#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:26:17 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179377 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/74/4327440.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_4327440
loop_
_publ_author_name
'Beth R. Cameron'
'Marilyn C. Darkes'
'Helen Yee'
'Micki Olsen'
'Simon P. Fricker'
'Renato T. Skerlj'
'Gary J. Bridger'
'Nathan A. Davies'
'Michael T. Wilson'
'David J. Rose'
'Jon Zubieta'
_publ_section_title
;
 Ruthenium(III) Polyaminocarboxylate Complexes: Efficient and Effective
 Nitric Oxide Scavengers
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1868
_journal_page_last               1876
_journal_paper_doi               10.1021/ic020219+
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C10 H14 N2 O9 Ru'
_chemical_formula_weight         407.30
_chemical_name_common            anormed2
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 99.603(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.4382(2)
_cell_length_b                   8.8304(2)
_cell_length_c                   17.6321(4)
_cell_measurement_temperature    293(2)
_cell_volume                     1295.40(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.929
_diffrn_measured_fraction_theta_max 0.929
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\alpha
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0483
_diffrn_reflns_av_sigmaI/netI    0.0696
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            2068
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.66
_exptl_absorpt_coefficient_mu    1.265
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.089
_exptl_crystal_description       plate
_exptl_crystal_F_000             816
_exptl_crystal_size_max          .22
_exptl_crystal_size_mid          .22
_exptl_crystal_size_min          .11
_refine_diff_density_max         0.685
_refine_diff_density_min         -0.699
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.226
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     207
_refine_ls_number_reflns         1871
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.226
_refine_ls_R_factor_all          0.0974
_refine_ls_R_factor_gt           0.0559
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0000P)²+18.8504P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1094
_refine_ls_wR_factor_ref         0.1223
_reflns_number_gt                1375
_reflns_number_total             1871
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0202192B_2.cif
_cod_data_source_block           AMD6245
_cod_original_cell_volume        1295.3(2)
_cod_database_code               4327440
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Ru1 Ru 0.19714(11) 0.17465(10) 0.14307(5) 0.0149(3) Uani 1 1 d .
O1 O 0.3590(8) 0.1566(8) 0.2388(4) 0.0228(17) Uani 1 1 d .
O2 O 0.4799(9) 0.2916(9) 0.3384(4) 0.031(2) Uani 1 1 d .
O3 O -0.0015(8) 0.1468(9) 0.1914(4) 0.0273(19) Uani 1 1 d .
O4 O -0.2045(9) 0.2773(9) 0.2255(5) 0.036(2) Uani 1 1 d .
O5 O 0.0510(7) 0.1920(8) 0.0373(4) 0.0194(16) Uani 1 1 d .
O6 O 0.0458(8) 0.2282(9) -0.0884(4) 0.029(2) Uani 1 1 d .
O7 O 0.6686(8) 0.3353(9) 0.0253(4) 0.0270(18) Uani 1 1 d .
O8 O 0.7516(8) 0.0975(8) 0.0499(4) 0.0254(18) Uani 1 1 d .
O9 O 0.2235(15) -0.0574(14) 0.1182(8) 0.025(3) Uani 1 1 d .
H9C H 0.185(17) -0.044(19) 0.099(8) 0.00(5) Uiso 1 1 d .
H9D H 0.296(14) -0.092(13) 0.146(7) 0.03(4) Uiso 1 1 d .
N1 N 0.1709(10) 0.3926(10) 0.1766(5) 0.021(2) Uani 1 1 d .
N2 N 0.3669(9) 0.2619(9) 0.0780(5) 0.0146(19) Uani 1 1 d .
C1 C 0.2499(12) 0.4925(13) 0.1253(6) 0.024(3) Uani 1 1 d .
H1A H 0.2734 0.5906 0.1493 0.029 Uiso 1 1 calc R
H1B H 0.1784 0.5077 0.0768 0.029 Uiso 1 1 calc R
C2 C 0.4060(13) 0.4176(12) 0.1109(6) 0.021(3) Uani 1 1 d .
H2A H 0.4551 0.4781 0.0752 0.025 Uiso 1 1 calc R
H2B H 0.4812 0.4100 0.1588 0.025 Uiso 1 1 calc R
C3 C 0.2567(14) 0.4040(12) 0.2588(6) 0.027(3) Uani 1 1 d .
H3A H 0.3122 0.5005 0.2657 0.032 Uiso 1 1 calc R
H3B H 0.1774 0.4025 0.2928 0.032 Uiso 1 1 calc R
C4 C 0.3766(13) 0.2786(12) 0.2819(6) 0.022(3) Uani 1 1 d .
C5 C -0.0034(12) 0.4151(13) 0.1720(6) 0.024(3) Uani 1 1 d .
H5A H -0.0518 0.4370 0.1193 0.028 Uiso 1 1 calc R
H5B H -0.0228 0.5007 0.2037 0.028 Uiso 1 1 calc R
C6 C -0.0788(14) 0.2748(12) 0.1993(6) 0.023(3) Uani 1 1 d .
C7 C 0.2953(12) 0.2705(13) -0.0055(6) 0.022(3) Uani 1 1 d .
H7A H 0.3545 0.2036 -0.0343 0.027 Uiso 1 1 calc R
H7B H 0.3070 0.3729 -0.0237 0.027 Uiso 1 1 calc R
C8 C 0.1182(13) 0.2270(12) -0.0215(6) 0.022(3) Uani 1 1 d .
C9 C 0.5104(11) 0.1619(13) 0.0892(6) 0.023(2) Uani 1 1 d .
H9A H 0.4767 0.0618 0.0704 0.027 Uiso 1 1 calc R
H9B H 0.5487 0.1530 0.1440 0.027 Uiso 1 1 calc R
C10 C 0.6506(13) 0.2104(12) 0.0510(6) 0.022(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 0.0000 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'
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
O1 Ru1 O3 97.6(3)
O1 Ru1 N1 85.5(3)
O3 Ru1 N1 81.6(3)
O1 Ru1 O5 173.6(3)
O3 Ru1 O5 88.7(3)
N1 Ru1 O5 96.6(3)
O1 Ru1 O9 91.0(4)
O3 Ru1 O9 95.4(4)
N1 Ru1 O9 175.0(4)
O5 Ru1 O9 87.3(4)
O1 Ru1 N2 93.3(3)
O3 Ru1 N2 162.7(3)
N1 Ru1 N2 86.0(3)
O5 Ru1 N2 80.8(3)
O9 Ru1 N2 97.8(4)
C4 O1 Ru1 114.8(6)
C6 O3 Ru1 113.5(7)
C8 O5 Ru1 117.7(6)
C5 N1 C1 115.4(8)
C5 N1 C3 111.0(8)
C1 N1 C3 110.5(8)
C5 N1 Ru1 105.5(7)
C1 N1 Ru1 107.5(6)
C3 N1 Ru1 106.5(6)
C9 N2 C7 110.4(8)
C9 N2 C2 111.7(8)
C7 N2 C2 111.1(8)
C9 N2 Ru1 108.7(6)
C7 N2 Ru1 110.6(6)
C2 N2 Ru1 104.3(6)
N1 C1 C2 109.1(8)
N2 C2 C1 108.6(8)
C4 C3 N1 113.7(9)
O2 C4 O1 123.3(10)
O2 C4 C3 120.6(10)
O1 C4 C3 116.1(9)
N1 C5 C6 110.0(9)
O4 C6 O3 121.8(10)
O4 C6 C5 122.9(10)
O3 C6 C5 115.3(10)
N2 C7 C8 113.1(8)
O6 C8 O5 123.5(9)
O6 C8 C7 119.2(9)
O5 C8 C7 117.2(9)
N2 C9 C10 116.8(9)
O7 C10 O8 124.2(10)
O7 C10 C9 125.4(10)
O8 C10 C9 110.4(9)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Ru1 O1 1.993(7)
Ru1 O3 2.018(7)
Ru1 N1 2.036(9)
Ru1 O5 2.062(6)
Ru1 O9 2.115(12)
Ru1 N2 2.124(8)
O1 C4 1.312(12)
O2 C4 1.215(12)
O3 C6 1.323(13)
O4 C6 1.226(13)
O5 C8 1.300(12)
O6 C8 1.235(12)
O7 C10 1.212(12)
O8 C10 1.314(12)
N1 C5 1.473(13)
N1 C1 1.498(13)
N1 C3 1.511(13)
N2 C9 1.485(12)
N2 C7 1.497(12)
N2 C2 1.507(13)
C1 C2 1.532(14)
C3 C4 1.510(14)
C5 C6 1.508(14)
C7 C8 1.523(14)
C9 C10 1.517(14)
