#------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/56/1515649.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_1515649
loop_
_publ_author_name
'Lai-Fung Chan, Sharon'
'Wai-Yin Sun, Raymond'
'Choi, Mei-Yuk'
'Zeng, Yibo'
'Shek, Lam'
'Sin-Yin Chui, Stephen'
'Che, Chi-Ming'
_publ_section_title
;
 An anti-cancer trinuclear ruthenium(iii) complex with 2-thiosalicylate
 ligands attenuates Wnt-β-catenin signaling
;
_journal_issue                   9
_journal_name_full               'Chemical Science'
_journal_page_first              1788
_journal_paper_doi               10.1039/c1sc00203a
_journal_volume                  2
_journal_year                    2011
_chemical_formula_moiety         'C42 H26 O12 Ru3 S6, C8 H20 N, 6(H2 O)'
_chemical_formula_sum            'C50 H58 N O18 Ru3 S6'
_chemical_formula_weight         1456.60
_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                106.03(3)
_cell_angle_beta                 90.59(4)
_cell_angle_gamma                105.44(2)
_cell_formula_units_Z            1
_cell_length_a                   10.577(2)
_cell_length_b                   10.715(2)
_cell_length_c                   13.367(3)
_cell_measurement_reflns_used    100
_cell_measurement_temperature    298
_cell_measurement_theta_max      35
_cell_measurement_theta_min      3
_cell_volume                     1397.7(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_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  0.0157
_diffrn_reflns_av_sigmaI/netI    0.0211
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7179
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    1.097
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.730
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             737
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.078
_refine_diff_density_min         -0.682
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         4794
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      2.457
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0279
_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)+(0.0505P)²+0.6185P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0754
_refine_ls_wR_factor_ref         0.0782
_reflns_number_gt                4307
_reflns_number_total             4794
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1sc00203a.txt
_cod_data_source_block           fung1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1515649
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 0.64556(5) 0.53667(5) 0.68277(4) 0.0295(2) Uani 1 1 d . . .
Ru2 Ru 0.5000 0.5000 0.5000 0.0262(2) Uani 1 2 d S . .
S1 S 0.51903(16) 0.33240(16) 0.58147(12) 0.0308(4) Uani 1 1 d . . .
S2 S 0.73497(15) 0.58492(16) 0.53842(12) 0.0311(4) Uani 1 1 d . . .
S3 S 0.48752(16) 0.64008(16) 0.67181(12) 0.0304(4) Uani 1 1 d . . .
O1 O 0.4289(6) 0.4199(7) 0.9260(4) 0.0665(18) Uani 1 1 d . . .
O2 O 0.5683(5) 0.4915(5) 0.8190(4) 0.0397(11) Uani 1 1 d . . .
O3 O 0.9394(6) 0.3301(6) 0.6709(5) 0.0550(14) Uani 1 1 d . . .
H3 H 0.9508 0.3569 0.7356 0.083 Uiso 1 1 d . . .
O4 O 0.7966(5) 0.4483(5) 0.7028(4) 0.0406(11) Uani 1 1 d . . .
O5 O 0.8838(6) 0.9298(6) 0.8394(5) 0.0726(19) Uani 1 1 d . . .
O6 O 0.7675(5) 0.7167(5) 0.7813(4) 0.0428(12) Uani 1 1 d . . .
C1 C 0.3744(7) 0.2783(7) 0.6428(5) 0.0329(14) Uani 1 1 d . . .
C2 C 0.2746(7) 0.1754(7) 0.5759(6) 0.0422(16) Uani 1 1 d . . .
H2A H 0.2870 0.1448 0.5055 0.051 Uiso 1 1 calc R . .
C3 C 0.1575(8) 0.1177(9) 0.6121(7) 0.051(2) Uani 1 1 d . . .
H3A H 0.0923 0.0485 0.5667 0.062 Uiso 1 1 calc R . .
C4 C 0.1390(8) 0.1640(10) 0.7161(7) 0.057(2) Uani 1 1 d . . .
H4A H 0.0601 0.1273 0.7410 0.068 Uiso 1 1 calc R . .
C5 C 0.2355(8) 0.2633(9) 0.7825(6) 0.0513(19) Uani 1 1 d . . .
H5A H 0.2210 0.2931 0.8525 0.062 Uiso 1 1 calc R . .
C6 C 0.3566(7) 0.3226(7) 0.7492(5) 0.0371(15) Uani 1 1 d . . .
C7 C 0.4604(8) 0.4190(7) 0.8333(5) 0.0406(16) Uani 1 1 d . . .
C11 C 0.8086(6) 0.4550(7) 0.4770(5) 0.0351(15) Uani 1 1 d . . .
C12 C 0.8254(7) 0.4409(8) 0.3709(6) 0.0427(17) Uani 1 1 d . . .
H12A H 0.7996 0.4982 0.3390 0.051 Uiso 1 1 calc R . .
C13 C 0.8797(8) 0.3427(9) 0.3128(7) 0.055(2) Uani 1 1 d . . .
H13A H 0.8893 0.3341 0.2423 0.066 Uiso 1 1 calc R . .
C14 C 0.9193(8) 0.2582(9) 0.3590(7) 0.060(2) Uani 1 1 d . . .
H14A H 0.9531 0.1904 0.3194 0.072 Uiso 1 1 calc R . .
C15 C 0.9090(8) 0.2738(8) 0.4633(7) 0.053(2) Uani 1 1 d . . .
H15A H 0.9393 0.2181 0.4942 0.063 Uiso 1 1 calc R . .
C16 C 0.8540(6) 0.3715(7) 0.5252(6) 0.0376(15) Uani 1 1 d . . .
C17 C 0.8584(7) 0.3879(7) 0.6390(6) 0.0392(16) Uani 1 1 d . . .
C21 C 0.5671(7) 0.8122(6) 0.6806(5) 0.0326(14) Uani 1 1 d . . .
C22 C 0.4864(8) 0.8767(7) 0.6423(5) 0.0416(16) Uani 1 1 d . . .
H22A H 0.4003 0.8282 0.6157 0.050 Uiso 1 1 calc R . .
C23 C 0.5311(9) 1.0090(8) 0.6431(7) 0.052(2) Uani 1 1 d . . .
H23A H 0.4758 1.0499 0.6176 0.062 Uiso 1 1 calc R . .
C24 C 0.6576(10) 1.0808(9) 0.6817(8) 0.065(2) Uani 1 1 d . . .
H24A H 0.6893 1.1700 0.6804 0.078 Uiso 1 1 calc R . .
C25 C 0.7386(9) 1.0217(8) 0.7225(7) 0.055(2) Uani 1 1 d . . .
H25A H 0.8237 1.0729 0.7499 0.066 Uiso 1 1 calc R . .
C26 C 0.6959(7) 0.8861(7) 0.7240(5) 0.0386(15) Uani 1 1 d . . .
C27 C 0.7881(7) 0.8389(8) 0.7834(6) 0.0423(17) Uani 1 1 d . . .
N1 N 0.5000 1.0000 1.0000 0.070(3) Uani 1 2 d S . .
C20A C 0.537(3) 1.147(3) 1.068(2) 0.090(8) Uani 0.50 1 d P A -1
H20A H 0.57(3) 1.16(3) 1.14(2) 0.108 Uiso 0.50 1 d P B -1
H20B H 0.44(3) 1.16(3) 1.09(2) 0.108 Uiso 0.50 1 d P C -1
C20B C 0.599(3) 1.083(3) 0.943(2) 0.090(7) Uani 0.50 1 d PD A -2
H20C H 0.546(9) 1.05(3) 0.877(5) 0.109 Uiso 0.50 1 d PD D -2
H20D H 0.674(16) 1.05(3) 0.941(16) 0.109 Uiso 0.50 1 d PD E -2
C10 C 0.6424(19) 1.2391(17) 1.0153(16) 0.136(6) Uani 1 1 d . . .
H10A H 0.6658 1.3312 1.0586 0.203 Uiso 1 1 calc R A .
H10B H 0.6054 1.2340 0.9479 0.203 Uiso 1 1 calc R . .
H10C H 0.7196 1.2076 1.0073 0.203 Uiso 1 1 calc R . .
C30 C 0.6837(18) 0.963(2) 1.1018(14) 0.139(7) Uani 1 1 d . . .
H30A H 0.7178 0.9716 1.1711 0.208 Uiso 1 1 calc R A .
H30B H 0.7494 1.0149 1.0692 0.208 Uiso 1 1 calc R . .
H30C H 0.6608 0.8691 1.0614 0.208 Uiso 1 1 calc R . .
C40A C 0.555(3) 1.016(3) 1.1081(17) 0.086(7) Uani 0.50 1 d PD A -1
H40A H 0.484(16) 0.959(19) 1.133(18) 0.103 Uiso 0.50 1 d PD F -1
H40B H 0.57(3) 1.110(6) 1.146(19) 0.103 Uiso 0.50 1 d PD G -1
C40B C 0.623(3) 0.948(3) 0.9877(19) 0.085(7) Uani 0.50 1 d PD A -2
H40C H 0.680(16) 1.000(19) 0.949(15) 0.102 Uiso 0.50 1 d PD H -2
H40D H 0.59(3) 0.855(9) 0.948(15) 0.102 Uiso 0.50 1 d PD I -2
O1W O 0.8468(10) 0.5880(10) 0.9606(7) 0.105(3) Uani 1 1 d D . .
H1WA H 0.9211(10) 0.6416(10) 0.9637(7) 0.126 Uiso 1 1 d RD . .
H1WB H 0.7946(10) 0.6031(10) 0.9212(7) 0.126 Uiso 1 1 d RD . .
O2W O 0.9576(12) 0.3867(12) 0.8662(7) 0.131(4) Uani 1 1 d D . .
H2WA H 0.8997(12) 0.4185(12) 0.8964(7) 0.157 Uiso 1 1 d RD . .
H2WB H 1.0069(12) 0.3761(12) 0.9104(7) 0.157 Uiso 1 1 d RD . .
O3W O 1.0227(12) 0.8394(9) 0.9773(8) 0.150(5) Uani 1 1 d D . .
H3WA H 1.0535(12) 0.9101(9) 1.0341(8) 0.180 Uiso 1 1 d RD . .
H3WB H 0.9598(12) 0.8780(9) 0.9577(8) 0.180 Uiso 1 1 d RD . .
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
O6 Ru1 O4 86.5(2) . .
O6 Ru1 O2 87.5(2) . .
O4 Ru1 O2 88.43(19) . .
O6 Ru1 S3 90.42(15) . .
O4 Ru1 S3 176.35(14) . .
O2 Ru1 S3 89.49(14) . .
O6 Ru1 S1 175.97(14) . .
O4 Ru1 S1 90.02(15) . .
O2 Ru1 S1 90.34(14) . .
S3 Ru1 S1 92.99(6) . .
O6 Ru1 S2 91.63(15) . .
O4 Ru1 S2 89.89(14) . .
O2 Ru1 S2 178.17(14) . .
S3 Ru1 S2 92.16(6) . .
S1 Ru1 S2 90.39(6) . .
O6 Ru1 Ru2 128.07(14) . .
O4 Ru1 Ru2 127.42(14) . .
O2 Ru1 Ru2 125.58(13) . .
S3 Ru1 Ru2 56.17(5) . .
S1 Ru1 Ru2 55.86(5) . .
S2 Ru1 Ru2 56.14(4) . .
S1 Ru2 S1 180.0 2_666 .
S1 Ru2 S3 86.81(6) 2_666 2_666
S1 Ru2 S3 93.19(6) . 2_666
S1 Ru2 S3 93.19(6) 2_666 .
S1 Ru2 S3 86.81(6) . .
S3 Ru2 S3 180.0 2_666 .
S1 Ru2 S2 95.16(6) 2_666 .
S1 Ru2 S2 84.84(6) . .
S3 Ru2 S2 94.06(7) 2_666 .
S3 Ru2 S2 85.94(7) . .
S1 Ru2 S2 84.84(6) 2_666 2_666
S1 Ru2 S2 95.16(6) . 2_666
S3 Ru2 S2 85.94(7) 2_666 2_666
S3 Ru2 S2 94.06(7) . 2_666
S2 Ru2 S2 180.0 . 2_666
S1 Ru2 Ru1 51.98(5) 2_666 2_666
S1 Ru2 Ru1 128.02(5) . 2_666
S3 Ru2 Ru1 51.56(4) 2_666 2_666
S3 Ru2 Ru1 128.44(4) . 2_666
S2 Ru2 Ru1 127.94(5) . 2_666
S2 Ru2 Ru1 52.06(5) 2_666 2_666
S1 Ru2 Ru1 128.02(5) 2_666 .
S1 Ru2 Ru1 51.98(5) . .
S3 Ru2 Ru1 128.44(4) 2_666 .
S3 Ru2 Ru1 51.56(4) . .
S2 Ru2 Ru1 52.06(5) . .
S2 Ru2 Ru1 127.94(5) 2_666 .
Ru1 Ru2 Ru1 180.0 2_666 .
C1 S1 Ru1 109.9(2) . .
C1 S1 Ru2 110.9(2) . .
Ru1 S1 Ru2 72.15(5) . .
C11 S2 Ru1 107.8(2) . .
C11 S2 Ru2 109.1(2) . .
Ru1 S2 Ru2 71.80(5) . .
C21 S3 Ru1 107.8(2) . .
C21 S3 Ru2 109.4(2) . .
Ru1 S3 Ru2 72.27(5) . .
C7 O2 Ru1 132.1(4) . .
C17 O4 Ru1 131.2(5) . .
C27 O6 Ru1 132.7(5) . .
C2 C1 C6 119.3(6) . .
C2 C1 S1 114.0(5) . .
C6 C1 S1 126.6(5) . .
C3 C2 C1 121.4(7) . .
C4 C3 C2 119.2(8) . .
C5 C4 C3 120.2(8) . .
C4 C5 C6 122.4(8) . .
C1 C6 C5 117.6(7) . .
C1 C6 C7 125.6(6) . .
C5 C6 C7 116.5(6) . .
O2 C7 O1 121.0(7) . .
O2 C7 C6 125.9(6) . .
O1 C7 C6 113.1(7) . .
C12 C11 C16 118.7(6) . .
C12 C11 S2 114.7(5) . .
C16 C11 S2 126.6(5) . .
C13 C12 C11 121.0(8) . .
C14 C13 C12 120.2(8) . .
C15 C14 C13 119.8(8) . .
C14 C15 C16 122.0(8) . .
C15 C16 C11 118.2(7) . .
C15 C16 C17 117.4(7) . .
C11 C16 C17 124.1(6) . .
O4 C17 O3 119.4(7) . .
O4 C17 C16 127.2(6) . .
O3 C17 C16 113.4(6) . .
C22 C21 C26 119.5(6) . .
C22 C21 S3 113.7(5) . .
C26 C21 S3 126.8(5) . .
C23 C22 C21 121.6(7) . .
C24 C23 C22 119.6(8) . .
C23 C24 C25 120.3(8) . .
C24 C25 C26 121.8(8) . .
C21 C26 C25 117.1(7) . .
C21 C26 C27 126.1(6) . .
C25 C26 C27 116.4(7) . .
O6 C27 O5 121.3(7) . .
O6 C27 C26 122.4(6) . .
O5 C27 C26 116.3(7) . .
C40A N1 C40A 180.000(15) 2_677 .
C40A N1 C20A 112.3(15) 2_677 .
C40A N1 C20A 67.7(15) . .
C40A N1 C20A 67.7(15) 2_677 2_677
C40A N1 C20A 112.3(15) . 2_677
C20A N1 C20A 180.000(10) . 2_677
C40A N1 C20B 68.3(16) 2_677 .
C40A N1 C20B 111.7(16) . .
C20A N1 C20B 73.3(15) . .
C20A N1 C20B 106.7(15) 2_677 .
C40A N1 C20B 111.7(16) 2_677 2_677
C40A N1 C20B 68.3(16) . 2_677
C20A N1 C20B 106.7(15) . 2_677
C20A N1 C20B 73.3(15) 2_677 2_677
C20B N1 C20B 180(2) . 2_677
C40A N1 C40B 106.9(13) 2_677 .
C40A N1 C40B 73.1(13) . .
C20A N1 C40B 110.1(17) . .
C20A N1 C40B 69.9(16) 2_677 .
C20B N1 C40B 70.8(15) . .
C20B N1 C40B 109.2(15) 2_677 .
C40A N1 C40B 73.1(13) 2_677 2_677
C40A N1 C40B 106.9(13) . 2_677
C20A N1 C40B 69.9(16) . 2_677
C20A N1 C40B 110.1(17) 2_677 2_677
C20B N1 C40B 109.2(15) . 2_677
C20B N1 C40B 70.8(15) 2_677 2_677
C40B N1 C40B 180.00(2) . 2_677
N1 C20A C10 109.7(16) . .
N1 C20A C40A 55.3(13) . .
C10 C20A C40A 127(2) . .
N1 C20B C10 107.8(16) . .
N1 C20B C40B 54.8(12) . .
C10 C20B C40B 123(2) . .
C20A C10 C20B 69.3(14) . .
C40B C30 C40A 69.1(12) . .
N1 C40A C30 109.9(14) . .
N1 C40A C20A 57.0(12) . .
C30 C40A C20A 126(2) . .
N1 C40B C30 107.9(15) . .
N1 C40B C20B 54.4(11) . .
C30 C40B C20B 126(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ru1 O6 2.087(5) .
Ru1 O4 2.111(5) .
Ru1 O2 2.127(5) .
Ru1 S3 2.2615(17) .
Ru1 S1 2.276(2) .
Ru1 S2 2.2831(18) .
Ru1 Ru2 2.7502(10) .
Ru2 S1 2.3915(16) 2_666
Ru2 S1 2.3915(16) .
Ru2 S3 2.3985(18) 2_666
Ru2 S3 2.3985(18) .
Ru2 S2 2.4040(17) .
Ru2 S2 2.4040(17) 2_666
Ru2 Ru1 2.7502(10) 2_666
S1 C1 1.779(7) .
S2 C11 1.783(7) .
S3 C21 1.782(7) .
O1 C7 1.284(9) .
O2 C7 1.247(9) .
O3 C17 1.311(9) .
O4 C17 1.227(9) .
O5 C27 1.262(9) .
O6 C27 1.261(9) .
C1 C2 1.395(10) .
C1 C6 1.402(10) .
C2 C3 1.386(11) .
C3 C4 1.376(12) .
C4 C5 1.357(12) .
C5 C6 1.406(11) .
C6 C7 1.505(10) .
C11 C12 1.403(10) .
C11 C16 1.409(10) .
C12 C13 1.385(11) .
C13 C14 1.372(13) .
C14 C15 1.367(13) .
C15 C16 1.406(11) .
C16 C17 1.481(10) .
C21 C22 1.403(10) .
C21 C26 1.405(10) .
C22 C23 1.366(11) .
C23 C24 1.366(13) .
C24 C25 1.379(13) .
C25 C26 1.408(11) .
C26 C27 1.518(10) .
N1 C40A 1.50(2) 2_677
N1 C40A 1.50(2) .
N1 C20A 1.53(3) .
N1 C20A 1.53(3) 2_677
N1 C20B 1.53(3) .
N1 C20B 1.53(3) 2_677
N1 C40B 1.54(2) .
N1 C40B 1.54(2) 2_677
C20A C10 1.59(3) .
C20A C40A 1.69(4) .
C20B C10 1.63(3) .
C20B C40B 1.78(4) .
C30 C40B 1.60(3) .
C30 C40A 1.60(3) .
