#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:23:56 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179788 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/84/7008486.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_7008486
loop_
_publ_author_name
'Bratsos, Ioannis'
'Zangrando, Ennio'
'Serli, Barbara'
'Katsaros, Nikos'
'Alessio, Enzo'
_publ_section_title
;
 The unprecedented bridging coordination mode of 1,1-cyclobutane
 dicarboxylate (mu-cbdc-O,O') stabilized by intramolecular hydrogen
 bonds in ruthenium(II) complexes.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3881
_journal_page_last               3885
_journal_paper_doi               10.1039/b503412d
_journal_year                    2005
_chemical_formula_moiety
'C24 H54 N2 O14 Ru2 S6, 2(C H4 O), 2(C0.50 H2 O0.50)'
_chemical_formula_sum            'C27 H66 N2 O17 Ru2 S6'
_chemical_formula_weight         1085.32
_chemical_name_systematic
;
bis[tris(dimethylsulfoxide,S)-amino-(mu-cyclobutane-1,1-dicarboxylato)
-ruthenium(II)] methanol 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                94.01(3)
_cell_angle_beta                 102.58(3)
_cell_angle_gamma                119.68(3)
_cell_formula_units_Z            1
_cell_length_a                   11.132(3)
_cell_length_b                   11.097(4)
_cell_length_c                   11.975(4)
_cell_measurement_temperature    150(2)
_cell_volume                     1226.5(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 0.893
_diffrn_measured_fraction_theta_max 0.893
_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  0.0885
_diffrn_reflns_av_sigmaI/netI    0.0941
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12929
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    0.931
_exptl_absorpt_correction_T_max  0.9032
_exptl_absorpt_correction_T_min  0.7338
_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            colourless
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             562
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.351
_refine_diff_density_min         -0.880
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         4468
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0903
_refine_ls_R_factor_gt           0.0668
_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)+(0.1395P)²+0.3381P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1808
_refine_ls_wR_factor_ref         0.2030
_reflns_number_gt                3205
_reflns_number_total             4468
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b503412d.txt
_cod_data_source_block           4
_cod_original_cell_volume        1226.5(7)
_cod_database_code               7008486
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 0.43038(6) 0.60861(5) 0.26294(5) 0.0527(3) Uani 1 1 d . . .
N1 N 0.4362(7) 0.4363(6) 0.1807(5) 0.0578(14) Uani 1 1 d . . .
H1A H 0.5188 0.4405 0.2188 0.087 Uiso 1 1 calc R . .
H1B H 0.4339 0.4415 0.1048 0.087 Uiso 1 1 calc R . .
H1C H 0.3584 0.3530 0.1832 0.087 Uiso 1 1 calc R . .
S1 S 0.4421(2) 0.79214(18) 0.37985(16) 0.0575(5) Uani 1 1 d . . .
S2 S 0.5673(2) 0.74501(18) 0.15707(16) 0.0600(5) Uani 1 1 d . . .
S3 S 0.2273(2) 0.54866(19) 0.12443(16) 0.0604(5) Uani 1 1 d . . .
O11 O 0.5376(7) 0.9390(5) 0.3676(5) 0.0717(14) Uani 1 1 d . . .
O12 O 0.5675(7) 0.6676(6) 0.0512(5) 0.0764(16) Uani 1 1 d . . .
O13 O 0.2002(7) 0.6632(6) 0.0953(5) 0.0743(15) Uani 1 1 d . . .
C1 C 0.4990(10) 0.7882(8) 0.5290(7) 0.070(2) Uani 1 1 d . . .
H1D H 0.5943 0.7988 0.5469 0.105 Uiso 1 1 calc R . .
H1E H 0.4294 0.6975 0.5442 0.105 Uiso 1 1 calc R . .
H1F H 0.5047 0.8661 0.5785 0.105 Uiso 1 1 calc R . .
C2 C 0.2711(10) 0.7696(11) 0.3725(8) 0.079(2) Uani 1 1 d . . .
H2A H 0.2841 0.8485 0.4266 0.119 Uiso 1 1 calc R . .
H2B H 0.2106 0.6800 0.3943 0.119 Uiso 1 1 calc R . .
H2C H 0.2241 0.7680 0.2926 0.119 Uiso 1 1 calc R . .
C3 C 0.7515(10) 0.8603(10) 0.2410(8) 0.081(2) Uani 1 1 d . . .
H3A H 0.7901 0.8041 0.2745 0.122 Uiso 1 1 calc R . .
H3B H 0.7579 0.9262 0.3042 0.122 Uiso 1 1 calc R . .
H3C H 0.8077 0.9140 0.1904 0.122 Uiso 1 1 calc R . .
C4 C 0.5290(12) 0.8761(9) 0.1095(9) 0.083(3) Uani 1 1 d . . .
H4A H 0.5959 0.9315 0.0662 0.124 Uiso 1 1 calc R . .
H4B H 0.5409 0.9393 0.1778 0.124 Uiso 1 1 calc R . .
H4C H 0.4294 0.8286 0.0585 0.124 Uiso 1 1 calc R . .
C5 C 0.0682(8) 0.4158(9) 0.1519(8) 0.070(2) Uani 1 1 d . . .
H5A H -0.0141 0.3797 0.0817 0.106 Uiso 1 1 calc R . .
H5B H 0.0501 0.4565 0.2169 0.106 Uiso 1 1 calc R . .
H5C H 0.0807 0.3378 0.1722 0.106 Uiso 1 1 calc R . .
C6 C 0.2094(10) 0.4567(9) -0.0118(7) 0.074(2) Uani 1 1 d . . .
H6A H 0.1162 0.4276 -0.0673 0.111 Uiso 1 1 calc R . .
H6B H 0.2145 0.3726 -0.0002 0.111 Uiso 1 1 calc R . .
H6C H 0.2878 0.5193 -0.0429 0.111 Uiso 1 1 calc R . .
O1 O 0.2339(6) 0.2637(5) 0.2939(5) 0.0685(13) Uani 1 1 d . . .
O2 O 0.3142(5) 0.4876(5) 0.3703(4) 0.0575(11) Uani 1 1 d . . .
O3 O 0.6145(5) 0.6614(4) 0.4013(4) 0.0525(10) Uani 1 1 d . . .
O4 O 0.7023(7) 0.5357(8) 0.3415(5) 0.090(2) Uani 1 1 d . . .
C7 C 0.7028(8) 0.6199(7) 0.4143(6) 0.0561(16) Uani 1 1 d . . .
C9 C 0.2476(7) 0.3543(7) 0.3685(6) 0.0530(15) Uani 1 1 d . . .
C8 C 0.1783(7) 0.3140(7) 0.4673(6) 0.0535(15) Uani 1 1 d . . .
C10 C 0.0744(8) 0.1534(8) 0.4574(7) 0.0651(18) Uani 1 1 d . . .
H10A H 0.0340 0.0966 0.3766 0.078 Uiso 1 1 calc R . .
H10B H 0.1151 0.1113 0.5124 0.078 Uiso 1 1 calc R . .
C11 C -0.0285(11) 0.1869(10) 0.4976(10) 0.088(3) Uani 1 1 d . . .
H11A H -0.0187 0.1921 0.5823 0.106 Uiso 1 1 calc R . .
H11B H -0.1309 0.1247 0.4504 0.106 Uiso 1 1 calc R . .
C12 C 0.0510(8) 0.3366(9) 0.4641(7) 0.0670(19) Uani 1 1 d . . .
H12A H 0.0027 0.3405 0.3857 0.080 Uiso 1 1 calc R . .
H12B H 0.0748 0.4169 0.5245 0.080 Uiso 1 1 calc R . .
O1M O 0.8312(8) 0.4103(8) 0.2602(7) 0.096(2) Uani 1 1 d . . .
H1M H 0.8005 0.4567 0.2894 0.144 Uiso 1 1 calc R . .
C1M C 0.7197(12) 0.2679(13) 0.2204(12) 0.111(4) Uani 1 1 d . . .
H2M H 0.7478 0.2185 0.1707 0.167 Uiso 1 1 calc R . .
H3M H 0.6317 0.2623 0.1752 0.167 Uiso 1 1 calc R . .
H4M H 0.7015 0.2233 0.2876 0.167 Uiso 1 1 calc R . .
O2M O 0.1199(19) -0.0259(16) 0.2030(15) 0.145(7) Uani 0.50 1 d PRU . .
H8M H 0.1538 0.0611 0.2302 0.218 Uiso 0.50 1 d PR . .
C2M C 0.2015(19) -0.0132(16) 0.1269(15) 0.108(7) Uani 0.50 1 d PU . .
H5M H 0.1763 0.0282 0.0629 0.162 Uiso 0.50 1 calc PR . .
H6M H 0.1814 -0.1072 0.0948 0.162 Uiso 0.50 1 calc PR . .
H7M H 0.3045 0.0483 0.1693 0.162 Uiso 0.50 1 calc PR . .
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'
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'
N N 0.0061 0.0033 '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
O2 Ru O3 84.47(18) . . ?
O2 Ru N1 92.3(2) . . ?
O3 Ru N1 90.3(2) . . ?
O2 Ru S3 92.14(15) . . ?
O3 Ru S3 176.41(13) . . ?
N1 Ru S3 91.07(18) . . ?
O2 Ru S2 176.50(14) . . ?
O3 Ru S2 92.12(14) . . ?
N1 Ru S2 88.48(17) . . ?
S3 Ru S2 91.26(8) . . ?
O2 Ru S1 82.97(14) . . ?
O3 Ru S1 81.69(13) . . ?
N1 Ru S1 171.00(17) . . ?
S3 Ru S1 96.74(8) . . ?
S2 Ru S1 95.78(7) . . ?
O11 S1 C1 106.5(4) . . ?
O11 S1 C2 107.4(4) . . ?
C1 S1 C2 99.7(5) . . ?
O11 S1 Ru 118.0(2) . . ?
C1 S1 Ru 109.4(3) . . ?
C2 S1 Ru 114.0(3) . . ?
O12 S2 C3 106.7(4) . . ?
O12 S2 C4 105.9(4) . . ?
C3 S2 C4 98.9(5) . . ?
O12 S2 Ru 115.6(2) . . ?
C3 S2 Ru 112.4(3) . . ?
C4 S2 Ru 115.7(3) . . ?
O13 S3 C5 106.2(4) . . ?
O13 S3 C6 105.2(4) . . ?
C5 S3 C6 98.7(4) . . ?
O13 S3 Ru 118.4(3) . . ?
C5 S3 Ru 113.3(3) . . ?
C6 S3 Ru 113.0(3) . . ?
C9 O2 Ru 132.5(5) . . ?
C7 O3 Ru 132.5(4) . . ?
O4 C7 O3 126.0(7) . . ?
O4 C7 C8 119.1(6) . 2_666 ?
O3 C7 C8 114.9(6) . 2_666 ?
O1 C9 O2 125.1(6) . . ?
O1 C9 C8 121.1(6) . . ?
O2 C9 C8 113.8(6) . . ?
C9 C8 C7 109.4(6) . 2_666 ?
C9 C8 C10 116.0(6) . . ?
C7 C8 C10 110.7(6) 2_666 . ?
C9 C8 C12 116.5(6) . . ?
C7 C8 C12 114.0(6) 2_666 . ?
C10 C8 C12 89.0(5) . . ?
C11 C10 C8 89.1(6) . . ?
C10 C11 C12 88.8(6) . . ?
C8 C12 C11 87.0(6) . . ?
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 O2 2.091(5) . ?
Ru O3 2.118(5) . ?
Ru N1 2.126(5) . ?
Ru S3 2.242(2) . ?
Ru S2 2.247(2) . ?
Ru S1 2.320(2) . ?
S1 O11 1.481(5) . ?
S1 C1 1.772(8) . ?
S1 C2 1.773(9) . ?
S2 O12 1.482(5) . ?
S2 C3 1.782(9) . ?
S2 C4 1.801(8) . ?
S3 O13 1.492(5) . ?
S3 C5 1.776(8) . ?
S3 C6 1.780(9) . ?
O1 C9 1.223(8) . ?
O2 C9 1.282(8) . ?
O3 C7 1.262(8) . ?
O4 C7 1.230(9) . ?
C7 C8 1.541(10) 2_666 ?
C9 C8 1.525(9) . ?
C8 C7 1.541(10) 2_666 ?
C8 C10 1.549(10) . ?
C8 C12 1.551(10) . ?
C10 C11 1.524(12) . ?
C11 C12 1.581(12) . ?
O1M C1M 1.399(13) . ?
C2M O2M 1.3881 . ?
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 S1 O11 170.9(3) . . . . ?
O3 Ru S1 O11 85.5(3) . . . . ?
N1 Ru S1 O11 112.2(11) . . . . ?
S3 Ru S1 O11 -97.8(3) . . . . ?
S2 Ru S1 O11 -5.8(3) . . . . ?
O2 Ru S1 C1 49.0(4) . . . . ?
O3 Ru S1 C1 -36.4(4) . . . . ?
N1 Ru S1 C1 -9.7(11) . . . . ?
S3 Ru S1 C1 140.3(3) . . . . ?
S2 Ru S1 C1 -127.7(3) . . . . ?
O2 Ru S1 C2 -61.7(4) . . . . ?
O3 Ru S1 C2 -147.1(4) . . . . ?
N1 Ru S1 C2 -120.4(11) . . . . ?
S3 Ru S1 C2 29.7(4) . . . . ?
S2 Ru S1 C2 121.6(4) . . . . ?
O2 Ru S2 O12 123(2) . . . . ?
O3 Ru S2 O12 109.9(3) . . . . ?
N1 Ru S2 O12 19.7(3) . . . . ?
S3 Ru S2 O12 -71.3(3) . . . . ?
S1 Ru S2 O12 -168.2(3) . . . . ?
O2 Ru S2 C3 0(2) . . . . ?
O3 Ru S2 C3 -12.9(4) . . . . ?
N1 Ru S2 C3 -103.1(4) . . . . ?
S3 Ru S2 C3 165.9(4) . . . . ?
S1 Ru S2 C3 69.0(4) . . . . ?
O2 Ru S2 C4 -113(2) . . . . ?
O3 Ru S2 C4 -125.5(4) . . . . ?
N1 Ru S2 C4 144.3(4) . . . . ?
S3 Ru S2 C4 53.3(4) . . . . ?
S1 Ru S2 C4 -43.6(4) . . . . ?
O2 Ru S3 O13 117.3(3) . . . . ?
O3 Ru S3 O13 98.0(19) . . . . ?
N1 Ru S3 O13 -150.4(3) . . . . ?
S2 Ru S3 O13 -61.9(3) . . . . ?
S1 Ru S3 O13 34.1(3) . . . . ?
O2 Ru S3 C5 -7.9(4) . . . . ?
O3 Ru S3 C5 -27.2(19) . . . . ?
N1 Ru S3 C5 84.4(4) . . . . ?
S2 Ru S3 C5 172.9(3) . . . . ?
S1 Ru S3 C5 -91.1(3) . . . . ?
O2 Ru S3 C6 -119.1(3) . . . . ?
O3 Ru S3 C6 -138.4(19) . . . . ?
N1 Ru S3 C6 -26.8(3) . . . . ?
S2 Ru S3 C6 61.7(3) . . . . ?
S1 Ru S3 C6 157.7(3) . . . . ?
O3 Ru O2 C9 -102.6(6) . . . . ?
N1 Ru O2 C9 -12.5(6) . . . . ?
S3 Ru O2 C9 78.6(6) . . . . ?
S2 Ru O2 C9 -116(2) . . . . ?
S1 Ru O2 C9 175.2(6) . . . . ?
O2 Ru O3 C7 103.1(6) . . . . ?
N1 Ru O3 C7 10.8(6) . . . . ?
S3 Ru O3 C7 122.5(18) . . . . ?
S2 Ru O3 C7 -77.6(5) . . . . ?
S1 Ru O3 C7 -173.2(6) . . . . ?
Ru O3 C7 O4 2.4(11) . . . . ?
Ru O3 C7 C8 -178.9(4) . . . 2_666 ?
Ru O2 C9 O1 -3.1(11) . . . . ?
Ru O2 C9 C8 179.4(4) . . . . ?
O1 C9 C8 C7 118.1(7) . . . 2_666 ?
O2 C9 C8 C7 -64.3(7) . . . 2_666 ?
O1 C9 C8 C10 -8.0(10) . . . . ?
O2 C9 C8 C10 169.6(6) . . . . ?
O1 C9 C8 C12 -110.8(8) . . . . ?
O2 C9 C8 C12 66.8(8) . . . . ?
C9 C8 C10 C11 -138.1(7) . . . . ?
C7 C8 C10 C11 96.5(7) 2_666 . . . ?
C12 C8 C10 C11 -18.8(6) . . . . ?
C8 C10 C11 C12 18.5(6) . . . . ?
C9 C8 C12 C11 136.9(7) . . . . ?
C7 C8 C12 C11 -94.1(7) 2_666 . . . ?
C10 C8 C12 C11 18.2(6) . . . . ?
C10 C11 C12 C8 -18.5(6) . . . . ?
