Supplementary Material (ESI) for Dalton Transactions
This journal is (c) The Royal Society of Chemistry 2003

data_global

_journal_coden_Cambridge         186

loop_
_publ_author_name
'Vito Lippolis'
'Andrea Bencini'
'Claudia Caltagirone'
'Francesco Demartin'
'F. A. Devillanova'
'Alessandra Garau'
'Francesco Isaia'
'Palma Mariani'
P.Ulrich
T.Lorenzo
V.Gaetano

_publ_contact_author_name        'Prof Vito Lippolis'
_publ_contact_author_address     
;
Dipartimento di Chimica Inorganica ed Analitica 
Universita di Monserrato 
S.S. 554 bivio Sestu 
Monserrato-Cagliari 
I-9042 
ITALY 
;

_publ_contact_author_email       LIPPOLIS@UNICA.IT

_publ_requested_journal          'Dalton Transactions'

_publ_section_title              
;
Redox chemosensors: coordination towards Cu(II),
Zn(II), Cd(II), Hg(II), and Pb(II) of
1-aza-4,10-dithia-7-oxacyclododecane ([12]aneNS2O) and its
N-ferrocenylmethyl derivative
;

data_da200
_database_code_CSD               196822

_audit_creation_method           SHELXL
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_structural     ?
_chemical_formula_analytical     'C23 H37 Cd Fe N3 O8 S2'
_chemical_formula_sum            'C23 H37 Cd Fe N3 O8 S2'
_chemical_formula_weight         715.93
_chemical_melting_point          ?
_chemical_compound_source        ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_symmetry_cell_setting           othorhombic
_symmetry_space_group_name_H-M   P212121

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

_cell_length_a                   12.1242(9)
_cell_length_b                   13.6318(10)
_cell_length_c                   18.1656(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3002.3(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    942
_cell_measurement_theta_min      4.42
_cell_measurement_theta_max      22.24

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow-orange
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1464
_exptl_absorpt_coefficient_mu    1.378
_exptl_absorpt_correction_type   SADABS
_exptl_absorpt_correction_T_min  0.80
_exptl_absorpt_correction_T_max  1.00

_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       'SMART CCD DIFFRACTOMETER'
_diffrn_measurement_method       omega
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            28172
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_sigmaI/netI    0.0691
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.87
_diffrn_reflns_theta_max         26.01
_reflns_number_total             5895
_reflns_number_observed          4522
_reflns_observed_criterion       >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^
or flagged by the user for potential systematic errors.  Weighted R-factors
wR and all goodnesses 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 observed criterion
of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0590P)^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    ?
_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(3)
_refine_ls_number_reflns         5895
_refine_ls_number_parameters     406
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_obs          0.0350
_refine_ls_wR_factor_all         0.1003
_refine_ls_wR_factor_obs         0.0982
_refine_ls_goodness_of_fit_all   1.022
_refine_ls_goodness_of_fit_obs   1.153
_refine_ls_restrained_S_all      1.022
_refine_ls_restrained_S_obs      1.153
_refine_ls_shift/esd_max         0.595
_refine_ls_shift/esd_mean        0.358

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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Cd Cd 0.01250(3) 0.25811(3) 0.86505(2) 0.05078(12) Uani 1 d . .
Fe Fe 0.23915(8) 0.65173(6) 0.96884(6) 0.0762(3) Uani 1 d . .
S4 S 0.0966(2) 0.2813(2) 0.73219(9) 0.0862(5) Uani 1 d . .
S10 S 0.04699(12) 0.17160(12) 0.99395(10) 0.0739(5) Uani 1 d . .
OS O 0.5921(23) 0.4254(16) 0.6979(10) 0.313(11) Uani 0.80 d P .
O7 O 0.1428(4) 0.1132(3) 0.8420(3) 0.0762(13) Uani 1 d . .
O21 O -0.1173(8) 0.1312(10) 0.7618(6) 0.202(5) Uani 1 d . .
O22 O -0.1511(5) 0.1743(5) 0.8643(4) 0.132(3) Uani 1 d . .
O23 O -0.2644(4) 0.0885(4) 0.8057(3) 0.112(2) Uani 1 d . .
O31 O -0.0781(4) 0.4108(4) 0.8401(3) 0.0834(14) Uani 1 d . .
O32 O -0.0976(3) 0.3666(3) 0.9519(3) 0.0734(11) Uani 1 d . .
O33 O -0.1667(5) 0.5031(4) 0.9164(4) 0.123(2) Uani 1 d . .
N1 N 0.1830(3) 0.3411(3) 0.8992(3) 0.0486(10) Uani 1 d . .
N2 N -0.1807(4) 0.1336(5) 0.8109(3) 0.0710(15) Uani 1 d . .
N3 N -0.1155(4) 0.4280(4) 0.9029(4) 0.0698(14) Uani 1 d . .
C1S C 0.5443(12) 0.5566(16) 0.6319(11) 0.210(10) Uani 0.80 d P .
C2 C 0.2588(5) 0.3372(4) 0.8356(3) 0.0606(14) Uani 1 d . .
H2A H 0.2876(1251) 0.2711(1328) 0.8313(1518) 1.200 Uiso 1 calc . .
H2B H 0.3206(1319) 0.3806(1118) 0.8450(1125) 1.200 Uiso 1 calc . .
C2S C 0.5220(19) 0.5087(19) 0.6986(18) 0.252(13) Uani 0.80 d P .
C3 C 0.2056(7) 0.3663(5) 0.7622(4) 0.085(2) Uani 1 d . .
H3A H 0.2623(1279) 0.3690(1581) 0.7246(950) 1.200 Uiso 1 calc . .
H3B H 0.1744(1694) 0.4315(1074) 0.7670(1205) 1.200 Uiso 1 calc . .
C3S C 0.5984(26) 0.3730(33) 0.7816(21) 0.328(23) Uani 0.80 d P .
C4S C 0.5533(30) 0.2922(33) 0.7455(16) 0.296(18) Uani 0.80 d P .
C5 C 0.1759(8) 0.1711(7) 0.7188(5) 0.109(3) Uani 1 d . .
H5A H 0.1714(1597) 0.1522(997) 0.6674(643) 1.200 Uiso 1 calc . .
H5B H 0.2527(1153) 0.1851(1514) 0.7297(996) 1.200 Uiso 1 calc . .
C6 C 0.1378(8) 0.0824(6) 0.7674(5) 0.104(3) Uani 1 d . .
H6A H 0.0631(1321) 0.0635(1259) 0.7547(1235) 1.200 Uiso 1 calc . .
H6B H 0.1859(1625) 0.0265(1404) 0.7596(1195) 1.200 Uiso 1 calc . .
C8 C 0.1110(7) 0.0327(5) 0.8890(6) 0.095(3) Uani 1 d . .
H8A H 0.1567(1352) -0.0241(1083) 0.8785(1519) 1.200 Uiso 1 calc . .
H8B H 0.0348(1041) 0.0151(998) 0.8796(1357) 1.200 Uiso 1 calc . .
C9 C 0.1249(6) 0.0628(5) 0.9700(6) 0.089(2) Uani 1 d . .
H9A H 0.2024(1412) 0.0746(1617) 0.9798(1037) 1.200 Uiso 1 calc . .
H9B H 0.1013(1246) 0.0090(919) 1.0012(1097) 1.200 Uiso 1 calc . .
C11 C 0.1532(5) 0.2569(5) 1.0213(3) 0.0689(14) Uani 1 d . .
H11A H 0.1181(1168) 0.3158(1220) 1.0398(1003) 1.200 Uiso 1 calc . .
H11B H 0.1947(1354) 0.2281(1242) 1.0615(909) 1.200 Uiso 1 calc . .
C12 C 0.2345(4) 0.2862(4) 0.9603(3) 0.0592(14) Uani 1 d . .
H12A H 0.2925(1577) 0.3262(1159) 0.9816(1123) 1.200 Uiso 1 calc . .
H12B H 0.2685(1623) 0.2274(1789) 0.9406(1641) 1.200 Uiso 1 calc . .
C13 C 0.1548(4) 0.4451(4) 0.9203(4) 0.0550(14) Uani 1 d . .
H13A H 0.1023(1351) 0.4435(1628) 0.9606(974) 1.200 Uiso 1 calc . .
H13B H 0.1187(1468) 0.4764(1117) 0.8788(1267) 1.200 Uiso 1 calc . .
C14 C 0.2526(4) 0.5076(4) 0.9431(3) 0.0554(13) Uani 1 d . .
C15 C 0.2902(6) 0.5246(4) 1.0170(4) 0.078(2) Uani 1 d . .
H15 H 0.2619(6) 0.4961(4) 1.0596(4) 0.119(32) Uiso 1 calc R .
C16 C 0.3791(6) 0.5934(5) 1.0131(6) 0.091(3) Uani 1 d . .
H16 H 0.4182(6) 0.6182(5) 1.0531(6) 2.000(2388) Uiso 1 calc R .
C17 C 0.3974(6) 0.6171(5) 0.9393(7) 0.104(3) Uani 1 d . .
H17 H 0.4511(6) 0.6598(5) 0.9216(7) 0.079(19) Uiso 1 calc R .
C18 C 0.3205(5) 0.5651(4) 0.8965(5) 0.076(2) Uani 1 d . .
H18 H 0.3149(5) 0.5681(4) 0.8455(5) 0.115(31) Uiso 1 calc R .
C19 C 0.1947(28) 0.7742(17) 1.0234(15) 0.237(17) Uani 1 d . .
H19 H 0.2300(28) 0.8005(17) 1.0644(15) 0.497(213) Uiso 1 calc R .
C20 C 0.1161(21) 0.7101(16) 1.0292(15) 0.209(11) Uani 1 d . .
H20 H 0.0890(21) 0.6827(16) 1.0725(15) 0.148(46) Uiso 1 calc R .
C21 C 0.0796(10) 0.6899(9) 0.9568(15) 0.152(6) Uani 1 d . .
H21 H 0.0229(10) 0.6478(9) 0.9429(15) 2.000(2435) Uiso 1 calc R .
C22 C 0.1464(13) 0.7464(11) 0.9102(7) 0.142(4) Uani 1 d . .
H22 H 0.1449(13) 0.7505(11) 0.8591(7) 0.147(40) Uiso 1 calc R .
C23 C 0.2189(13) 0.7973(8) 0.9615(16) 0.186(9) Uani 1 d . .
H23 H 0.2749(13) 0.8406(8) 0.9486(16) 0.166(47) Uiso 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
Cd 0.0447(2) 0.0474(2) 0.0602(2) 0.0049(2) -0.0044(2) -0.0038(2)
Fe 0.0809(6) 0.0380(4) 0.1098(7) -0.0166(5) -0.0398(5) 0.0106(4)
S4 0.0933(11) 0.1094(15) 0.0558(9) -0.0024(9) -0.0021(8) -0.0114(10)
S10 0.0568(8) 0.0761(10) 0.0889(12) 0.0331(9) -0.0007(8) -0.0016(7)
OS 0.446(32) 0.274(20) 0.219(17) 0.122(16) 0.006(17) 0.051(23)
O7 0.080(3) 0.045(2) 0.103(4) -0.021(2) -0.004(2) -0.001(2)
O21 0.167(8) 0.275(13) 0.164(8) -0.038(8) 0.059(7) -0.051(8)
O22 0.123(4) 0.170(6) 0.102(4) -0.044(4) 0.015(4) -0.090(5)
O23 0.079(3) 0.107(4) 0.149(5) -0.029(4) -0.023(3) -0.026(3)
O31 0.073(3) 0.098(3) 0.079(3) 0.031(3) 0.014(2) 0.023(3)
O32 0.066(2) 0.067(3) 0.087(3) 0.022(2) 0.002(2) 0.003(2)
O33 0.128(4) 0.083(3) 0.158(6) 0.046(4) 0.061(4) 0.054(3)
N1 0.043(2) 0.035(2) 0.067(3) -0.002(2) 0.003(2) -0.002(2)
N2 0.050(3) 0.104(4) 0.060(4) -0.007(3) -0.002(3) -0.015(3)
N3 0.052(3) 0.056(3) 0.102(5) 0.025(3) 0.012(3) 0.008(2)
C1S 0.124(11) 0.274(21) 0.233(19) 0.169(18) -0.012(11) 0.011(12)
C2 0.055(3) 0.061(3) 0.067(4) -0.010(3) 0.012(3) -0.011(3)
C2S 0.176(18) 0.224(23) 0.356(35) 0.108(23) 0.069(21) 0.101(17)
C3 0.103(5) 0.068(4) 0.085(5) 0.010(4) 0.024(4) -0.017(4)
C3S 0.249(29) 0.430(57) 0.306(39) 0.215(41) -0.061(27) -0.114(34)
C4S 0.262(30) 0.416(50) 0.210(25) -0.033(29) 0.032(21) -0.117(31)
C5 0.122(7) 0.109(7) 0.095(6) -0.049(5) 0.017(5) -0.005(6)
C6 0.122(7) 0.083(5) 0.108(6) -0.052(5) -0.026(5) 0.003(5)
C8 0.102(5) 0.043(3) 0.139(7) 0.001(4) -0.040(5) -0.009(3)
C9 0.080(5) 0.044(3) 0.143(7) 0.018(4) -0.029(4) 0.003(3)
C11 0.073(3) 0.066(4) 0.067(3) 0.008(4) -0.008(3) 0.000(4)
C12 0.052(3) 0.051(3) 0.075(4) -0.003(3) -0.020(3) 0.001(2)
C13 0.048(3) 0.034(3) 0.083(4) -0.010(3) -0.008(3) 0.000(2)
C14 0.050(3) 0.037(2) 0.079(4) -0.010(2) -0.013(3) 0.004(2)
C15 0.091(4) 0.052(3) 0.090(5) -0.014(3) -0.036(4) 0.017(3)
C16 0.073(4) 0.055(4) 0.144(8) -0.023(4) -0.050(5) 0.011(3)
C17 0.064(4) 0.052(4) 0.196(11) -0.016(5) -0.021(5) -0.018(3)
C18 0.064(4) 0.052(3) 0.112(6) -0.009(3) -0.008(4) -0.010(3)
C19 0.370(34) 0.110(14) 0.233(20) -0.102(16) -0.175(24) 0.148(18)
C20 0.257(24) 0.125(13) 0.245(22) 0.018(16) 0.103(21) 0.128(15)
C21 0.100(7) 0.073(7) 0.283(20) -0.064(10) -0.060(10) 0.054(6)
C22 0.163(11) 0.104(9) 0.159(11) 0.018(8) -0.051(9) 0.073(9)
C23 0.142(10) 0.034(4) 0.383(29) 0.007(11) -0.092(16) 0.021(5)

_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
Cd O22 2.290(5) . ?
Cd O31 2.396(4) . ?
Cd N1 2.436(4) . ?
Cd O32 2.541(5) . ?
Cd O7 2.564(4) . ?
Cd S4 2.639(2) . ?
Cd S10 2.655(2) . ?
Fe C23 2.004(10) . ?
Fe C19 2.015(14) . ?
Fe C20 2.015(14) . ?
Fe C21 2.015(10) . ?
Fe C22 2.016(8) . ?
Fe C18 2.022(7) . ?
Fe C14 2.026(5) . ?
Fe C15 2.038(7) . ?
Fe C16 2.040(6) . ?
Fe C17 2.048(8) . ?
S4 C5 1.800(10) . ?
S4 C3 1.841(8) . ?
S10 C11 1.805(7) . ?
S10 C9 1.811(8) . ?
OS C2S 1.42(2) . ?
OS C3S 1.68(3) . ?
O7 C6 1.418(10) . ?
O7 C8 1.443(9) . ?
O21 N2 1.179(9) . ?
O22 N2 1.173(7) . ?
O23 N2 1.190(7) . ?
O31 N3 1.251(7) . ?
O32 N3 1.241(6) . ?
O33 N3 1.222(7) . ?
N1 C12 1.477(7) . ?
N1 C2 1.478(7) . ?
N1 C13 1.508(6) . ?
C1S C2S 1.40(3) . ?
C2 C3 1.533(10) . ?
C3S C4S 1.39(5) . ?
C5 C6 1.567(15) . ?
C8 C9 1.538(14) . ?
C11 C12 1.536(8) . ?
C13 C14 1.519(8) . ?
C14 C18 1.417(9) . ?
C14 C15 1.436(9) . ?
C15 C16 1.431(10) . ?
C16 C17 1.398(12) . ?
C17 C18 1.406(10) . ?
C19 C23 1.20(3) . ?
C19 C20 1.30(3) . ?
C20 C21 1.41(3) . ?
C21 C22 1.40(2) . ?
C22 C23 1.46(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O22 Cd O31 92.0(2) . . ?
O22 Cd N1 165.5(2) . . ?
O31 Cd N1 91.9(2) . . ?
O22 Cd O32 80.7(2) . . ?
O31 Cd O32 51.1(2) . . ?
N1 Cd O32 91.00(14) . . ?
O22 Cd O7 98.5(2) . . ?
O31 Cd O7 157.0(2) . . ?
N1 Cd O7 82.93(13) . . ?
O32 Cd O7 150.9(2) . . ?
O22 Cd S4 112.9(2) . . ?
O31 Cd S4 84.26(13) . . ?
N1 Cd S4 81.36(11) . . ?
O32 Cd S4 134.52(10) . . ?
O7 Cd S4 72.81(12) . . ?
O22 Cd S10 85.4(2) . . ?
O31 Cd S10 128.68(13) . . ?
N1 Cd S10 81.25(11) . . ?
O32 Cd S10 78.09(10) . . ?
O7 Cd S10 72.84(12) . . ?
S4 Cd S10 143.03(6) . . ?
C23 Fe C19 34.9(9) . . ?
C23 Fe C20 63.5(8) . . ?
C19 Fe C20 37.6(9) . . ?
C23 Fe C21 67.6(6) . . ?
C19 Fe C21 65.3(8) . . ?
C20 Fe C21 41.1(8) . . ?
C23 Fe C22 42.5(6) . . ?
C19 Fe C22 65.2(6) . . ?
C20 Fe C22 67.8(7) . . ?
C21 Fe C22 40.7(6) . . ?
C23 Fe C18 126.5(8) . . ?
C19 Fe C18 159.0(13) . . ?
C20 Fe C18 160.8(10) . . ?
C21 Fe C18 123.2(6) . . ?
C22 Fe C18 107.6(4) . . ?
C23 Fe C14 162.7(9) . . ?
C19 Fe C14 159.8(12) . . ?
C20 Fe C14 124.6(8) . . ?
C21 Fe C14 107.6(3) . . ?
C22 Fe C14 123.0(5) . . ?
C18 Fe C14 41.0(2) . . ?
C23 Fe C15 155.2(8) . . ?
C19 Fe C15 125.0(8) . . ?
C20 Fe C15 109.1(6) . . ?
C21 Fe C15 123.9(7) . . ?
C22 Fe C15 160.2(6) . . ?
C18 Fe C15 68.6(3) . . ?
C14 Fe C15 41.4(2) . . ?
C23 Fe C16 120.9(5) . . ?
C19 Fe C16 110.6(6) . . ?
C20 Fe C16 123.7(9) . . ?
C21 Fe C16 160.4(9) . . ?
C22 Fe C16 157.2(6) . . ?
C18 Fe C16 67.9(3) . . ?
C14 Fe C16 69.2(2) . . ?
C15 Fe C16 41.1(3) . . ?
C23 Fe C17 109.0(6) . . ?
C19 Fe C17 124.8(11) . . ?
C20 Fe C17 158.0(11) . . ?
C21 Fe C17 158.5(9) . . ?
C22 Fe C17 122.1(6) . . ?
C18 Fe C17 40.4(3) . . ?
C14 Fe C17 68.9(2) . . ?
C15 Fe C17 68.4(4) . . ?
C16 Fe C17 40.0(3) . . ?
C5 S4 C3 100.5(4) . . ?
C5 S4 Cd 103.3(3) . . ?
C3 S4 Cd 94.7(2) . . ?
C11 S10 C9 102.8(3) . . ?
C11 S10 Cd 93.9(2) . . ?
C9 S10 Cd 103.6(3) . . ?
C2S OS C3S 111.0(26) . . ?
C6 O7 C8 109.2(6) . . ?
C6 O7 Cd 111.0(4) . . ?
C8 O7 Cd 108.9(4) . . ?
N2 O22 Cd 120.4(5) . . ?
N3 O31 Cd 99.0(3) . . ?
N3 O32 Cd 92.3(4) . . ?
C12 N1 C2 107.8(4) . . ?
C12 N1 C13 112.5(4) . . ?
C2 N1 C13 111.9(4) . . ?
C12 N1 Cd 108.4(3) . . ?
C2 N1 Cd 108.2(3) . . ?
C13 N1 Cd 108.0(3) . . ?
O22 N2 O21 116.1(7) . . ?
O22 N2 O23 124.8(6) . . ?
O21 N2 O23 118.8(8) . . ?
O33 N3 O32 120.7(7) . . ?
O33 N3 O31 121.6(6) . . ?
O32 N3 O31 117.7(5) . . ?
N1 C2 C3 114.1(5) . . ?
C1S C2S OS 104.4(20) . . ?
C2 C3 S4 113.4(4) . . ?
C4S C3S OS 83.8(28) . . ?
C6 C5 S4 114.2(6) . . ?
O7 C6 C5 107.3(6) . . ?
O7 C8 C9 109.6(5) . . ?
C8 C9 S10 113.0(5) . . ?
C12 C11 S10 115.3(4) . . ?
N1 C12 C11 113.7(4) . . ?
N1 C13 C14 114.8(4) . . ?
C18 C14 C15 106.6(6) . . ?
C18 C14 C13 126.9(6) . . ?
C15 C14 C13 126.4(6) . . ?
C18 C14 Fe 69.4(3) . . ?
C15 C14 Fe 69.8(3) . . ?
C13 C14 Fe 123.0(4) . . ?
C16 C15 C14 107.4(7) . . ?
C16 C15 Fe 69.5(4) . . ?
C14 C15 Fe 68.8(3) . . ?
C17 C16 C15 108.6(6) . . ?
C17 C16 Fe 70.3(4) . . ?
C15 C16 Fe 69.4(3) . . ?
C16 C17 C18 107.9(7) . . ?
C16 C17 Fe 69.7(5) . . ?
C18 C17 Fe 68.8(4) . . ?
C17 C18 C14 109.5(8) . . ?
C17 C18 Fe 70.8(5) . . ?
C14 C18 Fe 69.6(4) . . ?
C23 C19 C20 115.5(20) . . ?
C23 C19 Fe 72.1(11) . . ?
C20 C19 Fe 71.2(8) . . ?
C19 C20 C21 106.6(20) . . ?
C19 C20 Fe 71.2(11) . . ?
C21 C20 Fe 69.5(8) . . ?
C22 C21 C20 105.9(14) . . ?
C22 C21 Fe 69.7(7) . . ?
C20 C21 Fe 69.4(7) . . ?
C21 C22 C23 102.9(14) . . ?
C21 C22 Fe 69.6(6) . . ?
C23 C22 Fe 68.3(6) . . ?
C19 C23 C22 109.1(19) . . ?
C19 C23 Fe 73.1(9) . . ?
C22 C23 Fe 69.2(6) . . ?

_refine_diff_density_max         0.474
_refine_diff_density_min         -0.288
_refine_diff_density_rms         0.087

data_da145
_database_code_CSD               196823

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H17 Cu N O S2 2+, 2 (Cl 1-)'
_chemical_formula_sum            'C8 H17 Cl2 Cu N O S2'
_chemical_formula_weight         341.79

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/n

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

_cell_length_a                   8.744(3)
_cell_length_b                   11.315(3)
_cell_length_c                   13.913(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.81(2)
_cell_angle_gamma                90.00
_cell_volume                     1375.9(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    25
_cell_measurement_theta_min      8.4
_cell_measurement_theta_max      13.6

_exptl_crystal_description       prism
_exptl_crystal_colour            Green
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.650
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             700
_exptl_absorpt_coefficient_mu    2.254
_exptl_absorpt_correction_type   psi-scans
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   ?

_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  'CAD$ diffractometer'
_diffrn_measurement_method       omega
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         3
_diffrn_standards_interval_count 150
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            2407
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0229
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.26
_diffrn_reflns_theta_max         24.96
_reflns_number_total             2407
_reflns_number_gt                1866
_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^)+(0.0287P)^2^+0.6148P] 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    'riding model'
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2407
_refine_ls_number_parameters     156
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0230
_refine_ls_wR_factor_ref         0.0603
_refine_ls_wR_factor_gt          0.0553
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.062
_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
Cu Cu 0.01636(3) 0.20511(3) 0.838587(19) 0.02960(10) Uani 1 1 d . . .
Cl1 Cl 0.02135(8) 0.20297(6) 0.67680(4) 0.04566(18) Uani 1 1 d . . .
Cl2 Cl -0.01648(10) -0.01040(6) 0.85839(5) 0.0556(2) Uani 1 1 d . . .
N1 N 0.0134(3) 0.21536(19) 0.98412(14) 0.0342(5) Uani 1 1 d . . .
H H 0.000(3) 0.139(3) 0.9981(18) 0.036(7) Uiso 1 1 d . . .
S4 S -0.24104(8) 0.28099(7) 0.83805(5) 0.04467(18) Uani 1 1 d . . .
S10 S 0.29110(8) 0.22177(6) 0.85554(5) 0.04296(18) Uani 1 1 d . . .
O7 O 0.0582(2) 0.43205(16) 0.84531(13) 0.0437(4) Uani 1 1 d . . .
C2 C -0.1165(4) 0.2812(3) 1.0230(2) 0.0514(8) Uani 1 1 d . . .
H2A H -0.0958 0.3654 1.0205 0.044(8) Uiso 1 1 calc R . .
H2B H -0.1293 0.2594 1.0897 0.055(8) Uiso 1 1 calc R . .
C3 C -0.2614(4) 0.2539(3) 0.9653(2) 0.0583(8) Uani 1 1 d . . .
H3A H -0.3440 0.3022 0.9886 0.066(10) Uiso 1 1 calc R . .
H3B H -0.2885 0.1717 0.9749 0.061(9) Uiso 1 1 calc R . .
C5 C -0.2137(3) 0.4405(3) 0.8355(2) 0.0538(8) Uani 1 1 d . . .
H5A H -0.2993 0.4762 0.8003 0.072(10) Uiso 1 1 calc R . .
H5B H -0.2140 0.4703 0.9009 0.063(9) Uiso 1 1 calc R . .
C6 C -0.0677(3) 0.4777(2) 0.7902(2) 0.0503(7) Uani 1 1 d . . .
H6A H -0.0652 0.4480 0.7249 0.042(7) Uiso 1 1 calc R . .
H6B H -0.0618 0.5633 0.7880 0.052(8) Uiso 1 1 calc R . .
C8 C 0.2009(3) 0.4481(3) 0.7988(2) 0.0516(7) Uani 1 1 d . . .
H8A H 0.2267 0.5315 0.7975 0.049(8) Uiso 1 1 calc R . .
H8B H 0.1919 0.4201 0.7330 0.046(8) Uiso 1 1 calc R . .
C9 C 0.3248(3) 0.3808(3) 0.8524(2) 0.0514(7) Uani 1 1 d . . .
H9A H 0.3333 0.4102 0.9178 0.065(10) Uiso 1 1 calc R . .
H9B H 0.4215 0.3955 0.8223 0.064(9) Uiso 1 1 calc R . .
C11 C 0.2900(3) 0.1923(3) 0.9833(2) 0.0528(8) Uani 1 1 d . . .
H11A H 0.2825 0.1078 0.9937 0.056(9) Uiso 1 1 calc R . .
H11B H 0.3856 0.2193 1.0130 0.060(9) Uiso 1 1 calc R . .
C12 C 0.1589(3) 0.2532(3) 1.02986(18) 0.0470(7) Uani 1 1 d . . .
H12A H 0.1597 0.2340 1.0978 0.051(8) Uiso 1 1 calc R . .
H12B H 0.1699 0.3381 1.0236 0.042(7) 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
Cu 0.03174(17) 0.03528(17) 0.02185(15) 0.00005(12) 0.00191(11) -0.00004(13)
Cl1 0.0549(4) 0.0590(4) 0.0231(3) 0.0034(3) 0.0021(3) 0.0083(3)
Cl2 0.1041(6) 0.0327(4) 0.0300(3) 0.0001(3) 0.0030(3) -0.0117(4)
N1 0.0480(13) 0.0298(12) 0.0249(10) -0.0005(9) 0.0040(9) -0.0053(10)
S4 0.0324(4) 0.0520(4) 0.0497(4) -0.0056(3) 0.0027(3) 0.0003(3)
S10 0.0343(4) 0.0509(4) 0.0437(4) -0.0037(3) 0.0012(3) 0.0005(3)
O7 0.0429(10) 0.0408(11) 0.0477(11) 0.0090(9) 0.0036(8) -0.0019(8)
C2 0.070(2) 0.0530(19) 0.0327(14) -0.0023(13) 0.0181(14) 0.0038(15)
C3 0.0484(18) 0.069(2) 0.059(2) -0.0030(16) 0.0280(15) -0.0002(16)
C5 0.0524(18) 0.0466(17) 0.0619(19) -0.0019(15) -0.0067(15) 0.0173(15)
C6 0.0617(19) 0.0365(16) 0.0524(18) 0.0084(13) -0.0038(14) 0.0080(13)
C8 0.0554(18) 0.0436(17) 0.0563(18) 0.0100(14) 0.0121(14) -0.0169(14)
C9 0.0388(16) 0.0571(19) 0.0586(19) 0.0044(15) 0.0082(13) -0.0180(14)
C11 0.0488(18) 0.061(2) 0.0473(17) 0.0053(15) -0.0200(14) -0.0066(15)
C12 0.064(2) 0.0494(16) 0.0268(13) -0.0004(12) -0.0058(12) -0.0189(14)

_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
Cu N1 2.0292(19) . ?
Cu Cl1 2.2530(8) . ?
Cu S4 2.4087(10) . ?
Cu S10 2.4139(11) . ?
Cu Cl2 2.4716(10) . ?
Cu O7 2.595(2) . ?
Cl2 H 2.47(3) 3_557 ?
N1 C12 1.469(3) . ?
N1 C2 1.475(4) . ?
S4 C3 1.811(3) . ?
S4 C5 1.820(3) . ?
S10 C11 1.808(3) . ?
S10 C9 1.824(3) . ?
O7 C6 1.419(3) . ?
O7 C8 1.435(3) . ?
C2 C3 1.511(4) . ?
C5 C6 1.502(4) . ?
C8 C9 1.503(4) . ?
C11 C12 1.502(4) . ?

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 Cu Cl1 177.31(7) . . ?
N1 Cu S4 86.63(7) . . ?
Cl1 Cu S4 92.77(3) . . ?
N1 Cu S10 86.69(7) . . ?
Cl1 Cu S10 92.74(3) . . ?
S4 Cu S10 154.08(3) . . ?
N1 Cu Cl2 86.56(6) . . ?
Cl1 Cu Cl2 96.13(3) . . ?
S4 Cu Cl2 103.90(3) . . ?
S10 Cu Cl2 100.66(3) . . ?
N1 Cu O7 85.05(7) . . ?
Cl1 Cu O7 92.26(4) . . ?
S4 Cu O7 77.18(5) . . ?
S10 Cu O7 77.31(4) . . ?
Cl2 Cu O7 171.46(4) . . ?
Cu Cl2 H 131.9(6) . 3_557 ?
C12 N1 C2 111.1(2) . . ?
C12 N1 Cu 114.25(16) . . ?
C2 N1 Cu 115.43(17) . . ?
C3 S4 C5 101.75(16) . . ?
C3 S4 Cu 93.29(11) . . ?
C5 S4 Cu 103.31(10) . . ?
C11 S10 C9 102.20(14) . . ?
C11 S10 Cu 92.62(10) . . ?
C9 S10 Cu 103.64(9) . . ?
C6 O7 C8 112.4(2) . . ?
C6 O7 Cu 103.58(15) . . ?
C8 O7 Cu 103.46(15) . . ?
N1 C2 C3 110.1(2) . . ?
C2 C3 S4 112.2(2) . . ?
C6 C5 S4 113.6(2) . . ?
O7 C6 C5 109.0(2) . . ?
O7 C8 C9 109.6(2) . . ?
C8 C9 S10 113.4(2) . . ?
C12 C11 S10 111.57(19) . . ?
N1 C12 C11 110.0(2) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        24.96
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.465
_refine_diff_density_min         -0.433
_refine_diff_density_rms         0.073

data_da146
_database_code_CSD               196824

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H17 Cu N O S2 2+, 2 (Br 1-)'
_chemical_formula_sum            'C8 H17 Br2 Cu N O S2'
_chemical_formula_weight         430.71

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Br Br -0.2901 2.4595 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/n

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

_cell_length_a                   9.708(3)
_cell_length_b                   10.823(4)
_cell_length_c                   13.658(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.76(3)
_cell_angle_gamma                90.00
_cell_volume                     1381.0(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    25
_cell_measurement_theta_min      8.66
_cell_measurement_theta_max      13.30

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.072
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             844
_exptl_absorpt_coefficient_mu    7.646
_exptl_absorpt_correction_type   psi-scans
_exptl_absorpt_correction_T_min  0.51
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   ?

_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  'CAD4 diffractometer'
_diffrn_measurement_method       omega
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         3
_diffrn_standards_interval_count 150
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            2427
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0917
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.00
_diffrn_reflns_theta_max         24.98
_reflns_number_total             2427
_reflns_number_gt                1426
_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^)+(0.0335P)^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    'riding model'
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2427
_refine_ls_number_parameters     153
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1162
_refine_ls_R_factor_gt           0.0316
_refine_ls_wR_factor_ref         0.0737
_refine_ls_wR_factor_gt          0.0615
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_restrained_S_all      0.975
_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
Cu Cu 0.07697(7) 0.20623(6) 0.76409(5) 0.03176(19) Uani 1 1 d . . .
Br1 Br -0.04617(7) 0.39680(6) 0.70424(5) 0.0453(2) Uani 1 1 d . . .
Br2 Br 0.16574(7) 0.16178(6) 0.59951(4) 0.0432(2) Uani 1 1 d . . .
S4 S -0.14522(16) 0.10444(15) 0.74283(11) 0.0395(4) Uani 1 1 d . . .
S10 S 0.28984(16) 0.30494(14) 0.85792(11) 0.0357(4) Uani 1 1 d . . .
O7 O 0.0338(4) 0.2379(4) 0.9411(3) 0.0380(10) Uani 1 1 d . . .
N1 N 0.1714(5) 0.0427(4) 0.8201(3) 0.0305(11) Uani 1 1 d . . .
C2 C 0.0719(7) -0.0498(6) 0.8421(5) 0.0441(16) Uani 1 1 d . . .
H2A H 0.0564 -0.0325 0.9080 0.052(18) Uiso 1 1 calc R . .
H2B H 0.1140 -0.1314 0.8449 0.036(16) Uiso 1 1 calc R . .
C3 C -0.0701(7) -0.0479(6) 0.7616(5) 0.0467(17) Uani 1 1 d . . .
H3A H -0.1364 -0.1030 0.7816 0.039(16) Uiso 1 1 calc R . .
H3B H -0.0567 -0.0781 0.6979 0.08(2) Uiso 1 1 calc R . .
H H 0.1840 -0.0203 0.7439 0.14(3) Uiso 1 1 d R . .
C5 C -0.1854(7) 0.1339(6) 0.8640(5) 0.0476(17) Uani 1 1 d . . .
H5A H -0.2884 0.1405 0.8516 0.032(15) Uiso 1 1 calc R . .
H5B H -0.1541 0.0632 0.9082 0.06(2) Uiso 1 1 calc R . .
C6 C -0.1188(6) 0.2462(6) 0.9180(5) 0.0447(17) Uani 1 1 d . . .
H6A H -0.1517 0.3182 0.8758 0.046(18) Uiso 1 1 calc R . .
H6B H -0.1471 0.2557 0.9804 0.037(15) Uiso 1 1 calc R . .
C8 C 0.1021(7) 0.3523(6) 0.9758(4) 0.0450(16) Uani 1 1 d . . .
H8A H 0.0920 0.3713 1.0429 0.049(17) Uiso 1 1 calc R . .
H8B H 0.0580 0.4183 0.9299 0.08(2) Uiso 1 1 calc R . .
C9 C 0.2594(6) 0.3421(6) 0.9798(4) 0.0414(15) Uani 1 1 d . . .
H9A H 0.3030 0.2786 1.0285 0.040(17) Uiso 1 1 calc R . .
H9B H 0.3063 0.4198 1.0037 0.037(16) Uiso 1 1 calc R . .
C11 C 0.3902(6) 0.1631(5) 0.8874(5) 0.0426(16) Uani 1 1 d . . .
H11A H 0.4278 0.1407 0.8308 0.055(19) Uiso 1 1 calc R . .
H11B H 0.4706 0.1754 0.9468 0.044(17) Uiso 1 1 calc R . .
C12 C 0.2976(6) 0.0595(6) 0.9077(4) 0.0391(16) Uani 1 1 d . . .
H12A H 0.3527 -0.0165 0.9202 0.045(17) Uiso 1 1 calc R . .
H12B H 0.2669 0.0784 0.9679 0.041(16) 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
Cu 0.0318(4) 0.0326(4) 0.0311(4) 0.0057(3) 0.0089(3) 0.0013(4)
Br1 0.0496(4) 0.0394(4) 0.0479(4) 0.0138(3) 0.0150(3) 0.0125(3)
Br2 0.0535(4) 0.0468(4) 0.0358(3) 0.0026(3) 0.0233(3) 0.0013(3)
S4 0.0347(9) 0.0492(10) 0.0342(8) 0.0049(7) 0.0086(7) -0.0022(8)
S10 0.0388(9) 0.0352(9) 0.0348(8) -0.0008(7) 0.0129(7) -0.0002(8)
O7 0.031(2) 0.046(3) 0.038(2) -0.004(2) 0.0134(19) 0.002(2)
N1 0.033(3) 0.028(3) 0.028(3) 0.000(2) 0.004(2) 0.003(2)
C2 0.050(4) 0.034(4) 0.051(4) 0.011(3) 0.017(3) 0.003(3)
C3 0.050(4) 0.040(4) 0.055(4) -0.001(3) 0.022(4) -0.012(4)
C5 0.038(4) 0.061(5) 0.050(4) 0.008(4) 0.023(3) -0.002(4)
C6 0.044(4) 0.057(5) 0.041(4) 0.001(3) 0.026(3) 0.010(4)
C8 0.051(4) 0.052(4) 0.032(3) -0.012(3) 0.012(3) 0.003(4)
C9 0.049(4) 0.042(4) 0.032(3) -0.009(3) 0.009(3) -0.004(4)
C11 0.029(3) 0.041(4) 0.055(4) -0.007(3) 0.008(3) 0.002(3)
C12 0.041(4) 0.036(4) 0.037(4) 0.003(3) 0.005(3) 0.016(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
Cu N1 2.044(4) . ?
Cu S4 2.3686(18) . ?
Cu S10 2.3697(18) . ?
Cu Br1 2.4125(12) . ?
Cu O7 2.587(4) . ?
Cu Br2 2.6607(12) . ?
S4 C3 1.793(6) . ?
S4 C5 1.829(6) . ?
S10 C11 1.804(6) . ?
S10 C9 1.812(5) . ?
O7 C8 1.423(7) . ?
O7 C6 1.431(6) . ?
N1 C12 1.473(6) . ?
N1 C2 1.478(7) . ?
C2 C3 1.512(8) . ?
C5 C6 1.477(8) . ?
C8 C9 1.517(8) . ?
C11 C12 1.508(8) . ?

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 Cu S4 86.80(13) . . ?
N1 Cu S10 87.21(13) . . ?
S4 Cu S10 155.14(6) . . ?
N1 Cu Br1 176.16(13) . . ?
S4 Cu Br1 90.29(5) . . ?
S10 Cu Br1 94.41(5) . . ?
N1 Cu O7 86.28(15) . . ?
S4 Cu O7 78.63(10) . . ?
S10 Cu O7 76.91(10) . . ?
Br1 Cu O7 90.70(9) . . ?
N1 Cu Br2 86.81(12) . . ?
S4 Cu Br2 107.79(5) . . ?
S10 Cu Br2 95.94(5) . . ?
Br1 Cu Br2 96.47(3) . . ?
O7 Cu Br2 170.28(9) . . ?
C3 S4 C5 102.1(3) . . ?
C3 S4 Cu 95.1(2) . . ?
C5 S4 Cu 102.7(2) . . ?
C11 S10 C9 101.3(3) . . ?
C11 S10 Cu 94.3(2) . . ?
C9 S10 Cu 105.1(2) . . ?
C8 O7 C6 112.3(5) . . ?
C8 O7 Cu 104.3(3) . . ?
C6 O7 Cu 102.9(3) . . ?
C12 N1 C2 111.4(4) . . ?
C12 N1 Cu 112.7(3) . . ?
C2 N1 Cu 114.3(3) . . ?
N1 C2 C3 111.1(5) . . ?
C2 C3 S4 111.8(4) . . ?
C6 C5 S4 115.0(4) . . ?
O7 C6 C5 110.2(5) . . ?
O7 C8 C9 108.8(5) . . ?
C8 C9 S10 113.4(4) . . ?
C12 C11 S10 111.1(4) . . ?
N1 C12 C11 110.4(5) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        24.98
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.566
_refine_diff_density_min         -0.562
_refine_diff_density_rms         0.125

data_da148
_database_code_CSD               196825

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C10 H20 Hg N2 O S2 2+, 2 (ClO4 1-)'
_chemical_formula_sum            'C10 H20 Cl2 Hg N2 O9 S2'
_chemical_formula_weight         647.89

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pbca
_symmetry_Int_Tables_number      61

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

_cell_length_a                   7.940(3)
_cell_length_b                   15.503(2)
_cell_length_c                   31.611(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3891.1(16)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    25
_cell_measurement_theta_min      9.4
_cell_measurement_theta_max      16.7

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.212
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2496
_exptl_absorpt_coefficient_mu    8.446
_exptl_absorpt_correction_type   psi-scans
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   ?

_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  'CAD4 diffractometer'
_diffrn_measurement_method       omega
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         3
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            3373
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1063
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         3.16
_diffrn_reflns_theta_max         24.96
_reflns_number_total             3368
_reflns_number_gt                1687
_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^)+(0.0700P)^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    'riding model'
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3368
_refine_ls_number_parameters     255
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1542
_refine_ls_R_factor_gt           0.0415
_refine_ls_wR_factor_ref         0.1246
_refine_ls_wR_factor_gt          0.0982
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_restrained_S_all      0.968
_refine_ls_shift/su_max          1.529
_refine_ls_shift/su_mean         0.019

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
Hg Hg 0.15051(6) 0.26531(3) 0.116923(17) 0.0518(2) Uani 1 1 d . . .
N1 N 0.361(2) 0.3473(8) 0.0809(4) 0.077(5) Uani 1 1 d . . .
H H 0.363(12) 0.325(5) 0.065(3) 0.00(2) Uiso 1 1 d . . .
S4 S 0.0152(4) 0.4136(2) 0.12466(12) 0.0681(10) Uani 1 1 d . . .
S10 S 0.4088(5) 0.1957(2) 0.14831(15) 0.0736(11) Uani 1 1 d . . .
O7 O 0.1444(16) 0.3039(7) 0.2018(3) 0.095(3) Uani 1 1 d . . .
C2 C 0.289(4) 0.4328(10) 0.0746(8) 0.173(14) Uani 1 1 d . . .
H2A H 0.3849 0.4715 0.0720 0.27(14) Uiso 1 1 calc R . .
H2B H 0.2365 0.4312 0.0469 2(2) Uiso 1 1 calc R . .
C3 C 0.184(2) 0.4718(11) 0.0989(10) 0.125(8) Uani 1 1 d . . .
H3A H 0.1325 0.5173 0.0823 2(2) Uiso 1 1 calc R . .
H3B H 0.2492 0.4997 0.1209 0.14(9) Uiso 1 1 calc R . .
C5 C 0.039(3) 0.4331(13) 0.1833(6) 0.145(10) Uani 1 1 d . . .
H5A H 0.0551 0.4946 0.1872 0.08(4) Uiso 1 1 calc R . .
H5B H -0.0671 0.4183 0.1965 0.18(11) Uiso 1 1 calc R . .
C6 C 0.166(4) 0.3914(12) 0.2064(7) 0.126(8) Uani 1 1 d . . .
H6A H 0.2764 0.4084 0.1959 0.5(4) Uiso 1 1 calc R . .
H6B H 0.1591 0.4072 0.2361 2(3) Uiso 1 1 calc R . .
C8 C 0.289(2) 0.256(2) 0.2207(6) 0.135(9) Uani 1 1 d . . .
H8A H 0.3231 0.2882 0.2457 0.23(13) Uiso 1 1 calc R . .
H8B H 0.2454 0.2014 0.2305 0.3(2) Uiso 1 1 calc R . .
C9 C 0.429(3) 0.2392(17) 0.1989(7) 0.131(8) Uani 1 1 d . . .
H9A H 0.4963 0.1996 0.2156 0.07(4) Uiso 1 1 calc R . .
H9B H 0.4925 0.2924 0.1965 0.9(9) Uiso 1 1 calc R . .
C11 C 0.556(2) 0.2669(13) 0.1222(12) 0.185(16) Uani 1 1 d . . .
H11A H 0.6376 0.2834 0.1435 0.4(2) Uiso 1 1 calc R . .
H11B H 0.6159 0.2316 0.1018 0.23(15) Uiso 1 1 calc R . .
C12 C 0.516(3) 0.338(2) 0.1023(6) 0.142(11) Uani 1 1 d . . .
H12A H 0.6041 0.3482 0.0817 0.16(8) Uiso 1 1 calc R . .
H12B H 0.5224 0.3841 0.1229 0.19(12) Uiso 1 1 calc R . .
Cl1 Cl 0.2727(4) 0.15605(18) 0.00287(10) 0.0488(7) Uani 1 1 d . . .
Cl2 Cl -0.0910(5) 0.0634(2) 0.19039(13) 0.0711(10) Uani 1 1 d . . .
O11 O 0.3916(14) 0.1295(8) -0.0270(4) 0.112(4) Uani 1 1 d . . .
O12 O 0.3403(13) 0.1481(7) 0.0447(3) 0.089(3) Uani 1 1 d . . .
O13 O 0.1222(11) 0.1049(6) -0.0016(3) 0.078(3) Uani 1 1 d . . .
O14 O 0.2352(16) 0.2441(6) -0.0029(4) 0.096(3) Uani 1 1 d . . .
O21 O -0.123(2) -0.0169(14) 0.1784(8) 0.283(15) Uani 1 1 d . . .
O22 O -0.081(3) 0.0654(12) 0.2329(4) 0.217(9) Uani 1 1 d . . .
O23 O 0.0682(14) 0.0857(8) 0.1715(4) 0.118(4) Uani 1 1 d . . .
O24 O -0.206(2) 0.1163(16) 0.1785(8) 0.287(15) Uani 1 1 d . . .
N1S N -0.0372(13) 0.1818(6) 0.0872(3) 0.055(3) Uani 1 1 d . . .
C1S C -0.2420(18) 0.0724(7) 0.0519(4) 0.066(4) Uani 1 1 d . . .
C2S C -0.1249(15) 0.1337(7) 0.0725(4) 0.048(3) 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
Hg 0.0446(3) 0.0470(3) 0.0638(3) -0.0087(3) -0.0036(3) -0.0106(2)
N1 0.107(11) 0.064(8) 0.061(9) -0.034(7) 0.027(9) -0.030(8)
S4 0.057(2) 0.065(2) 0.083(3) -0.004(2) -0.0138(19) 0.0181(17)
S10 0.065(2) 0.0440(17) 0.112(3) -0.001(2) -0.025(2) 0.0061(16)
O7 0.138(10) 0.070(6) 0.077(7) 0.006(6) 0.002(7) 0.011(7)
C2 0.24(3) 0.034(9) 0.24(3) 0.005(12) 0.19(2) 0.012(13)
C3 0.100(15) 0.057(10) 0.22(2) 0.028(14) 0.001(17) 0.014(10)
C5 0.14(2) 0.143(16) 0.147(18) -0.130(15) -0.087(16) 0.100(15)
C6 0.21(3) 0.079(12) 0.091(14) -0.013(10) -0.045(15) 0.040(14)
C8 0.061(11) 0.28(3) 0.060(11) 0.038(18) -0.019(10) -0.010(17)
C9 0.117(17) 0.17(2) 0.108(16) 0.005(15) -0.046(15) 0.063(16)
C11 0.036(9) 0.092(13) 0.43(5) 0.12(2) -0.003(18) 0.008(9)
C12 0.102(16) 0.28(3) 0.048(11) 0.045(16) -0.033(11) -0.108(19)
Cl1 0.0552(18) 0.0415(16) 0.0498(19) -0.0059(14) -0.0022(17) 0.0005(14)
Cl2 0.062(2) 0.079(2) 0.073(3) -0.009(2) 0.0083(19) 0.0087(19)
O11 0.076(8) 0.144(10) 0.115(10) -0.058(8) 0.036(7) -0.017(7)
O12 0.101(8) 0.106(8) 0.061(7) 0.004(6) -0.030(6) -0.013(6)
O13 0.071(6) 0.082(6) 0.081(7) -0.024(5) 0.004(6) -0.019(5)
O14 0.117(9) 0.063(6) 0.110(8) 0.019(6) 0.007(8) 0.018(6)
O21 0.182(17) 0.24(2) 0.43(3) -0.24(2) 0.17(2) -0.125(16)
O22 0.37(3) 0.207(16) 0.071(10) 0.012(11) 0.026(14) 0.004(19)
O23 0.069(8) 0.126(10) 0.160(12) 0.013(9) 0.024(8) -0.003(7)
O24 0.159(16) 0.39(3) 0.31(2) 0.21(2) 0.107(16) 0.203(19)
N1S 0.052(7) 0.053(6) 0.059(7) 0.004(5) -0.005(6) -0.019(6)
C1S 0.064(8) 0.043(7) 0.092(10) -0.020(7) -0.011(8) -0.024(6)
C2S 0.043(7) 0.041(6) 0.060(8) 0.003(6) 0.008(7) -0.002(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
Hg N1S 2.187(10) . ?
Hg N1 2.389(13) . ?
Hg S10 2.521(4) . ?
Hg S4 2.550(3) . ?
Hg O7 2.748(10) . ?
N1 C12 1.41(2) . ?
N1 C2 1.46(2) . ?
S4 C3 1.809(19) . ?
S4 C5 1.888(17) . ?
S10 C9 1.74(2) . ?
S10 C11 1.81(2) . ?
O7 C6 1.38(2) . ?
O7 C8 1.49(2) . ?
C2 C3 1.29(2) . ?
C5 C6 1.40(2) . ?
C8 C9 1.33(2) . ?
C11 C12 1.30(2) . ?
Cl1 O11 1.398(10) . ?
Cl1 O14 1.410(9) . ?
Cl1 O12 1.433(9) . ?
Cl1 O13 1.441(9) . ?
Cl2 O24 1.285(13) . ?
Cl2 O21 1.324(16) . ?
Cl2 O22 1.348(14) . ?
Cl2 O23 1.440(11) . ?
N1S C2S 1.121(13) . ?
C1S C2S 1.480(17) . ?

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
N1S Hg N1 125.9(4) . . ?
N1S Hg S10 118.0(3) . . ?
N1 Hg S10 81.2(4) . . ?
N1S Hg S4 106.7(3) . . ?
N1 Hg S4 82.0(4) . . ?
S10 Hg S4 133.72(12) . . ?
N1S Hg O7 122.4(4) . . ?
N1 Hg O7 111.2(4) . . ?
S10 Hg O7 73.9(3) . . ?
S4 Hg O7 72.7(2) . . ?
C12 N1 C2 120(2) . . ?
C12 N1 Hg 108.9(11) . . ?
C2 N1 Hg 106.1(12) . . ?
C3 S4 C5 106.7(13) . . ?
C3 S4 Hg 95.4(6) . . ?
C5 S4 Hg 101.3(5) . . ?
C9 S10 C11 97.1(16) . . ?
C9 S10 Hg 105.7(7) . . ?
C11 S10 Hg 94.8(7) . . ?
C6 O7 C8 110.3(18) . . ?
C6 O7 Hg 108.5(11) . . ?
C8 O7 Hg 105.7(11) . . ?
C3 C2 N1 126.8(18) . . ?
C2 C3 S4 121.1(15) . . ?
C6 C5 S4 120.7(14) . . ?
O7 C6 C5 108(2) . . ?
C9 C8 O7 122.2(18) . . ?
C8 C9 S10 118.3(18) . . ?
C12 C11 S10 125.3(16) . . ?
C11 C12 N1 122(2) . . ?
O11 Cl1 O14 109.9(7) . . ?
O11 Cl1 O12 110.2(7) . . ?
O14 Cl1 O12 106.4(7) . . ?
O11 Cl1 O13 109.4(6) . . ?
O14 Cl1 O13 110.2(7) . . ?
O12 Cl1 O13 110.7(6) . . ?
O24 Cl2 O21 112.4(18) . . ?
O24 Cl2 O22 108.6(15) . . ?
O21 Cl2 O22 108.5(15) . . ?
O24 Cl2 O23 110.5(10) . . ?
O21 Cl2 O23 105.9(9) . . ?
O22 Cl2 O23 110.9(13) . . ?
C2S N1S Hg 174.5(10) . . ?
N1S C2S C1S 177.9(14) . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        24.96
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         0.803
_refine_diff_density_min         -1.943
_refine_diff_density_rms         0.169

data_da152
_database_code_CSD               196826

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H17 Cd N3 O7 S2'
_chemical_formula_sum            'C8 H17 Cd N3 O7 S2'
_chemical_formula_weight         443.77

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cd Cd -0.8075 1.2024 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   P212121

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

_cell_length_a                   8.950(2)
_cell_length_b                   11.980(3)
_cell_length_c                   14.746(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1581.1(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    25
_cell_measurement_theta_min      9.8
_cell_measurement_theta_max      15.5

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.864
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             888
_exptl_absorpt_coefficient_mu    1.678
_exptl_absorpt_correction_type   psi-scans
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   ?

_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  'CAD4 diffractometer'
_diffrn_measurement_method       omega
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         3
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            3436
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0241
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.16
_diffrn_reflns_theta_max         26.96
_reflns_number_total             3436
_reflns_number_gt                2892
_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^)+(0.0267P)^2^+0.3667P] 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    'riding model'
_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   -0.06(3)
_refine_ls_number_reflns         3436
_refine_ls_number_parameters     194
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0226
_refine_ls_wR_factor_ref         0.0564
_refine_ls_wR_factor_gt          0.0524
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.045
_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
Cd Cd 0.14851(2) 0.511931(18) 0.221571(15) 0.05177(7) Uani 1 1 d . . .
N1 N 0.0995(4) 0.3677(3) 0.1202(3) 0.0672(9) Uani 1 1 d . . .
H H 0.030(4) 0.341(3) 0.137(2) 0.040(10) Uiso 1 1 d . . .
S4 S 0.04152(16) 0.63050(10) 0.08326(8) 0.0847(4) Uani 1 1 d . . .
S10 S 0.36943(13) 0.37159(10) 0.26397(8) 0.0840(3) Uani 1 1 d . . .
O7 O 0.3639(3) 0.5465(2) 0.1108(2) 0.0812(8) Uani 1 1 d . . .
C2 C 0.0664(6) 0.4083(4) 0.0281(3) 0.0830(13) Uani 1 1 d . . .
H2A H 0.0191 0.3489 -0.0062 0.100 Uiso 1 1 calc R . .
H2B H 0.1593 0.4272 -0.0020 0.100 Uiso 1 1 calc R . .
C3 C -0.0323(5) 0.5071(5) 0.0280(3) 0.0980(14) Uani 1 1 d . . .
H3A H -0.1255 0.4870 0.0574 0.118 Uiso 1 1 calc R . .
H3B H -0.0553 0.5259 -0.0345 0.118 Uiso 1 1 calc R . .
C5 C 0.2096(7) 0.6615(5) 0.0191(3) 0.1060(18) Uani 1 1 d . . .
H5A H 0.2155 0.6101 -0.0316 0.127 Uiso 1 1 calc R . .
H5B H 0.2008 0.7362 -0.0056 0.127 Uiso 1 1 calc R . .
C6 C 0.3496(7) 0.6544(4) 0.0706(4) 0.1061(17) Uani 1 1 d . . .
H6A H 0.4335 0.6681 0.0305 0.127 Uiso 1 1 calc R . .
H6B H 0.3504 0.7110 0.1176 0.127 Uiso 1 1 calc R . .
C8 C 0.5057(5) 0.5264(5) 0.1495(4) 0.0987(16) Uani 1 1 d . . .
H8A H 0.5253 0.5825 0.1955 0.118 Uiso 1 1 calc R . .
H8B H 0.5816 0.5337 0.1030 0.118 Uiso 1 1 calc R . .
C9 C 0.5169(5) 0.4144(5) 0.1911(4) 0.112(2) Uani 1 1 d . . .
H9A H 0.6094 0.4113 0.2253 0.135 Uiso 1 1 calc R . .
H9B H 0.5249 0.3601 0.1425 0.135 Uiso 1 1 calc R . .
C11 C 0.2850(7) 0.2574(4) 0.2055(4) 0.1080(18) Uani 1 1 d . . .
H11A H 0.3604 0.2003 0.1967 0.130 Uiso 1 1 calc R . .
H11B H 0.2085 0.2260 0.2445 0.130 Uiso 1 1 calc R . .
C12 C 0.2167(6) 0.2816(4) 0.1170(4) 0.0939(15) Uani 1 1 d . . .
H12A H 0.1740 0.2133 0.0930 0.113 Uiso 1 1 calc R . .
H12B H 0.2943 0.3057 0.0755 0.113 Uiso 1 1 calc R . .
N2 N -0.0968(5) 0.4485(3) 0.3354(3) 0.0905(12) Uani 1 1 d . . .
O21 O 0.0373(4) 0.4308(3) 0.3526(3) 0.1104(12) Uani 1 1 d . . .
O22 O -0.1253(3) 0.4912(3) 0.2608(2) 0.0934(9) Uani 1 1 d . . .
O23 O -0.1963(5) 0.4250(4) 0.3885(3) 0.161(2) Uani 1 1 d . . .
N3 N 0.2183(4) 0.6965(3) 0.3413(2) 0.0694(8) Uani 1 1 d . . .
O31 O 0.3213(5) 0.6370(3) 0.3177(3) 0.1251(14) Uani 1 1 d . . .
O32 O 0.1001(5) 0.6811(3) 0.3024(3) 0.1227(15) Uani 1 1 d . . .
O33 O 0.2308(4) 0.7701(3) 0.3976(2) 0.0893(10) 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
Cd 0.04728(11) 0.05597(12) 0.05206(12) 0.00164(11) 0.00167(11) 0.00371(11)
N1 0.057(2) 0.066(2) 0.078(2) -0.0036(17) -0.0064(18) -0.0045(16)
S4 0.0983(9) 0.0786(7) 0.0772(7) 0.0137(6) -0.0070(7) 0.0284(7)
S10 0.0764(7) 0.0927(7) 0.0830(7) 0.0053(6) -0.0180(6) 0.0215(6)
O7 0.0642(17) 0.0954(19) 0.0839(18) 0.0117(15) 0.0124(16) -0.0136(17)
C2 0.086(3) 0.094(3) 0.069(3) -0.016(2) -0.016(2) -0.001(3)
C3 0.078(3) 0.124(4) 0.092(3) 0.001(3) -0.032(2) 0.013(3)
C5 0.137(5) 0.104(4) 0.076(3) 0.035(3) 0.008(3) -0.005(3)
C6 0.118(4) 0.106(4) 0.094(3) 0.024(3) 0.017(4) -0.044(4)
C8 0.053(2) 0.138(5) 0.105(4) -0.014(3) 0.011(2) -0.021(3)
C9 0.046(2) 0.148(5) 0.144(5) -0.005(4) -0.008(3) 0.015(3)
C11 0.110(4) 0.069(3) 0.145(5) 0.002(3) -0.022(4) 0.021(2)
C12 0.095(3) 0.066(3) 0.120(4) -0.025(3) -0.016(3) 0.017(2)
N2 0.079(3) 0.094(3) 0.099(3) 0.006(2) 0.038(3) -0.007(2)
O21 0.080(2) 0.145(3) 0.106(3) 0.039(2) 0.015(2) 0.016(2)
O22 0.0637(16) 0.109(2) 0.107(2) -0.003(2) 0.0073(15) -0.0053(18)
O23 0.121(3) 0.190(5) 0.172(4) 0.018(4) 0.096(3) -0.018(3)
N3 0.079(2) 0.063(2) 0.066(2) -0.0076(16) -0.0077(19) 0.0029(18)
O31 0.107(3) 0.125(3) 0.144(3) -0.050(3) 0.005(3) 0.027(3)
O32 0.109(3) 0.102(2) 0.158(4) -0.047(3) -0.045(3) 0.013(2)
O33 0.098(2) 0.081(2) 0.089(2) -0.0260(17) -0.0140(19) 0.0043(17)

_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
Cd N1 2.326(4) . ?
Cd O21 2.381(4) . ?
Cd O32 2.391(4) . ?
Cd O22 2.530(3) . ?
Cd O7 2.561(3) . ?
Cd O31 2.578(4) . ?
Cd S4 2.6635(12) . ?
Cd S10 2.6697(11) . ?
N1 C12 1.472(6) . ?
N1 C2 1.473(6) . ?
S4 C3 1.813(5) . ?
S4 C5 1.816(6) . ?
S10 C9 1.778(6) . ?
S10 C11 1.785(5) . ?
O7 C8 1.413(5) . ?
O7 C6 1.428(6) . ?
C2 C3 1.476(6) . ?
C5 C6 1.467(7) . ?
C8 C9 1.479(8) . ?
C11 C12 1.469(8) . ?
N2 O23 1.219(5) . ?
N2 O22 1.240(5) . ?
N2 O21 1.245(5) . ?
N3 O31 1.216(5) . ?
N3 O33 1.217(4) . ?
N3 O32 1.217(4) . ?

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 Cd O21 98.01(15) . . ?
N1 Cd O32 156.33(13) . . ?
O21 Cd O32 82.26(16) . . ?
N1 Cd O22 83.76(12) . . ?
O21 Cd O22 50.92(12) . . ?
O32 Cd O22 78.09(13) . . ?
N1 Cd O7 81.50(12) . . ?
O21 Cd O7 153.97(12) . . ?
O32 Cd O7 108.52(13) . . ?
O22 Cd O7 152.97(11) . . ?
N1 Cd O31 153.91(13) . . ?
O21 Cd O31 92.40(15) . . ?
O32 Cd O31 48.83(12) . . ?
O22 Cd O31 120.82(12) . . ?
O7 Cd O31 78.77(13) . . ?
N1 Cd S4 80.59(10) . . ?
O21 Cd S4 133.54(10) . . ?
O32 Cd S4 82.23(11) . . ?
O22 Cd S4 83.05(9) . . ?
O7 Cd S4 72.29(8) . . ?
O31 Cd S4 109.06(11) . . ?
N1 Cd S10 79.76(9) . . ?
O21 Cd S10 82.10(10) . . ?
O32 Cd S10 123.45(10) . . ?
O22 Cd S10 127.02(9) . . ?
O7 Cd S10 72.17(8) . . ?
O31 Cd S10 78.06(10) . . ?
S4 Cd S10 141.39(4) . . ?
C12 N1 C2 110.2(4) . . ?
C12 N1 Cd 114.0(3) . . ?
C2 N1 Cd 112.6(3) . . ?
C3 S4 C5 103.6(3) . . ?
C3 S4 Cd 92.31(16) . . ?
C5 S4 Cd 102.12(17) . . ?
C9 S10 C11 104.1(3) . . ?
C9 S10 Cd 103.09(19) . . ?
C11 S10 Cd 93.19(16) . . ?
C8 O7 C6 113.8(4) . . ?
C8 O7 Cd 113.0(3) . . ?
C6 O7 Cd 110.1(3) . . ?
N1 C2 C3 112.7(4) . . ?
C2 C3 S4 115.8(3) . . ?
C6 C5 S4 115.2(3) . . ?
O7 C6 C5 110.1(4) . . ?
O7 C8 C9 112.5(4) . . ?
C8 C9 S10 117.5(4) . . ?
C12 C11 S10 117.0(4) . . ?
C11 C12 N1 113.9(4) . . ?
O23 N2 O22 121.1(5) . . ?
O23 N2 O21 122.2(5) . . ?
O22 N2 O21 116.7(4) . . ?
N2 O21 Cd 99.7(3) . . ?
N2 O22 Cd 92.5(2) . . ?
O31 N3 O33 123.4(4) . . ?
O31 N3 O32 115.8(4) . . ?
O33 N3 O32 120.8(4) . . ?
N3 O31 Cd 92.5(3) . . ?
N3 O32 Cd 101.9(3) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        26.96
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.272
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.055

data_da177
_database_code_CSD               196827

_audit_creation_method           SHELXL
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_structural     ?
_chemical_formula_analytical     'C19 H28 Fe N O S2 1+, I 1-'
_chemical_formula_sum            'C19 H28 Fe I N O S2'
_chemical_formula_weight         533.29
_chemical_melting_point          ?
_chemical_compound_source        ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pna21

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

_cell_length_a                   11.4740(10)
_cell_length_b                   17.1420(10)
_cell_length_c                   10.7710(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2118.5(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6840
_cell_measurement_theta_min      3.0
_cell_measurement_theta_max      48.9

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow-orange
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1072
_exptl_absorpt_coefficient_mu    2.374
_exptl_absorpt_correction_type   SADABS
_exptl_absorpt_correction_T_min  0.903
_exptl_absorpt_correction_T_max  1.000

_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       'SMART CCD DIFFRACTOMETER'
_diffrn_measurement_method       'omega scan'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            27925
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_sigmaI/netI    0.3150
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.14
_diffrn_reflns_theta_max         32.23
_reflns_number_total             3762
_reflns_number_observed          2354
_reflns_observed_criterion       >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^
or flagged by the user for potential systematic errors.  Weighted R-factors
wR and all goodnesses 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 observed criterion
of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0000P)^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    ?
_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   0.05(2)
_refine_ls_number_reflns         3762
_refine_ls_number_parameters     282
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_obs          0.0246
_refine_ls_wR_factor_all         0.0485
_refine_ls_wR_factor_obs         0.0470
_refine_ls_goodness_of_fit_all   0.550
_refine_ls_goodness_of_fit_obs   0.690
_refine_ls_restrained_S_all      0.550
_refine_ls_restrained_S_obs      0.690
_refine_ls_shift/esd_max         0.414
_refine_ls_shift/esd_mean        0.006

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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
I I 0.63690(2) 0.606247(13) 0.37904(3) 0.05699(8) Uani 1 d . .
Fe Fe -0.32232(5) 0.33602(3) 0.49558(5) 0.04139(12) Uani 1 d . .
S10 S -0.25086(9) 0.56015(5) 0.02815(10) 0.0548(3) Uani 1 d . .
S4 S 0.04126(8) 0.33569(6) 0.07638(10) 0.0516(2) Uani 1 d . .
O7 O -0.0922(2) 0.43897(12) -0.1169(3) 0.0504(5) Uani 1 d . .
N1 N -0.2250(2) 0.38247(15) 0.1045(3) 0.0336(6) Uani 1 d . .
C12 C -0.3379(3) 0.4068(2) 0.0448(4) 0.0402(8) Uani 1 d . .
H12A H -0.4007(3) 0.3754(2) 0.0787(4) 0.030(9) Uiso 1 calc R .
H12B H -0.3337(3) 0.3965(2) -0.0436(4) 0.043(10) Uiso 1 calc R .
C11 C -0.3656(3) 0.4923(2) 0.0648(4) 0.0467(8) Uani 1 d . .
H11A H -0.3870(3) 0.4995(2) 0.1512(4) 0.033(9) Uiso 1 calc R .
H11B H -0.4332(3) 0.5054(2) 0.0149(4) 0.066(12) Uiso 1 calc R .
C9 C -0.2297(4) 0.5436(2) -0.1369(4) 0.0566(10) Uani 1 d . .
H9A H -0.2868(4) 0.5060(2) -0.1657(4) 0.043(10) Uiso 1 calc R .
H9B H -0.2430(4) 0.5921(2) -0.1812(4) 2.000(721) Uiso 1 calc R .
C8 C -0.1096(4) 0.5141(2) -0.1668(4) 0.0597(11) Uani 1 d . .
H8A H -0.0993(4) 0.5123(2) -0.2562(4) 0.065(12) Uiso 1 calc R .
H8B H -0.0519(4) 0.5496(2) -0.1330(4) 0.051(10) Uiso 1 calc R .
C6 C 0.0211(3) 0.4110(2) -0.1482(4) 0.0580(11) Uani 1 d . .
H6A H 0.0794(3) 0.4474(2) -0.1185(4) 0.051(9) Uiso 1 calc R .
H6B H 0.0283(3) 0.4075(2) -0.2378(4) 0.067(12) Uiso 1 calc R .
C5 C 0.0422(3) 0.3327(2) -0.0921(4) 0.0545(10) Uani 1 d . .
H5A H 0.1170(3) 0.3131(2) -0.1203(4) 0.050(9) Uiso 1 calc R .
H5B H -0.0175(3) 0.2968(2) -0.1204(4) 0.055(10) Uiso 1 calc R .
C3 C -0.0801(3) 0.2729(2) 0.1120(4) 0.0480(9) Uani 1 d . .
H3A H -0.0651(3) 0.2218(2) 0.0767(4) 0.066(12) Uiso 1 calc R .
H3B H -0.0847(3) 0.2668(2) 0.2014(4) 0.028(8) Uiso 1 calc R .
C2 C -0.1961(3) 0.3013(2) 0.0654(3) 0.0386(8) Uani 1 d . .
H2A H -0.1963(3) 0.2989(2) -0.0246(3) 0.051(11) Uiso 1 calc R .
H2B H -0.2565(3) 0.2665(2) 0.0952(3) 0.035(9) Uiso 1 calc R .
C13 C -0.2252(3) 0.3935(2) 0.2447(3) 0.0354(7) Uani 1 d . .
C14 C -0.3135(3) 0.3462(2) 0.3104(3) 0.0343(8) Uani 1 d . .
C15 C -0.4228(3) 0.3739(2) 0.3540(3) 0.0416(8) Uani 1 d . .
C16 C -0.4797(3) 0.3124(2) 0.4173(3) 0.0497(9) Uani 1 d . .
C17 C -0.4060(3) 0.2464(2) 0.4128(4) 0.0537(10) Uani 1 d . .
H17 H -0.4223(3) 0.1980(2) 0.4479(4) 0.067(13) Uiso 1 calc R .
C18 C -0.3040(3) 0.2654(2) 0.3469(3) 0.0445(9) Uani 1 d . .
C19A C -0.3549(10) 0.3740(10) 0.6738(8) 0.067(3) Uani 0.60 d P .
C20A C -0.2923(15) 0.4316(5) 0.6073(10) 0.069(3) Uani 0.60 d P .
C19B C -0.1764(15) 0.3499(14) 0.5867(17) 0.056(6) Uani 0.40 d P .
C22A C -0.1730(16) 0.3192(11) 0.6148(14) 0.078(4) Uani 0.60 d P .
H1 H -0.1634(30) 0.4121(20) 0.0768(35) 0.042(10) Uiso 1 d . .
C22B C -0.3450(15) 0.3379(10) 0.6849(14) 0.051(4) Uiso 0.40 d P .
C21B C -0.3359(13) 0.4139(10) 0.6372(17) 0.048(4) Uiso 0.40 d P .
C21A C -0.1903(11) 0.3974(8) 0.5702(9) 0.058(2) Uiso 0.60 d P .
C20B C -0.2263(16) 0.4266(9) 0.5747(14) 0.051(3) Uiso 0.40 d P .
C23B C -0.2437(17) 0.2979(9) 0.6614(15) 0.054(3) Uiso 0.40 d P .
C23A C -0.2876(12) 0.3028(7) 0.6767(9) 0.067(3) Uiso 0.60 d P .
H15 H -0.4513(27) 0.4217(19) 0.3431(32) 0.038(9) Uiso 1 d . .
H16 H -0.5507(30) 0.3165(19) 0.4609(33) 0.046(10) Uiso 1 d . .
H18 H -0.2426(26) 0.2349(18) 0.3282(32) 0.035(9) Uiso 1 d . .
H13A H -0.1488(31) 0.3873(19) 0.2691(35) 0.035(9) Uiso 1 d . .
H13B H -0.2331(29) 0.4477(21) 0.2534(35) 0.040(9) Uiso 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
I 0.04815(11) 0.04902(11) 0.0738(2) -0.0157(2) 0.0070(2) -0.00317(11)
Fe 0.0460(3) 0.0449(3) 0.0333(2) -0.0007(2) 0.0044(3) 0.0033(2)
S10 0.0706(6) 0.0381(5) 0.0557(6) -0.0040(4) -0.0051(5) -0.0029(4)
S4 0.0366(5) 0.0636(6) 0.0547(6) -0.0102(5) -0.0040(4) 0.0043(4)
O7 0.0483(12) 0.0514(12) 0.0515(14) 0.004(2) 0.005(2) -0.0069(10)
N1 0.0343(14) 0.0335(14) 0.0329(15) -0.0011(11) 0.0005(12) -0.0031(11)
C12 0.036(2) 0.046(2) 0.038(2) 0.000(2) -0.006(2) -0.0011(15)
C11 0.044(2) 0.051(2) 0.044(2) 0.003(2) -0.006(2) 0.007(2)
C9 0.078(3) 0.048(2) 0.045(2) 0.004(2) -0.008(2) -0.001(2)
C8 0.079(3) 0.053(2) 0.047(2) 0.006(2) 0.009(2) -0.019(2)
C6 0.047(2) 0.077(3) 0.050(3) -0.002(2) 0.013(2) -0.011(2)
C5 0.044(2) 0.068(2) 0.051(3) -0.013(2) 0.009(2) 0.001(2)
C3 0.050(2) 0.044(2) 0.050(2) -0.006(2) 0.006(2) 0.007(2)
C2 0.038(2) 0.038(2) 0.039(2) -0.007(2) 0.007(2) -0.0054(14)
C13 0.035(2) 0.035(2) 0.037(2) -0.004(2) -0.0031(15) -0.0016(15)
C14 0.038(2) 0.034(2) 0.031(2) -0.0023(14) 0.0014(15) 0.0009(15)
C15 0.038(2) 0.045(2) 0.041(2) -0.004(2) -0.002(2) 0.0049(14)
C16 0.043(2) 0.061(2) 0.045(2) -0.007(2) 0.007(2) -0.004(2)
C17 0.067(2) 0.039(2) 0.054(3) -0.003(2) 0.010(2) -0.010(2)
C18 0.055(2) 0.033(2) 0.046(2) -0.0033(15) 0.012(2) 0.003(2)
C19A 0.081(7) 0.088(8) 0.032(4) -0.014(5) 0.009(4) 0.030(6)
C20A 0.096(9) 0.069(6) 0.042(5) -0.016(4) -0.021(6) -0.014(6)
C19B 0.034(5) 0.096(16) 0.039(8) -0.026(8) -0.024(6) 0.052(9)
C22A 0.084(9) 0.096(11) 0.054(7) -0.013(6) -0.041(6) 0.047(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
Fe C19B 1.96(2) . ?
Fe C14 2.005(4) . ?
Fe C21A 2.011(9) . ?
Fe C18 2.018(4) . ?
Fe C17 2.019(4) . ?
Fe C15 2.019(4) . ?
Fe C21B 2.03(2) . ?
Fe C16 2.034(4) . ?
Fe C22B 2.056(15) . ?
Fe C19A 2.061(7) . ?
Fe C20A 2.062(8) . ?
Fe C23A 2.071(10) . ?
S10 C11 1.801(4) . ?
S10 C9 1.817(5) . ?
S4 C3 1.802(4) . ?
S4 C5 1.815(4) . ?
O7 C8 1.410(4) . ?
O7 C6 1.426(4) . ?
N1 C2 1.490(4) . ?
N1 C12 1.505(4) . ?
N1 C13 1.522(5) . ?
C12 C11 1.515(5) . ?
C9 C8 1.504(6) . ?
C6 C5 1.492(5) . ?
C3 C2 1.503(5) . ?
C13 C14 1.478(5) . ?
C14 C15 1.421(5) . ?
C14 C18 1.444(5) . ?
C15 C16 1.416(5) . ?
C16 C17 1.413(5) . ?
C17 C18 1.407(5) . ?
C19A C22B 0.639(13) . ?
C19A C21B 0.819(15) . ?
C19A C20A 1.42(2) . ?
C19A C23A 1.444(13) . ?
C19A C23B 1.83(2) . ?
C19A C20B 2.03(2) . ?
C20A C21B 0.668(14) . ?
C20A C20B 0.839(14) . ?
C20A C21A 1.37(2) . ?
C20A C22B 1.91(2) . ?
C20A C19B 1.94(2) . ?
C19B C22A 0.61(2) . ?
C19B C21A 0.85(2) . ?
C19B C23B 1.43(3) . ?
C19B C20B 1.44(2) . ?
C19B C23A 1.79(2) . ?
C22A C23B 1.02(2) . ?
C22A C21A 1.44(2) . ?
C22A C23A 1.50(2) . ?
C22A C20B 1.99(2) . ?
C22B C23A 0.896(14) . ?
C22B C23B 1.37(2) . ?
C22B C21B 1.40(2) . ?
C21B C20B 1.44(2) . ?
C21B C21A 1.84(2) . ?
C21B C23A 2.03(2) . ?
C21A C20B 0.651(14) . ?
C23B C23A 0.54(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C19B Fe C14 116.5(6) . . ?
C19B Fe C21A 24.6(5) . . ?
C14 Fe C21A 108.3(3) . . ?
C19B Fe C18 112.4(5) . . ?
C14 Fe C18 42.08(14) . . ?
C21A Fe C18 123.5(4) . . ?
C19B Fe C17 136.1(6) . . ?
C14 Fe C17 69.6(2) . . ?
C21A Fe C17 158.8(5) . . ?
C18 Fe C17 40.79(14) . . ?
C19B Fe C15 146.0(8) . . ?
C14 Fe C15 41.36(15) . . ?
C21A Fe C15 124.3(4) . . ?
C18 Fe C15 69.72(15) . . ?
C17 Fe C15 68.88(15) . . ?
C19B Fe C21B 67.0(6) . . ?
C14 Fe C21B 133.9(5) . . ?
C21A Fe C21B 54.2(5) . . ?
C18 Fe C21B 175.6(6) . . ?
C17 Fe C21B 142.6(5) . . ?
C15 Fe C21B 108.2(5) . . ?
C19B Fe C16 173.0(7) . . ?
C14 Fe C16 69.5(2) . . ?
C21A Fe C16 159.8(5) . . ?
C18 Fe C16 69.17(15) . . ?
C17 Fe C16 40.82(15) . . ?
C15 Fe C16 40.88(14) . . ?
C21B Fe C16 112.0(4) . . ?
C19B Fe C22B 67.0(7) . . ?
C14 Fe C22B 172.7(5) . . ?
C21A Fe C22B 72.0(5) . . ?
C18 Fe C22B 144.0(5) . . ?
C17 Fe C22B 112.9(4) . . ?
C15 Fe C22B 132.2(5) . . ?
C21B Fe C22B 40.1(5) . . ?
C16 Fe C22B 107.6(5) . . ?
C19B Fe C19A 69.5(6) . . ?
C14 Fe C19A 155.3(5) . . ?
C21A Fe C19A 66.4(4) . . ?
C18 Fe C19A 161.3(5) . . ?
C17 Fe C19A 124.4(5) . . ?
C15 Fe C19A 119.9(3) . . ?
C21B Fe C19A 23.1(4) . . ?
C16 Fe C19A 106.7(3) . . ?
C22B Fe C19A 17.9(4) . . ?
C19B Fe C20A 57.8(5) . . ?
C14 Fe C20A 120.2(4) . . ?
C21A Fe C20A 39.2(4) . . ?
C18 Fe C20A 157.3(5) . . ?
C17 Fe C20A 160.4(5) . . ?
C15 Fe C20A 106.3(3) . . ?
C21B Fe C20A 18.8(4) . . ?
C16 Fe C20A 123.3(4) . . ?
C22B Fe C20A 55.2(5) . . ?
C19A Fe C20A 40.2(5) . . ?
C19B Fe C23A 52.8(7) . . ?
C14 Fe C23A 162.1(4) . . ?
C21A Fe C23A 67.8(4) . . ?
C18 Fe C23A 124.2(4) . . ?
C17 Fe C23A 107.4(3) . . ?
C15 Fe C23A 155.5(4) . . ?
C21B Fe C23A 59.2(5) . . ?
C16 Fe C23A 120.4(3) . . ?
C22B Fe C23A 25.1(4) . . ?
C19A Fe C23A 40.9(4) . . ?
C20A Fe C23A 68.7(4) . . ?
C11 S10 C9 102.2(2) . . ?
C3 S4 C5 101.6(2) . . ?
C8 O7 C6 110.2(3) . . ?
C2 N1 C12 109.2(3) . . ?
C2 N1 C13 113.4(3) . . ?
C12 N1 C13 112.8(3) . . ?
N1 C12 C11 112.8(3) . . ?
C12 C11 S10 116.1(3) . . ?
C8 C9 S10 112.6(3) . . ?
O7 C8 C9 110.8(3) . . ?
O7 C6 C5 110.8(3) . . ?
C6 C5 S4 112.2(3) . . ?
C2 C3 S4 114.8(2) . . ?
N1 C2 C3 113.9(3) . . ?
C14 C13 N1 114.1(3) . . ?
C15 C14 C18 107.3(3) . . ?
C15 C14 C13 125.4(3) . . ?
C18 C14 C13 127.2(3) . . ?
C15 C14 Fe 69.9(2) . . ?
C18 C14 Fe 69.5(2) . . ?
C13 C14 Fe 124.0(3) . . ?
C16 C15 C14 108.5(3) . . ?
C16 C15 Fe 70.1(2) . . ?
C14 C15 Fe 68.8(2) . . ?
C17 C16 C15 107.7(3) . . ?
C17 C16 Fe 69.0(2) . . ?
C15 C16 Fe 69.0(2) . . ?
C18 C17 C16 109.3(3) . . ?
C18 C17 Fe 69.6(2) . . ?
C16 C17 Fe 70.2(2) . . ?
C17 C18 C14 107.2(3) . . ?
C17 C18 Fe 69.6(2) . . ?
C14 C18 Fe 68.5(2) . . ?
C22B C19A C21B 148.2(26) . . ?
C22B C19A C20A 132.7(21) . . ?
C21B C19A C20A 16.0(13) . . ?
C22B C19A C23A 23.8(17) . . ?
C21B C19A C23A 125.0(16) . . ?
C20A C19A C23A 109.2(8) . . ?
C22B C19A C23B 37.0(18) . . ?
C21B C19A C23B 112.0(16) . . ?
C20A C19A C23B 96.1(8) . . ?
C23A C19A C23B 13.2(7) . . ?
C22B C19A C20B 113.4(21) . . ?
C21B C19A C20B 35.2(13) . . ?
C20A C19A C20B 19.3(6) . . ?
C23A C19A C20B 89.9(7) . . ?
C23B C19A C20B 76.8(7) . . ?
C22B C19A Fe 80.6(17) . . ?
C21B C19A Fe 76.6(13) . . ?
C20A C19A Fe 69.9(5) . . ?
C23A C19A Fe 69.9(5) . . ?
C23B C19A Fe 65.2(5) . . ?
C20B C19A Fe 61.3(5) . . ?
C21B C20A C20B 146.3(26) . . ?
C21B C20A C21A 125.9(21) . . ?
C20B C20A C21A 20.3(11) . . ?
C21B C20A C19A 19.8(16) . . ?
C20B C20A C19A 126.8(15) . . ?
C21A C20A C19A 106.4(8) . . ?
C21B C20A C22B 33.8(17) . . ?
C20B C20A C22B 112.6(15) . . ?
C21A C20A C22B 92.2(8) . . ?
C19A C20A C22B 14.3(6) . . ?
C21B C20A C19B 103.9(20) . . ?
C20B C20A C19B 42.4(13) . . ?
C21A C20A C19B 22.0(7) . . ?
C19A C20A C19B 84.4(9) . . ?
C22B C20A C19B 70.2(9) . . ?
C21B C20A Fe 78.2(18) . . ?
C20B C20A Fe 79.9(12) . . ?
C21A C20A Fe 68.4(5) . . ?
C19A C20A Fe 69.9(5) . . ?
C22B C20A Fe 62.2(5) . . ?
C19B C20A Fe 58.4(6) . . ?
C22A C19B C21A 161.2(39) . . ?
C22A C19B C23B 38.2(30) . . ?
C21A C19B C23B 128.0(16) . . ?
C22A C19B C20B 149.4(36) . . ?
C21A C19B C20B 14.1(10) . . ?
C23B C19B C20B 113.9(12) . . ?
C22A C19B C23A 52.3(30) . . ?
C21A C19B C23A 114.2(15) . . ?
C23B C19B C23A 14.1(7) . . ?
C20B C19B C23A 100.1(11) . . ?
C22A C19B C20A 127.7(34) . . ?
C21A C19B C20A 37.2(10) . . ?
C23B C19B C20A 90.9(10) . . ?
C20B C19B C20A 23.1(6) . . ?
C23A C19B C20A 77.0(8) . . ?
C22A C19B Fe 101.5(36) . . ?
C21A C19B Fe 81.4(11) . . ?
C23B C19B Fe 75.1(10) . . ?
C20B C19B Fe 74.0(8) . . ?
C23A C19B Fe 66.9(8) . . ?
C20A C19B Fe 63.8(5) . . ?
C19B C22A C23B 120.1(37) . . ?
C19B C22A C21A 11.0(22) . . ?
C23B C22A C21A 112.8(16) . . ?
C19B C22A C23A 109.0(30) . . ?
C23B C22A C23A 11.2(12) . . ?
C21A C22A C23A 101.6(10) . . ?
C19B C22A C20B 21.7(25) . . ?
C23B C22A C20B 101.1(15) . . ?
C21A C22A C20B 11.8(6) . . ?
C23A C22A C20B 90.0(8) . . ?
C19B C22A Fe 62.5(29) . . ?
C23B C22A Fe 73.1(13) . . ?
C21A C22A Fe 64.3(6) . . ?
C23A C22A Fe 66.0(6) . . ?
C20B C22A Fe 60.2(5) . . ?
C19A C22B C23A 139.5(28) . . ?
C19A C22B C23B 126.8(23) . . ?
C23A C22B C23B 12.7(12) . . ?
C19A C22B C21B 17.9(16) . . ?
C23A C22B C21B 122.1(17) . . ?
C23B C22B C21B 109.4(13) . . ?
C19A C22B C20A 33.0(16) . . ?
C23A C22B C20A 106.8(15) . . ?
C23B C22B C20A 94.1(10) . . ?
C21B C22B C20A 15.4(7) . . ?
C19A C22B Fe 81.6(17) . . ?
C23A C22B Fe 78.4(13) . . ?
C23B C22B Fe 72.7(9) . . ?
C21B C22B Fe 69.1(9) . . ?
C20A C22B Fe 62.5(5) . . ?
C20A C21B C19A 144.2(29) . . ?
C20A C21B C22B 130.8(24) . . ?
C19A C21B C22B 13.9(11) . . ?
C20A C21B C20B 18.8(15) . . ?
C19A C21B C20B 125.6(18) . . ?
C22B C21B C20B 112.1(13) . . ?
C20A C21B C21A 37.0(16) . . ?
C19A C21B C21A 107.6(16) . . ?
C22B C21B C21A 93.9(11) . . ?
C20B C21B C21A 18.2(6) . . ?
C20A C21B C23A 108.8(20) . . ?
C19A C21B C23A 35.7(11) . . ?
C22B C21B C23A 22.0(7) . . ?
C20B C21B C23A 90.1(10) . . ?
C21A C21B C23A 71.9(7) . . ?
C20A C21B Fe 83.0(18) . . ?
C19A C21B Fe 80.4(13) . . ?
C22B C21B Fe 70.8(10) . . ?
C20B C21B Fe 71.5(9) . . ?
C21A C21B Fe 62.3(6) . . ?
C23A C21B Fe 61.3(5) . . ?
C20B C21A C19B 147.4(24) . . ?
C20B C21A C20A 26.6(15) . . ?
C19B C21A C20A 120.7(16) . . ?
C20B C21A C22A 141.3(22) . . ?
C19B C21A C22A 7.8(17) . . ?
C20A C21A C22A 114.9(12) . . ?
C20B C21A C21B 43.7(16) . . ?
C19B C21A C21B 103.7(15) . . ?
C20A C21A C21B 17.1(6) . . ?
C22A C21A C21B 97.9(11) . . ?
C20B C21A Fe 87.4(17) . . ?
C19B C21A Fe 74.0(13) . . ?
C20A C21A Fe 72.4(5) . . ?
C22A C21A Fe 75.6(8) . . ?
C21B C21A Fe 63.5(6) . . ?
C21A C20B C20A 133.0(25) . . ?
C21A C20B C19B 18.5(14) . . ?
C20A C20B C19B 114.5(17) . . ?
C21A C20B C21B 118.1(20) . . ?
C20A C20B C21B 14.9(11) . . ?
C19B C20B C21B 99.6(13) . . ?
C21A C20B C22A 26.9(16) . . ?
C20A C20B C22A 106.4(14) . . ?
C19B C20B C22A 9.0(12) . . ?
C21B C20B C22A 91.6(10) . . ?
C21A C20B C19A 99.1(18) . . ?
C20A C20B C19A 33.9(10) . . ?
C19B C20B C19A 80.6(11) . . ?
C21B C20B C19A 19.1(7) . . ?
C22A C20B C19A 72.5(7) . . ?
C21A C20B Fe 74.4(16) . . ?
C20A C20B Fe 76.7(11) . . ?
C19B C20B Fe 64.4(9) . . ?
C21B C20B Fe 67.6(9) . . ?
C22A C20B Fe 64.0(6) . . ?
C19A C20B Fe 60.1(4) . . ?
C23A C23B C22A 147.1(33) . . ?
C23A C23B C22B 21.6(20) . . ?
C22A C23B C22B 125.7(17) . . ?
C23A C23B C19B 125.6(28) . . ?
C22A C23B C19B 21.6(9) . . ?
C22B C23B C19B 104.5(12) . . ?
C23A C23B C19A 37.8(21) . . ?
C22A C23B C19A 109.6(15) . . ?
C22B C23B C19A 16.3(7) . . ?
C19B C23B C19A 88.5(10) . . ?
C23A C23B Fe 79.0(23) . . ?
C22A C23B Fe 79.2(11) . . ?
C22B C23B Fe 68.8(8) . . ?
C19B C23B Fe 63.9(8) . . ?
C19A C23B Fe 62.7(5) . . ?
C23B C23A C22B 145.7(31) . . ?
C23B C23A C19A 129.0(26) . . ?
C22B C23A C19A 16.7(12) . . ?
C23B C23A C22A 21.7(22) . . ?
C22B C23A C22A 124.2(15) . . ?
C19A C23A C22A 107.5(9) . . ?
C23B C23A C19B 40.3(22) . . ?
C22B C23A C19B 105.9(14) . . ?
C19A C23A C19B 89.4(8) . . ?
C22A C23A C19B 18.7(5) . . ?
C23B C23A C21B 109.9(25) . . ?
C22B C23A C21B 35.9(11) . . ?
C19A C23A C21B 19.3(6) . . ?
C22A C23A C21B 88.3(8) . . ?
C19B C23A C21B 70.1(7) . . ?
C23B C23A Fe 86.2(23) . . ?
C22B C23A Fe 76.5(12) . . ?
C19A C23A Fe 69.2(5) . . ?
C22A C23A Fe 72.5(6) . . ?
C19B C23A Fe 60.3(6) . . ?
C21B C23A Fe 59.5(5) . . ?

_refine_diff_density_max         0.483
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.057

data_da144
_database_code_CSD               196828

_audit_creation_method           SHELXL
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_structural     ?
_chemical_formula_analytical     'C8 H17 Cu N O S2 2+, 2 (NO3 1-)'
_chemical_formula_sum            'C8 H17 Cu N3 O7 S2'
_chemical_formula_weight         394.91
_chemical_melting_point          ?
_chemical_compound_source        ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_symmetry_cell_setting           'monoclinic unique axis b'
_symmetry_space_group_name_H-M   ' P21/c'
_symmetry_Int_Tables_number      14

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                   14.7630(10)
_cell_length_b                   14.9520(10)
_cell_length_c                   14.7470(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 111.320(10)
_cell_angle_gamma                90.00
_cell_volume                     3032.4(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1024
_cell_measurement_theta_min      2.7
_cell_measurement_theta_max      24.9

_exptl_crystal_description       prism
_exptl_crystal_colour            Blue
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.730
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1624
_exptl_absorpt_coefficient_mu    1.750
_exptl_absorpt_correction_type   SADABS
_exptl_absorpt_correction_T_min  0.814
_exptl_absorpt_correction_T_max  1.000

_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       'SMART CCD diffractometer'
_diffrn_measurement_method       'omega scan'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            26392
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_av_sigmaI/netI    0.1217
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.48
_diffrn_reflns_theta_max         25.01
_reflns_number_total             5339
_reflns_number_observed          3655
_reflns_observed_criterion       >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^
or flagged by the user for potential systematic errors.  Weighted R-factors
wR and all goodnesses 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 observed criterion
of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0421P)^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    ?
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5339
_refine_ls_number_parameters     440
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_obs          0.0356
_refine_ls_wR_factor_all         0.0888
_refine_ls_wR_factor_obs         0.0870
_refine_ls_goodness_of_fit_all   0.893
_refine_ls_goodness_of_fit_obs   1.078
_refine_ls_restrained_S_all      0.910
_refine_ls_restrained_S_obs      1.100
_refine_ls_shift/esd_max         0.040
_refine_ls_shift/esd_mean        0.002

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
CuA Cu 0.28545(3) 0.78290(3) 0.02627(3) 0.04466(13) Uani 1 d . .
CuB Cu 0.23749(3) 0.20772(3) 0.43556(3) 0.04368(13) Uani 1 d . .
S4A S 0.25695(8) 0.70786(7) -0.12126(8) 0.0634(3) Uani 1 d . .
S4B S 0.18811(9) 0.10557(8) 0.29699(7) 0.0699(3) Uani 1 d . .
S10A S 0.26786(9) 0.89545(7) 0.13525(8) 0.0686(3) Uani 1 d . .
S10B S 0.26213(8) 0.26030(8) 0.59380(8) 0.0686(3) Uani 1 d . .
O7A O 0.1357(2) 0.8584(2) -0.0768(2) 0.0671(8) Uani 1 d . .
O7B O 0.1394(2) 0.1021(2) 0.4818(2) 0.0571(7) Uani 1 d . .
O21 O 0.4160(2) 0.7363(2) 0.1517(2) 0.0679(8) Uani 1 d . .
O22 O 0.4618(2) 0.6607(2) 0.0526(2) 0.0795(9) Uani 1 d . .
O23 O 0.5031(2) 0.6183(2) 0.2022(2) 0.0973(11) Uani 1 d . .
O31A O 0.2092(6) 0.7158(5) 0.0840(6) 0.048(2) Uani 0.50 d PD .
O32A O 0.1963(10) 0.5829(11) 0.1371(11) 0.162(8) Uani 0.50 d PD .
O33A O 0.1523(8) 0.6101(6) -0.0069(7) 0.153(4) Uani 0.50 d PD .
O31B O 0.1896(10) 0.6982(9) 0.0622(10) 0.165(7) Uani 0.50 d PD .
O32B O 0.1506(7) 0.5905(7) 0.1190(9) 0.085(4) Uani 0.50 d PD .
O33B O 0.2734(5) 0.5878(4) 0.0779(6) 0.087(2) Uani 0.50 d PD .
O41 O 0.1138(2) 0.2703(2) 0.3672(2) 0.0840(10) Uani 1 d . .
O42 O 0.1782(3) 0.3975(3) 0.4027(4) 0.151(2) Uani 1 d . .
O43 O 0.0292(3) 0.3906(3) 0.3430(4) 0.147(2) Uani 1 d . .
O51 O 0.3155(2) 0.2820(2) 0.3513(2) 0.0658(8) Uani 1 d . .
O52 O 0.4182(2) 0.3296(2) 0.4889(2) 0.0664(8) Uani 1 d . .
O53 O 0.4105(2) 0.3930(2) 0.3567(2) 0.0811(9) Uani 1 d . .
N1A N 0.3659(2) 0.8702(2) -0.0139(2) 0.0449(7) Uani 1 d . .
N1B N 0.3560(2) 0.1317(2) 0.4942(2) 0.0461(7) Uani 1 d . .
N2 N 0.4604(2) 0.6704(2) 0.1355(2) 0.0560(8) Uani 1 d . .
N4 N 0.1019(3) 0.3526(3) 0.3698(3) 0.0838(13) Uani 1 d . .
N3 N 0.1948(3) 0.6316(3) 0.0826(3) 0.0705(11) Uani 1 d D .
N5 N 0.3815(2) 0.3358(2) 0.3991(2) 0.0516(8) Uani 1 d . .
C5A C 0.1431(3) 0.7582(4) -0.1995(3) 0.0801(14) Uani 1 d . .
H5AA H 0.1572(3) 0.8073(4) -0.2353(3) 0.052(11) Uiso 1 calc R .
H5AB H 0.1057(3) 0.7141(4) -0.2464(3) 0.108(18) Uiso 1 calc R .
C5B C 0.1126(3) 0.0270(3) 0.3327(3) 0.0787(14) Uani 1 d . .
H5BA H 0.0625(3) 0.0037(3) 0.2746(3) 0.112(17) Uiso 1 calc R .
H5BB H 0.1525(3) -0.0230(3) 0.3668(3) 0.089(16) Uiso 1 calc R .
C6A C 0.0827(3) 0.7927(4) -0.1437(4) 0.0843(15) Uani 1 d . .
H6AA H 0.0227(3) 0.8182(4) -0.1885(4) 0.094(15) Uiso 1 calc R .
H6AB H 0.0663(3) 0.7438(4) -0.1093(4) 0.084(15) Uiso 1 calc R .
C6B C 0.0657(3) 0.0688(3) 0.3966(3) 0.0723(12) Uani 1 d . .
H6BA H 0.0234(3) 0.1172(3) 0.3623(3) 0.076(14) Uiso 1 calc R .
H6BB H 0.0267(3) 0.0247(3) 0.4142(3) 0.074(13) Uiso 1 calc R .
C8A C 0.0887(3) 0.8898(4) -0.0154(4) 0.0859(15) Uani 1 d . .
H8AA H 0.0703(3) 0.8397(4) 0.0160(4) 0.095(17) Uiso 1 calc R .
H8AB H 0.0301(3) 0.9220(4) -0.0533(4) 0.109(17) Uiso 1 calc R .
C8B C 0.1029(3) 0.1464(4) 0.5462(3) 0.0767(13) Uani 1 d . .
H8BA H 0.0649(3) 0.1051(4) 0.5687(3) 0.117(18) Uiso 1 calc R .
H8BB H 0.0610(3) 0.1955(4) 0.5128(3) 0.104(19) Uiso 1 calc R .
C9A C 0.1556(4) 0.9501(3) 0.0595(4) 0.091(2) Uani 1 d . .
H9AA H 0.1224(4) 0.9724(3) 0.1008(4) 0.101(16) Uiso 1 calc R .
H9AB H 0.1714(4) 1.0009(3) 0.0272(4) 0.077(14) Uiso 1 calc R .
C9B C 0.1870(4) 0.1817(4) 0.6316(3) 0.086(2) Uani 1 d . .
H9BA H 0.2271(4) 0.1320(4) 0.6659(3) 0.100(20) Uiso 1 calc R .
H9BB H 0.1623(4) 0.2116(4) 0.6762(3) 0.097(16) Uiso 1 calc R .
C11A C 0.3610(4) 0.9658(3) 0.1199(3) 0.0762(13) Uani 1 d . .
H11A H 0.3511(4) 1.0270(3) 0.1362(3) 0.079(13) Uiso 1 calc R .
H11A' H 0.4242(4) 0.9465(3) 0.1645(3) 0.128(22) Uiso 1 calc R .
C11B C 0.3803(3) 0.2106(3) 0.6482(3) 0.0703(13) Uani 1 d . .
H11B H 0.4288(3) 0.2515(3) 0.6422(3) 0.090(15) Uiso 1 calc R .
H11B' H 0.3940(3) 0.2009(3) 0.7169(3) 0.060(11) Uiso 1 calc R .
C12A C 0.3598(3) 0.9628(2) 0.0176(3) 0.0623(11) Uani 1 d . .
H12A H 0.3004(3) 0.9902(2) -0.0261(3) 0.058(11) Uiso 1 calc R .
H12A' H 0.4143(3) 0.9970(2) 0.0140(3) 0.063(11) Uiso 1 calc R .
C12B C 0.3874(3) 0.1229(3) 0.6009(3) 0.0691(12) Uani 1 d . .
H12B H 0.4541(3) 0.1018(3) 0.6270(3) 0.084(14) Uiso 1 calc R .
H12B' H 0.3470(3) 0.0788(3) 0.6165(3) 0.054(11) Uiso 1 calc R .
C2A C 0.3500(3) 0.8672(3) -0.1195(2) 0.0577(10) Uani 1 d . .
H2AA H 0.4030(3) 0.8974(3) -0.1309(2) 0.057(11) Uiso 1 calc R .
H2AB H 0.2900(3) 0.8978(3) -0.1564(2) 0.059(11) Uiso 1 calc R .
C2B C 0.3469(3) 0.0433(3) 0.4477(3) 0.0735(13) Uani 1 d . .
H2BA H 0.3061(3) 0.0051(3) 0.4700(3) 0.063(12) Uiso 1 calc R .
H2BB H 0.4106(3) 0.0158(3) 0.4666(3) 0.104(16) Uiso 1 calc R .
C3A C 0.3447(3) 0.7719(3) -0.1526(3) 0.0656(12) Uani 1 d . .
H3AA H 0.4082(3) 0.7445(3) -0.1231(3) 0.049(10) Uiso 1 calc R .
H3AB H 0.3274(3) 0.7707(3) -0.2226(3) 0.081(13) Uiso 1 calc R .
C3B C 0.3039(3) 0.0507(3) 0.3399(3) 0.0795(14) Uani 1 d . .
H3BA H 0.2966(3) -0.0087(3) 0.3119(3) 0.082(13) Uiso 1 calc R .
H3BB H 0.3484(3) 0.0837(3) 0.3175(3) 0.082(14) Uiso 1 calc R .
HN1B H 0.4062(3) 0.1720(3) 0.4791(3) 0.052(10) Uiso 1 d R .
HN1A H 0.4257(3) 0.8530(3) 0.0217(3) 0.054(11) Uiso 1 d 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
CuA 0.0468(3) 0.0438(2) 0.0441(2) 0.0038(2) 0.0175(2) -0.0005(2)
CuB 0.0415(2) 0.0429(2) 0.0417(2) -0.0004(2) 0.0092(2) 0.0006(2)
S4A 0.0658(7) 0.0624(6) 0.0604(6) -0.0160(5) 0.0212(5) -0.0073(5)
S4B 0.0837(8) 0.0722(7) 0.0508(6) -0.0130(5) 0.0211(6) -0.0251(6)
S10A 0.0986(9) 0.0613(7) 0.0573(6) 0.0020(5) 0.0418(6) 0.0143(6)
S10B 0.0692(7) 0.0791(8) 0.0642(7) -0.0274(6) 0.0322(6) -0.0161(6)
O7A 0.055(2) 0.081(2) 0.067(2) 0.010(2) 0.0242(15) 0.014(2)
O7B 0.049(2) 0.063(2) 0.059(2) -0.0046(13) 0.0195(13) -0.0083(13)
O21 0.076(2) 0.067(2) 0.054(2) 0.0034(14) 0.0154(15) 0.023(2)
O22 0.066(2) 0.108(3) 0.068(2) -0.003(2) 0.029(2) 0.011(2)
O23 0.088(2) 0.091(2) 0.101(3) 0.045(2) 0.020(2) 0.032(2)
O31A 0.073(5) 0.032(3) 0.068(4) -0.017(3) 0.061(4) -0.020(3)
O32A 0.244(19) 0.109(9) 0.087(7) 0.025(6) 0.007(10) 0.014(11)
O33A 0.211(11) 0.142(8) 0.134(8) -0.041(7) 0.097(8) -0.050(8)
O31B 0.125(9) 0.084(8) 0.204(13) 0.059(9) -0.038(7) -0.052(7)
O32B 0.095(6) 0.052(4) 0.158(11) 0.024(5) 0.106(8) -0.017(4)
O33B 0.082(5) 0.056(4) 0.157(7) -0.011(4) 0.083(5) -0.001(3)
O41 0.059(2) 0.055(2) 0.110(3) 0.002(2) -0.003(2) 0.0027(15)
O42 0.113(4) 0.087(3) 0.228(5) -0.034(3) 0.031(3) -0.005(3)
O43 0.079(3) 0.088(3) 0.228(5) 0.025(3) -0.001(3) 0.026(2)
O51 0.069(2) 0.076(2) 0.0450(15) 0.0024(14) 0.0121(13) -0.024(2)
O52 0.074(2) 0.059(2) 0.053(2) -0.0009(14) 0.0068(14) -0.0064(15)
O53 0.114(3) 0.068(2) 0.080(2) -0.007(2) 0.057(2) -0.029(2)
N1A 0.044(2) 0.044(2) 0.044(2) 0.0047(14) 0.0132(14) 0.0007(14)
N1B 0.044(2) 0.049(2) 0.046(2) 0.0045(14) 0.0163(14) 0.0034(14)
N2 0.044(2) 0.061(2) 0.059(2) 0.011(2) 0.015(2) 0.000(2)
N4 0.046(2) 0.046(2) 0.137(4) 0.002(2) 0.006(2) 0.001(2)
N3 0.097(3) 0.064(3) 0.058(3) -0.006(2) 0.039(3) -0.011(3)
N5 0.058(2) 0.044(2) 0.058(2) -0.001(2) 0.028(2) 0.001(2)
C5A 0.066(3) 0.109(4) 0.051(2) -0.006(3) 0.004(2) -0.013(3)
C5B 0.080(3) 0.074(3) 0.078(3) -0.019(3) 0.023(3) -0.035(3)
C6A 0.046(3) 0.115(4) 0.078(3) 0.018(3) 0.006(2) 0.008(3)
C6B 0.057(3) 0.069(3) 0.084(3) -0.007(3) 0.018(3) -0.023(3)
C8A 0.066(3) 0.105(4) 0.096(4) 0.024(3) 0.040(3) 0.037(3)
C8B 0.064(3) 0.092(3) 0.088(3) -0.012(3) 0.044(3) -0.018(3)
C9A 0.111(4) 0.083(4) 0.102(4) 0.019(3) 0.067(4) 0.045(3)
C9B 0.077(3) 0.127(5) 0.070(3) -0.028(3) 0.047(3) -0.031(3)
C11A 0.101(4) 0.050(3) 0.078(3) -0.017(2) 0.032(3) -0.005(3)
C11B 0.063(3) 0.108(4) 0.034(2) -0.001(2) 0.010(2) -0.026(3)
C12A 0.077(3) 0.041(2) 0.073(3) 0.008(2) 0.032(2) -0.002(2)
C12B 0.053(3) 0.090(3) 0.058(3) 0.029(2) 0.013(2) 0.009(2)
C2A 0.056(3) 0.077(3) 0.042(2) 0.014(2) 0.020(2) -0.004(2)
C2B 0.064(3) 0.049(2) 0.113(4) 0.001(3) 0.039(3) 0.011(2)
C3A 0.065(3) 0.090(3) 0.045(2) -0.008(2) 0.025(2) 0.003(2)
C3B 0.099(4) 0.070(3) 0.085(3) -0.034(3) 0.053(3) -0.014(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
CuA O31A 1.922(6) . ?
CuA N1A 1.995(3) . ?
CuA O31B 2.106(13) . ?
CuA O21 2.242(3) . ?
CuA S4A 2.3459(11) . ?
CuA S10A 2.4054(11) . ?
CuB O41 1.972(3) . ?
CuB N1B 2.000(3) . ?
CuB O51 2.268(3) . ?
CuB S10B 2.3620(11) . ?
CuB O7B 2.402(2) . ?
CuB S4B 2.4406(11) . ?
S4A C3A 1.801(4) . ?
S4A C5A 1.820(5) . ?
S4B C3B 1.791(5) . ?
S4B C5B 1.824(4) . ?
S10A C11A 1.810(5) . ?
S10A C9A 1.821(5) . ?
S10B C11B 1.794(4) . ?
S10B C9B 1.836(4) . ?
O7A C8A 1.407(5) . ?
O7A C6A 1.412(5) . ?
O7B C8B 1.417(5) . ?
O7B C6B 1.420(4) . ?
O21 N2 1.254(4) . ?
O22 N2 1.238(4) . ?
O23 N2 1.233(4) . ?
O31A N3 1.276(9) . ?
O32A O32B 0.64(2) . ?
O32A N3 1.077(14) . ?
O32A O33B 1.669(15) . ?
O33A N3 1.280(10) . ?
O33A O31B 1.633(14) . ?
O33A O33B 1.802(13) . ?
O31B N3 1.035(13) . ?
O32B N3 1.159(9) . ?
O33B N3 1.356(6) . ?
O41 N4 1.246(4) . ?
O42 N4 1.247(5) . ?
O43 N4 1.150(5) . ?
O51 N5 1.263(4) . ?
O52 N5 1.239(4) . ?
O53 N5 1.225(4) . ?
N1A C12A 1.473(4) . ?
N1A C2A 1.488(4) . ?
N1B C2B 1.473(5) . ?
N1B C12B 1.476(4) . ?
C5A C6A 1.506(6) . ?
C5B C6B 1.495(6) . ?
C8A C9A 1.488(7) . ?
C8B C9B 1.506(6) . ?
C11A C12A 1.504(5) . ?
C11B C12B 1.507(6) . ?
C2A C3A 1.498(5) . ?
C2B C3B 1.485(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O31A CuA N1A 168.9(2) . . ?
O31A CuA O31B 11.2(5) . . ?
N1A CuA O31B 174.8(4) . . ?
O31A CuA O21 86.5(3) . . ?
N1A CuA O21 91.28(11) . . ?
O31B CuA O21 93.4(4) . . ?
O31A CuA S4A 103.0(2) . . ?
N1A CuA S4A 87.86(8) . . ?
O31B CuA S4A 92.0(4) . . ?
O21 CuA S4A 115.27(8) . . ?
O31A CuA S10A 81.2(2) . . ?
N1A CuA S10A 87.78(9) . . ?
O31B CuA S10A 90.4(4) . . ?
O21 CuA S10A 86.30(8) . . ?
S4A CuA S10A 158.08(4) . . ?
O41 CuB N1B 173.05(12) . . ?
O41 CuB O51 92.75(12) . . ?
N1B CuB O51 88.70(11) . . ?
O41 CuB S10B 97.37(10) . . ?
N1B CuB S10B 88.02(9) . . ?
O51 CuB S10B 116.84(7) . . ?
O41 CuB O7B 85.14(11) . . ?
N1B CuB O7B 91.49(10) . . ?
O51 CuB O7B 162.90(9) . . ?
S10B CuB O7B 80.25(7) . . ?
O41 CuB S4B 85.98(10) . . ?
N1B CuB S4B 87.39(9) . . ?
O51 CuB S4B 84.52(7) . . ?
S10B CuB S4B 158.03(4) . . ?
O7B CuB S4B 78.40(7) . . ?
C3A S4A C5A 101.7(2) . . ?
C3A S4A CuA 94.61(13) . . ?
C5A S4A CuA 101.7(2) . . ?
C3B S4B C5B 102.0(2) . . ?
C3B S4B CuB 91.96(14) . . ?
C5B S4B CuB 100.93(14) . . ?
C11A S10A C9A 103.1(3) . . ?
C11A S10A CuA 92.98(13) . . ?
C9A S10A CuA 101.5(2) . . ?
C11B S10B C9B 101.3(2) . . ?
C11B S10B CuB 94.54(13) . . ?
C9B S10B CuB 101.16(14) . . ?
C8A O7A C6A 113.9(4) . . ?
C8B O7B C6B 113.6(3) . . ?
C8B O7B CuB 107.4(2) . . ?
C6B O7B CuB 109.1(2) . . ?
N2 O21 CuA 116.1(2) . . ?
N3 O31A CuA 129.0(4) . . ?
O32B O32A N3 80.6(20) . . ?
O32B O32A O33B 126.2(24) . . ?
N3 O32A O33B 54.1(7) . . ?
N3 O33A O31B 39.3(5) . . ?
N3 O33A O33B 48.7(5) . . ?
O31B O33A O33B 72.0(7) . . ?
N3 O31B O33A 51.6(7) . . ?
N3 O31B CuA 131.8(12) . . ?
O33A O31B CuA 115.6(9) . . ?
O32A O32B N3 66.5(17) . . ?
N3 O33B O32A 40.1(5) . . ?
N3 O33B O33A 45.1(4) . . ?
O32A O33B O33A 71.2(6) . . ?
N4 O41 CuB 124.6(3) . . ?
N5 O51 CuB 116.7(2) . . ?
C12A N1A C2A 110.8(3) . . ?
C12A N1A CuA 114.2(2) . . ?
C2A N1A CuA 114.0(2) . . ?
C2B N1B C12B 110.9(3) . . ?
C2B N1B CuB 113.0(2) . . ?
C12B N1B CuB 113.5(2) . . ?
O23 N2 O22 121.7(4) . . ?
O23 N2 O21 119.7(4) . . ?
O22 N2 O21 118.5(3) . . ?
O43 N4 O41 127.0(4) . . ?
O43 N4 O42 117.7(4) . . ?
O41 N4 O42 115.2(4) . . ?
O31B N3 O32A 147.7(13) . . ?
O31B N3 O32B 130.5(11) . . ?
O32A N3 O32B 33.0(9) . . ?
O31B N3 O31A 18.1(9) . . ?
O32A N3 O31A 134.1(10) . . ?
O32B N3 O31A 129.4(7) . . ?
O31B N3 O33A 89.1(9) . . ?
O32A N3 O33A 118.0(11) . . ?
O32B N3 O33A 101.3(8) . . ?
O31A N3 O33A 106.2(6) . . ?
O31B N3 O33B 115.0(10) . . ?
O32A N3 O33B 85.8(8) . . ?
O32B N3 O33B 113.9(7) . . ?
O31A N3 O33B 109.6(5) . . ?
O33A N3 O33B 86.2(6) . . ?
O53 N5 O52 120.0(3) . . ?
O53 N5 O51 120.1(3) . . ?
O52 N5 O51 119.8(3) . . ?
C6A C5A S4A 112.9(3) . . ?
C6B C5B S4B 112.6(3) . . ?
O7A C6A C5A 109.4(4) . . ?
O7B C6B C5B 108.8(4) . . ?
O7A C8A C9A 109.2(4) . . ?
O7B C8B C9B 108.9(4) . . ?
C8A C9A S10A 113.2(3) . . ?
C8B C9B S10B 112.1(3) . . ?
C12A C11A S10A 112.1(3) . . ?
C12B C11B S10B 111.9(3) . . ?
N1A C12A C11A 111.4(3) . . ?
N1B C12B C11B 111.6(3) . . ?
N1A C2A C3A 109.9(3) . . ?
N1B C2B C3B 111.2(3) . . ?
C2A C3A S4A 112.3(3) . . ?
C2B C3B S4B 113.2(3) . . ?

_refine_diff_density_max         0.634
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.059