#------------------------------------------------------------------------------
#$Date: 2016-03-22 12:34:31 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178954 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/83/4118324.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_4118324
loop_
_publ_author_name
'Sven O. Sylvester'
'Jacqueline M. Cole'
'Paul G. Waddell'
_publ_section_title
;
 Photoconversion Bonding Mechanism in Ruthenium Sulfur Dioxide Linkage
 Photoisomers Revealed by in Situ Diffraction
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11860
_journal_page_last               11863
_journal_paper_doi               10.1021/ja303943q
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C5 H18 Cl3 N5 O3 Ru1 S1'
_chemical_formula_sum            'C5 H18 Cl3 N5 O3 Ru S'
_chemical_formula_weight         435.72
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2a'
_symmetry_space_group_name_H-M   'P m c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-03-15T11:10:05-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.952(2)
_cell_length_b                   9.772(3)
_cell_length_c                   23.295(7)
_cell_measurement_reflns_used    3408
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      32.8
_cell_measurement_theta_min      1.7
_cell_volume                     1582.5(8)
_computing_cell_refinement
;
        CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)
;
_computing_data_collection
;
        CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)
;
_computing_data_reduction
;
        CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.884
_diffrn_measurement_device_type
;
        Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0507
_diffrn_reflns_av_unetI/netI     0.0732
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4644
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         32.84
_diffrn_reflns_theta_min         2.72
_diffrn_source                   'Sealed Tube'
_exptl_absorpt_coefficient_mu    1.636
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.672
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.829
_exptl_crystal_description       Prism
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.281
_refine_diff_density_min         -1.22
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     117
_refine_ls_number_reflns         2786
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0525
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0481P)²+0.5895P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1267
_reflns_number_gt                2248
_reflns_number_total             2786
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ja303943q_si_002_38.cif
_cod_data_source_block           3-cl-pyr-light-200K-1
_cod_original_cell_volume        1582.4(8)
_cod_database_code               4118324
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'-x-1/2, y, z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Ru1 0.25 0.07119(4) 0.847649(17) 0.02451(13) Uani d S 1 . . Ru
Cl2 0.25 0.83338(14) 1.00737(6) 0.0380(3) Uani d S 1 . . Cl
Cl3 0.75 0.88592(15) 0.79120(7) 0.0410(3) Uani d S 1 . . Cl
S1 0.25 -0.10014(16) 0.79405(8) 0.0307(5) Uani d SP 0.879(8) A 1 S
Cl1 0.25 0.32474(17) 1.06731(7) 0.0495(4) Uani d S 1 . . Cl
N3 0.25 0.2469(4) 0.9007(2) 0.0297(9) Uani d S 1 A . n
N2 0.4709(4) -0.0134(3) 0.90015(13) 0.0296(6) Uani d . 1 A . n
H2A 0.5565 -0.0593 0.8777 0.044 Uiso calc R 1 . . H
H2B 0.4179 -0.0721 0.926 0.044 Uiso calc R 1 . . H
H2C 0.5326 0.0552 0.9191 0.044 Uiso calc R 1 . . H
N1 0.4679(5) 0.1651(3) 0.79770(14) 0.0330(7) Uani d . 1 A . n
H1A 0.5488 0.0998 0.7838 0.05 Uiso calc R 1 . . H
H1B 0.5353 0.2248 0.8199 0.05 Uiso calc R 1 . . H
H1C 0.4131 0.211 0.7679 0.05 Uiso calc R 1 . . H
O1 0.25 -0.0847(6) 0.7328(2) 0.0487(15) Uani d SP 0.879(8) A 1 O
C3 0.25 0.4785(6) 0.9706(3) 0.0443(14) Uani d S 1 . . C
H3 0.25 0.5573 0.9945 0.053 Uiso calc SR 1 . . H
C1 0.25 0.2362(5) 0.9586(2) 0.0293(10) Uani d S 1 . . C
H1 0.25 0.1478 0.9755 0.035 Uiso calc SR 1 A . H
C2 0.25 0.3498(6) 0.9938(3) 0.0353(12) Uani d S 1 A . C
O2 0.25 -0.2405(6) 0.8147(3) 0.0490(15) Uani d SP 0.879(8) A 1 O
C4 0.25 0.4908(6) 0.9123(3) 0.0449(15) Uani d S 1 A . C
H4 0.25 0.5788 0.8949 0.054 Uiso calc SR 1 . . H
C5 0.25 0.3739(6) 0.8784(3) 0.0376(12) Uani d S 1 . . C
H5 0.25 0.3839 0.8378 0.045 Uiso calc SR 1 A . H
O3 0.25 -0.1878(6) 0.6228(2) 0.0559(12) Uani d S 1 . . O
S1A 0.214(4) -0.180(3) 0.8167(11) 0.056(8) Uiso d P 0.061(4) . 2 S
O1A 0.25 -0.065(5) 0.764(3) 0.058(13) Uiso d SP 0.121(8) . 2 O
O2A 0.389(8) -0.275(6) 0.829(3) 0.049(13) Uiso d P 0.061(4) . 2 O
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 0 '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 0.006 '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'
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
S1 Ru1 N3 179.05(14) . .
S1 Ru1 N1 91.08(10) . .
N3 Ru1 N1 88.25(13) . .
S1 Ru1 N1 91.08(10) . 7_655
N3 Ru1 N1 88.25(13) . 7_655
N1 Ru1 N1 91.27(18) . 7_655
S1 Ru1 N2 91.85(9) . 7_655
N3 Ru1 N2 88.81(12) . 7_655
N1 Ru1 N2 177.03(13) . 7_655
N1 Ru1 N2 88.16(13) 7_655 7_655
S1 Ru1 N2 91.85(9) . .
N3 Ru1 N2 88.81(12) . .
N1 Ru1 N2 88.16(13) . .
N1 Ru1 N2 177.03(13) 7_655 .
N2 Ru1 N2 92.27(17) 7_655 .
S1 Ru1 O1A 19.1(14) . .
N3 Ru1 O1A 160.0(15) . .
N1 Ru1 O1A 77.8(10) . .
N1 Ru1 O1A 77.8(10) 7_655 .
N2 Ru1 O1A 104.9(10) 7_655 .
N2 Ru1 O1A 104.9(10) . .
S1 Ru1 S1A 21.1(6) . .
N3 Ru1 S1A 159.8(6) . .
N1 Ru1 S1A 109.2(6) . .
N1 Ru1 S1A 101.0(6) 7_655 .
N2 Ru1 S1A 73.8(6) 7_655 .
N2 Ru1 S1A 82.0(6) . .
O1A Ru1 S1A 39.8(16) . .
S1 Ru1 S1A 21.1(6) . 7_655
N3 Ru1 S1A 159.8(6) . 7_655
N1 Ru1 S1A 101.0(6) . 7_655
N1 Ru1 S1A 109.2(6) 7_655 7_655
N2 Ru1 S1A 82.0(6) 7_655 7_655
N2 Ru1 S1A 73.8(6) . 7_655
O1A Ru1 S1A 39.8(16) . 7_655
S1A Ru1 S1A 11.1(12) . 7_655
O1 S1 O2 115.4(3) . .
O1 S1 Ru1 120.7(3) . .
O2 S1 Ru1 123.9(3) . .
C5 N3 C1 117.2(5) . .
C5 N3 Ru1 121.5(4) . .
C1 N3 Ru1 121.3(3) . .
Ru1 N2 H2A 109.5 . .
Ru1 N2 H2B 109.5 . .
H2A N2 H2B 109.5 . .
Ru1 N2 H2C 109.5 . .
H2A N2 H2C 109.5 . .
H2B N2 H2C 109.5 . .
Ru1 N1 H1A 109.5 . .
Ru1 N1 H1B 109.5 . .
H1A N1 H1B 109.5 . .
Ru1 N1 H1C 109.5 . .
H1A N1 H1C 109.5 . .
H1B N1 H1C 109.5 . .
C4 C3 C2 118.3(6) . .
C4 C3 H3 120.8 . .
C2 C3 H3 120.8 . .
N3 C1 C2 122.1(5) . .
N3 C1 H1 119 . .
C2 C1 H1 119 . .
C3 C2 C1 120.2(6) . .
C3 C2 Cl1 121.4(4) . .
C1 C2 Cl1 118.3(5) . .
C3 C4 C5 119.6(6) . .
C3 C4 H4 120.2 . .
C5 C4 H4 120.2 . .
N3 C5 C4 122.6(6) . .
N3 C5 H5 118.7 . .
C4 C5 H5 118.7 . .
S1A S1A O2A 126(3) 7_655 7_655
S1A S1A O2A 38(2) 7_655 .
O2A S1A O2A 88(5) 7_655 .
S1A S1A O1A 81.5(9) 7_655 .
O2A S1A O1A 140(4) 7_655 .
O2A S1A O1A 114(3) . .
S1A S1A Ru1 84.4(6) 7_655 .
O2A S1A Ru1 137(3) 7_655 .
O2A S1A Ru1 116(2) . .
O1A S1A Ru1 64(2) . .
S1A O1A S1A 17.0(18) 7_655 .
S1A O1A Ru1 77(3) 7_655 .
S1A O1A Ru1 77(3) . .
S1A O2A S1A 15.0(18) 7_655 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Ru1 S1 . 2.0884(16)
Ru1 N3 . 2.116(4)
Ru1 N1 . 2.119(3)
Ru1 N1 7_655 2.119(3)
Ru1 N2 7_655 2.130(3)
Ru1 N2 . 2.130(3)
Ru1 O1A . 2.37(6)
Ru1 S1A . 2.57(2)
Ru1 S1A 7_655 2.57(2)
S1 O1 . 1.435(6)
S1 O2 . 1.454(6)
Cl1 C2 . 1.729(6)
N3 C5 . 1.346(7)
N3 C1 . 1.352(7)
N2 H2A . 0.91
N2 H2B . 0.91
N2 H2C . 0.91
N1 H1A . 0.91
N1 H1B . 0.91
N1 H1C . 0.91
C3 C4 . 1.365(10)
C3 C2 . 1.369(9)
C3 H3 . 0.95
C1 C2 . 1.381(7)
C1 H1 . 0.95
C4 C5 . 1.389(8)
C4 H4 . 0.95
C5 H5 . 0.95
S1A S1A 7_655 0.50(5)
S1A O2A 7_655 1.20(6)
S1A O2A . 1.55(6)
S1A O1A . 1.69(7)
O1A S1A 7_655 1.69(7)
O2A S1A 7_655 1.20(6)
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_4
N3 Ru1 S1 O1 0.00(2) . .
N1 Ru1 S1 O1 -45.64(9) . .
N1 Ru1 S1 O1 45.64(9) 7_655 .
N2 Ru1 S1 O1 133.84(8) 7_655 .
N2 Ru1 S1 O1 -133.84(8) . .
O1A Ru1 S1 O1 0.000(2) . .
S1A Ru1 S1 O1 164.3(16) . .
S1A Ru1 S1 O1 -164.3(16) 7_655 .
N3 Ru1 S1 O2 180.00(2) . .
N1 Ru1 S1 O2 134.36(9) . .
N1 Ru1 S1 O2 -134.36(9) 7_655 .
N2 Ru1 S1 O2 -46.16(8) 7_655 .
N2 Ru1 S1 O2 46.16(8) . .
O1A Ru1 S1 O2 180.000(2) . .
S1A Ru1 S1 O2 -15.7(16) . .
S1A Ru1 S1 O2 15.7(16) 7_655 .
S1 Ru1 N3 C5 0.00(7) . .
N1 Ru1 N3 C5 45.66(9) . .
N1 Ru1 N3 C5 -45.66(9) 7_655 .
N2 Ru1 N3 C5 -133.85(8) 7_655 .
N2 Ru1 N3 C5 133.85(8) . .
O1A Ru1 N3 C5 0.000(4) . .
S1A Ru1 N3 C5 -163.6(17) . .
S1A Ru1 N3 C5 163.6(17) 7_655 .
S1 Ru1 N3 C1 180.00(6) . .
N1 Ru1 N3 C1 -134.34(9) . .
N1 Ru1 N3 C1 134.34(9) 7_655 .
N2 Ru1 N3 C1 46.15(8) 7_655 .
N2 Ru1 N3 C1 -46.15(8) . .
O1A Ru1 N3 C1 180.000(3) . .
S1A Ru1 N3 C1 16.4(17) . .
S1A Ru1 N3 C1 -16.4(17) 7_655 .
C5 N3 C1 C2 0.000(4) . .
Ru1 N3 C1 C2 180.000(3) . .
C4 C3 C2 C1 0.000(5) . .
C4 C3 C2 Cl1 180.000(3) . .
N3 C1 C2 C3 0.000(5) . .
N3 C1 C2 Cl1 180.000(2) . .
C2 C3 C4 C5 0.000(5) . .
C1 N3 C5 C4 0.000(4) . .
Ru1 N3 C5 C4 180.000(3) . .
C3 C4 C5 N3 0.000(4) . .
S1 Ru1 S1A S1A 75.3(15) . 7_655
N3 Ru1 S1A S1A -105.4(16) . 7_655
N1 Ru1 S1A S1A 43.40(19) . 7_655
N1 Ru1 S1A S1A 138.63(18) 7_655 7_655
N2 Ru1 S1A S1A -136.56(16) 7_655 7_655
N2 Ru1 S1A S1A -41.82(16) . 7_655
O1A Ru1 S1A S1A 83.3(8) . 7_655
S1 Ru1 S1A O2A -145(5) . 7_655
N3 Ru1 S1A O2A 35(6) . 7_655
N1 Ru1 S1A O2A -176(5) . 7_655
N1 Ru1 S1A O2A -81(5) 7_655 7_655
N2 Ru1 S1A O2A 4(5) 7_655 7_655
N2 Ru1 S1A O2A 98(5) . 7_655
O1A Ru1 S1A O2A -137(5) . 7_655
S1A Ru1 S1A O2A 140(5) 7_655 7_655
S1 Ru1 S1A O2A 98(3) . .
N3 Ru1 S1A O2A -83(3) . .
N1 Ru1 S1A O2A 66(3) . .
N1 Ru1 S1A O2A 161(3) 7_655 .
N2 Ru1 S1A O2A -114(3) 7_655 .
N2 Ru1 S1A O2A -20(3) . .
O1A Ru1 S1A O2A 106(3) . .
S1A Ru1 S1A O2A 22(3) 7_655 .
S1 Ru1 S1A O1A -7.9(9) . .
N3 Ru1 S1A O1A 171.3(10) . .
N1 Ru1 S1A O1A -39.9(9) . .
N1 Ru1 S1A O1A 55.4(8) 7_655 .
N2 Ru1 S1A O1A 140.2(9) 7_655 .
N2 Ru1 S1A O1A -125.1(8) . .
S1A Ru1 S1A O1A -83.3(8) 7_655 .
O2A S1A O1A S1A -140(6) 7_655 7_655
O2A S1A O1A S1A -21(3) . 7_655
Ru1 S1A O1A S1A 88.0(4) . 7_655
S1A S1A O1A Ru1 -88.0(4) 7_655 .
O2A S1A O1A Ru1 132(6) 7_655 .
O2A S1A O1A Ru1 -108(3) . .
S1 Ru1 O1A S1A -8.7(9) . 7_655
N3 Ru1 O1A S1A 171.3(9) . 7_655
N1 Ru1 O1A S1A 124.3(9) . 7_655
N1 Ru1 O1A S1A -141.7(10) 7_655 7_655
N2 Ru1 O1A S1A -57.0(9) 7_655 7_655
N2 Ru1 O1A S1A 39.5(10) . 7_655
S1A Ru1 O1A S1A -17.5(19) . 7_655
S1 Ru1 O1A S1A 8.7(9) . .
N3 Ru1 O1A S1A -171.3(9) . .
N1 Ru1 O1A S1A 141.7(10) . .
N1 Ru1 O1A S1A -124.3(9) 7_655 .
N2 Ru1 O1A S1A -39.5(10) 7_655 .
N2 Ru1 O1A S1A 57.0(9) . .
S1A Ru1 O1A S1A 17.5(19) 7_655 .
O2A S1A O2A S1A 180.00(4) 7_655 7_655
O1A S1A O2A S1A 34(5) . 7_655
Ru1 S1A O2A S1A -37(4) . 7_655
