#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/40/7204093.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_7204093
loop_
_publ_author_name
'Rashid, Samina'
'Turner, Scott S.'
'Day, Peter'
'Howard, Judith A. K.'
'Guionneau, Philippe'
'McInnes, Eric J. L.'
'Mabbs, Frank E.'
'Clark, Robin J. H.'
'Firth, Steven'
'Biggs, Tim'
_publ_section_title
;
 New superconducting charge-transfer salts
 (BEDT-TTF)4[A·M(C2O4)3]·C6H5NO2 (A = H3O or NH4, M = Cr
 or Fe, BEDT-TTF = bis(ethylenedithio)tetrathiafulvalene)
;
_journal_issue                   9
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              2095
_journal_paper_doi               10.1039/b101134k
_journal_volume                  11
_journal_year                    2001
_chemical_formula_sum            'C26 H20.5 Cr0.5 N O7 S16'
_chemical_formula_weight         997.89
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 92.7010(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.3039(2)
_cell_length_b                   20.0908(3)
_cell_length_c                   35.2508(4)
_cell_measurement_temperature    298(2)
_cell_volume                     7289.3(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.1170
_diffrn_reflns_av_sigmaI/netI    0.1172
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            34583
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.16
_exptl_absorpt_coefficient_mu    1.137
_exptl_crystal_density_diffrn    1.819
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4060
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.915
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     472
_refine_ls_number_reflns         8365
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.1637
_refine_ls_R_factor_gt           0.0646
_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)+(0.0642P)²+1.3023P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1265
_refine_ls_wR_factor_ref         0.1719
_reflns_number_gt                4188
_reflns_number_total             8365
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b101134k.txt
_cod_data_source_block           etcrno
_cod_original_formula_sum        'C26 H20.50 Cr0.50 N O7 S16'
_cod_database_code               7204093
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cr1 Cr 1.0000 0.42207(6) -0.2500 0.0344(3) Uani 1 2 d S . .
S8 S 1.25685(14) 0.01188(8) 0.04381(4) 0.0380(4) Uani 1 1 d . . .
S7 S 1.38372(14) 0.04290(8) -0.03665(4) 0.0385(4) Uani 1 1 d . . .
S6 S 1.02560(15) 0.08849(8) 0.01930(4) 0.0400(4) Uani 1 1 d . . .
S16 S 0.78063(14) 0.17438(8) -0.04950(4) 0.0376(4) Uani 1 1 d . . .
S5 S 1.15042(15) 0.11844(8) -0.06066(4) 0.0402(4) Uani 1 1 d . . .
S15 S 0.66373(14) 0.14363(8) 0.03115(4) 0.0373(4) Uani 1 1 d . . .
S14 S 0.42295(14) 0.21414(8) 0.00821(5) 0.0392(4) Uani 1 1 d . . .
S13 S 0.54317(15) 0.24575(8) -0.07388(4) 0.0392(4) Uani 1 1 d . . .
S4 S 1.52326(15) 0.07253(8) -0.10624(5) 0.0443(4) Uani 1 1 d . . .
S3 S 0.89134(16) 0.07156(10) 0.08993(5) 0.0572(5) Uani 1 1 d . . .
S12 S 0.58517(15) 0.11061(8) 0.10822(5) 0.0428(4) Uani 1 1 d . . .
S11 S 0.29483(15) 0.19267(8) 0.07953(5) 0.0462(4) Uani 1 1 d . . .
S2 S 1.16976(15) -0.01692(9) 0.12078(5) 0.0468(5) Uani 1 1 d . . .
S10 S 0.91119(16) 0.19290(8) -0.12112(5) 0.0476(5) Uani 1 1 d . . .
S1 S 1.24904(18) 0.15804(9) -0.13502(5) 0.0524(5) Uani 1 1 d . . .
S9 S 0.62258(19) 0.27354(9) -0.15108(5) 0.0548(5) Uani 1 1 d . . .
C20 C 0.4329(5) 0.1802(3) 0.05395(16) 0.0322(13) Uani 1 1 d . . .
C10 C 1.2788(5) 0.1177(3) -0.09179(16) 0.0343(14) Uani 1 1 d . . .
C19 C 0.7745(6) 0.2075(3) -0.09534(16) 0.0330(14) Uani 1 1 d . . .
C9 C 1.1353(5) 0.0202(3) 0.07608(16) 0.0329(14) Uani 1 1 d . . .
C18 C 0.6650(6) 0.2398(3) -0.10675(16) 0.0345(14) Uani 1 1 d . . .
C8 C 1.3852(5) 0.0839(3) -0.08047(16) 0.0319(13) Uani 1 1 d . . .
C17 C 0.5772(5) 0.1884(3) -0.00391(16) 0.0299(13) Uani 1 1 d . . .
C16 C 0.5443(5) 0.1473(3) 0.06439(16) 0.0323(14) Uani 1 1 d . . .
C7 C 1.1778(5) 0.0594(3) 0.00881(16) 0.0311(13) Uani 1 1 d . . .
C6 C 1.0290(5) 0.0548(3) 0.06486(16) 0.0337(14) Uani 1 1 d . . .
C5 C 1.2321(5) 0.0729(3) -0.02517(16) 0.0328(14) Uani 1 1 d . . .
C15 C 0.6283(5) 0.2017(3) -0.03855(16) 0.0329(14) Uani 1 1 d . . .
C14 C 0.7695(7) 0.2618(4) -0.17621(19) 0.063(2) Uani 1 1 d . . .
H14A H 0.7482 0.2643 -0.2033 0.075 Uiso 1 1 calc R . .
H14B H 0.8288 0.2979 -0.1697 0.075 Uiso 1 1 calc R . .
C13 C 0.4305(6) 0.1057(3) 0.12934(18) 0.0433(16) Uani 1 1 d . . .
H13A H 0.3800 0.0706 0.1168 0.052 Uiso 1 1 calc R . .
H13B H 0.4444 0.0933 0.1558 0.052 Uiso 1 1 calc R . .
C4 C 1.0217(8) -0.0064(5) 0.1434(2) 0.093(3) Uani 1 1 d . . .
H4A H 0.9674 -0.0443 0.1364 0.112 Uiso 1 1 calc R . .
H4B H 1.0413 -0.0096 0.1705 0.112 Uiso 1 1 calc R . .
C12 C 0.3522(6) 0.1695(3) 0.12722(17) 0.0443(16) Uani 1 1 d . . .
H12A H 0.4054 0.2054 0.1378 0.053 Uiso 1 1 calc R . .
H12B H 0.2779 0.1647 0.1429 0.053 Uiso 1 1 calc R . .
C3 C 0.9455(8) 0.0506(4) 0.1375(2) 0.079(3) Uani 1 1 d . . .
H3A H 0.9944 0.0882 0.1478 0.095 Uiso 1 1 calc R . .
H3B H 0.8691 0.0459 0.1523 0.095 Uiso 1 1 calc R . .
C2 C 1.3565(8) 0.1162(5) -0.1646(2) 0.102(3) Uani 1 1 d . . .
H2A H 1.3019 0.0919 -0.1829 0.122 Uiso 1 1 calc R . .
H2B H 1.3990 0.1507 -0.1787 0.122 Uiso 1 1 calc R . .
C11 C 0.8378(7) 0.1969(3) -0.1679(2) 0.061(2) Uani 1 1 d . . .
H11A H 0.9043 0.1905 -0.1861 0.073 Uiso 1 1 calc R . .
H11B H 0.7757 0.1608 -0.1711 0.073 Uiso 1 1 calc R . .
C1 C 1.4497(10) 0.0743(5) -0.1529(2) 0.117(4) Uani 1 1 d . . .
H1A H 1.5200 0.0804 -0.1700 0.140 Uiso 1 1 calc R . .
H1B H 1.4157 0.0300 -0.1578 0.140 Uiso 1 1 calc R . .
O1 O 0.8499(4) 0.4329(2) -0.21761(11) 0.0392(10) Uani 1 1 d . . .
O2 O 1.0788(4) 0.3472(2) -0.22031(12) 0.0454(11) Uani 1 1 d . . .
O3 O 1.0964(4) 0.48710(18) -0.21800(11) 0.0373(10) Uani 1 1 d . . .
O4 O 1.2836(4) 0.5433(2) -0.21451(12) 0.0494(12) Uani 1 1 d . . .
O5 O 0.6804(4) 0.5015(2) -0.21148(13) 0.0594(13) Uani 1 1 d . . .
N2 N 1.0000 -0.1014(5) 0.2500 0.059(2) Uani 1 2 d SD . .
C23 C 1.2038(6) 0.5067(3) -0.23106(16) 0.0322(14) Uani 1 1 d . . .
C27 C 0.5000 0.2516(5) -0.2500 0.061(3) Uani 1 2 d S . .
O6 O 1.0885(5) 0.2362(2) -0.21915(15) 0.0655(15) Uani 1 1 d . . .
C22 C 0.7707(6) 0.4790(3) -0.22925(18) 0.0391(15) Uani 1 1 d . . .
C21 C 1.0483(6) 0.2890(3) -0.23271(17) 0.0438(16) Uani 1 1 d . . .
N1 N 0.5000 0.1788(6) -0.2500 0.086(4) Uani 1 2 d S . .
C26 C 0.5981(7) 0.2832(4) -0.2679(2) 0.062(2) Uani 1 1 d . . .
H26A H 0.6631 0.2594 -0.2793 0.075 Uiso 1 1 calc R . .
C25 C 0.5958(8) 0.3521(4) -0.2680(3) 0.087(3) Uani 1 1 d . . .
H25A H 0.6593 0.3754 -0.2804 0.105 Uiso 1 1 calc R . .
C24 C 0.5000 0.3867(6) -0.2500 0.099(5) Uani 1 2 d S . .
H24A H 0.5000 0.4330 -0.2500 0.118 Uiso 1 2 calc SR . .
O30 O 0.6044(8) 0.1502(3) -0.2491(2) 0.129(3) Uani 1 1 d . . .
H124 H 0.944(9) -0.125(6) 0.235(3) 0.04(4) Uiso 0.50 1 d PD . .
H121 H 1.068(11) -0.082(7) 0.239(5) 0.07(5) Uiso 0.50 1 d PD . .
H123 H 1.0000 -0.1464(11) 0.2500 0.18(9) Uiso 1 2 d SD . .
H122 H 0.96(2) -0.070(6) 0.235(5) 0.11(7) Uiso 0.50 1 d PD . .
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'
Cr Cr 0.3209 0.6236 '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
_geom_angle_publ_flag
O3 Cr1 O3 96.6(2) . 2_754 ?
O3 Cr1 O1 89.05(16) . . ?
O3 Cr1 O1 82.56(16) 2_754 . ?
O3 Cr1 O1 82.56(16) . 2_754 ?
O3 Cr1 O1 89.05(16) 2_754 2_754 ?
O1 Cr1 O1 167.4(2) . 2_754 ?
O3 Cr1 O2 171.96(18) . 2_754 ?
O3 Cr1 O2 91.03(17) 2_754 2_754 ?
O1 Cr1 O2 94.36(17) . 2_754 ?
O1 Cr1 O2 95.19(17) 2_754 2_754 ?
O3 Cr1 O2 91.03(17) . . ?
O3 Cr1 O2 171.96(18) 2_754 . ?
O1 Cr1 O2 95.19(17) . . ?
O1 Cr1 O2 94.36(16) 2_754 . ?
O2 Cr1 O2 81.4(3) 2_754 . ?
C7 S8 C9 94.8(3) . . ?
C5 S7 C8 95.0(3) . . ?
C7 S6 C6 95.0(3) . . ?
C15 S16 C19 95.3(3) . . ?
C5 S5 C10 95.3(3) . . ?
C17 S15 C16 95.8(3) . . ?
C17 S14 C20 95.5(3) . . ?
C15 S13 C18 94.9(3) . . ?
C8 S4 C1 99.1(4) . . ?
C6 S3 C3 101.8(3) . . ?
C16 S12 C13 102.0(3) . . ?
C20 S11 C12 101.8(3) . . ?
C9 S2 C4 102.2(3) . . ?
C19 S10 C11 99.0(3) . . ?
C10 S1 C2 101.8(4) . . ?
C18 S9 C14 102.0(3) . . ?
C16 C20 S11 129.1(5) . . ?
C16 C20 S14 116.8(4) . . ?
S11 C20 S14 114.1(3) . . ?
C8 C10 S1 127.4(4) . . ?
C8 C10 S5 116.7(4) . . ?
S1 C10 S5 115.8(3) . . ?
C18 C19 S10 127.9(5) . . ?
C18 C19 S16 117.0(4) . . ?
S10 C19 S16 115.1(3) . . ?
C6 C9 S8 117.4(4) . . ?
C6 C9 S2 127.6(4) . . ?
S8 C9 S2 115.0(3) . . ?
C19 C18 S9 128.9(5) . . ?
C19 C18 S13 116.9(4) . . ?
S9 C18 S13 114.2(3) . . ?
C10 C8 S4 126.3(4) . . ?
C10 C8 S7 117.5(4) . . ?
S4 C8 S7 116.1(3) . . ?
C15 C17 S15 121.7(4) . . ?
C15 C17 S14 123.4(4) . . ?
S15 C17 S14 114.9(3) . . ?
C20 C16 S15 117.0(4) . . ?
C20 C16 S12 127.6(4) . . ?
S15 C16 S12 115.4(3) . . ?
C5 C7 S6 122.1(4) . . ?
C5 C7 S8 122.2(4) . . ?
S6 C7 S8 115.7(3) . . ?
C9 C6 S3 128.7(4) . . ?
C9 C6 S6 117.0(4) . . ?
S3 C6 S6 114.4(3) . . ?
C7 C5 S5 122.0(4) . . ?
C7 C5 S7 122.8(4) . . ?
S5 C5 S7 115.2(3) . . ?
C17 C15 S16 121.8(4) . . ?
C17 C15 S13 122.3(4) . . ?
S16 C15 S13 115.9(3) . . ?
C11 C14 S9 114.4(5) . . ?
C12 C13 S12 114.5(4) . . ?
C3 C4 S2 121.4(6) . . ?
C13 C12 S11 114.3(4) . . ?
C4 C3 S3 118.7(6) . . ?
C1 C2 S1 125.7(7) . . ?
C14 C11 S10 113.2(5) . . ?
C2 C1 S4 124.7(6) . . ?
C22 O1 Cr1 113.3(4) . . ?
C21 O2 Cr1 115.1(4) . . ?
C23 O3 Cr1 114.8(4) . . ?
O4 C23 O3 125.7(6) . . ?
O4 C23 C22 120.6(5) . 2_754 ?
O3 C23 C22 113.7(5) . 2_754 ?
C26 C27 C26 124.9(10) . 2_654 ?
C26 C27 N1 117.6(5) . . ?
C26 C27 N1 117.6(5) 2_654 . ?
O5 C22 O1 125.7(6) . . ?
O5 C22 C23 119.6(6) . 2_754 ?
O1 C22 C23 114.7(5) . 2_754 ?
O6 C21 O2 125.7(6) . . ?
O6 C21 C21 120.2(4) . 2_754 ?
O2 C21 C21 114.2(3) . 2_754 ?
O30 N1 O30 123.7(14) 2_654 . ?
O30 N1 C27 118.1(7) 2_654 . ?
O30 N1 C27 118.1(7) . . ?
C27 C26 C25 116.9(9) . . ?
C24 C25 C26 120.9(10) . . ?
C25 C24 C25 119.7(12) 2_654 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cr1 O3 1.965(4) . ?
Cr1 O3 1.965(4) 2_754 ?
Cr1 O1 1.977(4) . ?
Cr1 O1 1.977(4) 2_754 ?
Cr1 O2 1.984(4) 2_754 ?
Cr1 O2 1.984(4) . ?
S8 C7 1.733(6) . ?
S8 C9 1.739(6) . ?
S7 C5 1.740(5) . ?
S7 C8 1.751(6) . ?
S6 C7 1.730(6) . ?
S6 C6 1.742(5) . ?
S16 C15 1.724(6) . ?
S16 C19 1.746(6) . ?
S5 C5 1.735(6) . ?
S5 C10 1.758(5) . ?
S15 C17 1.741(6) . ?
S15 C16 1.740(6) . ?
S14 C17 1.743(5) . ?
S14 C20 1.749(6) . ?
S13 C15 1.732(6) . ?
S13 C18 1.752(6) . ?
S4 C8 1.739(6) . ?
S4 C1 1.780(9) . ?
S3 C6 1.739(6) . ?
S3 C3 1.790(7) . ?
S12 C16 1.746(6) . ?
S12 C13 1.793(6) . ?
S11 C20 1.738(6) . ?
S11 C12 1.816(6) . ?
S2 C9 1.764(6) . ?
S2 C4 1.767(7) . ?
S10 C19 1.737(6) . ?
S10 C11 1.782(7) . ?
S1 C10 1.741(6) . ?
S1 C2 1.768(8) . ?
S9 C18 1.740(6) . ?
S9 C14 1.805(7) . ?
C20 C16 1.360(8) . ?
C10 C8 1.335(7) . ?
C19 C18 1.346(8) . ?
C9 C6 1.342(7) . ?
C17 C15 1.379(7) . ?
C7 C5 1.373(7) . ?
C14 C11 1.503(9) . ?
C13 C12 1.514(8) . ?
C4 C3 1.399(9) . ?
C2 C1 1.328(10) . ?
O1 C22 1.288(7) . ?
O2 C21 1.283(7) . ?
O3 C23 1.281(6) . ?
O4 C23 1.230(6) . ?
O5 C22 1.232(7) . ?
C23 C22 1.540(8) 2_754 ?
C27 C26 1.371(8) . ?
C27 C26 1.371(8) 2_654 ?
C27 N1 1.462(14) . ?
O6 C21 1.227(7) . ?
C22 C23 1.540(8) 2_754 ?
C21 C21 1.537(13) 2_754 ?
N1 O30 1.219(7) 2_654 ?
N1 O30 1.219(7) . ?
C26 C25 1.385(10) . ?
C25 C24 1.386(10) . ?
C24 C25 1.386(10) 2_654 ?
