# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2007

data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'Xian-He Bu'
_publ_contact_author_address     
;
Department of Chemistry
Nankai University
Tianjin
300071
CHINA
;

_publ_contact_author_email       BUXH@NANKAI.EDU.CN

_publ_section_title              
;
Magnetic Canting or Not? Two Isostructural 3D CoII and
NiII Coordination Polymers with the Rare Non-interpenetrated (10,3)-d
Topological Network, Showing Spin-canted Antiferromagnetism Only in the
CoII System
;
loop_
_publ_author_name
'Xian-He Bu.'
'S. Batten'
'Jian-Rong Li.'
'Joan Ribas'
'Qun Yu.'

data_1
_database_code_depnum_ccdc_archive 'CCDC 626633'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H4 Co2 N4 O10 S2'
_chemical_formula_sum            'C8 H4 Co2 N4 O10 S2'
_chemical_formula_weight         498.13

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)
_symmetry_space_group_name_Hall  'P 2yb'

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

_cell_length_a                   7.1024(14)
_cell_length_b                   7.0967(14)
_cell_length_c                   13.380(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.81(3)
_cell_angle_gamma                90.00
_cell_volume                     674.3(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6449
_cell_measurement_theta_min      3.05
_cell_measurement_theta_max      27.50

_exptl_crystal_description       Block
_exptl_crystal_colour            'Brownish red'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.453
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             492
_exptl_absorpt_coefficient_mu    2.842
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9637
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'

_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  'Rigaku R-AXIS RAPID IP'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean 10.000
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            6722
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_sigmaI/netI    0.0420
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.05
_diffrn_reflns_theta_max         27.48
_reflns_number_total             3068
_reflns_number_gt                2891
_reflns_threshold_expression     I>2sigma(I)

_computing_data_collection       'RAPID-AUTO (Rigaku, 2004)'
_computing_cell_refinement       RAPID-AUTO
_computing_data_reduction        "CrystalStructure (Rigaku/MSC'2004)"
_computing_structure_solution    SHELXS-97
_computing_structure_refinement  SHELXL-97
_computing_molecular_graphics    'SHELXTL (Bruker, 1998)'
_computing_publication_material  SHELXTL

_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^)+(0.0242P)^2^] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.002(1)
_refine_ls_number_reflns         3068
_refine_ls_number_parameters     247
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0247
_refine_ls_R_factor_gt           0.0226
_refine_ls_wR_factor_ref         0.0523
_refine_ls_wR_factor_gt          0.0515
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_restrained_S_all      1.009
_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
Co1 Co 0.73058(4) 0.50089(5) 0.679920(18) 0.01364(8) Uani 1 1 d . . .
Co2 Co 0.79070(4) 0.49944(5) 0.180662(18) 0.01391(8) Uani 1 1 d . . .
S1 S 0.68948(10) 0.36489(10) 0.42778(4) 0.01873(14) Uani 1 1 d . . .
S2 S 0.91189(8) 0.48716(12) -0.07410(4) 0.01766(12) Uani 1 1 d . . .
N1 N 0.7080(3) 0.5181(4) 0.51843(12) 0.0155(4) Uani 1 1 d . . .
N2 N 0.7610(3) 0.5071(4) 0.34040(12) 0.0151(4) Uani 1 1 d . . .
N3 N 0.7767(3) 0.5294(3) 0.02011(13) 0.0155(5) Uani 1 1 d . . .
N4 N 0.7501(3) 0.5191(4) -0.15989(12) 0.0147(4) Uani 1 1 d . . .
C1 C 0.7901(4) 0.8366(4) 0.56112(17) 0.0158(5) Uani 1 1 d . . .
C2 C 0.7720(4) 0.6804(4) 0.48375(17) 0.0138(5) Uani 1 1 d . . .
C3 C 0.8035(3) 0.6736(4) 0.37959(16) 0.0142(5) Uani 1 1 d . . .
C4 C 0.8970(4) 0.8106(4) 0.30966(17) 0.0166(5) Uani 1 1 d . . .
C5 C 0.4529(4) 0.5802(4) 0.06780(16) 0.0170(5) Uani 1 1 d . . .
C6 C 0.6025(3) 0.5677(4) -0.01253(15) 0.0139(5) Uani 1 1 d . . .
C7 C 0.5891(3) 0.5658(4) -0.11862(15) 0.0132(5) Uani 1 1 d . . .
C8 C 0.4346(3) 0.6307(4) -0.19006(17) 0.0161(5) Uani 1 1 d . . .
O1 O 0.7849(3) 0.7797(3) 0.65111(12) 0.0203(4) Uani 1 1 d . . .
O2 O 0.7992(3) 1.0018(4) 0.53547(12) 0.0321(4) Uani 1 1 d . . .
O3 O 0.9931(3) 0.9377(3) 0.34840(13) 0.0234(4) Uani 1 1 d . . .
O4 O 0.8792(3) 0.7739(3) 0.21804(12) 0.0235(4) Uani 1 1 d . . .
O5 O 0.6521(3) 0.2257(3) 0.67957(14) 0.0269(4) Uani 1 1 d D . .
H5A H 0.616(4) 0.181(4) 0.7350(13) 0.032 Uiso 1 1 d D . .
H5B H 0.729(4) 0.161(4) 0.6457(19) 0.032 Uiso 1 1 d D . .
O6 O 0.5177(3) 0.5887(3) 0.15637(12) 0.0240(4) Uani 1 1 d . . .
O7 O 0.2875(3) 0.5733(4) 0.04377(13) 0.0372(6) Uani 1 1 d . . .
O8 O 0.3038(3) 0.7259(3) -0.15531(13) 0.0233(4) Uani 1 1 d . . .
O9 O 0.4602(3) 0.5907(3) -0.28023(12) 0.0232(4) Uani 1 1 d . . .
O10 O 1.0632(3) 0.4191(3) 0.18072(13) 0.0235(4) Uani 1 1 d D . .
H10A H 1.141(3) 0.468(4) 0.1409(15) 0.028 Uiso 1 1 d D . .
H10B H 1.109(3) 0.378(4) 0.2361(12) 0.028 Uiso 1 1 d 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
Co1 0.01704(15) 0.01516(15) 0.00879(12) 0.00053(16) 0.00272(10) 0.00148(18)
Co2 0.01334(15) 0.01936(16) 0.00904(12) -0.00120(16) 0.00062(9) -0.00124(18)
S1 0.0286(4) 0.0168(3) 0.0108(2) -0.0005(2) 0.0009(2) -0.0068(3)
S2 0.0133(3) 0.0295(3) 0.0102(2) -0.0004(3) 0.00121(18) 0.0033(3)
N1 0.0205(10) 0.0175(12) 0.0087(7) 0.0000(10) 0.0014(6) -0.0004(10)
N2 0.0180(9) 0.0191(10) 0.0081(7) 0.0018(11) 0.0010(6) -0.0009(11)
N3 0.0168(10) 0.0198(14) 0.0099(8) -0.0010(9) 0.0011(7) 0.0012(9)
N4 0.0153(9) 0.0194(12) 0.0096(7) 0.0012(10) 0.0010(6) 0.0000(9)
C1 0.0136(12) 0.0191(14) 0.0149(10) -0.0015(10) 0.0046(9) -0.0004(10)
C2 0.0160(12) 0.0141(12) 0.0112(10) -0.0003(9) -0.0006(8) 0.0000(9)
C3 0.0108(12) 0.0184(12) 0.0135(10) -0.0008(9) 0.0007(9) 0.0008(9)
C4 0.0169(13) 0.0176(12) 0.0155(11) 0.0015(9) 0.0065(9) -0.0004(10)
C5 0.0165(13) 0.0223(12) 0.0123(10) 0.0024(10) 0.0035(9) 0.0043(10)
C6 0.0138(12) 0.0175(11) 0.0106(10) -0.0016(9) 0.0018(8) 0.0011(9)
C7 0.0151(12) 0.0139(10) 0.0105(10) 0.0010(9) 0.0023(8) 0.0000(9)
C8 0.0177(13) 0.0172(12) 0.0135(10) 0.0034(9) 0.0007(9) 0.0000(10)
O1 0.0334(11) 0.0168(9) 0.0107(7) -0.0024(7) -0.0013(7) -0.0014(8)
O2 0.0606(13) 0.0154(9) 0.0207(8) -0.0014(9) 0.0123(8) 0.0006(13)
O3 0.0223(10) 0.0254(10) 0.0227(8) -0.0066(8) 0.0082(7) -0.0103(8)
O4 0.0362(12) 0.0241(10) 0.0103(8) -0.0004(7) 0.0046(7) -0.0082(9)
O5 0.0400(13) 0.0177(10) 0.0235(9) 0.0003(8) 0.0153(9) -0.0021(9)
O6 0.0174(10) 0.0440(12) 0.0106(8) -0.0019(8) 0.0056(7) 0.0080(8)
O7 0.0177(10) 0.0762(18) 0.0179(8) 0.0089(10) 0.0051(7) -0.0003(10)
O8 0.0249(11) 0.0251(10) 0.0202(8) 0.0047(8) 0.0064(7) 0.0115(8)
O9 0.0211(10) 0.0365(11) 0.0121(8) 0.0025(8) -0.0006(7) 0.0066(8)
O10 0.0149(10) 0.0347(11) 0.0209(8) 0.0089(8) 0.0010(7) 0.0000(8)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O5 2.031(2) . ?
Co1 O3 2.0534(19) 2_746 ?
Co1 O1 2.0536(19) . ?
Co1 O9 2.099(2) 1_556 ?
Co1 N4 2.1498(17) 1_556 ?
Co1 N1 2.1680(17) . ?
Co2 O10 2.0178(19) . ?
Co2 O6 2.0611(19) . ?
Co2 O8 2.080(2) 2_645 ?
Co2 O4 2.105(2) . ?
Co2 N2 2.1513(16) . ?
Co2 N3 2.1596(17) . ?
S1 N2 1.631(2) . ?
S1 N1 1.633(2) . ?
S2 N3 1.623(2) . ?
S2 N4 1.6285(19) . ?
N1 C2 1.324(4) . ?
N2 C3 1.326(4) . ?
N3 C6 1.334(3) . ?
N4 C7 1.319(3) . ?
N4 Co1 2.1498(17) 1_554 ?
C1 O2 1.223(4) . ?
C1 O1 1.271(3) . ?
C1 C2 1.521(3) . ?
C2 C3 1.415(3) . ?
C3 C4 1.510(3) . ?
C4 O3 1.241(3) . ?
C4 O4 1.258(3) . ?
C5 O7 1.215(3) . ?
C5 O6 1.267(3) . ?
C5 C6 1.525(3) . ?
C6 C7 1.422(3) . ?
C7 C8 1.517(3) . ?
C8 O8 1.244(3) . ?
C8 O9 1.255(3) . ?
O3 Co1 2.0534(19) 2_756 ?
O5 H5A 0.849(10) . ?
O5 H5B 0.850(10) . ?
O8 Co2 2.080(2) 2_655 ?
O9 Co1 2.099(2) 1_554 ?
O10 H10A 0.845(10) . ?
O10 H10B 0.856(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
O5 Co1 O3 93.03(9) . 2_746 ?
O5 Co1 O1 168.08(7) . . ?
O3 Co1 O1 89.60(8) 2_746 . ?
O5 Co1 O9 92.32(9) . 1_556 ?
O3 Co1 O9 173.28(8) 2_746 1_556 ?
O1 Co1 O9 85.99(8) . 1_556 ?
O5 Co1 N4 94.25(9) . 1_556 ?
O3 Co1 N4 98.55(8) 2_746 1_556 ?
O1 Co1 N4 96.86(9) . 1_556 ?
O9 Co1 N4 77.00(7) 1_556 1_556 ?
O5 Co1 N1 92.04(9) . . ?
O3 Co1 N1 83.45(8) 2_746 . ?
O1 Co1 N1 76.70(9) . . ?
O9 Co1 N1 100.42(8) 1_556 . ?
N4 Co1 N1 173.29(12) 1_556 . ?
O10 Co2 O6 170.79(7) . . ?
O10 Co2 O8 92.51(8) . 2_645 ?
O6 Co2 O8 87.74(8) . 2_645 ?
O10 Co2 O4 88.74(8) . . ?
O6 Co2 O4 91.72(8) . . ?
O8 Co2 O4 175.47(7) 2_645 . ?
O10 Co2 N2 96.55(8) . . ?
O6 Co2 N2 92.51(7) . . ?
O8 Co2 N2 98.60(10) 2_645 . ?
O4 Co2 N2 76.92(9) . . ?
O10 Co2 N3 93.37(8) . . ?
O6 Co2 N3 77.46(8) . . ?
O8 Co2 N3 85.38(8) 2_645 . ?
O4 Co2 N3 98.89(8) . . ?
N2 Co2 N3 169.12(10) . . ?
N2 S1 N1 95.61(14) . . ?
N3 S2 N4 95.89(10) . . ?
C2 N1 S1 110.08(15) . . ?
C2 N1 Co1 112.17(16) . . ?
S1 N1 Co1 134.97(15) . . ?
C3 N2 S1 109.83(14) . . ?
C3 N2 Co2 112.98(18) . . ?
S1 N2 Co2 137.10(17) . . ?
C6 N3 S2 109.83(15) . . ?
C6 N3 Co2 112.02(15) . . ?
S2 N3 Co2 137.31(12) . . ?
C7 N4 S2 110.30(14) . . ?
C7 N4 Co1 112.85(14) . 1_554 ?
S2 N4 Co1 136.84(12) . 1_554 ?
O2 C1 O1 124.9(2) . . ?
O2 C1 C2 120.8(2) . . ?
O1 C1 C2 114.2(2) . . ?
N1 C2 C3 112.0(2) . . ?
N1 C2 C1 114.9(2) . . ?
C3 C2 C1 133.0(2) . . ?
N2 C3 C2 112.4(2) . . ?
N2 C3 C4 115.4(2) . . ?
C2 C3 C4 131.7(2) . . ?
O3 C4 O4 127.2(2) . . ?
O3 C4 C3 117.0(2) . . ?
O4 C4 C3 115.6(2) . . ?
O7 C5 O6 125.9(2) . . ?
O7 C5 C6 119.5(2) . . ?
O6 C5 C6 114.5(2) . . ?
N3 C6 C7 111.9(2) . . ?
N3 C6 C5 115.69(19) . . ?
C7 C6 C5 131.8(2) . . ?
N4 C7 C6 112.0(2) . . ?
N4 C7 C8 115.88(19) . . ?
C6 C7 C8 131.6(2) . . ?
O8 C8 O9 127.0(2) . . ?
O8 C8 C7 117.8(2) . . ?
O9 C8 C7 115.0(2) . . ?
C1 O1 Co1 119.48(16) . . ?
C4 O3 Co1 127.12(17) . 2_756 ?
C4 O4 Co2 116.66(17) . . ?
Co1 O5 H5A 116(2) . . ?
Co1 O5 H5B 110(2) . . ?
H5A O5 H5B 118.1(18) . . ?
C5 O6 Co2 117.48(16) . . ?
C8 O8 Co2 133.38(17) . 2_655 ?
C8 O9 Co1 117.28(16) . 1_554 ?
Co2 O10 H10A 121.3(19) . . ?
Co2 O10 H10B 116.7(18) . . ?
H10A O10 H10B 116.1(17) . . ?

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

N2 S1 N1 C2 -0.93(19) . . . . ?
N2 S1 N1 Co1 -159.84(16) . . . . ?
O5 Co1 N1 C2 -172.44(18) . . . . ?
O3 Co1 N1 C2 -79.62(17) 2_746 . . . ?
O1 Co1 N1 C2 11.52(17) . . . . ?
O9 Co1 N1 C2 94.83(18) 1_556 . . . ?
O5 Co1 N1 S1 -13.85(17) . . . . ?
O3 Co1 N1 S1 78.97(16) 2_746 . . . ?
O1 Co1 N1 S1 170.12(18) . . . . ?
O9 Co1 N1 S1 -106.58(16) 1_556 . . . ?
N1 S1 N2 C3 1.08(18) . . . . ?
N1 S1 N2 Co2 -175.13(17) . . . . ?
O10 Co2 N2 C3 89.63(17) . . . . ?
O6 Co2 N2 C3 -88.72(17) . . . . ?
O8 Co2 N2 C3 -176.81(16) 2_645 . . . ?
O4 Co2 N2 C3 2.46(16) . . . . ?
N3 Co2 N2 C3 -66.0(6) . . . . ?
O10 Co2 N2 S1 -94.24(18) . . . . ?
O6 Co2 N2 S1 87.41(18) . . . . ?
O8 Co2 N2 S1 -0.68(19) 2_645 . . . ?
O4 Co2 N2 S1 178.59(19) . . . . ?
N3 Co2 N2 S1 110.1(6) . . . . ?
N4 S2 N3 C6 0.5(2) . . . . ?
N4 S2 N3 Co2 168.74(18) . . . . ?
O10 Co2 N3 C6 174.25(19) . . . . ?
O6 Co2 N3 C6 -6.72(19) . . . . ?
O8 Co2 N3 C6 81.99(19) 2_645 . . . ?
O4 Co2 N3 C6 -96.50(19) . . . . ?
N2 Co2 N3 C6 -30.0(7) . . . . ?
O10 Co2 N3 S2 6.2(2) . . . . ?
O6 Co2 N3 S2 -174.7(2) . . . . ?
O8 Co2 N3 S2 -86.0(2) 2_645 . . . ?
O4 Co2 N3 S2 95.5(2) . . . . ?
N2 Co2 N3 S2 162.0(4) . . . . ?
N3 S2 N4 C7 1.0(3) . . . . ?
N3 S2 N4 Co1 -177.8(2) . . . 1_554 ?
S1 N1 C2 C3 0.5(3) . . . . ?
Co1 N1 C2 C3 164.57(16) . . . . ?
S1 N1 C2 C1 178.36(17) . . . . ?
Co1 N1 C2 C1 -17.6(3) . . . . ?
O2 C1 C2 N1 -160.7(2) . . . . ?
O1 C1 C2 N1 15.9(3) . . . . ?
O2 C1 C2 C3 16.5(4) . . . . ?
O1 C1 C2 C3 -166.8(3) . . . . ?
S1 N2 C3 C2 -0.9(3) . . . . ?
Co2 N2 C3 C2 176.27(16) . . . . ?
S1 N2 C3 C4 171.93(17) . . . . ?
Co2 N2 C3 C4 -10.9(2) . . . . ?
N1 C2 C3 N2 0.3(3) . . . . ?
C1 C2 C3 N2 -177.0(2) . . . . ?
N1 C2 C3 C4 -171.1(2) . . . . ?
C1 C2 C3 C4 11.6(5) . . . . ?
N2 C3 C4 O3 -156.8(2) . . . . ?
C2 C3 C4 O3 14.4(4) . . . . ?
N2 C3 C4 O4 18.2(3) . . . . ?
C2 C3 C4 O4 -170.6(3) . . . . ?
S2 N3 C6 C7 -1.8(3) . . . . ?
Co2 N3 C6 C7 -173.20(17) . . . . ?
S2 N3 C6 C5 170.85(19) . . . . ?
Co2 N3 C6 C5 -0.6(3) . . . . ?
O7 C5 C6 N3 -164.0(3) . . . . ?
O6 C5 C6 N3 12.9(4) . . . . ?
O7 C5 C6 C7 6.8(5) . . . . ?
O6 C5 C6 C7 -176.2(3) . . . . ?
S2 N4 C7 C6 -2.1(3) . . . . ?
Co1 N4 C7 C6 177.00(18) 1_554 . . . ?
S2 N4 C7 C8 170.41(19) . . . . ?
Co1 N4 C7 C8 -10.5(3) 1_554 . . . ?
N3 C6 C7 N4 2.6(3) . . . . ?
C5 C6 C7 N4 -168.5(3) . . . . ?
N3 C6 C7 C8 -168.4(3) . . . . ?
C5 C6 C7 C8 20.5(5) . . . . ?
N4 C7 C8 O8 -159.5(2) . . . . ?
C6 C7 C8 O8 11.2(4) . . . . ?
N4 C7 C8 O9 16.3(4) . . . . ?
C6 C7 C8 O9 -173.0(2) . . . . ?
O2 C1 O1 Co1 171.0(2) . . . . ?
C2 C1 O1 Co1 -5.4(3) . . . . ?
O5 Co1 O1 C1 -22.3(5) . . . . ?
O3 Co1 O1 C1 80.6(2) 2_746 . . . ?
O9 Co1 O1 C1 -104.5(2) 1_556 . . . ?
N4 Co1 O1 C1 179.12(19) 1_556 . . . ?
N1 Co1 O1 C1 -2.80(18) . . . . ?
O4 C4 O3 Co1 -49.0(4) . . . 2_756 ?
C3 C4 O3 Co1 125.3(2) . . . 2_756 ?
O3 C4 O4 Co2 158.4(2) . . . . ?
C3 C4 O4 Co2 -16.0(3) . . . . ?
O10 Co2 O4 C4 -89.0(2) . . . . ?
O6 Co2 O4 C4 100.2(2) . . . . ?
N2 Co2 O4 C4 8.01(19) . . . . ?
N3 Co2 O4 C4 177.77(19) . . . . ?
O7 C5 O6 Co2 157.3(3) . . . . ?
C6 C5 O6 Co2 -19.4(3) . . . . ?
O8 Co2 O6 C5 -70.8(2) 2_645 . . . ?
O4 Co2 O6 C5 113.7(2) . . . . ?
N2 Co2 O6 C5 -169.4(2) . . . . ?
N3 Co2 O6 C5 14.9(2) . . . . ?
O9 C8 O8 Co2 -58.0(4) . . . 2_655 ?
C7 C8 O8 Co2 117.3(2) . . . 2_655 ?
O8 C8 O9 Co1 161.8(2) . . . 1_554 ?
C7 C8 O9 Co1 -13.6(3) . . . 1_554 ?

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
O5 H5A O6 0.85(1) 1.87(1) 2.701(3) 167(3) 2_646
O5 H5B O2 0.85(1) 1.93(2) 2.719(3) 154(3) 1_545
O10 H10A O7 0.85(1) 1.84(1) 2.679(3) 173(2) 1_655
O10 H10B O1 0.856(9) 1.82(1) 2.671(2) 176(3) 2_746

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.245
_refine_diff_density_min         -0.419
_refine_diff_density_rms         0.069

#====end

data_2
_database_code_depnum_ccdc_archive 'CCDC 626634'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H4 N4 Ni2 O10 S2'
_chemical_formula_sum            'C8 H4 N4 Ni2 O10 S2'
_chemical_formula_weight         497.69

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)
_symmetry_space_group_name_Hall  'P 2yb'

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

_cell_length_a                   7.1244(14)
_cell_length_b                   7.1131(14)
_cell_length_c                   13.153(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.85(3)
_cell_angle_gamma                90.00
_cell_volume                     666.5(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6248
_cell_measurement_theta_min      3.10
_cell_measurement_theta_max      27.53

_exptl_crystal_description       Block
_exptl_crystal_colour            Green
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.480
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             496
_exptl_absorpt_coefficient_mu    3.212
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.9542
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'

_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  'Rigaku R-AXIS RAPID IP'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean 10.000
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            6603
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_sigmaI/netI    0.0604
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.10
_diffrn_reflns_theta_max         27.48
_reflns_number_total             3009
_reflns_number_gt                2806
_reflns_threshold_expression     I>2sigma(I)

_computing_data_collection       'RAPID-AUTO (Rigaku, 2004)'
_computing_cell_refinement       RAPID-AUTO
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2004)'
_computing_structure_solution    SHELXS-97
_computing_structure_refinement  SHELXL-97
_computing_molecular_graphics    'SHELXTL (Bruker, 1998)'
_computing_publication_material  SHELXTL

_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^)+(0.0187P)^2^] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(1)
_refine_ls_number_reflns         3009
_refine_ls_number_parameters     247
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0280
_refine_ls_wR_factor_ref         0.0631
_refine_ls_wR_factor_gt          0.0617
_refine_ls_goodness_of_fit_ref   1.040
_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
Ni1 Ni 0.26981(5) 0.49830(6) 0.31983(2) 0.01327(9) Uani 1 1 d . . .
Ni2 Ni 0.21253(4) 0.50147(7) 0.81943(2) 0.01411(9) Uani 1 1 d . . .
S1 S 0.31541(12) 0.63301(13) 0.57141(6) 0.01908(18) Uani 1 1 d . . .
S2 S 0.09153(9) 0.51320(15) 1.07313(5) 0.01717(16) Uani 1 1 d . . .
N1 N 0.2924(3) 0.4802(5) 0.47958(17) 0.0147(5) Uani 1 1 d . . .
N2 N 0.2399(3) 0.4939(6) 0.66074(16) 0.0157(5) Uani 1 1 d . . .
N3 N 0.2276(3) 0.4696(4) 0.97804(17) 0.0146(6) Uani 1 1 d . . .
N4 N 0.2518(3) 0.4801(5) 1.16094(17) 0.0141(6) Uani 1 1 d . . .
C1 C 0.2019(4) 0.1654(5) 0.4368(2) 0.0160(7) Uani 1 1 d . . .
C2 C 0.2251(4) 0.3193(4) 0.5147(2) 0.0129(6) Uani 1 1 d . . .
C3 C 0.1953(4) 0.3279(5) 0.6209(2) 0.0144(6) Uani 1 1 d . . .
C4 C 0.0988(4) 0.1939(5) 0.6931(2) 0.0175(7) Uani 1 1 d . . .
C5 C 0.5498(4) 0.4145(5) 0.9300(2) 0.0175(6) Uani 1 1 d . . .
C6 C 0.4009(4) 0.4317(5) 1.0121(2) 0.0147(6) Uani 1 1 d . . .
C7 C 0.4136(4) 0.4327(4) 1.1192(2) 0.0129(6) Uani 1 1 d . . .
C8 C 0.5657(4) 0.3704(5) 1.1931(2) 0.0158(6) Uani 1 1 d . . .
O1 O 0.2074(3) 0.2238(3) 0.34508(17) 0.0190(5) Uani 1 1 d . . .
O2 O 0.1854(3) 0.0014(4) 0.46184(17) 0.0302(5) Uani 1 1 d . . .
O3 O 0.0020(3) 0.0676(4) 0.65368(17) 0.0243(6) Uani 1 1 d . . .
O4 O 0.1166(3) 0.2328(4) 0.78552(17) 0.0236(5) Uani 1 1 d . . .
O5 O 0.3477(4) 0.7712(4) 0.3238(2) 0.0280(6) Uani 1 1 d D . .
H5A H 0.376(5) 0.814(5) 0.2661(15) 0.034 Uiso 1 1 d D . .
H5B H 0.261(5) 0.824(5) 0.356(3) 0.034 Uiso 1 1 d D . .
O6 O 0.4844(3) 0.4167(4) 0.83974(16) 0.0242(5) Uani 1 1 d . . .
O7 O 0.7142(3) 0.4101(5) 0.95352(18) 0.0332(7) Uani 1 1 d . . .
O8 O 0.6969(3) 0.2744(4) 1.15986(18) 0.0238(6) Uani 1 1 d . . .
O9 O 0.5385(3) 0.4133(4) 1.28513(17) 0.0227(5) Uani 1 1 d . . .
O10 O -0.0562(3) 0.5869(4) 0.82441(19) 0.0227(5) Uani 1 1 d D . .
H10A H -0.124(4) 0.508(4) 0.856(2) 0.027 Uiso 1 1 d D . .
H10B H -0.109(4) 0.638(5) 0.7719(18) 0.027 Uiso 1 1 d 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
Ni1 0.01761(16) 0.01582(19) 0.00642(16) 0.00048(19) 0.00134(13) 0.0021(2)
Ni2 0.01455(15) 0.0206(2) 0.00718(16) -0.0011(2) -0.00058(12) -0.0018(2)
S1 0.0298(4) 0.0180(4) 0.0094(3) -0.0003(3) -0.0008(3) -0.0076(3)
S2 0.0136(3) 0.0290(4) 0.0089(3) -0.0007(4) 0.0003(2) 0.0042(4)
N1 0.0203(10) 0.0160(16) 0.0078(10) 0.0012(12) -0.0004(9) 0.0018(12)
N2 0.0200(10) 0.0205(13) 0.0065(10) 0.0020(15) -0.0010(9) -0.0003(14)
N3 0.0161(10) 0.0198(19) 0.0079(11) -0.0013(11) 0.0010(9) -0.0004(10)
N4 0.0163(10) 0.0176(17) 0.0084(10) -0.0004(13) 0.0015(9) -0.0004(11)
C1 0.0157(13) 0.0204(19) 0.0119(14) -0.0009(12) 0.0029(12) 0.0011(12)
C2 0.0133(12) 0.0138(16) 0.0115(14) -0.0008(12) -0.0031(11) -0.0016(11)
C3 0.0133(12) 0.0157(16) 0.0140(15) -0.0009(12) -0.0017(12) -0.0007(11)
C4 0.0182(14) 0.0203(17) 0.0142(16) 0.0002(12) 0.0039(13) 0.0024(12)
C5 0.0192(14) 0.0211(16) 0.0123(14) 0.0018(13) 0.0029(12) 0.0035(12)
C6 0.0167(13) 0.0192(16) 0.0084(13) 0.0011(12) 0.0044(12) 0.0021(11)
C7 0.0153(12) 0.0138(14) 0.0096(13) 0.0002(11) -0.0004(11) 0.0016(11)
C8 0.0125(13) 0.0236(18) 0.0113(15) 0.0028(12) 0.0003(12) 0.0002(12)
O1 0.0308(12) 0.0151(12) 0.0110(11) -0.0037(9) -0.0029(9) -0.0015(9)
O2 0.0556(14) 0.0160(12) 0.0193(10) -0.0013(12) 0.0093(10) -0.0011(15)
O3 0.0252(11) 0.0288(14) 0.0191(12) -0.0087(10) 0.0075(10) -0.0123(10)
O4 0.0378(13) 0.0242(14) 0.0089(11) 0.0001(10) 0.0040(10) -0.0066(11)
O5 0.0420(15) 0.0210(14) 0.0216(13) 0.0007(11) 0.0155(12) -0.0011(12)
O6 0.0186(10) 0.0459(16) 0.0081(11) -0.0015(10) 0.0031(9) 0.0091(10)
O7 0.0169(10) 0.068(2) 0.0154(11) 0.0078(13) 0.0043(10) 0.0024(12)
O8 0.0255(11) 0.0287(15) 0.0173(12) 0.0063(11) 0.0047(10) 0.0135(10)
O9 0.0204(10) 0.0381(15) 0.0097(10) 0.0028(10) -0.0011(9) 0.0069(10)
O10 0.0184(10) 0.0303(15) 0.0192(11) 0.0086(10) -0.0009(9) -0.0004(10)

_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 O5 2.019(3) . ?
Ni1 O1 2.031(2) . ?
Ni1 O3 2.034(2) 2_556 ?
Ni1 O9 2.065(2) 1_554 ?
Ni1 N4 2.096(2) 1_554 ?
Ni1 N1 2.109(2) . ?
Ni2 O10 2.010(2) . ?
Ni2 O6 2.042(2) . ?
Ni2 O8 2.063(3) 2_657 ?
Ni2 O4 2.076(3) . ?
Ni2 N3 2.100(2) . ?
Ni2 N2 2.100(2) . ?
S1 N1 1.631(3) . ?
S1 N2 1.633(3) . ?
S2 N3 1.623(2) . ?
S2 N4 1.629(3) . ?
N1 C2 1.327(4) . ?
N2 C3 1.329(5) . ?
N3 C6 1.335(4) . ?
N4 C7 1.328(4) . ?
N4 Ni1 2.096(2) 1_556 ?
C1 O2 1.218(4) . ?
C1 O1 1.277(4) . ?
C1 C2 1.507(4) . ?
C2 C3 1.418(4) . ?
C3 C4 1.517(4) . ?
C4 O3 1.241(4) . ?
C4 O4 1.251(4) . ?
C5 O7 1.207(4) . ?
C5 O6 1.269(4) . ?
C5 C6 1.529(4) . ?
C6 C7 1.410(4) . ?
C7 C8 1.512(4) . ?
C8 O8 1.242(4) . ?
C8 O9 1.266(4) . ?
O3 Ni1 2.034(2) 2_546 ?
O5 H5A 0.845(10) . ?
O5 H5B 0.845(10) . ?
O8 Ni2 2.063(3) 2_647 ?
O9 Ni1 2.065(2) 1_556 ?
O10 H10A 0.850(10) . ?
O10 H10B 0.861(10) . ?

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
O5 Ni1 O1 168.71(11) . . ?
O5 Ni1 O3 91.40(10) . 2_556 ?
O1 Ni1 O3 89.64(10) . 2_556 ?
O5 Ni1 O9 91.83(10) . 1_554 ?
O1 Ni1 O9 87.74(10) . 1_554 ?
O3 Ni1 O9 175.71(11) 2_556 1_554 ?
O5 Ni1 N4 95.64(13) . 1_554 ?
O1 Ni1 N4 95.34(12) . 1_554 ?
O3 Ni1 N4 98.12(10) 2_556 1_554 ?
O9 Ni1 N4 78.75(9) 1_554 1_554 ?
O5 Ni1 N1 90.90(12) . . ?
O1 Ni1 N1 78.01(11) . . ?
O3 Ni1 N1 84.44(9) 2_556 . ?
O9 Ni1 N1 98.33(9) 1_554 . ?
N4 Ni1 N1 172.91(16) 1_554 . ?
O10 Ni2 O6 170.61(9) . . ?
O10 Ni2 O8 90.43(11) . 2_657 ?
O6 Ni2 O8 88.08(11) . 2_657 ?
O10 Ni2 O4 88.54(10) . . ?
O6 Ni2 O4 93.72(11) . . ?
O8 Ni2 O4 175.03(10) 2_657 . ?
O10 Ni2 N3 92.00(10) . . ?
O6 Ni2 N3 78.68(9) . . ?
O8 Ni2 N3 87.66(11) 2_657 . ?
O4 Ni2 N3 97.23(11) . . ?
O10 Ni2 N2 98.20(10) . . ?
O6 Ni2 N2 91.18(9) . . ?
O8 Ni2 N2 97.00(13) 2_657 . ?
O4 Ni2 N2 78.35(13) . . ?
N3 Ni2 N2 168.73(13) . . ?
N1 S1 N2 95.66(19) . . ?
N3 S2 N4 95.64(13) . . ?
C2 N1 S1 110.49(19) . . ?
C2 N1 Ni1 112.1(2) . . ?
S1 N1 Ni1 134.64(19) . . ?
C3 N2 S1 109.53(19) . . ?
C3 N2 Ni2 112.9(2) . . ?
S1 N2 Ni2 137.4(2) . . ?
C6 N3 S2 109.9(2) . . ?
C6 N3 Ni2 112.86(18) . . ?
S2 N3 Ni2 136.26(15) . . ?
C7 N4 S2 110.31(19) . . ?
C7 N4 Ni1 112.8(2) . 1_556 ?
S2 N4 Ni1 136.88(13) . 1_556 ?
O2 C1 O1 124.9(3) . . ?
O2 C1 C2 121.4(3) . . ?
O1 C1 C2 113.6(3) . . ?
N1 C2 C3 111.5(3) . . ?
N1 C2 C1 115.3(3) . . ?
C3 C2 C1 133.2(3) . . ?
N2 C3 C2 112.9(3) . . ?
N2 C3 C4 114.8(3) . . ?
C2 C3 C4 131.7(3) . . ?
O3 C4 O4 127.9(3) . . ?
O3 C4 C3 116.6(3) . . ?
O4 C4 C3 115.4(3) . . ?
O7 C5 O6 125.5(3) . . ?
O7 C5 C6 120.1(3) . . ?
O6 C5 C6 114.2(3) . . ?
N3 C6 C7 112.3(2) . . ?
N3 C6 C5 115.3(2) . . ?
C7 C6 C5 132.1(3) . . ?
N4 C7 C6 111.8(3) . . ?
N4 C7 C8 115.3(2) . . ?
C6 C7 C8 132.5(3) . . ?
O8 C8 O9 126.6(3) . . ?
O8 C8 C7 118.1(3) . . ?
O9 C8 C7 115.2(2) . . ?
C1 O1 Ni1 118.5(2) . . ?
C4 O3 Ni1 128.9(2) . 2_546 ?
C4 O4 Ni2 116.2(2) . . ?
Ni1 O5 H5A 113(3) . . ?
Ni1 O5 H5B 104(3) . . ?
H5A O5 H5B 118.5(19) . . ?
C5 O6 Ni2 117.43(18) . . ?
C8 O8 Ni2 135.0(2) . 2_647 ?
C8 O9 Ni1 115.9(2) . 1_556 ?
Ni2 O10 H10A 111(2) . . ?
Ni2 O10 H10B 120(2) . . ?
H10A O10 H10B 114.9(17) . . ?

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
N2 S1 N1 C2 0.5(2) . . . . ?
N2 S1 N1 Ni1 159.49(19) . . . . ?
O5 Ni1 N1 C2 171.1(2) . . . . ?
O1 Ni1 N1 C2 -11.08(19) . . . . ?
O3 Ni1 N1 C2 79.7(2) 2_556 . . . ?
O9 Ni1 N1 C2 -97.0(2) 1_554 . . . ?
N4 Ni1 N1 C2 -31.8(8) 1_554 . . . ?
O5 Ni1 N1 S1 12.30(19) . . . . ?
O1 Ni1 N1 S1 -169.8(2) . . . . ?
O3 Ni1 N1 S1 -79.03(19) 2_556 . . . ?
O9 Ni1 N1 S1 104.28(19) 1_554 . . . ?
N4 Ni1 N1 S1 169.5(6) 1_554 . . . ?
N1 S1 N2 C3 -0.2(2) . . . . ?
N1 S1 N2 Ni2 174.6(2) . . . . ?
O10 Ni2 N2 C3 -90.2(2) . . . . ?
O6 Ni2 N2 C3 90.1(2) . . . . ?
O8 Ni2 N2 C3 178.3(2) 2_657 . . . ?
O4 Ni2 N2 C3 -3.4(2) . . . . ?
N3 Ni2 N2 C3 64.5(7) . . . . ?
O10 Ni2 N2 S1 95.1(2) . . . . ?
O6 Ni2 N2 S1 -84.6(2) . . . . ?
O8 Ni2 N2 S1 3.6(2) 2_657 . . . ?
O4 Ni2 N2 S1 -178.2(3) . . . . ?
N3 Ni2 N2 S1 -110.3(8) . . . . ?
N4 S2 N3 C6 -1.1(3) . . . . ?
N4 S2 N3 Ni2 -168.4(2) . . . . ?
O10 Ni2 N3 C6 -172.6(2) . . . . ?
O6 Ni2 N3 C6 6.3(2) . . . . ?
O8 Ni2 N3 C6 -82.2(2) 2_657 . . . ?
O4 Ni2 N3 C6 98.6(2) . . . . ?
N2 Ni2 N3 C6 32.5(8) . . . . ?
O10 Ni2 N3 S2 -5.6(3) . . . . ?
O6 Ni2 N3 S2 173.3(3) . . . . ?
O8 Ni2 N3 S2 84.8(3) 2_657 . . . ?
O4 Ni2 N3 S2 -94.3(3) . . . . ?
N2 Ni2 N3 S2 -160.5(6) . . . . ?
N3 S2 N4 C7 -0.6(3) . . . . ?
N3 S2 N4 Ni1 177.7(3) . . . 1_556 ?
S1 N1 C2 C3 -0.6(3) . . . . ?
Ni1 N1 C2 C3 -164.61(19) . . . . ?
S1 N1 C2 C1 -178.7(2) . . . . ?
Ni1 N1 C2 C1 17.3(3) . . . . ?
O2 C1 C2 N1 162.1(3) . . . . ?
O1 C1 C2 N1 -15.8(4) . . . . ?
O2 C1 C2 C3 -15.4(5) . . . . ?
O1 C1 C2 C3 166.6(3) . . . . ?
S1 N2 C3 C2 -0.1(3) . . . . ?
Ni2 N2 C3 C2 -176.3(2) . . . . ?
S1 N2 C3 C4 -172.2(2) . . . . ?
Ni2 N2 C3 C4 11.6(3) . . . . ?
N1 C2 C3 N2 0.4(4) . . . . ?
C1 C2 C3 N2 178.0(3) . . . . ?
N1 C2 C3 C4 170.9(3) . . . . ?
C1 C2 C3 C4 -11.5(6) . . . . ?
N2 C3 C4 O3 157.2(3) . . . . ?
C2 C3 C4 O3 -13.1(5) . . . . ?
N2 C3 C4 O4 -18.0(4) . . . . ?
C2 C3 C4 O4 171.7(3) . . . . ?
S2 N3 C6 C7 2.5(4) . . . . ?
Ni2 N3 C6 C7 172.9(2) . . . . ?
S2 N3 C6 C5 -172.0(2) . . . . ?
Ni2 N3 C6 C5 -1.5(4) . . . . ?
O7 C5 C6 N3 168.3(3) . . . . ?
O6 C5 C6 N3 -7.9(5) . . . . ?
O7 C5 C6 C7 -4.7(6) . . . . ?
O6 C5 C6 C7 179.1(4) . . . . ?
S2 N4 C7 C6 2.1(4) . . . . ?
Ni1 N4 C7 C6 -176.6(2) 1_556 . . . ?
S2 N4 C7 C8 -171.4(3) . . . . ?
Ni1 N4 C7 C8 9.9(4) 1_556 . . . ?
N3 C6 C7 N4 -3.0(4) . . . . ?
C5 C6 C7 N4 170.2(4) . . . . ?
N3 C6 C7 C8 169.0(3) . . . . ?
C5 C6 C7 C8 -17.8(6) . . . . ?
N4 C7 C8 O8 159.3(3) . . . . ?
C6 C7 C8 O8 -12.4(6) . . . . ?
N4 C7 C8 O9 -16.5(5) . . . . ?
C6 C7 C8 O9 171.7(3) . . . . ?
O2 C1 O1 Ni1 -172.1(3) . . . . ?
C2 C1 O1 Ni1 5.8(3) . . . . ?
O5 Ni1 O1 C1 13.4(6) . . . . ?
O3 Ni1 O1 C1 -82.0(2) 2_556 . . . ?
O9 Ni1 O1 C1 101.4(2) 1_554 . . . ?
N4 Ni1 O1 C1 179.9(2) 1_554 . . . ?
N1 Ni1 O1 C1 2.4(2) . . . . ?
O4 C4 O3 Ni1 47.4(5) . . . 2_546 ?
C3 C4 O3 Ni1 -127.1(3) . . . 2_546 ?
O3 C4 O4 Ni2 -159.7(3) . . . . ?
C3 C4 O4 Ni2 14.9(4) . . . . ?
O10 Ni2 O4 C4 91.7(2) . . . . ?
O6 Ni2 O4 C4 -97.4(2) . . . . ?
O8 Ni2 O4 C4 13.7(12) 2_657 . . . ?
N3 Ni2 O4 C4 -176.4(2) . . . . ?
N2 Ni2 O4 C4 -7.0(2) . . . . ?
O7 C5 O6 Ni2 -162.3(3) . . . . ?
C6 C5 O6 Ni2 13.7(4) . . . . ?
O10 Ni2 O6 C5 -4.4(9) . . . . ?
O8 Ni2 O6 C5 76.5(3) 2_657 . . . ?
O4 Ni2 O6 C5 -108.1(3) . . . . ?
N3 Ni2 O6 C5 -11.5(3) . . . . ?
N2 Ni2 O6 C5 173.5(3) . . . . ?
O9 C8 O8 Ni2 61.9(5) . . . 2_647 ?
C7 C8 O8 Ni2 -113.4(3) . . . 2_647 ?
O8 C8 O9 Ni1 -161.0(3) . . . 1_556 ?
C7 C8 O9 Ni1 14.4(4) . . . 1_556 ?

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
O5 H5A O6 0.85(1) 1.87(2) 2.685(3) 161(4) 2_656
O5 H5B O2 0.85(1) 1.96(3) 2.716(4) 149(4) 1_565
O10 H10A O7 0.85(1) 1.88(2) 2.687(3) 160(4) 1_455
O10 H10B O1 0.86(1) 1.79(1) 2.647(3) 174(4) 2_556

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.082