#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:46:46 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179262 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/82/4318273.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_4318273
loop_
_publ_author_name
'Daniel A. Freedman'
'Daron E. Janzen'
'Jennifer L. Vreeland'
'Hannah M. Tully'
'Kent R. Mann'
_publ_section_title
;
 Ligand Substitution, pH Dependent Deoxygenation, and Linkage
 Isomerization Reactions of the 2,2'-Bipyridinetetranitroruthenate Dianion
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3820
_journal_page_last               3829
_journal_paper_doi               10.1021/ic0255205
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         'C10 H9 N5 O6 Ru'
_chemical_formula_sum            'C10 H9 N5 O6 Ru'
_chemical_formula_weight         396.29
_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                 102.0800(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.5607(6)
_cell_length_b                   14.2326(12)
_cell_length_c                   14.5402(12)
_cell_measurement_temperature    173(2)
_cell_volume                     1327.6(2)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'SMART, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'SMART Platform CCD, Bruker'
_diffrn_measurement_method       'omega scans'
_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  0.0402
_diffrn_reflns_av_sigmaI/netI    0.0336
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9774
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    1.221
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6686
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS R. Blessing, 1995'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.983
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.537
_refine_diff_density_min         -1.339
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     233
_refine_ls_number_reflns         3041
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0364
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0704P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.0983
_reflns_number_gt                2584
_reflns_number_total             3041
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0255205_s1_1.cif
_cod_data_source_block           00251
_cod_database_code               4318273
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.81537(3) 0.175234(15) 0.733844(15) 0.01597(11) Uani 1 1 d . . .
O2 O 1.2058(4) 0.2785(2) 0.75980(19) 0.0488(8) Uani 1 1 d . . .
O6 O 0.9339(3) 0.16618(14) 0.62435(16) 0.0229(5) Uani 1 1 d . . .
H6A H 1.0645 0.1676 0.6405 0.08(2) Uiso 1 1 calc R . .
O1 O 1.0051(4) 0.33272(15) 0.84495(19) 0.0332(6) Uani 1 1 d . . .
O4 O 0.9842(4) 0.02106(17) 0.85632(17) 0.0354(6) Uani 1 1 d . . .
O5 O 0.6613(5) 0.18263(17) 0.9068(2) 0.0447(7) Uani 1 1 d . . .
N2 N 0.6017(3) 0.26739(17) 0.65355(17) 0.0187(5) Uani 1 1 d . . .
N1 N 0.5881(3) 0.08182(16) 0.66484(17) 0.0178(5) Uani 1 1 d . . .
N4 N 1.0292(4) 0.07467(19) 0.79631(19) 0.0249(5) Uani 1 1 d . . .
N3 N 1.0408(4) 0.27543(18) 0.78619(18) 0.0231(5) Uani 1 1 d . . .
N5 N 0.7122(4) 0.18078(15) 0.83670(19) 0.0215(5) Uani 1 1 d . . .
C2 C 0.4459(4) -0.0689(2) 0.6225(2) 0.0235(6) Uani 1 1 d . . .
O3 O 1.1999(3) 0.0684(2) 0.77482(19) 0.0476(8) Uani 1 1 d . . .
C6 C 0.4401(4) 0.2256(2) 0.5943(2) 0.0194(6) Uani 1 1 d . . .
C4 C 0.2861(4) 0.0667(2) 0.5424(2) 0.0219(6) Uani 1 1 d . . .
C8 C 0.3049(5) 0.3759(2) 0.5386(2) 0.0291(7) Uani 1 1 d . . .
C3 C 0.2906(4) -0.0298(2) 0.5545(2) 0.0229(6) Uani 1 1 d . . .
C5 C 0.4354(4) 0.12168(19) 0.59965(19) 0.0174(5) Uani 1 1 d . . .
C1 C 0.5936(4) -0.0116(2) 0.6764(2) 0.0214(6) Uani 1 1 d . . .
C7 C 0.2892(5) 0.2783(2) 0.5361(2) 0.0253(6) Uani 1 1 d . . .
C9 C 0.4715(5) 0.4171(2) 0.5980(2) 0.0276(7) Uani 1 1 d . . .
C10 C 0.6185(5) 0.3612(2) 0.6546(2) 0.0244(6) Uani 1 1 d . . .
H3 H 0.196(4) -0.067(2) 0.514(2) 0.016(7) Uiso 1 1 d . A 1
H8 H 0.206(5) 0.411(2) 0.500(2) 0.022(8) Uiso 1 1 d . B 1
H4 H 0.178(5) 0.101(2) 0.489(2) 0.025(9) Uiso 1 1 d . C 1
H9 H 0.502(5) 0.481(2) 0.596(2) 0.034(9) Uiso 1 1 d . D 1
H1 H 0.696(6) -0.032(2) 0.724(3) 0.034(10) Uiso 1 1 d . E 1
H10 H 0.744(5) 0.389(3) 0.695(2) 0.031(9) Uiso 1 1 d . F 1
H7 H 0.181(5) 0.245(2) 0.495(2) 0.025(9) Uiso 1 1 d . G 1
H2 H 0.448(5) -0.127(3) 0.627(2) 0.027(9) Uiso 1 1 d . H 1
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N5 Ru1 O6 178.09(10) . . ?
N5 Ru1 N4 90.24(11) . . ?
O6 Ru1 N4 87.85(10) . . ?
N5 Ru1 N3 91.64(11) . . ?
O6 Ru1 N3 88.23(9) . . ?
N4 Ru1 N3 87.07(11) . . ?
N5 Ru1 N2 96.54(10) . . ?
O6 Ru1 N2 85.37(9) . . ?
N4 Ru1 N2 172.14(10) . . ?
N3 Ru1 N2 96.69(10) . . ?
N5 Ru1 N1 94.21(10) . . ?
O6 Ru1 N1 86.05(9) . . ?
N4 Ru1 N1 96.91(10) . . ?
N3 Ru1 N1 172.90(9) . . ?
N2 Ru1 N1 78.66(10) . . ?
Ru1 O6 H6A 109.5 . . ?
C10 N2 C6 119.7(2) . . ?
C10 N2 Ru1 125.14(19) . . ?
C6 N2 Ru1 115.09(19) . . ?
C1 N1 C5 120.1(2) . . ?
C1 N1 Ru1 124.97(19) . . ?
C5 N1 Ru1 114.77(18) . . ?
O3 N4 O4 119.9(3) . . ?
O3 N4 Ru1 120.5(2) . . ?
O4 N4 Ru1 119.55(19) . . ?
O2 N3 O1 120.0(3) . . ?
O2 N3 Ru1 121.2(2) . . ?
O1 N3 Ru1 118.8(2) . . ?
O5 N5 Ru1 174.5(3) . . ?
C1 C2 C3 119.6(3) . . ?
C1 C2 H2 123(2) . . ?
C3 C2 H2 117(2) . . ?
N2 C6 C7 121.1(3) . . ?
N2 C6 C5 115.2(2) . . ?
C7 C6 C5 123.6(2) . . ?
C3 C4 C5 119.4(3) . . ?
C3 C4 H4 123.1(18) . . ?
C5 C4 H4 117.4(18) . . ?
C9 C8 C7 119.1(3) . . ?
C9 C8 H8 122(2) . . ?
C7 C8 H8 119(2) . . ?
C2 C3 C4 119.0(3) . . ?
C2 C3 H3 121.2(18) . . ?
C4 C3 H3 119.7(18) . . ?
N1 C5 C4 120.7(3) . . ?
N1 C5 C6 115.8(2) . . ?
C4 C5 C6 123.5(2) . . ?
N1 C1 C2 121.2(3) . . ?
N1 C1 H1 114(2) . . ?
C2 C1 H1 125(2) . . ?
C6 C7 C8 119.1(3) . . ?
C6 C7 H7 117.4(19) . . ?
C8 C7 H7 123.5(19) . . ?
C8 C9 C10 119.5(3) . . ?
C8 C9 H9 123(2) . . ?
C10 C9 H9 117(2) . . ?
N2 C10 C9 121.4(3) . . ?
N2 C10 H10 118(2) . . ?
C9 C10 H10 121(2) . . ?
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
Ru1 N5 1.768(3) . ?
Ru1 O6 1.917(2) . ?
Ru1 N4 2.076(2) . ?
Ru1 N3 2.081(2) . ?
Ru1 N2 2.089(2) . ?
Ru1 N1 2.091(2) . ?
O2 N3 1.223(3) . ?
O6 H6A 0.8400 . ?
O1 N3 1.238(3) . ?
O4 N4 1.240(3) . ?
O5 N5 1.137(4) . ?
N2 C10 1.340(4) . ?
N2 C6 1.355(4) . ?
N1 C1 1.339(4) . ?
N1 C5 1.351(3) . ?
N4 O3 1.227(3) . ?
C2 C1 1.379(4) . ?
C2 C3 1.380(4) . ?
C2 H2 0.83(4) . ?
C6 C7 1.381(4) . ?
C6 C5 1.482(4) . ?
C4 C3 1.384(4) . ?
C4 C5 1.387(4) . ?
C4 H4 1.05(3) . ?
C8 C9 1.375(5) . ?
C8 C7 1.393(5) . ?
C8 H8 0.91(3) . ?
C3 H3 0.93(3) . ?
C1 H1 0.90(4) . ?
C7 H7 0.95(3) . ?
C9 C10 1.382(4) . ?
C9 H9 0.94(3) . ?
C10 H10 0.99(4) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O6 H6A O2 0.84 2.38 2.855(3) 116.0 .
O6 H6A O3 0.84 2.42 2.859(3) 113.1 .
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
N5 Ru1 N2 C10 84.7(2) . . . . ?
O6 Ru1 N2 C10 -95.4(2) . . . . ?
N4 Ru1 N2 C10 -126.0(7) . . . . ?
N3 Ru1 N2 C10 -7.7(2) . . . . ?
N1 Ru1 N2 C10 177.7(2) . . . . ?
N5 Ru1 N2 C6 -97.8(2) . . . . ?
O6 Ru1 N2 C6 82.1(2) . . . . ?
N4 Ru1 N2 C6 51.5(7) . . . . ?
N3 Ru1 N2 C6 169.8(2) . . . . ?
N1 Ru1 N2 C6 -4.7(2) . . . . ?
N5 Ru1 N1 C1 -83.1(2) . . . . ?
O6 Ru1 N1 C1 95.1(2) . . . . ?
N4 Ru1 N1 C1 7.7(2) . . . . ?
N3 Ru1 N1 C1 131.5(7) . . . . ?
N2 Ru1 N1 C1 -178.9(2) . . . . ?
N5 Ru1 N1 C5 101.8(2) . . . . ?
O6 Ru1 N1 C5 -80.10(19) . . . . ?
N4 Ru1 N1 C5 -167.5(2) . . . . ?
N3 Ru1 N1 C5 -43.6(8) . . . . ?
N2 Ru1 N1 C5 5.96(19) . . . . ?
N5 Ru1 N4 O3 -150.3(3) . . . . ?
O6 Ru1 N4 O3 29.7(3) . . . . ?
N3 Ru1 N4 O3 -58.6(3) . . . . ?
N2 Ru1 N4 O3 60.2(8) . . . . ?
N1 Ru1 N4 O3 115.5(3) . . . . ?
N5 Ru1 N4 O4 29.2(2) . . . . ?
O6 Ru1 N4 O4 -150.8(2) . . . . ?
N3 Ru1 N4 O4 120.8(2) . . . . ?
N2 Ru1 N4 O4 -120.3(6) . . . . ?
N1 Ru1 N4 O4 -65.1(2) . . . . ?
N5 Ru1 N3 O2 154.3(3) . . . . ?
O6 Ru1 N3 O2 -23.8(3) . . . . ?
N4 Ru1 N3 O2 64.1(3) . . . . ?
N2 Ru1 N3 O2 -109.0(3) . . . . ?
N1 Ru1 N3 O2 -60.2(8) . . . . ?
N5 Ru1 N3 O1 -25.9(2) . . . . ?
O6 Ru1 N3 O1 156.0(2) . . . . ?
N4 Ru1 N3 O1 -116.1(2) . . . . ?
N2 Ru1 N3 O1 70.9(2) . . . . ?
N1 Ru1 N3 O1 119.6(7) . . . . ?
O6 Ru1 N5 O5 30(5) . . . . ?
N4 Ru1 N5 O5 31(2) . . . . ?
N3 Ru1 N5 O5 -56(2) . . . . ?
N2 Ru1 N5 O5 -153(2) . . . . ?
N1 Ru1 N5 O5 128(2) . . . . ?
C10 N2 C6 C7 -1.3(4) . . . . ?
Ru1 N2 C6 C7 -179.0(2) . . . . ?
C10 N2 C6 C5 -179.4(2) . . . . ?
Ru1 N2 C6 C5 2.9(3) . . . . ?
C1 C2 C3 C4 -0.4(4) . . . . ?
C5 C4 C3 C2 -0.9(4) . . . . ?
C1 N1 C5 C4 -1.6(4) . . . . ?
Ru1 N1 C5 C4 173.8(2) . . . . ?
C1 N1 C5 C6 178.3(2) . . . . ?
Ru1 N1 C5 C6 -6.2(3) . . . . ?
C3 C4 C5 N1 2.0(4) . . . . ?
C3 C4 C5 C6 -178.0(2) . . . . ?
N2 C6 C5 N1 2.2(3) . . . . ?
C7 C6 C5 N1 -175.8(3) . . . . ?
N2 C6 C5 C4 -177.8(3) . . . . ?
C7 C6 C5 C4 4.2(4) . . . . ?
C5 N1 C1 C2 0.3(4) . . . . ?
Ru1 N1 C1 C2 -174.6(2) . . . . ?
C3 C2 C1 N1 0.8(4) . . . . ?
N2 C6 C7 C8 0.2(4) . . . . ?
C5 C6 C7 C8 178.1(3) . . . . ?
C9 C8 C7 C6 0.8(4) . . . . ?
C7 C8 C9 C10 -0.6(5) . . . . ?
C6 N2 C10 C9 1.6(4) . . . . ?
Ru1 N2 C10 C9 179.0(2) . . . . ?
C8 C9 C10 N2 -0.6(5) . . . . ?
