#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:26:17 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179377 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/74/4327439.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_4327439
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            'C14 H18 N4 O13.28 Ru'
_chemical_formula_weight         562.49
_chemical_name_systematic
;
  ?
;
_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                78.413(6)
_cell_angle_beta                 75.804(6)
_cell_angle_gamma                73.562(6)
_cell_formula_units_Z            2
_cell_length_a                   8.838(2)
_cell_length_b                   9.452(3)
_cell_length_c                   13.419(4)
_cell_measurement_temperature    293(2)
_cell_volume                     1031.9(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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0221
_diffrn_reflns_av_sigmaI/netI    0.0279
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            4870
_diffrn_reflns_theta_full        26.31
_diffrn_reflns_theta_max         26.31
_diffrn_reflns_theta_min         2.27
_exptl_absorpt_coefficient_mu    0.843
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.814
_exptl_crystal_description       Block
_exptl_crystal_F_000             574.12
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.117
_refine_diff_density_min         -0.676
_refine_diff_density_rms         0.117
_refine_ls_extinction_coef       0.0043(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         2970
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0385
_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)+(0.0639P)²+2.9785P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1060
_refine_ls_wR_factor_ref         0.1087
_reflns_number_gt                2709
_reflns_number_total             2970
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0202192B_1.cif
_cod_data_source_block           AMD3689
_cod_original_cell_volume        1031.8(5)
_cod_database_code               4327439
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
Ru1 Ru 0.05697(4) 1.04068(4) 0.21268(3) 0.01270(19) Uani 1 1 d .
N1 N -0.1053(5) 1.1666(4) 0.1625(3) 0.0159(9) Uani 1 1 d .
N2 N -0.0372(5) 0.8461(4) 0.2466(3) 0.0153(9) Uani 1 1 d .
N3 N 0.2709(5) 0.8881(4) 0.2407(3) 0.0156(9) Uani 1 1 d .
N4 N 0.1876(5) 1.1991(4) 0.2114(3) 0.0156(9) Uani 1 1 d .
O1 O -0.1936(4) 1.2399(4) 0.1124(3) 0.0259(8) Uani 1 1 d .
O2 O 0.1569(4) 0.9943(4) 0.0652(2) 0.0172(7) Uani 1 1 d .
O3 O -0.0174(4) 1.0764(4) 0.3627(3) 0.0200(8) Uani 1 1 d .
O4 O -0.0742(5) 1.2572(4) 0.4590(3) 0.0315(9) Uani 1 1 d .
O5 O 0.3882(4) 0.9110(4) -0.0405(2) 0.0204(8) Uani 1 1 d .
O6 O -0.3376(4) 1.0559(4) 0.3171(3) 0.0237(8) Uani 1 1 d .
O7 O -0.3674(6) 0.9155(6) 0.4717(3) 0.0663(17) Uani 1 1 d .
O8 O -0.3029(4) 0.6849(4) 0.2355(3) 0.0250(8) Uani 1 1 d .
O9 O -0.0755(4) 0.5930(4) 0.1272(3) 0.0289(9) Uani 1 1 d .
O10 O 0.3993(4) 1.4316(4) 0.0046(3) 0.0254(8) Uani 1 1 d .
O11 O 0.3564(4) 1.4250(4) 0.1772(3) 0.0238(8) Uani 1 1 d .
O12 O 0.6090(5) 0.4460(4) 0.2577(3) 0.0337(9) Uani 1 1 d .
O13 O 0.5760(12) 0.6066(11) 0.5444(6) 0.056(2) Uani 0.56 1 d P
O14 O 0.1031(16) 0.4807(10) 0.4745(8) 0.060(3) Uani 0.46 1 d P
O15 O 0.436(3) 0.710(2) 0.5588(13) 0.054(5) Uani 0.27 1 d P
C1 C -0.1393(6) 0.8286(6) 0.3539(4) 0.0182(11) Uani 1 1 d .
H1A H -0.0737 0.8235 0.4035 0.022 Uiso 1 1 calc R
H1B H -0.1674 0.7338 0.3656 0.022 Uiso 1 1 calc R
C2 C -0.2924(6) 0.9475(7) 0.3778(4) 0.0273(13) Uani 1 1 d .
C3 C -0.1229(6) 0.8413(5) 0.1643(4) 0.0183(11) Uani 1 1 d .
H3A H -0.0558 0.8611 0.0967 0.022 Uiso 1 1 calc R
H3B H -0.2217 0.9197 0.1689 0.022 Uiso 1 1 calc R
C4 C -0.1635(6) 0.6927(5) 0.1729(4) 0.0187(11) Uani 1 1 d .
C5 C 0.1097(6) 0.7164(5) 0.2459(4) 0.0182(11) Uani 1 1 d .
H5A H 0.0780 0.6265 0.2823 0.022 Uiso 1 1 calc R
H5B H 0.1608 0.7007 0.1749 0.022 Uiso 1 1 calc R
C6 C 0.2269(6) 0.7488(5) 0.2983(4) 0.0168(10) Uani 1 1 d .
H6A H 0.1777 0.7612 0.3700 0.020 Uiso 1 1 calc R
H6B H 0.3224 0.6669 0.2972 0.020 Uiso 1 1 calc R
C7 C 0.3842(6) 0.8604(5) 0.1392(4) 0.0174(10) Uani 1 1 d .
H7A H 0.4746 0.9027 0.1331 0.021 Uiso 1 1 calc R
H7B H 0.4258 0.7538 0.1394 0.021 Uiso 1 1 calc R
C8 C 0.3087(6) 0.9246(5) 0.0465(4) 0.0151(10) Uani 1 1 d .
C9 C 0.3369(6) 0.9607(5) 0.3046(4) 0.0181(11) Uani 1 1 d .
H9A H 0.4443 0.9031 0.3124 0.022 Uiso 1 1 calc R
H9B H 0.2687 0.9656 0.3731 0.022 Uiso 1 1 calc R
C10 C 0.3424(6) 1.1156(5) 0.2502(4) 0.0177(10) Uani 1 1 d .
H10A H 0.4327 1.1092 0.1917 0.021 Uiso 1 1 calc R
H10B H 0.3600 1.1716 0.2977 0.021 Uiso 1 1 calc R
C11 C 0.2274(6) 1.2864(5) 0.1068(4) 0.0187(11) Uani 1 1 d .
H11A H 0.1275 1.3460 0.0869 0.022 Uiso 1 1 calc R
H11B H 0.2789 1.2170 0.0571 0.022 Uiso 1 1 calc R
C12 C 0.3365(6) 1.3893(5) 0.0988(4) 0.0205(11) Uani 1 1 d .
C13 C 0.0768(6) 1.2962(6) 0.2877(4) 0.0215(11) Uani 1 1 d .
H13A H -0.0012 1.3718 0.2535 0.026 Uiso 1 1 calc R
H13B H 0.1380 1.3461 0.3137 0.026 Uiso 1 1 calc R
C14 C -0.0105(6) 1.2049(6) 0.3775(4) 0.0205(11) 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
N1 Ru1 O3 98.60(16)
N1 Ru1 O2 87.49(15)
O3 Ru1 O2 173.61(13)
N1 Ru1 N3 168.43(16)
O3 Ru1 N3 92.81(14)
O2 Ru1 N3 81.05(14)
N1 Ru1 N4 97.24(17)
O3 Ru1 N4 80.37(14)
O2 Ru1 N4 97.00(14)
N3 Ru1 N4 82.72(15)
N1 Ru1 N2 97.57(16)
O3 Ru1 N2 91.23(14)
O2 Ru1 N2 89.91(14)
N3 Ru1 N2 84.04(15)
N4 Ru1 N2 163.91(15)
O1 N1 Ru1 167.0(4)
C3 N2 C1 112.2(4)
C3 N2 C5 109.3(4)
C1 N2 C5 105.9(4)
C3 N2 Ru1 111.1(3)
C1 N2 Ru1 113.2(3)
C5 N2 Ru1 104.6(3)
C6 N3 C9 112.5(4)
C6 N3 C7 111.0(4)
C9 N3 C7 111.6(4)
C6 N3 Ru1 106.9(3)
C9 N3 Ru1 105.1(3)
C7 N3 Ru1 109.4(3)
C13 N4 C11 111.7(4)
C13 N4 C10 110.7(4)
C11 N4 C10 109.9(4)
C13 N4 Ru1 102.9(3)
C11 N4 Ru1 113.3(3)
C10 N4 Ru1 108.1(3)
C8 O2 Ru1 117.2(3)
C14 O3 Ru1 113.8(3)
N2 C1 C2 117.2(4)
O6 C2 O7 125.7(5)
O6 C2 C1 124.5(5)
O7 C2 C1 109.8(5)
N2 C3 C4 113.2(4)
O9 C4 O8 124.2(5)
O9 C4 C3 122.6(5)
O8 C4 C3 113.2(4)
C6 C5 N2 109.6(4)
N3 C6 C5 108.0(4)
C8 C7 N3 113.8(4)
O5 C8 O2 123.4(4)
O5 C8 C7 120.3(4)
O2 C8 C7 116.3(4)
N3 C9 C10 108.5(4)
C9 C10 N4 112.5(4)
N4 C11 C12 115.5(4)
O11 C12 O10 126.4(5)
O11 C12 C11 121.0(4)
O10 C12 C11 112.6(4)
N4 C13 C14 110.7(4)
O4 C14 O3 123.4(5)
O4 C14 C13 119.3(5)
O3 C14 C13 117.2(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ru1 N1 1.764(4) .
Ru1 O3 2.024(3) .
Ru1 O2 2.040(3) .
Ru1 N3 2.094(4) .
Ru1 N4 2.129(4) .
Ru1 N2 2.151(4) .
N1 O1 1.142(5) .
N2 C3 1.498(6) .
N2 C1 1.506(6) .
N2 C5 1.512(6) .
N3 C6 1.488(6) .
N3 C9 1.501(6) .
N3 C7 1.501(6) .
N4 C13 1.493(6) .
N4 C11 1.493(6) .
N4 C10 1.529(6) .
O2 C8 1.304(6) .
O3 C14 1.290(6) .
O4 C14 1.231(6) .
O5 C8 1.217(6) .
O6 C2 1.211(7) .
O7 C2 1.293(7) .
O8 C4 1.322(6) .
O9 C4 1.206(6) .
O10 C12 1.282(6) .
O11 C12 1.232(6) .
O13 O15 1.34(2) .
O14 O14 1.74(3) 2_566
C1 C2 1.506(7) .
C3 C4 1.521(7) .
C5 C6 1.511(7) .
C7 C8 1.495(7) .
C9 C10 1.507(7) .
C11 C12 1.525(7) .
C13 C14 1.515(7) .
