# Electronic Supplementary Material (ESI) for New Journal of Chemistry
# This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2011
data_General
_journal_name_full 'New J.Chem.'
_journal_coden_cambridge 0440
#TrackingRef '- wt2105w-shelxl.cif'
_audit_creation_date 2011-May-20
_audit_creation_method SHELXL97
_audit_update_record
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2011-May-20 # Formatted by publCIF
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#==============================================================================
# PROCESSING SUMMARY (IUCr Office Use Only)
_journal_date_recd_electronic ?
_journal_date_from_coeditor ?
_journal_date_accepted ?
_journal_coeditor_code ?
#==============================================================================
# SUBMISSION DETAILS
_publ_contact_author_name 'Professor V.W.W. YAM'
_publ_contact_author_email wwyam@hku.hk
_publ_contact_author_fax '(852)2915 5176'
_publ_contact_author_phone '(852)2859 2153'
_publ_contact_author_address
;
Department of Chemistry
The University of Hong Kong
Pokfulam Road, Pokfulam,
Hong Kong SAR,
P. R. CHINA
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_publ_contact_letter
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ENTER TEXT OF LETTER
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_publ_requested_category ? #'CHOOSE FI FM FO CI CM CO or AD'
_publ_requested_coeditor_name ?
#==============================================================================
# TITLE AND AUTHOR LIST
_publ_section_title
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Directory Reference: COM648 wt2105w YAM-Duan Gong Ping's YAM-DGP100617--2
18--6--2010
;
_publ_section_title_footnote .
loop_
_publ_author_name
_publ_author_footnote
_publ_author_address
'Gong Ping Duan' .
;
Department of Chemistry
The University of Hong Kong
Pokfulam Road, Pokfulam,
Hong Kong SAR,
P. R. CHINA
;
'Vivian Wing-Wah Yam' .
;
Department of Chemistry
The University of Hong Kong
Pokfulam Road, Pokfulam,
Hong Kong SAR,
P. R. CHINA
;
_publ_section_synopsis .
#==============================================================================
# TEXT
_publ_section_abstract
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(type here to add abstract)
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_publ_section_comment
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The complex is consisted of a Ru bonded to a 2-[4,5-bis-(2,5-dimethyl-
thiophen-3-yl)-3-methyl-2,3-dihydro-imidazol-1-yl]-4,5-dimethyl-oxazole ligand
(TIO), a mesitylene, a chloride and a hexafluoro phosphate ion. There is a
total of 881.3 \%A^3^ (11.0% per unit cell volume) of potential solvent area
volumes. There are four big void areas in the unit cell, each occupies about
220 \%A^3^, centred at the special positions, i.e. (1/2, 0, 0), (1, 0,
1/2), (1, 1/2, 0) and (1/2, 1/2, 1/2). H-bond and \p...\p interactions also
observed in the lattice. unfortunately, only two locations of water molecules
could be confirmed, and the occupancies of the water molecules are refined.
There are residual electron densities close to water molecules O3, which
indicated that the water molecules are heavily disordered.
;
_publ_section_references
;
Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M. C.,
Polidori, G. & Camalli, M. (1994). SIR92 - Aprogram for automatic
solution of crystal structures by direct methods. J. Appl. Cryst. 27, 435.
Bruker AXS Inc. (1998). SMART, version 5.059, Madison, Wisconsin, USA.
Bruker AXS Inc. (2006). SAINT, version 7.34A, Madison, Wisconsin, USA.
Johnson, C. K. (1976). ORTEPII, A FORTRAN Thermal-Ellipsoid Plot
Program, Report ORNL-5138, Oak Ridge National Laboratory, Oak Ridge,
Tennessee, USA.
Macrae, C. F., Bruno, I. J., Chisholm, J. A., Edgington, P. R., McCabe, P.,
Pidcock, E., Rodriguez-Monge, L., Taylor, R., van de Streek, J. & Wood, P. A.
(2008). Mercury J. Appl. Cryst, 41, 466--470.
Rigaku/MSC and Rigaku Corporation. (2006). CrystalStructure. Single
Crystal Structure Analysis Software. Version 3.8.1. Rigaku/MSC, 9009 New
Trails Drive, The Woodlands, TX, USA 77381-5209. Rigaku, 3-9-12 Akishima,
Tokyo 196-8666, Japan.
Sheldrick, G. M. (1996). SADABS, G\"ottingen University, G\"ottingen,
Germany.
Sheldrick, G. M. (2008). SHELX programs:SHELXL97. Acta
Cryst. E68, 112-122.
;
_publ_section_acknowledgements
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(type here to add acknowledgements)
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_publ_section_figure_captions
;
Fig. 1. The ORTEP plot of the compound was shown at 30% probability
thermal ellipsoids with the atom numbering scheme.
;
_publ_section_exptl_prep
;
An orange block crystal of, C~30~H~37~ClF~6~N~3~O~2~PRuS~2~, having approximate
dimensions of 0.14 x 0.15 x 0.49 mm was mounted in glass
capillary. All measurements were made on a Bruker SMART 1000 CCD
detector with graphite monochromated Mo---K\a radiation.
Indexing was performed from 60 images that were exposed for 10 s for a
preliminary unit cell determination. Of which, 70 out of total of 72
reflections were successfully indexed. The crystal-to-detector distance was
50.00 mm.
Cell constants and an orientation matrix for data collection corresponded to a
primitive orthorhombic cell with dimensions: a = 17.267(3)\%A,
b = 14.598(2)\%A, c = 31.643(5)\%A, V = 7976(2)\%A^3^.
For Z = 8 and F.W. = 817.24, the calculated density is 1.361 g/cm^3^.
Based on a statistical analysis of intensity distribution, and the successful
solution and refinement of the structure, the space group was determined to
be: P bca (#61)
The data were collected at a temperature of 32(1)\%C to a maximum 2\q value of
54.96\%. A total of 1491 oscillation images were collected in 4 runs. A sweep
of data was done using \w scans from 330.0 to 148.2\% in -0.3\% step, at
\c=54.7\% and \f = 0.0\%. The exposure rate was 40.0 [sec./\%]. The detector
swing angle was -30.00\%. A second sweep was performed using \w scans from
330.0 to 199.5\% in -0.3\% step, at \c=54.7\% and \f = 90.0\%. The exposure
rate was 40.0 [sec./\%]. The detector swing angle was -30.00\%. Another sweep
was performed using \w scans from 330.0 to 255\% in -0.3\% step, at \c=54.7\%
and \f = 180.0\%. The exposure rate was 40.0 [sec./\%]. The detector swing
angle was -30.00\%. A last sweep was performed using \w scans from 330.0 to
270\% in -0.3\% step, at \c=54.7\% and \f = 90.0\%. The exposure rate was 40.0
[sec./\%].The crystal-to-detector distance was 50.00 mm.
Of the 44176 reflections that was collected, 7543 reflections were unique.
(R~int~ = 0.0868); equivalent reflections were merged.
;
_publ_section_exptl_refinement
;
The structure was solved by Direct methods (SIR92, Altomare et
al., 1994) and expanded using Fourier techniques. Most non-H atoms were
refined anisotropically, except atoms O2 and O3 which are disordered, they
were refined isotropically only.
All of the C-bound H atoms were observable from difference Fourier map but were
all placed at geometrical positions with C---H = 0.93 and 0.96\%A for phenyl
and methyl H-atoms. All H-atoms were refined using riding model with
U~iso~(H) = 1.2U~eq~(Carrier). The occupancies of O2 and O3 were
refined with restraint of summation to unity. 18 restraints were used in the
refinement. They are related to the refinement of three fluorine atoms, F1, F2
and F3, using isotropic restraints of standard deviation of 0.005 for F1, F2
and F3, in the anisotropic atom displacement components (six restraints for
each fluorine atoms).
Highest peak is 1.13 at (0.1458, 0.9164, 0.4956) [0.14\%A from H3A] Deepest
hole is -2.26 at (0.1473, 0.7953, 0.2887) [1.41\%A from H7A]
;
#============================================================================
data_wt2105w-shelxl
_database_code_depnum_ccdc_archive 'CCDC 814059'
#TrackingRef '- wt2105w-shelxl.cif'
#wt2105w-YAM-Duan Gong Ping's DGP100617-2_18-June-2010
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C30 H35 Cl N3 O Ru S2, F6 P, H2 O'
_chemical_formula_sum 'C30 H37 Cl F6 N3 O2 P Ru S2'
_chemical_formula_weight 817.24
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'
O O 0.0106 0.0060 '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'
P P 0.1023 0.0942 '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'
F F 0.0171 0.0103 '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'
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_H-M 'P b c a'
_symmetry_space_group_name_Hall '-P 2ac 2ab'
_symmetry_Int_Tables_number 61
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, z'
'x, -y+1/2, z+1/2'
'-x+1/2, -y, z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, -z'
'-x, y-1/2, -z-1/2'
'x-1/2, y, -z-1/2'
_cell_length_a 17.267(3)
_cell_length_b 14.598(2)
_cell_length_c 31.643(5)
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_volume 7976(2)
_cell_formula_units_Z 8
_cell_measurement_temperature 305(2)
_cell_measurement_reflns_used 44176
_cell_measurement_theta_min 1.86
_cell_measurement_theta_max 25.68
_exptl_crystal_description block
_exptl_crystal_colour brown
_exptl_crystal_size_max 0.49
_exptl_crystal_size_mid 0.15
_exptl_crystal_size_min 0.14
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.361
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 3328
_exptl_absorpt_coefficient_mu 0.661
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.7376
_exptl_absorpt_correction_T_max 0.9131
_exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 305(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker SMART 1000 CCD'
_diffrn_measurement_method \w
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number 0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time .
_diffrn_standards_decay_% ?
_diffrn_reflns_number 44148
_diffrn_reflns_av_R_equivalents 0.0868
_diffrn_reflns_av_sigmaI/netI 0.0621
_diffrn_reflns_limit_h_min -21
_diffrn_reflns_limit_h_max 20
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_l_min -37
_diffrn_reflns_limit_l_max 38
_diffrn_reflns_theta_min 1.75
_diffrn_reflns_theta_max 25.68
_reflns_number_total 7538
_reflns_number_gt 4642
_reflns_threshold_expression I>2\s(I)
_computing_data_collection 'SMART (Bruker AXS Inc, 1998)'
_computing_cell_refinement 'SAINT v7.34A (Bruker AXS Inc, 2006)'
_computing_data_reduction
'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2006)'
_computing_structure_solution 'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics
'ORTEP-II (Johnson, 1976) & MERCURY (Macrae et al., 2008)'
_computing_publication_material 'SHELXL97 (Sheldrick, 2008)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0878P)^2^+74.6933P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 7538
_refine_ls_number_parameters 425
_refine_ls_number_restraints 18
_refine_ls_R_factor_all 0.1467
_refine_ls_R_factor_gt 0.0994
_refine_ls_wR_factor_ref 0.2715
_refine_ls_wR_factor_gt 0.2443
_refine_ls_goodness_of_fit_ref 1.135
_refine_ls_restrained_S_all 1.147
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.64723(4) 0.40234(5) 0.21238(3) 0.0425(3) Uani 1 1 d . . .
Cl1 Cl 0.76953(16) 0.4556(2) 0.18524(11) 0.0710(9) Uani 1 1 d . . .
S1 S 0.4073(2) 0.8431(2) 0.12463(12) 0.0763(10) Uani 1 1 d . . .
S2 S 0.3931(3) 0.5467(3) 0.01506(13) 0.0938(13) Uani 1 1 d . . .
P1 P 0.39624(19) 0.2088(2) 0.15561(12) 0.0672(9) Uani 1 1 d . . .
F1 F 0.4336(6) 0.3040(6) 0.1672(3) 0.120(3) Uani 1 1 d U . .
F2 F 0.3461(7) 0.2034(9) 0.1954(4) 0.147(4) Uani 1 1 d U . .
F3 F 0.3283(5) 0.2616(6) 0.1324(3) 0.105(3) Uani 1 1 d U . .
F4 F 0.3628(6) 0.1140(6) 0.1423(4) 0.133(4) Uani 1 1 d . . .
F5 F 0.4449(7) 0.2118(9) 0.1144(4) 0.150(4) Uani 1 1 d . . .
F6 F 0.4631(5) 0.1570(5) 0.1813(3) 0.102(3) Uani 1 1 d . . .
O1 O 0.5713(4) 0.3516(5) 0.0903(2) 0.0584(19) Uani 1 1 d . . .
O2 O 0.7138(12) 0.5101(14) 0.0862(6) 0.108(8) Uiso 0.55(2) 1 d P . .
H2A H 0.7491 0.4818 0.0726 0.130 Uiso 0.55 1 d P . .
H2B H 0.6948 0.5047 0.1096 0.130 Uiso 0.55 1 d P . .
O3 O 0.8289(15) 0.4647(19) 0.0235(8) 0.111(10) Uiso 0.45(2) 1 d P . .
H3A H 0.8478 0.4193 0.0065 0.133 Uiso 0.45 1 d P . .
H3B H 0.8559 0.5050 0.0271 0.133 Uiso 0.45 1 d P . .
N1 N 0.6304(5) 0.3411(5) 0.1519(3) 0.050(2) Uani 1 1 d . . .
N2 N 0.5568(5) 0.4703(5) 0.1418(3) 0.047(2) Uani 1 1 d . . .
N3 N 0.5752(5) 0.5892(5) 0.1793(3) 0.049(2) Uani 1 1 d . . .
C1 C 0.7176(8) 0.2017(8) 0.1399(5) 0.087(4) Uani 1 1 d . . .
H1A H 0.7584 0.2348 0.1538 0.104 Uiso 1 1 calc R . .
H1B H 0.7379 0.1711 0.1155 0.104 Uiso 1 1 calc R . .
H1C H 0.6963 0.1573 0.1590 0.104 Uiso 1 1 calc R . .
C2 C 0.6551(7) 0.2675(6) 0.1266(4) 0.057(3) Uani 1 1 d . . .
C3 C 0.6190(7) 0.2717(7) 0.0901(4) 0.063(3) Uani 1 1 d . . .
C4 C 0.6158(10) 0.2164(10) 0.0504(5) 0.100(5) Uani 1 1 d . . .
H4A H 0.6314 0.2537 0.0270 0.120 Uiso 1 1 calc R . .
H4B H 0.5638 0.1951 0.0460 0.120 Uiso 1 1 calc R . .
H4C H 0.6500 0.1649 0.0529 0.120 Uiso 1 1 calc R . .
C5 C 0.5835(6) 0.3866(7) 0.1282(3) 0.047(2) Uani 1 1 d . . .
C6 C 0.5924(6) 0.5005(7) 0.1782(3) 0.047(2) Uani 1 1 d . . .
C7 C 0.6016(7) 0.6508(7) 0.2130(4) 0.061(3) Uani 1 1 d . . .
H7A H 0.6183 0.7077 0.2008 0.073 Uiso 1 1 calc R . .
H7B H 0.6439 0.6229 0.2278 0.073 Uiso 1 1 calc R . .
H7C H 0.5598 0.6620 0.2323 0.073 Uiso 1 1 calc R . .
C8 C 0.5288(6) 0.6169(6) 0.1453(3) 0.047(2) Uani 1 1 d . . .
C9 C 0.5167(6) 0.5419(7) 0.1204(3) 0.051(3) Uani 1 1 d . . .
C10 C 0.5349(10) 0.9640(8) 0.1220(5) 0.100(5) Uani 1 1 d . . .
H10A H 0.5016 1.0065 0.1363 0.120 Uiso 1 1 calc R . .
H10B H 0.5364 0.9787 0.0924 0.120 Uiso 1 1 calc R . .
H10C H 0.5862 0.9680 0.1335 0.120 Uiso 1 1 calc R . .
C11 C 0.5042(8) 0.8673(7) 0.1277(4) 0.070(4) Uani 1 1 d . . .
C12 C 0.5450(7) 0.7899(8) 0.1358(4) 0.062(3) Uani 1 1 d . . .
H12 H 0.5986 0.7891 0.1387 0.074 Uiso 1 1 calc R . .
C13 C 0.4981(6) 0.7101(7) 0.1395(4) 0.054(3) Uani 1 1 d . . .
C14 C 0.4202(7) 0.7279(8) 0.1350(4) 0.063(3) Uani 1 1 d . . .
C15 C 0.3532(7) 0.6637(10) 0.1367(5) 0.082(4) Uani 1 1 d . . .
H15A H 0.3111 0.6922 0.1516 0.098 Uiso 1 1 calc R . .
H15B H 0.3682 0.6087 0.1512 0.098 Uiso 1 1 calc R . .
H15C H 0.3371 0.6488 0.1085 0.098 Uiso 1 1 calc R . .
C16 C 0.5165(9) 0.6614(10) 0.0379(4) 0.089(4) Uani 1 1 d . . .
H16A H 0.5260 0.6621 0.0081 0.107 Uiso 1 1 calc R . .
H16B H 0.5648 0.6558 0.0528 0.107 Uiso 1 1 calc R . .
H16C H 0.4913 0.7173 0.0461 0.107 Uiso 1 1 calc R . .
C17 C 0.4650(8) 0.5807(8) 0.0488(4) 0.068(3) Uani 1 1 d . . .
C18 C 0.4679(6) 0.5263(7) 0.0837(3) 0.052(3) Uani 1 1 d . . .
C19 C 0.4098(7) 0.4565(8) 0.0824(4) 0.069(3) Uani 1 1 d . . .
H19 H 0.4038 0.4135 0.1038 0.083 Uiso 1 1 calc R . .
C20 C 0.3645(8) 0.4579(9) 0.0478(5) 0.085(4) Uani 1 1 d . . .
C21 C 0.3011(10) 0.3915(12) 0.0357(7) 0.134(8) Uani 1 1 d . . .
H21A H 0.3015 0.3825 0.0057 0.160 Uiso 1 1 calc R . .
H21B H 0.2519 0.4159 0.0442 0.160 Uiso 1 1 calc R . .
H21C H 0.3097 0.3340 0.0497 0.160 Uiso 1 1 calc R . .
C22 C 0.5630(6) 0.3160(7) 0.2451(4) 0.054(3) Uani 1 1 d . . .
H22 H 0.5220 0.2862 0.2319 0.065 Uiso 1 1 calc R . .
C23 C 0.5541(6) 0.4091(7) 0.2597(3) 0.051(3) Uani 1 1 d . . .
C24 C 0.6194(7) 0.4529(8) 0.2768(4) 0.059(3) Uani 1 1 d . . .
H24 H 0.6139 0.5120 0.2873 0.071 Uiso 1 1 calc R . .
C25 C 0.6926(6) 0.4114(7) 0.2787(4) 0.054(3) Uani 1 1 d . . .
C26 C 0.6976(6) 0.3177(7) 0.2661(4) 0.056(3) Uani 1 1 d . . .
H26 H 0.7451 0.2881 0.2682 0.067 Uiso 1 1 calc R . .
C27 C 0.6353(6) 0.2696(6) 0.2511(4) 0.050(3) Uani 1 1 d . . .
C28 C 0.4759(7) 0.4540(10) 0.2566(5) 0.078(4) Uani 1 1 d . . .
H28A H 0.4517 0.4370 0.2304 0.094 Uiso 1 1 calc R . .
H28B H 0.4820 0.5193 0.2577 0.094 Uiso 1 1 calc R . .
H28C H 0.4442 0.4343 0.2798 0.094 Uiso 1 1 calc R . .
C29 C 0.7611(7) 0.4599(9) 0.2959(4) 0.078(4) Uani 1 1 d . . .
H29A H 0.7535 0.5248 0.2936 0.094 Uiso 1 1 calc R . .
H29B H 0.8064 0.4424 0.2803 0.094 Uiso 1 1 calc R . .
H29C H 0.7677 0.4438 0.3251 0.094 Uiso 1 1 calc R . .
C30 C 0.6383(9) 0.1697(8) 0.2388(5) 0.086(4) Uani 1 1 d . . .
H30A H 0.6102 0.1608 0.2129 0.103 Uiso 1 1 calc R . .
H30B H 0.6153 0.1334 0.2607 0.103 Uiso 1 1 calc R . .
H30C H 0.6912 0.1515 0.2349 0.103 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ru1 0.0334(4) 0.0299(4) 0.0643(5) 0.0054(4) -0.0027(4) 0.0019(3)
Cl1 0.0501(16) 0.073(2) 0.090(2) 0.0094(17) 0.0087(15) -0.0147(15)
S1 0.081(2) 0.0578(19) 0.090(2) 0.0073(17) -0.0032(19) 0.0344(17)
S2 0.111(3) 0.085(3) 0.086(3) 0.019(2) -0.038(2) -0.001(2)
P1 0.0555(18) 0.0530(18) 0.093(3) 0.0120(17) -0.0057(18) -0.0014(15)
F1 0.134(6) 0.073(5) 0.153(7) -0.004(5) -0.049(6) -0.015(5)
F2 0.141(7) 0.169(8) 0.133(7) 0.031(6) 0.047(6) 0.057(6)
F3 0.076(5) 0.098(5) 0.141(6) 0.036(5) -0.033(5) -0.008(4)
F4 0.137(8) 0.080(6) 0.183(10) 0.001(6) -0.052(8) -0.038(6)
F5 0.160(10) 0.158(10) 0.132(9) 0.010(8) 0.048(8) -0.024(9)
F6 0.081(5) 0.075(5) 0.149(8) 0.009(5) -0.029(5) 0.028(4)
O1 0.066(5) 0.041(4) 0.068(5) 0.001(4) -0.007(4) 0.002(4)
N1 0.048(5) 0.034(4) 0.068(6) 0.005(4) -0.003(4) 0.005(4)
N2 0.046(5) 0.036(4) 0.058(5) 0.003(4) -0.001(4) 0.011(4)
N3 0.050(5) 0.036(4) 0.063(5) 0.001(4) -0.002(4) 0.013(4)
C1 0.088(10) 0.044(7) 0.128(12) -0.004(7) -0.015(9) 0.025(7)
C2 0.069(7) 0.025(5) 0.078(8) -0.005(5) 0.003(6) 0.001(5)
C3 0.065(7) 0.043(6) 0.081(9) -0.012(6) -0.005(7) 0.013(5)
C4 0.135(14) 0.065(9) 0.099(11) -0.022(8) -0.015(10) 0.030(9)
C5 0.040(5) 0.040(6) 0.060(7) 0.006(5) 0.000(5) 0.005(4)
C6 0.050(6) 0.038(5) 0.054(6) -0.004(5) 0.010(5) 0.007(4)
C7 0.068(7) 0.045(6) 0.069(7) -0.006(6) -0.003(6) 0.001(5)
C8 0.046(6) 0.033(5) 0.062(6) 0.008(4) 0.000(5) 0.009(4)
C9 0.051(6) 0.045(6) 0.058(7) 0.010(5) 0.000(5) 0.013(5)
C10 0.137(14) 0.038(7) 0.124(13) 0.015(7) -0.001(11) 0.016(8)
C11 0.090(9) 0.035(6) 0.086(9) 0.007(6) 0.001(7) 0.025(6)
C12 0.052(7) 0.052(7) 0.081(8) 0.015(6) 0.003(6) 0.011(5)
C13 0.056(6) 0.039(5) 0.066(7) 0.005(5) -0.004(6) 0.015(5)
C14 0.057(7) 0.056(7) 0.076(8) 0.006(6) 0.006(6) 0.022(6)
C15 0.061(8) 0.088(10) 0.097(10) 0.003(8) 0.018(8) 0.019(7)
C16 0.109(12) 0.079(10) 0.079(9) 0.018(8) 0.008(9) -0.017(9)
C17 0.081(9) 0.049(7) 0.075(8) 0.006(6) -0.014(7) 0.004(6)
C18 0.050(6) 0.051(6) 0.057(6) 0.012(5) -0.003(5) 0.003(5)
C19 0.066(8) 0.047(7) 0.095(9) 0.016(6) -0.011(7) 0.003(6)
C20 0.070(9) 0.062(8) 0.123(12) 0.021(8) -0.038(9) -0.008(7)
C21 0.107(13) 0.096(12) 0.20(2) 0.015(13) -0.071(14) -0.030(11)
C22 0.041(6) 0.045(6) 0.076(8) 0.007(5) -0.007(5) -0.003(5)
C23 0.039(5) 0.055(6) 0.060(6) 0.005(5) 0.000(5) 0.014(5)
C24 0.063(7) 0.046(6) 0.068(7) 0.007(5) 0.001(6) 0.005(5)
C25 0.047(6) 0.039(5) 0.074(7) 0.013(5) 0.000(5) 0.002(5)
C26 0.053(6) 0.046(6) 0.069(7) 0.015(5) -0.014(6) 0.014(5)
C27 0.050(6) 0.030(5) 0.069(7) 0.022(5) -0.004(5) -0.007(4)
C28 0.055(7) 0.083(9) 0.096(10) 0.012(8) 0.005(7) 0.019(7)
C29 0.063(8) 0.070(8) 0.102(10) -0.003(8) -0.020(7) -0.017(7)
C30 0.098(11) 0.046(7) 0.114(12) 0.016(7) 0.008(9) -0.011(7)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ru1 C6 2.029(10) . ?
Ru1 N1 2.131(9) . ?
Ru1 C22 2.186(10) . ?
Ru1 C23 2.199(10) . ?
Ru1 C24 2.220(12) . ?
Ru1 C25 2.243(11) . ?
Ru1 C26 2.274(10) . ?
Ru1 C27 2.302(9) . ?
Ru1 Cl1 2.409(3) . ?
S1 C11 1.712(15) . ?
S1 C14 1.727(12) . ?
S2 C17 1.712(13) . ?
S2 C20 1.731(14) . ?
P1 F2 1.530(11) . ?
P1 F5 1.551(11) . ?
P1 F4 1.558(9) . ?
P1 F1 1.575(9) . ?
P1 F3 1.585(8) . ?
P1 F6 1.602(8) . ?
O1 C5 1.321(12) . ?
O1 C3 1.428(12) . ?
O2 H2A 0.8532 . ?
O2 H2B 0.8140 . ?
O3 H3A 0.9132 . ?
O3 H3B 0.7600 . ?
N1 C5 1.289(12) . ?
N1 C2 1.407(13) . ?
N2 C5 1.377(12) . ?
N2 C6 1.378(13) . ?
N2 C9 1.424(12) . ?
N3 C6 1.329(12) . ?
N3 C8 1.402(13) . ?
N3 C7 1.465(13) . ?
C1 C2 1.504(15) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.315(16) . ?
C3 C4 1.492(17) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 C9 1.367(14) . ?
C8 C13 1.471(13) . ?
C9 C18 1.453(15) . ?
C10 C11 1.519(17) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C12 1.355(14) . ?
C12 C13 1.423(15) . ?
C12 H12 0.9300 . ?
C13 C14 1.377(15) . ?
C14 C15 1.490(17) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 C17 1.516(17) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 C18 1.360(15) . ?
C18 C19 1.430(15) . ?
C19 C20 1.347(17) . ?
C19 H19 0.9300 . ?
C20 C21 1.509(19) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 C27 1.432(14) . ?
C22 C23 1.444(14) . ?
C22 H22 0.9300 . ?
C23 C24 1.405(15) . ?
C23 C28 1.503(14) . ?
C24 C25 1.403(15) . ?
C24 H24 0.9300 . ?
C25 C26 1.427(14) . ?
C25 C29 1.483(15) . ?
C26 C27 1.371(14) . ?
C26 H26 0.9300 . ?
C27 C30 1.509(16) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C6 Ru1 N1 75.8(4) . . ?
C6 Ru1 C22 110.4(4) . . ?
N1 Ru1 C22 95.3(4) . . ?
C6 Ru1 C23 89.4(4) . . ?
N1 Ru1 C23 122.0(4) . . ?
C22 Ru1 C23 38.5(4) . . ?
C6 Ru1 C24 98.8(4) . . ?
N1 Ru1 C24 159.0(4) . . ?
C22 Ru1 C24 67.2(4) . . ?
C23 Ru1 C24 37.1(4) . . ?
C6 Ru1 C25 128.3(4) . . ?
N1 Ru1 C25 155.7(3) . . ?
C22 Ru1 C25 79.8(4) . . ?
C23 Ru1 C25 67.5(4) . . ?
C24 Ru1 C25 36.6(4) . . ?
C6 Ru1 C26 163.8(4) . . ?
N1 Ru1 C26 119.7(4) . . ?
C22 Ru1 C26 65.6(4) . . ?
C23 Ru1 C26 78.2(4) . . ?
C24 Ru1 C26 65.0(4) . . ?
C25 Ru1 C26 36.8(4) . . ?
C6 Ru1 C27 146.7(4) . . ?
N1 Ru1 C27 96.4(4) . . ?
C22 Ru1 C27 37.1(4) . . ?
C23 Ru1 C27 67.1(4) . . ?
C24 Ru1 C27 76.9(4) . . ?
C25 Ru1 C27 65.4(4) . . ?
C26 Ru1 C27 34.9(4) . . ?
C6 Ru1 Cl1 89.5(3) . . ?
N1 Ru1 Cl1 86.3(2) . . ?
C22 Ru1 Cl1 159.8(3) . . ?
C23 Ru1 Cl1 150.4(3) . . ?
C24 Ru1 Cl1 114.2(3) . . ?
C25 Ru1 Cl1 90.5(3) . . ?
C26 Ru1 Cl1 96.1(3) . . ?
C27 Ru1 Cl1 122.7(3) . . ?
C11 S1 C14 93.7(5) . . ?
C17 S2 C20 92.9(6) . . ?
F2 P1 F5 177.9(8) . . ?
F2 P1 F4 88.2(7) . . ?
F5 P1 F4 89.9(7) . . ?
F2 P1 F1 95.0(7) . . ?
F5 P1 F1 87.0(6) . . ?
F4 P1 F1 176.8(7) . . ?
F2 P1 F3 89.4(6) . . ?
F5 P1 F3 89.8(6) . . ?
F4 P1 F3 91.8(5) . . ?
F1 P1 F3 89.0(5) . . ?
F2 P1 F6 88.0(6) . . ?
F5 P1 F6 92.8(6) . . ?
F4 P1 F6 89.1(5) . . ?
F1 P1 F6 90.2(5) . . ?
F3 P1 F6 177.2(6) . . ?
C5 O1 C3 103.1(8) . . ?
H2A O2 H2B 134.4 . . ?
H3A O3 H3B 115.5 . . ?
C5 N1 C2 104.6(9) . . ?
C5 N1 Ru1 113.1(7) . . ?
C2 N1 Ru1 142.2(7) . . ?
C5 N2 C6 113.3(8) . . ?
C5 N2 C9 131.7(9) . . ?
C6 N2 C9 112.4(8) . . ?
C6 N3 C8 112.9(9) . . ?
C6 N3 C7 123.2(9) . . ?
C8 N3 C7 123.9(8) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C2 N1 108.7(10) . . ?
C3 C2 C1 128.1(11) . . ?
N1 C2 C1 123.0(11) . . ?
C2 C3 O1 108.0(10) . . ?
C2 C3 C4 137.0(11) . . ?
O1 C3 C4 115.1(11) . . ?
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 O1 115.6(9) . . ?
N1 C5 N2 119.1(10) . . ?
O1 C5 N2 125.0(9) . . ?
N3 C6 N2 103.5(9) . . ?
N3 C6 Ru1 141.1(8) . . ?
N2 C6 Ru1 115.4(7) . . ?
N3 C7 H7A 109.5 . . ?
N3 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N3 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C8 N3 107.4(8) . . ?
C9 C8 C13 127.8(10) . . ?
N3 C8 C13 124.7(9) . . ?
C8 C9 N2 103.8(9) . . ?
C8 C9 C18 132.5(9) . . ?
N2 C9 C18 123.2(9) . . ?
C11 C10 H10A 109.5 . . ?
C11 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C11 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 C10 128.0(13) . . ?
C12 C11 S1 110.2(9) . . ?
C10 C11 S1 121.7(9) . . ?
C11 C12 C13 113.7(11) . . ?
C11 C12 H12 123.1 . . ?
C13 C12 H12 123.1 . . ?
C14 C13 C12 113.1(10) . . ?
C14 C13 C8 122.6(10) . . ?
C12 C13 C8 124.2(10) . . ?
C13 C14 C15 129.5(11) . . ?
C13 C14 S1 109.2(9) . . ?
C15 C14 S1 121.3(9) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 H16A 109.5 . . ?
C17 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C17 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C17 C16 128.1(12) . . ?
C18 C17 S2 111.4(9) . . ?
C16 C17 S2 120.6(10) . . ?
C17 C18 C19 111.5(11) . . ?
C17 C18 C9 125.3(10) . . ?
C19 C18 C9 122.8(10) . . ?
C20 C19 C18 114.9(11) . . ?
C20 C19 H19 122.6 . . ?
C18 C19 H19 122.6 . . ?
C19 C20 C21 128.1(14) . . ?
C19 C20 S2 109.4(10) . . ?
C21 C20 S2 122.5(12) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C27 C22 C23 119.7(10) . . ?
C27 C22 Ru1 75.8(6) . . ?
C23 C22 Ru1 71.3(6) . . ?
C27 C22 H22 120.1 . . ?
C23 C22 H22 120.1 . . ?
Ru1 C22 H22 124.3 . . ?
C24 C23 C22 117.8(9) . . ?
C24 C23 C28 123.1(11) . . ?
C22 C23 C28 119.1(10) . . ?
C24 C23 Ru1 72.3(6) . . ?
C22 C23 Ru1 70.3(6) . . ?
C28 C23 Ru1 129.2(8) . . ?
C25 C24 C23 122.9(10) . . ?
C25 C24 Ru1 72.5(7) . . ?
C23 C24 Ru1 70.6(6) . . ?
C25 C24 H24 118.6 . . ?
C23 C24 H24 118.6 . . ?
Ru1 C24 H24 131.3 . . ?
C24 C25 C26 117.2(10) . . ?
C24 C25 C29 121.9(10) . . ?
C26 C25 C29 120.8(10) . . ?
C24 C25 Ru1 70.8(7) . . ?
C26 C25 Ru1 72.8(6) . . ?
C29 C25 Ru1 130.7(8) . . ?
C27 C26 C25 122.7(10) . . ?
C27 C26 Ru1 73.7(6) . . ?
C25 C26 Ru1 70.4(6) . . ?
C27 C26 H26 118.6 . . ?
C25 C26 H26 118.6 . . ?
Ru1 C26 H26 130.1 . . ?
C26 C27 C22 119.2(9) . . ?
C26 C27 C30 123.9(10) . . ?
C22 C27 C30 116.9(10) . . ?
C26 C27 Ru1 71.5(5) . . ?
C22 C27 Ru1 67.0(5) . . ?
C30 C27 Ru1 132.3(9) . . ?
C23 C28 H28A 109.5 . . ?
C23 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C23 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C25 C29 H29A 109.5 . . ?
C25 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C25 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2 H2A O3 0.85 2.09 2.89(3) 154.6 .
O2 H2B N2 0.81 2.64 3.28(2) 137.2 .
O2 H2B Cl1 0.81 2.81 3.37(2) 127.9 .
_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full 25.68
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max 1.135
_refine_diff_density_min -2.265
_refine_diff_density_rms 0.149
# start Validation Reply Form
_vrf_PLAT420_wt2105w-shelxl
;
PROBLEM: D-H without Acceptor >O2 - >H2A ... ?
RESPONSE: The acceptor for O2-H2A is O3 as shown in the H-bond table.
Unfortunately, the acceptor for O3 could not be found. This is mainly due
to the fact that the water molecules were quite disordered. There are still
about 99A**3 solvent accessible void areas. Data was collected at ambient
temperature of 32 degree Celsius, and the crystal quality is not very good.
Furthermore, there are residual electron peaks close to O3, which indicated
that the water molecules may be very disordered. Under the circumstances of
high thermal mobility of the solvent molecules at room temperature and the
quality of the crystal provided, to locate all the disordered water molecules
is unsuccessful.
;
_vrf_PLAT601_wt2105w-shelxl
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of . 99.00 A**3
RESPONSE: This may due to the heavily disordered water molecules.
;
_vrf_PLAT003_wt2105w-shelxl
;
PROBLEM: Number of Uiso or Uij Restrained Atom Sites .... 3
RESPONSE: The fluorine atoms in PF~6~ ions are showing high rotational
disorder. As a result, atoms F1, F2 and F3 were refined with
isotropic restraints.
;
_vrf_PLAT860_wt2105w-shelxl
;
PROBLEM: Note: Number of Least-Squares Restraints ....... 18
RESPONSE: The fluorine atoms in PF~6~ ions are showing high rotational
disorder. As a result, 18 restraints were used in the refinement. They are
related to the refinement of three fluorine atoms, F1, F2 and F3, using
isotropic restraints of standard deviation of 0.005 for F1, F2 and F3,
in the anisotropic atom displacement components (six restraints for
each fluorine atoms).
;
# Attachment '- wt2106w-shelxl.cif'
data_wt2106w-shelxl
_database_code_depnum_ccdc_archive 'CCDC 814060'
#TrackingRef '- wt2106w-shelxl.cif'
#wt2106w-TAM-Duan Gong Ping's DGP100617-1_19-June-2010
_audit_creation_method SHELXL-97
_chemical_name_systematic ?
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C31 H37 Cl N3 O Ru S2, P F6, 0.5(H2 O)'
_chemical_formula_sum 'C31 H38 Cl F6 N3 O1.50 P Ru S2'
_chemical_formula_weight 822.25
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'
O O 0.0106 0.0060 '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'
P P 0.1023 0.0942 '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'
Cl Cl 0.1484 0.1585 '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'
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'C 2/c'
_symmetry_space_group_name_Hall '-C 2yc'
_symmetry_Int_Tables_number 15
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'
_cell_length_a 18.598(7)
_cell_length_b 17.640(7)
_cell_length_c 22.631(8)
_cell_angle_alpha 90.00
_cell_angle_beta 102.867(5)
_cell_angle_gamma 90.00
_cell_volume 7238(5)
_cell_formula_units_Z 8
_cell_measurement_temperature 305(2)
_cell_measurement_reflns_used 24147
_cell_measurement_theta_min 1.73
_cell_measurement_theta_max 28.27
_exptl_crystal_description block
_exptl_crystal_colour orange
_exptl_crystal_size_max 0.39
_exptl_crystal_size_mid 0.30
_exptl_crystal_size_min 0.20
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.509
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 3352
_exptl_absorpt_coefficient_mu 0.728
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.7643
_exptl_absorpt_correction_T_max 0.8680
_exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)'
_exptl_special_details ?
_diffrn_ambient_temperature 305(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker SMART 1000 CCD'
_diffrn_measurement_method \w
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number 0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time .
_diffrn_standards_decay_% ?
_diffrn_reflns_number 20165
_diffrn_reflns_av_R_equivalents 0.0190
_diffrn_reflns_av_sigmaI/netI 0.0205
_diffrn_reflns_limit_h_min -22
_diffrn_reflns_limit_h_max 20
_diffrn_reflns_limit_k_min -21
_diffrn_reflns_limit_k_max 21
_diffrn_reflns_limit_l_min -23
_diffrn_reflns_limit_l_max 27
_diffrn_reflns_theta_min 1.73
_diffrn_reflns_theta_max 25.68
_reflns_number_total 6867
_reflns_number_gt 5982
_reflns_threshold_expression I>2\s(I)
_computing_data_collection 'SMART (Bruker AXS Inc, 1998)'
_computing_cell_refinement 'SAINT v7.34A (Bruker AXS Inc, 2006)'
_computing_data_reduction
'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2006)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics 'MERCURY (Macrae et al., 2008)'
_computing_publication_material 'SHELXL97 (Sheldrick, 2008)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1093P)^2^+25.3766P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 6867
_refine_ls_number_parameters 437
_refine_ls_number_restraints 30
_refine_ls_R_factor_all 0.0607
_refine_ls_R_factor_gt 0.0546
_refine_ls_wR_factor_ref 0.1731
_refine_ls_wR_factor_gt 0.1661
_refine_ls_goodness_of_fit_ref 1.042
_refine_ls_restrained_S_all 1.079
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.260005(17) 0.649425(19) 0.176379(15) 0.03847(15) Uani 1 1 d . . .
Cl1 Cl 0.16940(7) 0.70831(8) 0.09755(6) 0.0599(3) Uani 1 1 d . . .
S1 S 0.12738(13) 0.27604(10) -0.00878(9) 0.0934(6) Uani 1 1 d . . .
S2 S 0.43316(7) 0.40281(8) -0.05134(6) 0.0545(3) Uani 1 1 d . . .
P1 P 0.5000 0.43304(11) 0.2500 0.0541(4) Uani 1 2 d S . .
P2 P 0.0000 0.46800(17) 0.2500 0.0885(8) Uani 1 2 d S . .
F1 F 0.5000 0.5239(5) 0.2500 0.135(3) Uani 1 2 d SU . .
F2 F 0.4626(3) 0.4367(4) 0.3050(3) 0.1297(17) Uani 1 1 d U . .
F3 F 0.5000 0.3472(5) 0.2500 0.153(3) Uani 1 2 d SU . .
F4 F 0.41996(18) 0.4351(2) 0.20608(16) 0.0792(10) Uani 1 1 d . . .
F5 F 0.0000 0.5570(5) 0.2500 0.197(5) Uani 1 2 d S . .
F6 F 0.0716(4) 0.4730(5) 0.3010(4) 0.203(4) Uani 1 1 d . . .
F7 F 0.0000 0.3786(8) 0.2500 0.199(5) Uani 1 2 d SU . .
F8 F 0.0450(5) 0.4742(5) 0.2013(4) 0.191(3) Uani 1 1 d U . .
O1 O 0.42898(18) 0.70647(18) 0.08851(15) 0.0489(7) Uani 1 1 d . . .
O2 O 0.2250(6) 0.8365(6) 0.0063(5) 0.095(3) Uani 0.50 1 d P . .
H2A H 0.2603 0.8231 -0.0132 0.114 Uiso 0.50 1 d P . .
H2B H 0.2169 0.7949 0.0327 0.114 Uiso 0.50 1 d P . .
N1 N 0.2056(2) 0.5191(2) 0.08463(17) 0.0424(8) Uani 1 1 d . . .
N2 N 0.32003(18) 0.54318(19) 0.09315(15) 0.0368(7) Uani 1 1 d . . .
N3 N 0.3373(2) 0.7017(2) 0.13438(17) 0.0417(8) Uani 1 1 d . . .
C1 C 0.1915(3) 0.6087(4) 0.2383(2) 0.0582(13) Uani 1 1 d . . .
H1 H 0.1448 0.5870 0.2281 0.070 Uiso 1 1 calc R . .
C2 C 0.1988(3) 0.6882(4) 0.2467(2) 0.0616(14) Uani 1 1 d . . .
C3 C 0.2694(3) 0.7203(3) 0.2605(2) 0.0602(13) Uani 1 1 d . . .
H3 H 0.2745 0.7724 0.2662 0.072 Uiso 1 1 calc R . .
C4 C 0.3331(3) 0.6745(3) 0.2660(2) 0.0568(12) Uani 1 1 d . . .
C5 C 0.3252(3) 0.5966(3) 0.2587(2) 0.0548(12) Uani 1 1 d . . .
H5 H 0.3670 0.5664 0.2628 0.066 Uiso 1 1 calc R . .
C6 C 0.2543(3) 0.5622(3) 0.2451(2) 0.0542(12) Uani 1 1 d . . .
C7 C 0.1313(4) 0.7379(5) 0.2380(3) 0.095(2) Uani 1 1 d . . .
H7A H 0.0902 0.7084 0.2441 0.114 Uiso 1 1 calc R . .
H7B H 0.1205 0.7583 0.1977 0.114 Uiso 1 1 calc R . .
H7C H 0.1404 0.7787 0.2668 0.114 Uiso 1 1 calc R . .
C8 C 0.4085(3) 0.7089(4) 0.2803(3) 0.0821(19) Uani 1 1 d . . .
H8A H 0.4443 0.6709 0.2772 0.099 Uiso 1 1 calc R . .
H8B H 0.4187 0.7289 0.3208 0.099 Uiso 1 1 calc R . .
H8C H 0.4107 0.7491 0.2521 0.099 Uiso 1 1 calc R . .
C9 C 0.2477(4) 0.4767(3) 0.2384(3) 0.0784(18) Uani 1 1 d . . .
H9A H 0.1995 0.4639 0.2151 0.094 Uiso 1 1 calc R . .
H9B H 0.2549 0.4538 0.2778 0.094 Uiso 1 1 calc R . .
H9C H 0.2843 0.4583 0.2181 0.094 Uiso 1 1 calc R . .
C10 C 0.2601(2) 0.5651(2) 0.11375(18) 0.0370(8) Uani 1 1 d . . .
C11 C 0.2309(2) 0.4676(2) 0.04692(19) 0.0417(9) Uani 1 1 d . . .
C12 C 0.3035(2) 0.4832(2) 0.05166(19) 0.0397(9) Uani 1 1 d . . .
C13 C 0.1286(3) 0.5201(3) 0.0908(3) 0.0574(12) Uani 1 1 d . . .
H13A H 0.1187 0.4749 0.1113 0.069 Uiso 1 1 calc R . .
H13B H 0.0963 0.5222 0.0513 0.069 Uiso 1 1 calc R . .
H13C H 0.1206 0.5638 0.1138 0.069 Uiso 1 1 calc R . .
C14 C 0.0376(5) 0.3305(5) -0.1153(4) 0.107(3) Uani 1 1 d . . .
H14A H -0.0039 0.3069 -0.1041 0.129 Uiso 1 1 calc R . .
H14B H 0.0570 0.2973 -0.1416 0.129 Uiso 1 1 calc R . .
H14C H 0.0223 0.3772 -0.1361 0.129 Uiso 1 1 calc R . .
C15 C 0.0960(4) 0.3464(4) -0.0597(3) 0.0711(17) Uani 1 1 d . . .
C16 C 0.1321(3) 0.4130(3) -0.0409(2) 0.0598(13) Uani 1 1 d . . .
H16 H 0.1231 0.4580 -0.0626 0.072 Uiso 1 1 calc R . .
C17 C 0.1850(3) 0.4061(3) 0.0155(2) 0.0479(10) Uani 1 1 d . . .
C18 C 0.1890(4) 0.3349(3) 0.0383(3) 0.0650(14) Uani 1 1 d . . .
C19 C 0.2378(6) 0.3059(5) 0.0952(4) 0.114(3) Uani 1 1 d . . .
H19A H 0.2271 0.2533 0.1003 0.137 Uiso 1 1 calc R . .
H19B H 0.2292 0.3343 0.1292 0.137 Uiso 1 1 calc R . .
H19C H 0.2884 0.3112 0.0929 0.137 Uiso 1 1 calc R . .
C20 C 0.2950(4) 0.4721(4) -0.0879(3) 0.0771(18) Uani 1 1 d . . .
H20A H 0.3167 0.4948 -0.1184 0.093 Uiso 1 1 calc R . .
H20B H 0.2654 0.5089 -0.0731 0.093 Uiso 1 1 calc R . .
H20C H 0.2646 0.4301 -0.1052 0.093 Uiso 1 1 calc R . .
C21 C 0.3545(3) 0.4447(3) -0.0369(2) 0.0470(10) Uani 1 1 d . . .
C22 C 0.3597(2) 0.4487(2) 0.0240(2) 0.0403(9) Uani 1 1 d . . .
C23 C 0.4266(3) 0.4181(2) 0.0583(2) 0.0440(10) Uani 1 1 d . . .
H23 H 0.4376 0.4160 0.1005 0.053 Uiso 1 1 calc R . .
C24 C 0.4730(3) 0.3923(2) 0.0246(2) 0.0455(10) Uani 1 1 d . . .
C25 C 0.5477(3) 0.3575(3) 0.0456(3) 0.0669(15) Uani 1 1 d . . .
H25A H 0.5590 0.3532 0.0889 0.080 Uiso 1 1 calc R . .
H25B H 0.5839 0.3890 0.0333 0.080 Uiso 1 1 calc R . .
H25C H 0.5481 0.3081 0.0279 0.080 Uiso 1 1 calc R . .
C26 C 0.3918(2) 0.5796(2) 0.1107(2) 0.0416(9) Uani 1 1 d . . .
H26A H 0.4216 0.5660 0.0822 0.050 Uiso 1 1 calc R . .
H26B H 0.4169 0.5618 0.1505 0.050 Uiso 1 1 calc R . .
C27 C 0.3838(2) 0.6634(2) 0.11193(19) 0.0405(9) Uani 1 1 d . . .
C28 C 0.3519(3) 0.7784(3) 0.1245(3) 0.0542(11) Uani 1 1 d . . .
C29 C 0.4078(3) 0.7809(3) 0.0963(3) 0.0571(12) Uani 1 1 d . . .
C30 C 0.4487(5) 0.8416(3) 0.0724(4) 0.087(2) Uani 1 1 d . . .
H30A H 0.4250 0.8895 0.0749 0.105 Uiso 1 1 calc R . .
H30B H 0.4491 0.8310 0.0309 0.105 Uiso 1 1 calc R . .
H30C H 0.4984 0.8436 0.0959 0.105 Uiso 1 1 calc R . .
C31 C 0.3099(4) 0.8425(3) 0.1440(4) 0.082(2) Uani 1 1 d . . .
H31A H 0.3337 0.8580 0.1843 0.099 Uiso 1 1 calc R . .
H31B H 0.2605 0.8263 0.1435 0.099 Uiso 1 1 calc R . .
H31C H 0.3085 0.8844 0.1167 0.099 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ru1 0.0359(2) 0.0431(2) 0.0379(2) -0.00660(13) 0.01145(15) 0.00207(13)
Cl1 0.0515(7) 0.0626(7) 0.0619(8) 0.0029(6) 0.0050(5) 0.0157(5)
S1 0.1267(16) 0.0636(9) 0.0872(12) -0.0153(8) 0.0177(11) -0.0436(10)
S2 0.0621(7) 0.0610(7) 0.0446(6) -0.0015(5) 0.0207(5) 0.0141(6)
P1 0.0527(10) 0.0596(10) 0.0465(9) 0.000 0.0033(8) 0.000
P2 0.0751(16) 0.0834(17) 0.118(2) 0.000 0.0457(16) 0.000
F1 0.130(3) 0.126(3) 0.143(3) 0.000 0.018(2) 0.000
F2 0.121(2) 0.159(3) 0.113(2) 0.0037(18) 0.0342(18) 0.0081(18)
F3 0.148(4) 0.146(4) 0.162(4) 0.000 0.029(2) 0.000
F4 0.0558(18) 0.101(3) 0.073(2) -0.0065(19) -0.0036(16) -0.0091(17)
F5 0.256(13) 0.109(6) 0.189(10) 0.000 -0.029(9) 0.000
F6 0.140(6) 0.200(8) 0.227(9) 0.001(6) -0.045(6) 0.043(5)
F7 0.200(5) 0.194(5) 0.204(5) 0.000 0.044(2) 0.000
F8 0.191(4) 0.198(4) 0.191(4) 0.000(2) 0.056(2) -0.007(2)
O1 0.0523(18) 0.0438(16) 0.0566(19) -0.0043(14) 0.0248(15) -0.0050(14)
O2 0.109(8) 0.096(7) 0.080(6) 0.019(5) 0.020(6) 0.014(6)
N1 0.0389(18) 0.0456(19) 0.044(2) -0.0048(15) 0.0119(15) -0.0026(15)
N2 0.0373(17) 0.0352(16) 0.0390(18) -0.0051(14) 0.0110(14) 0.0009(13)
N3 0.0425(19) 0.0367(17) 0.048(2) -0.0055(15) 0.0145(16) 0.0010(14)
C1 0.047(3) 0.090(4) 0.043(3) -0.010(3) 0.022(2) -0.015(3)
C2 0.054(3) 0.091(4) 0.044(3) -0.019(3) 0.021(2) 0.008(3)
C3 0.071(3) 0.064(3) 0.047(3) -0.022(2) 0.017(2) -0.002(3)
C4 0.051(3) 0.082(4) 0.037(2) -0.008(2) 0.008(2) -0.004(3)
C5 0.054(3) 0.071(3) 0.039(2) 0.005(2) 0.009(2) 0.008(2)
C6 0.068(3) 0.065(3) 0.034(2) 0.003(2) 0.019(2) -0.008(2)
C7 0.072(4) 0.129(6) 0.088(5) -0.027(4) 0.029(4) 0.034(4)
C8 0.057(3) 0.111(5) 0.072(4) -0.003(4) 0.000(3) -0.022(3)
C9 0.109(5) 0.069(4) 0.062(4) 0.013(3) 0.028(3) -0.010(3)
C10 0.036(2) 0.040(2) 0.036(2) -0.0019(16) 0.0107(16) -0.0004(16)
C11 0.045(2) 0.042(2) 0.038(2) -0.0042(17) 0.0095(17) -0.0010(18)
C12 0.046(2) 0.036(2) 0.038(2) -0.0028(16) 0.0093(17) 0.0017(17)
C13 0.038(2) 0.071(3) 0.065(3) -0.014(3) 0.016(2) -0.008(2)
C14 0.087(5) 0.136(7) 0.091(5) -0.037(5) 0.003(4) -0.035(5)
C15 0.062(3) 0.085(4) 0.066(4) -0.020(3) 0.012(3) -0.023(3)
C16 0.056(3) 0.062(3) 0.056(3) -0.009(2) 0.002(2) -0.009(2)
C17 0.051(3) 0.049(2) 0.045(2) -0.009(2) 0.013(2) -0.006(2)
C18 0.088(4) 0.054(3) 0.052(3) -0.002(2) 0.013(3) -0.020(3)
C19 0.164(9) 0.082(5) 0.081(5) 0.022(4) -0.005(5) -0.015(5)
C20 0.079(4) 0.104(5) 0.047(3) 0.007(3) 0.010(3) 0.032(4)
C21 0.057(3) 0.048(2) 0.038(2) -0.0015(18) 0.0121(19) 0.010(2)
C22 0.047(2) 0.0323(19) 0.043(2) -0.0058(16) 0.0131(18) 0.0015(17)
C23 0.053(2) 0.041(2) 0.037(2) -0.0037(17) 0.0081(18) 0.0041(18)
C24 0.051(2) 0.039(2) 0.046(2) -0.0047(18) 0.0108(19) 0.0043(18)
C25 0.059(3) 0.074(4) 0.068(4) -0.004(3) 0.013(3) 0.020(3)
C26 0.036(2) 0.039(2) 0.050(2) -0.0057(18) 0.0114(18) 0.0018(16)
C27 0.041(2) 0.041(2) 0.040(2) -0.0036(17) 0.0099(17) -0.0029(17)
C28 0.058(3) 0.040(2) 0.067(3) -0.006(2) 0.018(2) 0.001(2)
C29 0.071(3) 0.040(2) 0.065(3) -0.002(2) 0.025(3) -0.007(2)
C30 0.114(6) 0.051(3) 0.110(6) -0.001(3) 0.054(5) -0.024(3)
C31 0.086(5) 0.040(3) 0.129(6) -0.009(3) 0.042(4) 0.006(3)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ru1 C10 2.055(4) . ?
Ru1 N3 2.105(4) . ?
Ru1 C5 2.191(5) . ?
Ru1 C6 2.207(5) . ?
Ru1 C1 2.212(5) . ?
Ru1 C4 2.220(5) . ?
Ru1 C3 2.252(5) . ?
Ru1 C2 2.258(5) . ?
Ru1 Cl1 2.4004(14) . ?
S1 C15 1.706(7) . ?
S1 C18 1.728(6) . ?
S2 C24 1.723(5) . ?
S2 C21 1.733(5) . ?
P1 F3 1.513(9) . ?
P1 F2 1.557(6) . ?
P1 F2 1.557(6) 2_655 ?
P1 F4 1.596(3) . ?
P1 F4 1.596(3) 2_655 ?
P1 F1 1.603(9) . ?
P2 F8 1.530(9) 2 ?
P2 F8 1.530(9) . ?
P2 F6 1.558(7) . ?
P2 F6 1.558(7) 2 ?
P2 F5 1.570(10) . ?
P2 F7 1.577(14) . ?
O1 C27 1.327(5) . ?
O1 C29 1.394(6) . ?
O2 H2A 0.9004 . ?
O2 H2B 0.9799 . ?
N1 C10 1.349(5) . ?
N1 C11 1.397(6) . ?
N1 C13 1.469(6) . ?
N2 C10 1.357(5) . ?
N2 C12 1.403(5) . ?
N2 C26 1.455(5) . ?
N3 C27 1.288(6) . ?
N3 C28 1.407(6) . ?
C1 C6 1.407(8) . ?
C1 C2 1.418(9) . ?
C1 H1 0.9300 . ?
C2 C3 1.400(8) . ?
C2 C7 1.508(8) . ?
C3 C4 1.417(8) . ?
C3 H3 0.9300 . ?
C4 C5 1.388(8) . ?
C4 C8 1.495(8) . ?
C5 C6 1.421(7) . ?
C5 H5 0.9300 . ?
C6 C9 1.518(8) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C11 C12 1.359(6) . ?
C11 C17 1.463(6) . ?
C12 C22 1.464(6) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C15 1.493(9) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 C16 1.374(7) . ?
C16 C17 1.433(7) . ?
C16 H16 0.9300 . ?
C17 C18 1.352(7) . ?
C18 C19 1.492(10) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 C21 1.492(7) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 C22 1.363(6) . ?
C22 C23 1.418(6) . ?
C23 C24 1.352(6) . ?
C23 H23 0.9300 . ?
C24 C25 1.496(7) . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 C27 1.486(6) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C28 C29 1.336(8) . ?
C28 C31 1.496(7) . ?
C29 C30 1.484(7) . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C10 Ru1 N3 84.27(15) . . ?
C10 Ru1 C5 101.15(18) . . ?
N3 Ru1 C5 105.42(17) . . ?
C10 Ru1 C6 89.32(19) . . ?
N3 Ru1 C6 140.20(18) . . ?
C5 Ru1 C6 37.7(2) . . ?
C10 Ru1 C1 106.85(19) . . ?
N3 Ru1 C1 167.36(17) . . ?
C5 Ru1 C1 67.1(2) . . ?
C6 Ru1 C1 37.1(2) . . ?
C10 Ru1 C4 132.84(19) . . ?
N3 Ru1 C4 89.09(18) . . ?
C5 Ru1 C4 36.7(2) . . ?
C6 Ru1 C4 67.1(2) . . ?
C1 Ru1 C4 78.96(19) . . ?
C10 Ru1 C3 166.73(19) . . ?
N3 Ru1 C3 101.92(18) . . ?
C5 Ru1 C3 66.0(2) . . ?
C6 Ru1 C3 78.4(2) . . ?
C1 Ru1 C3 66.0(2) . . ?
C4 Ru1 C3 36.9(2) . . ?
C10 Ru1 C2 141.50(19) . . ?
N3 Ru1 C2 133.47(19) . . ?
C5 Ru1 C2 78.4(2) . . ?
C6 Ru1 C2 66.7(2) . . ?
C1 Ru1 C2 37.0(2) . . ?
C4 Ru1 C2 66.3(2) . . ?
C3 Ru1 C2 36.2(2) . . ?
C10 Ru1 Cl1 84.78(12) . . ?
N3 Ru1 Cl1 84.96(11) . . ?
C5 Ru1 Cl1 168.41(14) . . ?
C6 Ru1 Cl1 133.58(15) . . ?
C1 Ru1 Cl1 101.73(15) . . ?
C4 Ru1 Cl1 141.11(16) . . ?
C3 Ru1 Cl1 107.29(16) . . ?
C2 Ru1 Cl1 90.69(15) . . ?
C15 S1 C18 93.4(3) . . ?
C24 S2 C21 92.9(2) . . ?
F3 P1 F2 92.4(2) . . ?
F3 P1 F2 92.4(2) . 2_655 ?
F2 P1 F2 175.2(5) . 2_655 ?
F3 P1 F4 91.29(16) . . ?
F2 P1 F4 88.7(3) . . ?
F2 P1 F4 91.2(3) 2_655 . ?
F3 P1 F4 91.29(16) . 2_655 ?
F2 P1 F4 91.2(3) . 2_655 ?
F2 P1 F4 88.7(3) 2_655 2_655 ?
F4 P1 F4 177.4(3) . 2_655 ?
F3 P1 F1 180.000(2) . . ?
F2 P1 F1 87.6(2) . . ?
F2 P1 F1 87.6(2) 2_655 . ?
F4 P1 F1 88.71(16) . . ?
F4 P1 F1 88.71(16) 2_655 . ?
F8 P2 F8 171.7(7) 2 . ?
F8 P2 F6 88.7(5) 2 . ?
F8 P2 F6 90.9(5) . . ?
F8 P2 F6 90.9(5) 2 2 ?
F8 P2 F6 88.7(5) . 2 ?
F6 P2 F6 173.5(7) . 2 ?
F8 P2 F5 85.9(4) 2 . ?
F8 P2 F5 85.9(4) . . ?
F6 P2 F5 86.8(4) . . ?
F6 P2 F5 86.8(4) 2 . ?
F8 P2 F7 94.1(4) 2 . ?
F8 P2 F7 94.1(4) . . ?
F6 P2 F7 93.2(4) . . ?
F6 P2 F7 93.2(4) 2 . ?
F5 P2 F7 180.000(3) . . ?
C27 O1 C29 105.5(4) . . ?
H2A O2 H2B 109.2 . . ?
C10 N1 C11 111.8(3) . . ?
C10 N1 C13 126.0(4) . . ?
C11 N1 C13 122.2(4) . . ?
C10 N2 C12 111.7(3) . . ?
C10 N2 C26 123.7(3) . . ?
C12 N2 C26 124.5(3) . . ?
C27 N3 C28 105.8(4) . . ?
C27 N3 Ru1 122.3(3) . . ?
C28 N3 Ru1 131.9(3) . . ?
C6 C1 C2 120.6(5) . . ?
C6 C1 Ru1 71.2(3) . . ?
C2 C1 Ru1 73.3(3) . . ?
C6 C1 H1 119.7 . . ?
C2 C1 H1 119.7 . . ?
Ru1 C1 H1 128.0 . . ?
C3 C2 C1 119.2(5) . . ?
C3 C2 C7 120.3(6) . . ?
C1 C2 C7 120.4(6) . . ?
C3 C2 Ru1 71.7(3) . . ?
C1 C2 Ru1 69.8(3) . . ?
C7 C2 Ru1 128.3(4) . . ?
C2 C3 C4 120.8(5) . . ?
C2 C3 Ru1 72.2(3) . . ?
C4 C3 Ru1 70.3(3) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 H3 119.6 . . ?
Ru1 C3 H3 130.7 . . ?
C5 C4 C3 119.3(5) . . ?
C5 C4 C8 119.8(5) . . ?
C3 C4 C8 120.9(6) . . ?
C5 C4 Ru1 70.6(3) . . ?
C3 C4 Ru1 72.8(3) . . ?
C8 C4 Ru1 129.3(4) . . ?
C4 C5 C6 121.2(5) . . ?
C4 C5 Ru1 72.8(3) . . ?
C6 C5 Ru1 71.7(3) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 H5 119.4 . . ?
Ru1 C5 H5 128.4 . . ?
C1 C6 C5 118.8(5) . . ?
C1 C6 C9 121.4(5) . . ?
C5 C6 C9 119.8(5) . . ?
C1 C6 Ru1 71.7(3) . . ?
C5 C6 Ru1 70.6(3) . . ?
C9 C6 Ru1 129.7(4) . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C4 C8 H8A 109.5 . . ?
C4 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C4 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N1 C10 N2 104.3(3) . . ?
N1 C10 Ru1 131.0(3) . . ?
N2 C10 Ru1 124.7(3) . . ?
C12 C11 N1 106.4(4) . . ?
C12 C11 C17 130.6(4) . . ?
N1 C11 C17 122.7(4) . . ?
C11 C12 N2 105.7(4) . . ?
C11 C12 C22 132.3(4) . . ?
N2 C12 C22 121.9(4) . . ?
N1 C13 H13A 109.5 . . ?
N1 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N1 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 H14A 109.5 . . ?
C15 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C15 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 C14 129.4(7) . . ?
C16 C15 S1 110.0(5) . . ?
C14 C15 S1 120.6(5) . . ?
C15 C16 C17 113.3(5) . . ?
C15 C16 H16 123.4 . . ?
C17 C16 H16 123.4 . . ?
C18 C17 C16 112.8(4) . . ?
C18 C17 C11 121.7(5) . . ?
C16 C17 C11 125.5(4) . . ?
C17 C18 C19 128.3(6) . . ?
C17 C18 S1 110.5(4) . . ?
C19 C18 S1 121.2(5) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C21 C20 H20A 109.5 . . ?
C21 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C21 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 C20 129.7(4) . . ?
C22 C21 S2 110.0(3) . . ?
C20 C21 S2 120.3(4) . . ?
C21 C22 C23 112.9(4) . . ?
C21 C22 C12 123.9(4) . . ?
C23 C22 C12 123.2(4) . . ?
C24 C23 C22 114.3(4) . . ?
C24 C23 H23 122.9 . . ?
C22 C23 H23 122.9 . . ?
C23 C24 C25 128.5(5) . . ?
C23 C24 S2 109.9(3) . . ?
C25 C24 S2 121.5(4) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N2 C26 C27 110.8(3) . . ?
N2 C26 H26A 109.5 . . ?
C27 C26 H26A 109.5 . . ?
N2 C26 H26B 109.5 . . ?
C27 C26 H26B 109.5 . . ?
H26A C26 H26B 108.1 . . ?
N3 C27 O1 113.4(4) . . ?
N3 C27 C26 127.4(4) . . ?
O1 C27 C26 119.2(4) . . ?
C29 C28 N3 107.8(4) . . ?
C29 C28 C31 128.9(5) . . ?
N3 C28 C31 123.3(5) . . ?
C28 C29 O1 107.5(4) . . ?
C28 C29 C30 135.7(5) . . ?
O1 C29 C30 116.8(5) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C28 C31 H31A 109.5 . . ?
C28 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C28 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2 H2A Cl1 0.90 2.60 3.473(12) 162.8 7_565
O2 H2B Cl1 0.98 2.42 3.377(11) 166.1 .
_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full 25.68
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max 1.849
_refine_diff_density_min -1.158
_refine_diff_density_rms 0.107
loop_
_publ_manuscript_incl_extra_item
I
J
CgI...CgJ
'Dihedral angle'
CgI_Perp
CgJ_Perp
CgI_Offset
X--Y
CgJ
Y...CgJ
X--Y...CgJ
X...CgJ
loop_
_geom_extra_tableA_col_1
_geom_extra_tableA_col_2
_geom_extra_tableA_col_3
_geom_extra_tableA_col_4
_geom_extra_tableA_col_5
_geom_extra_tableA_col_6
_geom_extra_tableA_col_7
I J CgI...CgJ 'Dihedral angle' CgI_Perp
CgJ_Perp CgI_Offset
1 1^i^ 5.308(4) 0 3.758(3) 3.758(3) 3.750
2 2^ii^ 4.399(3) 0 3.9690(17) 3.9690(17) 1.896
_geom_extra_table_head_A
;
Table 1. \p...\p interactions (\%A, \%)
Cg1 and Cg2 are centroids of the rings S1/C15-C18 and
S2/C21-C24 respectively, CgI...CgJ is the distance between
ring centroids. The dihedral angle is that between the planes of the
rings I and J. CgI_Perp is the perpendicular
distance of CgI from ring J. CgJ_Perp is the
perpendicular distance of CgJ from ring I. CgI_
Offset is the distance between CgI and perpendicular projection
of CgJ on ring I.
;
_geom_table_footnote_A
;
symmetry operators:
^i^: 1/2-X, 1/2-Y, -Z
^ii^: 1-X, 1-Y, 1-Z
;
loop_
_geom_extra_tableB_col_1
_geom_extra_tableB_col_2
_geom_extra_tableB_col_3
_geom_extra_tableB_col_4
_geom_extra_tableB_col_5
X--Y CgJ Y...CgJ X-Y...CgJ X...CgJ
Ru1--Cl1 Cg3^iii^ 3.736(3) 20.88(4) 1.721(2)
_geom_extra_table_head_B
;
Table 2. X-Y...\p interactions (\%A, \%)
Cg3 is centroid of the ring C1-C6,
Y...CgJ and 'X...CgJ' are the distances between ring
centroid and the specified atom Y and X respectively. X--Y...CgJ
is the angle between the X-Y bond and the ring centroid CgJ.
;
_geom_table_footnote_B
;
symmetry operators:
^iii^: X, Y, Z
;
# start Validation Reply Form
_vrf_PLAT231_wt2106w-shelxl
;
PROBLEM: Hirshfeld Test (Solvent) P1 -- F1 .. 22.00 su
RESPONSE: The PF~6~ anions were known to show rotational disorder.
Furthermore, the data were collected at ambient temperature of 31 degree
Celsius. The high thermal motion of F atoms made it very difficult to
resolve the disorder, as a result the ISOR command was applied to atoms
F1, F2, F3, F7 and F8 atoms, which resulted in large Hirshfeld difference
between P and F atoms.
;
_vrf_PLAT042_wt2106w-shelxl
;
PROBLEM: Calc. and Reported MoietyFormula Strings Differ ?
RESPONSE: This is because, checkCIF like to make the formula into whole
numbers, thus the Calc. and Reported Moiety Formula were doubled, while
in this CIF, the water present as half occupancy only.
;
_vrf_PLAT045_wt2106w-shelxl
;
PROBLEM: Calculated and Reported Z Differ by ............ 0.50 Ratio
RESPONSE: same as above
;
# end Validation Reply Form