# Supplementary Material (ESI) for ChemComm
# This journal is © The Royal Society of Chemistry 2001
# CCDC Number: 182/1869
 
data_1    
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C44 H56 Cl8 Cu2 Fe2 N4 S8' 
_chemical_formula_weight         1419.78 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0033   0.0016 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'N'  'N'   0.0061   0.0033 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'   0.0106   0.0060 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 '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' 
 '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' 
 
_symmetry_cell_setting            triclinic
_symmetry_space_group_name_H-M    P-1
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, -y, -z' 
 
_cell_length_a                    10.751(12) 
_cell_length_b                    12.229(14) 
_cell_length_c                    12.598(14) 
_cell_angle_alpha                 95.657(10) 
_cell_angle_beta                  107.331(10) 
_cell_angle_gamma                 98.744(10) 
_cell_volume                      1544(3) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           ? 
_exptl_crystal_size_mid           ? 
_exptl_crystal_size_min           ? 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.526 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              722 
_exptl_absorpt_coefficient_mu     1.790 
_exptl_absorpt_correction_type    'DIFABS(Walker and Stuart, 1983)'
_exptl_absorpt_correction_T_min   0.536
_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        'Marresearch Image Plate'
_diffrn_measurement_method
  '95 frames at 2^o intervals, counting time 2 min.'
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             5535 
_diffrn_reflns_av_R_equivalents   0.0000 
_diffrn_reflns_av_sigmaI/netI     0.0442 
_diffrn_reflns_limit_h_min        0 
_diffrn_reflns_limit_h_max        13 
_diffrn_reflns_limit_k_min        -14 
_diffrn_reflns_limit_k_max        14 
_diffrn_reflns_limit_l_min        -15 
_diffrn_reflns_limit_l_max        14 
_diffrn_reflns_theta_min          1.70 
_diffrn_reflns_theta_max          26.00 
_reflns_number_total              5535 
_reflns_number_gt                 3563 
_reflns_threshold_expression      >2sigma(I) 
 
 
_computing_data_collection        'XDS (Kabsch, 1991)'
_computing_cell_refinement        XDS
_computing_data_reduction         XDS
_computing_structure_solution     'SHELXS-86 (Sheldrick, 1990)'
_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)'
_computing_molecular_graphics     'PLATON(Spek,1994)'

_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 w=1/[\s^2^(Fo^2^)+(0.1123P)^2^+0.4468P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          5535 
_refine_ls_number_parameters      309 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.1075 
_refine_ls_R_factor_gt            0.0578 
_refine_ls_wR_factor_ref          0.1841 
_refine_ls_wR_factor_gt           0.1590 
_refine_ls_goodness_of_fit_ref    1.054 
_refine_ls_restrained_S_all       1.054 
_refine_ls_shift/su_max           0.016 
_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_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Cu1 Cu 0.26545(6) 0.86973(5) 0.98381(6) 0.0570(2) Uani 1 d . . . 
S11 S 0.42535(14) 0.91307(11) 1.14885(12) 0.0598(4) Uani 1 d . . . 
S12 S 0.24749(14) 1.03977(12) 0.94163(12) 0.0606(4) Uani 1 d . . . 
S21 S 0.25886(15) 0.70569(12) 1.04603(13) 0.0624(4) Uani 1 d . . . 
S22 S 0.09350(14) 0.83143(12) 0.82677(13) 0.0618(4) Uani 1 d . . . 
C13 C 0.3770(5) 0.7761(4) 1.1663(4) 0.0473(11) Uani 1 d . . . 
N14 N 0.4248(4) 0.7349(3) 1.2590(4) 0.0491(10) Uani 1 d . . . 
C15 C 0.3694(6) 0.6186(5) 1.2688(5) 0.0605(14) Uani 1 d . . . 
H15A H 0.4375 0.5881 1.3201 0.073 Uiso 1 calc R . . 
H15B H 0.3419 0.5720 1.1958 0.073 Uiso 1 calc R . . 
C16 C 0.2501(6) 0.6168(5) 1.3123(5) 0.0684(16) Uani 1 d . . . 
H16A H 0.2768 0.6667 1.3833 0.082 Uiso 1 calc R . . 
H16B H 0.1806 0.6441 1.2590 0.082 Uiso 1 calc R . . 
C17 C 0.1964(7) 0.5011(6) 1.3287(6) 0.088(2) Uani 1 d . . . 
H17A H 0.1627 0.4530 1.2573 0.106 Uiso 1 calc R . . 
H17B H 0.1262 0.5040 1.3607 0.106 Uiso 1 calc R . . 
H17C H 0.2662 0.4724 1.3784 0.106 Uiso 1 calc R . . 
C23 C 0.1146(5) 0.9732(4) 0.8272(4) 0.0485(12) Uani 1 d . . . 
N24 N 0.0418(4) 1.0242(3) 0.7513(3) 0.0483(10) Uani 1 d . . . 
C25 C -0.0683(5) 0.9613(5) 0.6509(5) 0.0643(15) Uani 1 d . . . 
H25A H -0.0547 0.8852 0.6374 0.077 Uiso 1 calc R . . 
H25B H -0.0657 0.9960 0.5854 0.077 Uiso 1 calc R . . 
C26 C -0.2051(6) 0.9583(6) 0.6654(6) 0.082(2) Uani 1 d . . . 
H26A H -0.2145 1.0344 0.6861 0.098 Uiso 1 calc R . . 
H26B H -0.2725 0.9285 0.5935 0.098 Uiso 1 calc R . . 
C27 C -0.2304(8) 0.8913(7) 0.7500(8) 0.106(3) Uani 1 d . . . 
H27A H -0.2117 0.8181 0.7353 0.127 Uiso 1 calc R . . 
H27B H -0.3217 0.8849 0.7464 0.127 Uiso 1 calc R . . 
H27C H -0.1743 0.9272 0.8235 0.127 Uiso 1 calc R . . 
C31 C 0.0652(5) 1.1477(4) 0.7619(5) 0.0541(13) Uani 1 d . . . 
H31A H 0.1173 1.1792 0.8389 0.065 Uiso 1 calc R . . 
H31B H -0.0195 1.1718 0.7459 0.065 Uiso 1 calc R . . 
C32 C 0.1368(5) 1.1930(4) 0.6833(4) 0.0477(11) Uani 1 d . . . 
C33 C 0.0828(6) 1.2623(5) 0.6100(5) 0.0574(13) Uani 1 d . . . 
H33 H -0.0018 1.2758 0.6031 0.069 Uiso 1 calc R . . 
C34 C 0.1542(6) 1.3122(5) 0.5460(5) 0.0666(16) Uani 1 d . . . 
H34 H 0.1171 1.3587 0.4964 0.080 Uiso 1 calc R . . 
C35 C 0.2796(6) 1.2927(5) 0.5562(5) 0.0624(14) Uani 1 d . . . 
H35 H 0.3277 1.3273 0.5143 0.075 Uiso 1 calc R . . 
C36 C 0.3354(5) 1.2213(4) 0.6293(4) 0.0472(11) Uani 1 d . . . 
C37 C 0.2630(5) 1.1713(4) 0.6926(4) 0.0498(12) Uani 1 d . . . 
H37 H 0.2988 1.1234 0.7411 0.060 Uiso 1 calc R . . 
C38 C 0.4723(5) 1.1981(4) 0.6399(4) 0.0524(12) Uani 1 d . . . 
H38A H 0.4717 1.1192 0.6436 0.063 Uiso 1 calc R . . 
H38B H 0.4946 1.2148 0.5734 0.063 Uiso 1 calc R . . 
Fe2 Fe 0.34833(8) 0.73848(6) 0.66804(7) 0.0552(3) Uani 1 d . . . 
Cl1 Cl 0.3185(3) 0.87606(17) 0.56961(18) 0.1148(8) Uani 1 d . . . 
Cl2 Cl 0.16031(17) 0.62305(15) 0.63274(18) 0.0890(6) Uani 1 d . . . 
Cl3 Cl 0.48422(19) 0.64224(18) 0.61777(17) 0.0909(6) Uani 1 d . . . 
Cl4 Cl 0.43964(15) 0.81071(14) 0.84866(13) 0.0694(4) Uani 1 d . . . 
C41 C 0.1013(8) 0.4120(7) 0.9368(9) 0.099(3) Uani 1 d . . . 
H41 H 0.0147 0.4233 0.9243 0.119 Uiso 1 calc R . . 
C42 C 0.1557(9) 0.3588(7) 1.0212(8) 0.100(3) Uani 1 d . . . 
H42 H 0.1060 0.3323 1.0656 0.120 Uiso 1 calc R . . 
C43 C 0.2799(10) 0.3430(7) 1.0429(8) 0.102(3) Uani 1 d . . . 
H43 H 0.3166 0.3072 1.1033 0.123 Uiso 1 calc R . . 
C44 C 0.3540(9) 0.3785(7) 0.9780(9) 0.104(3) Uani 1 d . . . 
H44 H 0.4406 0.3668 0.9926 0.125 Uiso 1 calc R . . 
C45 C 0.2970(12) 0.4326(8) 0.8893(9) 0.115(3) Uani 1 d . . . 
H45 H 0.3453 0.4573 0.8432 0.138 Uiso 1 calc R . . 
C46 C 0.1692(12) 0.4498(7) 0.8695(8) 0.107(3) Uani 1 d . . . 
H46 H 0.1304 0.4868 0.8107 0.129 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 
Cu1 0.0561(4) 0.0552(4) 0.0591(4) 0.0162(3) 0.0152(3) 0.0107(3) 
S11 0.0674(9) 0.0465(7) 0.0597(9) 0.0155(6) 0.0121(7) 0.0054(6) 
S12 0.0640(9) 0.0539(8) 0.0572(8) 0.0100(6) 0.0101(7) 0.0093(6) 
S21 0.0669(9) 0.0524(8) 0.0620(9) 0.0125(6) 0.0155(7) 0.0018(6) 
S22 0.0584(8) 0.0527(8) 0.0693(9) 0.0089(7) 0.0133(7) 0.0098(6) 
C13 0.056(3) 0.043(3) 0.051(3) 0.008(2) 0.024(2) 0.017(2) 
N14 0.050(2) 0.046(2) 0.056(3) 0.0142(19) 0.022(2) 0.0101(17) 
C15 0.066(3) 0.059(3) 0.066(4) 0.025(3) 0.029(3) 0.012(3) 
C16 0.068(4) 0.081(4) 0.057(4) 0.020(3) 0.022(3) 0.007(3) 
C17 0.095(5) 0.085(5) 0.085(5) 0.029(4) 0.035(4) -0.005(4) 
C23 0.051(3) 0.054(3) 0.051(3) 0.014(2) 0.027(2) 0.016(2) 
N24 0.049(2) 0.054(2) 0.048(2) 0.0099(19) 0.0231(19) 0.0087(18) 
C25 0.063(4) 0.078(4) 0.048(3) 0.010(3) 0.014(3) 0.009(3) 
C26 0.057(4) 0.097(5) 0.085(5) 0.017(4) 0.012(3) 0.014(3) 
C27 0.090(6) 0.121(7) 0.133(8) 0.031(6) 0.068(5) 0.026(5) 
C31 0.059(3) 0.053(3) 0.059(3) 0.009(2) 0.027(3) 0.019(2) 
C32 0.050(3) 0.047(3) 0.049(3) 0.005(2) 0.019(2) 0.012(2) 
C33 0.059(3) 0.059(3) 0.061(3) 0.020(3) 0.021(3) 0.020(2) 
C34 0.074(4) 0.063(4) 0.070(4) 0.032(3) 0.020(3) 0.026(3) 
C35 0.064(4) 0.068(4) 0.062(4) 0.024(3) 0.025(3) 0.014(3) 
C36 0.049(3) 0.049(3) 0.047(3) 0.010(2) 0.019(2) 0.010(2) 
C37 0.061(3) 0.051(3) 0.046(3) 0.017(2) 0.021(2) 0.022(2) 
C38 0.057(3) 0.058(3) 0.048(3) 0.013(2) 0.020(2) 0.016(2) 
Fe2 0.0597(5) 0.0577(5) 0.0532(5) 0.0153(4) 0.0201(4) 0.0173(3) 
Cl1 0.178(2) 0.0746(13) 0.0862(14) 0.0364(10) 0.0223(13) 0.0301(12) 
Cl2 0.0659(10) 0.0790(11) 0.1134(15) -0.0039(10) 0.0268(9) 0.0027(8) 
Cl3 0.0853(12) 0.1156(14) 0.0909(13) 0.0122(10) 0.0466(10) 0.0412(10) 
Cl4 0.0639(9) 0.0879(10) 0.0573(9) 0.0086(7) 0.0212(7) 0.0149(7) 
C41 0.080(5) 0.083(5) 0.117(7) -0.022(5) 0.013(5) 0.025(4) 
C42 0.100(6) 0.095(6) 0.100(6) -0.017(5) 0.043(5) 0.000(5) 
C43 0.101(6) 0.096(6) 0.092(6) -0.010(4) 0.013(5) 0.016(5) 
C44 0.081(5) 0.100(6) 0.123(8) -0.013(5) 0.026(5) 0.026(4) 
C45 0.143(9) 0.097(6) 0.110(7) -0.011(5) 0.071(7) -0.007(6) 
C46 0.140(9) 0.079(5) 0.088(6) -0.006(4) 0.021(6) 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 
Cu1 S12 2.219(3) . ? 
Cu1 S22 2.219(2) . ? 
Cu1 S11 2.222(2) . ? 
Cu1 S21 2.223(3) . ? 
S11 C13 1.731(5) . ? 
S12 C23 1.723(6) . ? 
S21 C13 1.707(5) . ? 
S22 C23 1.713(6) . ? 
C13 N14 1.312(6) . ? 
N14 C38 1.482(7) 2_677 ? 
N14 C15 1.488(6) . ? 
C15 C16 1.536(8) . ? 
C16 C17 1.503(8) . ? 
C23 N24 1.318(6) . ? 
N24 C31 1.479(7) . ? 
N24 C25 1.494(7) . ? 
C25 C26 1.531(9) . ? 
C26 C27 1.469(10) . ? 
C31 C32 1.521(7) . ? 
C32 C33 1.376(7) . ? 
C32 C37 1.395(7) . ? 
C33 C34 1.390(8) . ? 
C34 C35 1.375(8) . ? 
C35 C36 1.400(7) . ? 
C36 C37 1.390(7) . ? 
C36 C38 1.511(7) . ? 
C38 N14 1.482(7) 2_677 ? 
Fe2 Cl2 2.179(3) . ? 
Fe2 Cl1 2.193(3) . ? 
Fe2 Cl3 2.202(2) . ? 
Fe2 Cl4 2.221(3) . ? 
C41 C42 1.334(11) . ? 
C41 C46 1.345(13) . ? 
C42 C43 1.329(12) . ? 
C43 C44 1.358(12) . ? 
C44 C45 1.387(13) . ? 
C45 C46 1.374(14) . ? 
 
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 
S12 Cu1 S22 78.53(6) . . ? 
S12 Cu1 S11 100.16(7) . . ? 
S22 Cu1 S11 174.86(7) . . ? 
S12 Cu1 S21 169.02(7) . . ? 
S22 Cu1 S21 101.86(7) . . ? 
S11 Cu1 S21 78.47(7) . . ? 
C13 S11 Cu1 85.48(18) . . ? 
C23 S12 Cu1 85.81(18) . . ? 
C13 S21 Cu1 85.98(18) . . ? 
C23 S22 Cu1 86.00(18) . . ? 
N14 C13 S21 126.1(4) . . ? 
N14 C13 S11 124.2(4) . . ? 
S21 C13 S11 109.7(3) . . ? 
C13 N14 C38 122.8(4) . 2_677 ? 
C13 N14 C15 120.1(4) . . ? 
C38 N14 C15 117.0(4) 2_677 . ? 
N14 C15 C16 110.6(5) . . ? 
C17 C16 C15 111.8(6) . . ? 
N24 C23 S22 125.5(4) . . ? 
N24 C23 S12 124.9(4) . . ? 
S22 C23 S12 109.7(3) . . ? 
C23 N24 C31 121.2(4) . . ? 
C23 N24 C25 122.3(4) . . ? 
C31 N24 C25 116.5(4) . . ? 
N24 C25 C26 112.6(5) . . ? 
C27 C26 C25 114.7(6) . . ? 
N24 C31 C32 113.2(4) . . ? 
C33 C32 C37 119.9(5) . . ? 
C33 C32 C31 120.5(5) . . ? 
C37 C32 C31 119.4(5) . . ? 
C32 C33 C34 120.3(5) . . ? 
C35 C34 C33 120.0(5) . . ? 
C34 C35 C36 120.4(5) . . ? 
C37 C36 C35 119.2(5) . . ? 
C37 C36 C38 120.0(5) . . ? 
C35 C36 C38 120.8(4) . . ? 
C32 C37 C36 120.1(5) . . ? 
N14 C38 C36 112.4(4) 2_677 . ? 
Cl2 Fe2 Cl1 109.76(11) . . ? 
Cl2 Fe2 Cl3 106.79(12) . . ? 
Cl1 Fe2 Cl3 110.03(11) . . ? 
Cl2 Fe2 Cl4 113.19(8) . . ? 
Cl1 Fe2 Cl4 108.53(11) . . ? 
Cl3 Fe2 Cl4 108.52(9) . . ? 
C42 C41 C46 121.3(9) . . ? 
C43 C42 C41 121.1(9) . . ? 
C42 C43 C44 120.8(9) . . ? 
C43 C44 C45 118.3(9) . . ? 
C46 C45 C44 120.0(9) . . ? 
C45 C46 C41 118.6(10) . . ? 
 
_refine_diff_density_max    0.575 
_refine_diff_density_min   -0.642 
_refine_diff_density_rms    0.083 

_publ_section_references

;

Kabsch, W. (1988), J.Appl.Cryst 21 916-932.

Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480.

Sheldrick, G.M. (1993) SHELXL program for crystallography refinement.
University of Gottingen, Germany.

Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands

Walker, N. and Stuart, D., Acta Crystl 1983 A39 158.


;