#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/16/4341612.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_4341612
loop_
_publ_author_name
'Fritsch, Nico'
'Wick, Christian R.'
'Waidmann, Thomas'
'Dral, Pavlo O.'
'Tucher, Johannes'
'Heinemann, Frank W.'
'Shubina, Tatyana E.'
'Clark, Timothy'
'Burzlaff, Nicolai'
_publ_section_title
;
 Multiply Bonded Metal(II) Acetate (Rhodium, Ruthenium, and Molybdenum)
 Complexes with the trans-1,2-Bis(N-methylimidazol-2-yl)ethylene Ligand.
;
_journal_name_full               'Inorganic chemistry'
_journal_page_first              141113134903008
_journal_paper_doi               10.1021/ic501435a
_journal_year                    2014
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C9 H12 N2 O4 Ru, 0.5(C4 H8 O)'
_chemical_formula_sum            'C11 H16 N2 O4.5 Ru'
_chemical_formula_weight         349.33
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_date             2014-04-10T17:05:09-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                105.369(12)
_cell_angle_beta                 107.452(7)
_cell_angle_gamma                93.312(10)
_cell_formula_units_Z            2
_cell_length_a                   8.2774(8)
_cell_length_b                   8.3739(17)
_cell_length_c                   10.5985(11)
_cell_measurement_reflns_used    28
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      6
_cell_measurement_wavelength     0.71073
_cell_volume                     668.18(18)
_computing_cell_refinement       'EVALCCD (Duisenberg, 2003)'
_computing_data_collection       'COLLECT (Bruker-Nonius, 2002)'
_computing_data_reduction        'EVALCCD (Duisenberg, 2003)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method
;
 φ- and ω-rotations with 1.60 ° and 192 sec per frame
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0712
_diffrn_reflns_av_unetI/netI     0.0775
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7188
_diffrn_reflns_theta_full        26.5
_diffrn_reflns_theta_max         26.5
_diffrn_reflns_theta_min         6.25
_exptl_absorpt_coefficient_mu    1.186
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.3785
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2002'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.736
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             352
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.104
_exptl_crystal_size_min          0.067
_refine_diff_density_max         2.291
_refine_diff_density_min         -3.417
_refine_diff_density_rms         0.228
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         2723
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0924
_refine_ls_R_factor_gt           0.077
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1704P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.206
_refine_ls_wR_factor_ref         0.2228
_reflns_number_gt                2193
_reflns_number_total             2723
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic501435a_si_002.cif
_cod_data_source_block           compound2
_cod_original_cell_volume        668.18(17)
_cod_original_formula_sum        'C11 H16 N2 O4.50 Ru'
_cod_database_code               4341612
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
C1 C 0.6448(10) 0.7970(9) 0.5142(8) 0.0360(17) Uani 1 1 d . . .
C2 C 0.7245(12) 0.9694(11) 0.5257(11) 0.055(2) Uani 1 1 d . . .
H2A H 0.6914 1.0521 0.5915 0.082 Uiso 1 1 calc R . .
H2B H 0.6858 0.989 0.437 0.082 Uiso 1 1 calc R . .
H2C H 0.847 0.9766 0.556 0.082 Uiso 1 1 calc R . .
C3 C 0.2435(10) 0.6396(10) 0.5614(8) 0.0341(16) Uani 1 1 d . . .
C4 C 0.0967(10) 0.7205(11) 0.5973(9) 0.0404(18) Uani 1 1 d . . .
H4A H 0.1412 0.8274 0.6659 0.061 Uiso 1 1 calc R . .
H4B H 0.0386 0.6497 0.633 0.061 Uiso 1 1 calc R . .
H4C H 0.0178 0.7356 0.5155 0.061 Uiso 1 1 calc R . .
C11 C 0.6981(9) 0.5752(10) 0.9580(7) 0.0316(16) Uani 1 1 d . . .
C12 C 0.9621(12) 0.7102(13) 1.0356(9) 0.054(2) Uani 1 1 d . . .
H12 H 1.0704 0.766 1.0929 0.065 Uiso 1 1 calc R . .
C13 C 0.8968(11) 0.6758(13) 0.8956(9) 0.052(2) Uani 1 1 d . . .
H13 H 0.9544 0.7052 0.8401 0.062 Uiso 1 1 calc R . .
C14 C 0.8577(13) 0.6471(17) 1.2170(10) 0.064(3) Uani 1 1 d . . .
H14A H 0.8021 0.7339 1.2582 0.097 Uiso 1 1 calc R . .
H14B H 0.9777 0.6677 1.2692 0.097 Uiso 1 1 calc R . .
H14C H 0.8081 0.5407 1.2173 0.097 Uiso 1 1 calc R . .
C15 C 0.5330(10) 0.4949(11) 0.9491(8) 0.0380(17) Uani 1 1 d . . .
H15 H 0.4648 0.4283 0.8616 0.046 Uiso 1 1 calc R . .
N11 N 0.8353(9) 0.6454(11) 1.0750(7) 0.0467(18) Uani 1 1 d . . .
N12 N 0.7320(9) 0.5907(9) 0.8483(7) 0.0398(16) Uani 1 1 d . . .
O1 O 0.6819(8) 0.7520(7) 0.6215(6) 0.0435(14) Uani 1 1 d . . .
O2 O 0.5449(8) 0.7087(7) 0.3966(6) 0.0431(14) Uani 1 1 d . . .
O3 O 0.7703(7) 0.4107(7) 0.5649(5) 0.0344(12) Uani 1 1 d . . .
O5 O 0.3668(7) 0.6286(7) 0.6605(6) 0.0376(12) Uani 1 1 d . . .
C40 C 0.645(3) 0.961(3) 0.138(3) 0.076(7) Uani 0.5 1 d PDU A 1
H40A H 0.7226 1.0233 0.2292 0.091 Uiso 0.5 1 calc PR A 1
H40B H 0.6751 0.85 0.1084 0.091 Uiso 0.5 1 calc PR A 1
C41 C 0.623(4) 1.055(7) 0.032(4) 0.086(9) Uani 0.5 1 d PDU . 1
H41A H 0.7132 1.034 -0.0091 0.103 Uiso 0.5 1 calc PR . 1
H41B H 0.6434 1.1741 0.0809 0.103 Uiso 0.5 1 calc PR . 1
C42 C 0.548(5) 0.981(5) 0.087(4) 0.108(9) Uani 0.5 1 d PDU . 2
H42A H 0.5449 1.0671 0.1676 0.13 Uiso 0.5 1 calc PR . 2
H42B H 0.5775 0.8811 0.1119 0.13 Uiso 0.5 1 calc PR . 2
C43 C 0.670(6) 1.042(9) 0.021(5) 0.113(11) Uani 0.5 1 d PDU . 2
H43A H 0.754 0.9673 0.013 0.136 Uiso 0.5 1 calc PR . 2
H43B H 0.7297 1.154 0.0759 0.136 Uiso 0.5 1 calc PR . 2
O40 O 0.451(3) 0.958(4) 0.127(4) 0.160(14) Uani 0.5 1 d PD . .
Ru1 Ru 0.57043(7) 0.52199(7) 0.61505(5) 0.0290(3) Uani 1 1 d . . .
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 0 '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 0.006 '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
O1 C1 O2 124.8(7) . .
O1 C1 C2 117.5(7) . .
O2 C1 C2 117.7(7) . .
O5 C3 O3 126.0(7) . 2_666
O5 C3 C4 116.9(7) . .
O3 C3 C4 117.1(7) 2_666 .
N12 C11 N11 110.8(7) . .
N12 C11 C15 122.1(7) . .
N11 C11 C15 127.2(7) . .
C13 C12 N11 105.8(7) . .
C12 C13 N12 109.7(7) . .
C15 C15 C11 128.0(10) 2_667 .
C11 N11 C12 107.4(7) . .
C11 N11 C14 129.2(9) . .
C12 N11 C14 123.3(8) . .
C11 N12 C13 106.2(7) . .
C11 N12 Ru1 133.4(5) . .
C13 N12 Ru1 120.2(5) . .
C1 O1 Ru1 119.6(6) . .
C1 O2 Ru1 117.0(5) . 2_666
C3 O3 Ru1 117.4(5) 2_666 .
C3 O5 Ru1 117.8(5) . .
C41 C40 O40 91(3) . .
C40 C41 C42 118(3) . 2_675
C40 C41 C41 83(2) . 2_675
C42 C41 C41 37(2) 2_675 2_675
C43 C42 C41 101(3) . 2_675
C42 C43 O40 104(3) . 2_675
C40 O40 C41 98(2) . 2_675
C40 O40 C43 114(3) . 2_675
C41 O40 C43 16(3) 2_675 2_675
O2 Ru1 O1 178.5(2) 2_666 .
O2 Ru1 O5 89.5(2) 2_666 .
O1 Ru1 O5 90.3(2) . .
O2 Ru1 O3 89.7(2) 2_666 .
O1 Ru1 O3 90.5(2) . .
O5 Ru1 O3 178.53(18) . .
O2 Ru1 Ru1 90.33(18) 2_666 2_666
O1 Ru1 Ru1 88.20(18) . 2_666
O5 Ru1 Ru1 89.44(16) . 2_666
O3 Ru1 Ru1 89.36(15) . 2_666
O2 Ru1 N12 95.6(2) 2_666 .
O1 Ru1 N12 85.8(3) . .
O5 Ru1 N12 92.0(2) . .
O3 Ru1 N12 89.3(2) . .
Ru1 Ru1 N12 173.89(17) 2_666 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O1 1.249(10) .
C1 O2 1.268(10) .
C1 C2 1.511(10) .
C3 O5 1.254(10) .
C3 O3 1.260(9) 2_666
C3 C4 1.521(10) .
C11 N12 1.311(10) .
C11 N11 1.365(10) .
C11 C15 1.453(10) .
C12 C13 1.362(12) .
C12 N11 1.373(12) .
C13 N12 1.381(10) .
C14 N11 1.457(11) .
C15 C15 1.334(15) 2_667
N12 Ru1 2.325(7) .
O1 Ru1 2.063(6) .
O2 Ru1 2.061(6) 2_666
O3 C3 1.260(9) 2_666
O3 Ru1 2.081(5) .
O5 Ru1 2.074(5) .
C40 C41 1.52(2) .
C40 O40 1.57(3) .
C41 C42 1.53(3) 2_675
C41 C41 2.03(8) 2_675
C42 C43 1.52(2) .
C42 C41 1.53(3) 2_675
C43 O40 1.59(3) 2_675
O40 C41 1.58(6) 2_675
O40 C43 1.59(3) 2_675
Ru1 O2 2.061(6) 2_666
Ru1 Ru1 2.2829(11) 2_666
