# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_jc0106
_database_code_depnum_ccdc_archive 'CCDC 1028031'
_audit_update_record             
;
2014-10-07 deposited with the CCDC.
2015-02-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H20 Cl N4 O8 Ru'
_chemical_formula_weight         628.96

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   10.0833(2)
_cell_length_b                   9.8576(2)
_cell_length_c                   12.7262(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.3270(10)
_cell_angle_gamma                90.00
_cell_volume                     1259.48(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9125
_cell_measurement_theta_min      2.47
_cell_measurement_theta_max      29.95

_exptl_crystal_description       PLATE
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.658
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             634
_exptl_absorpt_coefficient_mu    0.785
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6687
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_process_details   
; 
      SADABS Version 2007/2 (Sheldrick, Bruker AXS Inc.) 
;
_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(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 APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            20199
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_sigmaI/netI    0.0478
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.47
_diffrn_reflns_theta_max         30.18
_reflns_number_total             7318
_reflns_number_gt                6424
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0340P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_number_reflns         7318
_refine_ls_number_parameters     343
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0310
_refine_ls_wR_factor_ref         0.0649
_refine_ls_wR_factor_gt          0.0614
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_restrained_S_all      0.993
_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 0.574071(18) 0.749236(14) 0.775196(12) 0.01397(5) Uani 1 1 d . . .
N111 N 0.5673(2) 0.9513(2) 0.76922(16) 0.0155(4) Uani 1 1 d . . .
C112 C 0.6038(3) 1.0150(2) 0.68227(19) 0.0167(5) Uani 1 1 d . . .
C113 C 0.6079(3) 1.1554(3) 0.6804(2) 0.0232(6) Uani 1 1 d . . .
H113 H 0.6341 1.2018 0.6202 0.028 Uiso 1 1 calc R . .
C114 C 0.5731(3) 1.2276(3) 0.7678(2) 0.0257(7) Uani 1 1 d . . .
H114 H 0.5755 1.3240 0.7674 0.031 Uiso 1 1 calc R . .
C115 C 0.5352(3) 1.1592(3) 0.8554(2) 0.0234(6) Uani 1 1 d . . .
H115 H 0.5100 1.2076 0.9149 0.028 Uiso 1 1 calc R . .
C116 C 0.5347(3) 1.0189(2) 0.85408(19) 0.0180(5) Uani 1 1 d . . .
C117 C 0.5025(3) 0.9256(2) 0.9429(2) 0.0201(5) Uani 1 1 d . . .
O171 O 0.51276(19) 0.79684(16) 0.91982(13) 0.0191(4) Uani 1 1 d . . .
O172 O 0.4711(2) 0.9697(2) 1.02631(14) 0.0295(5) Uani 1 1 d . . .
N121 N 0.6241(2) 0.78780(19) 0.63016(16) 0.0145(4) Uani 1 1 d . . .
C122 C 0.6357(3) 0.9183(3) 0.5990(2) 0.0169(6) Uani 1 1 d . . .
C123 C 0.6735(3) 0.9459(3) 0.4999(2) 0.0233(6) Uani 1 1 d . . .
H123 H 0.6830 1.0369 0.4773 0.028 Uiso 1 1 calc R . .
C124 C 0.6975(3) 0.8390(3) 0.4340(2) 0.0255(6) Uani 1 1 d . . .
H124 H 0.7239 0.8569 0.3656 0.031 Uiso 1 1 calc R . .
C125 C 0.6833(3) 0.7060(3) 0.4666(2) 0.0211(6) Uani 1 1 d . . .
H125 H 0.6988 0.6323 0.4211 0.025 Uiso 1 1 calc R . .
C126 C 0.6462(3) 0.6832(2) 0.56696(19) 0.0168(5) Uani 1 1 d . . .
C127 C 0.6314(3) 0.5477(3) 0.6205(2) 0.0172(7) Uani 1 1 d . . .
O271 O 0.6065(2) 0.55704(17) 0.71883(15) 0.0202(4) Uani 1 1 d . . .
O272 O 0.6439(2) 0.44272(18) 0.57156(15) 0.0274(4) Uani 1 1 d . . .
N151 N 0.76976(19) 0.7556(4) 0.84321(14) 0.0202(4) Uani 1 1 d . . .
C152 C 0.8660(3) 0.8364(3) 0.8140(2) 0.0258(6) Uani 1 1 d . . .
H152 H 0.8459 0.8964 0.7563 0.031 Uiso 1 1 calc R . .
C153 C 0.9939(3) 0.8365(3) 0.8642(2) 0.0305(6) Uani 1 1 d . . .
H153 H 1.0596 0.8951 0.8403 0.037 Uiso 1 1 calc R . .
C154 C 1.0256(3) 0.7521(6) 0.9483(2) 0.0362(6) Uani 1 1 d . . .
C155 C 0.9253(4) 0.6704(4) 0.9794(3) 0.0512(10) Uani 1 1 d . . .
H155 H 0.9425 0.6122 1.0386 0.061 Uiso 1 1 calc R . .
C156 C 0.8011(3) 0.6725(3) 0.9258(3) 0.0383(8) Uani 1 1 d . . .
H156 H 0.7346 0.6132 0.9476 0.046 Uiso 1 1 calc R . .
C157 C 1.1634(3) 0.7497(8) 1.0054(2) 0.0586(10) Uani 1 1 d . . .
H57A H 1.2259 0.7945 0.9621 0.088 Uiso 1 1 calc R . .
H57B H 1.1913 0.6555 1.0184 0.088 Uiso 1 1 calc R . .
H57C H 1.1627 0.7975 1.0729 0.088 Uiso 1 1 calc R . .
N161 N 0.3754(2) 0.71987(19) 0.72292(15) 0.0184(5) Uani 1 1 d . . .
C162 C 0.3162(3) 0.6168(3) 0.7715(2) 0.0233(6) Uani 1 1 d . . .
H162 H 0.3659 0.5686 0.8266 0.028 Uiso 1 1 calc R . .
C163 C 0.1858(3) 0.5800(3) 0.7431(2) 0.0292(6) Uani 1 1 d . . .
H163 H 0.1466 0.5082 0.7792 0.035 Uiso 1 1 calc R . .
C164 C 0.1119(3) 0.6473(3) 0.6623(2) 0.0305(7) Uani 1 1 d . . .
C165 C 0.1740(3) 0.7550(6) 0.6133(2) 0.0323(6) Uani 1 1 d . . .
H165 H 0.1266 0.8051 0.5581 0.039 Uiso 1 1 calc R . .
C166 C 0.3043(3) 0.7870(3) 0.6461(2) 0.0257(6) Uani 1 1 d . . .
H166 H 0.3453 0.8599 0.6126 0.031 Uiso 1 1 calc R . .
C167 C -0.0283(4) 0.6088(5) 0.6281(3) 0.0530(10) Uani 1 1 d . . .
H67A H -0.0302 0.5504 0.5657 0.080 Uiso 1 1 calc R . .
H67B H -0.0808 0.6908 0.6108 0.080 Uiso 1 1 calc R . .
H67C H -0.0662 0.5599 0.6854 0.080 Uiso 1 1 calc R . .
Cl1 Cl 1.01235(10) 1.14995(11) 0.68830(7) 0.0488(2) Uani 1 1 d . . .
O11 O 1.0208(3) 1.2684(4) 0.6250(2) 0.0732(9) Uani 1 1 d . . .
O12 O 1.1389(3) 1.1008(4) 0.7228(3) 0.0909(13) Uani 1 1 d . . .
O13 O 0.9331(4) 1.1625(5) 0.7720(3) 0.0964(13) Uani 1 1 d . . .
O14 O 0.9469(5) 1.0464(5) 0.6223(3) 0.1204(18) Uani 1 1 d . . .


_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 N111 1.9945(19) . ?
Ru1 N121 1.995(2) . ?
Ru1 O171 2.0496(17) . ?
Ru1 O271 2.0626(18) . ?
Ru1 N161 2.072(2) . ?
Ru1 N151 2.0807(19) . ?
N111 C116 1.335(3) . ?
N111 C112 1.353(3) . ?
C112 C113 1.385(3) . ?
C112 C122 1.483(4) . ?
C113 C114 1.393(4) . ?
C113 H113 0.9500 . ?
C114 C115 1.387(4) . ?
C114 H114 0.9500 . ?
C115 C116 1.383(3) . ?
C115 H115 0.9500 . ?
C116 C117 1.516(3) . ?
C117 O172 1.216(3) . ?
C117 O171 1.309(3) . ?
N121 C126 1.339(3) . ?
N121 C122 1.355(3) . ?
C122 C123 1.377(4) . ?
C123 C124 1.382(4) . ?
C123 H123 0.9500 . ?
C124 C125 1.387(4) . ?
C124 H124 0.9500 . ?
C125 C126 1.382(4) . ?
C125 H125 0.9500 . ?
C126 C127 1.513(4) . ?
C127 O272 1.221(3) . ?
C127 O271 1.302(3) . ?
N151 C152 1.334(4) . ?
N151 C156 1.346(4) . ?
C152 C153 1.385(4) . ?
C152 H152 0.9500 . ?
C153 C154 1.370(5) . ?
C153 H153 0.9500 . ?
C154 C155 1.380(5) . ?
C154 C157 1.507(4) . ?
C155 C156 1.370(4) . ?
C155 H155 0.9500 . ?
C156 H156 0.9500 . ?
C157 H57A 0.9800 . ?
C157 H57B 0.9800 . ?
C157 H57C 0.9800 . ?
N161 C166 1.333(3) . ?
N161 C162 1.356(3) . ?
C162 C163 1.380(4) . ?
C162 H162 0.9500 . ?
C163 C164 1.382(4) . ?
C163 H163 0.9500 . ?
C164 C165 1.408(6) . ?
C164 C167 1.489(4) . ?
C165 C166 1.378(4) . ?
C165 H165 0.9500 . ?
C166 H166 0.9500 . ?
C167 H67A 0.9800 . ?
C167 H67B 0.9800 . ?
C167 H67C 0.9800 . ?
Cl1 O13 1.395(4) . ?
Cl1 O12 1.397(3) . ?
Cl1 O11 1.426(3) . ?
Cl1 O14 1.442(4) . ?

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
N111 Ru1 N121 77.59(8) . . ?
N111 Ru1 O171 78.08(7) . . ?
N121 Ru1 O171 155.59(7) . . ?
N111 Ru1 O271 155.52(9) . . ?
N121 Ru1 O271 77.96(7) . . ?
O171 Ru1 O271 126.39(7) . . ?
N111 Ru1 N161 95.66(8) . . ?
N121 Ru1 N161 92.85(8) . . ?
O171 Ru1 N161 87.54(8) . . ?
O271 Ru1 N161 86.54(8) . . ?
N111 Ru1 N151 90.78(12) . . ?
N121 Ru1 N151 93.87(8) . . ?
O171 Ru1 N151 88.45(8) . . ?
O271 Ru1 N151 89.86(11) . . ?
N161 Ru1 N151 171.56(10) . . ?
C116 N111 C112 122.4(2) . . ?
C116 N111 Ru1 118.51(16) . . ?
C112 N111 Ru1 118.94(17) . . ?
N111 C112 C113 119.3(2) . . ?
N111 C112 C122 112.3(2) . . ?
C113 C112 C122 128.4(2) . . ?
C112 C113 C114 119.1(2) . . ?
C112 C113 H113 120.4 . . ?
C114 C113 H113 120.4 . . ?
C115 C114 C113 120.1(2) . . ?
C115 C114 H114 119.9 . . ?
C113 C114 H114 119.9 . . ?
C116 C115 C114 118.5(2) . . ?
C116 C115 H115 120.7 . . ?
C114 C115 H115 120.7 . . ?
N111 C116 C115 120.5(2) . . ?
N111 C116 C117 112.7(2) . . ?
C115 C116 C117 126.8(2) . . ?
O172 C117 O171 125.1(2) . . ?
O172 C117 C116 121.7(2) . . ?
O171 C117 C116 113.2(2) . . ?
C117 O171 Ru1 117.39(15) . . ?
C126 N121 C122 122.1(2) . . ?
C126 N121 Ru1 118.64(15) . . ?
C122 N121 Ru1 119.22(17) . . ?
N121 C122 C123 119.6(3) . . ?
N121 C122 C112 111.8(2) . . ?
C123 C122 C112 128.6(3) . . ?
C122 C123 C124 119.0(2) . . ?
C122 C123 H123 120.5 . . ?
C124 C123 H123 120.5 . . ?
C123 C124 C125 120.7(2) . . ?
C123 C124 H124 119.7 . . ?
C125 C124 H124 119.7 . . ?
C126 C125 C124 118.3(2) . . ?
C126 C125 H125 120.8 . . ?
C124 C125 H125 120.8 . . ?
N121 C126 C125 120.3(2) . . ?
N121 C126 C127 112.4(2) . . ?
C125 C126 C127 127.3(2) . . ?
O272 C127 O271 126.1(3) . . ?
O272 C127 C126 119.9(3) . . ?
O271 C127 C126 114.0(2) . . ?
C127 O271 Ru1 116.74(17) . . ?
C152 N151 C156 117.2(2) . . ?
C152 N151 Ru1 126.0(2) . . ?
C156 N151 Ru1 116.8(2) . . ?
N151 C152 C153 122.8(3) . . ?
N151 C152 H152 118.6 . . ?
C153 C152 H152 118.6 . . ?
C154 C153 C152 120.0(3) . . ?
C154 C153 H153 120.0 . . ?
C152 C153 H153 120.0 . . ?
C153 C154 C155 117.0(3) . . ?
C153 C154 C157 121.6(4) . . ?
C155 C154 C157 121.4(4) . . ?
C156 C155 C154 120.6(3) . . ?
C156 C155 H155 119.7 . . ?
C154 C155 H155 119.7 . . ?
N151 C156 C155 122.4(3) . . ?
N151 C156 H156 118.8 . . ?
C155 C156 H156 118.8 . . ?
C154 C157 H57A 109.5 . . ?
C154 C157 H57B 109.5 . . ?
H57A C157 H57B 109.5 . . ?
C154 C157 H57C 109.5 . . ?
H57A C157 H57C 109.5 . . ?
H57B C157 H57C 109.5 . . ?
C166 N161 C162 118.5(2) . . ?
C166 N161 Ru1 127.16(18) . . ?
C162 N161 Ru1 114.28(18) . . ?
N161 C162 C163 121.7(3) . . ?
N161 C162 H162 119.1 . . ?
C163 C162 H162 119.1 . . ?
C162 C163 C164 120.3(3) . . ?
C162 C163 H163 119.9 . . ?
C164 C163 H163 119.9 . . ?
C163 C164 C165 117.4(3) . . ?
C163 C164 C167 121.8(3) . . ?
C165 C164 C167 120.8(3) . . ?
C166 C165 C164 119.3(3) . . ?
C166 C165 H165 120.4 . . ?
C164 C165 H165 120.4 . . ?
N161 C166 C165 122.8(3) . . ?
N161 C166 H166 118.6 . . ?
C165 C166 H166 118.6 . . ?
C164 C167 H67A 109.5 . . ?
C164 C167 H67B 109.5 . . ?
H67A C167 H67B 109.5 . . ?
C164 C167 H67C 109.5 . . ?
H67A C167 H67C 109.5 . . ?
H67B C167 H67C 109.5 . . ?
O13 Cl1 O12 111.2(2) . . ?
O13 Cl1 O11 115.3(2) . . ?
O12 Cl1 O11 111.20(19) . . ?
O13 Cl1 O14 104.1(3) . . ?
O12 Cl1 O14 107.0(3) . . ?
O11 Cl1 O14 107.4(2) . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        30.18
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.705
_refine_diff_density_min         -0.799
_refine_diff_density_rms         0.078

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Acetone, diethyl ether'
####################################################################### 
# 
# 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_jc1220
_database_code_depnum_ccdc_archive 'CCDC 1028032'
_audit_update_record             
;
2014-10-07 deposited with the CCDC.
2015-02-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H20 Cl N4 O8 Ru'
_chemical_formula_weight         701.02

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'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   P2(1)2(1)2(1)

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   7.6696(18)
_cell_length_b                   11.321(2)
_cell_length_c                   32.206(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2796.3(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    2505
_cell_measurement_theta_min      2.61
_cell_measurement_theta_max      20.13

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.665
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1412
_exptl_absorpt_coefficient_mu    0.717
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5351
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   
; 
      SADABS Version 2007/2 (Sheldrick, Bruker AXS Inc.) 
;
_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(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 APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            32740
_diffrn_reflns_av_R_equivalents  0.2025
_diffrn_reflns_av_sigmaI/netI    0.1549
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_theta_min         2.20
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4903
_reflns_number_gt                3181
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0883P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     HEAVY
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(8)
_refine_ls_number_reflns         4903
_refine_ls_number_parameters     415
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1378
_refine_ls_R_factor_gt           0.0745
_refine_ls_wR_factor_ref         0.1693
_refine_ls_wR_factor_gt          0.1497
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_restrained_S_all      0.974
_refine_ls_shift/su_max          0.002
_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 0.06966(11) 0.47155(8) 0.09428(2) 0.0258(2) Uani 1 1 d . . .
N111 N -0.1224(10) 0.4930(7) 0.1344(2) 0.026(2) Uani 1 1 d . . .
C112 C -0.0952(14) 0.4551(10) 0.1750(3) 0.030(2) Uani 1 1 d . . .
C113 C -0.2263(17) 0.4796(12) 0.2043(3) 0.046(3) Uani 1 1 d . . .
H113 H -0.2163 0.4498 0.2317 0.056 Uiso 1 1 calc R . .
C114 C -0.3670(16) 0.5453(12) 0.1936(3) 0.045(3) Uani 1 1 d . . .
H114 H -0.4515 0.5664 0.2138 0.054 Uiso 1 1 calc R . .
C115 C -0.3871(15) 0.5833(10) 0.1507(3) 0.037(3) Uani 1 1 d . . .
H115 H -0.4872 0.6266 0.1423 0.044 Uiso 1 1 calc R . .
C116 C -0.2623(15) 0.5561(9) 0.1232(3) 0.029(3) Uani 1 1 d . . .
N121 N 0.1699(12) 0.3984(7) 0.1441(2) 0.028(2) Uani 1 1 d . . .
C122 C 0.0676(17) 0.3955(9) 0.1808(3) 0.036(3) Uani 1 1 d . . .
C123 C 0.1345(16) 0.3359(10) 0.2149(3) 0.036(3) Uani 1 1 d . . .
H123 H 0.0676 0.3293 0.2396 0.043 Uiso 1 1 calc R . .
C124 C 0.2989(19) 0.2863(12) 0.2128(4) 0.049(4) Uani 1 1 d . . .
H124 H 0.3450 0.2468 0.2364 0.059 Uiso 1 1 calc R . .
C125 C 0.3983(17) 0.2931(9) 0.1766(3) 0.037(3) Uani 1 1 d . . .
H125 H 0.5112 0.2589 0.1753 0.045 Uiso 1 1 calc R . .
C126 C 0.3283(14) 0.3509(9) 0.1428(3) 0.027(3) Uani 1 1 d . . .
C117 C -0.2599(17) 0.5816(11) 0.0760(4) 0.035(3) Uani 1 1 d . . .
O171 O -0.1208(9) 0.5445(7) 0.0579(2) 0.0369(19) Uani 1 1 d . . .
O172 O -0.3786(11) 0.6377(7) 0.0614(2) 0.042(2) Uani 1 1 d . . .
C127 C 0.4177(19) 0.3708(9) 0.1005(3) 0.038(3) Uani 1 1 d . . .
O271 O 0.3172(10) 0.4296(7) 0.0756(2) 0.0350(19) Uani 1 1 d . . .
O272 O 0.5608(11) 0.3342(6) 0.0938(3) 0.0454(18) Uani 1 1 d . . .
N131 N 0.0001(11) 0.3055(7) 0.0738(3) 0.030(2) Uani 1 1 d . . .
C132 C -0.0778(14) 0.2221(8) 0.0946(4) 0.033(2) Uani 1 1 d . . .
H132 H -0.1118 0.2385 0.1224 0.039 Uiso 1 1 calc R . .
C133 C -0.0690(17) 0.0850(10) 0.0361(3) 0.035(3) Uani 1 1 d . . .
C134 C -0.1148(14) 0.1086(9) 0.0785(3) 0.031(3) Uani 1 1 d . . .
C135 C 0.0051(15) 0.1770(10) 0.0137(4) 0.039(3) Uani 1 1 d . . .
H135 H 0.0310 0.1667 -0.0149 0.047 Uiso 1 1 calc R . .
C136 C 0.0401(14) 0.2801(10) 0.0323(3) 0.030(3) Uani 1 1 d . . .
H136 H 0.0955 0.3399 0.0163 0.037 Uiso 1 1 calc R . .
C137 C -0.1906(15) 0.0179(11) 0.1038(3) 0.039(3) Uani 1 1 d . . .
H137 H -0.2165 0.0322 0.1322 0.046 Uiso 1 1 calc R . .
C138 C -0.2247(16) -0.0889(11) 0.0864(4) 0.048(3) Uani 1 1 d . . .
H138 H -0.2771 -0.1494 0.1026 0.057 Uiso 1 1 calc R . .
C139 C -0.1833(17) -0.1104(12) 0.0449(4) 0.046(3) Uani 1 1 d . . .
H139 H -0.2086 -0.1858 0.0334 0.055 Uiso 1 1 calc R . .
C130 C -0.1073(14) -0.0261(12) 0.0203(3) 0.041(3) Uani 1 1 d . . .
H130 H -0.0807 -0.0439 -0.0079 0.049 Uiso 1 1 calc R . .
N141 N 0.1540(12) 0.6435(8) 0.1072(3) 0.032(2) Uani 1 1 d . . .
C142 C 0.1999(15) 0.7095(10) 0.0756(4) 0.035(3) Uani 1 1 d . . .
H142 H 0.1918 0.6766 0.0485 0.041 Uiso 1 1 calc R . .
C143 C 0.2608(14) 0.8267(10) 0.0796(3) 0.032(3) Uani 1 1 d . . .
C144 C 0.2664(17) 0.8748(11) 0.1201(4) 0.043(3) Uani 1 1 d . . .
C145 C 0.2121(19) 0.8070(11) 0.1520(3) 0.047(4) Uani 1 1 d . . .
H145 H 0.2122 0.8388 0.1793 0.057 Uiso 1 1 calc R . .
C146 C 0.1567(17) 0.6931(11) 0.1460(3) 0.040(3) Uani 1 1 d . . .
H146 H 0.1195 0.6477 0.1692 0.048 Uiso 1 1 calc R . .
C147 C 0.3110(18) 0.8925(11) 0.0446(4) 0.048(4) Uani 1 1 d . . .
H147 H 0.3082 0.8583 0.0177 0.058 Uiso 1 1 calc R . .
C148 C 0.3634(17) 1.0060(11) 0.0499(4) 0.059(4) Uani 1 1 d . . .
H148 H 0.3930 1.0524 0.0264 0.071 Uiso 1 1 calc R . .
C149 C 0.3747(17) 1.0561(10) 0.0901(5) 0.059(4) Uani 1 1 d . . .
H149 H 0.4175 1.1344 0.0932 0.071 Uiso 1 1 calc R . .
C140 C 0.3259(17) 0.9948(13) 0.1237(5) 0.066(4) Uani 1 1 d . . .
H140 H 0.3306 1.0311 0.1503 0.079 Uiso 1 1 calc R . .
Cl1 Cl -0.2157(5) 0.1140(3) 0.22657(10) 0.0603(11) Uani 1 1 d . . .
O11 O -0.2020(12) 0.1906(7) 0.1920(2) 0.053(2) Uani 1 1 d . . .
O12 O -0.3474(14) 0.0335(10) 0.2232(3) 0.096(4) Uani 1 1 d . . .
O13B O -0.188(8) 0.146(3) 0.2621(6) 0.141(16) Uani 0.50 1 d P . .
O13A O -0.316(4) 0.209(3) 0.2546(6) 0.093(9) Uani 0.50 1 d P . .
O14A O -0.063(3) 0.095(3) 0.2464(10) 0.085(8) Uani 0.50 1 d P . .
O14B O -0.060(4) 0.026(2) 0.2149(7) 0.108(9) Uani 0.50 1 d P . .


_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 N121 1.964(8) . ?
Ru1 N111 1.974(7) . ?
Ru1 O171 2.046(7) . ?
Ru1 O271 2.047(7) . ?
Ru1 N131 2.062(8) . ?
Ru1 N141 2.093(9) . ?
N111 C116 1.338(12) . ?
N111 C112 1.393(12) . ?
C112 C113 1.405(14) . ?
C112 C122 1.431(16) . ?
C113 C114 1.356(16) . ?
C113 H113 0.9500 . ?
C114 C115 1.454(16) . ?
C114 H114 0.9500 . ?
C115 C116 1.341(14) . ?
C115 H115 0.9500 . ?
C116 C117 1.547(14) . ?
N121 C126 1.329(13) . ?
N121 C122 1.417(13) . ?
C122 C123 1.389(15) . ?
C123 C124 1.382(17) . ?
C123 H123 0.9500 . ?
C124 C125 1.395(16) . ?
C124 H124 0.9500 . ?
C125 C126 1.378(14) . ?
C125 H125 0.9500 . ?
C126 C127 1.542(15) . ?
C117 O172 1.206(13) . ?
C117 O171 1.286(13) . ?
C127 O272 1.194(14) . ?
C127 O271 1.296(13) . ?
N131 C132 1.304(12) . ?
N131 C136 1.401(13) . ?
C132 C134 1.415(13) . ?
C132 H132 0.9500 . ?
C133 C135 1.389(15) . ?
C133 C130 1.390(15) . ?
C133 C134 1.433(14) . ?
C134 C137 1.435(14) . ?
C135 C136 1.339(14) . ?
C135 H135 0.9500 . ?
C136 H136 0.9500 . ?
C137 C138 1.358(15) . ?
C137 H137 0.9500 . ?
C138 C139 1.393(16) . ?
C138 H138 0.9500 . ?
C139 C130 1.371(16) . ?
C139 H139 0.9500 . ?
C130 H130 0.9500 . ?
N141 C142 1.311(13) . ?
N141 C146 1.368(13) . ?
C142 C143 1.413(15) . ?
C142 H142 0.9500 . ?
C143 C147 1.404(15) . ?
C143 C144 1.415(14) . ?
C144 C145 1.350(16) . ?
C144 C140 1.438(18) . ?
C145 C146 1.371(16) . ?
C145 H145 0.9500 . ?
C146 H146 0.9500 . ?
C147 C148 1.357(17) . ?
C147 H147 0.9500 . ?
C148 C149 1.414(18) . ?
C148 H148 0.9500 . ?
C149 C140 1.341(17) . ?
C149 H149 0.9500 . ?
C140 H140 0.9500 . ?
Cl1 O13B 1.22(2) . ?
Cl1 O14A 1.35(2) . ?
Cl1 O12 1.365(10) . ?
Cl1 O11 1.415(8) . ?
Cl1 O13A 1.60(2) . ?
Cl1 O14B 1.60(2) . ?
O13B O14A 1.22(5) . ?
O13B O13A 1.24(5) . ?
O14A O14B 1.29(4) . ?

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
N121 Ru1 N111 79.0(4) . . ?
N121 Ru1 O171 156.6(3) . . ?
N111 Ru1 O171 78.0(3) . . ?
N121 Ru1 O271 77.2(3) . . ?
N111 Ru1 O271 155.8(3) . . ?
O171 Ru1 O271 126.0(3) . . ?
N121 Ru1 N131 88.8(3) . . ?
N111 Ru1 N131 97.4(3) . . ?
O171 Ru1 N131 90.0(3) . . ?
O271 Ru1 N131 86.3(3) . . ?
N121 Ru1 N141 96.2(3) . . ?
N111 Ru1 N141 89.2(3) . . ?
O171 Ru1 N141 87.7(3) . . ?
O271 Ru1 N141 89.3(3) . . ?
N131 Ru1 N141 172.4(3) . . ?
C116 N111 C112 122.5(8) . . ?
C116 N111 Ru1 119.2(6) . . ?
C112 N111 Ru1 117.7(6) . . ?
N111 C112 C113 117.5(10) . . ?
N111 C112 C122 113.4(8) . . ?
C113 C112 C122 129.1(10) . . ?
C114 C113 C112 120.5(11) . . ?
C114 C113 H113 119.8 . . ?
C112 C113 H113 119.8 . . ?
C113 C114 C115 119.2(10) . . ?
C113 C114 H114 120.4 . . ?
C115 C114 H114 120.4 . . ?
C116 C115 C114 119.0(11) . . ?
C116 C115 H115 120.5 . . ?
C114 C115 H115 120.5 . . ?
N111 C116 C115 121.1(10) . . ?
N111 C116 C117 110.8(9) . . ?
C115 C116 C117 128.0(11) . . ?
C126 N121 C122 121.5(9) . . ?
C126 N121 Ru1 120.2(7) . . ?
C122 N121 Ru1 118.3(8) . . ?
C123 C122 N121 117.8(11) . . ?
C123 C122 C112 130.8(10) . . ?
N121 C122 C112 111.4(9) . . ?
C124 C123 C122 119.7(11) . . ?
C124 C123 H123 120.2 . . ?
C122 C123 H123 120.2 . . ?
C123 C124 C125 121.1(11) . . ?
C123 C124 H124 119.4 . . ?
C125 C124 H124 119.4 . . ?
C126 C125 C124 118.2(12) . . ?
C126 C125 H125 120.9 . . ?
C124 C125 H125 120.9 . . ?
N121 C126 C125 121.5(11) . . ?
N121 C126 C127 112.0(9) . . ?
C125 C126 C127 126.4(11) . . ?
O172 C117 O171 128.5(11) . . ?
O172 C117 C116 118.3(11) . . ?
O171 C117 C116 113.1(11) . . ?
C117 O171 Ru1 117.8(7) . . ?
O272 C127 O271 127.8(11) . . ?
O272 C127 C126 121.3(11) . . ?
O271 C127 C126 110.9(11) . . ?
C127 O271 Ru1 119.3(8) . . ?
C132 N131 C136 116.3(9) . . ?
C132 N131 Ru1 127.9(7) . . ?
C136 N131 Ru1 115.8(7) . . ?
N131 C132 C134 124.0(10) . . ?
N131 C132 H132 118.0 . . ?
C134 C132 H132 118.0 . . ?
C135 C133 C130 125.0(10) . . ?
C135 C133 C134 117.1(10) . . ?
C130 C133 C134 117.8(10) . . ?
C132 C134 C133 118.1(10) . . ?
C132 C134 C137 121.5(10) . . ?
C133 C134 C137 120.4(10) . . ?
C136 C135 C133 120.2(10) . . ?
C136 C135 H135 119.9 . . ?
C133 C135 H135 119.9 . . ?
C135 C136 N131 124.2(10) . . ?
C135 C136 H136 117.9 . . ?
N131 C136 H136 117.9 . . ?
C138 C137 C134 118.7(10) . . ?
C138 C137 H137 120.6 . . ?
C134 C137 H137 120.6 . . ?
C137 C138 C139 120.5(12) . . ?
C137 C138 H138 119.7 . . ?
C139 C138 H138 119.7 . . ?
C130 C139 C138 122.0(12) . . ?
C130 C139 H139 119.0 . . ?
C138 C139 H139 119.0 . . ?
C139 C130 C133 120.5(11) . . ?
C139 C130 H130 119.8 . . ?
C133 C130 H130 119.8 . . ?
C142 N141 C146 118.1(9) . . ?
C142 N141 Ru1 117.2(7) . . ?
C146 N141 Ru1 124.6(7) . . ?
N141 C142 C143 123.6(11) . . ?
N141 C142 H142 118.2 . . ?
C143 C142 H142 118.2 . . ?
C147 C143 C142 121.1(11) . . ?
C147 C143 C144 121.8(11) . . ?
C142 C143 C144 117.0(10) . . ?
C145 C144 C143 118.3(11) . . ?
C145 C144 C140 125.0(11) . . ?
C143 C144 C140 116.7(12) . . ?
C144 C145 C146 121.6(10) . . ?
C144 C145 H145 119.2 . . ?
C146 C145 H145 119.2 . . ?
N141 C146 C145 121.3(11) . . ?
N141 C146 H146 119.4 . . ?
C145 C146 H146 119.4 . . ?
C148 C147 C143 118.7(13) . . ?
C148 C147 H147 120.6 . . ?
C143 C147 H147 120.6 . . ?
C147 C148 C149 121.0(13) . . ?
C147 C148 H148 119.5 . . ?
C149 C148 H148 119.5 . . ?
C140 C149 C148 120.9(11) . . ?
C140 C149 H149 119.5 . . ?
C148 C149 H149 119.5 . . ?
C149 C140 C144 120.8(13) . . ?
C149 C140 H140 119.6 . . ?
C144 C140 H140 119.6 . . ?
O13B Cl1 O14A 57(2) . . ?
O13B Cl1 O12 114(2) . . ?
O14A Cl1 O12 125.1(13) . . ?
O13B Cl1 O11 122.9(15) . . ?
O14A Cl1 O11 113.9(11) . . ?
O12 Cl1 O11 113.6(6) . . ?
O13B Cl1 O13A 50(2) . . ?
O14A Cl1 O13A 104.6(18) . . ?
O12 Cl1 O13A 98.1(13) . . ?
O11 Cl1 O13A 93.8(10) . . ?
O13B Cl1 O14B 106(3) . . ?
O14A Cl1 O14B 50.9(15) . . ?
O12 Cl1 O14B 96.7(13) . . ?
O11 Cl1 O14B 98.1(8) . . ?
O13A Cl1 O14B 155.4(14) . . ?
O14A O13B Cl1 67(2) . . ?
O14A O13B O13A 144(3) . . ?
Cl1 O13B O13A 81(3) . . ?
O13B O13A Cl1 48.7(14) . . ?
O13B O14A O14B 129(3) . . ?
O13B O14A Cl1 56.4(17) . . ?
O14B O14A Cl1 75(2) . . ?
O14A O14B Cl1 54.5(13) . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         1.636
_refine_diff_density_min         -1.130
_refine_diff_density_rms         0.137

# start Validation Reply Form
_vrf_PLAT213_I                   
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PROBLEM: Atom N111 has ADP max/min Ratio ..... 5.6 oblate
RESPONSE: ...There is some disordering in the crystal and this disordering is reflected in
the thermal paprameters of N111 and O13B. No disordered model could be found for N111.
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_vrf_PLAT216_I                   
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PROBLEM: Disordered O13B (An/Solv) ADP max/min Ratio 14.7
RESPONSE: ...RESPONSE: ...There is some disordering in the crystal and this disordering is reflected in
the thermal paprameters of N111 and O13B. A partially disordered model for the perchlorate ion was
included in the model.
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# end Validation Reply Form

