#------------------------------------------------------------------------------
#$Date: 2016-03-26 14:28:44 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180264 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/50/7115031.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_7115031
loop_
_publ_author_name
'Barbour, Leonard J.'
'Atwood, Jerry L.'
_publ_section_title
;
 Non-covalent interactions exert extraordinary influence over conformation
 and properties of a well-known supramolecular building block
;
_journal_issue                   19
_journal_name_full               'Chemical Communications'
_journal_page_first              2020
_journal_paper_doi               10.1039/b105182m
_journal_year                    2001
_chemical_formula_sum            'C48 H40 N4 O16 S4'
_chemical_formula_weight         1057.08
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           114
_symmetry_space_group_name_Hall  'P -4 2n'
_symmetry_space_group_name_H-M   'P -4 21 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.8339(9)
_cell_length_b                   11.8339(9)
_cell_length_c                   14.9028(16)
_cell_measurement_temperature    173(2)
_cell_volume                     2087.0(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_sigmaI/netI    0.0249
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12722
_diffrn_reflns_theta_full        27.11
_diffrn_reflns_theta_max         27.11
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    0.317
_exptl_absorpt_correction_T_max  0.9250
_exptl_absorpt_correction_T_min  0.9110
_exptl_crystal_density_diffrn    1.682
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.674
_refine_diff_density_min         -0.212
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.06(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         2302
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0437
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0723P)²+0.8113P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1128
_refine_ls_wR_factor_ref         0.1153
_reflns_number_gt                2131
_reflns_number_total             2302
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b105182m.txt
_cod_data_source_block           d:\xray\recent\c4s1-3~1\sad
_cod_database_code               7115031
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'y, -x, -z'
'-x, -y, z'
'-y, x, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'
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
S1 S 0.54881(5) 0.27002(6) 0.81094(5) 0.02219(18) Uani 1 1 d .
O1 O 0.55289(17) 0.26307(16) 0.41492(12) 0.0252(4) Uani 1 1 d .
C3 C 0.4494(2) 0.2635(2) 0.64463(17) 0.0197(5) Uani 1 1 d .
H3 H 0.3807 0.2519 0.6764 0.024 Uiso 1 1 calc R
C4 C 0.5491(2) 0.2814(2) 0.69192(17) 0.0201(5) Uani 1 1 d .
C1 C 0.5522(2) 0.2779(2) 0.50648(17) 0.0192(5) Uani 1 1 d .
O3 O 0.46974(19) 0.1822(2) 0.83414(14) 0.0354(5) Uani 1 1 d .
N3A N 0.7939(2) 0.0436(2) 0.63167(18) 0.0310(6) Uani 1 1 d .
H3A H 0.8671 0.0568 0.6323 0.037 Uiso 1 1 calc R
C5 C 0.6485(2) 0.3049(2) 0.64680(17) 0.0197(5) Uani 1 1 d .
H5 H 0.7156 0.3193 0.6798 0.024 Uiso 1 1 calc R
O4 O 0.66285(17) 0.24456(17) 0.83494(13) 0.0295(5) Uani 1 1 d .
O2 O 0.51452(19) 0.38024(18) 0.84718(14) 0.0331(5) Uani 1 1 d .
C2 C 0.4491(2) 0.2624(2) 0.55094(16) 0.0181(5) Uani 1 1 d .
C7 C 0.7575(2) 0.3420(2) 0.50344(17) 0.0197(5) Uani 1 1 d .
H7A H 0.7809 0.2800 0.4628 0.024 Uiso 1 1 calc R
H7B H 0.8193 0.3550 0.5470 0.024 Uiso 1 1 calc R
C4A C 0.7409(3) 0.0232(3) 0.7079(2) 0.0311(7) Uani 1 1 d .
H4A H 0.7824 0.0214 0.7625 0.037 Uiso 1 1 calc R
C6 C 0.6509(2) 0.3077(2) 0.55329(17) 0.0190(5) Uani 1 1 d .
C2A C 0.7386(3) 0.0446(3) 0.5536(2) 0.0333(7) Uani 1 1 d .
H2A H 0.7790 0.0579 0.4996 0.040 Uiso 1 1 calc R
C1A C 0.6238(3) 0.0268(3) 0.5504(2) 0.0314(7) Uani 1 1 d .
H1A H 0.5857 0.0267 0.4943 0.038 Uiso 1 1 calc R
C6A C 0.5631(2) 0.0089(2) 0.62971(18) 0.0277(6) Uani 1 1 d .
C5A C 0.6254(3) 0.0042(3) 0.70912(19) 0.0288(6) Uani 1 1 d .
H5A H 0.5884 -0.0120 0.7642 0.035 Uiso 1 1 calc R
H1 H 0.6273 0.2360 0.3936 0.038(9) Uiso 1 1 d R
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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_3
O4 S1 O3 113.67(13) .
O4 S1 O2 110.87(13) .
O3 S1 O2 111.89(13) .
O4 S1 C4 105.31(12) .
O3 S1 C4 107.17(12) .
O2 S1 C4 107.45(12) .
C4 C3 C2 120.7(2) .
C5 C4 C3 120.4(2) .
C5 C4 S1 120.1(2) .
C3 C4 S1 119.5(2) .
O1 C1 C2 117.2(2) .
O1 C1 C6 121.3(2) .
C2 C1 C6 121.5(2) .
C4A N3A C2A 121.3(3) .
C4 C5 C6 120.6(2) .
C3 C2 C1 118.0(2) .
C3 C2 C7 122.4(2) 2_566
C1 C2 C7 119.6(2) 2_566
C6 C7 C2 110.7(2) 4_656
N3A C4A C5A 120.6(3) .
C5 C6 C1 118.2(2) .
C5 C6 C7 120.8(2) .
C1 C6 C7 121.0(2) .
N3A C2A C1A 120.9(3) .
C2A C1A C6A 120.1(3) .
C5A C6A C1A 116.8(3) .
C5A C6A C6A 121.18(18) 3_655
C1A C6A C6A 121.97(18) 3_655
C4A C5A C6A 120.3(3) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
S1 O4 1.428(2) .
S1 O3 1.440(2) .
S1 O2 1.469(2) .
S1 C4 1.779(3) .
O1 C1 1.376(3) .
C3 C4 1.391(4) .
C3 C2 1.396(3) .
C4 C5 1.383(4) .
C1 C2 1.400(4) .
C1 C6 1.406(4) .
N3A C4A 1.320(4) .
N3A C2A 1.335(4) .
C5 C6 1.394(3) .
C2 C7 1.523(3) 2_566
C7 C6 1.519(3) .
C7 C2 1.523(3) 4_656
C4A C5A 1.386(4) .
C2A C1A 1.376(5) .
C1A C6A 1.399(4) .
C6A C5A 1.395(4) .
C6A C6A 1.507(6) 3_655
