#------------------------------------------------------------------------------
#$Date: 2016-02-16 02:10:39 +0100 (mar 16 de feb de 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/36/7013610.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_7013610
loop_
_publ_author_name
'Zangrando, Ennio'
'Serli, Barbara'
'Yellowlees, Lesley'
'Alessio, Enzo'
_publ_section_title
;
 The first examples of four and five O-bonded dmso ligands on a
 ruthenium centre
;
_journal_issue                   23
_journal_name_full               'Dalton Transactions'
_journal_page_first              4391
_journal_page_last               4392
_journal_paper_doi               10.1039/b310510e
_journal_year                    2003
_chemical_formula_moiety
'[(C2 H6 S O)4 (N O 1+) (Cl -1) Ru 2+] 2(C F3 S O3 1-) (0.5 C H2 Cl2)'
_chemical_formula_sum            'C10.5 H25 Cl2 F6 N O11 Ru S6'
_chemical_formula_weight         819.65
_chemical_name_common
;
cis-nitrosyl-chloride-tetra-dimethylsulfoxide,O-ruthenium(ii)
bistriflate dichloromethane solvated
;
_chemical_name_systematic
;
cis-nitrosyl-chloride-tetra-dimethylsulfoxide,O-ruthenium(II)
bistriflate dichloromethane solvated
;
_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                110.87(3)
_cell_angle_beta                 89.77(2)
_cell_angle_gamma                104.79(3)
_cell_formula_units_Z            2
_cell_length_a                   8.540(3)
_cell_length_b                   13.012(4)
_cell_length_c                   15.407(4)
_cell_measurement_temperature    150(2)
_cell_volume                     1539.6(9)
_computing_cell_refinement       'Mosflm (Acta Cryst. D50, 760, 1994)'
_computing_data_collection       'Nonius Xpress'
_computing_data_reduction        'Scala (Acta Cryst. D50, 760, 1994)'
_computing_molecular_graphics    'Ortep3/windows (Farrugia,1997)'
_computing_publication_material  'Wingx 1.64.04 (Farrugia, 1999)'
_computing_structure_refinement  'SHELX97 (Sheldrick, 1998)'
_computing_structure_solution    'SHELX97 (Sheldrick, 1998)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.915
_diffrn_measured_fraction_theta_max 0.915
_diffrn_measurement_device_type  'image plate dip1030'
_diffrn_measurement_method       'laser scanner'
_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  0.0435
_diffrn_reflns_av_sigmaI/netI    0.0588
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10297
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         2.73
_exptl_absorpt_coefficient_mu    1.171
_exptl_absorpt_correction_T_max  0.8130
_exptl_absorpt_correction_T_min  0.5332
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56
Cubic fit to sin(theta)/lambda - 24 parameters
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.768
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             822
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.585
_refine_diff_density_min         -0.810
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         6218
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0493
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0758P)²+2.5613P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1396
_refine_ls_wR_factor_ref         0.1462
_reflns_number_gt                5390
_reflns_number_total             6219
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b310510e.txt
_cod_data_source_block           2
_cod_original_cell_volume        1539.5(8)
_cod_original_formula_sum        'C10.50 H25 Cl2 F6 N O11 Ru S6'
_cod_database_code               7013610
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
Ru Ru 0.49394(4) 0.21917(3) 0.30540(2) 0.03128(13) Uani 1 1 d . . .
Cl1 Cl 0.62520(14) 0.25993(10) 0.18223(8) 0.0424(3) Uani 1 1 d . . .
N1 N 0.6506(4) 0.1655(3) 0.3252(3) 0.0374(8) Uani 1 1 d . . .
O5 O 0.7520(5) 0.1219(4) 0.3252(3) 0.0597(10) Uani 1 1 d . . .
S1 S 0.24261(14) 0.24640(10) 0.17319(8) 0.0416(3) Uani 1 1 d . . .
S2 S 0.74303(13) 0.46487(9) 0.39975(8) 0.0381(2) Uani 1 1 d . . .
S3 S 0.41866(14) -0.01867(10) 0.13622(9) 0.0462(3) Uani 1 1 d . . .
S4 S 0.31211(13) 0.07606(9) 0.41708(8) 0.0360(2) Uani 1 1 d . . .
O1 O 0.3120(4) 0.2793(3) 0.2757(2) 0.0390(7) Uani 1 1 d . . .
O2 O 0.5774(4) 0.3803(2) 0.4003(2) 0.0401(7) Uani 1 1 d . . .
O3 O 0.3502(4) 0.0630(3) 0.2186(2) 0.0393(7) Uani 1 1 d . . .
O4 O 0.3600(4) 0.1970(2) 0.4112(2) 0.0373(6) Uani 1 1 d . . .
C1 C 0.0329(6) 0.2369(5) 0.1849(4) 0.0567(13) Uani 1 1 d . . .
H1A H -0.0223 0.1625 0.1879 0.085 Uiso 1 1 calc R . .
H1B H -0.0158 0.2449 0.1310 0.085 Uiso 1 1 calc R . .
H1C H 0.0213 0.2979 0.2422 0.085 Uiso 1 1 calc R . .
C2 C 0.3047(8) 0.3760(5) 0.1527(4) 0.0556(13) Uani 1 1 d . . .
H2A H 0.2766 0.4372 0.2038 0.083 Uiso 1 1 calc R . .
H2B H 0.2491 0.3666 0.0937 0.083 Uiso 1 1 calc R . .
H2C H 0.4226 0.3960 0.1492 0.083 Uiso 1 1 calc R . .
C3 C 0.6884(8) 0.5574(5) 0.3502(5) 0.0642(16) Uani 1 1 d . . .
H3A H 0.6634 0.5176 0.2826 0.096 Uiso 1 1 calc R . .
H3B H 0.7793 0.6261 0.3632 0.096 Uiso 1 1 calc R . .
H3C H 0.5926 0.5793 0.3777 0.096 Uiso 1 1 calc R . .
C4 C 0.7787(7) 0.5578(4) 0.5185(4) 0.0516(12) Uani 1 1 d . . .
H4A H 0.6801 0.5814 0.5387 0.077 Uiso 1 1 calc R . .
H4B H 0.8683 0.6255 0.5256 0.077 Uiso 1 1 calc R . .
H4C H 0.8074 0.5181 0.5568 0.077 Uiso 1 1 calc R . .
C5 C 0.2954(8) -0.0335(6) 0.0365(4) 0.0636(16) Uani 1 1 d . . .
H5A H 0.1810 -0.0469 0.0494 0.095 Uiso 1 1 calc R . .
H5B H 0.3084 -0.0983 -0.0174 0.095 Uiso 1 1 calc R . .
H5C H 0.3294 0.0365 0.0228 0.095 Uiso 1 1 calc R . .
C6 C 0.3294(8) -0.1523(5) 0.1454(6) 0.0706(19) Uani 1 1 d . . .
H6A H 0.3678 -0.1513 0.2056 0.106 Uiso 1 1 calc R . .
H6B H 0.3602 -0.2126 0.0948 0.106 Uiso 1 1 calc R . .
H6C H 0.2107 -0.1672 0.1408 0.106 Uiso 1 1 calc R . .
C7 C 0.1029(6) 0.0224(4) 0.3788(4) 0.0465(11) Uani 1 1 d . . .
H7A H 0.0453 0.0777 0.4149 0.070 Uiso 1 1 calc R . .
H7B H 0.0597 -0.0501 0.3878 0.070 Uiso 1 1 calc R . .
H7C H 0.0873 0.0099 0.3125 0.070 Uiso 1 1 calc R . .
C8 C 0.3023(6) 0.1102(4) 0.5389(3) 0.0412(9) Uani 1 1 d . . .
H8A H 0.4103 0.1539 0.5718 0.062 Uiso 1 1 calc R . .
H8B H 0.2664 0.0395 0.5515 0.062 Uiso 1 1 calc R . .
H8C H 0.2249 0.1559 0.5607 0.062 Uiso 1 1 calc R . .
S10 S 0.81466(18) 0.84297(13) 0.10104(9) 0.0526(3) Uani 1 1 d . . .
O10 O 0.9199(6) 0.7810(5) 0.0447(3) 0.0826(15) Uani 1 1 d . . .
O11 O 0.6632(5) 0.8284(4) 0.0517(3) 0.0644(11) Uani 1 1 d . . .
O12 O 0.8953(9) 0.9560(4) 0.1616(4) 0.0980(18) Uani 1 1 d . . .
C10 C 0.7521(9) 0.7685(7) 0.1804(5) 0.0727(18) Uani 1 1 d . . .
F1 F 0.6664(8) 0.6630(5) 0.1363(5) 0.129(2) Uani 1 1 d . . .
F2 F 0.8805(6) 0.7654(5) 0.2275(4) 0.0985(15) Uani 1 1 d . . .
F3 F 0.6620(7) 0.8195(7) 0.2420(4) 0.132(2) Uani 1 1 d . . .
S20 S 0.83022(14) 0.24642(10) 0.55411(9) 0.0444(3) Uani 1 1 d . . .
O20 O 0.6904(5) 0.1514(4) 0.5278(4) 0.0713(13) Uani 1 1 d . . .
O21 O 0.9765(5) 0.2201(4) 0.5678(3) 0.0576(9) Uani 1 1 d . . .
O22 O 0.8441(6) 0.3194(4) 0.5028(3) 0.0683(11) Uani 1 1 d . . .
C20 C 0.7980(8) 0.3338(6) 0.6690(5) 0.0679(16) Uani 1 1 d . . .
F4 F 0.7904(9) 0.2818(6) 0.7278(4) 0.131(2) Uani 1 1 d . . .
F5 F 0.9125(6) 0.4328(4) 0.7009(3) 0.0929(14) Uani 1 1 d . . .
F6 F 0.6560(6) 0.3599(4) 0.6688(5) 0.117(2) Uani 1 1 d . . .
C30 C 1.0527(13) 0.5425(9) 0.0954(9) 0.058(3) Uani 0.50 1 d PDU . .
H30A H 1.0874 0.5720 0.1630 0.070 Uiso 0.50 1 calc PR . .
H30B H 1.0103 0.6020 0.0856 0.070 Uiso 0.50 1 calc PR . .
Cl2 Cl 0.9017(10) 0.4464(6) 0.0834(6) 0.165(3) Uani 0.50 1 d PDU . .
Cl3 Cl 1.2305(12) 0.5534(5) 0.0457(6) 0.175(3) Uani 0.50 1 d PDU . .
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'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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 Ru O2 98.32(16) . . ?
N1 Ru O1 177.31(14) . . ?
O2 Ru O1 83.36(13) . . ?
N1 Ru O4 97.95(15) . . ?
O2 Ru O4 82.26(12) . . ?
O1 Ru O4 84.34(13) . . ?
N1 Ru O3 94.44(16) . . ?
O2 Ru O3 164.73(12) . . ?
O1 Ru O3 84.21(13) . . ?
O4 Ru O3 87.72(12) . . ?
N1 Ru Cl1 89.59(13) . . ?
O2 Ru Cl1 95.04(10) . . ?
O1 Ru Cl1 88.16(10) . . ?
O4 Ru Cl1 172.27(9) . . ?
O3 Ru Cl1 93.39(10) . . ?
O5 N1 Ru 170.5(4) . . ?
O1 S1 C2 104.1(2) . . ?
O1 S1 C1 102.2(2) . . ?
C2 S1 C1 100.0(3) . . ?
O2 S2 C4 100.9(2) . . ?
O2 S2 C3 103.9(2) . . ?
C4 S2 C3 98.9(3) . . ?
O3 S3 C6 101.5(3) . . ?
O3 S3 C5 102.8(2) . . ?
C6 S3 C5 99.5(3) . . ?
O4 S4 C7 104.3(2) . . ?
O4 S4 C8 101.5(2) . . ?
C7 S4 C8 99.8(2) . . ?
S1 O1 Ru 121.25(17) . . ?
S2 O2 Ru 124.51(18) . . ?
S3 O3 Ru 121.75(17) . . ?
S4 O4 Ru 118.02(17) . . ?
O12 S10 O11 116.3(3) . . ?
O12 S10 O10 114.5(4) . . ?
O11 S10 O10 114.1(3) . . ?
O12 S10 C10 103.4(4) . . ?
O11 S10 C10 103.0(3) . . ?
O10 S10 C10 103.1(4) . . ?
F1 C10 F3 107.4(7) . . ?
F1 C10 F2 107.5(7) . . ?
F3 C10 F2 107.6(6) . . ?
F1 C10 S10 111.8(5) . . ?
F3 C10 S10 111.0(6) . . ?
F2 C10 S10 111.2(5) . . ?
O21 S20 O20 114.3(3) . . ?
O21 S20 O22 113.7(3) . . ?
O20 S20 O22 115.8(3) . . ?
O21 S20 C20 103.8(3) . . ?
O20 S20 C20 103.6(3) . . ?
O22 S20 C20 103.5(3) . . ?
F4 C20 F5 110.1(7) . . ?
F4 C20 F6 105.7(6) . . ?
F5 C20 F6 106.2(6) . . ?
F4 C20 S20 112.2(5) . . ?
F5 C20 S20 111.3(4) . . ?
F6 C20 S20 111.1(5) . . ?
Cl2 C30 Cl3 134.5(9) . . ?
C30 Cl2 Cl3 99.7(6) . 2_765 ?
C30 Cl3 Cl2 89.1(6) . 2_765 ?
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
Ru N1 1.733(4) . ?
Ru O2 2.025(3) . ?
Ru O1 2.029(3) . ?
Ru O4 2.050(3) . ?
Ru O3 2.056(3) . ?
Ru Cl1 2.3527(12) . ?
N1 O5 1.149(5) . ?
S1 O1 1.557(3) . ?
S1 C2 1.774(6) . ?
S1 C1 1.776(5) . ?
S2 O2 1.557(3) . ?
S2 C4 1.773(5) . ?
S2 C3 1.787(5) . ?
S3 O3 1.559(3) . ?
S3 C6 1.767(6) . ?
S3 C5 1.790(7) . ?
S4 O4 1.557(3) . ?
S4 C7 1.763(5) . ?
S4 C8 1.775(5) . ?
S10 O12 1.421(5) . ?
S10 O11 1.438(4) . ?
S10 O10 1.441(5) . ?
S10 C10 1.816(7) . ?
C10 F1 1.307(9) . ?
C10 F3 1.318(9) . ?
C10 F2 1.334(8) . ?
S20 O21 1.412(4) . ?
S20 O20 1.418(4) . ?
S20 O22 1.419(4) . ?
S20 C20 1.795(7) . ?
C20 F4 1.303(9) . ?
C20 F5 1.329(8) . ?
C20 F6 1.341(8) . ?
C30 Cl2 1.508(12) . ?
C30 Cl3 1.694(12) . ?
Cl2 Cl3 2.293(12) 2_765 ?
Cl3 Cl2 2.293(12) 2_765 ?
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 Ru N1 O5 -142(2) . . . . ?
O1 Ru N1 O5 -13(5) . . . . ?
O4 Ru N1 O5 135(2) . . . . ?
O3 Ru N1 O5 47(2) . . . . ?
Cl1 Ru N1 O5 -47(2) . . . . ?
C2 S1 O1 Ru -111.9(3) . . . . ?
C1 S1 O1 Ru 144.4(3) . . . . ?
N1 Ru O1 S1 10(3) . . . . ?
O2 Ru O1 S1 139.2(2) . . . . ?
O4 Ru O1 S1 -137.9(2) . . . . ?
O3 Ru O1 S1 -49.6(2) . . . . ?
Cl1 Ru O1 S1 43.9(2) . . . . ?
C4 S2 O2 Ru -156.9(3) . . . . ?
C3 S2 O2 Ru 101.0(3) . . . . ?
N1 Ru O2 S2 60.1(3) . . . . ?
O1 Ru O2 S2 -117.8(3) . . . . ?
O4 Ru O2 S2 157.0(3) . . . . ?
O3 Ru O2 S2 -153.5(4) . . . . ?
Cl1 Ru O2 S2 -30.3(2) . . . . ?
C6 S3 O3 Ru 137.7(3) . . . . ?
C5 S3 O3 Ru -119.7(3) . . . . ?
N1 Ru O3 S3 -48.9(3) . . . . ?
O2 Ru O3 S3 164.5(4) . . . . ?
O1 Ru O3 S3 128.8(2) . . . . ?
O4 Ru O3 S3 -146.7(2) . . . . ?
Cl1 Ru O3 S3 41.0(2) . . . . ?
C7 S4 O4 Ru -106.3(2) . . . . ?
C8 S4 O4 Ru 150.3(2) . . . . ?
N1 Ru O4 S4 -53.2(2) . . . . ?
O2 Ru O4 S4 -150.6(2) . . . . ?
O1 Ru O4 S4 125.4(2) . . . . ?
O3 Ru O4 S4 41.0(2) . . . . ?
Cl1 Ru O4 S4 139.4(5) . . . . ?
O12 S10 C10 F1 176.3(6) . . . . ?
O11 S10 C10 F1 54.8(7) . . . . ?
O10 S10 C10 F1 -64.2(7) . . . . ?
O12 S10 C10 F3 56.3(6) . . . . ?
O11 S10 C10 F3 -65.2(6) . . . . ?
O10 S10 C10 F3 175.9(5) . . . . ?
O12 S10 C10 F2 -63.5(6) . . . . ?
O11 S10 C10 F2 175.0(5) . . . . ?
O10 S10 C10 F2 56.1(6) . . . . ?
O21 S20 C20 F4 -57.7(6) . . . . ?
O20 S20 C20 F4 62.0(6) . . . . ?
O22 S20 C20 F4 -176.8(6) . . . . ?
O21 S20 C20 F5 66.1(6) . . . . ?
O20 S20 C20 F5 -174.2(5) . . . . ?
O22 S20 C20 F5 -53.0(6) . . . . ?
O21 S20 C20 F6 -175.8(5) . . . . ?
O20 S20 C20 F6 -56.1(6) . . . . ?
O22 S20 C20 F6 65.1(6) . . . . ?
Cl3 C30 Cl2 Cl3 -81.6(11) . . . 2_765 ?
Cl2 C30 Cl3 Cl2 77.2(11) . . . 2_765 ?
