# Electronic Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2013


#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication 
#  deposited with the CCDC, and may include chemical, crystal,   
#  experimental, refinement, atomic coordinates, 
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted. 
# 
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material 
#  of the CCDC or of third parties, and may not be copied or further 
#  disseminated in any form, whether machine-readable or not,  
#  except for the purpose of generating routine backup copies 
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and 
#  data retrieval see:
#                         www.ccdc.cam.ac.uk 
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively. 
#
####################################################################### 

data_md355
_database_code_depnum_ccdc_archive 'CCDC 921426'
#TrackingRef 'md355.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C14 H16 N4 O3 Ru), C6 H6'
_chemical_formula_sum            'C34 H38 N8 O6 Ru2'
_chemical_formula_weight         856.86
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru 0.0552 3.2960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           MONOCLINIC
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a                   20.5311(8)
_cell_length_b                   8.6613(3)
_cell_length_c                   20.6671(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.761(4)
_cell_angle_gamma                90.00
_cell_volume                     3553.9(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    7400
_cell_measurement_theta_min      3.5122
_cell_measurement_theta_max      74.6872
_exptl_crystal_description       fragment
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.1852
_exptl_crystal_size_mid          0.1090
_exptl_crystal_size_min          0.0463
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1736
_exptl_absorpt_coefficient_mu    7.349
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.53459
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug 3 2011,13:03:54)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      123.0(1)
_diffrn_radiation_wavelength     1.54180
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'Nova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'Xcalibur, Onyx, Nova'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12764
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_av_sigmaI/netI    0.0403
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.52
_diffrn_reflns_theta_max         67.50
_reflns_number_total             6367
_reflns_number_gt                5576
_reflns_threshold_expression     >2\s(I)
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug 3 2011,13:03:54)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug 3 2011,13:03:54)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug 3 2011,13:03:54)
;
_computing_structure_solution    'SIR-97 (Giacovazzo, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'PLATON (Spek, 2008)'
_computing_publication_material  'SHELXL-97 (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^ > 2\s(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^)+(0.0000P)^2^+108.1643P] 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         6367
_refine_ls_number_parameters     443
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0820
_refine_ls_R_factor_gt           0.0750
_refine_ls_wR_factor_ref         0.1981
_refine_ls_wR_factor_gt          0.1955
_refine_ls_goodness_of_fit_ref   1.193
_refine_ls_restrained_S_all      1.193
_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
C12 C 0.7093(5) 0.3661(11) 0.8150(5) 0.020(2) Uani 1 1 d . . .
C13 C 0.6069(6) 0.2615(17) 0.8502(7) 0.042(3) Uani 1 1 d . . .
H13A H 0.5585 0.2766 0.8313 0.062 Uiso 1 1 calc R . .
H13B H 0.6218 0.3235 0.8909 0.062 Uiso 1 1 calc R . .
H13C H 0.6159 0.1522 0.8610 0.062 Uiso 1 1 calc R . .
C14 C 0.6133(6) 0.3070(14) 0.7335(6) 0.033(3) Uani 1 1 d . . .
H14 H 0.5688 0.2740 0.7124 0.039 Uiso 1 1 calc R . .
C15 C 0.6599(6) 0.3608(13) 0.7029(6) 0.030(2) Uani 1 1 d . . .
H15 H 0.6547 0.3728 0.6561 0.036 Uiso 1 1 calc R . .
C16 C 0.7768(5) 0.4621(14) 0.7378(6) 0.029(2) Uani 1 1 d . . .
H16A H 0.7999 0.5311 0.7747 0.034 Uiso 1 1 calc R . .
H16B H 0.7628 0.5249 0.6966 0.034 Uiso 1 1 calc R . .
C17 C 0.8255(6) 0.3375(15) 0.7278(5) 0.032(3) Uani 1 1 d . . .
H17A H 0.8596 0.3847 0.7077 0.039 Uiso 1 1 calc R . .
H17B H 0.8004 0.2598 0.6959 0.039 Uiso 1 1 calc R . .
C18 C 0.8615(5) 0.2560(13) 0.7927(5) 0.026(2) Uani 1 1 d . . .
H18A H 0.8284 0.1969 0.8101 0.031 Uiso 1 1 calc R . .
H18B H 0.8949 0.1823 0.7836 0.031 Uiso 1 1 calc R . .
C19 C 0.9581(5) 0.4275(13) 0.8453(6) 0.027(2) Uani 1 1 d . . .
H19 H 0.9880 0.3946 0.8197 0.032 Uiso 1 1 calc R . .
C20 C 0.9686(5) 0.5405(14) 0.8909(6) 0.028(2) Uani 1 1 d . . .
H20 H 1.0078 0.6028 0.9043 0.034 Uiso 1 1 calc R . .
C22 C 0.8641(5) 0.4409(13) 0.8858(5) 0.024(2) Uani 1 1 d . . .
C21 C 0.9033(6) 0.6631(13) 0.9644(6) 0.032(3) Uani 1 1 d . . .
H21A H 0.8552 0.6816 0.9597 0.047 Uiso 1 1 calc R . .
H21B H 0.9252 0.7599 0.9574 0.047 Uiso 1 1 calc R . .
H21C H 0.9240 0.6239 1.0095 0.047 Uiso 1 1 calc R . .
C11 C 0.8796(5) 0.5648(12) 0.3706(5) 0.020(2) Uani 1 1 d . . .
C9 C 0.8819(6) 0.4698(16) 0.4744(6) 0.035(3) Uani 1 1 d . . .
H9 H 0.8937 0.4087 0.5138 0.042 Uiso 1 1 calc R . .
C8 C 0.8371(7) 0.5835(16) 0.4607(6) 0.039(3) Uani 1 1 d . . .
H8 H 0.8102 0.6182 0.4891 0.046 Uiso 1 1 calc R . .
C10 C 0.9587(6) 0.3444(14) 0.4128(6) 0.034(3) Uani 1 1 d . . .
H10A H 0.9536 0.3182 0.3657 0.052 Uiso 1 1 calc R . .
H10B H 0.9529 0.2512 0.4377 0.052 Uiso 1 1 calc R . .
H10C H 1.0038 0.3871 0.4316 0.052 Uiso 1 1 calc R . .
C7 C 0.7867(6) 0.7525(14) 0.3624(6) 0.034(3) Uani 1 1 d . . .
H7A H 0.8049 0.8074 0.3288 0.041 Uiso 1 1 calc R . .
H7B H 0.7771 0.8300 0.3939 0.041 Uiso 1 1 calc R . .
C6 C 0.7215(6) 0.6692(14) 0.3273(7) 0.036(3) Uani 1 1 d . . .
H6A H 0.7012 0.6235 0.3615 0.043 Uiso 1 1 calc R . .
H6B H 0.6892 0.7455 0.3015 0.043 Uiso 1 1 calc R . .
C5 C 0.7322(6) 0.5431(13) 0.2804(6) 0.032(3) Uani 1 1 d . . .
H5A H 0.7689 0.4740 0.3045 0.038 Uiso 1 1 calc R . .
H5B H 0.6906 0.4807 0.2660 0.038 Uiso 1 1 calc R . .
C4 C 0.6992(6) 0.6436(14) 0.1643(6) 0.038(3) Uani 1 1 d . . .
H4 H 0.6521 0.6323 0.1588 0.045 Uiso 1 1 calc R . .
C3 C 0.7306(7) 0.6971(15) 0.1192(7) 0.040(3) Uani 1 1 d . . .
H3 H 0.7095 0.7310 0.0751 0.048 Uiso 1 1 calc R . .
C1 C 0.8118(6) 0.6390(13) 0.2130(5) 0.026(2) Uani 1 1 d . . .
C2 C 0.8488(7) 0.7445(17) 0.1144(6) 0.041(3) Uani 1 1 d . . .
H2A H 0.8666 0.8455 0.1317 0.061 Uiso 1 1 calc R . .
H2B H 0.8277 0.7526 0.0663 0.061 Uiso 1 1 calc R . .
H2C H 0.8857 0.6694 0.1219 0.061 Uiso 1 1 calc R . .
C201 C 0.7206(6) 0.5507(13) 0.9300(6) 0.028(2) Uani 1 1 d . . .
C203 C 0.8220(5) 0.3825(12) 1.0043(5) 0.024(2) Uani 1 1 d . . .
C202 C 0.7679(7) 0.1603(16) 0.9197(6) 0.0432(18) Uani 1 1 d . . .
C102 C 0.9272(7) 0.8307(18) 0.2605(8) 0.053(2) Uani 1 1 d . . .
C103 C 0.9999(6) 0.6150(12) 0.3327(5) 0.024(2) Uani 1 1 d . . .
C101 C 0.9253(5) 0.4355(13) 0.2336(5) 0.024(2) Uani 1 1 d . . .
N7 N 0.8955(4) 0.3685(10) 0.8428(4) 0.0234(19) Uani 1 1 d . . .
N8 N 0.9114(4) 0.5494(10) 0.9148(4) 0.0221(18) Uani 1 1 d . . .
N4 N 0.9079(5) 0.4589(11) 0.4183(4) 0.027(2) Uani 1 1 d . . .
N2 N 0.7499(4) 0.6083(11) 0.2204(5) 0.027(2) Uani 1 1 d . . .
N1 N 0.7992(5) 0.6940(11) 0.1487(5) 0.030(2) Uani 1 1 d . . .
N6 N 0.7167(4) 0.3949(10) 0.7537(4) 0.0224(18) Uani 1 1 d . . .
N5 N 0.6433(4) 0.3095(11) 0.8015(5) 0.026(2) Uani 1 1 d . . .
N3 N 0.8362(5) 0.6430(11) 0.3985(5) 0.029(2) Uani 1 1 d . . .
O201 O 0.6866(5) 0.6497(11) 0.9410(5) 0.043(2) Uani 1 1 d . . .
O203 O 0.8498(5) 0.3792(10) 1.0609(4) 0.040(2) Uani 1 1 d . . .
O202 O 0.7587(5) 0.0315(10) 0.9302(4) 0.0432(18) Uani 1 1 d . . .
O102 O 0.9452(5) 0.9430(12) 0.2463(5) 0.053(2) Uani 1 1 d . . .
O103 O 1.0556(4) 0.6192(9) 0.3642(4) 0.0290(17) Uani 1 1 d . . .
O101 O 0.9420(4) 0.3307(9) 0.2059(4) 0.0337(19) Uani 1 1 d . . .
Ru2 Ru 0.77371(4) 0.38066(10) 0.91442(4) 0.0215(2) Uani 1 1 d . . .
Ru1 Ru 0.91109(4) 0.61668(9) 0.27982(4) 0.0199(2) Uani 1 1 d . . .
C23 C 0.9625(6) 0.9195(13) 0.4449(6) 0.027(2) Uani 1 1 d . . .
H23 H 0.9371 0.8644 0.4071 0.032 Uiso 1 1 calc R . .
C24 C 0.9323(6) 0.9663(13) 0.4946(6) 0.029(2) Uani 1 1 d . . .
H24 H 0.8863 0.9436 0.4911 0.035 Uiso 1 1 calc R . .
C25 C 1.0295(6) 0.9531(13) 0.4504(6) 0.030(3) Uani 1 1 d . . .
H25 H 1.0498 0.9207 0.4162 0.036 Uiso 1 1 calc R . .
C28 C 0.9522(6) 0.0529(14) 1.0317(7) 0.036(3) Uani 1 1 d . . .
H28 H 0.9195 0.0884 1.0536 0.043 Uiso 1 1 calc R . .
C26 C 0.9458(6) 0.0882(15) 0.9669(6) 0.037(3) Uani 1 1 d . . .
H26 H 0.9089 0.1493 0.9435 0.044 Uiso 1 1 calc R . .
C27 C 0.9935(6) 0.0352(15) 0.9331(7) 0.039(3) Uani 1 1 d . . .
H27 H 0.9886 0.0593 0.8873 0.047 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
C12 0.029(5) 0.010(4) 0.027(5) -0.001(4) 0.015(4) 0.006(4)
C13 0.032(6) 0.049(8) 0.048(7) -0.014(7) 0.016(6) -0.017(6)
C14 0.031(6) 0.029(6) 0.035(6) -0.006(5) 0.001(5) 0.000(5)
C15 0.032(6) 0.024(6) 0.030(6) -0.005(5) 0.000(5) -0.001(5)
C16 0.026(6) 0.030(6) 0.028(6) 0.006(5) 0.005(5) -0.002(5)
C17 0.036(6) 0.042(7) 0.022(5) -0.011(5) 0.013(5) -0.003(6)
C18 0.030(6) 0.021(5) 0.031(6) -0.004(5) 0.015(5) 0.000(5)
C19 0.017(5) 0.032(6) 0.033(6) 0.009(5) 0.012(4) 0.001(5)
C20 0.020(5) 0.033(6) 0.031(6) 0.009(5) 0.004(4) -0.007(5)
C22 0.027(5) 0.026(6) 0.019(5) -0.001(4) 0.004(4) -0.001(5)
C21 0.035(6) 0.025(6) 0.035(6) -0.004(5) 0.009(5) -0.007(5)
C11 0.022(5) 0.018(5) 0.021(5) 0.002(4) 0.009(4) -0.005(4)
C9 0.036(6) 0.046(8) 0.024(6) 0.001(5) 0.010(5) -0.018(6)
C8 0.044(7) 0.050(8) 0.031(6) -0.012(6) 0.026(6) -0.021(7)
C10 0.026(6) 0.030(6) 0.043(7) 0.009(6) 0.002(5) -0.003(5)
C7 0.034(6) 0.027(6) 0.047(7) -0.010(6) 0.024(6) 0.003(5)
C6 0.027(6) 0.030(6) 0.053(8) 0.002(6) 0.016(6) 0.000(5)
C5 0.023(6) 0.023(6) 0.047(7) 0.003(5) 0.005(5) -0.006(5)
C4 0.031(6) 0.024(6) 0.047(7) 0.002(6) -0.010(5) 0.005(5)
C3 0.040(7) 0.034(7) 0.037(7) 0.000(6) -0.007(6) 0.009(6)
C1 0.035(6) 0.022(5) 0.017(5) -0.002(4) 0.002(4) 0.005(5)
C2 0.053(8) 0.043(7) 0.028(6) 0.008(6) 0.014(6) 0.010(7)
C201 0.033(6) 0.024(6) 0.031(6) -0.001(5) 0.016(5) -0.005(5)
C203 0.028(5) 0.013(5) 0.032(6) -0.001(4) 0.011(5) -0.008(4)
C202 0.062(5) 0.035(4) 0.033(4) 0.007(3) 0.013(3) -0.023(4)
C102 0.042(5) 0.044(5) 0.068(5) 0.020(4) 0.005(4) -0.011(4)
C103 0.036(6) 0.017(5) 0.021(5) -0.001(4) 0.011(5) 0.001(5)
C101 0.011(5) 0.028(6) 0.032(6) 0.002(5) 0.005(4) -0.005(4)
N7 0.020(4) 0.023(5) 0.028(5) 0.002(4) 0.007(4) 0.001(4)
N8 0.024(4) 0.022(4) 0.023(4) 0.004(4) 0.011(4) -0.001(4)
N4 0.026(5) 0.033(5) 0.024(5) 0.003(4) 0.007(4) -0.006(4)
N2 0.019(4) 0.022(5) 0.035(5) 0.001(4) 0.001(4) 0.001(4)
N1 0.036(5) 0.025(5) 0.027(5) 0.002(4) 0.005(4) 0.004(4)
N6 0.023(4) 0.021(4) 0.020(4) -0.003(4) -0.001(3) 0.002(4)
N5 0.022(4) 0.028(5) 0.030(5) -0.005(4) 0.014(4) -0.004(4)
N3 0.031(5) 0.029(5) 0.029(5) -0.005(4) 0.012(4) -0.009(4)
O201 0.044(5) 0.040(5) 0.050(5) -0.004(4) 0.019(4) 0.010(4)
O203 0.050(5) 0.040(5) 0.024(4) 0.001(4) -0.002(4) -0.009(4)
O202 0.062(5) 0.035(4) 0.033(4) 0.007(3) 0.013(3) -0.023(4)
O102 0.042(5) 0.044(5) 0.068(5) 0.020(4) 0.005(4) -0.011(4)
O103 0.017(4) 0.036(4) 0.034(4) -0.002(4) 0.006(3) 0.000(3)
O101 0.029(4) 0.028(4) 0.047(5) -0.014(4) 0.017(4) -0.001(4)
Ru2 0.0202(4) 0.0250(4) 0.0209(4) -0.0012(3) 0.0082(3) -0.0033(3)
Ru1 0.0187(4) 0.0213(4) 0.0211(4) 0.0006(3) 0.0078(3) 0.0011(3)
C23 0.028(6) 0.022(5) 0.030(6) 0.002(5) 0.004(5) -0.001(5)
C24 0.028(6) 0.025(6) 0.036(6) -0.001(5) 0.011(5) -0.005(5)
C25 0.036(6) 0.021(6) 0.037(6) -0.004(5) 0.014(5) 0.000(5)
C28 0.033(6) 0.028(6) 0.051(8) -0.006(6) 0.019(6) -0.004(5)
C26 0.027(6) 0.034(7) 0.046(7) 0.013(6) 0.004(5) 0.001(5)
C27 0.042(7) 0.029(6) 0.041(7) 0.008(6) 0.000(6) -0.014(6)
_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_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C12 N6 1.337(13) . ?
C12 N5 1.400(13) . ?
C12 Ru2 2.145(10) . ?
C13 N5 1.459(15) . ?
C14 C15 1.357(17) . ?
C14 N5 1.383(14) . ?
C15 N6 1.388(13) . ?
C16 N6 1.476(13) . ?
C16 C17 1.521(16) . ?
C17 C18 1.529(16) . ?
C18 N7 1.463(14) . ?
C19 C20 1.338(17) . ?
C19 N7 1.371(13) . ?
C20 N8 1.387(14) . ?
C22 N8 1.375(14) . ?
C22 N7 1.376(14) . ?
C22 Ru2 2.151(11) . ?
C21 N8 1.462(14) . ?
C11 N3 1.361(14) . ?
C11 N4 1.362(14) . ?
C11 Ru1 2.181(10) . ?
C9 C8 1.328(19) . ?
C9 N4 1.398(14) . ?
C8 N3 1.381(15) . ?
C10 N4 1.465(15) . ?
C7 N3 1.450(16) . ?
C7 C6 1.531(16) . ?
C6 C5 1.513(17) . ?
C5 N2 1.489(15) . ?
C4 C3 1.343(19) . ?
C4 N2 1.380(14) . ?
C3 N1 1.386(16) . ?
C1 N2 1.344(14) . ?
C1 N1 1.373(14) . ?
C1 Ru1 2.160(11) . ?
C2 N1 1.449(16) . ?
C201 O201 1.165(14) . ?
C201 Ru2 1.908(12) . ?
C203 O203 1.165(13) . ?
C203 Ru2 1.869(11) . ?
C202 O202 1.161(15) . ?
C202 Ru2 1.917(13) . ?
C102 O102 1.106(17) . ?
C102 Ru1 1.942(15) . ?
C103 O103 1.164(13) . ?
C103 Ru1 1.871(11) . ?
C101 O101 1.170(13) . ?
C101 Ru1 1.898(11) . ?
C23 C25 1.382(16) . ?
C23 C24 1.389(16) . ?
C24 C25 1.393(16) 3_776 ?
C25 C24 1.393(16) 3_776 ?
C28 C26 1.349(18) . ?
C28 C27 1.392(18) 3_757 ?
C26 C27 1.416(19) . ?
C27 C28 1.392(18) 3_757 ?
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
N6 C12 N5 102.3(9) . . ?
N6 C12 Ru2 134.9(8) . . ?
N5 C12 Ru2 122.7(7) . . ?
C15 C14 N5 106.5(10) . . ?
C14 C15 N6 106.0(10) . . ?
N6 C16 C17 111.5(9) . . ?
C16 C17 C18 113.3(9) . . ?
N7 C18 C17 110.5(9) . . ?
C20 C19 N7 106.3(9) . . ?
C19 C20 N8 107.0(9) . . ?
N8 C22 N7 101.4(9) . . ?
N8 C22 Ru2 127.6(7) . . ?
N7 C22 Ru2 130.3(8) . . ?
N3 C11 N4 103.5(9) . . ?
N3 C11 Ru1 129.2(8) . . ?
N4 C11 Ru1 126.5(7) . . ?
C8 C9 N4 105.3(11) . . ?
C9 C8 N3 108.6(11) . . ?
N3 C7 C6 110.4(10) . . ?
C5 C6 C7 113.0(9) . . ?
N2 C5 C6 111.4(9) . . ?
C3 C4 N2 105.5(11) . . ?
C4 C3 N1 107.5(11) . . ?
N2 C1 N1 103.3(9) . . ?
N2 C1 Ru1 132.4(8) . . ?
N1 C1 Ru1 124.3(8) . . ?
O201 C201 Ru2 176.8(10) . . ?
O203 C203 Ru2 176.9(9) . . ?
O202 C202 Ru2 169.2(13) . . ?
O102 C102 Ru1 168.3(15) . . ?
O103 C103 Ru1 177.3(10) . . ?
O101 C101 Ru1 171.7(9) . . ?
C19 N7 C22 113.2(9) . . ?
C19 N7 C18 123.3(9) . . ?
C22 N7 C18 122.9(9) . . ?
C22 N8 C20 112.0(9) . . ?
C22 N8 C21 124.9(9) . . ?
C20 N8 C21 123.2(9) . . ?
C11 N4 C9 111.8(10) . . ?
C11 N4 C10 125.6(9) . . ?
C9 N4 C10 122.6(10) . . ?
C1 N2 C4 113.1(10) . . ?
C1 N2 C5 127.5(9) . . ?
C4 N2 C5 119.5(10) . . ?
C1 N1 C3 110.6(10) . . ?
C1 N1 C2 126.6(10) . . ?
C3 N1 C2 122.8(10) . . ?
C12 N6 C15 113.7(9) . . ?
C12 N6 C16 126.0(9) . . ?
C15 N6 C16 120.3(9) . . ?
C14 N5 C12 111.5(9) . . ?
C14 N5 C13 121.5(10) . . ?
C12 N5 C13 127.0(9) . . ?
C11 N3 C8 110.7(10) . . ?
C11 N3 C7 123.8(9) . . ?
C8 N3 C7 124.5(10) . . ?
C203 Ru2 C201 90.4(5) . . ?
C203 Ru2 C202 88.7(5) . . ?
C201 Ru2 C202 135.4(6) . . ?
C203 Ru2 C12 173.5(4) . . ?
C201 Ru2 C12 88.2(4) . . ?
C202 Ru2 C12 87.9(5) . . ?
C203 Ru2 C22 89.7(4) . . ?
C201 Ru2 C22 115.4(4) . . ?
C202 Ru2 C22 109.1(5) . . ?
C12 Ru2 C22 96.7(4) . . ?
C103 Ru1 C101 92.0(4) . . ?
C103 Ru1 C102 86.4(5) . . ?
C101 Ru1 C102 129.0(6) . . ?
C103 Ru1 C1 173.9(4) . . ?
C101 Ru1 C1 89.6(4) . . ?
C102 Ru1 C1 88.0(5) . . ?
C103 Ru1 C11 87.4(4) . . ?
C101 Ru1 C11 112.3(4) . . ?
C102 Ru1 C11 118.5(6) . . ?
C1 Ru1 C11 97.5(4) . . ?
C25 C23 C24 120.0(11) . . ?
C23 C24 C25 119.0(11) . 3_776 ?
C23 C25 C24 120.9(11) . 3_776 ?
C26 C28 C27 120.3(12) . 3_757 ?
C28 C26 C27 120.8(12) . . ?
C28 C27 C26 118.9(12) 3_757 . ?
_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        67.50
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         2.222
_refine_diff_density_min         -2.177
_refine_diff_density_rms         0.189


data_xn11180-md366
_database_code_depnum_ccdc_archive 'CCDC 921427'
#TrackingRef 'xn11180-md366.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C11 H O11 Ru3, C14 H15 N4 O3 Ru'
_chemical_formula_sum            'C25 H16 N4 O14 Ru4'
_chemical_formula_weight         1000.70
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru 0.0552 3.2960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           MONOCLINIC
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a                   13.3007(5)
_cell_length_b                   15.6862(5)
_cell_length_c                   15.2570(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.473(3)
_cell_angle_gamma                90.00
_cell_volume                     3180.22(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    2375
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?
_exptl_crystal_description       fragment
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.0634
_exptl_crystal_size_mid          0.0530
_exptl_crystal_size_min          0.0284
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.090
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1928
_exptl_absorpt_coefficient_mu    15.748
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_correction_T_min  0.0127
_exptl_absorpt_correction_T_max  0.0259
_exptl_absorpt_process_details   
;
Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56
Cubic fit to sin(theta)/lambda - 24 parameters
;
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     1.54180
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'Nova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'Xcalibur, Onyx, Nova'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4889
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0937
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         4.04
_diffrn_reflns_theta_max         62.51
_reflns_number_total             4889
_reflns_number_gt                3341
_reflns_threshold_expression     >2\s(I)
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_structure_solution    'SIR-97 (Giacovazzo, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'PLATON (Spek, 2008)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_refine_special_details          
;
The structure exhibits positional disorder on the C14 H15 N4 O3 Ru fragment which is
disordered over two positions in a 52:48 ratio. Restraints on
the geometrical and thermal parameters were required.
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^ > 2\s(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^)+(0.1012P)^2^+7.0087P] 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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4889
_refine_ls_number_parameters     457
_refine_ls_number_restraints     25
_refine_ls_R_factor_all          0.1233
_refine_ls_R_factor_gt           0.0777
_refine_ls_wR_factor_ref         0.2354
_refine_ls_wR_factor_gt          0.2013
_refine_ls_goodness_of_fit_ref   1.202
_refine_ls_restrained_S_all      1.199
_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 0.7434(6) 0.1425(4) 0.4512(5) 0.0298(12) Uani 0.520(10) 1 d P A 1
Ru1A Ru 0.7227(7) 0.1686(5) 0.4579(6) 0.0347(14) Uani 0.480(10) 1 d P A 2
C1 C 0.846(3) 0.150(2) 0.354(2) 0.034(9) Uani 0.520(10) 1 d PD A 1
C2 C 0.924(3) 0.0067(14) 0.324(2) 0.040(6) Uani 0.520(10) 1 d PD A 1
H2A H 0.9464 0.0001 0.3856 0.060 Uiso 0.520(10) 1 calc PR A 1
H2B H 0.9773 -0.0132 0.2863 0.060 Uiso 0.520(10) 1 calc PR A 1
H2C H 0.8631 -0.0269 0.3120 0.060 Uiso 0.520(10) 1 calc PR A 1
C3 C 0.955(3) 0.139(2) 0.244(2) 0.039(5) Uani 0.520(10) 1 d PD A 1
H3 H 1.0010 0.1154 0.2046 0.047 Uiso 0.520(10) 1 calc PR A 1
C4 C 0.929(4) 0.221(3) 0.250(3) 0.039(5) Uani 0.520(10) 1 d PD A 1
H4 H 0.9515 0.2664 0.2154 0.047 Uiso 0.520(10) 1 calc PR A 1
C5 C 0.816(4) 0.301(3) 0.360(3) 0.066(10) Uani 0.520(10) 1 d P A 1
H5A H 0.7985 0.3445 0.3152 0.079 Uiso 0.520(10) 1 calc PR A 1
H5B H 0.8657 0.3258 0.4028 0.079 Uiso 0.520(10) 1 calc PR A 1
C6 C 0.721(2) 0.273(2) 0.4070(19) 0.036(6) Uani 0.520(10) 1 d P A 1
H6 H 0.7136 0.3109 0.4594 0.043 Uiso 0.520(10) 1 calc PR A 1
C7 C 0.622(3) 0.278(2) 0.349(2) 0.048(7) Uani 0.520(10) 1 d P A 1
H7A H 0.5661 0.2961 0.3845 0.058 Uiso 0.520(10) 1 calc PR A 1
H7B H 0.6301 0.3202 0.3014 0.058 Uiso 0.520(10) 1 calc PR A 1
C8 C 0.527(3) 0.177(3) 0.249(3) 0.061(8) Uani 0.520(10) 1 d PD A 1
H8 H 0.4848 0.2161 0.2169 0.074 Uiso 0.520(10) 1 calc PR A 1
C9 C 0.524(3) 0.092(3) 0.241(3) 0.061(8) Uani 0.520(10) 1 d PD A 1
H9 H 0.4837 0.0602 0.2002 0.074 Uiso 0.520(10) 1 calc PR A 1
C10 C 0.613(3) -0.030(2) 0.324(3) 0.064(9) Uani 0.520(10) 1 d PD A 1
H10A H 0.6832 -0.0420 0.3120 0.095 Uiso 0.520(10) 1 calc PR A 1
H10B H 0.5686 -0.0669 0.2879 0.095 Uiso 0.520(10) 1 calc PR A 1
H10C H 0.6017 -0.0403 0.3862 0.095 Uiso 0.520(10) 1 calc PR A 1
C11 C 0.635(5) 0.123(2) 0.351(4) 0.043(11) Uani 0.520(10) 1 d PD A 1
C1A C 0.624(5) 0.145(2) 0.353(4) 0.034(9) Uani 0.480(10) 1 d PD A 2
C2A C 0.551(3) 0.2839(15) 0.297(2) 0.040(6) Uani 0.480(10) 1 d PD A 2
H2A1 H 0.5198 0.3010 0.3519 0.060 Uiso 0.480(10) 1 calc PR A 2
H2A2 H 0.5070 0.3009 0.2471 0.060 Uiso 0.480(10) 1 calc PR A 2
H2A3 H 0.6163 0.3118 0.2938 0.060 Uiso 0.480(10) 1 calc PR A 2
C3A C 0.514(3) 0.141(2) 0.237(2) 0.039(5) Uani 0.480(10) 1 d PD A 2
H3A H 0.4697 0.1600 0.1910 0.047 Uiso 0.480(10) 1 calc PR A 2
C4A C 0.538(3) 0.059(2) 0.255(2) 0.039(5) Uani 0.480(10) 1 d PD A 2
H4A H 0.5152 0.0092 0.2237 0.047 Uiso 0.480(10) 1 calc PR A 2
C5A C 0.659(4) -0.004(2) 0.383(3) 0.066(10) Uani 0.480(10) 1 d P A 2
H5A1 H 0.6138 -0.0284 0.4258 0.079 Uiso 0.480(10) 1 calc PR A 2
H5A2 H 0.6808 -0.0501 0.3439 0.079 Uiso 0.480(10) 1 calc PR A 2
C6A C 0.748(3) 0.035(2) 0.429(2) 0.036(6) Uani 0.480(10) 1 d P A 2
H6A H 0.7589 0.0044 0.4862 0.043 Uiso 0.480(10) 1 calc PR A 2
C7A C 0.847(3) 0.026(2) 0.377(3) 0.048(7) Uani 0.480(10) 1 d P A 2
H7A1 H 0.9034 0.0092 0.4175 0.058 Uiso 0.480(10) 1 calc PR A 2
H7A2 H 0.8377 -0.0189 0.3317 0.058 Uiso 0.480(10) 1 calc PR A 2
C8A C 0.941(4) 0.125(4) 0.274(3) 0.061(8) Uani 0.480(10) 1 d PD A 2
H8A H 0.9822 0.0847 0.2459 0.074 Uiso 0.480(10) 1 calc PR A 2
C9A C 0.939(5) 0.209(4) 0.263(4) 0.061(8) Uani 0.480(10) 1 d PD A 2
H9A H 0.9782 0.2414 0.2242 0.074 Uiso 0.480(10) 1 calc PR A 2
C10A C 0.846(4) 0.331(2) 0.326(4) 0.064(9) Uani 0.480(10) 1 d PD A 2
H10D H 0.7735 0.3400 0.3157 0.095 Uiso 0.480(10) 1 calc PR A 2
H10E H 0.8825 0.3628 0.2819 0.095 Uiso 0.480(10) 1 calc PR A 2
H10F H 0.8666 0.3517 0.3846 0.095 Uiso 0.480(10) 1 calc PR A 2
C11A C 0.824(4) 0.177(2) 0.366(3) 0.043(11) Uani 0.480(10) 1 d PD A 2
N1 N 0.903(2) 0.0959(13) 0.3057(19) 0.035(5) Uani 0.520(10) 1 d PD A 1
N2 N 0.863(3) 0.2267(19) 0.316(3) 0.035(5) Uani 0.520(10) 1 d PD A 1
N3 N 0.601(3) 0.196(2) 0.311(2) 0.047(6) Uani 0.520(10) 1 d PD A 1
N4 N 0.591(3) 0.058(2) 0.303(2) 0.047(6) Uani 0.520(10) 1 d PD A 1
N1A N 0.564(2) 0.1920(15) 0.297(2) 0.035(5) Uani 0.480(10) 1 d PD A 2
N2A N 0.601(3) 0.063(2) 0.328(2) 0.035(5) Uani 0.480(10) 1 d PD A 2
N3A N 0.871(3) 0.107(2) 0.335(2) 0.047(6) Uani 0.480(10) 1 d PD A 2
N4A N 0.869(4) 0.240(2) 0.319(4) 0.047(6) Uani 0.480(10) 1 d PD A 2
C101 C 0.827(3) 0.163(2) 0.543(3) 0.031(3) Uani 0.520(10) 1 d P A 1
C102 C 0.647(3) 0.153(3) 0.541(2) 0.031(3) Uani 0.520(10) 1 d P A 1
C103 C 0.764(2) 0.025(2) 0.476(2) 0.031(3) Uani 0.520(10) 1 d P A 1
O101 O 0.897(3) 0.1730(17) 0.596(2) 0.055(3) Uani 0.520(10) 1 d P A 1
O102 O 0.578(2) 0.1594(17) 0.585(2) 0.055(3) Uani 0.520(10) 1 d P A 1
O103 O 0.7836(19) -0.0450(16) 0.4911(16) 0.055(3) Uani 0.520(10) 1 d P A 1
C111 C 0.621(3) 0.141(3) 0.529(2) 0.031(3) Uani 0.480(10) 1 d PD A 2
C112 C 0.843(4) 0.186(3) 0.541(3) 0.031(3) Uani 0.480(10) 1 d P A 2
C113 C 0.690(2) 0.291(2) 0.467(2) 0.031(3) Uani 0.480(10) 1 d P A 2
O111 O 0.571(2) 0.1168(19) 0.586(2) 0.055(3) Uani 0.480(10) 1 d PD A 2
O112 O 0.900(3) 0.2067(19) 0.591(3) 0.055(3) Uani 0.480(10) 1 d P A 2
O113 O 0.670(2) 0.3592(17) 0.4799(18) 0.055(3) Uani 0.480(10) 1 d P A 2
C401 C 0.8844(17) 0.1680(12) 0.0229(13) 0.049(5) Uani 1 1 d . . .
C402 C 0.7208(14) 0.2463(12) 0.0995(11) 0.042(4) Uani 1 1 d . . .
C404 C 0.6051(17) 0.1260(13) 0.0052(12) 0.052(5) Uani 1 1 d . . .
C403 C 0.7600(13) 0.0549(11) 0.1061(14) 0.047(5) Uani 1 1 d . . .
C202 C 0.7838(14) 0.0343(10) -0.2556(12) 0.043(4) Uani 1 1 d . . .
C201 C 0.9187(18) 0.0372(13) -0.1051(11) 0.053(5) Uani 1 1 d . . .
C204 C 0.648(2) 0.1375(14) -0.1658(12) 0.063(6) Uani 1 1 d . . .
C203 C 0.7101(15) -0.0235(14) -0.0985(12) 0.053(5) Uani 1 1 d . . .
C302 C 0.7112(14) 0.2880(13) -0.2478(13) 0.049(5) Uani 1 1 d . . .
C301 C 0.8412(14) 0.3257(11) -0.0917(11) 0.039(4) Uani 1 1 d . . .
C303 C 0.6261(16) 0.3048(14) -0.0822(13) 0.056(5) Uani 1 1 d . . .
O401 O 0.9695(11) 0.1861(10) 0.0250(8) 0.060(4) Uani 1 1 d . . .
O402 O 0.7100(10) 0.3034(9) 0.1444(9) 0.059(4) Uani 1 1 d . . .
O404 O 0.5209(12) 0.1103(13) -0.0035(10) 0.085(5) Uani 1 1 d . . .
O403 O 0.7699(11) -0.0001(8) 0.1557(9) 0.061(4) Uani 1 1 d . . .
O202 O 0.7834(13) 0.0097(9) -0.3267(9) 0.075(5) Uani 1 1 d . . .
O201 O 1.0010(12) 0.0133(10) -0.0976(10) 0.073(4) Uani 1 1 d . . .
O204 O 0.5681(11) 0.1219(9) -0.1963(9) 0.060(4) Uani 1 1 d . . .
O203 O 0.6663(11) -0.0828(10) -0.0780(10) 0.071(4) Uani 1 1 d . . .
O302 O 0.6980(11) 0.3107(9) -0.3171(9) 0.063(4) Uani 1 1 d . . .
O301 O 0.9015(10) 0.3728(9) -0.0703(9) 0.058(4) Uani 1 1 d . . .
O303 O 0.5602(11) 0.3409(9) -0.0535(9) 0.061(4) Uani 1 1 d . . .
Ru4 Ru 0.74517(10) 0.14943(8) 0.02677(8) 0.0364(4) Uani 1 1 d . . .
Ru2 Ru 0.78151(11) 0.07093(8) -0.13763(9) 0.0400(4) Uani 1 1 d . . .
Ru3 Ru 0.73441(10) 0.24541(8) -0.13149(8) 0.0365(4) Uani 1 1 d . . .
H100 H 0.857(11) 0.171(9) -0.157(9) 0.03(4) Uiso 1 1 d . . .
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 0.028(3) 0.029(3) 0.032(2) 0.001(2) -0.0053(19) -0.001(2)
Ru1A 0.031(4) 0.040(4) 0.032(2) 0.001(3) -0.004(2) 0.000(2)
C1 0.02(2) 0.044(19) 0.032(16) 0.001(14) -0.004(14) 0.010(17)
C2 0.052(17) 0.016(11) 0.054(15) -0.001(10) 0.027(13) 0.011(11)
C3 0.037(13) 0.062(13) 0.017(8) -0.009(9) -0.011(8) -0.010(10)
C4 0.037(13) 0.062(13) 0.017(8) -0.009(9) -0.011(8) -0.010(10)
C5 0.10(3) 0.031(15) 0.06(2) 0.005(14) -0.004(18) -0.031(17)
C6 0.042(16) 0.044(15) 0.023(11) -0.014(11) 0.015(11) 0.007(12)
C7 0.048(18) 0.042(15) 0.054(16) -0.002(12) -0.007(13) 0.025(13)
C8 0.039(16) 0.072(17) 0.075(18) -0.014(15) 0.022(14) -0.001(13)
C9 0.039(16) 0.072(17) 0.075(18) -0.014(15) 0.022(14) -0.001(13)
C10 0.06(2) 0.044(17) 0.08(2) -0.008(16) -0.028(17) 0.022(16)
C11 0.026(19) 0.06(2) 0.042(19) 0.025(18) 0.008(14) 0.02(2)
C1A 0.02(2) 0.044(19) 0.032(16) 0.001(14) -0.004(14) 0.010(17)
C2A 0.052(17) 0.016(11) 0.054(15) -0.001(10) 0.027(13) 0.011(11)
C3A 0.037(13) 0.062(13) 0.017(8) -0.009(9) -0.011(8) -0.010(10)
C4A 0.037(13) 0.062(13) 0.017(8) -0.009(9) -0.011(8) -0.010(10)
C5A 0.10(3) 0.031(15) 0.06(2) 0.005(14) -0.004(18) -0.031(17)
C6A 0.042(16) 0.044(15) 0.023(11) -0.014(11) 0.015(11) 0.007(12)
C7A 0.048(18) 0.042(15) 0.054(16) -0.002(12) -0.007(13) 0.025(13)
C8A 0.039(16) 0.072(17) 0.075(18) -0.014(15) 0.022(14) -0.001(13)
C9A 0.039(16) 0.072(17) 0.075(18) -0.014(15) 0.022(14) -0.001(13)
C10A 0.06(2) 0.044(17) 0.08(2) -0.008(16) -0.028(17) 0.022(16)
C11A 0.026(19) 0.06(2) 0.042(19) 0.025(18) 0.008(14) 0.02(2)
N1 0.022(9) 0.028(9) 0.053(11) -0.013(8) -0.010(7) -0.014(7)
N2 0.022(9) 0.028(9) 0.053(11) -0.013(8) -0.010(7) -0.014(7)
N3 0.040(12) 0.062(15) 0.039(11) -0.004(9) 0.006(9) -0.001(10)
N4 0.040(12) 0.062(15) 0.039(11) -0.004(9) 0.006(9) -0.001(10)
N1A 0.022(9) 0.028(9) 0.053(11) -0.013(8) -0.010(7) -0.014(7)
N2A 0.022(9) 0.028(9) 0.053(11) -0.013(8) -0.010(7) -0.014(7)
N3A 0.040(12) 0.062(15) 0.039(11) -0.004(9) 0.006(9) -0.001(10)
N4A 0.040(12) 0.062(15) 0.039(11) -0.004(9) 0.006(9) -0.001(10)
C101 0.027(10) 0.033(9) 0.032(6) -0.006(7) -0.008(6) -0.015(7)
C102 0.027(10) 0.033(9) 0.032(6) -0.006(7) -0.008(6) -0.015(7)
C103 0.027(10) 0.033(9) 0.032(6) -0.006(7) -0.008(6) -0.015(7)
O101 0.053(6) 0.048(9) 0.063(6) -0.007(8) -0.005(5) 0.000(8)
O102 0.053(6) 0.048(9) 0.063(6) -0.007(8) -0.005(5) 0.000(8)
O103 0.053(6) 0.048(9) 0.063(6) -0.007(8) -0.005(5) 0.000(8)
C111 0.027(10) 0.033(9) 0.032(6) -0.006(7) -0.008(6) -0.015(7)
C112 0.027(10) 0.033(9) 0.032(6) -0.006(7) -0.008(6) -0.015(7)
C113 0.027(10) 0.033(9) 0.032(6) -0.006(7) -0.008(6) -0.015(7)
O111 0.053(6) 0.048(9) 0.063(6) -0.007(8) -0.005(5) 0.000(8)
O112 0.053(6) 0.048(9) 0.063(6) -0.007(8) -0.005(5) 0.000(8)
O113 0.053(6) 0.048(9) 0.063(6) -0.007(8) -0.005(5) 0.000(8)
C401 0.049(14) 0.044(11) 0.055(12) -0.004(9) 0.005(10) 0.004(9)
C402 0.050(12) 0.035(10) 0.039(10) 0.004(8) -0.010(8) -0.003(8)
C404 0.051(14) 0.059(12) 0.046(11) -0.005(9) 0.011(10) -0.002(10)
C403 0.033(11) 0.024(9) 0.083(14) -0.018(10) -0.001(10) -0.008(8)
C202 0.056(12) 0.025(8) 0.047(11) 0.010(8) 0.004(9) 0.015(8)
C201 0.078(16) 0.053(12) 0.028(9) -0.010(8) 0.002(9) 0.015(11)
C204 0.11(2) 0.056(13) 0.023(9) -0.002(9) 0.001(11) -0.010(13)
C203 0.050(13) 0.062(13) 0.050(11) 0.016(10) 0.021(9) -0.011(10)
C302 0.048(12) 0.060(12) 0.040(11) 0.011(9) 0.013(9) 0.000(10)
C301 0.041(11) 0.035(10) 0.043(10) 0.003(8) 0.011(8) 0.007(8)
C303 0.052(14) 0.065(14) 0.048(11) -0.013(10) -0.011(10) 0.009(11)
O401 0.047(9) 0.096(11) 0.039(7) -0.012(7) 0.009(6) -0.012(8)
O402 0.071(10) 0.054(9) 0.052(8) -0.004(7) 0.002(7) 0.013(7)
O404 0.049(10) 0.139(16) 0.068(10) 0.026(10) -0.004(8) -0.018(10)
O403 0.081(11) 0.033(7) 0.067(9) 0.016(7) -0.009(7) -0.006(7)
O202 0.126(14) 0.062(9) 0.039(8) -0.010(7) 0.021(8) 0.021(9)
O201 0.065(11) 0.078(11) 0.075(10) -0.010(8) 0.001(8) 0.022(9)
O204 0.066(10) 0.048(8) 0.062(9) -0.003(7) -0.029(8) 0.001(7)
O203 0.074(11) 0.070(10) 0.072(10) -0.008(8) 0.042(9) -0.020(8)
O302 0.085(11) 0.057(9) 0.048(8) 0.011(7) 0.009(7) -0.016(8)
O301 0.057(9) 0.047(8) 0.069(9) -0.025(7) -0.006(7) -0.018(7)
O303 0.055(9) 0.070(10) 0.056(8) -0.012(7) -0.006(7) 0.020(7)
Ru4 0.0352(8) 0.0387(8) 0.0352(7) 0.0005(6) 0.0016(6) -0.0019(6)
Ru2 0.0509(9) 0.0318(7) 0.0374(7) 0.0006(6) 0.0026(6) 0.0010(6)
Ru3 0.0406(8) 0.0311(7) 0.0378(7) -0.0007(5) 0.0001(6) -0.0006(6)
_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_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ru1 C101 1.78(4) . ?
Ru1 C103 1.91(4) . ?
Ru1 C102 1.93(4) . ?
Ru1 C1 2.07(3) . ?
Ru1 C11 2.08(4) . ?
Ru1 C6 2.18(3) . ?
Ru1A C111 1.83(3) . ?
Ru1A C113 1.97(4) . ?
Ru1A C11A 1.99(4) . ?
Ru1A C112 2.02(5) . ?
Ru1A C1A 2.06(4) . ?
Ru1A C6A 2.17(4) . ?
C1 N2 1.361(19) . ?
C1 N1 1.367(19) . ?
C2 N1 1.451(18) . ?
C3 C4 1.33(2) . ?
C3 N1 1.370(19) . ?
C4 N2 1.364(19) . ?
C5 N2 1.48(6) . ?
C5 C6 1.55(5) . ?
C6 C7 1.55(5) . ?
C7 N3 1.43(5) . ?
C8 C9 1.34(2) . ?
C8 N3 1.37(2) . ?
C9 N4 1.37(2) . ?
C10 N4 1.44(2) . ?
C11 N3 1.365(19) . ?
C11 N4 1.37(2) . ?
C1A N1A 1.36(2) . ?
C1A N2A 1.38(2) . ?
C2A N1A 1.453(19) . ?
C3A C4A 1.35(2) . ?
C3A N1A 1.362(19) . ?
C4A N2A 1.370(19) . ?
C5A C6A 1.48(6) . ?
C5A N2A 1.53(5) . ?
C6A C7A 1.57(5) . ?
C7A N3A 1.46(5) . ?
C8A C9A 1.34(2) . ?
C8A N3A 1.37(2) . ?
C9A N4A 1.381(19) . ?
C10A N4A 1.47(2) . ?
C11A N3A 1.36(2) . ?
C11A N4A 1.38(2) . ?
C101 O101 1.22(6) . ?
C102 O102 1.17(4) . ?
C103 O103 1.14(4) . ?
C111 O111 1.18(2) . ?
C112 O112 1.10(6) . ?
C113 O113 1.12(4) . ?
C401 O401 1.17(2) . ?
C401 Ru4 1.88(2) . ?
C402 O402 1.14(2) . ?
C402 Ru4 1.917(19) . ?
C404 O404 1.15(2) . ?
C404 Ru4 1.91(2) . ?
C403 O403 1.15(2) . ?
C403 Ru4 1.92(2) . ?
C202 O202 1.15(2) . ?
C202 Ru2 1.891(19) . ?
C201 O201 1.16(2) . ?
C201 Ru2 1.94(2) . ?
C204 O204 1.17(3) . ?
C204 Ru2 2.08(3) . ?
C204 Ru3 2.10(2) . ?
C203 O203 1.15(2) . ?
C203 Ru2 1.871(19) . ?
C302 O302 1.12(2) . ?
C302 Ru3 1.909(19) . ?
C301 O301 1.13(2) . ?
C301 Ru3 1.97(2) . ?
C303 O303 1.15(2) . ?
C303 Ru3 1.90(2) . ?
Ru4 Ru3 2.8439(18) . ?
Ru4 Ru2 2.8541(18) . ?
Ru2 Ru3 2.8101(18) . ?
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
C101 Ru1 C103 86.2(15) . . ?
C101 Ru1 C102 80.7(18) . . ?
C103 Ru1 C102 91.9(17) . . ?
C101 Ru1 C1 98.3(19) . . ?
C103 Ru1 C1 95.9(14) . . ?
C102 Ru1 C1 172.0(16) . . ?
C101 Ru1 C11 175(3) . . ?
C103 Ru1 C11 95.5(13) . . ?
C102 Ru1 C11 94(2) . . ?
C1 Ru1 C11 87(2) . . ?
C101 Ru1 C6 98.6(15) . . ?
C103 Ru1 C6 173.6(13) . . ?
C102 Ru1 C6 93.1(15) . . ?
C1 Ru1 C6 79.2(12) . . ?
C11 Ru1 C6 80.2(13) . . ?
C111 Ru1A C113 90.9(18) . . ?
C111 Ru1A C11A 167.7(19) . . ?
C113 Ru1A C11A 98.5(15) . . ?
C111 Ru1A C112 104.2(18) . . ?
C113 Ru1A C112 89.5(15) . . ?
C11A Ru1A C112 84(2) . . ?
C111 Ru1A C1A 88(3) . . ?
C113 Ru1A C1A 95.4(14) . . ?
C11A Ru1A C1A 84(3) . . ?
C112 Ru1A C1A 167(3) . . ?
C111 Ru1A C6A 90.9(18) . . ?
C113 Ru1A C6A 171.8(15) . . ?
C11A Ru1A C6A 78.8(14) . . ?
C112 Ru1A C6A 97.8(17) . . ?
C1A Ru1A C6A 76.7(15) . . ?
N2 C1 N1 102(3) . . ?
N2 C1 Ru1 118(3) . . ?
N1 C1 Ru1 139(3) . . ?
C4 C3 N1 106(3) . . ?
C3 C4 N2 107(4) . . ?
N2 C5 C6 111(3) . . ?
C5 C6 C7 114(3) . . ?
C5 C6 Ru1 107(2) . . ?
C7 C6 Ru1 109(2) . . ?
N3 C7 C6 110(3) . . ?
C9 C8 N3 107(4) . . ?
C8 C9 N4 108(4) . . ?
N3 C11 N4 105(3) . . ?
N3 C11 Ru1 114(3) . . ?
N4 C11 Ru1 140(3) . . ?
N1A C1A N2A 102(3) . . ?
N1A C1A Ru1A 137(3) . . ?
N2A C1A Ru1A 121(3) . . ?
C4A C3A N1A 109(3) . . ?
C3A C4A N2A 104(3) . . ?
C6A C5A N2A 111(3) . . ?
C5A C6A C7A 113(3) . . ?
C5A C6A Ru1A 111(3) . . ?
C7A C6A Ru1A 109(2) . . ?
N3A C7A C6A 110(3) . . ?
C9A C8A N3A 107(5) . . ?
C8A C9A N4A 106(5) . . ?
N3A C11A N4A 101(3) . . ?
N3A C11A Ru1A 122(3) . . ?
N4A C11A Ru1A 138(3) . . ?
C1 N1 C3 112(3) . . ?
C1 N1 C2 127(3) . . ?
C3 N1 C2 121(3) . . ?
C1 N2 C4 112(3) . . ?
C1 N2 C5 115(3) . . ?
C4 N2 C5 133(3) . . ?
C11 N3 C8 110(4) . . ?
C11 N3 C7 121(4) . . ?
C8 N3 C7 127(3) . . ?
C11 N4 C9 109(3) . . ?
C11 N4 C10 121(3) . . ?
C9 N4 C10 130(4) . . ?
C1A N1A C3A 111(3) . . ?
C1A N1A C2A 127(3) . . ?
C3A N1A C2A 122(3) . . ?
C4A N2A C1A 113(3) . . ?
C4A N2A C5A 133(3) . . ?
C1A N2A C5A 113(3) . . ?
C11A N3A C8A 114(4) . . ?
C11A N3A C7A 116(3) . . ?
C8A N3A C7A 130(4) . . ?
C11A N4A C9A 113(4) . . ?
C11A N4A C10A 125(4) . . ?
C9A N4A C10A 122(4) . . ?
O101 C101 Ru1 169(4) . . ?
O102 C102 Ru1 170(3) . . ?
O103 C103 Ru1 175(3) . . ?
O111 C111 Ru1A 166(4) . . ?
O112 C112 Ru1A 169(5) . . ?
O113 C113 Ru1A 174(3) . . ?
O401 C401 Ru4 173.9(16) . . ?
O402 C402 Ru4 177.2(16) . . ?
O404 C404 Ru4 176.5(18) . . ?
O403 C403 Ru4 177.9(16) . . ?
O202 C202 Ru2 177.7(17) . . ?
O201 C201 Ru2 170.6(15) . . ?
O204 C204 Ru2 136.7(17) . . ?
O204 C204 Ru3 138.2(18) . . ?
Ru2 C204 Ru3 84.5(10) . . ?
O203 C203 Ru2 177.1(18) . . ?
O302 C302 Ru3 178.0(18) . . ?
O301 C301 Ru3 178.5(17) . . ?
O303 C303 Ru3 179.1(18) . . ?
C401 Ru4 C404 168.1(8) . . ?
C401 Ru4 C402 95.0(8) . . ?
C404 Ru4 C402 93.7(8) . . ?
C401 Ru4 C403 93.7(8) . . ?
C404 Ru4 C403 91.9(8) . . ?
C402 Ru4 C403 105.3(7) . . ?
C401 Ru4 Ru3 84.5(6) . . ?
C404 Ru4 Ru3 86.7(6) . . ?
C402 Ru4 Ru3 93.9(5) . . ?
C403 Ru4 Ru3 160.8(5) . . ?
C401 Ru4 Ru2 80.5(6) . . ?
C404 Ru4 Ru2 88.1(6) . . ?
C402 Ru4 Ru2 152.8(5) . . ?
C403 Ru4 Ru2 101.8(5) . . ?
Ru3 Ru4 Ru2 59.10(4) . . ?
C203 Ru2 C202 95.3(8) . . ?
C203 Ru2 C201 100.8(9) . . ?
C202 Ru2 C201 96.1(7) . . ?
C203 Ru2 C204 91.4(9) . . ?
C202 Ru2 C204 90.3(7) . . ?
C201 Ru2 C204 165.7(9) . . ?
C203 Ru2 Ru3 130.0(6) . . ?
C202 Ru2 Ru3 109.9(5) . . ?
C201 Ru2 Ru3 117.7(6) . . ?
C204 Ru2 Ru3 48.0(6) . . ?
C203 Ru2 Ru4 87.3(6) . . ?
C202 Ru2 Ru4 167.9(5) . . ?
C201 Ru2 Ru4 94.9(5) . . ?
C204 Ru2 Ru4 77.9(5) . . ?
Ru3 Ru2 Ru4 60.27(4) . . ?
C303 Ru3 C302 95.8(8) . . ?
C303 Ru3 C301 96.5(8) . . ?
C302 Ru3 C301 98.5(8) . . ?
C303 Ru3 C204 94.6(9) . . ?
C302 Ru3 C204 89.2(8) . . ?
C301 Ru3 C204 165.8(9) . . ?
C303 Ru3 Ru2 131.7(7) . . ?
C302 Ru3 Ru2 109.7(6) . . ?
C301 Ru3 Ru2 118.2(5) . . ?
C204 Ru3 Ru2 47.6(7) . . ?
C303 Ru3 Ru4 86.2(6) . . ?
C302 Ru3 Ru4 167.1(6) . . ?
C301 Ru3 Ru4 93.8(5) . . ?
C204 Ru3 Ru4 77.9(5) . . ?
Ru2 Ru3 Ru4 60.63(4) . . ?
_diffrn_measured_fraction_theta_max 0.964
_diffrn_reflns_theta_full        62.51
_diffrn_measured_fraction_theta_full 0.964
_refine_diff_density_max         1.388
_refine_diff_density_min         -1.297
_refine_diff_density_rms         0.230