#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:29:14 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179181 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/29/4312907.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_4312907
loop_
_publ_author_name
'Andrey Yu. Kovalevsky'
'Kimberly A. Bagley'
'Jacqueline M. Cole'
'Philip Coppens'
_publ_section_title
;
 Light-Induced Metastable Linkage Isomers of Ruthenium Sulfur Dioxide
 Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              140
_journal_page_last               147
_journal_paper_doi               10.1021/ic025997g
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C14 H28 N4 O9 Ru S3'
_chemical_formula_weight         593.65
_chemical_melting_point          ?
_chemical_name_common            trans-[Ru(II)(NH3)4(H2O)(SO2)](Tos)2
_chemical_name_systematic
; 
 trans-Tetraammineaquo(sulfur dioxide)ruthenium(II) tosylate
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                94.445(1)
_cell_angle_beta                 92.840(1)
_cell_angle_gamma                103.597(1)
_cell_formula_units_Z            2
_cell_length_a                   6.6769(2)
_cell_length_b                   13.0777(3)
_cell_length_c                   13.6128(4)
_cell_measurement_reflns_used    847
_cell_measurement_temperature    90(1)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      4
_cell_volume                     1149.04(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(1)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0521
_diffrn_reflns_av_sigmaI/netI    0.0470
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20923
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    1.007
_exptl_absorpt_correction_T_max  0.9514
_exptl_absorpt_correction_T_min  0.8636
_exptl_absorpt_correction_type   'empirical SADABS'
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.716
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       brick
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.507
_refine_diff_density_min         -1.551
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         6711
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0294
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0319P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0625
_refine_ls_wR_factor_ref         0.0673
_reflns_number_gt                5613
_reflns_number_total             6711
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025997g_s2_5.cif
_cod_data_source_block           ruso2h2otosylate_dark
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/adriana/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius 

The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 
;
_cod_original_cell_volume        1149.04(5)
_cod_database_code               4312907
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
Ru1 Ru 0.31295(2) -0.505822(11) 0.244952(11) 0.00811(5) Uani 1 1 d . . .
S1 S 0.40156(7) -0.64328(4) 0.19697(4) 0.01240(10) Uani 1 1 d . . .
S2 S 0.30827(7) -0.31983(4) 0.55371(3) 0.01202(9) Uani 1 1 d . . .
S3 S -0.04132(7) -0.29450(4) 0.08150(3) 0.01062(9) Uani 1 1 d . . .
O1 O 0.2986(2) -0.74500(11) 0.22511(12) 0.0227(3) Uani 1 1 d . . .
O2 O 0.5646(2) -0.64230(12) 0.13123(11) 0.0185(3) Uani 1 1 d . . .
O3 O 0.2283(2) -0.36322(11) 0.29025(11) 0.0133(3) Uani 1 1 d . . .
H3OA H 0.139(4) -0.347(2) 0.2569(19) 0.020 Uiso 1 1 d . . .
H3OB H 0.195(4) -0.359(2) 0.347(2) 0.020 Uiso 1 1 d . . .
O4 O 0.2649(2) -0.36941(11) 0.64558(10) 0.0153(3) Uani 1 1 d . . .
O5 O 0.5063(2) -0.32913(11) 0.51797(11) 0.0163(3) Uani 1 1 d . . .
O6 O 0.1364(2) -0.35971(11) 0.47825(10) 0.0156(3) Uani 1 1 d . . .
O7 O -0.1727(2) -0.35775(11) -0.00066(11) 0.0197(3) Uani 1 1 d . . .
O8 O 0.1778(2) -0.27711(12) 0.06886(11) 0.0184(3) Uani 1 1 d . . .
O9 O -0.0948(2) -0.34156(11) 0.17500(10) 0.0147(3) Uani 1 1 d . . .
N1 N 0.6027(2) -0.42903(13) 0.31980(12) 0.0122(3) Uani 1 1 d . . .
H1A H 0.5820 -0.3886 0.3740 0.018 Uiso 1 1 calc R . .
H1B H 0.6810 -0.3873 0.2786 0.018 Uiso 1 1 calc R . .
H1C H 0.6690 -0.4784 0.3388 0.018 Uiso 1 1 calc R . .
N2 N 0.2115(3) -0.56647(13) 0.37800(12) 0.0139(3) Uani 1 1 d . . .
H2C H 0.3068 -0.5979 0.4047 0.021 Uiso 1 1 calc R . .
H2B H 0.0886 -0.6149 0.3654 0.021 Uiso 1 1 calc R . .
H2A H 0.1954 -0.5128 0.4212 0.021 Uiso 1 1 calc R . .
N3 N 0.0095(2) -0.56352(13) 0.17921(13) 0.0137(3) Uani 1 1 d . . .
H3A H -0.0666 -0.6082 0.2189 0.020 Uiso 1 1 calc R . .
H3B H 0.0140 -0.5988 0.1193 0.020 Uiso 1 1 calc R . .
H3C H -0.0495 -0.5084 0.1711 0.020 Uiso 1 1 calc R . .
N4 N 0.4039(3) -0.43695(13) 0.11364(12) 0.0129(3) Uani 1 1 d . . .
H4A H 0.3545 -0.4847 0.0607 0.019 Uiso 1 1 calc R . .
H4B H 0.5443 -0.4176 0.1152 0.019 Uiso 1 1 calc R . .
H4C H 0.3522 -0.3790 0.1086 0.019 Uiso 1 1 calc R . .
C1 C 0.3200(3) -0.18426(15) 0.57968(14) 0.0135(4) Uani 1 1 d . . .
C2 C 0.1390(3) -0.14957(17) 0.57250(16) 0.0178(4) Uani 1 1 d . . .
H2D H 0.0119 -0.1975 0.5497 0.021 Uiso 1 1 calc R . .
C3 C 0.1457(4) -0.04392(17) 0.59906(17) 0.0218(5) Uani 1 1 d . . .
H3D H 0.0217 -0.0202 0.5954 0.026 Uiso 1 1 calc R . .
C4 C 0.3311(4) 0.02767(16) 0.63094(15) 0.0196(4) Uani 1 1 d . . .
C5 C 0.5117(4) -0.00868(17) 0.63683(16) 0.0217(5) Uani 1 1 d . . .
H5A H 0.6395 0.0394 0.6582 0.026 Uiso 1 1 calc R . .
C6 C 0.5064(3) -0.11467(17) 0.61173(16) 0.0181(4) Uani 1 1 d . . .
H6A H 0.6295 -0.1390 0.6166 0.022 Uiso 1 1 calc R . .
C7 C 0.3353(5) 0.14208(18) 0.65810(18) 0.0294(6) Uani 1 1 d . . .
H7A H 0.4682 0.1774 0.6932 0.044 Uiso 1 1 calc R . .
H7B H 0.2233 0.1468 0.7008 0.044 Uiso 1 1 calc R . .
H7C H 0.3172 0.1765 0.5979 0.044 Uiso 1 1 calc R . .
C8 C -0.1015(3) -0.17026(15) 0.09174(14) 0.0110(4) Uani 1 1 d . . .
C9 C 0.0482(3) -0.08277(16) 0.13256(15) 0.0164(4) Uani 1 1 d . . .
H9A H 0.1841 -0.0891 0.1499 0.020 Uiso 1 1 calc R . .
C10 C -0.0023(4) 0.01413(16) 0.14783(16) 0.0193(4) Uani 1 1 d . . .
H10A H 0.1005 0.0742 0.1751 0.023 Uiso 1 1 calc R . .
C11 C -0.2010(4) 0.02458(16) 0.12393(15) 0.0179(4) Uani 1 1 d . . .
C12 C -0.3482(3) -0.06449(16) 0.08254(15) 0.0165(4) Uani 1 1 d . . .
H12A H -0.4846 -0.0586 0.0659 0.020 Uiso 1 1 calc R . .
C13 C -0.2999(3) -0.16173(15) 0.06508(15) 0.0139(4) Uani 1 1 d . . .
H13A H -0.4009 -0.2213 0.0354 0.017 Uiso 1 1 calc R . .
C14 C -0.2565(4) 0.12922(17) 0.14203(17) 0.0260(5) Uani 1 1 d . . .
H14C H -0.2257 0.1697 0.0847 0.039 Uiso 1 1 calc R . .
H14B H -0.1758 0.1688 0.2008 0.039 Uiso 1 1 calc R . .
H14A H -0.4041 0.1172 0.1524 0.039 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'
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'
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
S1 Ru1 N2 92.56(5) . . ?
S1 Ru1 N3 92.74(5) . . ?
N2 Ru1 N3 89.30(7) . . ?
S1 Ru1 N4 91.19(5) . . ?
N2 Ru1 N4 176.14(6) . . ?
N3 Ru1 N4 89.60(6) . . ?
S1 Ru1 N1 95.46(5) . . ?
N2 Ru1 N1 89.47(6) . . ?
N3 Ru1 N1 171.75(6) . . ?
N4 Ru1 N1 91.10(6) . . ?
S1 Ru1 O3 178.14(4) . . ?
N2 Ru1 O3 89.24(6) . . ?
N3 Ru1 O3 87.76(6) . . ?
N4 Ru1 O3 87.02(6) . . ?
N1 Ru1 O3 84.07(6) . . ?
O1 S1 O2 116.06(9) . . ?
O1 S1 Ru1 121.78(7) . . ?
O2 S1 Ru1 122.12(7) . . ?
O5 S2 O4 112.60(9) . . ?
O5 S2 O6 112.30(8) . . ?
O4 S2 O6 110.95(9) . . ?
O5 S2 C1 107.73(9) . . ?
O4 S2 C1 106.93(9) . . ?
O6 S2 C1 105.90(9) . . ?
O8 S3 O7 114.22(9) . . ?
O8 S3 O9 111.26(9) . . ?
O7 S3 O9 109.91(9) . . ?
O8 S3 C8 107.68(9) . . ?
O7 S3 C8 107.16(9) . . ?
O9 S3 C8 106.19(9) . . ?
C6 C1 C2 120.77(19) . . ?
C6 C1 S2 120.01(16) . . ?
C2 C1 S2 119.14(16) . . ?
C1 C2 C3 119.3(2) . . ?
C2 C3 C4 121.0(2) . . ?
C3 C4 C5 118.7(2) . . ?
C3 C4 C7 120.2(2) . . ?
C5 C4 C7 121.1(2) . . ?
C6 C5 C4 120.7(2) . . ?
C1 C6 C5 119.4(2) . . ?
C9 C8 C13 120.80(18) . . ?
C9 C8 S3 118.96(15) . . ?
C13 C8 S3 120.11(15) . . ?
C8 C9 C10 119.42(19) . . ?
C9 C10 C11 121.08(19) . . ?
C10 C11 C12 118.31(19) . . ?
C10 C11 C14 121.0(2) . . ?
C12 C11 C14 120.7(2) . . ?
C13 C12 C11 121.5(2) . . ?
C8 C13 C12 118.85(19) . . ?
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 S1 2.0892(5) . ?
Ru1 N2 2.1118(16) . ?
Ru1 N3 2.1147(16) . ?
Ru1 N4 2.1155(16) . ?
Ru1 N1 2.1263(16) . ?
Ru1 O3 2.1283(14) . ?
S1 O1 1.4368(16) . ?
S1 O2 1.4415(15) . ?
S2 O5 1.4593(15) . ?
S2 O4 1.4634(14) . ?
S2 O6 1.4706(15) . ?
S2 C1 1.763(2) . ?
S3 O8 1.4477(15) . ?
S3 O7 1.4569(15) . ?
S3 O9 1.4797(14) . ?
S3 C8 1.7603(19) . ?
C1 C6 1.385(3) . ?
C1 C2 1.389(3) . ?
C2 C3 1.390(3) . ?
C3 C4 1.392(3) . ?
C4 C5 1.397(3) . ?
C4 C7 1.507(3) . ?
C5 C6 1.393(3) . ?
C8 C9 1.388(3) . ?
C8 C13 1.388(3) . ?
C9 C10 1.389(3) . ?
C10 C11 1.391(3) . ?
C11 C12 1.395(3) . ?
C11 C14 1.505(3) . ?
C12 C13 1.390(3) . ?
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
N2 Ru1 S1 O1 30.02(10) . . . . ?
N3 Ru1 S1 O1 -59.40(10) . . . . ?
N4 Ru1 S1 O1 -149.05(10) . . . . ?
N1 Ru1 S1 O1 119.73(9) . . . . ?
O3 Ru1 S1 O1 -164.8(14) . . . . ?
N2 Ru1 S1 O2 -152.07(9) . . . . ?
N3 Ru1 S1 O2 118.51(9) . . . . ?
N4 Ru1 S1 O2 28.86(9) . . . . ?
N1 Ru1 S1 O2 -62.36(9) . . . . ?
O3 Ru1 S1 O2 13.1(14) . . . . ?
O5 S2 C1 C6 -31.44(19) . . . . ?
O4 S2 C1 C6 89.83(18) . . . . ?
O6 S2 C1 C6 -151.79(16) . . . . ?
O5 S2 C1 C2 151.87(16) . . . . ?
O4 S2 C1 C2 -86.86(18) . . . . ?
O6 S2 C1 C2 31.52(19) . . . . ?
C6 C1 C2 C3 -0.8(3) . . . . ?
S2 C1 C2 C3 175.88(16) . . . . ?
C1 C2 C3 C4 1.2(3) . . . . ?
C2 C3 C4 C5 -0.6(3) . . . . ?
C2 C3 C4 C7 179.2(2) . . . . ?
C3 C4 C5 C6 -0.3(3) . . . . ?
C7 C4 C5 C6 179.9(2) . . . . ?
C2 C1 C6 C5 -0.1(3) . . . . ?
S2 C1 C6 C5 -176.74(16) . . . . ?
C4 C5 C6 C1 0.7(3) . . . . ?
O8 S3 C8 C9 -30.08(18) . . . . ?
O7 S3 C8 C9 -153.38(16) . . . . ?
O9 S3 C8 C9 89.18(17) . . . . ?
O8 S3 C8 C13 153.98(16) . . . . ?
O7 S3 C8 C13 30.68(18) . . . . ?
O9 S3 C8 C13 -86.75(17) . . . . ?
C13 C8 C9 C10 0.7(3) . . . . ?
S3 C8 C9 C10 -175.18(16) . . . . ?
C8 C9 C10 C11 0.7(3) . . . . ?
C9 C10 C11 C12 -1.1(3) . . . . ?
C9 C10 C11 C14 179.01(19) . . . . ?
C10 C11 C12 C13 -0.1(3) . . . . ?
C14 C11 C12 C13 179.87(19) . . . . ?
C9 C8 C13 C12 -1.8(3) . . . . ?
S3 C8 C13 C12 174.05(15) . . . . ?
C11 C12 C13 C8 1.5(3) . . . . ?
