#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/24/2232415.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2232415
loop_
_publ_author_name
'Minaker, Samuel A.'
'Wang, Ruiyao'
'Aquino, Manuel A. S.'
_publ_section_title
;
 Tetra-μ-acetato-κ⁸O:O'-bis[(3-cyanopyridine-κN¹)ruthenium(II,III)](Ru---Ru)
 hexafluoridophosphate 1,2-dichloroethane monosolvate
;
_journal_coeditor_code           NK2113
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1554
_journal_paper_doi               10.1107/S1600536811041997
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac
'[Ru2 (C2 H3 O2)4 (C6 H4 N2)2] P F6, C2 H4 Cl2'
_chemical_formula_moiety         'C20 H20 N4 O8 Ru2 +, F6 P -, C2 H4 Cl2'
_chemical_formula_sum            'C22 H24 Cl2 F6 N4 O8 P Ru2'
_chemical_formula_weight         890.46
_chemical_name_systematic
;
Tetra-μ-acetato-κ⁸O:O'-bis[(3-cyanopyridine-
κN¹)ruthenium(II,III)](Ru---Ru) hexafluoridophosphate
1,2-dichloroethane monosolvate
;
_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                105.860(6)
_cell_angle_beta                 108.929(5)
_cell_angle_gamma                104.099(5)
_cell_formula_units_Z            1
_cell_length_a                   8.1743(6)
_cell_length_b                   10.3955(10)
_cell_length_c                   11.3970(10)
_cell_measurement_reflns_used    4068
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      27.12
_cell_measurement_theta_min      2.35
_cell_volume                     820.37(14)
_computing_cell_refinement       'SAINT (Bruker, 2010)'
_computing_data_collection       'APEX2 (Bruker, 2010)'
_computing_data_reduction        'SAINT (Bruker, 2010)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'φ and ω 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  0.0269
_diffrn_reflns_av_sigmaI/netI    0.0398
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6133
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    1.214
_exptl_absorpt_correction_T_max  0.8388
_exptl_absorpt_correction_T_min  0.7933
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2010)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.802
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             439
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.845
_refine_diff_density_min         -0.755
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3175
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0279
_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)+(0.0226P)²+1.1880P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0726
_refine_ls_wR_factor_ref         0.0775
_reflns_number_gt                2784
_reflns_number_total             3175
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            nk2113.cif
_cod_data_source_block           I
_cod_original_cell_volume        820.38(14)
_cod_database_code               2232415
_cod_database_fobs_code          2232415
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_disorder_assembly
_atom_site_disorder_group
P P1 0.0000 0.5000 0.0000 0.0346(3) Uani d S 1 2 . .
Ru Ru1 0.47865(3) 0.38173(3) 0.45928(2) 0.02328(10) Uani d . 1 1 . .
O O1 0.7543(3) 0.4309(2) 0.5531(2) 0.0269(5) Uani d . 1 1 . .
O O2 0.7964(3) 0.6638(2) 0.6343(2) 0.0270(5) Uani d . 1 1 . .
O O3 0.5095(3) 0.3989(2) 0.2954(2) 0.0271(5) Uani d . 1 1 . .
O O4 0.5481(3) 0.6314(2) 0.3736(2) 0.0270(5) Uani d . 1 1 . .
N N1 0.4058(4) 0.1379(3) 0.3754(3) 0.0256(6) Uani d . 1 1 . .
N N2 -0.0128(5) -0.2151(4) 0.4373(4) 0.0600(10) Uani d . 1 1 . .
C C1 0.8583(4) 0.5624(4) 0.6211(3) 0.0274(7) Uani d . 1 1 . .
C C2 1.0631(4) 0.6004(4) 0.6875(4) 0.0359(8) Uani d . 1 1 . .
H H2A 1.1126 0.6717 0.7792 0.054 Uiso calc R 1 1 . .
H H2B 1.1218 0.6405 0.6364 0.054 Uiso calc R 1 1 . .
H H2C 1.0893 0.5140 0.6906 0.054 Uiso calc R 1 1 . .
C C3 0.5368(4) 0.5203(4) 0.2848(3) 0.0272(7) Uani d . 1 1 . .
C C4 0.5549(5) 0.5324(4) 0.1623(4) 0.0373(8) Uani d . 1 1 . .
H H4A 0.6669 0.6146 0.1884 0.056 Uiso calc R 1 1 . .
H H4B 0.4457 0.5463 0.1073 0.056 Uiso calc R 1 1 . .
H H4C 0.5640 0.4443 0.1104 0.056 Uiso calc R 1 1 . .
C C5 0.2756(5) 0.0610(4) 0.4029(4) 0.0345(8) Uani d . 1 1 . .
H H5A 0.2130 0.1083 0.4463 0.041 Uiso calc R 1 1 . .
C C6 0.2307(4) -0.0857(4) 0.3693(4) 0.0324(7) Uani d . 1 1 . .
C C7 0.3223(5) -0.1549(4) 0.3063(4) 0.0347(8) Uani d . 1 1 . .
H H7A 0.2967 -0.2547 0.2849 0.042 Uiso calc R 1 1 . .
C C8 0.4511(5) -0.0752(4) 0.2759(4) 0.0391(8) Uani d . 1 1 . .
H H8A 0.5140 -0.1197 0.2307 0.047 Uiso calc R 1 1 . .
C C9 0.4882(5) 0.0701(4) 0.3115(4) 0.0341(8) Uani d . 1 1 . .
H H9A 0.5768 0.1239 0.2891 0.041 Uiso calc R 1 1 . .
C C10 0.0933(5) -0.1605(4) 0.4058(4) 0.0411(9) Uani d . 1 1 . .
F F1 -0.0541(3) 0.6132(3) 0.0917(2) 0.0518(6) Uani d . 1 1 . .
F F2 0.1696(3) 0.6283(3) 0.0146(2) 0.0474(6) Uani d . 1 1 . .
F F3 0.1334(3) 0.4879(3) 0.1314(2) 0.0485(6) Uani d . 1 1 . .
Cl Cl1A 0.242(4) 0.032(3) 0.9565(15) 0.163(4) Uani d P 0.51(6) 1 A 1
C C11A 0.056(5) 0.077(4) 1.010(4) 0.108(10) Uani d P 0.51(6) 1 . 1
H H11A 0.1094 0.1457 1.1040 0.129 Uiso calc PR 0.51(6) 1 A 1
H H11B -0.0193 0.1142 0.9496 0.129 Uiso calc PR 0.51(6) 1 A 1
Cl Cl1B 0.191(4) 0.0453(18) 0.914(4) 0.152(7) Uani d P 0.49(6) 1 A 2
C C11B 0.013(10) -0.052(7) 0.969(5) 0.21(3) Uani d P 0.49(6) 1 . 2
H H11C -0.1020 -0.1225 0.8912 0.246 Uiso calc PR 0.49(6) 1 A 2
H H11D 0.0663 -0.0995 1.0277 0.246 Uiso calc PR 0.49(6) 1 A 2
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'
F F 0.0171 0.0103 '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'
P P 0.1023 0.0942 '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'
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
F1 P1 F1 2_565 . 180.00(16)
F1 P1 F2 2_565 . 89.90(12)
F1 P1 F2 . . 90.10(12)
F1 P1 F2 2_565 2_565 90.11(12)
F1 P1 F2 . 2_565 89.89(12)
F2 P1 F2 . 2_565 180.0
F1 P1 F3 2_565 . 90.18(13)
F1 P1 F3 . . 89.82(13)
F2 P1 F3 . . 89.81(12)
F2 P1 F3 2_565 . 90.19(12)
F1 P1 F3 2_565 2_565 89.82(13)
F1 P1 F3 . 2_565 90.18(13)
F2 P1 F3 . 2_565 90.19(12)
F2 P1 F3 2_565 2_565 89.81(12)
F3 P1 F3 . 2_565 180.0
O3 Ru1 O1 . . 89.72(9)
O3 Ru1 O2 . 2_666 89.97(9)
O1 Ru1 O2 . 2_666 178.99(9)
O3 Ru1 O4 . 2_666 178.79(9)
O1 Ru1 O4 . 2_666 89.53(9)
O2 Ru1 O4 2_666 2_666 90.77(8)
O3 Ru1 Ru1 . 2_666 90.35(7)
O1 Ru1 Ru1 . 2_666 90.07(7)
O2 Ru1 Ru1 2_666 2_666 88.97(6)
O4 Ru1 Ru1 2_666 2_666 88.71(7)
O3 Ru1 N1 . . 92.05(9)
O1 Ru1 N1 . . 95.14(9)
O2 Ru1 N1 2_666 . 85.83(9)
O4 Ru1 N1 2_666 . 88.95(9)
Ru1 Ru1 N1 2_666 . 174.27(7)
C1 O1 Ru1 . . 118.3(2)
C1 O2 Ru1 . 2_666 119.4(2)
C3 O3 Ru1 . . 118.4(2)
C3 O4 Ru1 . 2_666 119.5(2)
C9 N1 C5 . . 118.7(3)
C9 N1 Ru1 . . 125.8(2)
C5 N1 Ru1 . . 115.4(2)
O2 C1 O1 . . 123.2(3)
O2 C1 C2 . . 118.0(3)
O1 C1 C2 . . 118.8(3)
C1 C2 H2A . . 109.5
C1 C2 H2B . . 109.5
H2A C2 H2B . . 109.5
C1 C2 H2C . . 109.5
H2A C2 H2C . . 109.5
H2B C2 H2C . . 109.5
O4 C3 O3 . . 123.1(3)
O4 C3 C4 . . 118.5(3)
O3 C3 C4 . . 118.5(3)
C3 C4 H4A . . 109.5
C3 C4 H4B . . 109.5
H4A C4 H4B . . 109.5
C3 C4 H4C . . 109.5
H4A C4 H4C . . 109.5
H4B C4 H4C . . 109.5
N1 C5 C6 . . 121.5(3)
N1 C5 H5A . . 119.3
C6 C5 H5A . . 119.3
C7 C6 C5 . . 119.4(3)
C7 C6 C10 . . 122.2(3)
C5 C6 C10 . . 118.4(3)
C8 C7 C6 . . 118.1(3)
C8 C7 H7A . . 120.9
C6 C7 H7A . . 120.9
C7 C8 C9 . . 119.4(3)
C7 C8 H8A . . 120.3
C9 C8 H8A . . 120.3
N1 C9 C8 . . 122.8(3)
N1 C9 H9A . . 118.6
C8 C9 H9A . . 118.6
N2 C10 C6 . . 177.9(4)
C11A C11A Cl1A 2_557 . 97(3)
C11A C11A H11A 2_557 . 112.3
Cl1A C11A H11A . . 112.3
C11A C11A H11B 2_557 . 112.3
Cl1A C11A H11B . . 112.3
H11A C11A H11B . . 109.9
C11B C11B Cl1B 2_557 . 99(9)
C11B C11B H11C 2_557 . 111.9
Cl1B C11B H11C . . 111.9
C11B C11B H11D 2_557 . 111.9
Cl1B C11B H11D . . 111.9
H11C C11B H11D . . 109.6
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
P1 F1 2_565 1.598(2)
P1 F1 . 1.598(2)
P1 F2 . 1.599(2)
P1 F2 2_565 1.599(2)
P1 F3 . 1.600(2)
P1 F3 2_565 1.600(2)
Ru1 O3 . 2.012(2)
Ru1 O1 . 2.015(2)
Ru1 O2 2_666 2.016(2)
Ru1 O4 2_666 2.023(2)
Ru1 Ru1 2_666 2.2702(6)
Ru1 N1 . 2.295(3)
O1 C1 . 1.273(4)
O2 C1 . 1.270(4)
O2 Ru1 2_666 2.016(2)
O3 C3 . 1.273(4)
O4 C3 . 1.272(4)
O4 Ru1 2_666 2.023(2)
N1 C9 . 1.323(4)
N1 C5 . 1.345(4)
N2 C10 . 1.130(5)
C1 C2 . 1.491(4)
C2 H2A . 0.9800
C2 H2B . 0.9800
C2 H2C . 0.9800
C3 C4 . 1.485(4)
C4 H4A . 0.9800
C4 H4B . 0.9800
C4 H4C . 0.9800
C5 C6 . 1.387(5)
C5 H5A . 0.9500
C6 C7 . 1.387(5)
C6 C10 . 1.447(5)
C7 C8 . 1.373(5)
C7 H7A . 0.9500
C8 C9 . 1.378(5)
C8 H8A . 0.9500
C9 H9A . 0.9500
Cl1A C11A . 1.93(4)
C11A C11A 2_557 1.56(7)
C11A H11A . 0.9900
C11A H11B . 0.9900
Cl1B C11B . 1.93(8)
C11B C11B 2_557 1.22(11)
C11B H11C . 0.9900
C11B H11D . 0.9900
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_site_symmetry_1
_geom_torsion
O3 Ru1 O1 C1 . 90.1(2)
O4 Ru1 O1 C1 2_666 -88.9(2)
Ru1 Ru1 O1 C1 2_666 -0.2(2)
N1 Ru1 O1 C1 . -177.8(2)
O1 Ru1 O3 C3 . -91.2(2)
O2 Ru1 O3 C3 2_666 87.8(2)
Ru1 Ru1 O3 C3 2_666 -1.2(2)
N1 Ru1 O3 C3 . 173.6(2)
O3 Ru1 N1 C9 . 41.4(3)
O1 Ru1 N1 C9 . -48.5(3)
O2 Ru1 N1 C9 2_666 131.3(3)
O4 Ru1 N1 C9 2_666 -137.9(3)
O3 Ru1 N1 C5 . -143.1(2)
O1 Ru1 N1 C5 . 127.0(2)
O2 Ru1 N1 C5 2_666 -53.3(2)
O4 Ru1 N1 C5 2_666 37.6(2)
Ru1 O2 C1 O1 2_666 -1.4(4)
Ru1 O2 C1 C2 2_666 177.8(2)
Ru1 O1 C1 O2 . 1.0(4)
Ru1 O1 C1 C2 . -178.2(2)
Ru1 O4 C3 O3 2_666 -0.1(4)
Ru1 O4 C3 C4 2_666 179.3(2)
Ru1 O3 C3 O4 . 1.0(4)
Ru1 O3 C3 C4 . -178.5(2)
C9 N1 C5 C6 . 1.9(5)
Ru1 N1 C5 C6 . -173.9(3)
N1 C5 C6 C7 . 0.2(5)
N1 C5 C6 C10 . 178.1(3)
C5 C6 C7 C8 . -2.0(5)
C10 C6 C7 C8 . -179.8(4)
C6 C7 C8 C9 . 1.6(5)
C5 N1 C9 C8 . -2.3(5)
Ru1 N1 C9 C8 . 173.0(3)
C7 C8 C9 N1 . 0.5(6)
