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#$Date: 2016-03-22 11:42:22 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178912 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/41/4114184.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_4114184
loop_
_publ_author_name
'Stéphane A. Baudron'
'Narcis Avarvari'
'Patrick Batail'
'Claude Coulon'
'Rodolphe Clérac'
'Enric Canadell'
'Pascale Auban-Senzier'
_publ_contact_author
; Dr Patrick Batail 
  Laboratoire Chimie Inorganique, Matériaux et Interfaces,
  FRE 2447 CNRS-Université d'Angers,
  Bat. K, 2, Boulevard Lavoisier, Angers, France 
;
_publ_contact_author_email       patrick.batail@univ-angers.fr
_publ_contact_author_fax         '33 2 41 73 50 11'
_publ_contact_author_phone       '33 2 41 73 52 64'
_publ_section_title
;
 Singular Crystalline β'-Layered Topologies Directed by Ribbons of
 Self-Complementary Amide...Amide Ring Motifs in [EDT-TTF-(CONH2)2]2X (X =
 HSO4-, ClO4-, ReO4-, AsF6-): Coupled Activation of Ribbon Curvature,
 Electron Interactions, and Magnetic Susceptibility
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11583
_journal_page_last               11590
_journal_paper_doi               10.1021/ja0356129
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C5 H4 N2 O3 S2'
_chemical_formula_weight         204.22
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                104.32(3)
_cell_angle_beta                 98.85(3)
_cell_angle_gamma                105.09(3)
_cell_formula_units_Z            2
_cell_length_a                   5.8330(16)
_cell_length_b                   7.4593(19)
_cell_length_c                   9.197(3)
_cell_measurement_reflns_used    2991
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      52.1
_cell_measurement_theta_min      3.3
_cell_volume                     364.0(2)
_computing_cell_refinement       'SELECT, CELL [STOE-IPDS]'
_computing_data_collection       'EXPOSE [STOE-IPDS]'
_computing_data_reduction        'INTEGRATE [STOE-IPDS]'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 6.66
_diffrn_measured_fraction_theta_full 0.926
_diffrn_measured_fraction_theta_max 0.926
_diffrn_measurement_device_type  STOE-IPDS
_diffrn_measurement_method       'Oscillation, Phi. incr. = 2.5'
_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  0.0390
_diffrn_reflns_av_sigmaI/netI    0.0385
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3614
_diffrn_reflns_theta_full        26.01
_diffrn_reflns_theta_max         26.01
_diffrn_reflns_theta_min         2.35
_exptl_absorpt_coefficient_mu    0.693
_exptl_absorpt_correction_T_max  0.9153
_exptl_absorpt_correction_T_min  0.8666
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'FACEIT, STOE-IPDS'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.863
_exptl_crystal_description       block
_exptl_crystal_F_000             208
_exptl_crystal_size_max          0.1924
_exptl_crystal_size_mid          0.1924
_exptl_crystal_size_min          0.1540
_refine_diff_density_max         0.294
_refine_diff_density_min         -0.188
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.951
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         1325
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.951
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0265
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0381P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0618
_refine_ls_wR_factor_ref         0.0658
_reflns_number_gt                1057
_reflns_number_total             1325
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0356129si20030414_071433.cif
_cod_data_source_block           sb88p3_a
_cod_original_cell_volume        364.02(17)
_cod_database_code               4114184
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 0.25214(9) 0.58486(6) 0.17386(5) 0.02629(16) Uani 1 1 d .
S2 S -0.00839(11) 0.17781(6) 0.12710(6) 0.03717(18) Uani 1 1 d .
C1 C -0.0064(4) 0.7293(2) 0.3596(2) 0.0240(4) Uani 1 1 d .
C2 C 0.0129(3) 0.5376(2) 0.26613(19) 0.0209(4) Uani 1 1 d .
C3 C -0.1133(4) 0.3472(2) 0.2432(2) 0.0229(4) Uani 1 1 d .
C4 C -0.3253(4) 0.2594(3) 0.3041(2) 0.0257(4) Uani 1 1 d .
C5 C 0.2244(4) 0.3417(3) 0.0809(2) 0.0290(5) Uani 1 1 d .
N1 N -0.1673(3) 0.7321(2) 0.44322(18) 0.0317(4) Uani 1 1 d .
H1A H -0.1745 0.8414 0.4976 0.038 Uiso 1 1 calc R
H1B H -0.2663 0.6246 0.4441 0.038 Uiso 1 1 calc R
N2 N -0.4233(3) 0.0662(2) 0.2518(2) 0.0413(5) Uani 1 1 d .
H2A H -0.5445 0.0093 0.2841 0.050 Uiso 1 1 calc R
H2B H -0.3653 -0.0015 0.1857 0.050 Uiso 1 1 calc R
O1 O 0.1419(3) 0.87886(18) 0.35301(17) 0.0400(4) Uani 1 1 d .
O2 O -0.4067(3) 0.35709(19) 0.39829(17) 0.0405(4) Uani 1 1 d .
O3 O 0.3513(3) 0.2901(2) -0.00299(18) 0.0441(4) 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
S1 0.0269(3) 0.0158(2) 0.0345(3) 0.00342(19) 0.0174(2) 0.00191(19)
S2 0.0431(4) 0.0140(2) 0.0537(4) 0.0008(2) 0.0344(3) 0.0032(2)
C1 0.0280(12) 0.0148(9) 0.0284(9) 0.0033(7) 0.0124(8) 0.0051(8)
C2 0.0208(11) 0.0177(9) 0.0241(9) 0.0049(7) 0.0102(8) 0.0046(7)
C3 0.0243(11) 0.0175(9) 0.0259(9) 0.0023(7) 0.0125(8) 0.0052(8)
C4 0.0270(12) 0.0178(9) 0.0317(10) 0.0055(8) 0.0140(8) 0.0037(8)
C5 0.0302(12) 0.0207(9) 0.0351(10) 0.0031(8) 0.0194(9) 0.0042(8)
N1 0.0377(11) 0.0137(7) 0.0427(10) 0.0013(7) 0.0238(8) 0.0047(7)
N2 0.0454(13) 0.0157(8) 0.0625(12) 0.0039(8) 0.0390(10) 0.0011(8)
O1 0.0487(10) 0.0148(6) 0.0567(9) 0.0044(6) 0.0363(8) 0.0024(6)
O2 0.0444(10) 0.0206(7) 0.0571(9) 0.0031(6) 0.0381(8) 0.0042(6)
O3 0.0485(11) 0.0248(7) 0.0612(10) 0.0038(7) 0.0419(8) 0.0072(7)
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'
S S 0.1246 0.1234 '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
C2 S1 C5 97.29(9)
C3 S2 C5 98.36(9)
O1 C1 N1 123.36(16)
O1 C1 C2 115.96(17)
N1 C1 C2 120.67(16)
C3 C2 C1 133.52(18)
C3 C2 S1 117.41(14)
C1 C2 S1 109.07(13)
C2 C3 C4 130.40(17)
C2 C3 S2 115.08(15)
C4 C3 S2 114.51(13)
O2 C4 N2 120.47(19)
O2 C4 C3 122.80(16)
N2 C4 C3 116.72(17)
O3 C5 S1 125.02(15)
O3 C5 S2 123.18(15)
S1 C5 S2 111.79(11)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
S1 C2 1.746(2)
S1 C5 1.7566(19)
S2 C3 1.7457(19)
S2 C5 1.757(2)
C1 O1 1.243(2)
C1 N1 1.303(3)
C1 C2 1.517(2)
C2 C3 1.365(3)
C3 C4 1.498(3)
C4 O2 1.225(2)
C4 N2 1.334(2)
C5 O3 1.212(2)
