##############################################################################
#                                                                            #
# This CIF contains the data in a paper accepted for publication in          #
# Acta Crystallographica Section B. It conforms to the requirements of       #
# Notes for Authors for Acta Crystallographica Section B, and has been       #
# peer reviewed under the auspices of the IUCr Commission on Journals.       #
#                                                                            #
# Full details of the Crystallographic Information File format               #
# are given in the paper "The Crystallographic Information File (CIF):       #
# a New Standard Archive File for Crystallography" by S. R. Hall, F. H.      #
# Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685].                  #
#                                                                            #
# The current version of the core CIF dictionary is obtainable from          #
# ftp://ftp.iucr.org/pub/cif_core.dic.                                       #
#                                                                            #
# Software is freely available for graphical display of the structure(s)     #
# in this CIF. For information consult the CIF software page                 #
# http://www.iucr.org/resources/cif/software.                                #
#                                                                            #
# This file may be used for bona fide research purposes within the           #
# scientific community so long as proper attribution is given to the journal # 
# article from which it was obtained.                                        #
#                                                                            #
##############################################################################
data_I
_audit_creation_method     SHELXL-97
_chemical_name_systematic
;
 Tris(2,2?-bipyridyl)dichlororuthenium(II) hexahydrate
;
_chemical_formula_moiety     'C30 H24 N6 Ru Cl2, 6(H2O)'
_chemical_formula_sum     'C30 H36 Cl2 N6 O6 Ru'
_chemical_formula_weight     748.62
_symmetry_cell_setting     hexagonal
_symmetry_space_group_name_H-M     P6/mcc
_space_group_name_Hall     '-P 6 2c'
loop_
    _symmetry_equiv_pos_as_xyz
    'x, y, z'
    '-x, -y, z'
    '-y, -x, -z+1/2'
    'y, x, -z+1/2'
    'x-y, -y, -z+1/2'
    '-x+y, y, -z+1/2'
    'x, x-y, -z+1/2'
    '-x, -x+y, -z+1/2'
    '-y, x-y, z'
    'y, -x+y, z'
    'x-y, x, z'
    '-x+y, -x, z'
    '-x, -y, -z'
    'x, y, -z'
    'y, x, z-1/2'
    '-y, -x, z-1/2'
    '-x+y, y, z-1/2'
    'x-y, -y, z-1/2'
    '-x, -x+y, z-1/2'
    'x, x-y, z-1/2'
    'y, -x+y, -z'
    '-y, x-y, -z'
    '-x+y, -x, -z'
    'x-y, x, -z'
_cell_length_a     13.1383(12)
_cell_length_b     13.1383(12)
_cell_length_c     20.995(3)
_cell_angle_alpha     90.00
_cell_angle_beta     90.00
_cell_angle_gamma     120.00
_cell_volume     3138.6(6)
_cell_formula_units_Z     4
_cell_measurement_reflns_used     3247
_cell_measurement_theta_min     5.280
_cell_measurement_theta_max     54.971
_cell_measurement_temperature     150(2)
_exptl_crystal_description     Chip
_exptl_crystal_colour     Red
_exptl_crystal_size_max     0.21
_exptl_crystal_size_mid     0.16
_exptl_crystal_size_min     0.12
_exptl_crystal_density_diffrn     1.5842
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     1536
_exptl_absorpt_coefficient_mu     0.723
_exptl_absorpt_correction_type     empirical
_exptl_absorpt_process_details     'CrystalClear (Rigaku Inc., 2008)'
_exptl_absorpt_correction_T_min     0.6762
_exptl_absorpt_correction_T_max     1.0000
_exptl_special_details
;
  ?
;
_diffrn_ambient_temperature     150(2)
_diffrn_radiation_type     MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source     'fine-focus sealed tube'
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device_type     'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method     'phi or omega oscillation scans'
_diffrn_detector_area_resol_mean     10
_diffrn_reflns_number     11174
_diffrn_reflns_av_R_equivalents     0.0861
_diffrn_reflns_av_sigmaI/netI     0.0461
_diffrn_reflns_theta_min     3.66
_diffrn_reflns_theta_max     27.50
_diffrn_reflns_theta_full     27.50
_diffrn_measured_fraction_theta_max     0.973
_diffrn_measured_fraction_theta_full     0.973
_diffrn_reflns_limit_h_min     -7
_diffrn_reflns_limit_h_max     17
_diffrn_reflns_limit_k_min     -17
_diffrn_reflns_limit_k_max     7
_diffrn_reflns_limit_l_min     -24
_diffrn_reflns_limit_l_max     26
_refine_special_details
;
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1 -0.010 -0.009 -0.103       930       363 ' '
   2  0.000  0.500  0.250         7         0 ' '
   3  0.000  0.500  0.750         7         0 ' '
   4  0.500  0.000  0.250         7         0 ' '
   5  0.500  0.000  0.750         7         0 ' '
   6  0.500  0.500  0.250         7         0 ' '
   7  0.500  0.500  0.750         7         0 ' '
;
_reflns_number_total     1220
_reflns_number_gt     994
_reflns_threshold_expression     >2σ(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all     0.0769
_refine_ls_R_factor_gt     0.0614
_refine_ls_wR_factor_gt     0.1439
_refine_ls_wR_factor_ref     0.1529
_refine_ls_goodness_of_fit_ref     1.087
_refine_ls_restrained_S_all     1.087
_refine_ls_number_reflns     1220
_refine_ls_number_parameters     57
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment     constr
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
         'calc w=1/[σ²(Fo²)+(0.0767P)²+5.4397P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens     geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary     difmap
_refine_ls_shift/su_max     0.000
_refine_ls_shift/su_mean     0.000
_refine_diff_density_max     0.977
_refine_diff_density_min     -0.561
_refine_ls_extinction_method     none
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'
    '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'
    'O' 'O' 0.0106 0.0060
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_computing_data_collection     'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement     'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction     'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement     'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics     'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
                                   'WinGX publication routines (Farrugia, 1999)'
_iucr_refine_instruction_details
;
TITL Ru-hexahy4-17-5-10-150k-Dstar2 in P 6/m c c
CELL  0.71073  13.1383  13.1383  20.9955   90.000   90.000  120.000
ZERR     4.00   0.0012   0.0012   0.0028    0.000    0.000    0.000
LATT   1
SYMM  - X, - Y,   Z
SYMM  - Y, - X, 1/2 - Z
SYMM    Y,   X, 1/2 - Z
SYMM    X - Y, - Y, 1/2 - Z
SYMM  - X + Y,   Y, 1/2 - Z
SYMM    X,   X - Y, 1/2 - Z
SYMM  - X, - X + Y, 1/2 - Z
SYMM  - Y,   X - Y,   Z
SYMM    Y, - X + Y,   Z
SYMM    X - Y,   X,   Z
SYMM  - X + Y, - X,   Z
SFAC  C    H    N    RU  Cl  O
UNIT  120  144   24   4   8   24
MERG   2
OMIT     0   1   2
OMIT     0   1   0
OMIT    -1   8   1
OMIT     0   0   4
OMIT     0   0   6
OMIT    -1   2   0
OMIT     0   2   0
OMIT    -2  10   1
OMIT    -3   9   1
OMIT    -1  10   2
OMIT     0   1  10
OMIT    -2  10   3
OMIT    -1  11   5
OMIT    -1   3   7
OMIT     0   0   8
OMIT    -1   3   0
OMIT     0   0  10
OMIT     0   2   6
OMIT     0   1   4
OMIT    -1   3   2
OMIT    -1   3   5
OMIT    -1   3   4
OMIT     0   4   4
OMIT     0   4   2
OMIT     0   5   6
OMIT    -1   3  11
OMIT    -2   5   9
OMIT    -2   5  13
OMIT    -2   8   9
OMIT    -2   8   1
FMAP   2
PLAN   20
ACTA
BOND   $H
L.S.   8
REM WGHT    0.200000
REM WGHT    0.084400    5.034300
WGHT    0.076700    5.439700
FVAR      17.17370
N1    3    0.681084    0.207661    0.198021    11.00000    0.02762    0.02392 =
         0.03553   -0.00011    0.00383    0.01242
C1    1    0.761816    0.179982    0.220536    11.00000    0.02836    0.02303 =
         0.03543    0.00370    0.00486    0.01339
C2    1    0.786076    0.102876    0.187185    11.00000    0.03681    0.02956 =
         0.04920   -0.00107    0.00221    0.01951
AFIX  43
H2    2    0.840926    0.084298    0.202990    11.00000   -1.20000
AFIX   0
C5    1    0.627147    0.159671    0.142553    11.00000    0.03035    0.03023 =
         0.03244   -0.00138    0.00091    0.01301
AFIX  43
H5    2    0.572167    0.178335    0.127057    11.00000   -1.20000
AFIX   0
C3    1    0.728782    0.054223    0.130820    11.00000    0.04242    0.02706 =
         0.04461    0.00016    0.00992    0.01958
AFIX  43
H3    2    0.743601    0.001656    0.108708    11.00000   -1.20000
AFIX   0
C4    1    0.649447    0.084124    0.107553    11.00000    0.03589    0.02529 =
         0.04559   -0.00210    0.00126    0.01217
AFIX  43
H4    2    0.611525    0.053986    0.068942    11.00000   -1.20000
AFIX   0
RU1   4    0.666667    0.333333    0.250000    10.16667    0.02115    0.02115 =
         0.03069    0.00000    0.00000    0.01058
HKLF    4
REM  Ru-hexahy4-17-5-10-150k-Dstar2 in P 6/m c c
REM R1 =  0.0614 for    994 Fo > 4sig(Fo)  and  0.0769 for all   1220 data
REM     57 parameters refined using      0 restraints
END
WGHT      0.0756      5.6218
REM Highest difference peak  0.977,  deepest hole -0.561,  1-sigma level  0.108
Q1    1   0.6667  0.3333  0.2024  10.33333  0.05    0.98
Q2    1   1.0000  0.0000  0.2500  10.08333  0.05    0.77
Q3    1   0.6667  0.3333  0.1557  10.33333  0.05    0.54
Q4    1   0.5413 -0.0994  0.0000  10.50000  0.05    0.48
Q5    1   0.8472 -0.0169  0.0000  10.50000  0.05    0.46
Q6    1   0.5184  0.1414  0.0000  10.50000  0.05    0.41
Q7    1   1.0000  0.0000  0.0000  10.08333  0.05    0.33
Q8    1   0.8733  0.0177  0.2012  11.00000  0.05    0.32
Q9    1   0.6667  0.3333  0.0000  10.16667  0.05    0.32
Q10   1   0.7696  0.1381  0.1885  11.00000  0.05    0.32
Q11   1   0.7420  0.0624  0.1704  11.00000  0.05    0.31
Q12   1   0.6345  0.2690  0.2500  10.50000  0.05    0.31
Q13   1   0.7002  0.4005  0.2500  10.50000  0.05    0.31
Q14   1   0.6537  0.1859  0.1962  11.00000  0.05    0.31
Q15   1   0.5975 -0.0256  0.0614  11.00000  0.05    0.31
Q16   1   0.7771  0.0942  0.2486  11.00000  0.05    0.30
Q17   1   0.6694  0.1866  0.1696  11.00000  0.05    0.29
Q18   1   0.7222  0.1911  0.1812  11.00000  0.05    0.29
Q19   1   0.9555  0.0382  0.0444  11.00000  0.05    0.29
Q20   1   0.6596  0.0565  0.1455  11.00000  0.05    0.28
;
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
    N N1 0.6811(3) 0.2077(3) 0.19802(16) 0.0292(8) Uani d . 1 1 . .
    C C1 0.7618(3) 0.1800(3) 0.2205(2) 0.0287(8) Uani d . 1 1 . .
    C C2 0.7861(4) 0.1029(4) 0.1872(2) 0.0372(10) Uani d . 1 1 . .
    H H2 0.8409 0.0843 0.2030 0.045 Uiso calc R 1 1 . .
    C C5 0.6271(4) 0.1597(4) 0.1426(2) 0.0320(9) Uani d . 1 1 . .
    H H5 0.5722 0.1783 0.1271 0.038 Uiso calc R 1 1 . .
    C C3 0.7288(4) 0.0542(4) 0.1308(2) 0.0370(10) Uani d . 1 1 . .
    H H3 0.7436 0.0017 0.1087 0.044 Uiso calc R 1 1 . .
    C C4 0.6494(4) 0.0841(4) 0.1076(2) 0.0370(10) Uani d . 1 1 . .
    H H4 0.6115 0.0540 0.0689 0.044 Uiso calc R 1 1 . .
    Ru Ru1 0.6667 0.3333 0.2500 0.0243(3) Uani d S 1 6 . .
loop_
    _atom_site_aniso_label
    _atom_site_aniso_U_11
    _atom_site_aniso_U_22
    _atom_site_aniso_U_33
    _atom_site_aniso_U_12
    _atom_site_aniso_U_13
    _atom_site_aniso_U_23
    N1 0.0276(17) 0.0239(16) 0.0355(19) 0.0124(14) 0.0038(14) -0.0001(14)
    C1 0.0284(19) 0.0230(17) 0.035(2) 0.0134(15) 0.0049(16) 0.0037(15)
    C2 0.037(2) 0.030(2) 0.049(3) 0.020(2) 0.002(2) -0.0011(19)
    C5 0.030(2) 0.030(2) 0.032(2) 0.0130(18) 0.0009(17) -0.0014(16)
    C3 0.042(2) 0.027(2) 0.045(2) 0.020(2) 0.010(2) 0.0002(19)
    C4 0.036(2) 0.0253(19) 0.046(3) 0.0122(17) 0.0013(19) -0.0021(18)
    Ru1 0.0212(3) 0.0212(3) 0.0307(5) 0.01058(15) 0.000 0.000
_geom_special_details
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;
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
    N1 C5 . 1.345(5) ?
    N1 C1 . 1.366(5) ?
    N1 Ru1 . 2.065(3) ?
    C1 C2 . 1.393(6) ?
    C1 C1 3_665 1.454(9) ?
    C2 C3 . 1.376(7) ?
    C2 H2 . 0.9300 ?
    C5 C4 . 1.379(6) ?
    C5 H5 . 0.9300 ?
    C3 C4 . 1.374(6) ?
    C3 H3 . 0.9300 ?
    C4 H4 . 0.9300 ?
    Ru1 N1 3_665 2.065(3) ?
    Ru1 N1 9_655 2.065(3) ?
    Ru1 N1 6_655 2.065(3) ?
    Ru1 N1 12_665 2.065(3) ?
    Ru1 N1 7 2.065(3) ?
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
    C5 N1 C1 . . 118.2(3) ?
    C5 N1 Ru1 . . 126.5(3) ?
    C1 N1 Ru1 . . 115.1(3) ?
    N1 C1 C2 . . 120.7(4) ?
    N1 C1 C1 . 3_665 115.4(2) ?
    C2 C1 C1 . 3_665 124.0(3) ?
    C3 C2 C1 . . 119.9(4) ?
    C3 C2 H2 . . 120.0 ?
    C1 C2 H2 . . 120.0 ?
    N1 C5 C4 . . 123.2(4) ?
    N1 C5 H5 . . 118.4 ?
    C4 C5 H5 . . 118.4 ?
    C4 C3 C2 . . 119.3(4) ?
    C4 C3 H3 . . 120.3 ?
    C2 C3 H3 . . 120.3 ?
    C3 C4 C5 . . 118.7(4) ?
    C3 C4 H4 . . 120.6 ?
    C5 C4 H4 . . 120.6 ?
    N1 Ru1 N1 . 3_665 78.98(19) ?
    N1 Ru1 N1 . 9_655 94.66(13) ?
    N1 Ru1 N1 3_665 9_655 92.37(18) ?
    N1 Ru1 N1 . 6_655 92.37(18) ?
    N1 Ru1 N1 3_665 6_655 94.66(13) ?
    N1 Ru1 N1 9_655 6_655 170.89(18) ?
    N1 Ru1 N1 . 12_665 94.66(13) ?
    N1 Ru1 N1 3_665 12_665 170.89(18) ?
    N1 Ru1 N1 9_655 12_665 94.66(13) ?
    N1 Ru1 N1 6_655 12_665 78.98(19) ?
    N1 Ru1 N1 . 7 170.89(18) ?
    N1 Ru1 N1 3_665 7 94.66(13) ?
    N1 Ru1 N1 9_655 7 78.98(19) ?
    N1 Ru1 N1 6_655 7 94.66(13) ?
    N1 Ru1 N1 12_665 7 92.37(18) ?
_platon_squeeze_details
;
 The unit cell contains 6 water molecules and 2 chlorine ions which have been
 treated as a diffuse contribution to the overall scattering without specific
 atom positions by SQUEEZE/PLATON.
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
data_II
_audit_creation_method     SHELXL-97
_chemical_name_systematic
;
 tris(2,2'-bipyridyl) iron(II) dithiocyanate
;
_chemical_name_common     ?
_chemical_formula_moiety     'C30 H24 Fe N6, 2(NCS)'
_chemical_formula_sum     'C32 H24 Fe N8 S2'
_chemical_formula_weight     642.28
_chemical_melting_point     ?
_symmetry_cell_setting     hexagonal
_symmetry_space_group_name_H-M     P6/mcc
_space_group_name_Hall     '-P 6 2c'
loop_
    _symmetry_equiv_pos_as_xyz
    'x, y, z'
    'x-y, x, z'
    '-y, x-y, z'
    '-x, -y, z'
    '-x+y, -x, z'
    'y, -x+y, z'
    '-y, -x, -z+1/2'
    'x-y, -y, -z+1/2'
    'x, x-y, -z+1/2'
    'y, x, -z+1/2'
    '-x+y, y, -z+1/2'
    '-x, -x+y, -z+1/2'
    '-x, -y, -z'
    '-x+y, -x, -z'
    'y, -x+y, -z'
    'x, y, -z'
    'x-y, x, -z'
    '-y, x-y, -z'
    'y, x, z-1/2'
    '-x+y, y, z-1/2'
    '-x, -x+y, z-1/2'
    '-y, -x, z-1/2'
    'x-y, -y, z-1/2'
    'x, x-y, z-1/2'
_cell_length_a     13.1837(9)
_cell_length_b     13.1837(9)
_cell_length_c     21.2735(14)
_cell_angle_alpha     90.00
_cell_angle_beta     90.00
_cell_angle_gamma     120.00
_cell_volume     3202.2(4)
_cell_formula_units_Z     4
_cell_measurement_reflns_used     3247
_cell_measurement_theta_min     5.280
_cell_measurement_theta_max     54.971
_cell_measurement_temperature     150(2)
_exptl_crystal_description     Chip
_exptl_crystal_colour     Red
_exptl_crystal_size_max     0.18
_exptl_crystal_size_mid     0.12
_exptl_crystal_size_min     0.10
_exptl_crystal_density_diffrn     1.213
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     1216
_exptl_absorpt_coefficient_mu     0.200
_exptl_absorpt_correction_type     empirical
_exptl_absorpt_process_details     'CrystalClear (Rigaku Inc., 2008)'
_exptl_absorpt_correction_T_min     0.8573
_exptl_absorpt_correction_T_max     1.0000
_exptl_special_details
;
  ?
;
_diffrn_ambient_temperature     150(2)
_diffrn_radiation_type     MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_source     'fine-focus sealed tube'
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device_type     'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method     'phi or omega oscillation scans'
_diffrn_detector_area_resol_mean     10
_diffrn_reflns_number     26491
_diffrn_reflns_av_R_equivalents     0.0434
_diffrn_reflns_av_sigmaI/netI     0.0275
_diffrn_reflns_theta_min     3.57
_diffrn_reflns_theta_max     27.48
_diffrn_reflns_theta_full     27.48
_diffrn_measured_fraction_theta_max     0.987
_diffrn_measured_fraction_theta_full     0.987
_diffrn_reflns_limit_h_min     -17
_diffrn_reflns_limit_h_max     17
_diffrn_reflns_limit_k_min     -16
_diffrn_reflns_limit_k_max     17
_diffrn_reflns_limit_l_min     -27
_diffrn_reflns_limit_l_max     25
_refine_special_details
;
;
_reflns_number_total     1259
_reflns_number_gt     1165
_reflns_threshold_expression     >2σ(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all     0.0541
_refine_ls_R_factor_gt     0.0487
_refine_ls_wR_factor_gt     0.1118
_refine_ls_wR_factor_ref     0.1145
_refine_ls_goodness_of_fit_ref     1.134
_refine_ls_restrained_S_all     1.134
_refine_ls_number_reflns     1259
_refine_ls_number_parameters     57
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment     constr
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
         'calc w=1/[σ²(Fo²)+(0.0452P)²+3.3496P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens     geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary     difmap
_refine_ls_shift/su_max     0.000
_refine_ls_shift/su_mean     0.000
_refine_diff_density_max     0.323
_refine_diff_density_min     -0.270
_refine_ls_extinction_method     none
_refine_ls_extinction_coef     ?
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'
    'S' 'S' 0.1246 0.1234
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'Fe' 'Fe' 0.3463 0.8444
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_computing_data_collection     'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement     'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction     'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution
;
 SIR92 (Altomare et al., J. Appl. Cryst. (1994). 27, 435)
;
_computing_structure_refinement     'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics     'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
                                   'WinGX publication routines (Farrugia, 1999)'
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
    N N1 0.67794(13) 0.21313(14) 0.19921(8) 0.0230(4) Uani d . 1 1 . .
    C C4 0.78247(19) 0.10828(18) 0.18768(11) 0.0320(5) Uani d . 1 1 . .
    H H4A 0.8363 0.0889 0.2035 0.038 Uiso calc R 1 1 . .
    C C5 0.75801(15) 0.18462(15) 0.22066(10) 0.0235(4) Uani d . 1 1 . .
    C C1 0.62321(18) 0.16518(17) 0.14468(10) 0.0282(4) Uani d . 1 1 . .
    H H1A 0.5676 0.1831 0.1300 0.034 Uiso calc R 1 1 . .
    C C3 0.7263(2) 0.06123(18) 0.13113(11) 0.0351(5) Uani d . 1 1 . .
    H H3A 0.7426 0.0109 0.1083 0.042 Uiso calc R 1 1 . .
    C C2 0.64568(19) 0.09035(18) 0.10931(11) 0.0330(5) Uani d . 1 1 . .
    H H2A 0.6070 0.0602 0.0714 0.040 Uiso calc R 1 1 . .
    Fe Fe 0.6667 0.3333 0.2500 0.0189(2) Uani d S 1 6 . .
loop_
    _atom_site_aniso_label
    _atom_site_aniso_U_11
    _atom_site_aniso_U_22
    _atom_site_aniso_U_33
    _atom_site_aniso_U_12
    _atom_site_aniso_U_13
    _atom_site_aniso_U_23
    N1 0.0212(8) 0.0185(7) 0.0269(8) 0.0080(6) 0.0015(6) 0.0005(6)
    C4 0.0328(11) 0.0257(10) 0.0409(12) 0.0172(9) 0.0057(9) 0.0022(9)
    C5 0.0208(8) 0.0183(8) 0.0317(10) 0.0101(7) 0.0039(7) 0.0028(7)
    C1 0.0277(10) 0.0244(9) 0.0301(11) 0.0112(8) -0.0026(8) -0.0038(8)
    C3 0.0434(12) 0.0234(10) 0.0391(12) 0.0170(10) 0.0108(10) -0.0029(8)
    C2 0.0338(11) 0.0256(10) 0.0332(11) 0.0101(9) 0.0010(9) -0.0061(8)
    Fe 0.0170(2) 0.0170(2) 0.0229(3) 0.00848(12) 0.000 0.000
_geom_special_details
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;
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
    N1 C1 . 1.345(3) ?
    N1 C5 . 1.364(2) ?
    N1 Fe . 1.9841(16) ?
    C4 C3 . 1.386(3) ?
    C4 C5 . 1.391(3) ?
    C4 H4A . 0.9300 ?
    C5 C5 7_665 1.460(4) ?
    C1 C2 . 1.386(3) ?
    C1 H1A . 0.9300 ?
    C3 C2 . 1.378(3) ?
    C3 H3A . 0.9300 ?
    C2 H2A . 0.9300 ?
    Fe N1 7_665 1.9841(16) ?
    Fe N1 11_655 1.9841(16) ?
    Fe N1 3_655 1.9841(16) ?
    Fe N1 9 1.9841(16) ?
    Fe N1 5_665 1.9841(16) ?
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
    C1 N1 C5 . . 117.79(17) ?
    C1 N1 Fe . . 127.46(13) ?
    C5 N1 Fe . . 114.53(13) ?
    C3 C4 C5 . . 119.7(2) ?
    C3 C4 H4A . . 120.1 ?
    C5 C4 H4A . . 120.1 ?
    N1 C5 C4 . . 121.47(19) ?
    N1 C5 C5 . 7_665 114.54(11) ?
    C4 C5 C5 . 7_665 123.98(13) ?
    N1 C1 C2 . . 123.20(19) ?
    N1 C1 H1A . . 118.4 ?
    C2 C1 H1A . . 118.4 ?
    C2 C3 C4 . . 118.81(19) ?
    C2 C3 H3A . . 120.6 ?
    C4 C3 H3A . . 120.6 ?
    C3 C2 C1 . . 119.0(2) ?
    C3 C2 H2A . . 120.5 ?
    C1 C2 H2A . . 120.5 ?
    N1 Fe N1 7_665 . 81.67(9) ?
    N1 Fe N1 7_665 11_655 93.16(6) ?
    N1 Fe N1 . 11_655 92.47(9) ?
    N1 Fe N1 7_665 3_655 92.47(9) ?
    N1 Fe N1 . 3_655 93.16(6) ?
    N1 Fe N1 11_655 3_655 172.56(9) ?
    N1 Fe N1 7_665 9 93.16(6) ?
    N1 Fe N1 . 9 172.56(9) ?
    N1 Fe N1 11_655 9 93.16(6) ?
    N1 Fe N1 3_655 9 81.67(9) ?
    N1 Fe N1 7_665 5_665 172.56(9) ?
    N1 Fe N1 . 5_665 93.16(6) ?
    N1 Fe N1 11_655 5_665 81.67(9) ?
    N1 Fe N1 3_655 5_665 93.16(6) ?
    N1 Fe N1 9 5_665 92.47(9) ?
loop_
    _platon_squeeze_void_nr
    _platon_squeeze_void_average_x
    _platon_squeeze_void_average_y
    _platon_squeeze_void_average_z
    _platon_squeeze_void_volume
    _platon_squeeze_void_count_electrons
    _platon_squeeze_void_content
    1 -0.009 -0.008 -0.072 1005 285 ' '
    2 0.000 0.500 0.250 7 1 ' '
    3 0.000 0.500 0.750 7 1 ' '
    4 0.500 0.000 0.250 7 1 ' '
    5 0.500 0.000 0.750 7 1 ' '
    6 0.500 0.500 0.250 7 1 ' '
    7 0.500 0.500 0.750 7 1 ' '
_platon_squeeze_details
;
 The unit cell contains 2 NCS counterions and 3 acetonitirile molecules
 which have been treated as a diffuse contribution to the overall
 scattering without specific atom positions by SQUEEZE/PLATON.
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
data_global
_journal_data_validation_number     ?
_journal_date_recd_electronic     2011-10-06
_journal_date_accepted     2012-03-01
_journal_name_full     'Acta Crystallographica, Section B'
_journal_year     2012
_journal_volume     68
_journal_issue      2
_journal_page_first     137
_journal_page_last     149
_journal_paper_category     FA
_journal_paper_doi     10.1107/S0108768112009263
_journal_coeditor_code     ZB5022
_publ_contact_author_name     'Jacqueline M. Cole'
_publ_contact_author_address
;
Department of Physics, University of Cambridge,
Cavendish Laboratory, J J Thompson Ave, Cambridge CB3 0HE
;
_publ_contact_author_email     'jmc61@cam.ac.uk'
_publ_section_title
;
Molecular Origins of Dyes for Dye Sensitized Solar Cells
;
loop_
    _publ_author_name
    _publ_author_address
    'Low, Kian Sing '
;
Department of Physics, University of Cambridge,
Cavendish Laboratory, J J Thompson Ave, Cambridge CB3 0HE
;
    'Cole, Jacqueline M. '
;
Department of Physics, University of Cambridge,
Cavendish Laboratory, J J Thompson Ave, Cambridge CB3 0HE
and
Departments of Chemistry and Physics, University of New Brunswick,
P. O. Box 4400, Fredericton, New Brunswick E3B5A3, Canada
;
    'Zhou, Xiaolan'
;
Department of Physics, University of Cambridge,
Cavendish Laboratory, J J Thompson Ave, Cambridge CB3 0HE
;
    'Yufa, Nataliya'
;
Department of Physics, University of Cambridge,
Cavendish Laboratory, J J Thompson Ave, Cambridge CB3 0HE
;
