#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/99/2219957.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_2219957
loop_
_publ_author_name
'Jude, Hershel'
'White, Peter S.'
'Dattelbaum, Dana M.'
'Rocha, Reginaldo C.'
_publ_section_title
;
 trans-Diaquabis(2,2'-bipyridine-κ²N,N')ruthenium(II)
 bis(trifluoromethanesulfonate)
;
_journal_coeditor_code           PK2108
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1388
_journal_page_last               m1389
_journal_paper_doi               10.1107/S1600536808028195
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Ru (C10 H8 N2)2 (H2 O)2] (C F3 O3 S)2'
_chemical_formula_moiety         'C20 H20 N4 O2 Ru 2+ , 2C F3 O3 S -'
_chemical_formula_sum            'C22 H20 F6 N4 O8 Ru S2'
_chemical_formula_weight         747.61
_chemical_name_systematic
;
trans-Diaquabis(2,2'-bipyridine-κ²N,N')ruthenium(II)
bis(trifluoromethanesulfonate)
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.095(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.6569(5)
_cell_length_b                   14.1272(8)
_cell_length_c                   11.3226(6)
_cell_measurement_reflns_used    1677
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.33
_cell_measurement_theta_min      5.01
_cell_volume                     1382.71(13)
_computing_cell_refinement       'APEX2 (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD area-detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_sigmaI/netI    0.0240
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            15574
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         69.66
_diffrn_reflns_theta_min         5.01
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.877
_exptl_absorpt_correction_T_max  0.875
_exptl_absorpt_correction_T_min  0.340
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Numerical followed by SADABS (Bruker, 2007)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.796
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.692
_refine_diff_density_min         -0.454
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         2538
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0263
_refine_ls_R_factor_gt           0.0249
_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)+(0.0273P)²+1.4103P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0607
_refine_ls_wR_factor_ref         0.0615
_reflns_number_gt                2436
_reflns_number_total             2538
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            pk2108.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2219957
_cod_database_fobs_code          2219957
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_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
Ru Ru1 0.5000 0.5000 0.0000 0.01303(9) Uani d S 1
O O1 0.64907(19) 0.61137(12) 0.05421(17) 0.0181(3) Uani d . 1
N N2 0.6089(2) 0.42131(12) 0.13474(15) 0.0154(4) Uani d . 1
C C3 0.5507(3) 0.39407(15) 0.23786(19) 0.0192(4) Uani d . 1
H H3 0.4431 0.4020 0.2475 0.023 Uiso calc R 1
C C4 0.6412(3) 0.35501(17) 0.3302(2) 0.0243(5) Uani d . 1
H H4 0.5965 0.3365 0.4014 0.029 Uiso calc R 1
C C5 0.7986(3) 0.34355(18) 0.3164(2) 0.0271(5) Uani d . 1
H H5 0.8644 0.3208 0.3800 0.033 Uiso calc R 1
C C6 0.8584(3) 0.36563(17) 0.2090(2) 0.0230(5) Uani d . 1
H H6 0.9650 0.3559 0.1970 0.028 Uiso calc R 1
C C7 0.7606(3) 0.40225(15) 0.11871(19) 0.0179(4) Uani d . 1
C C8 0.8048(2) 0.41339(15) -0.00489(19) 0.0170(4) Uani d . 1
C C9 0.9491(3) 0.38753(16) -0.0439(2) 0.0208(5) Uani d . 1
H H9 1.0312 0.3708 0.0113 0.025 Uiso calc R 1
C C10 0.9709(3) 0.38668(17) -0.1642(2) 0.0240(5) Uani d . 1
H H10 1.0692 0.3716 -0.1926 0.029 Uiso calc R 1
C C11 0.8470(3) 0.40816(17) -0.2426(2) 0.0230(5) Uani d . 1
H H11 0.8578 0.4043 -0.3255 0.028 Uiso calc R 1
C C12 0.7075(3) 0.43527(16) -0.19861(19) 0.0194(4) Uani d . 1
H H12 0.6233 0.4499 -0.2528 0.023 Uiso calc R 1
N N13 0.6869(2) 0.44164(12) -0.08110(16) 0.0160(4) Uani d . 1
S S1 0.31188(6) 0.31728(4) 0.61491(5) 0.01857(13) Uani d . 1
C C14 0.2290(3) 0.3937(2) 0.4986(2) 0.0343(6) Uani d . 1
F F15 0.1904(2) 0.34309(16) 0.40134(15) 0.0556(5) Uani d . 1
F F16 0.3298(2) 0.45966(12) 0.46821(15) 0.0458(4) Uani d . 1
F F17 0.1035(2) 0.43667(17) 0.53333(18) 0.0652(6) Uani d . 1
O O19 0.44116(19) 0.27407(11) 0.55926(14) 0.0241(4) Uani d . 1
O O20 0.3551(2) 0.38361(12) 0.70808(14) 0.0271(4) Uani d . 1
O O21 0.1893(2) 0.25354(14) 0.64049(17) 0.0360(5) Uani d . 1
H H1A 0.644(3) 0.6198(19) 0.120(3) 0.016(7) Uiso d . 1
H H1B 0.619(4) 0.651(2) 0.018(3) 0.033(9) Uiso d . 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru 0.0552 3.2960 '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
N2 Ru1 N2 3_665 . 180.00(8)
N2 Ru1 N13 3_665 3_665 77.18(7)
N2 Ru1 N13 . 3_665 102.82(7)
N2 Ru1 N13 3_665 . 102.82(7)
N2 Ru1 N13 . . 77.18(7)
N13 Ru1 N13 3_665 . 180.0
N2 Ru1 O1 3_665 3_665 86.51(7)
N2 Ru1 O1 . 3_665 93.49(7)
N13 Ru1 O1 3_665 3_665 86.88(7)
N13 Ru1 O1 . 3_665 93.12(7)
N2 Ru1 O1 3_665 . 93.49(7)
N2 Ru1 O1 . . 86.51(7)
N13 Ru1 O1 3_665 . 93.12(7)
N13 Ru1 O1 . . 86.88(7)
O1 Ru1 O1 3_665 . 180.0
Ru1 O1 H1A . . 110(2)
Ru1 O1 H1B . . 102(3)
H1A O1 H1B . . 113(3)
C3 N2 C7 . . 117.74(19)
C3 N2 Ru1 . . 127.77(15)
C7 N2 Ru1 . . 114.28(14)
N2 C3 C4 . . 122.9(2)
N2 C3 H3 . . 118.6
C4 C3 H3 . . 118.6
C3 C4 C5 . . 118.6(2)
C3 C4 H4 . . 120.7
C5 C4 H4 . . 120.7
C6 C5 C4 . . 119.2(2)
C6 C5 H5 . . 120.4
C4 C5 H5 . . 120.4
C5 C6 C7 . . 119.2(2)
C5 C6 H6 . . 120.4
C7 C6 H6 . . 120.4
N2 C7 C6 . . 121.9(2)
N2 C7 C8 . . 113.93(19)
C6 C7 C8 . . 123.8(2)
N13 C8 C9 . . 122.0(2)
N13 C8 C7 . . 114.07(18)
C9 C8 C7 . . 123.6(2)
C10 C9 C8 . . 119.0(2)
C10 C9 H9 . . 120.5
C8 C9 H9 . . 120.5
C9 C10 C11 . . 119.0(2)
C9 C10 H10 . . 120.5
C11 C10 H10 . . 120.5
C12 C11 C10 . . 119.3(2)
C12 C11 H11 . . 120.4
C10 C11 H11 . . 120.4
N13 C12 C11 . . 122.4(2)
N13 C12 H12 . . 118.8
C11 C12 H12 . . 118.8
C12 N13 C8 . . 117.98(18)
C12 N13 Ru1 . . 127.48(15)
C8 N13 Ru1 . . 114.35(14)
O21 S1 O20 . . 115.16(10)
O21 S1 O19 . . 114.90(11)
O20 S1 O19 . . 114.53(10)
O21 S1 C14 . . 104.58(13)
O20 S1 C14 . . 102.69(12)
O19 S1 C14 . . 102.65(11)
F17 C14 F16 . . 108.4(2)
F17 C14 F15 . . 108.5(2)
F16 C14 F15 . . 107.4(2)
F17 C14 S1 . . 110.79(19)
F16 C14 S1 . . 111.30(19)
F15 C14 S1 . . 110.4(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Ru1 N2 3_665 2.0727(17)
Ru1 N2 . 2.0727(17)
Ru1 N13 3_665 2.0739(17)
Ru1 N13 . 2.0739(17)
Ru1 O1 3_665 2.1053(16)
Ru1 O1 . 2.1053(16)
O1 H1A . 0.75(3)
O1 H1B . 0.73(4)
N2 C3 . 1.352(3)
N2 C7 . 1.363(3)
C3 C4 . 1.387(3)
C3 H3 . 0.9500
C4 C5 . 1.389(4)
C4 H4 . 0.9500
C5 C6 . 1.383(3)
C5 H5 . 0.9500
C6 C7 . 1.391(3)
C6 H6 . 0.9500
C7 C8 . 1.479(3)
C8 N13 . 1.360(3)
C8 C9 . 1.396(3)
C9 C10 . 1.385(3)
C9 H9 . 0.9500
C10 C11 . 1.389(4)
C10 H10 . 0.9500
C11 C12 . 1.384(3)
C11 H11 . 0.9500
C12 N13 . 1.355(3)
C12 H12 . 0.9500
S1 O21 . 1.4334(18)
S1 O20 . 1.4451(17)
S1 O19 . 1.4486(16)
S1 C14 . 1.820(3)
C14 F17 . 1.323(3)
C14 F16 . 1.334(3)
C14 F15 . 1.340(3)
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O1 H1B O19 2_655 0.73(4) 2.01(4) 2.727(2) 169(4)
O1 H1A O20 3_666 0.75(3) 1.95(3) 2.695(2) 169(3)
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
N13 Ru1 N2 C3 3_665 16.01(19)
N13 Ru1 N2 C3 . -163.99(19)
O1 Ru1 N2 C3 3_665 -71.58(18)
O1 Ru1 N2 C3 . 108.42(18)
N13 Ru1 N2 C7 3_665 -158.51(14)
N13 Ru1 N2 C7 . 21.49(14)
O1 Ru1 N2 C7 3_665 113.90(15)
O1 Ru1 N2 C7 . -66.10(15)
C7 N2 C3 C4 . 5.3(3)
Ru1 N2 C3 C4 . -169.07(17)
N2 C3 C4 C5 . 0.2(4)
C3 C4 C5 C6 . -4.1(4)
C4 C5 C6 C7 . 2.5(4)
C3 N2 C7 C6 . -7.0(3)
Ru1 N2 C7 C6 . 168.14(17)
C3 N2 C7 C8 . 166.29(18)
Ru1 N2 C7 C8 . -18.6(2)
C5 C6 C7 N2 . 3.2(3)
C5 C6 C7 C8 . -169.4(2)
N2 C7 C8 N13 . 0.6(3)
C6 C7 C8 N13 . 173.7(2)
N2 C7 C8 C9 . -172.6(2)
C6 C7 C8 C9 . 0.5(3)
N13 C8 C9 C10 . -2.8(3)
C7 C8 C9 C10 . 169.9(2)
C8 C9 C10 C11 . -2.4(3)
C9 C10 C11 C12 . 3.8(4)
C10 C11 C12 N13 . -0.1(4)
C11 C12 N13 C8 . -5.0(3)
C11 C12 N13 Ru1 . 169.81(17)
C9 C8 N13 C12 . 6.5(3)
C7 C8 N13 C12 . -166.89(19)
C9 C8 N13 Ru1 . -169.01(16)
C7 C8 N13 Ru1 . 17.6(2)
N2 Ru1 N13 C12 3_665 -16.10(19)
N2 Ru1 N13 C12 . 163.90(19)
O1 Ru1 N13 C12 3_665 71.02(18)
O1 Ru1 N13 C12 . -108.98(18)
N2 Ru1 N13 C8 3_665 158.85(14)
N2 Ru1 N13 C8 . -21.15(14)
O1 Ru1 N13 C8 3_665 -114.03(15)
O1 Ru1 N13 C8 . 65.97(15)
O21 S1 C14 F17 . 57.2(2)
O20 S1 C14 F17 . -63.4(2)
O19 S1 C14 F17 . 177.4(2)
O21 S1 C14 F16 . 177.87(17)
O20 S1 C14 F16 . 57.3(2)
O19 S1 C14 F16 . -61.9(2)
O21 S1 C14 F15 . -63.0(2)
O20 S1 C14 F15 . 176.41(18)
O19 S1 C14 F15 . 57.3(2)
