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#$Date: 2016-03-23 03:46:46 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179262 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/82/4318247.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_4318247
loop_
_publ_author_name
'Barbara Serli'
'Ennio Zangrando'
'Elisabetta Iengo'
'Giovanni Mestroni'
'Lesley Yellowlees'
'Enzo Alessio'
_publ_section_title
;
 Synthesis and Structural, Spectroscopic, and Electrochemical
 Characterization of New Ruthenium Dimethyl Sulfoxide Nitrosyls
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4033
_journal_page_last               4043
_journal_paper_doi               10.1021/ic011291v
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety
'[4(Cl) (C3 H4 N2) (N O) Ru 1-] (C3 H4 N2)(C3 H5 N2 1+) '
_chemical_formula_sum            'C9 H13 Cl4 N7 O Ru'
_chemical_formula_weight         478.13
_chemical_name_systematic
;
   trans-tetrachloro-(imidazole)-nitrosyl-ruthenium(III)
   (imidazole-imidazolium)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.57(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.464(3)
_cell_length_b                   11.259(4)
_cell_length_c                   16.095(4)
_cell_measurement_temperature    293(2)
_cell_volume                     1797.5(10)
_computing_cell_refinement       'Mosflm (J. Appl. Cryst., 1993, 21, 67)'
_computing_data_collection       'Nonius xpress'
_computing_data_reduction        'Scala (J. Appl. Cryst., 1993, 21, 67)'
_computing_molecular_graphics    'Ortep3/windows (Farrugia,1997)'
_computing_publication_material  'Wingx 1.63 (Farrugia, 1999)'
_computing_structure_refinement  'Shelxl-97 (Sheldrick, 1997)'
_computing_structure_solution    'Shelxs-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0251
_diffrn_reflns_av_sigmaI/netI    0.0410
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7140
_diffrn_reflns_theta_full        27.87
_diffrn_reflns_theta_max         27.87
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    1.476
_exptl_absorpt_correction_T_max  1.1161
_exptl_absorpt_correction_T_min  0.6935
_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            deep_red
_exptl_crystal_density_diffrn    1.767
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             944
_refine_diff_density_max         1.094
_refine_diff_density_min         -0.354
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         4243
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0369
_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)+(0.0374P)²+1.1445P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0910
_refine_ls_wR_factor_ref         0.0961
_reflns_number_gt                3584
_reflns_number_total             4243
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic011291v_5.cif
_cod_data_source_block           runo#6
_cod_original_cell_volume        1797.5(9)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4318247
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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 0.77557(2) 0.744107(18) 0.098470(14) 0.04038(10) Uani 1 1 d . . .
Cl1 Cl 0.89129(9) 0.88736(8) 0.04077(5) 0.0591(2) Uani 1 1 d . . .
Cl2 Cl 0.63242(8) 0.70130(7) -0.04539(5) 0.05436(19) Uani 1 1 d . . .
Cl3 Cl 0.64231(8) 0.61962(7) 0.15682(5) 0.05238(18) Uani 1 1 d . . .
Cl4 Cl 0.91106(8) 0.79838(7) 0.24254(5) 0.05029(18) Uani 1 1 d . . .
N1 N 0.8878(3) 0.6324(2) 0.09357(18) 0.0526(6) Uani 1 1 d . . .
O1 O 0.9629(3) 0.5626(3) 0.0894(3) 0.1001(11) Uani 1 1 d . . .
N2 N 0.6435(2) 0.8800(2) 0.10599(16) 0.0456(5) Uani 1 1 d . . .
C3 C 0.4593(4) 0.9801(4) 0.1004(3) 0.0743(10) Uani 1 1 d . . .
H3 H 0.3696 1.0013 0.0897 0.089 Uiso 1 1 calc R . .
C2 C 0.5057(4) 0.8765(3) 0.0799(3) 0.0654(9) Uani 1 1 d . . .
H2 H 0.4526 0.8126 0.0524 0.078 Uiso 1 1 calc R . .
C1 C 0.6781(4) 0.9853(3) 0.1424(2) 0.0571(8) Uani 1 1 d . . .
H1 H 0.7664 1.0118 0.1664 0.068 Uiso 1 1 calc R . .
N3 N 0.5701(4) 1.0479(3) 0.1400(2) 0.0712(8) Uani 1 1 d . . .
H3A H 0.5698 1.1187 0.1599 0.085 Uiso 1 1 calc R . .
N4 N 0.2747(3) 0.6525(3) 0.1797(2) 0.0690(8) Uani 1 1 d . . .
H4 H 0.2579 0.6647 0.1245 0.083 Uiso 1 1 calc R . .
C6 C 0.3530(5) 0.5751(4) 0.3104(3) 0.0808(12) Uani 1 1 d . . .
H6 H 0.3981 0.5262 0.3571 0.097 Uiso 1 1 calc R . .
C5 C 0.3503(4) 0.5640(4) 0.2277(3) 0.0718(10) Uani 1 1 d . . .
H5A H 0.3934 0.5049 0.2062 0.086 Uiso 1 1 calc R . .
C4 C 0.2319(5) 0.7157(4) 0.2336(3) 0.0763(11) Uani 1 1 d . . .
H4A H 0.1772 0.7825 0.2177 0.092 Uiso 1 1 calc R . .
N5 N 0.2771(4) 0.6718(4) 0.3136(2) 0.0826(10) Uani 1 1 d . . .
H5 H 0.2614 0.6992 0.3592 0.099 Uiso 1 1 calc R . .
N6 N 0.2248(3) 0.6746(3) 0.0077(2) 0.0625(7) Uani 1 1 d . . .
N7 N 0.2525(4) 0.6481(3) -0.1172(2) 0.0764(9) Uani 1 1 d . . .
H7 H 0.2846 0.6218 -0.1567 0.092 Uiso 1 1 calc R . .
C7 C 0.2959(4) 0.6190(3) -0.0335(3) 0.0678(9) Uani 1 1 d . . .
H7A H 0.3663 0.5668 -0.0078 0.081 Uiso 1 1 calc R . .
C8 C 0.1319(5) 0.7415(4) -0.0528(3) 0.0815(13) Uani 1 1 d . . .
H8 H 0.0669 0.7899 -0.0419 0.098 Uiso 1 1 calc R . .
C9 C 0.1503(6) 0.7256(4) -0.1309(3) 0.0841(13) Uani 1 1 d . . .
H9 H 0.1019 0.7610 -0.1838 0.101 Uiso 1 1 calc R . .
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'
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'
O O 0.0106 0.0060 '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'
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
N1 Ru N2 178.98(11) . . ?
N1 Ru Cl3 94.64(10) . . ?
N2 Ru Cl3 85.81(8) . . ?
N1 Ru Cl2 91.97(9) . . ?
N2 Ru Cl2 88.95(7) . . ?
Cl3 Ru Cl2 89.90(3) . . ?
N1 Ru Cl1 92.18(10) . . ?
N2 Ru Cl1 87.38(8) . . ?
Cl3 Ru Cl1 173.18(3) . . ?
Cl2 Ru Cl1 89.91(3) . . ?
N1 Ru Cl4 91.64(9) . . ?
N2 Ru Cl4 87.44(7) . . ?
Cl3 Ru Cl4 90.51(3) . . ?
Cl2 Ru Cl4 176.32(3) . . ?
Cl1 Ru Cl4 89.25(3) . . ?
O1 N1 Ru 177.7(3) . . ?
C1 N2 C2 105.9(3) . . ?
C1 N2 Ru 126.2(2) . . ?
C2 N2 Ru 127.8(2) . . ?
C2 C3 N3 106.2(3) . . ?
C3 C2 N2 109.1(3) . . ?
N2 C1 N3 110.8(3) . . ?
C1 N3 C3 107.9(3) . . ?
C4 N4 C5 106.6(3) . . ?
C5 C6 N5 106.7(4) . . ?
C6 C5 N4 109.0(4) . . ?
N4 C4 N5 110.6(4) . . ?
C4 N5 C6 107.2(4) . . ?
C7 N6 C8 107.2(3) . . ?
C7 N7 C9 109.0(3) . . ?
N6 C7 N7 109.5(4) . . ?
C9 C8 N6 108.2(4) . . ?
C8 C9 N7 106.2(4) . . ?
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 N1 1.740(3) . ?
Ru N2 2.091(2) . ?
Ru Cl3 2.3717(9) . ?
Ru Cl2 2.3724(10) . ?
Ru Cl1 2.3762(10) . ?
Ru Cl4 2.3804(10) . ?
N1 O1 1.128(4) . ?
N2 C1 1.321(4) . ?
N2 C2 1.369(4) . ?
C3 C2 1.344(5) . ?
C3 N3 1.365(5) . ?
C1 N3 1.321(4) . ?
N4 C4 1.306(5) . ?
N4 C5 1.350(5) . ?
C6 C5 1.329(6) . ?
C6 N5 1.358(6) . ?
C4 N5 1.319(6) . ?
N6 C7 1.303(5) . ?
N6 C8 1.363(5) . ?
N7 C7 1.320(5) . ?
N7 C9 1.343(6) . ?
C8 C9 1.343(6) . ?
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
N2 Ru N1 O1 -61(12) . . . . ?
Cl3 Ru N1 O1 -177(100) . . . . ?
Cl2 Ru N1 O1 93(8) . . . . ?
Cl1 Ru N1 O1 3(8) . . . . ?
Cl4 Ru N1 O1 -87(8) . . . . ?
N1 Ru N2 C1 13(7) . . . . ?
Cl3 Ru N2 C1 129.3(3) . . . . ?
Cl2 Ru N2 C1 -140.7(3) . . . . ?
Cl1 Ru N2 C1 -50.7(3) . . . . ?
Cl4 Ru N2 C1 38.6(3) . . . . ?
N1 Ru N2 C2 -162(6) . . . . ?
Cl3 Ru N2 C2 -46.1(3) . . . . ?
Cl2 Ru N2 C2 43.8(3) . . . . ?
Cl1 Ru N2 C2 133.8(3) . . . . ?
Cl4 Ru N2 C2 -136.8(3) . . . . ?
N3 C3 C2 N2 -0.3(5) . . . . ?
C1 N2 C2 C3 0.5(4) . . . . ?
Ru N2 C2 C3 176.7(3) . . . . ?
C2 N2 C1 N3 -0.4(4) . . . . ?
Ru N2 C1 N3 -176.7(2) . . . . ?
N2 C1 N3 C3 0.2(4) . . . . ?
C2 C3 N3 C1 0.1(5) . . . . ?
N5 C6 C5 N4 0.3(5) . . . . ?
C4 N4 C5 C6 -0.3(5) . . . . ?
C5 N4 C4 N5 0.1(5) . . . . ?
N4 C4 N5 C6 0.1(5) . . . . ?
C5 C6 N5 C4 -0.2(5) . . . . ?
C8 N6 C7 N7 0.3(5) . . . . ?
C9 N7 C7 N6 0.3(5) . . . . ?
C7 N6 C8 C9 -0.7(5) . . . . ?
N6 C8 C9 N7 0.8(6) . . . . ?
C7 N7 C9 C8 -0.7(6) . . . . ?
C5 N4 N6 C7 -16.6(5) . . . . ?
