#------------------------------------------------------------------------------
#$Date: 2016-03-26 14:08:46 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180249 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/35/7113518.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7113518
loop_
_publ_author_name
'V�zquez, Miguel'
'Taglietti, Angelo'
'Gatteschi, Dante'
'Sorace, Lorenzo'
'Sangregorio, Claudio'
'Gonz�lez, Ana M.'
'Maneiro, Marcelino'
'Pedrido, Rosa M.'
'Bermejo, Manuel R.'
_publ_section_title
;
 A 3D network of helicates fully assembled by ?-stacking interactions
;
_journal_issue                   15
_journal_name_full               'Chemical Communications'
_journal_page_first              1840
_journal_paper_doi               10.1039/b303549b
_journal_year                    2003
_chemical_formula_sum            'C86 H74 Cu2 N10 O8 S4'
_chemical_formula_weight         1630.87
_chemical_name_systematic
;
?
;
_space_group_IT_number           70
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-F 2uv 2vw'
_symmetry_space_group_name_H-M   'F d d d :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.000
_cell_angle_beta                 90.000
_cell_angle_gamma                90.000
_cell_formula_units_Z            8
_cell_length_a                   17.156(2)
_cell_length_b                   21.443(3)
_cell_length_c                   41.221(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      45.575
_cell_measurement_theta_min      21.19
_cell_volume                     15164(3)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'MACH3 Enraf Nonius'
_diffrn_measurement_method       omega/2-theta
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealead tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0486
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            3910
_diffrn_reflns_theta_full        74.91
_diffrn_reflns_theta_max         74.90
_diffrn_reflns_theta_min         3.47
_diffrn_standards_decay_%        3
_diffrn_standards_interval_time  120'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.256
_exptl_absorpt_correction_T_max  0.9996
_exptl_absorpt_correction_T_min  0.8407
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            brown-red
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             6720
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.668
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         3910
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.1109
_refine_ls_R_factor_gt           0.0503
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0996P)²+16.4778P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1367
_refine_ls_wR_factor_ref         0.1680
_reflns_number_gt                2360
_reflns_number_total             3910
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b303549b.txt
_cod_data_source_block           cumdats
_cod_original_sg_symbol_H-M      Fddd
_cod_database_code               7113518
#BEGIN Tags that were not found in dictionaries:
_exptl_absorpt_correction_t_ave  0.9258
_diffrn_standards_decay_corr_max 1.04
_diffrn_standards_decay_corr_min 0.974
#END Tags that were not found in dictionaries
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'
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
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_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'
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
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) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
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) .
