#------------------------------------------------------------------------------
#$Date: 2023-12-22 17:07:40 +0200 (Fri, 22 Dec 2023) $
#$Revision: 288505 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/10/50/2105090.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_2105090
loop_
_publ_author_name
'Low, Kian Sing'
'Cole, Jacqueline M.'
'Zhou, Xiaolan'
'Yufa, Nataliya'
_publ_section_title
;
 Rationalizing the molecular origins of Ru- and Fe-based dyes for
 dye-sensitized solar cells
;
_journal_coeditor_code           ZB5022
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              137
_journal_page_last               149
_journal_paper_doi               10.1107/S0108768112009263
_journal_volume                  68
_journal_year                    2012
_chemical_formula_moiety         'C30 H24 N6 Ru Cl2, 6(H2O)'
_chemical_formula_sum            'C30 H36 Cl2 N6 O6 Ru'
_chemical_formula_weight         748.62
_chemical_name_systematic
;
 Tris(2,2?-bipyridyl)dichlororuthenium(II) hexahydrate
;
_space_group_IT_number           192
_space_group_name_Hall           '-P 6 2c'
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6 2c'
_symmetry_space_group_name_H-M   'P 6/m c c'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            4
_cell_length_a                   13.1383(12)
_cell_length_b                   13.1383(12)
_cell_length_c                   20.995(3)
_cell_measurement_reflns_used    3247
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      54.971
_cell_measurement_theta_min      5.280
_cell_volume                     3138.5(6)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'phi or omega oscillation 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  0.0861
_diffrn_reflns_av_sigmaI/netI    0.0461
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            11174
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.66
_exptl_absorpt_coefficient_mu    0.723
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6762
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2008)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.5842
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Chip
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_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.
;
_refine_diff_density_max         0.977
_refine_diff_density_min         -0.561
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     57
_refine_ls_number_reflns         1220
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0769
_refine_ls_R_factor_gt           0.0614
_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)+(0.0767P)²+5.4397P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1439
_refine_ls_wR_factor_ref         0.1529
_reflns_number_gt                994
_reflns_number_total             1220
_reflns_threshold_expression     >2σ(I)
_iucr_refine_instructions_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
;
_cod_data_source_file            zb5022.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '_iucr_refine_instruction_details' was replaced with
'_iucr_refine_instructions_details' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_cell_volume        3138.6(6)
_cod_original_sg_symbol_H-M      P6/mcc
_cod_database_code               2105090
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'
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
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
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'
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
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)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
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)
