# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2011


data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

loop_
_publ_author_name
_publ_author_address

L.Villalobos
; Department of Chemistry
Purdue University
W. Lafayette
IN 47907
USA
;
T.Ren
; Department of Chemistry
Purdue University
W. Lafayette
IN 47907
USA
;
P.E.Fanwick
; Department of Chemistry
Purdue University
W. Lafayette
IN 47907
USA
;
_publ_contact_author_address     
; Department of Chemistry
Purdue University
560 Oval Dr.
W. Lafayette
IN 47907-2084
USA
;
_publ_contact_author_email       pfanwick@purdue.edu
_publ_contact_author_fax         1(765)4940239
_publ_contact_author_phone       1(765)4944572

_publ_section_title              
;
Diruthenium(II,III)
tetramidates as a new class of oxygenation catalysts
;

# Attachment '- Cif-all.cif'

#============================================================================

#TrackingRef '- Cif-all.cif'

#============================================================================

_audit_creation_date             12-06-09
_audit_creation_method           'SHELXL and local programs'
_audit_update_record             
; ?
;

data_LVC1
_database_code_depnum_ccdc_archive 'CCDC 827246'
#TrackingRef '- Cif-all.cif'

# 5. CRYSTAL DATA

_chemical_compound_source        ?
_exptl_crystal_description       needle
_exptl_crystal_colour_primary    brown
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_chemical_name_systematic        
; ?
;
_chemical_formula_sum            'C18 H40 Cl1 N4 O6 Ru2'
_chemical_formula_moiety         'C16 H32 Cl1 N4 O4 Ru2,2(C1 H4 O1)'
_chemical_formula_structural     ?
_chemical_formula_weight         646.14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'

_cell_length_a                   11.6827(8)
_cell_length_b                   9.4837(5)
_cell_length_c                   12.5641(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.481(7)
_cell_angle_gamma                90.00
_cell_volume                     1364.19(15)
_cell_measurement_reflns_used    3440
_cell_measurement_theta_min      3
_cell_measurement_theta_max      72
_cell_formula_units_z            2
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'

loop_
_atom_type_symbol
_atom_type_radius_bond
Ru 1.25
Cl 0.99
O 0.73
N 0.75
C 0.77
H 0.32

_diffrn_radiation_type           CU-K\a
_diffrn_radiation_wavelength     1.54184
_exptl_absorpt_coefficient_mu    10.423
_cell_measurement_temperature    150(2)
_exptl_crystal_F_000             658

# 6. DATA COLLECTION

_diffrn_ambient__temperature     150(2)
_diffrn_measurement_device_type  Rigaku_Rapid_II
_diffrn_radiation_monochromator  'confocal optics'
_diffrn_measurement_method       \w
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt__process_details  'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  0.5322
_exptl_absorpt_correction_T_max  0.5938
_diffrn_reflns_number            5761
_diffrn_measured_fraction_theta_max 0.8740
_diffrn_reflns_theta_full        72.2
_diffrn_measured_fraction_theta_full 0.8740
_reflns_number_total             2357
_reflns_number_gt                2262
_reflns_threshold_expression     >2.0\s(I)
_diffrn_reflns_av_R_equivalents  0.057
_diffrn_reflns_theta_min         3.59
_diffrn_reflns_theta_max         72.15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_max       15
_diffrn_special_details          'mosaicity from Denzo/Scalepack is 1.13'
_diffrn_standards_number         0
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        ?

# 7. REFINEMENT DATA

_refine_special_details          
;
Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^
or flagged by the user for potential systematic errors. Weighted R-factors
wR and all goodnesses 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 observed criterion
of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs 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_R_factor_all          0.049
_refine_ls_R_factor_gt           0.047
_refine_ls_wR_factor_ref         0.138
_refine_ls_wR_factor_gt          0.135
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_reflns         2357
_refine_ls_number_parameters     138
_refine_ls_number_restraints     0
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_weighting_scheme      'calc '
_refine_ls_weighting_details     
'1/[\s^2^(Fo^2^)+(0.0795P)^2^+3.2703P] where P=(Fo^2^+2Fc^2^)/3 '

_refine_ls_shift/su_max          0.001
_refine_diff_density_max         1.05
_refine_diff_density_min         -1.09
_refine_ls_extinction_method     none
_atom_type_scat_source           
'International Tables for Crystallography (Vol C)'

# 8. COMPUTING DATA

_computing_data_collection       'CrystalClear(Rigaku, 2001)'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1996)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1996)'
_computing_structure_solution    
;
Direct methods (SIR2004, Burla et al., 2005)
;
_computing_structure_refinement  'SHELX97 (Sheldrick, 2008)'
_computing_molecular_graphics    
;
ORTEP (Johnson, 1976)
PLATON (Spek, 1997)
;
_computing_publication_material  'SHELX97(Sheldrick, 2008) and local programs'

# 9. ATOMIC COORDINATES AND THERMAL PARAMETERS

loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group

Ru1 0.00222(3) 0.56499(4) 0.07765(3) 0.02903(19) Uani 1 1 d . . .
Cl1 0.0000 0.70949(17) 0.2500 0.0330(4) Uani 1 2 d S . .
O1 0.1605(3) 0.4782(4) 0.1513(3) 0.0336(7) Uani 1 1 d . . .
O2 0.0912(3) 0.7251(4) 0.0203(3) 0.0348(7) Uani 1 1 d . . .
O91 0.3003(5) 0.6800(7) 0.3208(4) 0.0737(15) Uani 1 1 d . . .
N1 -0.1536(4) 0.6476(5) 0.0027(3) 0.0365(9) Uani 1 1 d . . .
N2 -0.0829(4) 0.4026(5) 0.1323(3) 0.0331(9) Uani 1 1 d . . .
C11 0.2081(4) 0.3902(6) 0.0924(4) 0.0351(10) Uani 1 1 d . . .
C12 0.3306(5) 0.3428(6) 0.1410(5) 0.0414(12) Uiso 1 1 d . . .
C13 0.4161(6) 0.4411(6) 0.1001(6) 0.0542(16) Uiso 1 1 d . . .
C14 0.3534(6) 0.1889(7) 0.1159(6) 0.0565(16) Uiso 1 1 d . . .
C21 0.1132(4) 0.7116(6) -0.0748(4) 0.0343(10) Uani 1 1 d . . .
C22 0.1735(5) 0.8328(6) -0.1184(4) 0.0394(11) Uani 1 1 d . . .
C23 0.3027(5) 0.8342(7) -0.0641(6) 0.0551(16) Uani 1 1 d . . .
C24 0.1144(6) 0.9720(7) -0.1030(6) 0.0559(16) Uani 1 1 d . . .
C91 0.3284(9) 0.7903(10) 0.2581(7) 0.087(3) Uani 1 1 d . . .
H1 -0.186(8) 0.691(9) 0.041(8) 0.087 Uiso 1 1 d . . .
H2 -0.097(9) 0.401(11) 0.187(9) 0.104 Uiso 1 1 d . . .
H12 0.3426 0.3534 0.2217 0.050 Uiso 1 1 calc R . .
H22 0.1678 0.8175 -0.1981 0.047 Uiso 1 1 calc R . .
H91 0.2664 0.6162 0.2799 0.111 Uiso 1 1 calc R . .
H13A 0.4961 0.4182 0.1366 0.081 Uiso 1 1 calc R . .
H13B 0.3987 0.5391 0.1159 0.081 Uiso 1 1 calc R . .
H13C 0.4085 0.4291 0.0215 0.081 Uiso 1 1 calc R . .
H14A 0.2948 0.1288 0.1392 0.085 Uiso 1 1 calc R . .
H14B 0.4315 0.1616 0.1547 0.085 Uiso 1 1 calc R . .
H14C 0.3486 0.1778 0.0375 0.085 Uiso 1 1 calc R . .
H23A 0.3103 0.8506 0.0141 0.083 Uiso 1 1 calc R . .
H23B 0.3427 0.9098 -0.0955 0.083 Uiso 1 1 calc R . .
H23C 0.3381 0.7433 -0.0758 0.083 Uiso 1 1 calc R . .
H24A 0.0325 0.9684 -0.1404 0.084 Uiso 1 1 calc R . .
H24B 0.1542 1.0487 -0.1333 0.084 Uiso 1 1 calc R . .
H24C 0.1186 0.9887 -0.0254 0.084 Uiso 1 1 calc R . .
H91A 0.3772 0.8588 0.3051 0.130 Uiso 1 1 calc R . .
H91B 0.2566 0.8364 0.2205 0.130 Uiso 1 1 calc R . .
H91C 0.3714 0.7536 0.2046 0.130 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_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Ru1 0.0288(3) 0.0370(3) 0.0203(3) -0.00075(12) 0.00240(17) -0.00103(12)
Cl1 0.0406(8) 0.0359(8) 0.0219(7) 0.0000 0.0050(6) 0.0000
O1 0.0310(17) 0.0461(18) 0.0223(17) 0.0000(15) 0.0018(13) -0.0012(15)
O2 0.0412(19) 0.0397(18) 0.0234(16) -0.0052(15) 0.0061(14) -0.0019(14)
O91 0.060(3) 0.113(5) 0.046(3) -0.023(3) 0.006(2) 0.000(3)
N1 0.039(2) 0.044(2) 0.025(2) 0.0037(18) 0.0021(17) -0.0017(18)
N2 0.036(2) 0.040(2) 0.023(2) -0.0016(18) 0.0070(17) 0.0039(18)
C11 0.038(3) 0.044(3) 0.021(2) 0.000(2) 0.0025(19) 0.004(2)
C21 0.029(2) 0.046(3) 0.026(2) 0.002(2) 0.0010(18) 0.000(2)
C22 0.043(3) 0.046(3) 0.028(2) -0.003(2) 0.006(2) 0.005(2)
C23 0.038(3) 0.061(4) 0.067(4) -0.008(3) 0.011(3) 0.005(3)
C24 0.064(4) 0.043(3) 0.064(4) 0.002(3) 0.019(3) 0.012(3)
C91 0.108(7) 0.090(6) 0.075(6) -0.027(5) 0.051(5) -0.014(5)

# 10. MOLECULAR GEOMETRY

_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_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ru1 N2 2.026(4) . . ?
Ru1 N1 2.033(4) . . ?
Ru1 O2 2.050(3) . . ?
Ru1 O1 2.067(3) . . ?
Ru1 Ru1 2.2997(7) . 3_565 ?
Ru1 Cl1 2.5671(9) . . ?
Cl1 Ru1 2.5672(9) . 2_555 ?
O1 C11 1.310(7) . . ?
O2 C21 1.277(6) . . ?
O91 C91 1.387(10) . . ?
O91 H91 0.8400 . . ?
N1 C11 1.288(7) . 3_565 ?
N1 H1 0.79(9) . . ?
N2 C21 1.312(7) . 3_565 ?
N2 H2 0.74(11) . . ?
C11 N1 1.288(7) . 3_565 ?
C11 C12 1.509(7) . . ?
C12 C14 1.528(8) . . ?
C12 C13 1.528(8) . . ?
C12 H12 1.0000 . . ?
C13 H13A 0.9800 . . ?
C13 H13B 0.9800 . . ?
C13 H13C 0.9800 . . ?
C14 H14A 0.9800 . . ?
C14 H14B 0.9800 . . ?
C14 H14C 0.9800 . . ?
C21 N2 1.312(7) . 3_565 ?
C21 C22 1.507(7) . . ?
C22 C24 1.520(8) . . ?
C22 C23 1.528(8) . . ?
C22 H22 1.0000 . . ?
C23 H23A 0.9800 . . ?
C23 H23B 0.9800 . . ?
C23 H23C 0.9800 . . ?
C24 H24A 0.9800 . . ?
C24 H24B 0.9800 . . ?
C24 H24C 0.9800 . . ?
C91 H91A 0.9800 . . ?
C91 H91B 0.9800 . . ?
C91 H91C 0.9800 . . ?

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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Ru1 N1 89.73(18) . . . ?
N2 Ru1 O2 178.30(16) . . . ?
N1 Ru1 O2 91.26(17) . . . ?
N2 Ru1 O1 90.07(16) . . . ?
N1 Ru1 O1 178.85(15) . . . ?
O2 Ru1 O1 88.91(14) . . . ?
N2 Ru1 Ru1 87.16(13) . . 3_565 ?
N1 Ru1 Ru1 86.93(12) . . 3_565 ?
O2 Ru1 Ru1 91.51(9) . . 3_565 ?
O1 Ru1 Ru1 91.93(10) . . 3_565 ?
N2 Ru1 Cl1 91.82(13) . . . ?
N1 Ru1 Cl1 91.53(12) . . . ?
O2 Ru1 Cl1 89.54(10) . . . ?
O1 Ru1 Cl1 89.60(10) . . . ?
Ru1 Ru1 Cl1 178.16(2) 3_565 . . ?
Ru1 Cl1 Ru1 115.47(6) . . 2_555 ?
C11 O1 Ru1 116.3(3) . . . ?
C21 O2 Ru1 117.7(3) . . . ?
C91 O91 H91 109.50 . . . ?
C11 N1 Ru1 123.7(4) 3_565 . . ?
C11 N1 H1 121(7) 3_565 . . ?
Ru1 N1 H1 114(7) . . . ?
C21 N2 Ru1 122.5(4) 3_565 . . ?
C21 N2 H2 114(8) 3_565 . . ?
Ru1 N2 H2 123(8) . . . ?
N1 C11 O1 121.0(5) 3_565 . . ?
N1 C11 C12 123.1(5) 3_565 . . ?
O1 C11 C12 115.9(4) . . . ?
C11 C12 C14 113.0(5) . . . ?
C11 C12 C13 108.3(5) . . . ?
C14 C12 C13 111.1(5) . . . ?
C11 C12 H12 108.10 . . . ?
C14 C12 H12 108.10 . . . ?
C13 C12 H12 108.10 . . . ?
C12 C13 H13A 109.50 . . . ?
C12 C13 H13B 109.50 . . . ?
H13A C13 H13B 109.50 . . . ?
C12 C13 H13C 109.50 . . . ?
H13A C13 H13C 109.50 . . . ?
H13B C13 H13C 109.50 . . . ?
C12 C14 H14A 109.50 . . . ?
C12 C14 H14B 109.50 . . . ?
H14A C14 H14B 109.50 . . . ?
C12 C14 H14C 109.50 . . . ?
H14A C14 H14C 109.50 . . . ?
H14B C14 H14C 109.50 . . . ?
O2 C21 N2 121.0(5) . . 3_565 ?
O2 C21 C22 117.4(4) . . . ?
N2 C21 C22 121.6(4) 3_565 . . ?
C21 C22 C24 111.0(5) . . . ?
C21 C22 C23 109.6(5) . . . ?
C24 C22 C23 111.6(5) . . . ?
C21 C22 H22 108.10 . . . ?
C24 C22 H22 108.10 . . . ?
C23 C22 H22 108.10 . . . ?
C22 C23 H23A 109.50 . . . ?
C22 C23 H23B 109.50 . . . ?
H23A C23 H23B 109.50 . . . ?
C22 C23 H23C 109.50 . . . ?
H23A C23 H23C 109.50 . . . ?
H23B C23 H23C 109.50 . . . ?
C22 C24 H24A 109.50 . . . ?
C22 C24 H24B 109.50 . . . ?
H24A C24 H24B 109.50 . . . ?
C22 C24 H24C 109.50 . . . ?
H24A C24 H24C 109.50 . . . ?
H24B C24 H24C 109.50 . . . ?
O91 C91 H91A 109.50 . . . ?
O91 C91 H91B 109.50 . . . ?
H91A C91 H91B 109.50 . . . ?
O91 C91 H91C 109.50 . . . ?
H91A C91 H91C 109.50 . . . ?
H91B C91 H91C 109.50 . . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 Ru1 Cl1 Ru1 28.43(12) . . . 2 ?
N1 Ru1 Cl1 Ru1 118.21(13) . . . 2 ?
O2 Ru1 Cl1 Ru1 -150.55(10) . . . 2 ?
O1 Ru1 Cl1 Ru1 -61.63(10) . . . 2 ?
Ru1 Ru1 Cl1 Ru1 84.7(12) 3_565 . . 2 ?
N2 Ru1 O1 C11 89.9(4) . . . . ?
N1 Ru1 O1 C11 10(8) . . . . ?
O2 Ru1 O1 C11 -88.7(4) . . . . ?
Ru1 Ru1 O1 C11 2.8(4) 3_565 . . . ?
Cl1 Ru1 O1 C11 -178.3(4) . . . . ?
N2 Ru1 O2 C21 40(5) . . . . ?
N1 Ru1 O2 C21 -85.0(4) . . . . ?
O1 Ru1 O2 C21 93.9(4) . . . . ?
Ru1 Ru1 O2 C21 2.0(3) 3_565 . . . ?
Cl1 Ru1 O2 C21 -176.5(3) . . . . ?
N2 Ru1 N1 C11 -84.5(5) . . . 3_565 ?
O2 Ru1 N1 C11 94.1(5) . . . 3_565 ?
O1 Ru1 N1 C11 -4(9) . . . 3_565 ?
Ru1 Ru1 N1 C11 2.7(4) 3_565 . . 3_565 ?
Cl1 Ru1 N1 C11 -176.3(4) . . . 3_565 ?
N1 Ru1 N2 C21 86.4(4) . . . 3_565 ?
O2 Ru1 N2 C21 -39(5) . . . 3_565 ?
O1 Ru1 N2 C21 -92.5(4) . . . 3_565 ?
Ru1 Ru1 N2 C21 -0.6(4) 3_565 . . 3_565 ?
Cl1 Ru1 N2 C21 177.9(4) . . . 3_565 ?
Ru1 O1 C11 N1 -5.4(7) . . . 3_565 ?
Ru1 O1 C11 C12 172.0(3) . . . . ?
N1 C11 C12 C14 -39.2(8) 3_565 . . . ?
O1 C11 C12 C14 143.5(5) . . . . ?
N1 C11 C12 C13 84.4(7) 3_565 . . . ?
O1 C11 C12 C13 -93.0(6) . . . . ?
Ru1 O2 C21 N2 -2.0(6) . . . 3_565 ?
Ru1 O2 C21 C22 177.1(3) . . . . ?
O2 C21 C22 C24 -48.3(6) . . . . ?
N2 C21 C22 C24 130.9(6) 3_565 . . . ?
O2 C21 C22 C23 75.5(6) . . . . ?
N2 C21 C22 C23 -105.3(6) 3_565 . . . ?
#===END

#============================================================================

#TrackingRef '- Cif-all.cif'

#============================================================================

_audit_creation_date             24-07-09
_audit_creation_method           'SHELXL and local programs'
_audit_update_record             
; ?
;

data_LVC2
_database_code_depnum_ccdc_archive 'CCDC 827247'
#TrackingRef '- Cif-all.cif'

# 5. CRYSTAL DATA

_chemical_compound_source        ?
_exptl_crystal_description       needle
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_chemical_name_systematic        
; ?
;
_chemical_formula_sum            'C12 H20 Cl1 N4 O4 Ru2'
_chemical_formula_moiety         'C12 H20 Cl1 N4 O4 Ru2'
_chemical_formula_structural     ?
_chemical_formula_weight         521.91
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
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                   10.4362(12)
_cell_length_b                   12.8638(13)
_cell_length_c                   12.6574(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.192(4)
_cell_angle_gamma                90.00
_cell_volume                     1696.6(4)
_cell_measurement_reflns_used    1474
_cell_measurement_theta_min      3
_cell_measurement_theta_max      72
_cell_formula_units_z            4
_exptl_crystal_density_diffrn    2.043
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'

loop_
_atom_type_symbol
_atom_type_radius_bond
Ru 1.25
Cl 0.99
O 0.73
N 0.75
C 0.77
H 0.32

_diffrn_radiation_type           CU-K\a
_diffrn_radiation_wavelength     1.54184
_exptl_absorpt_coefficient_mu    16.501
_cell_measurement_temperature    150(2)
_exptl_crystal_F_000             1028

# 6. DATA COLLECTION

_diffrn_ambient__temperature     150(2)
_diffrn_measurement_device_type  Rigaku_Rapid_II
_diffrn_radiation_monochromator  'confocal optics'
_diffrn_measurement_method       \w
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt__process_details  'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  0.7446
_exptl_absorpt_correction_T_max  0.8479
_diffrn_reflns_number            5703
_diffrn_measured_fraction_theta_max 0.8978
_diffrn_reflns_theta_full        72.1
_diffrn_measured_fraction_theta_full 0.8978
_reflns_number_total             1403
_reflns_number_gt                1233
_reflns_threshold_expression     >2.0\s(I)
_diffrn_reflns_av_R_equivalents  0.043
_diffrn_reflns_theta_min         3.50
_diffrn_reflns_theta_max         72.07
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_max       15
_diffrn_special_details          'mosaicity from Denzo/Scalepack is 1.18'
_diffrn_standards_number         0
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        ?

# 7. REFINEMENT DATA

_refine_special_details          
;
Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^
or flagged by the user for potential systematic errors. Weighted R-factors
wR and all goodnesses 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 observed criterion
of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs 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_R_factor_all          0.067
_refine_ls_R_factor_gt           0.061
_refine_ls_wR_factor_ref         0.188
_refine_ls_wR_factor_gt          0.182
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         1403
_refine_ls_number_parameters     116
_refine_ls_number_restraints     3
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_weighting_scheme      'calc '
_refine_ls_weighting_details     
'1/[\s^2^(Fo^2^)+(0.1193P)^2^+7.9255P] where P=(Fo^2^+2Fc^2^)/3 '

_refine_ls_shift/su_max          0.002
_refine_diff_density_max         0.97
_refine_diff_density_min         -1.26
_refine_ls_extinction_method     none
_atom_type_scat_source           
'International Tables for Crystallography (Vol C)'

# 8. COMPUTING DATA

_computing_data_collection       'CrystalClear(Rigaku, 2001)'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1996)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1996)'
_computing_structure_solution    
;
Direct methods (SIR2004, Burla et al., 2005)
;
_computing_structure_refinement  'SHELX97 (Sheldrick, 2008)'
_computing_molecular_graphics    
;
ORTEP (Johnson, 1976)
PLATON (Spek, 1997)
;
_computing_publication_material  'SHELX97(Sheldrick, 2008) and local programs'

# 9. ATOMIC COORDINATES AND THERMAL PARAMETERS

loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group

Ru1 0.50292(6) 0.04740(5) 0.07658(5) 0.0582(4) Uani 1 1 d . . .
Cl1 0.5000 0.1527(2) 0.2500 0.0664(8) Uani 1 2 d S . .
O1 0.6766(6) 0.1070(5) 0.0435(5) 0.0695(16) Uani 1 1 d . . .
O2 0.4156(7) 0.1687(5) -0.0018(5) 0.0702(16) Uani 1 1 d . . .
N1 0.3283(6) -0.0144(5) 0.1080(5) 0.0546(15) Uani 1 1 d . . .
N2 0.5939(7) -0.0742(6) 0.1514(5) 0.0569(16) Uani 1 1 d . . .
C11 0.7275(10) 0.0790(8) -0.0419(9) 0.075(3) Uani 1 1 d . . .
C12 0.8554(12) 0.1247(10) -0.0635(11) 0.093(3) Uani 1 1 d D . .
C13 0.931(3) 0.074(2) -0.134(3) 0.245(16) Uani 1 1 d D . .
C21 0.6162(9) -0.1567(7) 0.1003(8) 0.066(2) Uani 1 1 d . . .
C22 0.6885(16) -0.2448(10) 0.1569(12) 0.097(4) Uani 1 1 d D . .
C23A 0.643(4) -0.287(2) 0.246(2) 0.19(2) Uani 0.60(3) 1 d PD B 1
C23B 0.628(5) -0.338(3) 0.141(5) 0.25(6) Uani 0.40(3) 1 d PD B 2
H12A 0.8405 0.1964 -0.0901 0.112 Uiso 1 1 calc R . .
H12B 0.9057 0.1304 0.0049 0.112 Uiso 1 1 calc R . .
H13A 0.9867 0.0244 -0.0949 0.368 Uiso 1 1 calc R . .
H13B 0.9833 0.1253 -0.1690 0.368 Uiso 1 1 calc R . .
H13C 0.8756 0.0374 -0.1864 0.368 Uiso 1 1 calc R . .
H22A 0.6962 -0.3018 0.1051 0.117 Uiso 1 1 calc R A 1
H22B 0.7765 -0.2196 0.1754 0.117 Uiso 1 1 calc R A 1
H23A 0.5537 -0.3089 0.2320 0.285 Uiso 0.60(3) 1 calc PR B 1
H23B 0.6478 -0.2358 0.3032 0.285 Uiso 0.60(3) 1 calc PR B 1
H23C 0.6953 -0.3480 0.2674 0.285 Uiso 0.60(3) 1 calc PR B 1
H23D 0.6481 -0.3836 0.2024 0.378 Uiso 0.40(3) 1 calc PR B 2
H23E 0.6586 -0.3713 0.0773 0.378 Uiso 0.40(3) 1 calc PR B 2
H23F 0.5355 -0.3276 0.1328 0.378 Uiso 0.40(3) 1 calc PR B 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Ru1 0.0731(5) 0.0581(5) 0.0434(5) 0.0005(3) 0.0028(3) 0.0000(2)
Cl1 0.0875(19) 0.0619(16) 0.0492(15) 0.0000 -0.0008(14) 0.0000
O1 0.077(4) 0.070(4) 0.062(4) -0.016(3) 0.013(3) -0.007(3)
O2 0.094(4) 0.061(3) 0.056(4) 0.012(3) 0.004(3) 0.006(3)
N1 0.064(4) 0.052(3) 0.048(4) -0.009(3) 0.006(3) -0.001(3)
N2 0.079(4) 0.058(4) 0.034(3) 0.010(3) 0.001(3) 0.001(3)
C11 0.075(6) 0.062(5) 0.088(7) -0.004(5) 0.009(5) 0.013(5)
C12 0.088(7) 0.098(8) 0.095(8) -0.013(6) 0.015(6) -0.011(7)
C13 0.19(2) 0.17(2) 0.39(5) -0.03(2) 0.12(3) -0.03(3)
C21 0.072(5) 0.070(5) 0.056(5) 0.003(4) 0.007(4) 0.013(4)
C22 0.130(11) 0.079(7) 0.082(8) 0.030(7) -0.002(8) 0.008(6)
C23A 0.32(5) 0.16(3) 0.09(2) 0.13(3) 0.04(2) 0.032(19)
C23B 0.16(5) 0.48(16) 0.12(4) 0.15(8) 0.04(4) 0.04(7)

# 10. MOLECULAR GEOMETRY

_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_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ru1 O1 2.033(6) . . ?
Ru1 N2 2.035(7) . . ?
Ru1 O2 2.037(6) . . ?
Ru1 N1 2.048(6) . . ?
Ru1 Ru1 2.2880(12) . 5_655 ?
Ru1 Cl1 2.5811(17) . . ?
Cl1 Ru1 2.5811(17) . 2_655 ?
O1 C11 1.282(13) . . ?
O2 C21 1.281(11) . 5_655 ?
N1 C11 1.294(13) . 5_655 ?
N2 C21 1.271(12) . . ?
C11 N1 1.294(13) . 5_655 ?
C11 C12 1.498(15) . . ?
C12 C13 1.38(2) . . ?
C12 H12A 0.9900 . . ?
C12 H12B 0.9900 . . ?
C13 H13A 0.9800 . . ?
C13 H13B 0.9800 . . ?
C13 H13C 0.9800 . . ?
C21 O2 1.281(11) . 5_655 ?
C21 C22 1.519(16) . . ?
C22 C23A 1.36(2) . . ?
C22 C23B 1.37(3) . . ?
C22 H22A 0.9900 . . ?
C22 H22B 0.9900 . . ?
C23A H23A 0.9800 . . ?
C23A H23B 0.9800 . . ?
C23A H23C 0.9800 . . ?
C23B H23D 0.9800 . . ?
C23B H23E 0.9800 . . ?
C23B H23F 0.9800 . . ?

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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ru1 N2 89.3(3) . . . ?
O1 Ru1 O2 89.4(3) . . . ?
N2 Ru1 O2 178.3(2) . . . ?
O1 Ru1 N1 179.1(3) . . . ?
N2 Ru1 N1 90.5(3) . . . ?
O2 Ru1 N1 90.8(3) . . . ?
O1 Ru1 Ru1 90.47(18) . . 5_655 ?
N2 Ru1 Ru1 88.52(19) . . 5_655 ?
O2 Ru1 Ru1 90.33(18) . . 5_655 ?
N1 Ru1 Ru1 88.63(19) . . 5_655 ?
O1 Ru1 Cl1 91.75(18) . . . ?
N2 Ru1 Cl1 92.02(19) . . . ?
O2 Ru1 Cl1 89.18(18) . . . ?
N1 Ru1 Cl1 89.15(19) . . . ?
Ru1 Ru1 Cl1 177.73(5) 5_655 . . ?
Ru1 Cl1 Ru1 116.68(11) . . 2_655 ?
C11 O1 Ru1 118.9(6) . . . ?
C21 O2 Ru1 117.8(6) 5_655 . . ?
C11 N1 Ru1 119.8(6) 5_655 . . ?
C21 N2 Ru1 119.9(6) . . . ?
O1 C11 N1 122.2(9) . . 5_655 ?
O1 C11 C12 117.4(10) . . . ?
N1 C11 C12 120.4(10) 5_655 . . ?
C13 C12 C11 118.6(16) . . . ?
C13 C12 H12A 107.70 . . . ?
C11 C12 H12A 107.70 . . . ?
C13 C12 H12B 107.70 . . . ?
C11 C12 H12B 107.70 . . . ?
H12A C12 H12B 107.10 . . . ?
C12 C13 H13A 109.50 . . . ?
C12 C13 H13B 109.50 . . . ?
H13A C13 H13B 109.50 . . . ?
C12 C13 H13C 109.50 . . . ?
H13A C13 H13C 109.50 . . . ?
H13B C13 H13C 109.50 . . . ?
N2 C21 O2 123.4(8) . . 5_655 ?
N2 C21 C22 118.9(10) . . . ?
O2 C21 C22 117.6(10) 5_655 . . ?
C23A C22 C23B 66(3) . . . ?
C23A C22 C21 120.3(17) . . . ?
C23B C22 C21 112(3) . . . ?
C23A C22 H22A 107.30 . . . ?
C23B C22 H22A 46.00 . . . ?
C21 C22 H22A 107.30 . . . ?
C23A C22 H22B 107.30 . . . ?
C23B C22 H22B 137.30 . . . ?
C21 C22 H22B 107.30 . . . ?
H22A C22 H22B 106.90 . . . ?
C22 C23A H23A 109.50 . . . ?
C22 C23A H23B 109.50 . . . ?
H23A C23A H23B 109.50 . . . ?
C22 C23A H23C 109.50 . . . ?
H23A C23A H23C 109.50 . . . ?
H23B C23A H23C 109.50 . . . ?
C22 C23B H23D 109.50 . . . ?
C22 C23B H23E 109.50 . . . ?
H23D C23B H23E 109.50 . . . ?
C22 C23B H23F 109.50 . . . ?
H23D C23B H23F 109.50 . . . ?
H23E C23B H23F 109.50 . . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 Ru1 Cl1 Ru1 -117.5(2) . . . 2_655 ?
N2 Ru1 Cl1 Ru1 -28.2(2) . . . 2_655 ?
O2 Ru1 Cl1 Ru1 153.1(2) . . . 2_655 ?
N1 Ru1 Cl1 Ru1 62.3(2) . . . 2_655 ?
Ru1 Ru1 Cl1 Ru1 75.5(17) 5_655 . . 2_655 ?
N2 Ru1 O1 C11 88.6(8) . . . . ?
O2 Ru1 O1 C11 -90.3(8) . . . . ?
N1 Ru1 O1 C11 13(18) . . . . ?
Ru1 Ru1 O1 C11 0.1(7) 5_655 . . . ?
Cl1 Ru1 O1 C11 -179.4(7) . . . . ?
O1 Ru1 O2 C21 92.3(7) . . . 5_655 ?
N2 Ru1 O2 C21 50(10) . . . 5_655 ?
N1 Ru1 O2 C21 -86.8(7) . . . 5_655 ?
Ru1 Ru1 O2 C21 1.8(7) 5_655 . . 5_655 ?
Cl1 Ru1 O2 C21 -176.0(7) . . . 5_655 ?
O1 Ru1 N1 C11 -13(18) . . . 5_655 ?
N2 Ru1 N1 C11 -88.9(7) . . . 5_655 ?
O2 Ru1 N1 C11 89.9(8) . . . 5_655 ?
Ru1 Ru1 N1 C11 -0.4(7) 5_655 . . 5_655 ?
Cl1 Ru1 N1 C11 179.1(7) . . . 5_655 ?
O1 Ru1 N2 C21 -91.7(7) . . . . ?
O2 Ru1 N2 C21 -50(10) . . . . ?
N1 Ru1 N2 C21 87.4(7) . . . . ?
Ru1 Ru1 N2 C21 -1.2(7) 5_655 . . . ?
Cl1 Ru1 N2 C21 176.6(7) . . . . ?
Ru1 O1 C11 N1 0.3(14) . . . 5_655 ?
Ru1 O1 C11 C12 179.9(8) . . . . ?
O1 C11 C12 C13 160(2) . . . . ?
N1 C11 C12 C13 -21(3) 5_655 . . . ?
Ru1 N2 C21 O2 0.1(13) . . . 5_655 ?
Ru1 N2 C21 C22 177.8(8) . . . . ?
N2 C21 C22 C23A 57(3) . . . . ?
O2 C21 C22 C23A -125(2) 5_655 . . . ?
N2 C21 C22 C23B 131(3) . . . . ?
O2 C21 C22 C23B -51(3) 5_655 . . . ?