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#$Date: 2016-03-23 20:15:11 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179404 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/01/4330158.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_4330158
loop_
_publ_author_name
'Sayak Roy'
'Biprajit Sarkar'
'Hans-Georg Imrich'
'Jan Fiedler'
'Stanislav Záliš'
'Reyes Jimenez-Aparicio'
'Francisco A. Urbanos'
'Shaikh M. Mobin'
'Goutam Kumar Lahiri'
'Wolfgang Kaim'
_publ_section_title
;
 Charged, but Found "Not Guilty": Innocence of the Suspect Bridging
 Ligands [RO(O)CNNC(O)OR]2-= L2-in [(acac)2Ru(μ-L)Ru(acac)2]n,n= +,0,-,2-
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9273
_journal_page_last               9281
_journal_paper_doi               10.1021/ic300809w
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C28 H42 N2 O13 Ru2'
_chemical_formula_weight         816.79
_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                118.523(3)
_cell_angle_beta                 106.467(3)
_cell_angle_gamma                94.777(3)
_cell_formula_units_Z            1
_cell_length_a                   8.3121(4)
_cell_length_b                   10.9994(6)
_cell_length_c                   11.3339(5)
_cell_measurement_temperature    293(2)
_cell_volume                     843.21(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    Ortep3
_computing_publication_material  Shelx97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0521
_diffrn_reflns_av_sigmaI/netI    0.0538
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7081
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.72
_exptl_absorpt_coefficient_mu    0.959
_exptl_absorpt_correction_T_max  0.8167
_exptl_absorpt_correction_T_min  0.7425
_exptl_absorpt_process_details   multi-scan
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_F_000             416
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.819
_refine_diff_density_min         -1.034
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         3832
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0374
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0459P)²+0.4406P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0932
_refine_ls_wR_factor_ref         0.0999
_reflns_number_gt                3353
_reflns_number_total             3832
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300809w_si_002.cif
_cod_data_source_block           gklgera
_cod_original_cell_volume        843.21(7)
_cod_database_code               4330158
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
Ru1 Ru 0.07698(3) -0.06808(3) 0.67481(3) 0.03119(10) Uani 1 1 d .
O1 O 0.2135(3) 0.1338(3) 0.8223(2) 0.0349(5) Uani 1 1 d .
O2 O 0.2873(3) -0.1471(2) 0.6894(2) 0.0338(5) Uani 1 1 d .
O4 O 0.0658(3) -0.0958(3) 0.8365(2) 0.0350(5) Uani 1 1 d .
O5 O -0.0754(3) -0.2670(3) 0.5252(3) 0.0451(6) Uani 1 1 d .
O6 O -0.1318(3) 0.0205(3) 0.6618(2) 0.0385(5) Uani 1 1 d .
O7 O -0.2703(3) 0.1335(3) 0.5578(3) 0.0439(6) Uani 1 1 d .
N1 N 0.0629(3) -0.0375(3) 0.5137(3) 0.0380(6) Uani 1 1 d .
C1 C 0.4475(5) 0.3264(4) 1.0079(5) 0.0538(10) Uani 1 1 d .
H1A H 0.4246 0.3795 0.9607 0.081 Uiso 1 1 calc R
H1B H 0.5706 0.3470 1.0557 0.081 Uiso 1 1 calc R
H1C H 0.3930 0.3535 1.0777 0.081 Uiso 1 1 calc R
C2 C 0.3762(4) 0.1691(4) 0.8979(4) 0.0372(7) Uani 1 1 d .
C3 C 0.4825(4) 0.0775(4) 0.8823(4) 0.0410(8) Uani 1 1 d .
H3 H 0.5973 0.1183 0.9464 0.049 Uiso 1 1 calc R
C4 C 0.4382(4) -0.0708(4) 0.7808(4) 0.0344(6) Uani 1 1 d .
C5 C 0.5828(4) -0.1445(4) 0.7780(4) 0.0438(8) Uani 1 1 d .
H5A H 0.5348 -0.2460 0.7284 0.066 Uiso 1 1 calc R
H5B H 0.6585 -0.1101 0.8752 0.066 Uiso 1 1 calc R
H5C H 0.6475 -0.1243 0.7285 0.066 Uiso 1 1 calc R
C6 C 0.0159(5) -0.2125(4) 0.9560(4) 0.0438(8) Uani 1 1 d .
H6A H 0.1254 -0.1488 1.0300 0.066 Uiso 1 1 calc R
H6B H 0.0115 -0.3075 0.9379 0.066 Uiso 1 1 calc R
H6C H -0.0767 -0.1806 0.9871 0.066 Uiso 1 1 calc R
C7 C -0.0032(4) -0.2132(4) 0.8205(4) 0.0363(7) Uani 1 1 d .
C8 C -0.0948(5) -0.3397(4) 0.6874(5) 0.0491(9) Uani 1 1 d .
H8 H -0.1366 -0.4186 0.6908 0.059 Uiso 1 1 calc R
C9 C -0.1297(4) -0.3599(4) 0.5526(4) 0.0475(9) Uani 1 1 d .
C10 C -0.2445(6) -0.5009(5) 0.4210(5) 0.0703(15) Uani 1 1 d .
H10A H -0.3617 -0.4932 0.3924 0.106 Uiso 1 1 calc R
H10B H -0.2411 -0.5747 0.4434 0.106 Uiso 1 1 calc R
H10C H -0.2037 -0.5244 0.3434 0.106 Uiso 1 1 calc R
C11 C -0.1515(4) 0.0627(4) 0.5739(3) 0.0372(7) Uani 1 1 d .
C12 C -0.3256(4) 0.2085(4) 0.6789(4) 0.0372(7) Uani 1 1 d .
H12 H -0.3568 0.1446 0.7109 0.045 Uiso 1 1 calc R
C13 C -0.4824(5) 0.2503(5) 0.6202(5) 0.0554(10) Uani 1 1 d .
H13A H -0.4503 0.3119 0.5882 0.083 Uiso 1 1 calc R
H13B H -0.5273 0.2999 0.6946 0.083 Uiso 1 1 calc R
H13C H -0.5697 0.1659 0.5404 0.083 Uiso 1 1 calc R
C14 C -0.1795(8) 0.3363(5) 0.7997(5) 0.0768(16) Uani 1 1 d .
H14A H -0.0797 0.3047 0.8291 0.115 Uiso 1 1 calc R
H14B H -0.2148 0.3873 0.8802 0.115 Uiso 1 1 calc R
H14C H -0.1509 0.3983 0.7672 0.115 Uiso 1 1 calc R
O111 O -0.1892(9) -0.3838(7) 0.2195(7) 0.0691(18) Uani 0.50 1 d P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2590 0.8360 '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
N1 Ru1 O1 92.00(11) . .
N1 Ru1 O5 87.48(13) . .
O1 Ru1 O5 176.12(9) . .
N1 Ru1 O2 100.53(10) . .
O1 Ru1 O2 93.90(9) . .
O5 Ru1 O2 89.98(9) . .
N1 Ru1 O4 173.91(9) . .
O1 Ru1 O4 88.84(9) . .
O5 Ru1 O4 91.27(11) . .
O2 Ru1 O4 85.43(9) . .
N1 Ru1 O6 78.33(10) . .
O1 Ru1 O6 84.08(10) . .
O5 Ru1 O6 92.05(10) . .
O2 Ru1 O6 177.62(9) . .
O4 Ru1 O6 95.77(9) . .
C2 O1 Ru1 123.4(2) . .
C4 O2 Ru1 123.1(2) . .
C7 O4 Ru1 125.3(2) . .
C9 O5 Ru1 125.0(2) . .
C11 O6 Ru1 111.70(18) . .
C11 O7 C12 116.5(3) . .
C11 N1 N1 109.6(3) 2_556 2_556
C11 N1 Ru1 135.0(2) 2_556 .
N1 N1 Ru1 115.3(3) 2_556 .
C2 C1 H1A 109.5 . .
C2 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
C2 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
O1 C2 C3 125.8(3) . .
O1 C2 C1 113.5(3) . .
C3 C2 C1 120.7(3) . .
C2 C3 C4 127.8(3) . .
C2 C3 H3 116.1 . .
C4 C3 H3 116.1 . .
O2 C4 C3 125.6(3) . .
O2 C4 C5 117.1(3) . .
C3 C4 C5 117.3(3) . .
C4 C5 H5A 109.5 . .
C4 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
C4 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
C7 C6 H6A 109.5 . .
C7 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
C7 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
O4 C7 C8 125.0(3) . .
O4 C7 C6 116.3(3) . .
C8 C7 C6 118.7(3) . .
C9 C8 C7 127.1(4) . .
C9 C8 H8 116.5 . .
C7 C8 H8 116.5 . .
O5 C9 C8 125.9(3) . .
O5 C9 C10 114.6(4) . .
C8 C9 C10 119.5(4) . .
C9 C10 H10A 109.5 . .
C9 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C9 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
O6 C11 O7 121.4(3) . .
O6 C11 N1 124.5(3) . 2_556
O7 C11 N1 114.0(3) . 2_556
O7 C12 C13 104.7(3) . .
O7 C12 C14 108.6(3) . .
C13 C12 C14 112.4(4) . .
O7 C12 H12 110.3 . .
C13 C12 H12 110.3 . .
C14 C12 H12 110.3 . .
C12 C13 H13A 109.5 . .
C12 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
C12 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
C12 C14 H14A 109.5 . .
C12 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C12 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ru1 N1 1.984(3) .
Ru1 O1 1.993(2) .
Ru1 O5 2.011(3) .
Ru1 O2 2.016(2) .
Ru1 O4 2.021(2) .
Ru1 O6 2.063(2) .
O1 C2 1.285(4) .
O2 C4 1.268(4) .
O4 C7 1.274(4) .
O5 C9 1.285(5) .
O6 C11 1.263(4) .
O7 C11 1.333(4) .
O7 C12 1.454(4) .
N1 C11 1.338(4) 2_556
N1 N1 1.440(5) 2_556
C1 C2 1.500(5) .
C1 H1A 0.9600 .
C1 H1B 0.9600 .
C1 H1C 0.9600 .
C2 C3 1.376(5) .
C3 C4 1.410(5) .
C3 H3 0.9300 .
C4 C5 1.504(4) .
C5 H5A 0.9600 .
C5 H5B 0.9600 .
C5 H5C 0.9600 .
C6 C7 1.494(5) .
C6 H6A 0.9600 .
C6 H6B 0.9600 .
C6 H6C 0.9600 .
C7 C8 1.400(5) .
C8 C9 1.372(6) .
C8 H8 0.9300 .
C9 C10 1.510(5) .
C10 H10A 0.9600 .
C10 H10B 0.9600 .
C10 H10C 0.9600 .
C11 N1 1.338(4) 2_556
C12 C13 1.501(5) .
C12 C14 1.503(5) .
C12 H12 0.9800 .
C13 H13A 0.9600 .
C13 H13B 0.9600 .
C13 H13C 0.9600 .
C14 H14A 0.9600 .
C14 H14B 0.9600 .
C14 H14C 0.9600 .
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_4
N1 Ru1 O1 C2 -107.7(2) .
O5 Ru1 O1 C2 170.1(14) .
O2 Ru1 O1 C2 -7.0(2) .
O4 Ru1 O1 C2 78.4(2) .
O6 Ru1 O1 C2 174.3(2) .
N1 Ru1 O2 C4 97.8(3) .
O1 Ru1 O2 C4 5.1(3) .
O5 Ru1 O2 C4 -174.7(3) .
O4 Ru1 O2 C4 -83.4(3) .
O6 Ru1 O2 C4 37(2) .
N1 Ru1 O4 C7 85.2(11) .
O1 Ru1 O4 C7 -176.8(2) .
O5 Ru1 O4 C7 7.0(2) .
O2 Ru1 O4 C7 -82.8(2) .
O6 Ru1 O4 C7 99.2(2) .
N1 Ru1 O5 C9 -178.8(3) .
O1 Ru1 O5 C9 -96.4(15) .
O2 Ru1 O5 C9 80.7(3) .
O4 Ru1 O5 C9 -4.7(3) .
O6 Ru1 O5 C9 -100.5(3) .
N1 Ru1 O6 C11 -7.0(2) .
O1 Ru1 O6 C11 86.2(2) .
O5 Ru1 O6 C11 -94.1(2) .
O2 Ru1 O6 C11 55(2) .
O4 Ru1 O6 C11 174.5(2) .
O1 Ru1 N1 C11 97.3(4) 2_556
O5 Ru1 N1 C11 -86.6(4) 2_556
O2 Ru1 N1 C11 3.0(4) 2_556
O4 Ru1 N1 C11 -164.9(8) 2_556
O6 Ru1 N1 C11 -179.2(4) 2_556
O1 Ru1 N1 N1 -77.8(3) 2_556
O5 Ru1 N1 N1 98.4(3) 2_556
O2 Ru1 N1 N1 -172.1(3) 2_556
O4 Ru1 N1 N1 20.0(13) 2_556
O6 Ru1 N1 N1 5.7(3) 2_556
Ru1 O1 C2 C3 5.0(5) .
Ru1 O1 C2 C1 -176.5(2) .
O1 C2 C3 C4 1.4(6) .
C1 C2 C3 C4 -177.0(4) .
Ru1 O2 C4 C3 -1.1(5) .
Ru1 O2 C4 C5 -179.5(2) .
C2 C3 C4 O2 -3.6(6) .
C2 C3 C4 C5 174.8(3) .
Ru1 O4 C7 C8 -5.3(4) .
Ru1 O4 C7 C6 175.1(2) .
O4 C7 C8 C9 -1.4(6) .
C6 C7 C8 C9 178.1(4) .
Ru1 O5 C9 C8 0.5(5) .
Ru1 O5 C9 C10 179.3(2) .
C7 C8 C9 O5 4.1(6) .
C7 C8 C9 C10 -174.6(3) .
Ru1 O6 C11 O7 -174.6(3) .
Ru1 O6 C11 N1 7.9(4) 2_556
C12 O7 C11 O6 23.6(5) .
C12 O7 C11 N1 -158.6(3) 2_556
C11 O7 C12 C13 -168.3(3) .
C11 O7 C12 C14 71.4(4) .
