#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/29/2002994.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2002994
loop_
_publ_author_name
'Madsen, Dennis'
'Burghammer, Manfred'
'Fiedler, Stefan'
'Muller, Harald'
_publ_section_title
;
 The single-crystal structure of the organic superconductor
 βCO-(BEDT-TTF)₂I₃ from a powder grain
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              601
_journal_page_last               606
_journal_paper_doi               10.1107/S0108768199003468
_journal_volume                  55
_journal_year                    1999
_chemical_formula_sum            'C10 H8 I1.5 S8'
_chemical_formula_weight         574.99
_chemical_name_common            beta-co-(BEDT-TTF)2I3
_chemical_name_systematic
;
  beta-co-(bis(ethylenedithio)tetrathiafulvalene)2 triiodide
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                94.90
_cell_angle_beta                 95.74
_cell_angle_gamma                110.00
_cell_formula_units_Z            2
_cell_length_a                   6.585
_cell_length_b                   9.038
_cell_length_c                   15.205
_cell_measurement_reflns_used    896
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24.9
_cell_measurement_theta_min      2.8
_cell_volume                     839.138
_computing_cell_refinement       'Denzo (Otwinoski & Minor, 1993)'
_computing_data_reduction
;
 Denzo (Otwinoski & Minor, 1993) & CCP4 (Scala (Evans, 1997))
;
_computing_molecular_graphics    'ORTEP (Johnson, 1976)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full .776
_diffrn_measured_fraction_theta_max .776
_diffrn_measurement_device_type  'Princeton CCD (1024x1024 pixels)'
_diffrn_measurement_method       φ
_diffrn_radiation_monochromator  Si(111)
_diffrn_radiation_source         'European Synchrotron Radiation Facility'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.68870
_diffrn_reflns_av_R_equivalents  0.032
_diffrn_reflns_av_sigmaI/netI    0.0232
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            13912
_diffrn_reflns_theta_full        27.33
_diffrn_reflns_theta_max         27.33
_diffrn_reflns_theta_min         3.22
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.807
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.276
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             551
_exptl_crystal_size_max          0.012
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.002
_refine_diff_density_max         2.283
_refine_diff_density_min         -1.719
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     198
_refine_ls_number_reflns         3230
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0371
_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)+(0.0097P)²+5.7148P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0812
_reflns_number_gt                2746
_reflns_number_total             3230
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ha0183.cif
_cod_data_source_block           beta
_cod_original_cell_volume        839.1
_cod_original_formula_sum        'C10 H8 I1.50 S8'
_cod_database_code               2002994
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
I1 0.0000 0.0000 0.0000 0.03994(17) Uani d SP 0.986(3) . . I
I2 0.40573(8) 0.25157(6) -0.01721(3) 0.05150(16) Uani d P 0.986(3) . . I
S1 0.0963(2) -0.14611(17) 0.43081(8) 0.0288(3) Uani d . 1 . . S
S2 0.4627(2) -0.26148(17) 0.44813(8) 0.0263(3) Uani d . 1 . . S
S3 0.2085(3) 0.0071(2) 0.27059(10) 0.0392(4) Uani d D 1 . . S
S4 0.6385(3) -0.1389(2) 0.28793(10) 0.0394(4) Uani d D 1 . . S
S5 0.2814(2) -0.43049(16) 0.61967(7) 0.0249(3) Uani d . 1 . . S
S6 -0.0835(2) -0.31358(17) 0.59826(7) 0.0256(3) Uani d . 1 . . S
S7 0.1971(2) -0.54159(18) 0.79329(8) 0.0322(3) Uani d DU 1 . . S
S8 -0.2374(2) -0.39674(18) 0.76841(8) 0.0322(3) Uani d DU 1 . . S
C1 0.2268(8) -0.2543(6) 0.4878(3) 0.0217(10) Uani d . 1 . . C
C2 0.2721(8) -0.1055(6) 0.3496(3) 0.0237(11) Uani d . 1 . . C
C3 0.4092(8) 0.0204(8) 0.1965(3) 0.0376(14) Uani d D 1 . . C
H3A 0.3478 -0.0834 0.1472 0.045 Uiso calc . 1 . . H
H3B 0.4265 0.1226 0.1619 0.045 Uiso calc . 1 . . H
C4 0.6299(9) 0.0335(6) 0.2389(4) 0.0350(13) Uani d D 1 . . C
H4A 0.6896 0.1347 0.2900 0.042 Uiso calc . 1 . . H
H4B 0.7393 0.0559 0.1892 0.042 Uiso calc . 1 . . H
C5 0.4378(9) -0.1576(6) 0.3580(3) 0.0251(11) Uani d . 1 . . C
C6 0.1496(8) -0.3259(6) 0.5590(3) 0.0214(10) Uani d . 1 . . C
C7 0.1177(8) -0.4523(6) 0.7054(3) 0.0205(10) Uani d . 1 A . C
C8A -0.0351(15) -0.5828(13) 0.8529(8) 0.030(3) Uani d PDU 0.490(17) A 1 C
H8A -0.1689 -0.6817 0.8160 0.036 Uiso calc P 0.49 A 1 H
H8B 0.0057 -0.6168 0.9169 0.036 Uiso calc P 0.49 A 1 H
C9A -0.106(2) -0.4432(14) 0.8670(5) 0.031(3) Uani d PDU 0.490(17) A 1 C
H9A 0.0357 -0.3405 0.8942 0.037 Uiso calc P 0.49 A 1 H
H9B -0.2168 -0.4649 0.9161 0.037 Uiso calc P 0.49 A 1 H
C8B 0.0429(15) -0.4891(17) 0.8747(5) 0.038(4) Uani d PDU 0.510(17) A 2 C
H8C 0.0594 -0.5481 0.9324 0.046 Uiso calc P 0.51 A 2 H
H8D 0.1146 -0.3628 0.8956 0.046 Uiso calc P 0.51 A 2 H
C9B -0.1946(15) -0.5298(13) 0.8437(8) 0.032(3) Uani d PDU 0.510(17) A 2 C
H9C -0.2785 -0.5228 0.9006 0.039 Uiso calc P 0.51 A 2 H
H9D -0.2623 -0.6502 0.8106 0.039 Uiso calc P 0.51 A 2 H
C10 -0.0491(8) -0.3979(6) 0.6958(3) 0.0210(10) Uani d . 1 A . C
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
I I -.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S .1246 .1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 '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_site_symmetry_1
_geom_angle
I2 I1 I2 2 180.0
C1 S1 C2 . 95.3(2)
C1 S2 C5 . 94.8(2)
C2 S3 C3 . 102.8(2)
C5 S4 C4 . 99.6(2)
C6 S5 C7 . 95.1(2)
C6 S6 C10 . 95.3(2)
C7 S7 C8A . 101.4(4)
C7 S7 C8B . 98.7(4)
C8A S7 C8B . 27.0(5)
C10 S8 C9B . 101.3(4)
C10 S8 C9A . 99.6(4)
C9B S8 C9A . 26.4(4)
C6 C1 S1 . 121.7(4)
C6 C1 S2 . 123.1(4)
S1 C1 S2 . 115.2(2)
C5 C2 S3 . 129.0(4)
C5 C2 S1 . 116.8(3)
S3 C2 S1 . 114.2(3)
C4 C3 S3 . 116.1(3)
C4 C3 H3A . 108.3
S3 C3 H3A . 108.3
C4 C3 H3B . 108.3
S3 C3 H3B . 108.3
H3A C3 H3B . 107.4
C3 C4 S4 . 114.6(4)
C3 C4 H4A . 108.6
S4 C4 H4A . 108.6
C3 C4 H4B . 108.6
S4 C4 H4B . 108.6
H4A C4 H4B . 107.6
C2 C5 S2 . 117.9(3)
C2 C5 S4 . 128.0(4)
S2 C5 S4 . 114.2(3)
C1 C6 S6 . 122.0(4)
C1 C6 S5 . 122.8(4)
S6 C6 S5 . 115.1(2)
C10 C7 S7 . 128.6(3)
C10 C7 S5 . 117.0(3)
S7 C7 S5 . 114.4(3)
C9A C8A S7 . 112.3(7)
C9A C8A H8A . 109.2
S7 C8A H8A . 109.2
C9A C8A H8B . 109.1
S7 C8A H8B . 109.1
H8A C8A H8B . 107.9
C8A C9A S8 . 115.3(7)
C8A C9A H9A . 108.4
S8 C9A H9A . 108.4
C8A C9A H9B . 108.4
S8 C9A H9B . 108.4
H9A C9A H9B . 107.5
C9B C8B S7 . 115.5(7)
C9B C8B H8C . 108.4
S7 C8B H8C . 108.4
C9B C8B H8D . 108.4
S7 C8B H8D . 108.4
H8C C8B H8D . 107.5
C8B C9B S8 . 111.0(7)
C8B C9B H9C . 109.4
S8 C9B H9C . 109.4
C8B C9B H9D . 109.4
S8 C9B H9D . 109.4
H9C C9B H9D . 108.0
C7 C10 S8 . 128.9(3)
C7 C10 S6 . 116.9(3)
S8 C10 S6 . 114.2(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
I1 I2 2 2.9089(8)
I1 I2 . 2.9089(8)
S1 C1 . 1.737(5)
S1 C2 . 1.753(5)
S2 C1 . 1.741(5)
S2 C5 . 1.752(5)
S3 C2 . 1.747(5)
S3 C3 . 1.800(4)
S4 C5 . 1.752(5)
S4 C4 . 1.799(4)
S5 C6 . 1.746(5)
S5 C7 . 1.755(5)
S6 C6 . 1.736(5)
S6 C10 . 1.754(4)
S7 C7 . 1.744(4)
S7 C8A . 1.801(5)
S7 C8B . 1.808(5)
S8 C10 . 1.743(5)
S8 C9B . 1.800(5)
S8 C9A . 1.808(5)
C1 C6 . 1.361(6)
C2 C5 . 1.327(7)
C3 C4 . 1.491(7)
C3 H3A . 1.0800
C3 H3B . 1.0800
C4 H4A . 1.0800
C4 H4B . 1.0800
C7 C10 . 1.349(7)
C8A C9A . 1.494(7)
C8A H8A . 1.0800
C8A H8B . 1.0800
C9A H9A . 1.0800
C9A H9B . 1.0800
C8B C9B . 1.495(7)
C8B H8C . 1.0800
C8B H8D . 1.0800
C9B H9C . 1.0800
C9B H9D . 1.0800
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
C2 S1 C1 C6 -176.7(5)
C2 S1 C1 S2 4.2(3)
C5 S2 C1 C6 176.8(5)
C5 S2 C1 S1 -4.0(3)
C3 S3 C2 C5 5.1(6)
C3 S3 C2 S1 -177.9(3)
C1 S1 C2 C5 -2.7(5)
C1 S1 C2 S3 179.9(3)
C2 S3 C3 C4 -35.9(5)
S3 C3 C4 S4 65.6(6)
C5 S4 C4 C3 -54.2(4)
S3 C2 C5 S2 177.3(3)
S1 C2 C5 S2 .3(6)
S3 C2 C5 S4 -3.9(9)
S1 C2 C5 S4 179.1(3)
C1 S2 C5 C2 2.2(5)
C1 S2 C5 S4 -176.7(3)
C4 S4 C5 C2 24.3(6)
C4 S4 C5 S2 -156.8(3)
S1 C1 C6 S6 -.3(7)
S2 C1 C6 S6 178.8(3)
S1 C1 C6 S5 -178.1(3)
S2 C1 C6 S5 1.0(7)
C10 S6 C6 C1 -170.3(5)
C10 S6 C6 S5 7.6(3)
C7 S5 C6 C1 170.5(5)
C7 S5 C6 S6 -7.4(3)
C8A S7 C7 C10 12.7(7)
C8B S7 C7 C10 -14.6(7)
C8A S7 C7 S5 -167.9(5)
C8B S7 C7 S5 164.8(5)
C6 S5 C7 C10 4.1(5)
C6 S5 C7 S7 -175.4(3)
C7 S7 C8A C9A -47.3(9)
C8B S7 C8A C9A 39.6(8)
S7 C8A C9A S8 72.0(13)
C10 S8 C9A C8A -49.5(10)
C9B S8 C9A C8A 46.7(9)
C7 S7 C8B C9B 51.7(10)
C8A S7 C8B C9B -46.3(8)
S7 C8B C9B S8 -73.9(13)
C10 S8 C9B C8B 47.9(9)
C9A S8 C9B C8B -40.8(8)
S7 C7 C10 S8 .9(8)
S5 C7 C10 S8 -178.5(3)
S7 C7 C10 S6 179.9(3)
S5 C7 C10 S6 .5(6)
C9B S8 C10 C7 -13.9(7)
C9A S8 C10 C7 12.8(7)
C9B S8 C10 S6 167.0(5)
C9A S8 C10 S6 -166.2(5)
C6 S6 C10 C7 -4.9(5)
C6 S6 C10 S8 174.3(3)
