#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:46:46 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179262 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/82/4318274.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_4318274
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 H8 N6 O7 Ru'
_chemical_formula_sum            'C10 H8 N6 O7 Ru'
_chemical_formula_weight         425.29
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_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                 95.169(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.3635(5)
_cell_length_b                   13.2109(9)
_cell_length_c                   14.6838(10)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    173(2)
_cell_volume                     1422.61(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0527
_diffrn_reflns_av_sigmaI/netI    0.0512
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8180
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    1.154
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7809
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.986
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.105
_refine_diff_density_min         -0.783
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         2522
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0729
_refine_ls_R_factor_gt           0.0467
_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)+(0.0790P)²+1.0212P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1163
_refine_ls_wR_factor_ref         0.1276
_reflns_number_gt                1884
_reflns_number_total             2522
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0255205_s1_2.cif
_cod_data_source_block           00285
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' tag value 'multi-scans' was replaced
with 'multi-scan' value.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4318274
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
N6 N 0.5592(11) 0.1949(6) 0.6802(7) 0.060(3) Uani 0.694(8) 1 d PDU A 1
O6 O 0.7153(10) 0.1989(6) 0.7211(6) 0.0502(17) Uani 0.694(8) 1 d PDU A 1
O7 O 0.4732(18) 0.1154(12) 0.6916(17) 0.073(4) Uani 0.694(8) 1 d PDU A 1
N6A N 0.663(3) 0.1677(19) 0.7226(19) 0.0502(17) Uani 0.306(8) 1 d PDU A 2
O6A O 0.7283(19) 0.2385(12) 0.6795(11) 0.0502(17) Uani 0.306(8) 1 d PDU A 2
O7A O 0.500(4) 0.148(4) 0.698(5) 0.073(4) Uani 0.306(8) 1 d PDU A 2
Ru1 Ru 0.83771(6) 0.08123(4) 0.79929(3) 0.0318(2) Uani 1 1 d U . .
N1 N 0.7081(6) 0.1379(4) 0.9091(3) 0.0302(10) Uani 1 1 d U A .
N2 N 1.0102(6) 0.1985(4) 0.8455(3) 0.0323(10) Uani 1 1 d U A .
C1 C 0.5488(8) 0.1041(4) 0.9355(4) 0.0350(13) Uani 1 1 d U . .
H1A H 0.4931 0.0474 0.9046 0.042 Uiso 1 1 calc R A .
C2 C 0.4630(8) 0.1473(5) 1.0046(4) 0.0366(13) Uani 1 1 d U A .
H2A H 0.3497 0.1216 1.0207 0.044 Uiso 1 1 calc R . .
C3 C 0.5449(8) 0.2296(5) 1.0508(4) 0.0419(15) Uani 1 1 d U . .
H3A H 0.4903 0.2597 1.1004 0.050 Uiso 1 1 calc R A .
C4 C 0.7059(8) 0.2669(5) 1.0239(4) 0.0385(14) Uani 1 1 d U A .
H4A H 0.7614 0.3245 1.0534 0.046 Uiso 1 1 calc R . .
C5 C 0.7875(7) 0.2197(4) 0.9530(4) 0.0312(12) Uani 1 1 d U . .
C6 C 0.9576(7) 0.2546(4) 0.9171(4) 0.0327(12) Uani 1 1 d U A .
C7 C 1.0576(8) 0.3372(5) 0.9510(4) 0.0398(14) Uani 1 1 d U . .
H7A H 1.0211 0.3746 1.0015 0.048 Uiso 1 1 calc R A .
C8 C 1.2134(9) 0.3640(5) 0.9092(5) 0.0463(16) Uani 1 1 d U A .
H8A H 1.2837 0.4209 0.9308 0.056 Uiso 1 1 calc R . .
C9 C 1.2655(8) 0.3087(5) 0.8371(4) 0.0448(15) Uani 1 1 d U . .
H9A H 1.3704 0.3277 0.8080 0.054 Uiso 1 1 calc R A .
C10 C 1.1648(8) 0.2257(5) 0.8071(4) 0.0381(14) Uani 1 1 d U A .
H10A H 1.2040 0.1862 0.7584 0.046 Uiso 1 1 calc R . .
N3 N 0.9436(9) 0.0172(5) 0.6166(4) 0.0559(15) Uani 1 1 d U . .
O1 O 0.9983(7) 0.0555(4) 0.6948(3) 0.0514(12) Uani 1 1 d U A .
O2 O 0.7873(8) -0.0155(5) 0.6082(4) 0.0815(18) Uani 1 1 d . A .
N4 N 0.6808(7) -0.0191(4) 0.7744(3) 0.0414(13) Uani 1 1 d . A .
O3 O 0.5834(8) -0.0837(4) 0.7686(4) 0.0632(14) Uani 1 1 d . . .
N5 N 1.0039(7) -0.0153(4) 0.8810(3) 0.0412(13) Uani 1 1 d . A .
O4 O 1.1744(6) -0.0104(4) 0.8789(3) 0.0577(13) Uani 1 1 d . . .
O5 O 0.9391(6) -0.0791(4) 0.9296(4) 0.0559(13) 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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O7 N6 O6 115.3(11) . . ?
N6 O6 Ru1 124.4(6) . . ?
O6A N6A O7A 114.5(14) . . ?
O6A N6A Ru1 117.3(14) . . ?
O7A N6A Ru1 127(2) . . ?
N4 Ru1 N6A 86.4(6) . . ?
N4 Ru1 O1 97.5(2) . . ?
N6A Ru1 O1 93.3(9) . . ?
N4 Ru1 N5 90.0(2) . . ?
N6A Ru1 N5 176.0(5) . . ?
O1 Ru1 N5 88.9(2) . . ?
N4 Ru1 N2 172.5(2) . . ?
N6A Ru1 N2 95.8(7) . . ?
O1 Ru1 N2 89.50(18) . . ?
N5 Ru1 N2 87.61(19) . . ?
N4 Ru1 N1 95.3(2) . . ?
N6A Ru1 N1 85.1(10) . . ?
O1 Ru1 N1 166.95(18) . . ?
N5 Ru1 N1 93.51(19) . . ?
N2 Ru1 N1 77.80(18) . . ?
N4 Ru1 O6 101.7(3) . . ?
N6A Ru1 O6 15.7(5) . . ?
O1 Ru1 O6 87.8(3) . . ?
N5 Ru1 O6 168.2(2) . . ?
N2 Ru1 O6 81.1(2) . . ?
N1 Ru1 O6 87.3(3) . . ?
C1 N1 C5 118.4(5) . . ?
C1 N1 Ru1 125.1(4) . . ?
C5 N1 Ru1 116.3(4) . . ?
C10 N2 C6 118.7(5) . . ?
C10 N2 Ru1 124.7(4) . . ?
C6 N2 Ru1 116.5(4) . . ?
N1 C1 C2 123.3(6) . . ?
C1 C2 C3 118.6(6) . . ?
C4 C3 C2 119.2(6) . . ?
C3 C4 C5 119.7(6) . . ?
N1 C5 C4 120.8(5) . . ?
N1 C5 C6 114.9(5) . . ?
C4 C5 C6 124.3(5) . . ?
N2 C6 C7 121.6(5) . . ?
N2 C6 C5 114.4(5) . . ?
C7 C6 C5 124.0(5) . . ?
C6 C7 C8 118.3(6) . . ?
C9 C8 C7 120.2(6) . . ?
C8 C9 C10 119.6(6) . . ?
N2 C10 C9 121.6(6) . . ?
O2 N3 O1 116.4(6) . . ?
N3 O1 Ru1 125.4(4) . . ?
O3 N4 Ru1 172.6(5) . . ?
O5 N5 O4 119.3(5) . . ?
O5 N5 Ru1 121.2(4) . . ?
O4 N5 Ru1 119.5(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
N6 O7 1.246(7) . ?
N6 O6 1.249(7) . ?
O6 Ru1 2.088(7) . ?
N6A O6A 1.248(8) . ?
N6A O7A 1.249(8) . ?
N6A Ru1 1.991(18) . ?
Ru1 N4 1.775(5) . ?
Ru1 O1 2.048(5) . ?
Ru1 N5 2.073(5) . ?
Ru1 N2 2.078(5) . ?
Ru1 N1 2.086(5) . ?
N1 C1 1.344(7) . ?
N1 C5 1.363(7) . ?
N2 C10 1.363(7) . ?
N2 C6 1.370(7) . ?
C1 C2 1.367(8) . ?
C2 C3 1.390(9) . ?
C3 C4 1.374(9) . ?
C4 C5 1.395(8) . ?
C5 C6 1.475(8) . ?
C6 C7 1.384(8) . ?
C7 C8 1.395(9) . ?
C8 C9 1.369(9) . ?
C9 C10 1.374(9) . ?
N3 O2 1.225(8) . ?
N3 O1 1.285(7) . ?
N4 O3 1.112(6) . ?
N5 O5 1.229(6) . ?
N5 O4 1.260(6) . ?
