# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2003

data_global

_audit_creation_method           SHELXL-97

_journal_coden_Cambridge         182

_publ_contact_author_name        'Dr Miguel Vazquez'
_publ_contact_author_address     
;
Chimica Generale
Universitą di Pavia
Via Taramelli 12
Pavia
27100
ITALY
;
_publ_contact_author_email       miguel.vazquez@unipv.it
_publ_requested_journal          'Chemical Communications'
_publ_section_title              
;
A 3D network of helicates fully assembled by p-stacking interactions
;

loop_
_publ_author_name
M.Vazquez
A.Taglietti
D.Gatteschi
L.Sorace
C.Sangregorio
A.M.Gonzalez
M.Maneiro
R.M.Pedrido
M.R.Bermejo

_pub1_section_acknowledgements   
;
Intensity measurementes were performed at the Unidade de Raios X. RIAIDT.
University of Santiago de Compostela. SPAIN.
;

data_cumdats
_database_code_CSD               207443

_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C86 H74 Cu2 N10 O8 S4'
_chemical_formula_weight         1630.87

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Fddd

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/4, -y+1/4, z'
'x, -y+1/4, -z+1/4'
'-x+1/4, y, -z+1/4'
'x, y+1/2, z+1/2'
'-x+1/4, -y+3/4, z+1/2'
'x, -y+3/4, -z+3/4'
'-x+1/4, y+1/2, -z+3/4'
'x+1/2, y, z+1/2'
'-x+3/4, -y+1/4, z+1/2'
'x+1/2, -y+1/4, -z+3/4'
'-x+3/4, y, -z+3/4'
'x+1/2, y+1/2, z'
'-x+3/4, -y+3/4, z'
'x+1/2, -y+3/4, -z+1/4'
'-x+3/4, y+1/2, -z+1/4'
'-x, -y, -z'
'x-1/4, y-1/4, -z'
'-x, y-1/4, z-1/4'
'x-1/4, -y, z-1/4'
'-x, -y+1/2, -z+1/2'
'x-1/4, y+1/4, -z+1/2'
'-x, y+1/4, z+1/4'
'x-1/4, -y+1/2, z+1/4'
'-x+1/2, -y, -z+1/2'
'x+1/4, y-1/4, -z+1/2'
'-x+1/2, y-1/4, z+1/4'
'x+1/4, -y, z+1/4'
'-x+1/2, -y+1/2, -z'
'x+1/4, y+1/4, -z'
'-x+1/2, y+1/4, z-1/4'
'x+1/4, -y+1/2, z-1/4'

_cell_length_a                   17.156(2)
_cell_length_b                   21.443(3)
_cell_length_c                   41.221(2)
_cell_angle_alpha                90.000
_cell_angle_beta                 90.000
_cell_angle_gamma                90.000
_cell_volume                     15164(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    25
_cell_measurement_theta_min      21.19
_cell_measurement_theta_max      45.575

_exptl_crystal_description       prism
_exptl_crystal_colour            brown-red
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6720
_exptl_absorpt_coefficient_mu    2.256
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_correction_T_min  0.8407
_exptl_absorpt_correction_T_max  0.9996
_exptl_absorpt_correction_t_ave  0.9258
_exptl_special_details           
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
Number of psi-scan sets used was   7
Theta correction was applied.
Averaged transmission function was used.
No Fourier smoothing was applied.
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealead tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'MACH3 Enraf Nonius'
_diffrn_measurement_method       omega/2-theta
_diffrn_standards_number         3

_diffrn_standards_interval_time  120'
_diffrn_standards_decay_%        3
_diffrn_standards_decay_corr_max 1.04
_diffrn_standards_decay_corr_min 0.974
_diffrn_reflns_number            3910
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0486
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_theta_min         3.47
_diffrn_reflns_theta_max         74.90
_reflns_number_total             3910
_reflns_number_gt                2360
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_structure_solution    SIR97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'

_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^)+(0.0996P)^2^+16.4778P] 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_number_reflns         3910
_refine_ls_number_parameters     299
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1109
_refine_ls_R_factor_gt           0.0503
_refine_ls_wR_factor_ref         0.1680
_refine_ls_wR_factor_gt          0.1367
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_restrained_S_all      0.995
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.1250 0.1250 0.270744(15) 0.0520(3) Uani 1 2 d S . .
S2 S 0.15220(6) 0.23746(5) 0.30934(2) 0.0606(3) Uani 1 1 d . . .
O3 O 0.07521(17) 0.22996(16) 0.29616(6) 0.0738(9) Uani 1 1 d . . .
N4 N 0.19655(17) 0.17488(16) 0.29870(6) 0.0534(8) Uani 1 1 d . . .
C5 C 0.1888(2) 0.07408(18) 0.21012(7) 0.0477(8) Uani 1 1 d . . .
C6 C 0.2786(2) 0.17252(19) 0.29894(8) 0.0520(9) Uani 1 1 d . . .
C7 C 0.1591(5) 0.2843(5) 0.40483(17) 0.104(3) Uani 1 1 d . . .
N8 N 0.20961(16) 0.10632(14) 0.23935(6) 0.0471(7) Uani 1 1 d . . .
C9 C 0.3177(2) 0.14396(18) 0.27306(8) 0.0508(9) Uani 1 1 d . . .
C10 C 0.1465(2) 0.00795(19) 0.15470(9) 0.0574(10) Uani 1 1 d . . .
C11 C 0.2192(2) 0.0911(2) 0.18020(8) 0.0536(9) Uani 1 1 d . . .
C12 C 0.1250 -0.0292(3) 0.1250 0.0687(19) Uani 1 2 d S . .
C90 C 0.3999(2) 0.1439(2) 0.27321(10) 0.0619(10) Uani 1 1 d . . .
O14 O 0.1943(2) 0.29262(16) 0.30061(7) 0.0829(9) Uani 1 1 d . . .
C15 C 0.1982(3) 0.0574(2) 0.15280(8) 0.0561(10) Uani 1 1 d . . .
C16 C 0.1368(2) 0.0255(2) 0.21237(9) 0.0570(10) Uani 1 1 d . . .
C17 C 0.1401(3) 0.2395(2) 0.35206(9) 0.0649(12) Uani 1 1 d . . .
C18 C 0.2828(2) 0.11437(19) 0.24523(8) 0.0514(9) Uani 1 1 d . . .
C19 C 0.1742(3) 0.2843(3) 0.37087(13) 0.0878(16) Uani 1 1 d . . .
C20 C 0.0923(3) 0.1959(3) 0.36652(11) 0.0786(14) Uani 1 1 d . . .
C21 C 0.1133(4) 0.2421(4) 0.41864(12) 0.098(2) Uani 1 1 d . . .
C22 C 0.3228(3) 0.1974(3) 0.32397(11) 0.0715(13) Uani 1 1 d . . .
C23 C 0.1164(3) -0.0072(2) 0.18437(9) 0.0646(11) Uani 1 1 d . . .
C24 C 0.4417(3) 0.1708(2) 0.29776(12) 0.0713(12) Uani 1 1 d . . .
C25 C 0.4023(3) 0.1968(3) 0.32365(12) 0.0769(14) Uani 1 1 d . . .
C26 C 0.0803(4) 0.1975(3) 0.39972(11) 0.0942(18) Uani 1 1 d . . .
C27 C 0.0991(4) 0.2434(4) 0.45516(13) 0.145(3) Uani 1 1 d . . .
H27A H 0.1377 0.2692 0.4654 0.218 Uiso 1 1 calc R . .
H27B H 0.1027 0.2018 0.4637 0.218 Uiso 1 1 calc R . .
H27C H 0.0481 0.2599 0.4595 0.218 Uiso 1 1 calc R . .
C97 C 0.3750 0.3750 0.3073(6) 0.220(8) Uiso 1 2 d S . .
C98 C 0.3750 0.3750 0.3511(6) 0.292(11) Uiso 1 2 d S . .
N99 N 0.3750 0.3750 0.2777(8) 0.44(2) Uiso 1 2 d S . .
H51 H 0.298(3) 0.212(3) 0.3374(12) 0.088(18) Uiso 1 1 d . . .
H52 H 0.495(3) 0.165(3) 0.2954(12) 0.102(17) Uiso 1 1 d . . .
H54 H 0.220(2) 0.0690(18) 0.1338(10) 0.064(12) Uiso 1 1 d . . .
H55 H 0.255(2) 0.1250(19) 0.1805(9) 0.061(12) Uiso 1 1 d . . .
H56 H 0.119(2) 0.0133(18) 0.2318(10) 0.060(11) Uiso 1 1 d . . .
H57 H 0.086(3) -0.042(2) 0.1846(11) 0.079(15) Uiso 1 1 d . . .
H58 H 0.160(2) -0.0538(19) 0.1210(10) 0.054(12) Uiso 1 1 d . . .
H59 H 0.426(3) 0.1283(19) 0.2556(10) 0.066(12) Uiso 1 1 d . . .
H60 H 0.318(3) 0.093(2) 0.2322(11) 0.076(13) Uiso 1 1 d . . .
H62 H 0.072(3) 0.165(3) 0.3542(13) 0.100(18) Uiso 1 1 d . . .
H63 H 0.210(3) 0.312(2) 0.3592(12) 0.087(17) Uiso 1 1 d . . .
H65 H 0.432(4) 0.220(3) 0.3378(14) 0.12(2) Uiso 1 1 d . . .
H72 H 0.179(4) 0.314(3) 0.4098(16) 0.12(3) Uiso 1 1 d . . .
H71 H 0.043(5) 0.159(4) 0.4101(19) 0.18(3) Uiso 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0438(4) 0.0818(6) 0.0305(3) 0.000 0.000 0.0006(4)
S2 0.0670(6) 0.0734(7) 0.0415(5) -0.0065(4) -0.0061(4) 0.0141(5)
O3 0.0618(17) 0.108(3) 0.0513(15) -0.0173(15) -0.0132(13) 0.0311(17)
N4 0.0472(16) 0.073(2) 0.0397(13) -0.0110(14) -0.0018(12) 0.0077(15)
C5 0.0494(19) 0.059(2) 0.0344(15) -0.0043(15) -0.0016(13) 0.0080(17)
C6 0.046(2) 0.068(2) 0.0421(16) -0.0021(16) -0.0059(14) -0.0040(18)
C7 0.097(5) 0.139(7) 0.076(4) -0.056(4) -0.019(3) 0.020(5)
N8 0.0460(16) 0.0630(19) 0.0323(12) -0.0027(12) 0.0014(11) 0.0003(14)
C9 0.0443(18) 0.063(2) 0.0453(18) 0.0005(16) -0.0030(14) 0.0009(16)
C10 0.075(3) 0.056(2) 0.0406(18) -0.0003(15) -0.0101(17) 0.003(2)
C11 0.056(2) 0.065(3) 0.0396(17) -0.0018(16) 0.0006(15) -0.002(2)
C12 0.109(6) 0.051(4) 0.046(3) 0.000 -0.023(3) 0.000
C90 0.047(2) 0.082(3) 0.056(2) 0.002(2) 0.0008(17) -0.0019(19)
O14 0.098(2) 0.070(2) 0.080(2) 0.0074(16) 0.0024(18) 0.0040(19)
C15 0.069(3) 0.065(3) 0.0338(16) -0.0009(15) -0.0015(16) 0.003(2)
C16 0.065(3) 0.069(3) 0.0369(17) 0.0013(17) -0.0022(16) -0.007(2)
C17 0.071(3) 0.077(3) 0.047(2) -0.0169(19) -0.0084(18) 0.023(2)
C18 0.0453(19) 0.066(3) 0.0427(16) -0.0022(16) 0.0014(14) 0.0042(18)
C19 0.089(4) 0.106(4) 0.068(3) -0.035(3) -0.008(3) 0.002(3)
C20 0.098(4) 0.085(4) 0.053(2) -0.011(2) 0.008(2) 0.015(3)
C21 0.098(4) 0.144(6) 0.052(3) -0.020(3) -0.006(3) 0.052(4)
C22 0.059(3) 0.102(4) 0.054(2) -0.017(2) -0.009(2) 0.001(3)
C23 0.083(3) 0.066(3) 0.045(2) 0.0067(18) -0.0159(19) -0.014(2)
C24 0.048(2) 0.087(3) 0.078(3) 0.003(2) -0.009(2) -0.011(2)
C25 0.063(3) 0.097(4) 0.071(3) -0.013(3) -0.017(2) -0.015(3)
C26 0.123(5) 0.110(4) 0.050(2) -0.006(3) 0.013(3) 0.029(4)
C27 0.158(6) 0.231(9) 0.046(3) -0.033(4) -0.011(3) 0.087(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
Cu1 N8 1.986(3) . ?
Cu1 N8 1.986(3) 2 ?
Cu1 N4 1.995(3) . ?
Cu1 N4 1.995(3) 2 ?
S2 O14 1.432(4) . ?
S2 O3 1.437(3) . ?
S2 N4 1.604(3) . ?
S2 C17 1.773(4) . ?
N4 C6 1.408(5) . ?
C5 C16 1.374(5) . ?
C5 C11 1.388(5) . ?
C5 N8 1.434(4) . ?
C6 C22 1.388(5) . ?
C6 C9 1.401(5) . ?
C7 C21 1.327(10) . ?
C7 C19 1.424(9) . ?
N8 C18 1.290(4) . ?
C9 C90 1.410(5) . ?
C9 C18 1.441(5) . ?
C10 C23 1.367(5) . ?
C10 C15 1.384(6) . ?
C10 C12 1.507(5) . ?
C11 C15 1.388(5) . ?
C12 C10 1.507(5) 4 ?
C90 C24 1.368(6) . ?
C16 C23 1.395(5) . ?
C17 C19 1.368(6) . ?
C17 C20 1.378(7) . ?
C20 C26 1.384(6) . ?
C21 C26 1.357(9) . ?
C21 C27 1.525(7) . ?
C22 C25 1.364(7) . ?
C24 C25 1.381(7) . ?
N99 C97 1.22(3) . ?
C98 C98 1.97(5) 7 ?
C98 C97 1.81(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N8 Cu1 N8 98.65(16) . 2 ?
N8 Cu1 N4 92.00(12) . . ?
N8 Cu1 N4 135.91(13) 2 . ?
N8 Cu1 N4 135.91(13) . 2 ?
N8 Cu1 N4 92.00(12) 2 2 ?
N4 Cu1 N4 109.42(17) . 2 ?
O14 S2 O3 117.4(2) . . ?
O14 S2 N4 112.53(19) . . ?
O3 S2 N4 103.82(17) . . ?
O14 S2 C17 106.8(2) . . ?
O3 S2 C17 105.68(19) . . ?
N4 S2 C17 110.34(18) . . ?
C6 N4 S2 120.2(3) . . ?
C6 N4 Cu1 126.9(2) . . ?
S2 N4 Cu1 108.35(16) . . ?
C16 C5 C11 120.2(3) . . ?
C16 C5 N8 118.0(3) . . ?
C11 C5 N8 121.8(3) . . ?
C22 C6 C9 118.2(4) . . ?
C22 C6 N4 122.6(4) . . ?
C9 C6 N4 119.3(3) . . ?
C21 C7 C19 122.0(6) . . ?
C18 N8 C5 117.7(3) . . ?
C18 N8 Cu1 124.2(2) . . ?
C5 N8 Cu1 117.6(2) . . ?
C6 C9 C90 118.4(3) . . ?
C6 C9 C18 126.8(3) . . ?
C90 C9 C18 114.8(3) . . ?
C23 C10 C15 118.3(4) . . ?
C23 C10 C12 120.6(4) . . ?
C15 C10 C12 121.1(3) . . ?
C5 C11 C15 119.3(4) . . ?
C10 C12 C10 116.2(5) 4 . ?
C24 C90 C9 121.9(4) . . ?
C10 C15 C11 121.2(4) . . ?
C5 C16 C23 119.2(4) . . ?
C19 C17 C20 119.1(5) . . ?
C19 C17 S2 122.0(4) . . ?
C20 C17 S2 118.9(3) . . ?
N8 C18 C9 127.8(3) . . ?
C17 C19 C7 118.7(7) . . ?
C26 C20 C17 120.0(6) . . ?
C7 C21 C26 118.7(5) . . ?
C7 C21 C27 120.3(7) . . ?
C26 C21 C27 120.9(7) . . ?
C25 C22 C6 122.4(5) . . ?
C10 C23 C16 121.7(4) . . ?
C90 C24 C25 119.0(4) . . ?
C22 C25 C24 120.0(4) . . ?
C21 C26 C20 121.6(7) . . ?
C98 C98 C97 180.000(3) 7 . ?
N99 C97 C98 180.000(4) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        74.91
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.668
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.061