#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/10/2211089.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2211089
loop_
_publ_author_name
'Fuma, Yasuhiro'
'Ebihara, Masahiro'
_publ_section_title
;Tetra-μ-acetamidato-κ⁴N:O;κ⁴O:N-bis[aquaruthenium(II,III)](Ru{---Ru)}
 perchlorate
;
_journal_coeditor_code           KP2034
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2802
_journal_page_last               m2804
_journal_paper_doi               10.1107/S1600536806039298
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Ru2 (C2 H4 N O)4 (H2 O)2] Cl O4'
_chemical_formula_moiety         'C8 H20 N4 O6 Ru2 +, Cl O4 -'
_chemical_formula_sum            'C8 H20 Cl N4 O10 Ru2'
_chemical_formula_weight         569.87
_chemical_name_systematic
;
Tetra-μ-acetamidato-κ⁴N:O;κ⁴O:N-diaquadiruthenium(II,III)(Ru---Ru)
perchlorate
;
_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                109.882(4)
_cell_angle_beta                 98.696(4)
_cell_angle_gamma                104.705(4)
_cell_formula_units_Z            2
_cell_length_a                   7.704(4)
_cell_length_b                   11.454(6)
_cell_length_c                   11.686(6)
_cell_measurement_reflns_used    2208
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.5
_cell_volume                     905.4(8)
_computing_cell_refinement       CrystalClear
_computing_data_collection
'CrystalClear (Molecular Structure Corporation & Rigaku, 2001)'
_computing_data_reduction        'TEXSAN (Rigaku/MSC, 2004)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  'SHELXL97 and TEXSAN'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al.,  1999)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 14.62
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_av_sigmaI/netI    0.0298
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7392
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.49
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.871
_exptl_absorpt_correction_T_max  0.825
_exptl_absorpt_correction_T_min  0.753
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1999)'
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    2.091
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             562
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.457
_refine_diff_density_min         -0.467
_refine_ls_extinction_coef       0.0045(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         4086
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0310
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0297P)²+0.3098P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0627
_refine_ls_wR_factor_ref         0.0694
_reflns_number_gt                3025
_reflns_number_total             4086
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            kp2034.cif
_cod_data_source_block           I
_cod_database_code               2211089
_cod_database_fobs_code          2211089
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_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
Ru Ru1 0.38565(3) 0.51790(2) 1.04840(2) 0.00755(9) Uani d . 1 . .
N N1 0.3533(4) 0.3414(2) 1.0606(2) 0.0120(6) Uani d . 1 . .
H H1 0.2654 0.3117 1.0937 0.014 Uiso calc R 1 . .
O O1 0.5789(3) 0.3046(2) 0.96454(19) 0.0124(5) Uani d . 1 . .
N N2 0.4183(4) 0.3950(2) 0.7862(2) 0.0120(6) Uani d . 1 . .
H H2 0.4507 0.3579 0.7172 0.014 Uiso calc R 1 . .
O O2 0.1898(3) 0.4340(2) 0.87734(19) 0.0114(5) Uani d . 1 . .
O O5 0.1581(4) 0.5388(3) 1.1549(2) 0.0168(6) Uani d . 1 . .
H H3 0.110(6) 0.483(4) 1.161(4) 0.025 Uiso d . 1 . .
H H4 0.082(6) 0.566(4) 1.141(4) 0.025 Uiso d . 1 . .
Ru Ru2 0.38694(3) 0.02088(2) 0.54850(2) 0.00746(9) Uani d . 1 . .
N N3 0.6680(4) 0.1626(2) 0.4523(2) 0.0118(6) Uani d . 1 . .
H H5 0.7581 0.1906 0.4201 0.014 Uiso calc R 1 . .
O O3 0.4440(3) 0.2045(2) 0.54699(19) 0.0119(5) Uani d . 1 . .
N N4 0.5813(3) 0.0960(2) 0.7154(2) 0.0100(5) Uani d . 1 . .
H H6 0.5500 0.1324 0.7851 0.012 Uiso calc R 1 . .
O O4 0.8045(3) 0.0479(2) 0.62249(19) 0.0103(5) Uani d . 1 . .
O O6 0.1655(3) 0.0477(3) 0.6584(2) 0.0162(6) Uani d . 1 . .
H H7 0.070(6) 0.049(4) 0.642(4) 0.024 Uiso d . 1 . .
H H8 0.156(6) 0.005(4) 0.691(4) 0.024 Uiso d . 1 . .
C C1 0.4569(4) 0.2699(3) 1.0217(3) 0.0113(7) Uani d . 1 . .
C C2 0.4423(5) 0.1452(3) 1.0418(3) 0.0204(8) Uani d . 1 . .
H H9 0.4060 0.0710 0.9600 0.031 Uiso calc R 1 . .
H H10 0.3486 0.1305 1.0881 0.031 Uiso calc R 1 . .
H H11 0.5630 0.1527 1.0905 0.031 Uiso calc R 1 . .
C C3 0.2464(4) 0.3909(3) 0.7764(3) 0.0095(6) Uani d . 1 . .
C C4 0.1090(4) 0.3409(3) 0.6522(3) 0.0170(7) Uani d . 1 . .
H H12 0.1599 0.2952 0.5851 0.026 Uiso calc R 1 . .
H H13 0.0829 0.4149 0.6377 0.026 Uiso calc R 1 . .
H H14 -0.0063 0.2799 0.6519 0.026 Uiso calc R 1 . .
C C5 0.5766(4) 0.2409(3) 0.4982(3) 0.0106(6) Uani d . 1 . .
C C6 0.6145(5) 0.3739(3) 0.4940(3) 0.0202(8) Uani d . 1 . .
H H15 0.5037 0.3768 0.4429 0.030 Uiso calc R 1 . .
H H16 0.7187 0.3912 0.4565 0.030 Uiso calc R 1 . .
H H17 0.6460 0.4407 0.5798 0.030 Uiso calc R 1 . .
C C7 0.7499(4) 0.0929(3) 0.7240(3) 0.0115(7) Uani d . 1 . .
C C8 0.8862(4) 0.1385(3) 0.8479(3) 0.0157(7) Uani d . 1 . .
H H18 0.8371 0.1854 0.9155 0.023 Uiso calc R 1 . .
H H19 1.0039 0.1976 0.8490 0.023 Uiso calc R 1 . .
H H20 0.9072 0.0625 0.8608 0.023 Uiso calc R 1 . .
Cl Cl1 1.00650(12) 0.24343(9) 0.25251(8) 0.01977(18) Uani d . 1 A 1
O O7 0.9754(5) 0.3000(3) 0.1628(3) 0.0521(9) Uani d . 1 A 1
O O8 1.1889(4) 0.2348(4) 0.2667(4) 0.0691(12) Uani d . 1 A 1
O O9 0.8699(4) 0.1145(3) 0.2057(2) 0.0347(7) Uani d . 1 A 1
O O10 0.9878(4) 0.3230(3) 0.3702(2) 0.0448(8) Uani d . 1 A 1
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'
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 0.0060 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
N2 Ru1 N1 2_667 . 89.42(11)
N2 Ru1 O1 2_667 2_667 90.42(10)
N1 Ru1 O1 . 2_667 179.29(9)
N2 Ru1 O2 2_667 . 177.97(9)
N1 Ru1 O2 . . 92.36(10)
O1 Ru1 O2 2_667 . 87.79(9)
N2 Ru1 Ru1 2_667 2_667 87.85(8)
N1 Ru1 Ru1 . 2_667 86.68(7)
O1 Ru1 Ru1 2_667 2_667 92.63(6)
O2 Ru1 Ru1 . 2_667 91.28(7)
N2 Ru1 O5 2_667 . 90.02(10)
N1 Ru1 O5 . . 87.88(9)
O1 Ru1 O5 2_667 . 92.81(8)
O2 Ru1 O5 . . 91.02(10)
Ru1 Ru1 O5 2_667 . 174.18(6)
C1 N1 Ru1 . . 123.0(2)
C1 N1 H1 . . 118.5
Ru1 N1 H1 . . 118.5
C1 O1 Ru1 . 2_667 116.70(17)
C3 N2 Ru1 . 2_667 123.2(2)
C3 N2 H2 . . 118.4
Ru1 N2 H2 2_667 . 118.4
C3 O2 Ru1 . . 117.37(19)
Ru1 O5 H3 . . 116(3)
Ru1 O5 H4 . . 126(3)
H3 O5 H4 . . 101(4)
N4 Ru2 N3 . 2_656 90.65(10)
N4 Ru2 O3 . . 89.68(9)
N3 Ru2 O3 2_656 . 179.10(8)
N4 Ru2 O4 . 2_656 177.35(9)
N3 Ru2 O4 2_656 2_656 91.82(9)
O3 Ru2 O4 . 2_656 87.84(8)
N4 Ru2 Ru2 . 2_656 87.79(8)
N3 Ru2 Ru2 2_656 2_656 86.60(7)
O3 Ru2 Ru2 . 2_656 92.57(6)
O4 Ru2 Ru2 2_656 2_656 91.37(7)
N4 Ru2 O6 . . 88.73(10)
N3 Ru2 O6 2_656 . 87.73(9)
O3 Ru2 O6 . . 93.12(8)
O4 Ru2 O6 2_656 . 92.35(10)
Ru2 Ru2 O6 2_656 . 173.31(6)
C5 N3 Ru2 . 2_656 123.3(2)
C5 N3 H5 . . 118.4
Ru2 N3 H5 2_656 . 118.4
C5 O3 Ru2 . . 116.93(17)
C7 N4 Ru2 . . 122.9(2)
C7 N4 H6 . . 118.6
Ru2 N4 H6 . . 118.6
C7 O4 Ru2 . 2_656 117.64(19)
Ru2 O6 H7 . . 135(3)
Ru2 O6 H8 . . 109(3)
H7 O6 H8 . . 102(4)
O1 C1 N1 . . 120.8(3)
O1 C1 C2 . . 116.9(3)
N1 C1 C2 . . 122.3(3)
C1 C2 H9 . . 109.5
C1 C2 H10 . . 109.5
H9 C2 H10 . . 109.5
C1 C2 H11 . . 109.5
H9 C2 H11 . . 109.5
H10 C2 H11 . . 109.5
N2 C3 O2 . . 120.1(3)
N2 C3 C4 . . 122.4(3)
O2 C3 C4 . . 117.5(3)
C3 C4 H12 . . 109.5
C3 C4 H13 . . 109.5
H12 C4 H13 . . 109.5
C3 C4 H14 . . 109.5
H12 C4 H14 . . 109.5
H13 C4 H14 . . 109.5
O3 C5 N3 . . 120.6(3)
O3 C5 C6 . . 116.8(3)
N3 C5 C6 . . 122.6(3)
C5 C6 H15 . . 109.5
C5 C6 H16 . . 109.5
H15 C6 H16 . . 109.5
C5 C6 H17 . . 109.5
H15 C6 H17 . . 109.5
H16 C6 H17 . . 109.5
N4 C7 O4 . . 120.1(3)
N4 C7 C8 . . 122.1(3)
O4 C7 C8 . . 117.8(3)
C7 C8 H18 . . 109.5
C7 C8 H19 . . 109.5
H18 C8 H19 . . 109.5
C7 C8 H20 . . 109.5
H18 C8 H20 . . 109.5
H19 C8 H20 . . 109.5
O10 Cl1 O8 . . 109.9(2)
O10 Cl1 O7 . . 109.8(2)
O8 Cl1 O7 . . 108.8(2)
O10 Cl1 O9 . . 109.70(18)
O8 Cl1 O9 . . 110.4(2)
O7 Cl1 O9 . . 108.15(17)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ru1 Ru1 2_667 2.2817(10) y
Ru1 O1 2_667 2.042(2) y
Ru1 O2 . 2.060(2) y
Ru1 O5 . 2.312(2) y
Ru1 N1 . 2.030(3) y
Ru1 N2 2_667 2.013(3) y
N1 C1 . 1.304(4) ?
N1 H1 . 0.8800 ?
O1 C1 . 1.292(4) ?
N2 C3 . 1.299(4) ?
N2 H2 . 0.8800 ?
O2 C3 . 1.302(3) ?
O5 H3 . 0.69(4) ?
O5 H4 . 0.75(4) ?
Ru2 Ru2 2_656 2.2804(10) y
Ru2 O3 . 2.044(2) y
Ru2 O4 2_656 2.058(2) y
Ru2 O6 . 2.305(2) y
Ru2 N3 2_656 2.032(3) y
Ru2 N4 . 2.027(3) y
N3 C5 . 1.302(4) ?
N3 H5 . 0.8800 ?
O3 C5 . 1.290(4) ?
N4 C7 . 1.299(4) ?
N4 H6 . 0.8800 ?
O4 C7 . 1.302(3) ?
O6 H7 . 0.73(4) ?
O6 H8 . 0.71(4) ?
C1 C2 . 1.504(4) ?
C2 H9 . 0.9800 ?
C2 H10 . 0.9800 ?
C2 H11 . 0.9800 ?
C3 C4 . 1.490(4) ?
C4 H12 . 0.9800 ?
C4 H13 . 0.9800 ?
C4 H14 . 0.9800 ?
C5 C6 . 1.496(4) ?
C6 H15 . 0.9800 ?
C6 H16 . 0.9800 ?
C6 H17 . 0.9800 ?
C7 C8 . 1.490(4) ?
C8 H18 . 0.9800 ?
C8 H19 . 0.9800 ?
C8 H20 . 0.9800 ?
Cl1 O10 . 1.421(3) ?
Cl1 O8 . 1.422(3) ?
Cl1 O7 . 1.429(3) ?
Cl1 O9 . 1.441(3) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O5 H4 O2 2_567 0.75(4) 2.07(4) 2.761(3) 152(4)
O5 H3 O7 1_456 0.69(4) 2.09(4) 2.780(4) 173(4)
O6 H7 O4 1_455 0.73(4) 2.02(4) 2.750(3) 171(4)
O6 H8 O9 2_656 0.71(4) 2.10(4) 2.816(4) 178(4)
N1 H1 O7 1_456 0.88 2.48 3.296(4) 155.2
N1 H1 O8 1_456 0.88 2.55 3.321(5) 146.2
N2 H2 O3 . 0.88 2.14 2.975(3) 157.5
N3 H5 O10 . 0.88 2.31 3.159(4) 163.0
N4 H6 O1 . 0.88 2.27 3.081(3) 152.8
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_site_symmetry_1
_geom_torsion
N2 Ru1 N1 C1 2_667 -85.6(3)
O2 Ru1 N1 C1 . 93.4(3)
Ru1 Ru1 N1 C1 2_667 2.3(2)
O5 Ru1 N1 C1 . -175.6(3)
N1 Ru1 O2 C3 . -87.0(2)
O1 Ru1 O2 C3 2_667 92.3(2)
Ru1 Ru1 O2 C3 2_667 -0.2(2)
O5 Ru1 O2 C3 . -174.9(2)
N4 Ru2 O3 C5 . 87.4(2)
O4 Ru2 O3 C5 2_656 -91.7(2)
Ru2 Ru2 O3 C5 2_656 -0.4(2)
O6 Ru2 O3 C5 . 176.1(2)
N3 Ru2 N4 C7 2_656 81.9(3)
O3 Ru2 N4 C7 . -97.2(3)
Ru2 Ru2 N4 C7 2_656 -4.6(2)
O6 Ru2 N4 C7 . 169.7(3)
Ru1 O1 C1 N1 2_667 4.8(4)
Ru1 O1 C1 C2 2_667 -174.7(2)
Ru1 N1 C1 O1 . -4.9(4)
Ru1 N1 C1 C2 . 174.5(2)
Ru1 N2 C3 O2 2_667 -6.2(4)
Ru1 N2 C3 C4 2_667 172.2(2)
Ru1 O2 C3 N2 . 3.8(4)
Ru1 O2 C3 C4 . -174.7(2)
Ru2 O3 C5 N3 . 0.1(4)
Ru2 O3 C5 C6 . 178.3(2)
Ru2 N3 C5 O3 2_656 0.3(4)
Ru2 N3 C5 C6 2_656 -177.8(2)
Ru2 N4 C7 O4 . 4.7(4)
Ru2 N4 C7 C8 . -174.8(2)
Ru2 O4 C7 N4 2_656 -1.5(4)
Ru2 O4 C7 C8 2_656 178.0(2)
