#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2006894.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_2006894
loop_
_publ_author_name
'Panneerselvam, K.'
'Lu, T.-H.'
'Huang, C.-H.'
'Tung, S.-F.'
'Shiu, K.-B.'
_publ_section_title
;
 Di-\m-acetato-bis[dicarbonyl(pyrazole)ruthenium(I)] and
 Di-\m-acetato-bis[dicarbonyl(3,5-dimethylpyrazole)ruthenium(I)]
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1782
_journal_page_last               1784
_journal_volume                  53
_journal_year                    1997
_chemical_formula_iupac          '[Ru2 (C2 H3 O2)2 (C5 H8 N2)2 (C O)4]'
_chemical_formula_moiety         'C9 H11 N2 O4 Ru'
_chemical_formula_sum            'C18 H22 N4 O8 Ru2'
_chemical_formula_weight         624.54
_chemical_name_systematic
;
Di-u-acetatobis(dicarbonyl(3,5-dimethylpyrazole)ruthenium(I))
;
_space_group_IT_number           36
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'B -2 -2b'
_symmetry_space_group_name_H-M   'B b 21 m'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.2920(10)
_cell_length_b                   13.7310(10)
_cell_length_c                   18.639(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.90
_cell_measurement_theta_min      14.78
_cell_volume                     2378.1(4)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'NRCVAX (Gabe et al., 1989)'
_computing_molecular_graphics    NRCVAX
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.70930
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_av_sigmaI/netI    0.0209
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1853
_diffrn_reflns_theta_max         29.90
_diffrn_reflns_theta_min         2.18
_diffrn_standards_decay_%        1
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.318
_exptl_absorpt_correction_T_max  0.719
_exptl_absorpt_correction_T_min  0.675
_exptl_absorpt_correction_type   '\y scan (North, Phillips & Mathews, 1989)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.744
_exptl_crystal_description       lump
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.861
_refine_diff_density_min         -0.848
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.199
_refine_ls_goodness_of_fit_obs   1.242
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         1853
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.198
_refine_ls_restrained_S_obs      1.241
_refine_ls_R_factor_all          0.054
_refine_ls_R_factor_obs          0.050
_refine_ls_shift/esd_max         0.048
_refine_ls_shift/esd_mean        0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
'calc w = 1/[\s^2^(Fo^2^)+(0.1137P)^2^+3.8418P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_wR_factor_all         0.169
_refine_ls_wR_factor_obs         0.168
_reflns_number_observed          1705
_reflns_number_total             1853
_reflns_observed_criterion       >2sigma(I)
_[local]_cod_data_source_file    ta1175.cif
_[local]_cod_data_source_block   II
_cod_original_cell_volume        2378.2(4)
_cod_database_code               2006894
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, z'
'-x, y+1/2, -z'
'x, y, -z'
'x+1/2, y, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Ru1 0.0427(3) 0.0376(3) 0.0238(3) -0.0010(4) -0.00210(10) 0.0022(4)
O1 0.047(3) 0.067(4) 0.025(2) 0.008(3) -0.005(2) -0.005(3)
O2 0.093(6) 0.046(4) 0.035(3) -0.017(4) -0.004(4) -0.005(3)
O3 0.133(9) 0.046(4) 0.077(6) -0.007(5) 0.003(6) 0.013(4)
O4 0.130(10) 0.175(18) 0.067(6) -0.070(12) -0.010(7) -0.014(9)
N1 0.054(3) 0.054(4) 0.025(3) -0.004(3) -0.001(3) 0.000(3)
N2 0.055(4) 0.056(4) 0.029(3) 0.000(3) -0.003(3) -0.006(3)
C1 0.050(4) 0.048(5) 0.028(3) -0.007(3) -0.008(3) 0.003(3)
C2 0.066(5) 0.074(6) 0.028(3) -0.019(5) 0.001(4) -0.008(4)
C3 0.055(5) 0.066(6) 0.041(4) -0.009(4) 0.003(4) -0.009(4)
C4 0.061(5) 0.073(7) 0.056(6) -0.003(5) -0.013(5) 0.021(6)
C5 0.075(6) 0.079(8) 0.050(5) 0.002(6) 0.017(5) -0.021(6)
C6 0.036(5) 0.053(6) 0.034(5) -0.003(4) 0.000 0.000
C7 0.040(6) 0.087(10) 0.040(6) 0.003(6) 0.000 0.000
C8 0.063(7) 0.041(5) 0.038(5) -0.020(5) 0.000 0.000
C9 0.092(11) 0.043(7) 0.053(8) -0.023(7) 0.000 0.000
C10 0.081(7) 0.045(5) 0.041(4) -0.005(5) -0.003(5) 0.004(4)
C11 0.068(7) 0.078(9) 0.052(6) -0.008(7) 0.004(5) 0.012(6)
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
Ru1 0.82698(5) 0.00080(11) 0.92804(2) 0.0347(2) Uani d . 1 Ru
O1 1.0429(7) -0.0497(6) 0.9408(3) 0.0460(10) Uani d . 1 O
O2 0.7713(11) -0.1462(6) 0.9408(4) 0.058(2) Uani d . 1 O
O3 0.9127(16) 0.2118(7) 0.9095(6) 0.085(3) Uani d . 1 O
O4 0.510(2) -0.0625(19) 0.9173(6) 0.124(7) Uani d . 1 O
N1 0.8591(9) -0.0468(7) 0.8163(4) 0.0440(10) Uani d . 1 N
N2 0.9501(8) -0.1240(6) 0.8066(4) 0.047(2) Uani d . 1 N
H1N2 0.9950(8) -0.1531(6) 0.8407(4) 0.080 Uiso calc R 1 H
C1 0.8064(10) -0.0237(7) 0.7533(5) 0.042(2) Uani d . 1 C
C2 0.8669(13) -0.0898(9) 0.7000(5) 0.056(2) Uani d . 1 C
H2 0.8463(13) -0.0916(9) 0.6512(5) 0.080 Uiso calc R 1 H
C3 0.9605(11) -0.1487(9) 0.7368(5) 0.054(2) Uani d . 1 C
C4 0.7066(12) 0.0550(11) 0.7408(7) 0.063(3) Uani d . 1 C
H41 0.6847(12) 0.0865(11) 0.7855(7) 0.080 Uiso calc R 1 H
H42 0.6197(12) 0.0296(11) 0.7201(7) 0.080 Uiso calc R 1 H
H43 0.7489(12) 0.1013(11) 0.7085(7) 0.080 Uiso calc R 1 H
C5 1.0574(13) -0.2267(10) 0.7147(6) 0.068(3) Uani d . 1 C
H51 1.1070(13) -0.2517(10) 0.7560(6) 0.080 Uiso calc R 1 H
H52 1.1261(13) -0.2017(10) 0.6810(6) 0.080 Uiso calc R 1 H
H53 1.0028(13) -0.2779(10) 0.6927(6) 0.080 Uiso calc R 1 H
C6 1.0997(12) -0.0639(9) 1.0000 0.041(2) Uani d S 1 C
C7 1.2523(14) -0.1023(14) 1.0000 0.056(3) Uani d S 1 C
C8 0.7612(15) -0.1893(10) 1.0000 0.047(3) Uani d S 1 C
C9 0.742(2) -0.2992(11) 1.0000 0.063(4) Uani d S 1 C
C10 0.8791(16) 0.1264(8) 0.9176(6) 0.056(2) Uani d . 1 C
C11 0.6490(17) -0.0441(15) 0.9214(7) 0.066(3) Uani d . 1 C
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'
Ru Ru -1.2594 0.8363 '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'
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
_geom_angle_publ_flag
C11 Ru1 C10 . . 125.3(8) yes
C11 Ru1 O2 . . 56.1(7) yes
C10 Ru1 O2 . . 178.7(5) yes
C11 Ru1 O1 . . 140.6(7) yes
C10 Ru1 O1 . . 94.0(5) yes
O2 Ru1 O1 . . 84.6(4) yes
C11 Ru1 N1 . . 87.5(5) yes
C10 Ru1 N1 . . 98.4(4) yes
O2 Ru1 N1 . . 81.7(3) yes
O1 Ru1 N1 . . 83.2(3) yes
C11 Ru1 Ru1 . 4_557 94.0(4) yes
C10 Ru1 Ru1 . 4_557 96.2(3) yes
O2 Ru1 Ru1 . 4_557 83.5(2) yes
O1 Ru1 Ru1 . 4_557 83.6(2) yes
N1 Ru1 Ru1 . 4_557 161.0(2) yes
C6 O1 Ru1 . . 123.4(6) no
C8 O2 C11 . . 119.1(10) no
C8 O2 Ru1 . . 124.9(7) no
C11 O2 Ru1 . . 52.9(6) no
C1 N1 N2 . . 107.5(7) no
C1 N1 Ru1 . . 136.4(7) no
N2 N1 Ru1 . . 116.0(5) no
C3 N2 N1 . . 111.6(8) no
C3 N2 H1N2 . . 124.2(6) no
N1 N2 H1N2 . . 124.2(4) no
N1 C1 C4 . . 124.4(9) no
N1 C1 C2 . . 108.4(9) no
C4 C1 C2 . . 127.2(9) no
C3 C2 C1 . . 105.7(8) no
C3 C2 H2 . . 127.1(6) no
C1 C2 H2 . . 127.1(6) no
N2 C3 C2 . . 106.8(9) no
N2 C3 C5 . . 120.1(10) no
C2 C3 C5 . . 133.1(10) no
C1 C4 H41 . . 109.5(6) no
C1 C4 H42 . . 109.5(6) no
H41 C4 H42 . . 109.5 no
C1 C4 H43 . . 109.5(6) no
H41 C4 H43 . . 109.5 no
H42 C4 H43 . . 109.5 no
C3 C5 H51 . . 109.5(6) no
C3 C5 H52 . . 109.5(7) no
H51 C5 H52 . . 109.5 no
C3 C5 H53 . . 109.5(6) no
H51 C5 H53 . . 109.5 no
H52 C5 H53 . . 109.5 no
O1 C6 O1 4_557 . 126.0(11) no
O1 C6 C7 4_557 . 117.0(6) no
O1 C6 C7 . . 117.0(6) no
O2 C8 O2 4_557 . 122.9(12) no
O2 C8 C9 4_557 . 118.5(6) no
O2 C8 C9 . . 118.5(6) no
O3 C10 Ru1 . . 178.8(12) no
O4 C11 Ru1 . . 171(2) no
O4 C11 O2 . . 118.1(17) no
Ru1 C11 O2 . . 71.0(7) no
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 C11 . 1.769(16) yes
Ru1 C10 . 1.802(12) yes
Ru1 O2 . 2.097(8) yes
Ru1 O1 . 2.136(7) yes
Ru1 N1 . 2.204(7) yes
Ru1 Ru1 4_557 2.6820(10) yes
O1 C6 . 1.239(8) no
O2 C8 . 1.255(9) no
O2 C11 . 1.84(2) no
O3 C10 . 1.223(15) no
O4 C11 . 1.32(2) no
N1 C1 . 1.311(11) no
N1 N2 . 1.367(12) no
N2 C3 . 1.347(12) no
N2 H1N2 . 0.86 no
C1 C4 . 1.44(2) no
C1 C2 . 1.457(14) no
C2 C3 . 1.37(2) no
C2 H2 . 0.93 no
C3 C5 . 1.46(2) no
C4 H41 . 0.96 no
C4 H42 . 0.96 no
C4 H43 . 0.96 no
C5 H51 . 0.96 no
C5 H52 . 0.96 no
C5 H53 . 0.96 no
C6 O1 4_557 1.239(8) no
C6 C7 . 1.51(2) no
C8 O2 4_557 1.255(9) no
C8 C9 . 1.52(2) no
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
_geom_hbond_publ_flag
N2 H1N2 O3 2_745 0.86 2.41 3.220(10) 157.4(3) yes