#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/49/2214904.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_2214904
loop_
_publ_author_name
'Xu, Feng'
'Huang, Wei'
_publ_section_title
;
 Redetermination of
 cis-diacetonitrilebis(2,2'-bipyridine)ruthenium(II)
 hexafluorophosphate
;
_journal_coeditor_code           WW2089
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2114
_journal_page_last               m2114
_journal_paper_doi               10.1107/S1600536807033065
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Ru (C10 H8 N2)2 (C2 H3 N)2] (F6 P)2'
_chemical_formula_moiety         'C24 H22 N6 Ru, 2(F6 P)'
_chemical_formula_sum            'C24 H22 F12 N6 P2 Ru'
_chemical_formula_weight         785.49
_chemical_name_systematic
;
cis-diacetonitrilebis(2,2'-bipyridine)ruthenium(II) hexafluorophosphate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 96.201(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.2499(18)
_cell_length_b                   10.5008(11)
_cell_length_c                   16.6600(17)
_cell_measurement_reflns_used    1829
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      19.099
_cell_measurement_theta_min      2.274
_cell_volume                     3000.1(5)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_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  0.0346
_diffrn_reflns_av_sigmaI/netI    0.0577
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7231
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.27
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.731
_exptl_absorpt_correction_T_max  0.9305
_exptl_absorpt_correction_T_min  0.8920
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.739
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.543
_refine_diff_density_min         -0.307
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         2641
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_gt           0.0479
_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)+(0.0345P)²+1.5660P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.0982
_reflns_number_gt                1718
_reflns_number_total             2641
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ww2089.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2214904
_cod_database_fobs_code          2214904
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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 0.0000 0.97826(5) 0.7500 0.0657(2) Uani d S 1
C C1 0.0270(3) 1.1608(4) 0.8777(3) 0.0689(12) Uani d . 1
C C2 0.0579(4) 1.2636(5) 0.9204(3) 0.1081(19) Uani d . 1
H H2 0.0346 1.2943 0.9644 0.130 Uiso calc R 1
C C3 0.1238(5) 1.3207(6) 0.8976(4) 0.147(3) Uani d . 1
H H3 0.1459 1.3898 0.9266 0.177 Uiso calc R 1
C C4 0.1562(4) 1.2770(7) 0.8338(4) 0.145(3) Uani d . 1
H H4 0.2005 1.3153 0.8174 0.174 Uiso calc R 1
C C5 0.1225(3) 1.1744(6) 0.7932(3) 0.0982(17) Uani d . 1
H H5 0.1456 1.1433 0.7492 0.118 Uiso calc R 1
C C6 -0.0394(3) 1.0877(4) 0.8992(3) 0.0652(12) Uani d . 1
C C7 -0.0783(3) 1.1116(5) 0.9658(3) 0.0906(15) Uani d . 1
H H7 -0.0651 1.1818 0.9985 0.109 Uiso calc R 1
C C8 -0.1358(3) 1.0317(7) 0.9831(3) 0.1064(19) Uani d . 1
H H8 -0.1619 1.0462 1.0282 0.128 Uiso calc R 1
C C9 -0.1549(3) 0.9330(7) 0.9356(3) 0.120(2) Uani d . 1
H H9 -0.1944 0.8777 0.9470 0.144 Uiso calc R 1
C C10 -0.1151(3) 0.9134(6) 0.8687(3) 0.1113(19) Uani d . 1
H H10 -0.1285 0.8435 0.8357 0.134 Uiso calc R 1
C C11 0.1279(11) 0.7826(11) 0.8336(6) 0.115(3) Uani d PU 0.546(11)
C C12 0.1854(8) 0.6918(10) 0.8694(6) 0.109(5) Uani d P 0.546(11)
H H12A 0.2363 0.7293 0.8712 0.163 Uiso d PR 0.546(11)
H H12B 0.1744 0.6717 0.9232 0.163 Uiso d PR 0.546(11)
H H12C 0.1837 0.6154 0.8376 0.163 Uiso d PR 0.546(11)
C C11' 0.0731(12) 0.7344(15) 0.8298(8) 0.120(2) Uani d PU 0.454(11)
C C12' 0.1042(13) 0.6169(14) 0.8608(8) 0.141(9) Uani d P 0.454(11)
H H12D 0.0652 0.5539 0.8676 0.212 Uiso d PR 0.454(11)
H H12E 0.1392 0.5854 0.8244 0.212 Uiso d PR 0.454(11)
H H12F 0.1330 0.6351 0.9122 0.212 Uiso d PR 0.454(11)
F F1 0.6154(3) 0.8889(5) 0.6588(3) 0.220(3) Uani d . 1
F F2 0.7125(6) 1.035(2) 0.5688(7) 0.183(7) Uani d P 0.559(18)
F F3 0.7302(9) 0.9507(18) 0.6692(13) 0.203(8) Uani d P 0.559(18)
F F4 0.6351(8) 1.0821(9) 0.6847(6) 0.384(7) Uani d . 1
F F5 0.5853(3) 1.0436(9) 0.5748(5) 0.288(4) Uani d . 1
F F6 0.7016(15) 0.887(2) 0.587(2) 0.326(13) Uani d P 0.559(18)
F F2' 0.6890(14) 1.1222(15) 0.5882(13) 0.180(9) Uani d P 0.441(18)
F F3' 0.7146(12) 1.006(3) 0.7012(8) 0.187(11) Uani d P 0.441(18)
F F6' 0.6389(14) 0.9189(12) 0.5469(6) 0.168(8) Uani d P 0.441(18)
N N1 0.0599(2) 1.1177(3) 0.8125(2) 0.0642(9) Uani d . 1
N N2 -0.0591(2) 0.9896(3) 0.8497(2) 0.0687(10) Uani d . 1
N N3 0.0682(3) 0.8417(4) 0.8050(2) 0.1189(17) Uani d U 1
P P1 0.65715(12) 0.9967(2) 0.62417(10) 0.1139(6) Uani 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 0.0033 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'
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'
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
_geom_angle_publ_flag
N3 Ru1 N3 2_556 . 89.1(3) ?
N3 Ru1 N1 2_556 . 174.27(17) ?
N3 Ru1 N1 . . 92.31(17) y
N3 Ru1 N1 2_556 2_556 92.31(17) ?
N3 Ru1 N1 . 2_556 174.27(17) ?
N1 Ru1 N1 . 2_556 86.83(19) ?
N3 Ru1 N2 2_556 . 95.34(16) ?
N3 Ru1 N2 . . 89.42(15) y
N1 Ru1 N2 . . 79.13(15) y
N1 Ru1 N2 2_556 . 95.98(15) ?
N3 Ru1 N2 2_556 2_556 89.42(15) ?
N3 Ru1 N2 . 2_556 95.34(16) ?
N1 Ru1 N2 . 2_556 95.98(15) ?
N1 Ru1 N2 2_556 2_556 79.13(15) ?
N2 Ru1 N2 . 2_556 173.3(2) ?
N1 C1 C2 . . 120.4(5) ?
N1 C1 C6 . . 115.5(4) ?
C2 C1 C6 . . 124.1(5) ?
C1 C2 C3 . . 119.2(6) ?
C1 C2 H2 . . 120.4 ?
C3 C2 H2 . . 120.4 ?
C4 C3 C2 . . 120.0(6) ?
C4 C3 H3 . . 120.0 ?
C2 C3 H3 . . 120.0 ?
C3 C4 C5 . . 118.2(6) ?
C3 C4 H4 . . 120.9 ?
C5 C4 H4 . . 120.9 ?
N1 C5 C4 . . 123.8(6) ?
N1 C5 H5 . . 118.1 ?
C4 C5 H5 . . 118.1 ?
N2 C6 C7 . . 121.4(5) ?
N2 C6 C1 . . 114.1(4) ?
C7 C6 C1 . . 124.4(5) ?
C8 C7 C6 . . 119.3(5) ?
C8 C7 H7 . . 120.4 ?
C6 C7 H7 . . 120.4 ?
C9 C8 C7 . . 120.0(6) ?
C9 C8 H8 . . 120.0 ?
C7 C8 H8 . . 120.0 ?
C8 C9 C10 . . 118.9(6) ?
C8 C9 H9 . . 120.5 ?
C10 C9 H9 . . 120.5 ?
N2 C10 C9 . . 122.8(5) ?
N2 C10 H10 . . 118.6 ?
C9 C10 H10 . . 118.6 ?
N3 C11 C12 . . 167.6(14) ?
C11 C12 H12A . . 109.0 ?
C11 C12 H12B . . 109.4 ?
H12A C12 H12B . . 109.5 ?
C11 C12 H12C . . 110.0 ?
H12A C12 H12C . . 109.5 ?
H12B C12 H12C . . 109.5 ?
C11 C12 H12E . . 89.0 ?
H12A C12 H12E . . 138.1 ?
H12B C12 H12E . . 98.8 ?
C11 C12 H12F . . 92.2 ?
H12A C12 H12F . . 145.9 ?
H12C C12 H12F . . 86.5 ?
H12E C12 H12F . . 65.8 ?
N3 C11' C12' . . 161.9(19) ?
C11' C12' H12C . . 104.0 ?
C11' C12' H12D . . 113.5 ?
H12C C12' H12D . . 135.4 ?
C11' C12' H12E . . 108.0 ?
H12D C12' H12E . . 109.5 ?
C11' C12' H12F . . 106.9 ?
H12C C12' H12F . . 80.2 ?
H12D C12' H12F . . 109.5 ?
H12E C12' H12F . . 109.5 ?
C5 N1 C1 . . 118.4(4) ?
C5 N1 Ru1 . . 126.7(4) ?
C1 N1 Ru1 . . 114.8(3) ?
C10 N2 C6 . . 117.6(4) ?
C10 N2 Ru1 . . 127.0(3) ?
C6 N2 Ru1 . . 115.4(3) ?
C11' N3 C11 . . 51.6(9) ?
C11' N3 Ru1 . . 147.3(12) ?
C11 N3 Ru1 . . 160.7(9) ?
F4 P1 F2 . . 121.0(11) ?
F4 P1 F3 . . 97.1(10) ?
F2 P1 F3 . . 80.2(10) ?
F4 P1 F1 . . 91.5(6) ?
F2 P1 F1 . . 146.6(10) ?
F3 P1 F1 . . 88.7(6) ?
F4 P1 F5 . . 85.0(6) ?
F2 P1 F5 . . 97.0(6) ?
F3 P1 F5 . . 177.1(9) ?
F1 P1 F5 . . 93.2(3) ?
F4 P1 F6' . . 151.9(10) ?
F2 P1 F6' . . 72.8(13) ?
F3 P1 F6' . . 109.9(15) ?
F1 P1 F6' . . 81.8(6) ?
F5 P1 F6' . . 68.3(8) ?
F4 P1 F3' . . 64.3(9) ?
F2 P1 F3' . . 95.9(8) ?
F1 P1 F3' . . 91.2(7) ?
F5 P1 F3' . . 149.1(12) ?
F6' P1 F3' . . 142.6(15) ?
F4 P1 F6 . . 158.4(15) ?
F2 P1 F6 . . 64.1(9) ?
F3 P1 F6 . . 62.0(18) ?
F1 P1 F6 . . 82.8(9) ?
F5 P1 F6 . . 116.1(15) ?
F6' P1 F6 . . 47.9(10) ?
F3' P1 F6 . . 94.8(19) ?
F4 P1 F2' . . 82.7(11) ?
F3 P1 F2' . . 98.8(9) ?
F1 P1 F2' . . 171.1(11) ?
F5 P1 F2' . . 79.5(7) ?
F6' P1 F2' . . 100.1(11) ?
F3' P1 F2' . . 92.4(9) ?
F6 P1 F2' . . 105.0(12) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ru1 N3 2_556 2.012(4) ?
Ru1 N3 . 2.012(4) y
Ru1 N1 . 2.016(3) y
Ru1 N1 2_556 2.016(3) ?
Ru1 N2 . 2.045(3) y
Ru1 N2 2_556 2.045(3) ?
C1 N1 . 1.358(5) y
C1 C2 . 1.369(6) ?
C1 C6 . 1.455(6) ?
C2 C3 . 1.375(8) ?
C2 H2 . 0.9300 ?
C3 C4 . 1.335(9) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.368(7) ?
C4 H4 . 0.9300 ?
C5 N1 . 1.303(5) y
C5 H5 . 0.9300 ?
C6 N2 . 1.340(5) y
C6 C7 . 1.381(6) ?
C7 C8 . 1.354(7) ?
C7 H7 . 0.9300 ?
C8 C9 . 1.323(8) ?
C8 H8 . 0.9300 ?
C9 C10 . 1.387(7) ?
C9 H9 . 0.9300 ?
C10 N2 . 1.319(6) y
C10 H10 . 0.9300 ?
C11 N3 . 1.251(14) y
C11 C12 . 1.456(13) ?
C12 H12A . 0.9599 ?
C12 H12B . 0.9601 ?
C12 H12C . 0.9600 ?
C11' N3 . 1.200(15) y
C11' C12' . 1.421(15) ?
C12' H12D . 0.9600 ?
C12' H12E . 0.9600 ?
C12' H12F . 0.9601 ?
F1 P1 . 1.490(4) ?
F2 P1 . 1.455(10) ?
F3 P1 . 1.477(12) ?
F4 P1 . 1.432(7) ?
F5 P1 . 1.495(5) ?
F6 P1 . 1.549(17) ?
F2' P1 . 1.571(11) ?
F3' P1 . 1.538(15) ?
F6' P1 . 1.529(10) ?
