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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/4/11/41/4114183.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_4114183
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            'C20 H16 Cl14 Mo6 N4 O4 S12'
_chemical_formula_weight         1833.03
_chemical_name_common            '(EDT-TTF-(CONH2))2 (Mo6Cl14)'
_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                114.258(13)
_cell_angle_beta                 105.477(14)
_cell_angle_gamma                92.126(14)
_cell_formula_units_Z            1
_cell_length_a                   8.9713(10)
_cell_length_b                   12.4561(14)
_cell_length_c                   12.7006(15)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      52.1
_cell_measurement_theta_min      3.3
_cell_volume                     1229.5(3)
_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 0.911
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_device_type  STOE-IPDS
_diffrn_measurement_method       'Oscillation, Phi. incr. = 1.8'
_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  0.0342
_diffrn_reflns_av_sigmaI/netI    0.0423
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12028
_diffrn_reflns_theta_full        26.07
_diffrn_reflns_theta_max         26.07
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    2.792
_exptl_absorpt_correction_T_max  0.8308
_exptl_absorpt_correction_T_min  0.6041
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'FACEIT, STOE-IPDS'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.476
_exptl_crystal_description       needle
_exptl_crystal_F_000             878
_exptl_crystal_size_max          0.3080
_exptl_crystal_size_mid          0.077
_exptl_crystal_size_min          0.077
_refine_diff_density_max         0.468
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.881
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         4446
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.881
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0224
_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)+(0.0203P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0462
_refine_ls_wR_factor_ref         0.0484
_reflns_number_gt                3325
_reflns_number_total             4446
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0356129si20030414_071358.cif
_cod_data_source_block           sb255eam
_cod_original_cell_volume        1229.5(2)
_cod_database_code               4114183
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
MoA Mo -0.06183(3) -0.01569(3) 0.12157(3) 0.01852(8) Uani 1 1 d .
MoB Mo 0.01735(4) 0.16332(3) 0.08005(3) 0.01885(8) Uani 1 1 d .
MoC Mo 0.20655(3) 0.00987(3) 0.08339(3) 0.01842(8) Uani 1 1 d .
Cl1 Cl -0.23619(11) 0.13080(9) 0.11229(8) 0.0265(2) Uani 1 1 d .
Cl2 Cl 0.15333(11) 0.14987(9) 0.26945(8) 0.0272(2) Uani 1 1 d .
Cl3 Cl -0.27115(11) -0.17920(9) -0.03969(9) 0.0277(2) Uani 1 1 d .
Cl4 Cl 0.11913(11) -0.16119(9) 0.11830(9) 0.0274(2) Uani 1 1 d .
ClA Cl -0.13688(12) -0.03897(10) 0.28468(9) 0.0357(3) Uani 1 1 d .
ClB Cl 0.03564(13) 0.37784(9) 0.18627(10) 0.0375(3) Uani 1 1 d .
ClC Cl 0.47504(10) 0.02130(10) 0.19343(9) 0.0333(2) Uani 1 1 d .
S1 S 0.40850(12) -0.41183(10) -0.16609(9) 0.0305(2) Uani 1 1 d .
S2 S 0.18744(12) -0.59947(9) -0.18293(8) 0.0293(2) Uani 1 1 d .
S3 S 0.47677(12) -0.27905(9) 0.12329(9) 0.0288(2) Uani 1 1 d .
S4 S 0.25561(13) -0.46738(10) 0.10613(9) 0.0335(3) Uani 1 1 d .
S5 S 0.53238(14) -0.12895(11) 0.38582(9) 0.0408(3) Uani 1 1 d .
S6 S 0.25111(15) -0.34926(11) 0.35776(9) 0.0437(3) Uani 1 1 d .
C1 C 0.3548(5) -0.4936(4) -0.4035(4) 0.0341(10) Uani 1 1 d .
C2 C 0.2971(5) -0.5150(4) -0.3109(3) 0.0276(9) Uani 1 1 d .
C3 C 0.1938(4) -0.6025(4) -0.3193(3) 0.0259(9) Uani 1 1 d .
C4 C 0.0823(5) -0.6988(4) -0.4364(3) 0.0282(9) Uani 1 1 d .
C5 C 0.3185(4) -0.4686(4) -0.0918(3) 0.0254(9) Uani 1 1 d .
C6 C 0.3487(5) -0.4116(4) 0.0327(3) 0.0270(9) Uani 1 1 d .
C7 C 0.4331(5) -0.2579(4) 0.2560(3) 0.0273(9) Uani 1 1 d .
C8 C 0.3282(5) -0.3440(4) 0.2479(3) 0.0260(9) Uani 1 1 d .
C9 C 0.5211(6) -0.1787(4) 0.4979(4) 0.0416(12) Uani 1 1 d .
H9A H 0.5756 -0.2464 0.4876 0.050 Uiso 1 1 calc R
H9B H 0.5745 -0.1151 0.5780 0.050 Uiso 1 1 calc R
C10 C 0.3557(6) -0.2143(5) 0.4908(4) 0.0513(14) Uani 1 1 d .
H10A H 0.2983 -0.1495 0.4921 0.062 Uiso 1 1 calc R
H10B H 0.3578 -0.2253 0.5625 0.062 Uiso 1 1 calc R
O1 O 0.4795(5) -0.4278(4) -0.3633(3) 0.0677(12) Uani 1 1 d .
N1 N 0.2684(2) -0.54941(19) -0.51934(17) 0.0522(12) Uani 1 1 d .
H1A H 0.2999 -0.5402 -0.5739 0.063 Uiso 1 1 calc R
H1B H 0.1809 -0.5947 -0.5399 0.063 Uiso 1 1 calc R
O2 O 0.0050(2) -0.67147(19) -0.51506(17) 0.0445(8) Uani 1 1 d R
N2 N 0.0665(2) -0.80742(19) -0.44477(17) 0.0449(10) Uani 1 1 d R
H2A H -0.0003 -0.8637 -0.5074 0.054 Uiso 1 1 calc R
H2B H 0.1230 -0.8223 -0.3876 0.054 Uiso 1 1 calc 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'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 '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
ClA MoA Cl1 93.92(4) . .
ClA MoA Cl2 91.85(4) . .
Cl1 MoA Cl2 89.55(4) . .
ClA MoA Cl3 92.82(4) . .
Cl1 MoA Cl3 90.06(4) . .
Cl2 MoA Cl3 175.33(3) . .
ClA MoA Cl4 90.46(4) . .
Cl1 MoA Cl4 175.62(3) . .
Cl2 MoA Cl4 90.33(4) . .
Cl3 MoA Cl4 89.71(4) . .
ClA MoA MoB 135.82(3) . .
Cl1 MoA MoB 58.02(3) . .
Cl2 MoA MoB 58.05(3) . .
Cl3 MoA MoB 118.02(3) . .
Cl4 MoA MoB 118.43(3) . .
ClA MoA MoC 136.65(3) . 2
Cl1 MoA MoC 58.25(3) . 2
Cl2 MoA MoC 117.83(3) . 2
Cl3 MoA MoC 58.24(3) . 2
Cl4 MoA MoC 118.14(3) . 2
MoB MoA MoC 59.790(19) . 2
ClA MoA MoC 133.58(3) . .
Cl1 MoA MoC 117.96(3) . .
Cl2 MoA MoC 58.24(3) . .
Cl3 MoA MoC 118.07(3) . .
Cl4 MoA MoC 58.50(3) . .
MoB MoA MoC 59.952(16) . .
MoC MoA MoC 89.768(18) 2 .
ClA MoA MoB 134.46(3) . 2
Cl1 MoA MoB 118.12(3) . 2
Cl2 MoA MoB 117.94(3) . 2
Cl3 MoA MoB 58.36(3) . 2
Cl4 MoA MoB 58.25(3) . 2
MoB MoA MoB 89.681(18) . 2
MoC MoA MoB 59.893(16) 2 2
MoC MoA MoB 59.73(2) . 2
ClB MoB Cl1 90.95(4) . .
ClB MoB Cl2 92.06(4) . .
Cl1 MoB Cl2 89.65(3) . .
ClB MoB Cl4 92.07(4) . 2
Cl1 MoB Cl4 90.62(4) . 2
Cl2 MoB Cl4 175.86(4) . 2
ClB MoB Cl3 93.44(4) . 2
Cl1 MoB Cl3 175.61(4) . 2
Cl2 MoB Cl3 90.08(4) . 2
Cl4 MoB Cl3 89.33(4) 2 2
ClB MoB MoC 134.16(3) . 2
Cl1 MoB MoC 58.42(3) . 2
Cl2 MoB MoC 118.31(3) . 2
Cl4 MoB MoC 58.58(3) 2 2
Cl3 MoB MoC 118.07(3) 2 2
ClB MoB MoA 133.98(3) . .
Cl1 MoB MoA 58.09(3) . .
Cl2 MoB MoA 58.13(3) . .
Cl4 MoB MoA 118.74(3) 2 .
Cl3 MoB MoA 118.27(3) 2 .
MoC MoB MoA 60.187(16) 2 .
ClB MoB MoC 135.74(3) . .
Cl1 MoB MoC 118.19(3) . .
Cl2 MoB MoC 58.32(3) . .
Cl4 MoB MoC 118.07(3) 2 .
Cl3 MoB MoC 58.17(3) 2 .
MoC MoB MoC 90.087(19) 2 .
MoA MoB MoC 60.110(15) . .
ClB MoB MoA 135.69(3) . 2
Cl1 MoB MoA 118.53(3) . 2
Cl2 MoB MoA 118.35(3) . 2
Cl4 MoB MoA 58.04(3) 2 2
Cl3 MoB MoA 57.95(3) 2 2
MoC MoB MoA 60.130(18) 2 2
MoA MoB MoA 90.319(18) . 2
MoC MoB MoA 60.043(17) . 2
ClC MoC Cl1 92.67(4) . 2
ClC MoC Cl2 92.24(4) . .
Cl1 MoC Cl2 175.09(3) 2 .
ClC MoC Cl3 92.97(4) . 2
Cl1 MoC Cl3 89.70(4) 2 2
Cl2 MoC Cl3 89.97(4) . 2
ClC MoC Cl4 91.66(4) . .
Cl1 MoC Cl4 90.14(4) 2 .
Cl2 MoC Cl4 89.80(4) . .
Cl3 MoC Cl4 175.37(3) 2 .
ClC MoC MoB 134.64(3) . 2
Cl1 MoC MoB 57.99(3) 2 2
Cl2 MoC MoB 118.08(3) . 2
Cl3 MoC MoB 118.02(3) 2 2
Cl4 MoC MoB 58.23(3) . 2
ClC MoC MoB 135.44(3) . .
Cl1 MoC MoB 117.94(3) 2 .
Cl2 MoC MoB 57.96(3) . .
Cl3 MoC MoB 58.35(3) 2 .
Cl4 MoC MoB 117.85(3) . .
MoB MoC MoB 89.913(19) 2 .
ClC MoC MoA 135.53(3) . 2
Cl1 MoC MoA 57.90(3) 2 2
Cl2 MoC MoA 118.01(3) . 2
Cl3 MoC MoA 58.01(3) 2 2
Cl4 MoC MoA 118.23(3) . 2
MoB MoC MoA 60.022(17) 2 2
MoB MoC MoA 60.064(17) . 2
ClC MoC MoA 134.23(3) . .
Cl1 MoC MoA 118.12(3) 2 .
Cl2 MoC MoA 57.96(3) . .
Cl3 MoC MoA 118.27(3) 2 .
Cl4 MoC MoA 57.93(3) . .
MoB MoC MoA 60.144(17) 2 .
MoB MoC MoA 59.938(15) . .
MoA MoC MoA 90.232(18) 2 .
MoB Cl1 MoA 63.89(3) . .
MoB Cl1 MoC 63.58(3) . 2
MoA Cl1 MoC 63.84(3) . 2
MoB Cl2 MoA 63.81(3) . .
MoB Cl2 MoC 63.72(3) . .
MoA Cl2 MoC 63.80(3) . .
MoA Cl3 MoC 63.74(3) . 2
MoA Cl3 MoB 63.69(3) . 2
MoC Cl3 MoB 63.48(3) 2 2
MoA Cl4 MoB 63.71(3) . 2
MoA Cl4 MoC 63.57(3) . .
MoB Cl4 MoC 63.20(3) 2 .
C5 S1 C2 95.11(19) . .
C5 S2 C3 95.73(19) . .
C6 S3 C7 95.20(18) . .
C6 S4 C8 95.64(19) . .
C7 S5 C9 98.8(2) . .
C8 S6 C10 102.7(2) . .
O1 C1 N1 126.2(4) . .
O1 C1 C2 115.6(4) . .
N1 C1 C2 118.2(3) . .
C3 C2 C1 133.2(4) . .
C3 C2 S1 117.2(3) . .
C1 C2 S1 109.1(3) . .
C2 C3 C4 125.6(3) . .
C2 C3 S2 116.0(3) . .
C4 C3 S2 118.4(3) . .
O2 C4 N2 123.2(3) . .
O2 C4 C3 119.7(3) . .
N2 C4 C3 117.0(3) . .
C6 C5 S1 121.9(3) . .
C6 C5 S2 122.6(3) . .
S1 C5 S2 115.5(2) . .
C5 C6 S4 121.7(3) . .
C5 C6 S3 122.5(3) . .
S4 C6 S3 115.8(2) . .
C8 C7 S5 126.7(3) . .
C8 C7 S3 116.9(3) . .
S5 C7 S3 116.3(2) . .
C7 C8 S6 129.4(3) . .
C7 C8 S4 116.1(3) . .
S6 C8 S4 114.5(2) . .
C10 C9 S5 113.2(3) . .
C9 C10 S6 114.4(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
MoA ClA 2.4601(10) .
MoA Cl1 2.4658(11) .
MoA Cl2 2.4685(11) .
MoA Cl3 2.4708(12) .
MoA Cl4 2.4728(11) .
MoA MoB 2.6083(5) .
MoA MoC 2.6126(6) 2
MoA MoC 2.6128(5) .
MoA MoB 2.6132(6) 2
MoB ClB 2.4237(12) .
MoB Cl1 2.4639(10) .
MoB Cl2 2.4663(10) .
MoB Cl4 2.4785(10) 2
MoB Cl3 2.4817(11) 2
MoB MoC 2.6022(8) 2
MoB MoC 2.6087(6) .
MoB MoA 2.6132(6) 2
MoC ClC 2.4062(10) .
MoC Cl1 2.4752(11) 2
MoC Cl2 2.4761(11) .
MoC Cl3 2.4770(10) 2
MoC Cl4 2.4879(10) .
MoC MoB 2.6022(8) 2
MoC MoA 2.6126(6) 2
Cl1 MoC 2.4752(11) 2
Cl3 MoC 2.4770(10) 2
Cl3 MoB 2.4817(11) 2
Cl4 MoB 2.4785(10) 2
S1 C5 1.719(4) .
S1 C2 1.736(4) .
S2 C5 1.721(4) .
S2 C3 1.733(4) .
S3 C6 1.721(4) .
S3 C7 1.749(4) .
S4 C6 1.719(4) .
S4 C8 1.748(4) .
S5 C7 1.739(4) .
S5 C9 1.793(4) .
S6 C8 1.737(4) .
S6 C10 1.807(5) .
C1 O1 1.211(5) .
C1 N1 1.327(4) .
C1 C2 1.515(5) .
C2 C3 1.355(5) .
C3 C4 1.517(5) .
C4 O2 1.234(4) .
C4 N2 1.312(4) .
C5 C6 1.382(5) .
C7 C8 1.352(5) .
C9 C10 1.502(7) .
