# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Complex_3
_database_code_depnum_ccdc_archive 'CCDC 1488194'
_audit_update_record             
;
2016-06-28 deposited with the CCDC.
2016-10-28 downloaded from the CCDC.
;
#===============================================================================
# 5. CHEMICAL DATA

_chemical_formula_moiety         'C16 H20 Cl2 N2 O3 Ru, C H Cl3'
_chemical_formula_sum            'C17 H21 Cl5 N2 O3 Ru'
_chemical_formula_weight         579.68
#=============================================================
# 6. CRYSTAL DATA

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x+, y+, z+'
'-x+, -y+, -z+'

#------------------------------------------------
_cell_length_a                   9.6767(2)
_cell_length_b                   11.0960(3)
_cell_length_c                   12.1079(3)
_cell_angle_alpha                69.1980(10)
_cell_angle_beta                 84.2960(10)
_cell_angle_gamma                75.4870(10)
_cell_volume                     1176.45(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9918
_cell_measurement_theta_min      2.20
_cell_measurement_theta_max      25.48

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?

_exptl_crystal_density_diffrn    1.636
_exptl_crystal_density_meas      ?
# Non-dispersive F(000): 
_exptl_crystal_F_000             580
_exptl_absorpt_coefficient_mu    1.254
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   '(Sheldrick , 1996)'
_exptl_absorpt_correction_T_min  0.6953
_exptl_absorpt_correction_T_max  0.7452

#=============================================================================
# 7. EXPERIMENTAL DATA

_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_method       'φ and ω scans'
_diffrn_ambient_temperature      296(2)
_diffrn_reflns_number            13126
_diffrn_reflns_av_unetI/netI     0.0162
_diffrn_reflns_av_R_equivalents  0.0156
_diffrn_reflns_theta_min         1.799
_diffrn_reflns_theta_max         25.479
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14


#==========================================================================
# 8. REFINEMENT DATA


_reflns_number_total             4350
_reflns_number_gt                3891
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0356P)²+0.9591P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .

_refine_ls_number_reflns         4350
_refine_ls_number_parameters     256
_refine_ls_number_restraints     90
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0287
_refine_ls_wR_factor_ref         0.0739
_refine_ls_wR_factor_gt          0.0705
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.022
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

_refine_diff_density_max         0.574
_refine_diff_density_min         -0.457

#========================================================== 
# 9. General computing 

_computing_data_collection       'Bruker APEX2 (Bruker, 2014)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2013)'
_computing_cell_refinement       'Bruker SAINT (Bruker, 2013)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2015)'
_computing_structure_refinement  
'SHELXL-2014/7 (Sheldrick, 2015), Shelxle (Hübschle et al., 2011)'


#===================================================================
# 10.  ATOMIC COORDINATES AND THERMAL PARAMETERS

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'
Cl Cl 0.1484 0.1585 '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'


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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
RU1 Ru 0.37852(2) 0.78110(2) 0.12683(2) 0.04227(9) Uani 1 1 d . . . . .
CL1 Cl 0.57633(9) 0.69203(8) 0.01922(6) 0.0579(2) Uani 1 1 d . . . . .
O1 O 0.2535(2) 0.19330(19) 0.52767(18) 0.0558(5) Uani 1 1 d . . . . .
N1 N 0.3929(3) 0.5821(2) 0.23994(18) 0.0435(5) Uani 1 1 d . . . . .
C1 C 0.4025(4) 0.4850(3) 0.1961(2) 0.0524(7) Uani 1 1 d . . . . .
H1 H 0.4111 0.5048 0.1147 0.063 Uiso 1 1 calc R U . . .
CL2 Cl 0.55447(7) 0.78790(6) 0.25132(6) 0.04554(16) Uani 1 1 d . . . . .
O2 O 0.3470(3) -0.0147(2) 0.6388(2) 0.0772(7) Uani 1 1 d . . . . .
N2 N 0.2480(3) 0.0775(3) 0.6226(2) 0.0626(7) Uani 1 1 d . . . . .
C2 C 0.4002(3) 0.3573(3) 0.2664(2) 0.0519(7) Uani 1 1 d . . . . .
H2 H 0.4072 0.2926 0.2328 0.062 Uiso 1 1 calc R U . . .
O3 O 0.1405(3) 0.0866(3) 0.6787(3) 0.1072(11) Uani 1 1 d . . . . .
C3 C 0.3874(3) 0.3258(3) 0.3870(2) 0.0430(6) Uani 1 1 d . . . . .
C4 C 0.3770(3) 0.4255(3) 0.4323(2) 0.0460(6) Uani 1 1 d . . . . .
H4 H 0.3679 0.4078 0.5134 0.055 Uiso 1 1 calc R U . . .
C5 C 0.3803(3) 0.5507(3) 0.3574(2) 0.0455(6) Uani 1 1 d . . . . .
H5 H 0.3733 0.6168 0.3895 0.055 Uiso 1 1 calc R U . . .
C6 C 0.3893(3) 0.1869(3) 0.4674(2) 0.0486(6) Uani 1 1 d . . . . .
H6A H 0.4017 0.1280 0.4222 0.058 Uiso 1 1 calc R U . . .
H6B H 0.4665 0.1547 0.5234 0.058 Uiso 1 1 calc R U . . .
CL21 Cl 0.03697(13) 0.49736(12) 0.86361(10) 0.0936(3) Uani 1 1 d . . . . .
C21 C 0.1472(4) 0.4710(4) 0.7472(3) 0.0655(8) Uani 1 1 d . . . . .
H21 H 0.2273 0.3958 0.7809 0.079 Uiso 1 1 calc R U . . .
CL22 Cl 0.05532(17) 0.42973(19) 0.65660(13) 0.1286(5) Uani 1 1 d . . . . .
CL23 Cl 0.21645(16) 0.60783(13) 0.67032(13) 0.1127(4) Uani 1 1 d . . . . .
C101 C 0.2396(5) 0.7631(5) -0.1041(3) 0.0934(14) Uani 1 1 d . . . . .
H10A H 0.1755 0.8171 -0.1680 0.140 Uiso 1 1 calc R U . . .
H10B H 0.2133 0.6799 -0.0657 0.140 Uiso 1 1 calc R U . . .
H10C H 0.3354 0.7476 -0.1345 0.140 Uiso 1 1 calc R U . . .
C102 C 0.2309(4) 0.8332(4) -0.0164(3) 0.0690(9) Uani 1 1 d . . . . .
C103 C 0.3019(4) 0.9386(3) -0.0379(3) 0.0702(10) Uani 1 1 d . . . . .
H103 H 0.3682 0.9561 -0.1052 0.084 Uiso 1 1 calc R U . . .
C104 C 0.3026(4) 0.9962(3) 0.0468(3) 0.0676(9) Uani 1 1 d . . . . .
H104 H 0.3706 1.0516 0.0367 0.081 Uiso 1 1 calc R U . . .
C105 C 0.2353(3) 0.9524(3) 0.1592(3) 0.0635(8) Uani 1 1 d . . . . .
C106 C 0.1608(3) 0.8510(3) 0.1811(3) 0.0637(8) Uani 1 1 d . . . . .
H106 H 0.1283 0.8077 0.2615 0.076 Uiso 1 1 calc R U . . .
C107 C 0.1604(3) 0.7940(3) 0.0929(3) 0.0647(9) Uani 1 1 d . . . . .
H107 H 0.1285 0.7111 0.1162 0.078 Uiso 1 1 calc R U . . .
C108 C 0.2443(4) 1.0139(4) 0.2512(4) 0.0810(11) Uani 1 1 d . . . . .
H108 H 0.3416 1.0266 0.2471 0.097 Uiso 1 1 calc R U . . .
C109 C 0.2191(5) 0.9296(5) 0.3761(5) 0.1018(14) Uani 1 1 d . . . . .
H10D H 0.1220 0.9208 0.3852 0.153 Uiso 1 1 calc R U . . .
H10E H 0.2367 0.9707 0.4293 0.153 Uiso 1 1 calc R U . . .
H10F H 0.2825 0.8436 0.3935 0.153 Uiso 1 1 calc R U . . .
C110 C 0.1430(5) 1.1523(5) 0.2168(6) 0.130(2) Uani 1 1 d . . . . .
H11A H 0.1561 1.1959 0.2694 0.196 Uiso 1 1 calc R U . . .
H11B H 0.0460 1.1438 0.2223 0.196 Uiso 1 1 calc R U . . .
H11C H 0.1637 1.2036 0.1372 0.196 Uiso 1 1 calc R U . . .


_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 N1 2.123(2) . ?
RU1 C107 2.150(3) . ?
RU1 C106 2.177(3) . ?
RU1 C103 2.179(3) . ?
RU1 C102 2.180(3) . ?
RU1 C105 2.188(3) . ?
RU1 C104 2.190(3) . ?
RU1 CL1 2.4102(8) . ?
RU1 CL2 2.4149(7) . ?
O1 N2 1.396(3) . ?
O1 C6 1.437(3) . ?
N1 C5 1.340(3) . ?
N1 C1 1.341(3) . ?
C1 C2 1.374(4) . ?
C1 H1 0.9300 . ?
O2 N2 1.186(3) . ?
N2 O3 1.187(4) . ?
C2 C3 1.376(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.377(4) . ?
C3 C6 1.500(3) . ?
C4 C5 1.369(4) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
CL21 C21 1.745(3) . ?
C21 CL22 1.721(4) . ?
C21 CL23 1.732(4) . ?
C21 H21 0.9800 . ?
C101 C102 1.509(6) . ?
C101 H10A 0.9600 . ?
C101 H10B 0.9600 . ?
C101 H10C 0.9600 . ?
C102 C107 1.402(5) . ?
C102 C103 1.434(5) . ?
C103 C104 1.388(5) . ?
C103 H103 0.9800 . ?
C104 C105 1.424(5) . ?
C104 H104 0.9800 . ?
C105 C106 1.419(4) . ?
C105 C108 1.517(5) . ?
C106 C107 1.421(5) . ?
C106 H106 0.9800 . ?
C107 H107 0.9800 . ?
C108 C109 1.502(6) . ?
C108 C110 1.537(5) . ?
C108 H108 0.9800 . ?
C109 H10D 0.9600 . ?
C109 H10E 0.9600 . ?
C109 H10F 0.9600 . ?
C110 H11A 0.9600 . ?
C110 H11B 0.9600 . ?
C110 H11C 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
N1 RU1 C107 88.76(11) . . ?
N1 RU1 C106 94.09(11) . . ?
C107 RU1 C106 38.35(13) . . ?
N1 RU1 C103 148.30(11) . . ?
C107 RU1 C103 67.72(12) . . ?
C106 RU1 C103 80.67(14) . . ?
N1 RU1 C102 110.47(11) . . ?
C107 RU1 C102 37.79(13) . . ?
C106 RU1 C102 69.47(15) . . ?
C103 RU1 C102 38.42(12) . . ?
N1 RU1 C105 123.83(11) . . ?
C107 RU1 C105 68.84(13) . . ?
C106 RU1 C105 37.93(12) . . ?
C103 RU1 C105 68.47(15) . . ?
C102 RU1 C105 82.64(14) . . ?
N1 RU1 C104 161.29(12) . . ?
C107 RU1 C104 79.76(12) . . ?
C106 RU1 C104 67.77(13) . . ?
C103 RU1 C104 37.06(14) . . ?
C102 RU1 C104 68.55(13) . . ?
C105 RU1 C104 37.96(14) . . ?
N1 RU1 CL1 86.02(6) . . ?
C107 RU1 CL1 122.46(11) . . ?
C106 RU1 CL1 160.71(10) . . ?
C103 RU1 CL1 89.11(12) . . ?
C102 RU1 CL1 92.39(11) . . ?
C105 RU1 CL1 149.64(9) . . ?
C104 RU1 CL1 112.60(11) . . ?
N1 RU1 CL2 86.61(6) . . ?
C107 RU1 CL2 150.10(10) . . ?
C106 RU1 CL2 112.60(10) . . ?
C103 RU1 CL2 124.38(9) . . ?
C102 RU1 CL2 162.80(9) . . ?
C105 RU1 CL2 89.51(9) . . ?
C104 RU1 CL2 95.97(9) . . ?
CL1 RU1 CL2 86.68(3) . . ?
N2 O1 C6 112.9(2) . . ?
C5 N1 C1 117.4(2) . . ?
C5 N1 RU1 121.20(17) . . ?
C1 N1 RU1 121.19(17) . . ?
N1 C1 C2 122.7(2) . . ?
N1 C1 H1 118.6 . . ?
C2 C1 H1 118.6 . . ?
O2 N2 O3 128.2(3) . . ?
O2 N2 O1 118.7(2) . . ?
O3 N2 O1 113.0(3) . . ?
C1 C2 C3 119.6(3) . . ?
C1 C2 H2 120.2 . . ?
C3 C2 H2 120.2 . . ?
C2 C3 C4 117.8(2) . . ?
C2 C3 C6 121.3(2) . . ?
C4 C3 C6 120.8(2) . . ?
C5 C4 C3 119.7(2) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
N1 C5 C4 122.8(2) . . ?
N1 C5 H5 118.6 . . ?
C4 C5 H5 118.6 . . ?
O1 C6 C3 105.7(2) . . ?
O1 C6 H6A 110.6 . . ?
C3 C6 H6A 110.6 . . ?
O1 C6 H6B 110.6 . . ?
C3 C6 H6B 110.6 . . ?
H6A C6 H6B 108.7 . . ?
CL22 C21 CL23 112.0(2) . . ?
CL22 C21 CL21 110.0(2) . . ?
CL23 C21 CL21 111.03(19) . . ?
CL22 C21 H21 107.9 . . ?
CL23 C21 H21 107.9 . . ?
CL21 C21 H21 107.9 . . ?
C102 C101 H10A 109.5 . . ?
C102 C101 H10B 109.5 . . ?
H10A C101 H10B 109.5 . . ?
C102 C101 H10C 109.5 . . ?
H10A C101 H10C 109.5 . . ?
H10B C101 H10C 109.5 . . ?
C107 C102 C103 116.5(3) . . ?
C107 C102 C101 121.9(3) . . ?
C103 C102 C101 121.5(3) . . ?
C107 C102 RU1 69.96(18) . . ?
C103 C102 RU1 70.77(17) . . ?
C101 C102 RU1 126.6(3) . . ?
C104 C103 C102 121.3(3) . . ?
C104 C103 RU1 71.88(18) . . ?
C102 C103 RU1 70.81(17) . . ?
C104 C103 H103 118.6 . . ?
C102 C103 H103 118.6 . . ?
RU1 C103 H103 118.6 . . ?
C103 C104 C105 121.8(3) . . ?
C103 C104 RU1 71.06(19) . . ?
C105 C104 RU1 70.97(17) . . ?
C103 C104 H104 118.2 . . ?
C105 C104 H104 118.2 . . ?
RU1 C104 H104 118.2 . . ?
C106 C105 C104 117.9(3) . . ?
C106 C105 C108 122.1(4) . . ?
C104 C105 C108 120.1(3) . . ?
C106 C105 RU1 70.60(19) . . ?
C104 C105 RU1 71.1(2) . . ?
C108 C105 RU1 129.5(2) . . ?
C105 C106 C107 119.4(3) . . ?
C105 C106 RU1 71.47(19) . . ?
C107 C106 RU1 69.81(19) . . ?
C105 C106 H106 119.6 . . ?
C107 C106 H106 119.6 . . ?
RU1 C106 H106 119.6 . . ?
C102 C107 C106 123.0(3) . . ?
C102 C107 RU1 72.25(18) . . ?
C106 C107 RU1 71.84(18) . . ?
C102 C107 H107 117.7 . . ?
C106 C107 H107 117.7 . . ?
RU1 C107 H107 117.7 . . ?
C109 C108 C105 114.5(3) . . ?
C109 C108 C110 112.0(4) . . ?
C105 C108 C110 109.0(4) . . ?
C109 C108 H108 107.0 . . ?
C105 C108 H108 107.0 . . ?
C110 C108 H108 107.0 . . ?
C108 C109 H10D 109.5 . . ?
C108 C109 H10E 109.5 . . ?
H10D C109 H10E 109.5 . . ?
C108 C109 H10F 109.5 . . ?
H10D C109 H10F 109.5 . . ?
H10E C109 H10F 109.5 . . ?
C108 C110 H11A 109.5 . . ?
C108 C110 H11B 109.5 . . ?
H11A C110 H11B 109.5 . . ?
C108 C110 H11C 109.5 . . ?
H11A C110 H11C 109.5 . . ?
H11B C110 H11C 109.5 . . ?



_chemical_melting_point          404-406
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_solvent_exptl_crystal_recrystallization_method Chloroform/ether
