# Electronic Supplementary Material (ESI) for Chemical Science.
# 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_jf1_91
_database_code_depnum_ccdc_archive 'CCDC 1059343'
_audit_update_record             
;
2015-04-13 deposited with the CCDC.
2015-06-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;

_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C50 H52 N6 O16 P2 Ru, C3 H6 O, 8(H2 O)'
_chemical_formula_sum            'C53 H69 N6 O25 P2 Ru'
_chemical_formula_weight         1353.15

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'
P P 0.2955 0.4335 '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           orthorhombic
_symmetry_space_group_name_H-M   Pnna

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

_cell_length_a                   21.3561(4)
_cell_length_b                   19.4016(3)
_cell_length_c                   14.9635(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6200.01(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9898
_cell_measurement_theta_min      3.61
_cell_measurement_theta_max      67.88

_exptl_crystal_description       lath
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2812
_exptl_absorpt_coefficient_mu    3.271
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1794
_exptl_absorpt_correction_T_max  0.5607
_exptl_absorpt_process_details   'Bruker SADABS'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\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         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            50722
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_av_sigmaI/netI    0.0209
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.61
_diffrn_reflns_theta_max         69.17
_reflns_number_total             5616
_reflns_number_gt                4727
_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, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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)+(0.0917P)²+14.7364P] where P=(Fo²+2Fc²)/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         5616
_refine_ls_number_parameters     404
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0680
_refine_ls_wR_factor_ref         0.1922
_refine_ls_wR_factor_gt          0.1842
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_restrained_S_all      1.108
_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
C1 C 0.3377(2) 0.1696(2) 0.3442(3) 0.0452(10) Uani 1 1 d . . .
H1 H 0.3304 0.1978 0.3950 0.054 Uiso 1 1 calc R . .
C2 C 0.3852(2) 0.1206(3) 0.3475(4) 0.0527(12) Uani 1 1 d . . .
H2 H 0.4098 0.1160 0.4000 0.063 Uiso 1 1 calc R . .
C3 C 0.3964(2) 0.0791(3) 0.2755(4) 0.0519(12) Uani 1 1 d . . .
H3 H 0.4285 0.0453 0.2780 0.062 Uiso 1 1 calc R . .
C4 C 0.3600(2) 0.0868(2) 0.1974(3) 0.0481(11) Uani 1 1 d . . .
C5 C 0.3137(2) 0.1378(2) 0.1987(3) 0.0429(10) Uani 1 1 d . . .
C6 C 0.2760(2) 0.1499(2) 0.1212(3) 0.0449(10) Uani 1 1 d . . .
C7 C 0.2834(2) 0.1088(3) 0.0447(3) 0.0499(11) Uani 1 1 d . . .
C8 C 0.2454(3) 0.1232(3) -0.0290(4) 0.0595(14) Uani 1 1 d . . .
H8 H 0.2484 0.0964 -0.0820 0.071 Uiso 1 1 calc R . .
C9 C 0.2042(3) 0.1760(3) -0.0236(4) 0.0649(15) Uani 1 1 d . . .
H9 H 0.1782 0.1863 -0.0734 0.078 Uiso 1 1 calc R . .
C10 C 0.1992(3) 0.2159(3) 0.0543(4) 0.0556(13) Uani 1 1 d . . .
H10 H 0.1699 0.2527 0.0560 0.067 Uiso 1 1 calc R . .
C11 C 0.3675(2) 0.0454(3) 0.1179(4) 0.0527(12) Uani 1 1 d . . .
C12 C 0.3300(3) 0.0553(3) 0.0452(4) 0.0542(12) Uani 1 1 d . . .
C13 C 0.4018(3) -0.0717(3) 0.1078(5) 0.0649(15) Uani 1 1 d . . .
H13A H 0.3716 -0.0782 0.0583 0.078 Uiso 1 1 calc R . .
H13B H 0.3833 -0.0907 0.1633 0.078 Uiso 1 1 calc R . .
C14 C 0.4624(3) -0.1067(3) 0.0872(6) 0.083(2) Uani 1 1 d . . .
H14A H 0.4825 -0.0840 0.0353 0.100 Uiso 1 1 calc R . .
H14B H 0.4910 -0.1026 0.1390 0.100 Uiso 1 1 calc R . .
C15 C 0.5046(4) -0.2058(4) 0.0237(6) 0.103(3) Uani 1 1 d . . .
H15A H 0.4988 -0.2563 0.0263 0.124 Uiso 1 1 calc R . .
H15B H 0.5432 -0.1948 0.0575 0.124 Uiso 1 1 calc R . .
C16 C 0.5147(5) -0.1857(5) -0.0720(8) 0.122(4) Uani 1 1 d . . .
H16A H 0.5264 -0.1364 -0.0762 0.146 Uiso 1 1 calc R . .
H16B H 0.5487 -0.2136 -0.0986 0.146 Uiso 1 1 calc R . .
C17 C 0.4541(6) -0.1658(5) -0.2034(6) 0.124(4) Uani 1 1 d . . .
H17A H 0.4970 -0.1685 -0.2284 0.149 Uiso 1 1 calc R . .
H17B H 0.4266 -0.1929 -0.2433 0.149 Uiso 1 1 calc R . .
C18 C 0.4349(7) -0.0969(6) -0.2080(8) 0.159(5) Uani 1 1 d . . .
H18A H 0.4693 -0.0690 -0.1824 0.191 Uiso 1 1 calc R . .
H18B H 0.4326 -0.0850 -0.2722 0.191 Uiso 1 1 calc R . .
C19 C 0.3693(5) -0.0045(4) -0.1781(5) 0.097(3) Uani 1 1 d . . .
H19A H 0.3249 0.0013 -0.1959 0.116 Uiso 1 1 calc R . .
H19B H 0.3956 0.0156 -0.2259 0.116 Uiso 1 1 calc R . .
C20 C 0.3806(4) 0.0347(4) -0.0926(5) 0.085(2) Uani 1 1 d . . .
H20A H 0.4227 0.0237 -0.0687 0.102 Uiso 1 1 calc R . .
H20B H 0.3785 0.0849 -0.1039 0.102 Uiso 1 1 calc R . .
C21 C 0.1004(2) 0.2171(2) 0.2742(3) 0.0454(11) Uani 1 1 d . . .
C22 C 0.0472(2) 0.1850(2) 0.3066(4) 0.0516(12) Uani 1 1 d . . .
H22 H 0.0073 0.2050 0.2965 0.062 Uiso 1 1 calc R . .
C23 C 0.0519(2) 0.1231(3) 0.3543(4) 0.0520(12) Uani 1 1 d . . .
C24 C 0.1108(2) 0.0950(3) 0.3640(4) 0.0518(12) Uani 1 1 d . . .
H24 H 0.1158 0.0525 0.3946 0.062 Uiso 1 1 calc R . .
C25 C 0.1627(2) 0.1282(2) 0.3298(3) 0.0476(11) Uani 1 1 d . . .
H25 H 0.2028 0.1077 0.3370 0.057 Uiso 1 1 calc R . .
N1 N 0.30217(18) 0.1783(2) 0.2719(3) 0.0433(9) Uani 1 1 d . . .
N2 N 0.23450(18) 0.2034(2) 0.1260(3) 0.0453(9) Uani 1 1 d . . .
N3 N 0.15803(18) 0.1890(2) 0.2863(3) 0.0445(9) Uani 1 1 d . . .
O1 O 0.41652(17) 0.00006(18) 0.1188(3) 0.0638(10) Uani 1 1 d . . .
O2 O 0.4525(2) -0.1738(2) 0.0685(4) 0.0923(15) Uani 1 1 d . . .
O3 O 0.4548(4) -0.1985(3) -0.1196(4) 0.112(2) Uani 1 1 d . . .
O4 O 0.3823(4) -0.0743(3) -0.1711(5) 0.147(3) Uani 1 1 d . . .
O5 O 0.3336(2) 0.01509(19) -0.0296(3) 0.0638(10) Uani 1 1 d . . .
O6 O -0.01515(19) 0.00937(19) 0.3780(3) 0.0689(11) Uani 1 1 d . . .
O7 O -0.0716(2) 0.1228(3) 0.3824(4) 0.1022(19) Uani 1 1 d . . .
O8 O 0.0006(2) 0.0878(2) 0.5102(3) 0.0801(13) Uani 1 1 d . . .
P2 P -0.01489(7) 0.08543(7) 0.41105(12) 0.0665(5) Uani 1 1 d . . .
Ru1 Ru 0.23191(2) 0.2500 0.2500 0.04137(19) Uani 1 2 d S . .
O9 O 0.2500 0.0000 0.4106(6) 0.105(3) Uani 1 2 d S . .
C26 C 0.3141(5) 0.0262(8) 0.5564(9) 0.176(6) Uani 1 1 d D . .
H26A H 0.3491 -0.0042 0.5410 0.264 Uiso 1 1 calc R . .
H26B H 0.3070 0.0248 0.6211 0.264 Uiso 1 1 calc R . .
H26C H 0.3240 0.0735 0.5382 0.264 Uiso 1 1 calc R . .
C27 C 0.2500 0.0000 0.5038(18) 0.169(8) Uani 1 2 d SD . .
O1W O 0.8468(3) 0.2250(3) 0.4502(4) 0.0994(16) Uani 1 1 d . . .
O2W O 0.8819(5) 0.1814(4) 0.2223(5) 0.165(3) Uani 1 1 d . . .
O3W O 0.3992(3) 0.6776(3) 0.9353(4) 0.1101(18) Uani 1 1 d . . .
O4W O 0.2241(10) 0.3609(12) 0.9219(14) 0.234(13) Uani 0.50 1 d P . .
O5W O 0.2453(8) 0.1347(16) 0.7497(9) 0.199(12) 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
C1 N1 1.332(6) . ?
C1 C2 1.391(7) . ?
C2 C3 1.367(8) . ?
C3 C4 1.411(7) . ?
C4 C5 1.400(7) . ?
C4 C11 1.444(7) . ?
C5 N1 1.369(6) . ?
C5 C6 1.431(7) . ?
C6 N2 1.367(6) . ?
C6 C7 1.403(7) . ?
C7 C8 1.399(8) . ?
C7 C12 1.437(8) . ?
C8 C9 1.352(9) . ?
C9 C10 1.403(8) . ?
C10 N2 1.334(6) . ?
C11 C12 1.364(8) . ?
C11 O1 1.368(6) . ?
C12 O5 1.367(6) . ?
C13 O1 1.438(6) . ?
C13 C14 1.495(8) . ?
C14 O2 1.349(8) . ?
C15 O2 1.440(8) . ?
C15 C16 1.499(13) . ?
C16 O3 1.486(12) . ?
C17 C18 1.399(13) . ?
C17 O3 1.405(11) . ?
C18 O4 1.326(12) . ?
C19 O4 1.386(9) . ?
C19 C20 1.508(10) . ?
C20 O5 1.428(7) . ?
C21 N3 1.359(6) . ?
C21 C22 1.382(7) . ?
C21 C21 1.469(9) 4 ?
C22 C23 1.401(7) . ?
C23 C24 1.379(7) . ?
C23 P2 1.813(5) . ?
C24 C25 1.380(7) . ?
C25 N3 1.352(6) . ?
N1 Ru1 2.073(4) . ?
N2 Ru1 2.065(4) . ?
N3 Ru1 2.046(4) . ?
O6 P2 1.556(4) . ?
O7 P2 1.475(5) . ?
O8 P2 1.521(5) . ?
Ru1 N3 2.046(4) 4 ?
Ru1 N2 2.065(4) 4 ?
Ru1 N1 2.073(4) 4 ?
O9 C27 1.39(3) . ?
C26 C27 1.658(14) . ?
C27 C26 1.659(14) 2 ?

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 C1 C2 122.0(5) . . ?
C3 C2 C1 120.1(5) . . ?
C2 C3 C4 119.6(5) . . ?
C5 C4 C3 116.9(5) . . ?
C5 C4 C11 118.9(5) . . ?
C3 C4 C11 124.3(5) . . ?
N1 C5 C4 122.9(4) . . ?
N1 C5 C6 116.9(4) . . ?
C4 C5 C6 120.1(4) . . ?
N2 C6 C7 123.2(4) . . ?
N2 C6 C5 116.5(4) . . ?
C7 C6 C5 120.3(4) . . ?
C8 C7 C6 117.7(5) . . ?
C8 C7 C12 123.4(5) . . ?
C6 C7 C12 118.9(5) . . ?
C9 C8 C7 118.7(5) . . ?
C8 C9 C10 121.2(5) . . ?
N2 C10 C9 121.6(5) . . ?
C12 C11 O1 123.3(5) . . ?
C12 C11 C4 120.9(5) . . ?
O1 C11 C4 115.7(5) . . ?
C11 C12 O5 122.6(5) . . ?
C11 C12 C7 120.8(5) . . ?
O5 C12 C7 116.6(5) . . ?
O1 C13 C14 105.8(5) . . ?
O2 C14 C13 110.1(6) . . ?
O2 C15 C16 116.4(8) . . ?
O3 C16 C15 106.9(7) . . ?
C18 C17 O3 118.6(8) . . ?
O4 C18 C17 123.0(10) . . ?
O4 C19 C20 113.3(8) . . ?
O5 C20 C19 108.2(6) . . ?
N3 C21 C22 121.1(4) . . ?
N3 C21 C21 114.5(3) . 4 ?
C22 C21 C21 124.4(3) . 4 ?
C21 C22 C23 120.4(5) . . ?
C24 C23 C22 117.2(5) . . ?
C24 C23 P2 120.7(4) . . ?
C22 C23 P2 121.9(4) . . ?
C23 C24 C25 120.7(5) . . ?
N3 C25 C24 121.7(4) . . ?
C1 N1 C5 118.4(4) . . ?
C1 N1 Ru1 128.7(3) . . ?
C5 N1 Ru1 112.9(3) . . ?
C10 N2 C6 117.6(5) . . ?
C10 N2 Ru1 128.9(4) . . ?
C6 N2 Ru1 113.4(3) . . ?
C25 N3 C21 118.8(4) . . ?
C25 N3 Ru1 125.1(3) . . ?
C21 N3 Ru1 115.6(3) . . ?
C11 O1 C13 117.0(4) . . ?
C14 O2 C15 112.9(6) . . ?
C17 O3 C16 111.2(8) . . ?
C18 O4 C19 117.6(8) . . ?
C12 O5 C20 115.4(4) . . ?
O7 P2 O8 116.6(3) . . ?
O7 P2 O6 111.8(3) . . ?
O8 P2 O6 109.9(2) . . ?
O7 P2 C23 108.1(3) . . ?
O8 P2 C23 105.9(3) . . ?
O6 P2 C23 103.7(2) . . ?
N3 Ru1 N3 79.1(2) 4 . ?
N3 Ru1 N2 92.06(16) 4 . ?
N3 Ru1 N2 90.31(16) . . ?
N3 Ru1 N2 90.31(16) 4 4 ?
N3 Ru1 N2 92.06(16) . 4 ?
N2 Ru1 N2 176.9(2) . 4 ?
N3 Ru1 N1 97.35(15) 4 4 ?
N3 Ru1 N1 171.43(15) . 4 ?
N2 Ru1 N1 97.64(15) . 4 ?
N2 Ru1 N1 80.11(15) 4 4 ?
N3 Ru1 N1 171.43(15) 4 . ?
N3 Ru1 N1 97.35(15) . . ?
N2 Ru1 N1 80.11(15) . . ?
N2 Ru1 N1 97.64(15) 4 . ?
N1 Ru1 N1 87.2(2) 4 . ?
O9 C27 C26 118.3(10) . . ?
O9 C27 C26 118.3(10) . 2 ?
C26 C27 C26 123.4(19) . 2 ?

_diffrn_measured_fraction_theta_max 0.968
_diffrn_reflns_theta_full        69.17
_diffrn_measured_fraction_theta_full 0.968
_refine_diff_density_max         1.000
_refine_diff_density_min         -0.704
_refine_diff_density_rms         0.100
_exptl_crystal_recrystallization_method 
'Vapour diffusion - acetone into aqueous solution of compound'
_chemical_properties_physical    Photo-sensitive
_exptl_crystal_preparation       Luminescent
