#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/37/7203726.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_7203726
loop_
_publ_author_name
'Simonov, Sergey V.'
'Shevyakova, Irina Yu.'
'Zorina, Leokadiya V.'
'Khasanov, Salavat S.'
'Buravov, Lev I.'
'Emel'yanov, Vyacheslav A.'
'Canadell, Enric'
'Shibaeva, Rimma P.'
'Yagubskii, Eduard B.'
_publ_section_title
;
 Variety of molecular conducting layers in the family of radical cation
 salts based on BEDT-TTF with the metal mononitrosyl complex
 [OsNOCl5]2--
;
_journal_issue                   25
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              2476
_journal_paper_doi               10.1039/b419134j
_journal_volume                  15
_journal_year                    2005
_chemical_formula_moiety         '(C10 H8 S8)2, OsNOCl5'
_chemical_formula_sum            'C20 H16 Cl5 N O Os S8'
_chemical_formula_weight         1166.74
_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                110.410(4)
_cell_angle_beta                 98.410(4)
_cell_angle_gamma                103.834(4)
_cell_formula_units_Z            1
_cell_length_a                   8.7249(3)
_cell_length_b                   10.3380(5)
_cell_length_c                   11.0927(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      18
_cell_volume                     881.06(8)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      291(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       'non-profiled omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           Mok\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0212
_diffrn_reflns_av_sigmaI/netI    0.0292
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10214
_diffrn_reflns_theta_full        30.01
_diffrn_reflns_theta_max         30.01
_diffrn_reflns_theta_min         2.02
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  9000
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.971
_exptl_absorpt_correction_T_max  0.6919
_exptl_absorpt_correction_T_min  0.3696
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
aplication absorption correction procedure based on psi-scans data
using WinGX facilities
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.199
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.411
_refine_diff_density_min         -1.130
_refine_diff_density_rms         0.121
_refine_ls_extinction_coef       0.0031(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         5134
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0258
_refine_ls_R_factor_gt           0.0247
_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)+(0.0392P)²+0.1655P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0630
_refine_ls_wR_factor_ref         0.0633
_reflns_number_gt                5031
_reflns_number_total             5134
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b419134j.txt
_cod_data_source_block           beta-(BEDT-TTF)2[OsNOCl5]
_cod_original_cell_volume        881.06(7)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C20 H16 Cl5 N1 O1 Os1 S8'
_cod_database_code               7203726
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Os1 Os 0.0000 0.0000 0.0000 0.02431(5) Uani 1 2 d S . .
Cl1 Cl 0.18543(9) 0.02682(8) 0.19303(7) 0.04111(15) Uani 1 1 d . . .
Cl2 Cl 0.18007(10) 0.21811(8) 0.00991(8) 0.04422(15) Uani 1 1 d . . .
Cl3 Cl 0.1380(3) -0.1313(3) -0.1374(3) 0.0286(6) Uani 0.50 1 d P . .
O1 O -0.1628(16) 0.1521(14) 0.1640(12) 0.050(2) Uani 0.50 1 d P . .
N1 N -0.1183(17) 0.1034(11) 0.1057(10) 0.043(3) Uani 0.50 1 d P . .
S1 S 0.28993(9) 0.65808(8) 0.59243(7) 0.03507(13) Uani 1 1 d . . .
S2 S 0.18747(8) 0.39091(7) 0.35347(6) 0.03203(12) Uani 1 1 d . . .
S3 S 0.47699(9) 0.51445(7) 0.75258(6) 0.03436(13) Uani 1 1 d . . .
S4 S 0.36957(8) 0.24005(7) 0.52058(6) 0.03128(12) Uani 1 1 d . . .
S5 S 0.08428(12) 0.80232(9) 0.48862(10) 0.05029(19) Uani 1 1 d . . .
S6 S -0.02643(10) 0.49423(9) 0.19812(9) 0.04730(18) Uani 1 1 d . . .
S7 S 0.63720(10) 0.40622(9) 0.93387(7) 0.04026(15) Uani 1 1 d . . .
S8 S 0.51612(10) 0.08493(8) 0.66568(7) 0.03971(15) Uani 1 1 d . . .
C1 C 0.2930(3) 0.4821(3) 0.5182(2) 0.0280(4) Uani 1 1 d . . .
C2 C 0.3722(3) 0.4183(3) 0.5880(2) 0.0281(4) Uani 1 1 d . . .
C3 C 0.1488(3) 0.6497(3) 0.4591(3) 0.0336(5) Uani 1 1 d . . .
C4 C 0.1032(3) 0.5257(3) 0.3481(3) 0.0330(5) Uani 1 1 d . . .
C5 C 0.5286(3) 0.3707(3) 0.7752(2) 0.0291(4) Uani 1 1 d . . .
C6 C 0.4809(3) 0.2441(3) 0.6661(2) 0.0300(4) Uani 1 1 d . . .
C7 C -0.0146(5) 0.7803(4) 0.3224(4) 0.0519(8) Uani 1 1 d . . .
H7A H -0.1318 0.7453 0.3095 0.062 Uiso 1 1 calc R . .
H7B H 0.0118 0.8750 0.3182 0.062 Uiso 1 1 calc R . .
C8 C 0.0311(4) 0.6790(4) 0.2104(4) 0.0451(7) Uani 1 1 d . . .
H8A H 0.1482 0.7135 0.2224 0.054 Uiso 1 1 calc R . .
H8B H -0.0210 0.6804 0.1276 0.054 Uiso 1 1 calc R . .
C9 C 0.6047(5) 0.2277(4) 0.9390(3) 0.0513(8) Uani 1 1 d . . .
H9A H 0.7077 0.2071 0.9432 0.062 Uiso 1 1 calc R . .
H9B H 0.5744 0.2322 1.0208 0.062 Uiso 1 1 calc R . .
C10 C 0.4786(4) 0.1031(4) 0.8259(4) 0.0464(7) Uani 1 1 d . . .
H10A H 0.3724 0.1163 0.8276 0.056 Uiso 1 1 calc R . .
H10B H 0.4759 0.0140 0.8377 0.056 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'
Cl Cl 0.1484 0.1585 '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'
Os Os -1.2165 7.6030 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Os1 N1 180.0(6) 2 . ?
N1 Os1 Cl3 177.9(4) 2 2 ?
N1 Os1 Cl3 2.1(4) . 2 ?
N1 Os1 Cl3 2.1(4) 2 . ?
N1 Os1 Cl3 177.9(4) . . ?
Cl3 Os1 Cl3 180.00(12) 2 . ?
N1 Os1 Cl1 90.9(4) 2 2 ?
N1 Os1 Cl1 89.1(4) . 2 ?
Cl3 Os1 Cl1 91.04(7) 2 2 ?
Cl3 Os1 Cl1 88.96(7) . 2 ?
N1 Os1 Cl1 89.1(4) 2 . ?
N1 Os1 Cl1 90.9(4) . . ?
Cl3 Os1 Cl1 88.96(7) 2 . ?
Cl3 Os1 Cl1 91.04(7) . . ?
Cl1 Os1 Cl1 180.0 2 . ?
N1 Os1 Cl2 88.2(4) 2 . ?
N1 Os1 Cl2 91.8(4) . . ?
Cl3 Os1 Cl2 91.09(8) 2 . ?
Cl3 Os1 Cl2 88.91(8) . . ?
Cl1 Os1 Cl2 92.17(3) 2 . ?
Cl1 Os1 Cl2 87.83(3) . . ?
N1 Os1 Cl2 91.8(4) 2 2 ?
N1 Os1 Cl2 88.2(4) . 2 ?
Cl3 Os1 Cl2 88.91(8) 2 2 ?
Cl3 Os1 Cl2 91.09(8) . 2 ?
Cl1 Os1 Cl2 87.83(3) 2 2 ?
Cl1 Os1 Cl2 92.17(3) . 2 ?
Cl2 Os1 Cl2 180.00(3) . 2 ?
N1 Cl3 Os1 8.8(18) 2 . ?
Cl3 O1 N1 4.4(11) 2 . ?
Cl3 N1 O1 4.1(11) 2 . ?
Cl3 N1 Os1 169(2) 2 . ?
O1 N1 Os1 172(2) . . ?
C1 S1 C3 95.71(12) . . ?
C1 S2 C4 95.30(12) . . ?
C2 S3 C5 96.04(12) . . ?
C2 S4 C6 95.40(12) . . ?
C3 S5 C7 103.58(16) . . ?
C4 S6 C8 97.43(15) . . ?
C5 S7 C9 104.42(14) . . ?
C6 S8 C10 96.90(14) . . ?
C2 C1 S2 122.7(2) . . ?
C2 C1 S1 121.98(19) . . ?
S2 C1 S1 115.25(14) . . ?
C1 C2 S4 123.65(19) . . ?
C1 C2 S3 121.0(2) . . ?
S4 C2 S3 115.36(14) . . ?
C4 C3 S5 129.0(2) . . ?
C4 C3 S1 115.9(2) . . ?
S5 C3 S1 115.09(17) . . ?
C3 C4 S2 117.27(19) . . ?
C3 C4 S6 125.0(2) . . ?
S2 C4 S6 117.67(16) . . ?
C6 C5 S3 115.95(18) . . ?
C6 C5 S7 127.5(2) . . ?
S3 C5 S7 116.51(14) . . ?
C5 C6 S4 117.19(19) . . ?
C5 C6 S8 124.06(19) . . ?
S4 C6 S8 118.68(15) . . ?
C8 C7 S5 115.3(2) . . ?
C7 C8 S6 113.2(2) . . ?
C10 C9 S7 116.6(2) . . ?
C9 C10 S8 113.0(2) . . ?
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
Os1 N1 1.895(11) 2 ?
Os1 N1 1.895(11) . ?
Os1 Cl3 2.343(2) 2 ?
Os1 Cl3 2.343(2) . ?
Os1 Cl1 2.3743(6) 2 ?
Os1 Cl1 2.3743(6) . ?
Os1 Cl2 2.3763(8) . ?
Os1 Cl2 2.3763(8) 2 ?
Cl3 N1 0.455(9) 2 ?
O1 Cl3 0.421(8) 2 ?
O1 N1 0.873(12) . ?
N1 Cl3 0.455(9) 2 ?
S1 C1 1.724(3) . ?
S1 C3 1.743(3) . ?
S2 C1 1.723(2) . ?
S2 C4 1.738(3) . ?
S3 C2 1.723(2) . ?
S3 C5 1.738(3) . ?
S4 C2 1.723(3) . ?
S4 C6 1.740(2) . ?
S5 C3 1.741(3) . ?
S5 C7 1.828(4) . ?
S6 C4 1.746(3) . ?
S6 C8 1.805(3) . ?
S7 C5 1.740(2) . ?
S7 C9 1.822(4) . ?
S8 C6 1.743(3) . ?
S8 C10 1.808(3) . ?
C1 C2 1.389(3) . ?
C3 C4 1.353(4) . ?
C5 C6 1.356(3) . ?
C7 C8 1.496(5) . ?
C9 C10 1.495(5) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C7 H7B Cl1 0.97 2.77 3.572(4) 140.2 1_565
C8 H8A Cl1 0.97 3.31 3.609(3) 100.0 1_565
C8 H8B Cl2 0.97 2.56 3.455(3) 153.6 2_565
C8 H8A S7 0.97 2.93 3.647(3) 131.3 2_666
C9 H9A O1 0.97 2.84 3.405(15) 117.9 1_656
C9 H9A N1 0.97 2.83 3.570(14) 133.3 1_656
C9 H9A Cl1 0.97 2.82 3.581(4) 136.1 2_656
C9 H9A Cl3 0.97 2.81 3.468(4) 125.7 2_656
C10 H10B Cl1 0.97 3.13 3.508(3) 104.8 2_656
C10 H10A Cl3 0.97 3.05 3.530(4) 112.0 1_556
C10 H10B O1 0.97 2.85 3.373(14) 114.7 2_556
