 O1 165.40(16) . . . . ?
C10 N1 C9 C1 -178.99(19) . . . . ?
Cu1 N1 C9 C1 -12.4(3) . . . . ?
C2 C1 C9 O1 156.8(3) . . . . ?
S1 C1 C9 O1 -17.3(2) . . . . ?
C2 C1 C9 N1 -25.2(4) . . . . ?
S1 C1 C9 N1 160.66(17) . . . . ?
C9 N1 C10 C11 -176.19(19) . . . . ?
Cu1 N1 C10 C11 14.5(2) . . . . ?
Cu1 N2 C11 C10 50.8(2) . . . . ?
N1 C10 C11 N2 -43.2(2) . . . . ?
C13 N3 C12 O2 -1.4(4) . . . . ?
Cu1 N3 C12 O2 -173.99(19) . . . . ?
C13 N3 C12 C2 173.8(2) . . . . ?
Cu1 N3 C12 C2 1.2(4) . . . . ?
C1 C2 C12 O2 -154.8(3) . . . . ?
S2 C2 C12 O2 19.3(3) . . . . ?
C1 C2 C12 N3 29.5(4) . . . . ?
S2 C2 C12 N3 -156.4(2) . . . . ?
C12 N3 C13 C14 179.9(2) . . . . ?
Cu1 N3 C13 C14 -5.9(3) . . . . ?
Cu1 N4 C14 C13 -54.1(2) . . . . ?
N3 C13 C14 N4 41.1(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C14 H14B S6 0.99 2.90 3.690(3) 137.0 4_646
C11 H11A S4 0.99 2.78 3.504(3) 130.0 4_646
C10 H10B S4 0.99 2.93 3.610(2) 127.0 4_646
C8 H8C S6 0.98 2.97 3.783(3) 141.6 2_656
C7 H7C S6 0.98 2.93 3.588(3) 125.5 .
N2 H2A O1 0.92 2.16 3.050(3) 162.7 5_656
N2 H2B O1 0.92 2.13 3.043(2) 170.5 6
N2 H2B S1 0.92 2.93 3.531(2) 124.2 6
N4 H4A O1 0.92 2.22 3.066(3) 153.4 6
O3 H3 O4 0.814(10) 1.898(11) 2.710(2) 174(3) .
O4 H4 O2 0.831(10) 1.814(15) 2.620(2) 163(4) 8_455

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.35
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.387
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.068

######################END

data_3
_database_code_depnum_ccdc_archive 'CCDC 750342'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C17 H27 Cu N5 O4 S6'
_chemical_formula_weight         621.34

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           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   9.5471(6)
_cell_length_b                   18.3348(12)
_cell_length_c                   14.6021(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.327(2)
_cell_angle_gamma                90.00
_cell_volume                     2522.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.636
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1284
_exptl_absorpt_coefficient_mu    1.398
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6048
_exptl_absorpt_correction_T_max  0.8502
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      223(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean 14.63
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14342
_diffrn_reflns_av_R_equivalents  0.0475
_diffrn_reflns_av_sigmaI/netI    0.0685
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.04
_diffrn_reflns_theta_max         27.48
_reflns_number_total             5710
_reflns_number_gt                4709
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0824P)^2^+0.1090P] where P=(Fo^2^+2Fc^2^)/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         5710
_refine_ls_number_parameters     309
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0785
_refine_ls_R_factor_gt           0.0597
_refine_ls_wR_factor_ref         0.1638
_refine_ls_wR_factor_gt          0.1512
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.071
_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 0.18966(5) 0.65987(3) 0.53503(3) 0.02346(16) Uani 1 1 d . . .
S1 S 0.14647(12) 0.63575(6) 0.87787(7) 0.0276(2) Uani 1 1 d . . .
S2 S -0.04770(11) 0.52992(6) 0.77715(7) 0.0266(2) Uani 1 1 d . . .
S3 S 0.26280(12) 0.50823(6) 1.03256(8) 0.0298(3) Uani 1 1 d . . .
S4 S 0.06932(12) 0.40353(6) 0.92495(8) 0.0300(3) Uani 1 1 d . . .
S5 S 0.46917(13) 0.39556(7) 1.11796(9) 0.0404(3) Uani 1 1 d . . .
S6 S 0.24508(14) 0.27294(6) 0.99830(9) 0.0407(3) Uani 1 1 d . . .
O1 O -0.1674(3) 0.55299(16) 0.6020(2) 0.0282(6) Uani 1 1 d . . .
O2 O 0.2141(4) 0.75926(16) 0.7957(2) 0.0339(7) Uani 1 1 d . . .
O3 O 0.3533(3) 0.56469(18) 0.6062(2) 0.0387(8) Uani 1 1 d . . .
O4 O 0.5726(5) 0.6063(2) 0.5130(3) 0.0536(11) Uani 1 1 d . . .
H4C H 0.510(6) 0.585(3) 0.550(4) 0.055(17) Uiso 1 1 d . . .
H4D H 0.649(7) 0.588(4) 0.535(5) 0.07(2) Uiso 1 1 d . . .
N1 N 0.0038(3) 0.61569(18) 0.5413(2) 0.0240(7) Uani 1 1 d . . .
N2 N 0.1525(4) 0.61770(19) 0.4045(2) 0.0267(8) Uani 1 1 d . . .
H2A H 0.2036 0.6414 0.3663 0.032 Uiso 1 1 calc R . .
H2B H 0.1734 0.5693 0.4047 0.032 Uiso 1 1 calc R . .
N3 N 0.2052(4) 0.72371(17) 0.6440(2) 0.0246(7) Uani 1 1 d . . .
N4 N 0.3515(4) 0.72110(19) 0.5014(2) 0.0272(8) Uani 1 1 d . . .
H4A H 0.4249 0.6916 0.4928 0.033 Uiso 1 1 calc R . .
H4B H 0.3217 0.7456 0.4476 0.033 Uiso 1 1 calc R . .
N5 N 0.4181(4) 0.4707(2) 0.7068(3) 0.0338(9) Uani 1 1 d . . .
C1 C 0.0186(4) 0.5983(2) 0.7092(3) 0.0216(8) Uani 1 1 d . . .
C2 C 0.1094(4) 0.6469(2) 0.7562(3) 0.0226(8) Uani 1 1 d . . .
C3 C 0.0836(4) 0.5456(2) 0.8728(3) 0.0253(8) Uani 1 1 d . . .
C4 C 0.1323(5) 0.4942(2) 0.9349(3) 0.0268(9) Uani 1 1 d . . .
C6 C 0.3123(5) 0.4156(2) 1.0431(3) 0.0295(9) Uani 1 1 d . . .
C5 C 0.2233(5) 0.3671(2) 0.9932(3) 0.0296(9) Uani 1 1 d . . .
C8 C 0.4051(8) 0.3444(3) 1.2087(4) 0.0633(17) Uani 1 1 d . . .
H8A H 0.4848 0.3300 1.2552 0.095 Uiso 1 1 calc R . .
H8B H 0.3556 0.3011 1.1822 0.095 Uiso 1 1 calc R . .
H8C H 0.3406 0.3744 1.2372 0.095 Uiso 1 1 calc R . .
C7 C 0.2059(6) 0.2487(3) 0.8773(4) 0.0422(12) Uani 1 1 d . . .
H7A H 0.2146 0.1963 0.8708 0.063 Uiso 1 1 calc R . .
H7B H 0.2721 0.2731 0.8437 0.063 Uiso 1 1 calc R . .
H7C H 0.1098 0.2636 0.8523 0.063 Uiso 1 1 calc R . .
C9 C -0.0531(4) 0.5892(2) 0.6103(3) 0.0232(8) Uani 1 1 d . . .
C10 C -0.0761(4) 0.5974(2) 0.4496(3) 0.0274(9) Uani 1 1 d . . .
H10A H -0.1729 0.6166 0.4436 0.033 Uiso 1 1 calc R . .
H10B H -0.0815 0.5443 0.4418 0.033 Uiso 1 1 calc R . .
C11 C -0.0009(5) 0.6305(2) 0.3770(3) 0.0306(9) Uani 1 1 d . . .
H11A H -0.0344 0.6081 0.3165 0.037 Uiso 1 1 calc R . .
H11B H -0.0202 0.6830 0.3720 0.037 Uiso 1 1 calc R . .
C12 C 0.1801(4) 0.7157(2) 0.7296(3) 0.0243(8) Uani 1 1 d . . .
C13 C 0.2751(5) 0.7925(2) 0.6246(3) 0.0328(10) Uani 1 1 d . . .
H13A H 0.3084 0.8186 0.6826 0.039 Uiso 1 1 calc R . .
H13B H 0.2080 0.8239 0.5847 0.039 Uiso 1 1 calc R . .
C14 C 0.3991(4) 0.7735(2) 0.5766(3) 0.0308(10) Uani 1 1 d . . .
H14A H 0.4355 0.8177 0.5509 0.037 Uiso 1 1 calc R . .
H14B H 0.4756 0.7520 0.6212 0.037 Uiso 1 1 calc R . .
C15 C 0.3294(5) 0.5199(3) 0.6652(3) 0.0325(10) Uani 1 1 d . . .
H15 H 0.2385 0.5212 0.6820 0.039 Uiso 1 1 calc R . .
C16 C 0.5630(5) 0.4639(3) 0.6886(4) 0.0500(14) Uani 1 1 d . . .
H16A H 0.5770 0.4155 0.6649 0.075 Uiso 1 1 calc R . .
H16B H 0.6288 0.4717 0.7457 0.075 Uiso 1 1 calc R . .
H16C H 0.5796 0.5001 0.6431 0.075 Uiso 1 1 calc R . .
C17 C 0.3776(6) 0.4221(3) 0.7756(4) 0.0518(14) Uani 1 1 d . . .
H17A H 0.2818 0.4335 0.7852 0.078 Uiso 1 1 calc R . .
H17B H 0.4424 0.4280 0.8335 0.078 Uiso 1 1 calc R . .
H17C H 0.3812 0.3721 0.7544 0.078 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0263(3) 0.0247(3) 0.0197(3) -0.00073(19) 0.0047(2) -0.0017(2)
S1 0.0377(6) 0.0254(5) 0.0191(5) -0.0001(4) 0.0030(4) -0.0040(5)
S2 0.0294(5) 0.0276(5) 0.0225(5) 0.0026(4) 0.0033(4) -0.0047(4)
S3 0.0380(6) 0.0264(5) 0.0232(5) 0.0014(4) -0.0007(4) -0.0007(5)
S4 0.0331(6) 0.0257(5) 0.0304(6) 0.0014(4) 0.0030(5) -0.0029(5)
S5 0.0378(6) 0.0408(7) 0.0388(7) 0.0042(5) -0.0048(5) 0.0036(5)
S6 0.0539(8) 0.0242(5) 0.0431(7) 0.0050(5) 0.0054(6) 0.0022(5)
O1 0.0239(14) 0.0324(16) 0.0270(16) 0.0019(13) 0.0003(12) -0.0026(13)
O2 0.0520(19) 0.0270(15) 0.0232(16) -0.0059(12) 0.0073(14) -0.0087(14)
O3 0.0301(17) 0.0402(18) 0.045(2) 0.0055(16) 0.0034(15) 0.0039(15)
O4 0.040(2) 0.054(2) 0.068(3) 0.020(2) 0.010(2) 0.009(2)
N1 0.0259(17) 0.0265(17) 0.0185(17) 0.0006(14) 0.0001(13) -0.0007(14)
N2 0.0308(18) 0.0270(18) 0.0232(18) -0.0015(14) 0.0068(14) 0.0020(15)
N3 0.0298(18) 0.0200(16) 0.0245(18) 0.0002(14) 0.0053(14) -0.0041(14)
N4 0.0299(18) 0.0271(18) 0.0242(18) 0.0059(15) 0.0027(15) 0.0018(15)
N5 0.0282(18) 0.036(2) 0.037(2) 0.0057(17) 0.0061(16) 0.0048(17)
C1 0.0215(19) 0.0214(18) 0.022(2) 0.0018(15) 0.0044(15) 0.0019(16)
C2 0.026(2) 0.0212(19) 0.020(2) 0.0018(15) 0.0041(16) 0.0008(16)
C3 0.029(2) 0.027(2) 0.021(2) 0.0003(16) 0.0071(17) -0.0003(17)
C4 0.035(2) 0.023(2) 0.023(2) 0.0006(16) 0.0063(17) 0.0006(18)
C6 0.035(2) 0.028(2) 0.026(2) 0.0025(18) 0.0039(18) 0.0006(19)
C5 0.036(2) 0.024(2) 0.030(2) 0.0042(18) 0.0062(19) 0.0003(18)
C8 0.090(5) 0.055(4) 0.040(3) 0.021(3) -0.003(3) -0.003(3)
C7 0.044(3) 0.029(2) 0.053(3) -0.006(2) 0.008(2) -0.002(2)
C9 0.0225(19) 0.0219(19) 0.025(2) -0.0020(16) 0.0036(16) -0.0001(16)
C10 0.031(2) 0.030(2) 0.020(2) -0.0053(17) 0.0005(17) 0.0013(18)
C11 0.036(2) 0.032(2) 0.024(2) 0.0024(18) 0.0052(18) 0.0017(19)
C12 0.026(2) 0.025(2) 0.021(2) -0.0033(16) -0.0005(16) 0.0048(17)
C13 0.046(3) 0.025(2) 0.029(2) -0.0045(18) 0.012(2) -0.009(2)
C14 0.028(2) 0.034(2) 0.030(2) 0.0036(19) 0.0032(18) -0.0084(19)
C15 0.028(2) 0.035(2) 0.035(3) -0.011(2) 0.0067(19) -0.001(2)
C16 0.030(2) 0.061(3) 0.060(4) 0.019(3) 0.008(2) 0.011(2)
C17 0.049(3) 0.052(3) 0.057(4) 0.017(3) 0.015(3) -0.002(3)

_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 N3 1.962(3) . ?
Cu1 N1 1.966(3) . ?
Cu1 N2 2.034(3) . ?
Cu1 N4 2.033(3) . ?
S1 C3 1.755(4) . ?
S1 C2 1.766(4) . ?
S2 C3 1.743(4) . ?
S2 C1 1.778(4) . ?
S3 C4 1.754(5) . ?
S3 C6 1.763(4) . ?
S4 C5 1.768(5) . ?
S4 C4 1.765(4) . ?
S5 C6 1.744(5) . ?
S5 C8 1.809(6) . ?
S6 C5 1.738(4) . ?
S6 C7 1.801(5) . ?
O1 C9 1.265(5) . ?
O2 C12 1.254(5) . ?
O3 C15 1.237(6) . ?
O4 H4C 0.95(6) . ?
O4 H4D 0.82(7) . ?
N1 C9 1.314(5) . ?
N1 C10 1.469(5) . ?
N2 C11 1.474(5) . ?
N2 H2A 0.9100 . ?
N2 H2B 0.9100 . ?
N3 C12 1.318(5) . ?
N3 C13 1.475(5) . ?
N4 C14 1.473(6) . ?
N4 H4A 0.9100 . ?
N4 H4B 0.9100 . ?
N5 C15 1.317(6) . ?
N5 C17 1.443(6) . ?
N5 C16 1.455(6) . ?
C1 C2 1.351(6) . ?
C1 C9 1.503(6) . ?
C2 C12 1.510(6) . ?
C3 C4 1.338(6) . ?
C6 C5 1.358(6) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 H8C 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 H7C 0.9700 . ?
C10 C11 1.502(6) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C13 C14 1.511(6) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C15 H15 0.9400 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 H16C 0.9700 . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 H17C 0.9700 . ?

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
N3 Cu1 N1 99.09(14) . . ?
N3 Cu1 N2 164.96(14) . . ?
N1 Cu1 N2 82.26(14) . . ?
N3 Cu1 N4 84.60(14) . . ?
N1 Cu1 N4 164.92(14) . . ?
N2 Cu1 N4 90.45(14) . . ?
C3 S1 C2 93.16(19) . . ?
C3 S2 C1 93.19(19) . . ?
C4 S3 C6 94.3(2) . . ?
C5 S4 C4 94.0(2) . . ?
C6 S5 C8 102.1(3) . . ?
C5 S6 C7 101.5(2) . . ?
H4C O4 H4D 101(6) . . ?
C9 N1 C10 113.3(3) . . ?
C9 N1 Cu1 132.6(3) . . ?
C10 N1 Cu1 113.0(3) . . ?
C11 N2 Cu1 102.1(2) . . ?
C11 N2 H2A 111.3 . . ?
Cu1 N2 H2A 111.3 . . ?
C11 N2 H2B 111.3 . . ?
Cu1 N2 H2B 111.3 . . ?
H2A N2 H2B 109.2 . . ?
C12 N3 C13 115.8(3) . . ?
C12 N3 Cu1 134.5(3) . . ?
C13 N3 Cu1 109.3(3) . . ?
C14 N4 Cu1 109.6(3) . . ?
C14 N4 H4A 109.8 . . ?
Cu1 N4 H4A 109.8 . . ?
C14 N4 H4B 109.8 . . ?
Cu1 N4 H4B 109.8 . . ?
H4A N4 H4B 108.2 . . ?
C15 N5 C17 121.3(4) . . ?
C15 N5 C16 122.2(4) . . ?
C17 N5 C16 116.4(4) . . ?
C2 C1 C9 135.8(4) . . ?
C2 C1 S2 116.0(3) . . ?
C9 C1 S2 108.0(3) . . ?
C1 C2 C12 134.2(4) . . ?
C1 C2 S1 116.2(3) . . ?
C12 C2 S1 109.3(3) . . ?
C4 C3 S2 123.5(3) . . ?
C4 C3 S1 123.8(3) . . ?
S2 C3 S1 112.7(2) . . ?
C3 C4 S3 124.8(3) . . ?
C3 C4 S4 122.1(3) . . ?
S3 C4 S4 113.1(2) . . ?
C5 C6 S5 126.7(4) . . ?
C5 C6 S3 116.7(3) . . ?
S5 C6 S3 116.7(3) . . ?
C6 C5 S6 124.6(4) . . ?
C6 C5 S4 116.4(3) . . ?
S6 C5 S4 118.8(3) . . ?
S5 C8 H8A 109.5 . . ?
S5 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
S5 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
S6 C7 H7A 109.5 . . ?
S6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
S6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O1 C9 N1 125.3(4) . . ?
O1 C9 C1 113.7(3) . . ?
N1 C9 C1 121.0(3) . . ?
N1 C10 C11 108.3(3) . . ?
N1 C10 H10A 110.0 . . ?
C11 C10 H10A 110.0 . . ?
N1 C10 H10B 110.0 . . ?
C11 C10 H10B 110.0 . . ?
H10A C10 H10B 108.4 . . ?
N2 C11 C10 108.1(3) . . ?
N2 C11 H11A 110.1 . . ?
C10 C11 H11A 110.1 . . ?
N2 C11 H11B 110.1 . . ?
C10 C11 H11B 110.1 . . ?
H11A C11 H11B 108.4 . . ?
O2 C12 N3 126.5(4) . . ?
O2 C12 C2 113.9(4) . . ?
N3 C12 C2 119.6(4) . . ?
N3 C13 C14 107.8(3) . . ?
N3 C13 H13A 110.2 . . ?
C14 C13 H13A 110.2 . . ?
N3 C13 H13B 110.2 . . ?
C14 C13 H13B 110.2 . . ?
H13A C13 H13B 108.5 . . ?
N4 C14 C13 109.0(3) . . ?
N4 C14 H14A 109.9 . . ?
C13 C14 H14A 109.9 . . ?
N4 C14 H14B 109.9 . . ?
C13 C14 H14B 109.9 . . ?
H14A C14 H14B 108.3 . . ?
O3 C15 N5 126.8(4) . . ?
O3 C15 H15 116.6 . . ?
N5 C15 H15 116.6 . . ?
N5 C16 H16A 109.5 . . ?
N5 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
N5 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N5 C17 H17A 109.5 . . ?
N5 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N5 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 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
N3 Cu1 N1 C9 -44.0(4) . . . . ?
N2 Cu1 N1 C9 151.1(4) . . . . ?
N4 Cu1 N1 C9 -147.2(5) . . . . ?
N3 Cu1 N1 C10 148.4(3) . . . . ?
N2 Cu1 N1 C10 -16.4(3) . . . . ?
N4 Cu1 N1 C10 45.3(7) . . . . ?
N3 Cu1 N2 C11 -57.7(6) . . . . ?
N1 Cu1 N2 C11 38.5(3) . . . . ?
N4 Cu1 N2 C11 -128.2(3) . . . . ?
N1 Cu1 N3 C12 44.2(4) . . . . ?
N2 Cu1 N3 C12 138.2(5) . . . . ?
N4 Cu1 N3 C12 -150.5(4) . . . . ?
N1 Cu1 N3 C13 -143.4(3) . . . . ?
N2 Cu1 N3 C13 -49.4(7) . . . . ?
N4 Cu1 N3 C13 21.8(3) . . . . ?
N3 Cu1 N4 C14 4.6(3) . . . . ?
N1 Cu1 N4 C14 109.6(6) . . . . ?
N2 Cu1 N4 C14 170.3(3) . . . . ?
C3 S2 C1 C2 -16.6(3) . . . . ?
C3 S2 C1 C9 167.5(3) . . . . ?
C9 C1 C2 C12 0.5(8) . . . . ?
S2 C1 C2 C12 -173.9(4) . . . . ?
C9 C1 C2 S1 173.7(4) . . . . ?
S2 C1 C2 S1 -0.7(4) . . . . ?
C3 S1 C2 C1 17.5(3) . . . . ?
C3 S1 C2 C12 -167.6(3) . . . . ?
C1 S2 C3 C4 -151.1(4) . . . . ?
C1 S2 C3 S1 28.2(2) . . . . ?
C2 S1 C3 C4 150.7(4) . . . . ?
C2 S1 C3 S2 -28.6(3) . . . . ?
S2 C3 C4 S3 -179.3(2) . . . . ?
S1 C3 C4 S3 1.6(6) . . . . ?
S2 C3 C4 S4 1.0(6) . . . . ?
S1 C3 C4 S4 -178.1(2) . . . . ?
C6 S3 C4 C3 -157.1(4) . . . . ?
C6 S3 C4 S4 22.7(3) . . . . ?
C5 S4 C4 C3 156.9(4) . . . . ?
C5 S4 C4 S3 -22.8(3) . . . . ?
C8 S5 C6 C5 -65.2(5) . . . . ?
C8 S5 C6 S3 113.8(3) . . . . ?
C4 S3 C6 C5 -13.5(4) . . . . ?
C4 S3 C6 S5 167.4(3) . . . . ?
S5 C6 C5 S6 3.1(6) . . . . ?
S3 C6 C5 S6 -175.9(2) . . . . ?
S5 C6 C5 S4 178.6(3) . . . . ?
S3 C6 C5 S4 -0.4(5) . . . . ?
C7 S6 C5 C6 -136.8(4) . . . . ?
C7 S6 C5 S4 47.8(3) . . . . ?
C4 S4 C5 C6 14.0(4) . . . . ?
C4 S4 C5 S6 -170.2(3) . . . . ?
C10 N1 C9 O1 -2.0(6) . . . . ?
Cu1 N1 C9 O1 -169.5(3) . . . . ?
C10 N1 C9 C1 176.2(3) . . . . ?
Cu1 N1 C9 C1 8.7(6) . . . . ?
C2 C1 C9 O1 -155.0(5) . . . . ?
S2 C1 C9 O1 19.7(4) . . . . ?
C2 C1 C9 N1 26.7(7) . . . . ?
S2 C1 C9 N1 -158.6(3) . . . . ?
C9 N1 C10 C11 180.0(4) . . . . ?
Cu1 N1 C10 C11 -9.9(4) . . . . ?
Cu1 N2 C11 C10 -54.3(4) . . . . ?
N1 C10 C11 N2 43.3(4) . . . . ?
C13 N3 C12 O2 -2.6(6) . . . . ?
Cu1 N3 C12 O2 169.4(3) . . . . ?
C13 N3 C12 C2 -179.8(3) . . . . ?
Cu1 N3 C12 C2 -7.8(6) . . . . ?
C1 C2 C12 O2 155.0(4) . . . . ?
S1 C2 C12 O2 -18.6(4) . . . . ?
C1 C2 C12 N3 -27.5(7) . . . . ?
S1 C2 C12 N3 158.9(3) . . . . ?
C12 N3 C13 C14 130.6(4) . . . . ?
Cu1 N3 C13 C14 -43.4(4) . . . . ?
Cu1 N4 C14 C13 -29.3(4) . . . . ?
N3 C13 C14 N4 47.6(5) . . . . ?
C17 N5 C15 O3 179.1(5) . . . . ?
C16 N5 C15 O3 1.3(8) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O4 H4C O3 0.95(6) 1.86(6) 2.783(5) 163(5) .
O4 H4D O1 0.82(7) 1.97(7) 2.786(5) 173(7) 1_655
N2 H2A O2 0.91 2.10 2.875(5) 142.0 4_575
N2 H2B O1 0.91 2.24 3.135(5) 166.1 3_566
N4 H4A O4 0.91 2.09 2.967(6) 160.1 .
N4 H4B O2 0.91 2.29 3.098(5) 147.8 4_575
N4 H4B S1 0.91 2.83 3.582(4) 140.6 4_575

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         0.399
_refine_diff_density_min         -0.591
_refine_diff_density_rms         0.088

########################END

data_4
_database_code_depnum_ccdc_archive 'CCDC 750343'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H18 N4 Ni O2 S6, 1.5(C H4 O)'
_chemical_formula_sum            'C15.50 H24 N4 Ni O3.50 S6'
_chemical_formula_weight         573.46

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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_Int_Tables_number      15

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                   19.402(3)
_cell_length_b                   19.006(2)
_cell_length_c                   14.2876(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 119.731(2)
_cell_angle_gamma                90.00
_cell_volume                     4575.1(10)
_cell_formula_units_Z            8
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    7338
_cell_measurement_theta_min      3.0
_cell_measurement_theta_max      25.3

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.665
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2376
_exptl_absorpt_coefficient_mu    1.425
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.642
_exptl_absorpt_correction_T_max  0.796
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71070
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean 7.31
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            22163
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_sigmaI/netI    0.0297
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.03
_diffrn_reflns_theta_max         25.35
_reflns_number_total             4190
_reflns_number_gt                3689
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       CrystalClear
_computing_cell_refinement       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0461P)^2^+19.9986P] where P=(Fo^2^+2Fc^2^)/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         4190
_refine_ls_number_parameters     271
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0513
_refine_ls_wR_factor_ref         0.1210
_refine_ls_wR_factor_gt          0.1143
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_restrained_S_all      1.130
_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 0.68531(3) 0.41538(3) 0.45653(4) 0.03078(17) Uani 1 1 d . . .
S1 S 0.77702(7) 0.26733(6) 0.79588(9) 0.0365(3) Uani 1 1 d . . .
S2 S 0.67318(8) 0.37587(6) 0.80184(10) 0.0433(3) Uani 1 1 d . . .
S3 S 0.70402(6) 0.15220(5) 0.88653(9) 0.0333(3) Uani 1 1 d . . .
S4 S 0.60009(7) 0.25805(5) 0.90163(9) 0.0348(3) Uani 1 1 d . . .
S5 S 0.61342(8) 0.02973(6) 0.90272(10) 0.0468(3) Uani 1 1 d . . .
S6 S 0.49155(7) 0.15242(7) 0.91656(10) 0.0435(3) Uani 1 1 d . . .
O1 O 0.85259(18) 0.2847(2) 0.6848(3) 0.0511(9) Uani 1 1 d . . .
O2 O 0.6592(2) 0.50085(15) 0.7030(3) 0.0495(9) Uani 1 1 d . . .
O3 O 0.5230(3) 0.3553(3) 0.1620(5) 0.1015(17) Uani 1 1 d . . .
H3 H 0.5462 0.3226 0.2061 0.152 Uiso 1 1 calc R . .
O4 O 0.5000 0.2454(6) 0.2500 0.137(3) Uiso 1 2 d SD . .
N1 N 0.7741(2) 0.36135(19) 0.5507(3) 0.0333(8) Uani 1 1 d . . .
N2 N 0.7038(2) 0.37629(19) 0.3468(3) 0.0351(8) Uani 1 1 d . . .
H2A H 0.6847 0.3310 0.3301 0.042 Uiso 1 1 calc R . .
H2B H 0.6801 0.4032 0.2852 0.042 Uiso 1 1 calc R . .
N3 N 0.6676(2) 0.46723(18) 0.5552(3) 0.0324(8) Uani 1 1 d . . .
N4 N 0.5978(2) 0.46732(18) 0.3479(3) 0.0351(8) Uani 1 1 d . . .
H4A H 0.6144 0.4922 0.3073 0.042 Uiso 1 1 calc R . .
H4B H 0.5589 0.4365 0.3028 0.042 Uiso 1 1 calc R . .
C1 C 0.7506(3) 0.3369(2) 0.7012(3) 0.0332(9) Uani 1 1 d . . .
C2 C 0.7034(3) 0.3871(2) 0.7047(3) 0.0333(9) Uani 1 1 d . . .
C3 C 0.7019(3) 0.2872(2) 0.8257(3) 0.0348(10) Uani 1 1 d . . .
C4 C 0.6720(2) 0.2400(2) 0.8644(3) 0.0287(9) Uani 1 1 d . . .
C5 C 0.6215(2) 0.1207(2) 0.8928(3) 0.0304(9) Uani 1 1 d . . .
C6 C 0.5742(2) 0.1693(2) 0.9010(3) 0.0321(9) Uani 1 1 d . . .
C7 C 0.6148(3) -0.0011(2) 0.7846(4) 0.0478(12) Uani 1 1 d . . .
H7A H 0.5740 0.0237 0.7210 0.072 Uiso 1 1 calc R . .
H7B H 0.6040 -0.0517 0.7762 0.072 Uiso 1 1 calc R . .
H7C H 0.6670 0.0080 0.7922 0.072 Uiso 1 1 calc R . .
C8 C 0.5373(3) 0.1134(3) 1.0488(4) 0.0544(13) Uani 1 1 d . . .
H8A H 0.5704 0.0736 1.0517 0.082 Uiso 1 1 calc R . .
H8B H 0.4960 0.0968 1.0640 0.082 Uiso 1 1 calc R . .
H8C H 0.5703 0.1486 1.1027 0.082 Uiso 1 1 calc R . .
C9 C 0.7950(2) 0.3279(2) 0.6417(3) 0.0360(10) Uani 1 1 d . . .
C10 C 0.8226(3) 0.3407(3) 0.5021(4) 0.0429(11) Uani 1 1 d . . .
H10A H 0.8200 0.2891 0.4912 0.051 Uiso 1 1 calc R . .
H10B H 0.8788 0.3540 0.5504 0.051 Uiso 1 1 calc R . .
C11 C 0.7911(3) 0.3776(3) 0.3964(4) 0.0418(11) Uani 1 1 d . . .
H11A H 0.8107 0.4267 0.4073 0.050 Uiso 1 1 calc R . .
H11B H 0.8079 0.3530 0.3499 0.050 Uiso 1 1 calc R . .
C12 C 0.6765(3) 0.4566(2) 0.6518(3) 0.0363(10) Uani 1 1 d . . .
C13 C 0.6305(3) 0.5344(2) 0.5044(3) 0.0418(11) Uani 1 1 d . . .
H13A H 0.6694 0.5655 0.4995 0.050 Uiso 1 1 calc R . .
H13B H 0.6098 0.5586 0.5468 0.050 Uiso 1 1 calc R . .
C14 C 0.5643(3) 0.5166(2) 0.3947(4) 0.0414(11) Uani 1 1 d . . .
H14A H 0.5199 0.4943 0.3993 0.050 Uiso 1 1 calc R . .
H14B H 0.5442 0.5595 0.3499 0.050 Uiso 1 1 calc R . .
C15 C 0.4962(5) 0.3311(5) 0.0589(8) 0.137(4) Uani 1 1 d . . .
H15A H 0.4779 0.3710 0.0088 0.206 Uiso 1 1 calc R . .
H15B H 0.4522 0.2983 0.0392 0.206 Uiso 1 1 calc R . .
H15C H 0.5395 0.3070 0.0554 0.206 Uiso 1 1 calc R . .
C16 C 0.5000 0.1679(11) 0.2500 0.303(15) Uiso 1 2 d SD . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni1 0.0368(3) 0.0320(3) 0.0261(3) 0.0004(2) 0.0176(2) -0.0057(2)
S1 0.0406(6) 0.0429(6) 0.0311(6) 0.0059(5) 0.0217(5) -0.0013(5)
S2 0.0802(9) 0.0272(5) 0.0431(6) 0.0017(5) 0.0463(7) -0.0016(5)
S3 0.0384(6) 0.0314(5) 0.0366(6) 0.0077(4) 0.0235(5) 0.0056(4)
S4 0.0484(6) 0.0281(5) 0.0387(6) 0.0027(4) 0.0298(5) 0.0032(5)
S5 0.0697(8) 0.0273(6) 0.0539(7) 0.0030(5) 0.0386(7) -0.0026(5)
S6 0.0369(6) 0.0516(7) 0.0486(7) -0.0048(6) 0.0262(6) -0.0060(5)
O1 0.0336(17) 0.076(2) 0.0449(19) 0.0210(18) 0.0208(15) 0.0063(17)
O2 0.094(3) 0.0269(16) 0.0429(18) -0.0002(14) 0.0459(19) -0.0029(16)
O3 0.074(3) 0.092(4) 0.116(4) -0.036(3) 0.031(3) -0.014(3)
N1 0.0295(18) 0.047(2) 0.0271(18) 0.0043(16) 0.0167(15) -0.0039(16)
N2 0.047(2) 0.0344(19) 0.0269(18) 0.0003(15) 0.0209(17) -0.0018(16)
N3 0.043(2) 0.0296(18) 0.0246(17) 0.0023(14) 0.0171(16) -0.0058(15)
N4 0.043(2) 0.0280(18) 0.0276(18) -0.0024(14) 0.0129(16) -0.0031(16)
C1 0.040(2) 0.036(2) 0.025(2) 0.0032(17) 0.0163(19) -0.0115(19)
C2 0.047(3) 0.033(2) 0.024(2) -0.0052(17) 0.0210(19) -0.011(2)
C3 0.051(3) 0.034(2) 0.027(2) 0.0017(17) 0.025(2) 0.000(2)
C4 0.039(2) 0.029(2) 0.0214(19) 0.0000(16) 0.0176(18) 0.0006(17)
C5 0.037(2) 0.028(2) 0.029(2) 0.0024(17) 0.0185(19) -0.0020(18)
C6 0.038(2) 0.032(2) 0.032(2) 0.0011(18) 0.0219(19) -0.0029(18)
C7 0.058(3) 0.034(2) 0.042(3) 0.000(2) 0.019(2) 0.008(2)
C8 0.055(3) 0.069(4) 0.050(3) 0.005(3) 0.034(3) -0.008(3)
C9 0.028(2) 0.049(3) 0.032(2) 0.001(2) 0.0158(19) -0.009(2)
C10 0.035(2) 0.064(3) 0.036(2) 0.005(2) 0.022(2) -0.003(2)
C11 0.041(3) 0.053(3) 0.042(3) 0.002(2) 0.029(2) -0.008(2)
C12 0.055(3) 0.028(2) 0.034(2) -0.0008(18) 0.028(2) -0.011(2)
C13 0.063(3) 0.031(2) 0.033(2) 0.0006(19) 0.026(2) -0.002(2)
C14 0.051(3) 0.037(2) 0.037(2) 0.000(2) 0.022(2) -0.001(2)
C15 0.079(5) 0.163(9) 0.167(9) -0.114(8) 0.060(6) -0.013(6)

_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 N1 1.879(3) . ?
Ni1 N3 1.886(3) . ?
Ni1 N4 1.911(3) . ?
Ni1 N2 1.922(3) . ?
S1 C3 1.750(4) . ?
S1 C1 1.776(4) . ?
S2 C3 1.755(4) . ?
S2 C2 1.767(4) . ?
S3 C5 1.753(4) . ?
S3 C4 1.754(4) . ?
S4 C4 1.757(4) . ?
S4 C6 1.758(4) . ?
S5 C5 1.748(4) . ?
S5 C7 1.799(5) . ?
S6 C6 1.755(4) . ?
S6 C8 1.802(5) . ?
O1 C9 1.271(5) . ?
O2 C12 1.264(5) . ?
O3 C15 1.375(9) . ?
O3 H3 0.8400 . ?
O4 C16 1.473(18) . ?
N1 C9 1.318(5) . ?
N1 C10 1.474(5) . ?
N2 C11 1.478(6) . ?
N2 H2A 0.9200 . ?
N2 H2B 0.9200 . ?
N3 C12 1.320(5) . ?
N3 C13 1.468(5) . ?
N4 C14 1.476(6) . ?
N4 H4A 0.9200 . ?
N4 H4B 0.9200 . ?
C1 C2 1.341(6) . ?
C1 C9 1.491(6) . ?
C2 C12 1.482(6) . ?
C3 C4 1.328(6) . ?
C5 C6 1.347(6) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C10 C11 1.493(6) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C13 C14 1.492(6) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ni1 N3 101.10(15) . . ?
N1 Ni1 N4 173.29(15) . . ?
N3 Ni1 N4 85.39(15) . . ?
N1 Ni1 N2 84.10(15) . . ?
N3 Ni1 N2 171.22(15) . . ?
N4 Ni1 N2 89.25(15) . . ?
C3 S1 C1 93.7(2) . . ?
C3 S2 C2 94.1(2) . . ?
C5 S3 C4 94.79(19) . . ?
C4 S4 C6 94.53(19) . . ?
C5 S5 C7 101.7(2) . . ?
C6 S6 C8 101.7(2) . . ?
C15 O3 H3 109.5 . . ?
C9 N1 C10 112.3(4) . . ?
C9 N1 Ni1 134.0(3) . . ?
C10 N1 Ni1 112.4(3) . . ?
C11 N2 Ni1 103.6(3) . . ?
C11 N2 H2A 111.0 . . ?
Ni1 N2 H2A 111.0 . . ?
C11 N2 H2B 111.0 . . ?
Ni1 N2 H2B 111.0 . . ?
H2A N2 H2B 109.0 . . ?
C12 N3 C13 115.3(4) . . ?
C12 N3 Ni1 136.4(3) . . ?
C13 N3 Ni1 108.2(2) . . ?
C14 N4 Ni1 111.9(3) . . ?
C14 N4 H4A 109.2 . . ?
Ni1 N4 H4A 109.2 . . ?
C14 N4 H4B 109.2 . . ?
Ni1 N4 H4B 109.2 . . ?
H4A N4 H4B 107.9 . . ?
C2 C1 C9 134.6(4) . . ?
C2 C1 S1 116.5(3) . . ?
C9 C1 S1 108.6(3) . . ?
C1 C2 C12 133.6(4) . . ?
C1 C2 S2 116.3(3) . . ?
C12 C2 S2 109.7(3) . . ?
C4 C3 S1 123.0(3) . . ?
C4 C3 S2 124.5(3) . . ?
S1 C3 S2 112.5(2) . . ?
C3 C4 S3 121.9(3) . . ?
C3 C4 S4 124.8(3) . . ?
S3 C4 S4 113.2(2) . . ?
C6 C5 S5 125.4(3) . . ?
C6 C5 S3 116.7(3) . . ?
S5 C5 S3 117.6(2) . . ?
C5 C6 S6 126.2(3) . . ?
C5 C6 S4 117.0(3) . . ?
S6 C6 S4 116.8(2) . . ?
S5 C7 H7A 109.5 . . ?
S5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
S5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
S6 C8 H8A 109.5 . . ?
S6 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
S6 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O1 C9 N1 123.9(4) . . ?
O1 C9 C1 114.5(4) . . ?
N1 C9 C1 121.6(4) . . ?
N1 C10 C11 108.3(4) . . ?
N1 C10 H10A 110.0 . . ?
C11 C10 H10A 110.0 . . ?
N1 C10 H10B 110.0 . . ?
C11 C10 H10B 110.0 . . ?
H10A C10 H10B 108.4 . . ?
N2 C11 C10 105.9(3) . . ?
N2 C11 H11A 110.6 . . ?
C10 C11 H11A 110.6 . . ?
N2 C11 H11B 110.6 . . ?
C10 C11 H11B 110.6 . . ?
H11A C11 H11B 108.7 . . ?
O2 C12 N3 124.7(4) . . ?
O2 C12 C2 115.2(4) . . ?
N3 C12 C2 120.0(4) . . ?
N3 C13 C14 106.2(4) . . ?
N3 C13 H13A 110.5 . . ?
C14 C13 H13A 110.5 . . ?
N3 C13 H13B 110.5 . . ?
C14 C13 H13B 110.5 . . ?
H13A C13 H13B 108.7 . . ?
N4 C14 C13 106.1(4) . . ?
N4 C14 H14A 110.5 . . ?
C13 C14 H14A 110.5 . . ?
N4 C14 H14B 110.5 . . ?
C13 C14 H14B 110.5 . . ?
H14A C14 H14B 108.7 . . ?
O3 C15 H15A 109.5 . . ?
O3 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O3 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 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
N3 Ni1 N1 C9 40.4(4) . . . . ?
N4 Ni1 N1 C9 -154.5(11) . . . . ?
N2 Ni1 N1 C9 -146.8(4) . . . . ?
N3 Ni1 N1 C10 -153.8(3) . . . . ?
N4 Ni1 N1 C10 11.3(14) . . . . ?
N2 Ni1 N1 C10 19.1(3) . . . . ?
N1 Ni1 N2 C11 -40.4(3) . . . . ?
N3 Ni1 N2 C11 86.4(10) . . . . ?
N4 Ni1 N2 C11 138.6(3) . . . . ?
N1 Ni1 N3 C12 -32.6(5) . . . . ?
N4 Ni1 N3 C12 149.1(5) . . . . ?
N2 Ni1 N3 C12 -158.4(9) . . . . ?
N1 Ni1 N3 C13 151.5(3) . . . . ?
N4 Ni1 N3 C13 -26.7(3) . . . . ?
N2 Ni1 N3 C13 25.8(11) . . . . ?
N1 Ni1 N4 C14 -165.8(12) . . . . ?
N3 Ni1 N4 C14 -0.5(3) . . . . ?
N2 Ni1 N4 C14 -173.6(3) . . . . ?
C3 S1 C1 C2 16.2(4) . . . . ?
C3 S1 C1 C9 -169.5(3) . . . . ?
C9 C1 C2 C12 -1.5(9) . . . . ?
S1 C1 C2 C12 170.9(4) . . . . ?
C9 C1 C2 S2 -173.4(4) . . . . ?
S1 C1 C2 S2 -1.0(5) . . . . ?
C3 S2 C2 C1 -14.7(4) . . . . ?
C3 S2 C2 C12 171.5(3) . . . . ?
C1 S1 C3 C4 155.8(4) . . . . ?
C1 S1 C3 S2 -25.6(3) . . . . ?
C2 S2 C3 C4 -156.1(4) . . . . ?
C2 S2 C3 S1 25.3(3) . . . . ?
S1 C3 C4 S3 -1.4(5) . . . . ?
S2 C3 C4 S3 -179.8(2) . . . . ?
S1 C3 C4 S4 176.8(2) . . . . ?
S2 C3 C4 S4 -1.6(6) . . . . ?
C5 S3 C4 C3 -162.4(4) . . . . ?
C5 S3 C4 S4 19.2(2) . . . . ?
C6 S4 C4 C3 163.0(4) . . . . ?
C6 S4 C4 S3 -18.6(3) . . . . ?
C7 S5 C5 C6 130.2(4) . . . . ?
C7 S5 C5 S3 -57.3(3) . . . . ?
C4 S3 C5 C6 -12.4(4) . . . . ?
C4 S3 C5 S5 174.4(2) . . . . ?
S5 C5 C6 S6 -3.4(6) . . . . ?
S3 C5 C6 S6 -176.0(2) . . . . ?
S5 C5 C6 S4 173.8(2) . . . . ?
S3 C5 C6 S4 1.3(5) . . . . ?
C8 S6 C6 C5 66.7(4) . . . . ?
C8 S6 C6 S4 -110.6(3) . . . . ?
C4 S4 C6 C5 10.6(4) . . . . ?
C4 S4 C6 S6 -171.9(2) . . . . ?
C10 N1 C9 O1 2.6(6) . . . . ?
Ni1 N1 C9 O1 168.4(3) . . . . ?
C10 N1 C9 C1 -175.9(4) . . . . ?
Ni1 N1 C9 C1 -10.0(7) . . . . ?
C2 C1 C9 O1 158.2(5) . . . . ?
S1 C1 C9 O1 -14.7(5) . . . . ?
C2 C1 C9 N1 -23.2(7) . . . . ?
S1 C1 C9 N1 163.9(3) . . . . ?
C9 N1 C10 C11 176.3(4) . . . . ?
Ni1 N1 C10 C11 7.2(5) . . . . ?
Ni1 N2 C11 C10 53.2(4) . . . . ?
N1 C10 C11 N2 -39.4(5) . . . . ?
C13 N3 C12 O2 -3.8(7) . . . . ?
Ni1 N3 C12 O2 -179.4(3) . . . . ?
C13 N3 C12 C2 172.0(4) . . . . ?
Ni1 N3 C12 C2 -3.7(7) . . . . ?
C1 C2 C12 O2 -153.0(5) . . . . ?
S2 C2 C12 O2 19.3(5) . . . . ?
C1 C2 C12 N3 30.9(7) . . . . ?
S2 C2 C12 N3 -156.9(4) . . . . ?
C12 N3 C13 C14 -128.8(4) . . . . ?
Ni1 N3 C13 C14 48.1(4) . . . . ?
Ni1 N4 C14 C13 26.9(4) . . . . ?
N3 C13 C14 N4 -47.5(5) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C13 H13A S3 0.99 2.73 3.577(5) 144.3 4_656
C11 H11B S1 0.99 2.98 3.644(5) 125.4 7_656
N4 H4B O3 0.92 2.44 3.117(6) 130.6 2_655
N4 H4B O3 0.92 2.35 3.141(6) 144.2 .
N4 H4A S2 0.92 2.77 3.523(4) 139.4 6_565
N4 H4A O2 0.92 2.07 2.918(5) 152.8 6_565
N2 H2B O2 0.92 2.10 2.942(5) 152.3 6_565
N2 H2A S1 0.92 2.94 3.536(4) 124.2 7_656
N2 H2A O1 0.92 2.29 3.205(5) 171.6 7_656
O3 H3 O4 0.84 1.98 2.587(11) 128.9 .

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.35
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.285
_refine_diff_density_min         -0.826
_refine_diff_density_rms         0.087

############################END