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#$Date: 2016-03-25 11:23:56 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179788 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/84/7008496.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_7008496
loop_
_publ_author_name
'Reisner, Erwin'
'Arion, Vladimir B.'
'Rufińska, Anna'
'Chiorescu, Ion'
'Schmid, Wolfgang F.'
'Keppler, Bernhard K.'
_publ_section_title
;
 Isomeric [RuCl2(dmso)2(indazole)2] complexes: ruthenium(II)-mediated
 coupling reaction of acetonitrile with 1H-indazole.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2355
_journal_page_last               2364
_journal_paper_doi               10.1039/b503650j
_journal_year                    2005
_chemical_formula_sum            'C13 H23 Cl2 N3 O3 Ru S2'
_chemical_formula_weight         505.43
_chemical_name_common
;trans-dichlorobis(dimethylsulfoxide)amidineruthenium(ii)
monohydrate
;
_chemical_name_systematic
;
trans-dichlorobis(dimethylsulfoxide)amidineruthenium(II) monohydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 113.56(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.726(4)
_cell_length_b                   8.367(2)
_cell_length_c                   14.415(3)
_cell_measurement_temperature    120(2)
_cell_volume                     1959.7(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0135
_diffrn_reflns_av_sigmaI/netI    0.0212
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11323
_diffrn_reflns_theta_full        30.50
_diffrn_reflns_theta_max         30.50
_diffrn_reflns_theta_min         2.74
_exptl_absorpt_coefficient_mu    1.302
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.713
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.791
_refine_diff_density_min         -1.005
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         5945
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0239
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0286P)²+1.3854P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0569
_refine_ls_wR_factor_ref         0.0592
_reflns_number_gt                5337
_reflns_number_total             5945
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b503650j.txt
_cod_data_source_block           erre740b
_cod_original_cell_volume        1959.7(8)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7008496
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Ru1 Ru 0.719836(7) 0.787752(14) 0.427958(8) 0.00859(4) Uani 1 1 d . . .
Cl1 Cl 0.62189(2) 0.59310(5) 0.32564(3) 0.01554(8) Uani 1 1 d . . .
Cl2 Cl 0.82772(2) 0.96196(5) 0.53373(3) 0.01563(8) Uani 1 1 d . . .
S1 S 0.68890(2) 0.94900(4) 0.29122(3) 0.01197(7) Uani 1 1 d . . .
S2 S 0.62926(2) 0.90994(4) 0.47738(3) 0.01130(7) Uani 1 1 d . . .
O1 O 0.73212(8) 0.90397(15) 0.22461(9) 0.0191(2) Uani 1 1 d . . .
O2 O 0.58834(7) 1.06022(14) 0.42627(9) 0.0184(2) Uani 1 1 d . . .
N1 N 0.80782(7) 0.65053(15) 0.40041(9) 0.0107(2) Uani 1 1 d . . .
N2 N 0.83639(8) 0.52179(15) 0.46656(9) 0.0114(2) Uani 1 1 d . . .
N3 N 0.75708(8) 0.62016(15) 0.54325(10) 0.0117(2) Uani 1 1 d . . .
H3 H 0.7386 0.6235 0.5901 0.014 Uiso 1 1 calc R . .
C1 C 0.84202(9) 0.64103(19) 0.33485(11) 0.0127(3) Uani 1 1 d . . .
H1 H 0.8332 0.7133 0.2825 0.015 Uiso 1 1 calc R . .
C2 C 0.89461(9) 0.50480(19) 0.35491(11) 0.0131(3) Uani 1 1 d . . .
C3 C 0.94465(10) 0.4424(2) 0.30895(12) 0.0163(3) Uani 1 1 d . . .
H3A H 0.9467 0.4897 0.2516 0.020 Uiso 1 1 calc R . .
C4 C 0.99071(10) 0.3083(2) 0.35174(13) 0.0182(3) Uani 1 1 d . . .
H4 H 1.0256 0.2661 0.3239 0.022 Uiso 1 1 calc R . .
C5 C 0.98580(10) 0.2343(2) 0.43671(13) 0.0182(3) Uani 1 1 d . . .
H5 H 1.0172 0.1434 0.4633 0.022 Uiso 1 1 calc R . .
C6 C 0.93573(10) 0.29223(19) 0.48217(13) 0.0156(3) Uani 1 1 d . . .
H6 H 0.9323 0.2416 0.5378 0.019 Uiso 1 1 calc R . .
C7 C 0.89066(9) 0.43049(18) 0.44049(11) 0.0117(3) Uani 1 1 d . . .
C8 C 0.83781(11) 0.3794(2) 0.61859(12) 0.0179(3) Uani 1 1 d . . .
H8A H 0.8141 0.3898 0.6676 0.027 Uiso 1 1 calc R . .
H8B H 0.8967 0.3843 0.6521 0.027 Uiso 1 1 calc R . .
H8C H 0.8219 0.2787 0.5843 0.027 Uiso 1 1 calc R . .
C9 C 0.80792(9) 0.51186(18) 0.54357(11) 0.0122(3) Uani 1 1 d . . .
C10 C 0.58234(10) 0.9583(2) 0.21020(12) 0.0200(3) Uani 1 1 d . . .
H10A H 0.5618 0.8522 0.1897 0.030 Uiso 1 1 calc R . .
H10B H 0.5752 1.0210 0.1515 0.030 Uiso 1 1 calc R . .
H10C H 0.5526 1.0067 0.2458 0.030 Uiso 1 1 calc R . .
C11 C 0.71000(12) 1.1567(2) 0.31695(14) 0.0217(3) Uani 1 1 d . . .
H11A H 0.7669 1.1707 0.3611 0.033 Uiso 1 1 calc R . .
H11B H 0.6759 1.1983 0.3489 0.033 Uiso 1 1 calc R . .
H11C H 0.6986 1.2128 0.2547 0.033 Uiso 1 1 calc R . .
C12 C 0.54796(12) 0.7810(2) 0.47249(17) 0.0259(4) Uani 1 1 d . . .
H12A H 0.5180 0.7458 0.4041 0.039 Uiso 1 1 calc R . .
H12B H 0.5115 0.8375 0.4955 0.039 Uiso 1 1 calc R . .
H12C H 0.5705 0.6900 0.5152 0.039 Uiso 1 1 calc R . .
C13 C 0.67237(11) 0.9542(2) 0.60946(12) 0.0218(4) Uani 1 1 d . . .
H13A H 0.7184 1.0249 0.6246 0.033 Uiso 1 1 calc R . .
H13B H 0.6904 0.8570 0.6473 0.033 Uiso 1 1 calc R . .
H13C H 0.6315 1.0045 0.6276 0.033 Uiso 1 1 calc R . .
O3 O 0.61750(10) 0.37001(19) 0.51015(12) 0.0341(3) Uani 1 1 d . . .
H30A H 0.603(2) 0.268(4) 0.481(2) 0.060(9) Uiso 1 1 d . . .
H30B H 0.621(2) 0.436(4) 0.461(3) 0.069(10) Uiso 1 1 d . . .
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'
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
N3 Ru1 N1 76.03(5) . . ?
N3 Ru1 S2 95.32(4) . . ?
N1 Ru1 S2 171.35(4) . . ?
N3 Ru1 S1 171.64(4) . . ?
N1 Ru1 S1 95.79(4) . . ?
S2 Ru1 S1 92.85(2) . . ?
N3 Ru1 Cl2 89.08(5) . . ?
N1 Ru1 Cl2 89.36(4) . . ?
S2 Ru1 Cl2 90.64(2) . . ?
S1 Ru1 Cl2 92.60(3) . . ?
N3 Ru1 Cl1 87.37(5) . . ?
N1 Ru1 Cl1 85.55(4) . . ?
S2 Ru1 Cl1 94.04(2) . . ?
S1 Ru1 Cl1 90.30(3) . . ?
Cl2 Ru1 Cl1 174.373(14) . . ?
O1 S1 C10 105.73(8) . . ?
O1 S1 C11 105.07(8) . . ?
C10 S1 C11 99.96(9) . . ?
O1 S1 Ru1 113.57(5) . . ?
C10 S1 Ru1 114.86(7) . . ?
C11 S1 Ru1 116.15(6) . . ?
O2 S2 C12 105.40(9) . . ?
O2 S2 C13 105.58(8) . . ?
C12 S2 C13 99.37(10) . . ?
O2 S2 Ru1 119.69(5) . . ?
C12 S2 Ru1 112.45(6) . . ?
C13 S2 Ru1 112.18(6) . . ?
C1 N1 N2 107.44(12) . . ?
C1 N1 Ru1 139.55(11) . . ?
N2 N1 Ru1 112.83(9) . . ?
C7 N2 N1 109.93(12) . . ?
C7 N2 C9 133.75(13) . . ?
N1 N2 C9 116.30(12) . . ?
C9 N3 Ru1 118.81(11) . . ?
C9 N3 H3 120.6 . . ?
Ru1 N3 H3 120.6 . . ?
N1 C1 C2 110.76(14) . . ?
N1 C1 H1 124.6 . . ?
C2 C1 H1 124.6 . . ?
C3 C2 C7 120.77(15) . . ?
C3 C2 C1 133.37(15) . . ?
C7 C2 C1 105.85(13) . . ?
C4 C3 C2 117.68(15) . . ?
C4 C3 H3A 121.2 . . ?
C2 C3 H3A 121.2 . . ?
C3 C4 C5 121.05(15) . . ?
C3 C4 H4 119.5 . . ?
C5 C4 H4 119.5 . . ?
C6 C5 C4 122.20(15) . . ?
C6 C5 H5 118.9 . . ?
C4 C5 H5 118.9 . . ?
C5 C6 C7 116.79(15) . . ?
C5 C6 H6 121.6 . . ?
C7 C6 H6 121.6 . . ?
N2 C7 C6 132.51(14) . . ?
N2 C7 C2 106.01(13) . . ?
C6 C7 C2 121.47(14) . . ?
C9 C8 H8A 109.5 . . ?
C9 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C9 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N3 C9 N2 115.76(14) . . ?
N3 C9 C8 125.19(14) . . ?
N2 C9 C8 119.05(13) . . ?
S1 C10 H10A 109.5 . . ?
S1 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
S1 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
S1 C11 H11A 109.5 . . ?
S1 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
S1 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
S2 C12 H12A 109.5 . . ?
S2 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
S2 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
S2 C13 H13A 109.5 . . ?
S2 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
S2 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
H30A O3 H30B 106(3) . . ?
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
Ru1 N3 2.0705(13) . ?
Ru1 N1 2.0984(13) . ?
Ru1 S2 2.2460(5) . ?
Ru1 S1 2.2677(6) . ?
Ru1 Cl2 2.4033(8) . ?
Ru1 Cl1 2.4074(7) . ?
S1 O1 1.4963(12) . ?
S1 C10 1.7817(18) . ?
S1 C11 1.7851(18) . ?
S2 O2 1.4909(12) . ?
S2 C12 1.7791(18) . ?
S2 C13 1.7840(17) . ?
N1 C1 1.3135(19) . ?
N1 N2 1.3928(18) . ?
N2 C7 1.3925(19) . ?
N2 C9 1.3935(19) . ?
N3 C9 1.277(2) . ?
N3 H3 0.8600 . ?
C1 C2 1.427(2) . ?
C1 H1 0.9300 . ?
C2 C3 1.403(2) . ?
C2 C7 1.408(2) . ?
C3 C4 1.380(2) . ?
C3 H3A 0.9300 . ?
C4 C5 1.406(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.385(2) . ?
C5 H5 0.9300 . ?
C6 C7 1.398(2) . ?
C6 H6 0.9300 . ?
C8 C9 1.490(2) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
O3 H30A 0.94(3) . ?
O3 H30B 0.92(4) . ?
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
N3 Ru1 S1 O1 -7.7(3) . . . . ?
N1 Ru1 S1 O1 4.14(7) . . . . ?
S2 Ru1 S1 O1 -175.48(6) . . . . ?
Cl2 Ru1 S1 O1 93.76(6) . . . . ?
Cl1 Ru1 S1 O1 -81.42(6) . . . . ?
N3 Ru1 S1 C10 114.2(3) . . . . ?
N1 Ru1 S1 C10 126.02(8) . . . . ?
S2 Ru1 S1 C10 -53.60(7) . . . . ?
Cl2 Ru1 S1 C10 -144.36(7) . . . . ?
Cl1 Ru1 S1 C10 40.46(7) . . . . ?
N3 Ru1 S1 C11 -129.7(3) . . . . ?
N1 Ru1 S1 C11 -117.88(8) . . . . ?
S2 Ru1 S1 C11 62.50(7) . . . . ?
Cl2 Ru1 S1 C11 -28.27(7) . . . . ?
Cl1 Ru1 S1 C11 156.56(7) . . . . ?
N3 Ru1 S2 O2 172.73(7) . . . . ?
N1 Ru1 S2 O2 173.5(2) . . . . ?
S1 Ru1 S2 O2 -9.03(6) . . . . ?
Cl2 Ru1 S2 O2 83.60(7) . . . . ?
Cl1 Ru1 S2 O2 -99.54(7) . . . . ?
N3 Ru1 S2 C12 -62.78(9) . . . . ?
N1 Ru1 S2 C12 -62.0(3) . . . . ?
S1 Ru1 S2 C12 115.46(9) . . . . ?
Cl2 Ru1 S2 C12 -151.91(8) . . . . ?
Cl1 Ru1 S2 C12 24.95(8) . . . . ?
N3 Ru1 S2 C13 48.23(8) . . . . ?
N1 Ru1 S2 C13 49.0(3) . . . . ?
S1 Ru1 S2 C13 -133.53(7) . . . . ?
Cl2 Ru1 S2 C13 -40.90(7) . . . . ?
Cl1 Ru1 S2 C13 135.96(7) . . . . ?
N3 Ru1 N1 C1 178.79(17) . . . . ?
S2 Ru1 N1 C1 178.00(16) . . . . ?
S1 Ru1 N1 C1 0.55(17) . . . . ?
Cl2 Ru1 N1 C1 -92.00(17) . . . . ?
Cl1 Ru1 N1 C1 90.40(17) . . . . ?
N3 Ru1 N1 N2 4.50(9) . . . . ?
S2 Ru1 N1 N2 3.7(3) . . . . ?
S1 Ru1 N1 N2 -173.74(9) . . . . ?
Cl2 Ru1 N1 N2 93.71(9) . . . . ?
Cl1 Ru1 N1 N2 -83.89(9) . . . . ?
C1 N1 N2 C7 0.33(16) . . . . ?
Ru1 N1 N2 C7 176.45(9) . . . . ?
C1 N1 N2 C9 179.02(13) . . . . ?
Ru1 N1 N2 C9 -4.86(15) . . . . ?
N1 Ru1 N3 C9 -4.00(11) . . . . ?
S2 Ru1 N3 C9 175.89(11) . . . . ?
S1 Ru1 N3 C9 8.1(3) . . . . ?
Cl2 Ru1 N3 C9 -93.56(12) . . . . ?
Cl1 Ru1 N3 C9 82.07(12) . . . . ?
N2 N1 C1 C2 0.18(17) . . . . ?
Ru1 N1 C1 C2 -174.31(12) . . . . ?
N1 C1 C2 C3 -179.55(16) . . . . ?
N1 C1 C2 C7 -0.61(18) . . . . ?
C7 C2 C3 C4 -1.3(2) . . . . ?
C1 C2 C3 C4 177.56(16) . . . . ?
C2 C3 C4 C5 1.8(2) . . . . ?
C3 C4 C5 C6 -0.7(3) . . . . ?
C4 C5 C6 C7 -1.0(2) . . . . ?
N1 N2 C7 C6 179.60(16) . . . . ?
C9 N2 C7 C6 1.2(3) . . . . ?
N1 N2 C7 C2 -0.70(16) . . . . ?
C9 N2 C7 C2 -179.08(15) . . . . ?
C5 C6 C7 N2 -178.87(16) . . . . ?
C5 C6 C7 C2 1.5(2) . . . . ?
C3 C2 C7 N2 179.87(14) . . . . ?
C1 C2 C7 N2 0.77(16) . . . . ?
C3 C2 C7 C6 -0.4(2) . . . . ?
C1 C2 C7 C6 -179.49(14) . . . . ?
Ru1 N3 C9 N2 2.57(18) . . . . ?
Ru1 N3 C9 C8 -177.34(12) . . . . ?
C7 N2 C9 N3 179.96(15) . . . . ?
N1 N2 C9 N3 1.66(19) . . . . ?
C7 N2 C9 C8 -0.1(2) . . . . ?
N1 N2 C9 C8 -178.42(13) . . . . ?
