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

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# 
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# Crystallographic Data Centre (CCDC).
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data_elod10_0m

_database_code_depnum_ccdc_archive 'CCDC 1046674'
_audit_update_record             
;
2015-02-04 deposited with the CCDC.
2015-04-07 downloaded from the CCDC.
;
_chemical_name_common            ?
_chemical_name_systematic        
"tris[4,4':2',2":4",4'"-quaterpyridine]ruthenium(II) bis(hexafluorophosphate) acetonitrile disolvate diethyl ether solvate"
_chemical_formula_moiety         
'C60 H42 N12 Ru1, 1(C4 H9 O), 2(F6 P), 2(C2 H3 N)'
_chemical_formula_sum            'C67.99 H56.99 F11.99 N14 O P2 Ru'
_chemical_formula_weight         1476.84
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0150 0.0070 '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'
F F 0.0600 0.0410 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0250 0.0140 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0389 0.0241 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2600 0.3350 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -0.0760 2.5660 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3'
_space_group_name_Hall           '-R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   17.6408(12)
_cell_length_b                   17.6408(12)
_cell_length_c                   44.355(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     11954.0(19)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    9774
_cell_measurement_temperature    100
_cell_measurement_theta_max      64.203
_cell_measurement_theta_min      2.601
_shelx_estimated_absorpt_T_max   0.875
_shelx_estimated_absorpt_T_min   0.782
_exptl_absorpt_coefficient_mu    1.721
_exptl_absorpt_correction_T_max  0.8893
_exptl_absorpt_correction_T_min  0.6936
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.1353 before and 0.0895 after correction.
The Ratio of minimum to maximum transmission is 0.7799.
The λ/2 correction factor is 0.00150.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_lustre     ?
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             4517
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile/diethyl ether'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_exptl_special_details           
;
X-ray crystallographic data for I were collected from a single crystal
sample, which was mounted on a loop fiber. Data were collected using
a Bruker Venture diffractometer equipped with a Photon 100 CMOS Detector,
a Helios MX optics and a Kappa goniometer. The crystal-to-detector distance 
was 4.0 cm, and the data collection was carried out in 1024 x 1024 pixel mode.
;

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0761
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            70653
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         53.893
_diffrn_reflns_theta_min         2.600
_diffrn_ambient_temperature      100.15
_diffrn_detector                 'CMOS Area detector'
_diffrn_detector_area_resol_mean 10.24
_diffrn_detector_type            'Bruker Photon 100 CMOS Detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker Venture Metaljet'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_collimation    'Focusing mirrors'
_diffrn_radiation_monochromator  'Helios MX Mirror Optics'
_diffrn_radiation_probe          X-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_source                   'Metal Jet'
_diffrn_source_target            Ga
_diffrn_source_type              'Gallium Liquid Metal Jet Source'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3687
_reflns_number_total             4875
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
'SAINT (2013) V8.34A; Bruker AXS Inc., Madison, WI 53719-1173.'
_computing_data_collection       
'APEX 2 (2013) Bruker AXS Inc., Madison, WI 53719-1173.'
_computing_data_reduction        
'SAINT (2013) V8.34A; Bruker AXS Inc., Madison, WI 53719-1173.'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         1.934
_refine_diff_density_min         -1.970
_refine_diff_density_rms         0.132
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         4875
_refine_ls_number_restraints     380
_refine_ls_R_factor_all          0.1188
_refine_ls_R_factor_gt           0.0872
_refine_ls_restrained_S_all      1.108
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1524P)²+71.5927P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2204
_refine_ls_wR_factor_ref         0.2673
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1A-C1A = N1B_$1-C1B_$1
 1 with sigma of 0.02
 C1A-C2A = C1B_$1-C2B_$1
 1.45 with sigma of 0.02
 C2A-N1A = C2B_$1-N1B_$1
 2.45 with sigma of 0.02
 O1E-C1E = O1E-C3E
 1.419 with sigma of 0.05
 O1E-C2E = O1E-C4E
 2.389 with sigma of 0.1
 C2E-C1E = C4E-C3E
 1.518 with sigma of 0.05
 C1E-C3E
 2.374 with sigma of 0.1
 C2E-C4E
 4.768 with sigma of 0.2
 P1-F1 \\sim P1-F2 \\sim P1-F3 \\sim P1-F4 \\sim P1-F5 \\sim P1-F6
 with sigma of 0.01
 F1-F6 \\sim F2-F5 \\sim F3-F4
 with sigma of 0.01
 F1-F2 \\sim F1-F3 \\sim F1-F4 \\sim F1-F5 \\sim F2-F3 \\sim F2-F4 \\sim F2-F6
\\sim F3-F5 \\sim F3-F6 \\sim F4-F5
 \\sim F4-F6 \\sim F5-F6
 with sigma of 0.01
 P1A-F1A \\sim P1A-F2A \\sim P1A-F3A \\sim P1A-F4A \\sim P1A-F5A \\sim P1A-F6A
 with sigma of 0.01
 F1A-F6A \\sim F2A-F5A \\sim F3A-F4A
 with sigma of 0.01
 F1A-F2A \\sim F1A-F3A \\sim F1A-F4A \\sim F1A-F5A \\sim F2A-F3A \\sim F2A-F4A
\\sim F2A-F6A \\sim F3A-F5A
 \\sim F3A-F6A \\sim F4A-F5A \\sim F4A-F6A \\sim F5A-F6A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
N1A \\sim C1A \\sim C2A: within 1.5A with sigma of 0.02 and sigma for terminal
atoms of 0.02
O1E \\sim C1E \\sim C2E \\sim C3E \\sim C4E: within 1.5A with sigma of 0.01 and
sigma for terminal atoms of 0.01
Uanis(N1B) \\sim Ueq, Uanis(C1B) \\sim Ueq, Uanis(C2B) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.03
4. Rigid body (RIGU) restrains
 P1, F1, F2, F3, F4, F5, F6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 P1A, F1A, F2A, F3A, F4A, F5A, F6A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N1B, C1B, C2B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1E, C1E, C2E, C3E, C4E, C4E
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1E, C1E, C2E, C3E, C4E
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: O1E(0.333) C1E(0.333) H1EA(0.333) H1EB(0.333) C2E(0.333)
 H2EA(0.333) H2EB(0.333) H2EC(0.333) C3E(0.333) H3E(0.333) C4E(0.333)
 H4EA(0.333) H4EB(0.333) H4EC(0.333) P1A(0.166) F1A(0.166) F2A(0.166)
 F3A(0.166) F4A(0.166) F5A(0.166) F6A(0.166) P1(0.5) F1(0.5) F2(0.5) F3(0.5)
 F4(0.5) F5(0.5) F6(0.5) N1B(0.5) C1B(0.5) C2B(0.5) H2BA(0.5) H2BB(0.5)
 H2BC(0.5) N1A(0.166) C1A(0.166) C2A(0.166) H2AA(0.166) H2AB(0.166) H2AC(0.166)
6.a Secondary CH2 refined with riding coordinates:
 C1E(H1EA,H1EB)
6.b Me refined with riding coordinates:
 C2E(H2EA,H2EB,H2EC), C4E(H4EA,H4EB,H4EC)
6.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
 C14(H14), C17(H17), C18(H18), C19(H19), C20(H20), C3E(H3E)
6.d Idealised Me refined with riding coordinates:
 C2A(H2AA,H2AB,H2AC)
6.e Idealised Me refined as rotating group:
 C2B(H2BA,H2BB,H2BC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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 0.3333 0.6667 0.40640(2) 0.0487(3) Uani 1 3 d S T P . .
N1 N 0.3093(3) 0.5572(3) 0.38234(9) 0.0489(10) Uani 1 1 d . . . . .
N2 N 0.3042(7) 0.2175(5) 0.29601(19) 0.122(3) Uani 1 1 d . . . . .
N3 N 0.4070(3) 0.6262(3) 0.42986(8) 0.0445(9) Uani 1 1 d . . . . .
N4 N 0.6875(5) 0.4862(5) 0.49091(13) 0.0866(18) Uani 1 1 d . . . . .
C1 C 0.2620(4) 0.5290(4) 0.35644(13) 0.0607(14) Uani 1 1 d . . . . .
H1 H 0.2308 0.5568 0.3498 0.073 Uiso 1 1 calc R . . . .
C2 C 0.2578(4) 0.4621(4) 0.33961(13) 0.0618(15) Uani 1 1 d . . . . .
H2 H 0.2257 0.4457 0.3213 0.074 Uiso 1 1 calc R . . . .
C3 C 0.2999(4) 0.4181(4) 0.34907(13) 0.0619(15) Uani 1 1 d . . . . .
C4 C 0.3456(4) 0.4447(4) 0.37638(12) 0.0562(13) Uani 1 1 d . . . . .
H4 H 0.3734 0.4146 0.3842 0.067 Uiso 1 1 calc R . . . .
C5 C 0.3502(4) 0.5146(4) 0.39204(12) 0.0518(13) Uani 1 1 d . . . . .
C6 C 0.3017(5) 0.3486(4) 0.33095(15) 0.0717(17) Uani 1 1 d . . . . .
C7 C 0.2971(5) 0.3504(5) 0.29964(16) 0.083(2) Uani 1 1 d . . . . .
H7 H 0.2934 0.3960 0.2896 0.100 Uiso 1 1 calc R . . . .
C8 C 0.2983(7) 0.2833(6) 0.28354(19) 0.106(3) Uani 1 1 d . . . . .
H8 H 0.2946 0.2844 0.2622 0.127 Uiso 1 1 calc R . . . .
C9 C 0.3050(8) 0.2157(6) 0.3264(2) 0.116(4) Uani 1 1 d . . . . .
H9 H 0.3057 0.1679 0.3360 0.139 Uiso 1 1 calc R . . . .
C10 C 0.3050(6) 0.2798(5) 0.34429(19) 0.095(3) Uani 1 1 d . . . . .
H10 H 0.3072 0.2765 0.3656 0.114 Uiso 1 1 calc R . . . .
C11 C 0.4582(4) 0.6671(4) 0.45334(11) 0.0530(13) Uani 1 1 d . . . . .
H11 H 0.4580 0.7168 0.4614 0.064 Uiso 1 1 calc R . . . .
C12 C 0.5113(4) 0.6400(4) 0.46633(12) 0.0563(14) Uani 1 1 d . . . . .
H12 H 0.5483 0.6721 0.4827 0.068 Uiso 1 1 calc R . . . .
C13 C 0.5113(3) 0.5664(4) 0.45586(11) 0.0497(12) Uani 1 1 d . . . . .
C14 C 0.4561(3) 0.5219(3) 0.43181(11) 0.0482(12) Uani 1 1 d . . . . .
H14 H 0.4535 0.4705 0.4240 0.058 Uiso 1 1 calc R . . . .
C15 C 0.4050(3) 0.5529(3) 0.41938(11) 0.0453(11) Uani 1 1 d . . . . .
C16 C 0.5721(4) 0.5381(4) 0.46785(11) 0.0549(13) Uani 1 1 d . . . . .
C17 C 0.6422(5) 0.5919(5) 0.48617(18) 0.0778(19) Uani 1 1 d . . . . .
H17 H 0.6525 0.6484 0.4915 0.093 Uiso 1 1 calc R . . . .
C18 C 0.6972(5) 0.5634(6) 0.49671(18) 0.084(2) Uani 1 1 d . . . . .
H18 H 0.7452 0.6022 0.5090 0.101 Uiso 1 1 calc R . . . .
C19 C 0.6177(6) 0.4324(6) 0.47455(18) 0.087(2) Uani 1 1 d . . . . .
H19 H 0.6077 0.3752 0.4707 0.105 Uiso 1 1 calc R . . . .
C20 C 0.5590(5) 0.4551(5) 0.46286(15) 0.0754(18) Uani 1 1 d . . . . .
H20 H 0.5100 0.4138 0.4515 0.090 Uiso 1 1 calc R . . . .
O1E O 0.430(2) 0.304(2) 0.4079(7) 0.151(9) Uani 0.333 1 d D U . A 2
C1E C 0.480(3) 0.283(3) 0.3894(8) 0.155(9) Uani 0.333 1 d D U . A 2
H1EA H 0.4433 0.2294 0.3774 0.186 Uiso 0.333 1 calc R . . A 2
H1EB H 0.5235 0.2751 0.4011 0.186 Uiso 0.333 1 calc R . . A 2
C2E C 0.525(3) 0.366(3) 0.3691(8) 0.148(11) Uani 0.333 1 d D U . A 2
H2EA H 0.5634 0.3603 0.3545 0.223 Uiso 0.333 1 calc R . . A 2
H2EB H 0.4799 0.3725 0.3583 0.223 Uiso 0.333 1 calc R . . A 2
H2EC H 0.5593 0.4178 0.3817 0.223 Uiso 0.333 1 calc R . . A 2
C3E C 0.377(3) 0.223(3) 0.4241(10) 0.157(10) Uani 0.333 1 d D U . A 2
H3E H 0.3819 0.1718 0.4239 0.188 Uiso 0.333 1 calc R . . A 2
C4E C 0.310(5) 0.238(5) 0.4415(18) 0.30(5) Uani 0.333 1 d D U . A 2
H4EA H 0.2714 0.1850 0.4532 0.457 Uiso 0.333 1 calc R . . A 2
H4EB H 0.3412 0.2873 0.4553 0.457 Uiso 0.333 1 calc R . . A 2
H4EC H 0.2752 0.2501 0.4273 0.457 Uiso 0.333 1 calc R . . A 2
P1A P 0.3519(10) 0.6490(8) 0.2711(2) 0.131(7) Uani 0.166 1 d D U . B -2
F1A F 0.3037(18) 0.6793(16) 0.2499(5) 0.152(9) Uani 0.166 1 d D U . B -2
F2A F 0.4034(17) 0.6433(17) 0.2442(4) 0.172(10) Uani 0.166 1 d D U . B -2
F3A F 0.4228(17) 0.7441(13) 0.2762(5) 0.166(10) Uani 0.166 1 d D U . B -2
F4A F 0.2807(17) 0.5535(12) 0.2657(5) 0.138(9) Uani 0.166 1 d D U . B -2
F5A F 0.2999(14) 0.6540(19) 0.2978(4) 0.151(10) Uani 0.166 1 d D U . B -2
F6A F 0.3997(14) 0.6180(15) 0.2921(4) 0.122(8) Uani 0.166 1 d D U . B -2
P1 P 0.1257(5) 0.2569(4) 0.44513(17) 0.166(3) Uani 0.5 1 d D U . C 1
F1 F 0.0435(8) 0.2546(10) 0.4326(3) 0.215(6) Uani 0.5 1 d D U . C 1
F2 F 0.1817(9) 0.3532(6) 0.4357(3) 0.197(5) Uani 0.5 1 d D U . C 1
F3 F 0.1422(9) 0.2280(8) 0.4143(3) 0.219(6) Uani 0.5 1 d D U . C 1
F4 F 0.1092(7) 0.2860(7) 0.4761(2) 0.148(4) Uani 0.5 1 d D U . C 1
F5 F 0.0700(10) 0.1605(7) 0.4548(3) 0.260(7) Uani 0.5 1 d D U . C 1
F6 F 0.2078(9) 0.2585(10) 0.4578(3) 0.259(7) Uani 0.5 1 d D U . C 1
N1B N 0.3913(14) 0.2989(11) 0.4157(5) 0.124(7) Uani 0.5 1 d D U . D 1
C1B C 0.3492(16) 0.2391(12) 0.4275(6) 0.118(6) Uani 0.5 1 d D U . D 1
C2B C 0.2926(17) 0.1453(10) 0.4267(7) 0.158(9) Uani 0.5 1 d D U . D 1
H2BA H 0.2471 0.1301 0.4114 0.237 Uiso 0.5 1 calc GR . . D 1
H2BB H 0.2651 0.1247 0.4465 0.237 Uiso 0.5 1 calc GR . . D 1
H2BC H 0.3271 0.1174 0.4217 0.237 Uiso 0.5 1 calc GR . . D 1
N1A N 0.066(4) 0.180(3) 0.4837(12) 0.140(17) Uani 0.166 1 d D U . E 2
C1A C 0.074(4) 0.232(4) 0.4714(13) 0.113(15) Uani 0.166 1 d D U . E 2
C2A C 0.088(3) 0.297(3) 0.4491(12) 0.092(13) Uani 0.166 1 d D U . E 2
H2AA H 0.0353 0.3020 0.4470 0.139 Uiso 0.166 1 calc R . . E 2
H2AB H 0.1021 0.2808 0.4296 0.139 Uiso 0.166 1 calc R . . E 2
H2AC H 0.1371 0.3541 0.4554 0.139 Uiso 0.166 1 calc R . . E 2


_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 2.056(4) 3_565 ?
Ru1 N1 2.056(4) . ?
Ru1 N1 2.056(4) 2_665 ?
Ru1 N3 2.052(4) 2_665 ?
Ru1 N3 2.052(4) . ?
Ru1 N3 2.052(4) 3_565 ?
N1 C1 1.359(7) . ?
N1 C5 1.347(7) . ?
N2 C8 1.337(12) . ?
N2 C9 1.349(12) . ?
N3 C11 1.330(7) . ?
N3 C15 1.357(7) . ?
N4 C18 1.310(10) . ?
N4 C19 1.333(10) . ?
C1 H1 0.9500 . ?
C1 C2 1.366(9) . ?
C2 H2 0.9500 . ?
C2 C3 1.380(9) . ?
C3 C4 1.400(8) . ?
C3 C6 1.480(9) . ?
C4 H4 0.9500 . ?
C4 C5 1.382(8) . ?
C5 C15 1.486(7) . ?
C6 C7 1.392(10) . ?
C6 C10 1.377(11) . ?
C7 H7 0.9500 . ?
C7 C8 1.391(11) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C9 C10 1.382(12) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C11 C12 1.374(8) . ?
C12 H12 0.9500 . ?
C12 C13 1.378(8) . ?
C13 C14 1.392(7) . ?
C13 C16 1.490(8) . ?
C14 H14 0.9500 . ?
C14 C15 1.381(7) . ?
C16 C17 1.385(9) . ?
C16 C20 1.381(9) . ?
C17 H17 0.9500 . ?
C17 C18 1.377(10) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C19 C20 1.385(10) . ?
C20 H20 0.9500 . ?
O1E C1E 1.39(3) . ?
O1E C3E 1.45(4) . ?
C1E H1EA 0.9900 . ?
C1E H1EB 0.9900 . ?
C1E C2E 1.56(4) . ?
C2E H2EA 0.9800 . ?
C2E H2EB 0.9800 . ?
C2E H2EC 0.9800 . ?
C3E H3E 0.9500 . ?
C3E C4E 1.53(4) . ?
C4E H4EA 0.9800 . ?
C4E H4EB 0.9800 . ?
C4E H4EC 0.9800 . ?
P1A F1A 1.532(15) . ?
P1A F2A 1.533(15) . ?
P1A F3A 1.528(15) . ?
P1A F4A 1.535(15) . ?
P1A F5A 1.530(15) . ?
P1A F6A 1.531(15) . ?
P1 F1 1.532(9) . ?
P1 F2 1.536(9) . ?
P1 F3 1.539(9) . ?
P1 F4 1.543(9) . ?
P1 F5 1.539(9) . ?
P1 F6 1.541(9) . ?
N1B C1B 1.076(16) . ?
C1B C2B 1.444(16) . ?
C2B H2BA 0.9800 . ?
C2B H2BB 0.9800 . ?
C2B H2BC 0.9800 . ?
N1A C1A 1.007(18) . ?
C1A C2A 1.449(18) . ?
C2A H2AA 0.9800 . ?
C2A H2AB 0.9800 . ?
C2A H2AC 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_3
_geom_angle_publ_flag
N1 Ru1 N1 95.49(15) 3_565 . ?
N1 Ru1 N1 95.49(15) 3_565 2_665 ?
N1 Ru1 N1 95.49(15) 2_665 . ?
N3 Ru1 N1 89.55(16) 3_565 . ?
N3 Ru1 N1 89.55(16) 2_665 3_565 ?
N3 Ru1 N1 172.73(16) 2_665 . ?
N3 Ru1 N1 78.78(17) 2_665 2_665 ?
N3 Ru1 N1 78.78(17) . . ?
N3 Ru1 N1 172.74(17) . 3_565 ?
N3 Ru1 N1 172.74(16) 3_565 2_665 ?
N3 Ru1 N1 78.79(17) 3_565 3_565 ?
N3 Ru1 N1 89.55(16) . 2_665 ?
N3 Ru1 N3 96.57(14) 2_665 3_565 ?
N3 Ru1 N3 96.57(14) 3_565 . ?
N3 Ru1 N3 96.57(14) 2_665 . ?
C1 N1 Ru1 125.7(4) . . ?
C5 N1 Ru1 116.2(3) . . ?
C5 N1 C1 117.8(5) . . ?
C8 N2 C9 116.2(7) . . ?
C11 N3 Ru1 125.8(4) . . ?
C11 N3 C15 118.2(4) . . ?
C15 N3 Ru1 116.0(3) . . ?
C18 N4 C19 116.1(6) . . ?
N1 C1 H1 118.8 . . ?
N1 C1 C2 122.5(6) . . ?
C2 C1 H1 118.8 . . ?
C1 C2 H2 119.8 . . ?
C1 C2 C3 120.4(5) . . ?
C3 C2 H2 119.8 . . ?
C2 C3 C4 117.2(6) . . ?
C2 C3 C6 122.8(5) . . ?
C4 C3 C6 120.0(6) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 C3 120.1(6) . . ?
C5 C4 H4 120.0 . . ?
N1 C5 C4 121.9(5) . . ?
N1 C5 C15 114.5(5) . . ?
C4 C5 C15 123.4(5) . . ?
C7 C6 C3 119.8(7) . . ?
C10 C6 C3 121.7(6) . . ?
C10 C6 C7 118.5(7) . . ?
C6 C7 H7 121.1 . . ?
C8 C7 C6 117.8(8) . . ?
C8 C7 H7 121.1 . . ?
N2 C8 C7 124.6(8) . . ?
N2 C8 H8 117.7 . . ?
C7 C8 H8 117.7 . . ?
N2 C9 H9 118.3 . . ?
N2 C9 C10 123.3(9) . . ?
C10 C9 H9 118.3 . . ?
C6 C10 C9 119.5(8) . . ?
C6 C10 H10 120.2 . . ?
C9 C10 H10 120.2 . . ?
N3 C11 H11 118.8 . . ?
N3 C11 C12 122.4(5) . . ?
C12 C11 H11 118.8 . . ?
C11 C12 H12 119.8 . . ?
C11 C12 C13 120.5(5) . . ?
C13 C12 H12 119.8 . . ?
C12 C13 C14 117.4(5) . . ?
C12 C13 C16 122.3(5) . . ?
C14 C13 C16 120.2(5) . . ?
C13 C14 H14 120.2 . . ?
C15 C14 C13 119.5(5) . . ?
C15 C14 H14 120.2 . . ?
N3 C15 C5 114.4(4) . . ?
N3 C15 C14 122.0(4) . . ?
C14 C15 C5 123.4(5) . . ?
C17 C16 C13 121.8(6) . . ?
C20 C16 C13 122.1(6) . . ?
C20 C16 C17 116.0(6) . . ?
C16 C17 H17 120.0 . . ?
C18 C17 C16 120.0(7) . . ?
C18 C17 H17 120.0 . . ?
N4 C18 C17 124.2(7) . . ?
N4 C18 H18 117.9 . . ?
C17 C18 H18 117.9 . . ?
N4 C19 H19 118.1 . . ?
N4 C19 C20 123.8(8) . . ?
C20 C19 H19 118.1 . . ?
C16 C20 C19 119.5(7) . . ?
C16 C20 H20 120.2 . . ?
C19 C20 H20 120.2 . . ?
C1E O1E C3E 102(3) . . ?
O1E C1E H1EA 111.7 . . ?
O1E C1E H1EB 111.7 . . ?
O1E C1E C2E 100(3) . . ?
H1EA C1E H1EB 109.5 . . ?
C2E C1E H1EA 111.7 . . ?
C2E C1E H1EB 111.7 . . ?
C1E C2E H2EA 109.5 . . ?
C1E C2E H2EB 109.5 . . ?
C1E C2E H2EC 109.5 . . ?
H2EA C2E H2EB 109.5 . . ?
H2EA C2E H2EC 109.5 . . ?
H2EB C2E H2EC 109.5 . . ?
O1E C3E H3E 127.7 . . ?
O1E C3E C4E 105(4) . . ?
C4E C3E H3E 127.7 . . ?
C3E C4E H4EA 109.5 . . ?
C3E C4E H4EB 109.5 . . ?
C3E C4E H4EC 109.5 . . ?
H4EA C4E H4EB 109.5 . . ?
H4EA C4E H4EC 109.5 . . ?
H4EB C4E H4EC 109.5 . . ?
F1A P1A F2A 89.8(4) . . ?
F1A P1A F4A 89.8(4) . . ?
F2A P1A F4A 89.7(4) . . ?
F3A P1A F1A 90.0(4) . . ?
F3A P1A F2A 90.1(4) . . ?
F3A P1A F4A 179.7(7) . . ?
F3A P1A F5A 90.3(4) . . ?
F3A P1A F6A 90.3(4) . . ?
F5A P1A F1A 90.1(4) . . ?
F5A P1A F2A 179.6(7) . . ?
F5A P1A F4A 89.9(4) . . ?
F5A P1A F6A 90.0(4) . . ?
F6A P1A F1A 179.6(6) . . ?
F6A P1A F2A 90.1(4) . . ?
F6A P1A F4A 89.8(4) . . ?
F1 P1 F2 90.5(4) . . ?
F1 P1 F3 90.2(4) . . ?
F1 P1 F4 89.9(4) . . ?
F1 P1 F5 89.9(4) . . ?
F1 P1 F6 179.5(6) . . ?
F2 P1 F3 90.0(4) . . ?
F2 P1 F4 89.9(4) . . ?
F2 P1 F5 179.5(6) . . ?
F2 P1 F6 90.0(4) . . ?
F3 P1 F4 179.9(8) . . ?
F3 P1 F5 90.2(4) . . ?
F3 P1 F6 89.9(4) . . ?
F5 P1 F4 89.9(4) . . ?
F5 P1 F6 89.6(4) . . ?
F6 P1 F4 90.0(4) . . ?
N1B C1B C2B 149(3) . . ?
C1B C2B H2BA 109.5 . . ?
C1B C2B H2BB 109.5 . . ?
C1B C2B H2BC 109.5 . . ?
H2BA C2B H2BB 109.5 . . ?
H2BA C2B H2BC 109.5 . . ?
H2BB C2B H2BC 109.5 . . ?
N1A C1A C2A 169(7) . . ?
C1A C2A H2AA 109.5 . . ?
C1A C2A H2AB 109.5 . . ?
C1A C2A H2AC 109.5 . . ?
H2AA C2A H2AB 109.5 . . ?
H2AA C2A H2AC 109.5 . . ?
H2AB C2A H2AC 109.5 . . ?

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
Ru1 N1 C1 C2 171.6(5) . . . . ?
Ru1 N1 C5 C4 -174.4(4) . . . . ?
Ru1 N1 C5 C15 1.5(6) . . . . ?
Ru1 N3 C11 C12 -174.4(4) . . . . ?
Ru1 N3 C15 C5 0.9(5) . . . . ?
Ru1 N3 C15 C14 175.6(4) . . . . ?
N1 C1 C2 C3 2.2(10) . . . . ?
N1 C5 C15 N3 -1.5(6) . . . . ?
N1 C5 C15 C14 -176.2(5) . . . . ?
N2 C9 C10 C6 1.8(17) . . . . ?
N3 C11 C12 C13 -2.1(9) . . . . ?
N4 C19 C20 C16 0.6(12) . . . . ?
C1 N1 C5 C4 0.5(8) . . . . ?
C1 N1 C5 C15 176.3(5) . . . . ?
C1 C2 C3 C4 0.5(9) . . . . ?
C1 C2 C3 C6 -176.5(6) . . . . ?
C2 C3 C4 C5 -2.6(9) . . . . ?
C2 C3 C6 C7 28.9(10) . . . . ?
C2 C3 C6 C10 -149.0(8) . . . . ?
C3 C4 C5 N1 2.2(9) . . . . ?
C3 C4 C5 C15 -173.2(5) . . . . ?
C3 C6 C7 C8 -179.5(7) . . . . ?
C3 C6 C10 C9 178.9(8) . . . . ?
C4 C3 C6 C7 -148.0(7) . . . . ?
C4 C3 C6 C10 34.1(10) . . . . ?
C4 C5 C15 N3 174.2(5) . . . . ?
C4 C5 C15 C14 -0.4(8) . . . . ?
C5 N1 C1 C2 -2.7(8) . . . . ?
C6 C3 C4 C5 174.4(6) . . . . ?
C6 C7 C8 N2 -0.6(16) . . . . ?
C7 C6 C10 C9 0.9(13) . . . . ?
C8 N2 C9 C10 -3.7(18) . . . . ?
C9 N2 C8 C7 3.1(17) . . . . ?
C10 C6 C7 C8 -1.5(12) . . . . ?
C11 N3 C15 C5 -176.6(4) . . . . ?
C11 N3 C15 C14 -1.9(7) . . . . ?
C11 C12 C13 C14 0.3(8) . . . . ?
C11 C12 C13 C16 175.7(5) . . . . ?
C12 C13 C14 C15 0.6(7) . . . . ?
C12 C13 C16 C17 -11.8(8) . . . . ?
C12 C13 C16 C20 164.3(6) . . . . ?
C13 C14 C15 N3 0.2(7) . . . . ?
C13 C14 C15 C5 174.4(5) . . . . ?
C13 C16 C17 C18 -179.8(6) . . . . ?
C13 C16 C20 C19 180.0(6) . . . . ?
C14 C13 C16 C17 163.5(6) . . . . ?
C14 C13 C16 C20 -20.4(8) . . . . ?
C15 N3 C11 C12 2.8(8) . . . . ?
C16 C13 C14 C15 -174.9(5) . . . . ?
C16 C17 C18 N4 -0.9(13) . . . . ?
C17 C16 C20 C19 -3.7(10) . . . . ?
C18 N4 C19 C20 2.5(12) . . . . ?
C19 N4 C18 C17 -2.4(12) . . . . ?
C20 C16 C17 C18 3.9(10) . . . . ?
C1E O1E C3E C4E -172(5) . . . . ?
C3E O1E C1E C2E 172(3) . . . . ?
_olex2_submission_special_instructions 'No special instructions were received'

_vrf_CELLZ01_elod10_0m           
;
PROBLEM: ...
RESPONSE: See PLAT041.
;
_vrf_FORMU01_elod10_0m           
;
PROBLEM: ...
RESPONSE: See PLAT041.
;
_vrf_PLAT041_elod10_0m           
;
PROBLEM: Calc. and Reported SumFormula Strings Differ
RESPONSE: This is due to rounding errors due to 1/6 and 1/3
occupancy. This applies to alerts PLAT068, FORMU01, CELLZ01,
PLAT042.
;
_vrf_PLAT042_elod10_0m           
;
PROBLEM: ...
RESPONSE: See PLAT041.
;
_vrf_PLAT068_elod10_0m           
;
PROBLEM: ...
RESPONSE: See PLAT041.
;
_vrf_PLAT082_elod10_0m           
;
PROBLEM: ...
RESPONSE: See PLAT973.
;
_vrf_PLAT083_elod10_0m           
;
PROBLEM: ...
RESPONSE: See PLAT973.
;
_vrf_PLAT084_elod10_0m           
;
PROBLEM: ...
RESPONSE: See RFACR01.
;
_vrf_PLAT250_elod10_0m           
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor ....        2.3/3.5
RESPONSE:
This is due to disordered ethyl ether and acetonitrile solvant molecules, 
the main molecule shows expected thermal motion.
;
_vrf_PLAT342_elod10_0m           
;
PROBLEM: ...
RESPONSE: See RFACR01.
;
_vrf_PLAT905_elod10_0m           
;
PROBLEM: Negative K value in the Analysis of Variance ...     -2.959   
RESPONSE: This apply only to the group Fc/Fc(max)   0.000 to 0.010. This group
is compromised of the lowest intensity peaks (calculated). It is the most 
subject to error since the observed data is (usually) more noisy. Since the 
Rint is high (due to poor quality of high angle data) this should be the
cause and not be a major concern for the structure quality.
;
_vrf_PLAT911_elod10_0m           
;
PROBLEM: Missing # FCF Refl Between THmin & STh/L= 0.600 12           
RESPONSE: These are omitted reflections where |Error/esd| > 5. These are 
mostly intense reflection that saturated the detector, but include 3 
reflections that had weaker observed value than calculated.
;
_vrf_PLAT972_elod10_0m           
;
PROBLEM: ...
RESPONSE: See PLAT973.
;
_vrf_PLAT973_elod10_0m           
;
PROBLEM: Check Calcd Positive Residual Density on Ru1 2.33 eA-3
RESPONSE: There is no doubt that the metal center is ruthenium from
other measurement techniques and from the synthetic approach. 
Residual density around the metal comes from absorption correction
error, which is not corrected beyond 2.33 eA-3 with different
mu*r values. Also no twinning was observed using CELLNOW or the
TWINROTMAT procedure in PLATON. This also applies to alerts PLAT972
and PLAT083.
;
_vrf_RADNT01_elod10_0m           
;
PROBLEM: The radiation type should contain one of the following
RESPONSE: Using a state of the art Gallium Liquid Metal Jet Source.
;
_vrf_RFACR01_elod10_0m           
;
PROBLEM: The value of the weighted R factor is > 0.25
RESPONSE: The data quality of the crystal was limited due to
presence of strong solvent disorder and by the decomposition
of the crystal due to the desolvatation of the cocrystalised
diethyl ether solvent molecule. This applies to PLAT084, 
PLAT342
;

loop_
_publcif_info_exptl_table_extra_item
sin_theta_over_lambda_max

loop_
_publcif_info_exptl_table_header_item
?
####################################################################### 
# 
# 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_dane33_0m

_database_code_depnum_ccdc_archive 'CCDC 1046675'
_audit_update_record             
;
2015-02-04 deposited with the CCDC.
2015-04-07 downloaded from the CCDC.
;


_audit_creation_date             2015-01-30
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_shelxl_version_number           2014/6
_publcif_datablock.id            {0cca4185-8c33-485d-a41b-837cd438fcd4}

_chemical_name_common            ?
_chemical_name_systematic        
"tris[4,4':2',2":4",4'"-quaterpyridine]ruthenium(II) bis(chloride) n hydrate"
_chemical_formula_moiety         'C60 H42 N12 Ru, 2(Cl), 5(O)'
_chemical_formula_sum            'C60 H42 Cl2 N12 O5 Ru'
_chemical_formula_weight         1183.02
_chemical_absolute_configuration ?
_chemical_melting_point          ?
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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru 0.0552 3.2960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      cubic
_space_group_IT_number           213
_space_group_name_H-M_alt        'P 41 3 2'
_space_group_name_Hall           'P 4bd 2ab 3'
loop_
_space_group_symop_operation_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'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'
'y+3/4, x+1/4, -z+1/4'
'-y+3/4, -x+3/4, -z+3/4'
'y+1/4, -x+1/4, z+3/4'
'-y+1/4, x+3/4, z+1/4'
'x+3/4, z+1/4, -y+1/4'
'-x+1/4, z+3/4, y+1/4'
'-x+3/4, -z+3/4, -y+3/4'
'x+1/4, -z+1/4, y+3/4'
'z+3/4, y+1/4, -x+1/4'
'z+1/4, -y+1/4, x+3/4'
'-z+1/4, y+3/4, x+1/4'
'-z+3/4, -y+3/4, -x+3/4'

_cell_length_a                   21.1118(3)
_cell_length_b                   21.1118(3)
_cell_length_c                   21.1118(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9409.7(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9803
_cell_measurement_temperature    100
_cell_measurement_theta_max      69.26
_cell_measurement_theta_min      2.96
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.168
_exptl_absorpt_correction_T_max  0.7534
_exptl_absorpt_correction_T_min  0.6230
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0900 before and 0.0791 after correction.
The Ratio of minimum to maximum transmission is 0.8269.
The λ/2 correction factor is 0.0015.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    0.835
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2416
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method 
"Re-crystallisation from solvent: waterédiethyl ether"
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_exptl_special_details           
;
X-ray crystallographic data for I were collected from a single crystal
sample, which was mounted on a loop fiber. Data were collected using
a Bruker Venture diffractometer equipped with a Photon 100 CMOS Detector,
a Helios MX optics and a Kappa goniometer. The crystal-to-detector distance 
was 4.0 cm, and the data collection was carried out in 1024 x 1024 pixel mode.
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0978
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            94438
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.568
_diffrn_reflns_theta_min         3.626
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_collimation    'Focusing mirrors'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_target            Ga
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.662
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                2708
_reflns_number_total             3021
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       
;
APEX 2 (2013) Bruker AXS Inc., Madison, WI 53719-1173.
;
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.747
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details 
;
 Flack x determined using 1021 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.029(8)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         3021
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0634
_refine_ls_restrained_S_all      1.005
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1426P)²+2.2050P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1737
_refine_ls_wR_factor_ref         0.1776
_refine_special_details          SQUEEZE
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
N2 \\sim C6 \\sim C7 \\sim C9 \\sim C10: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
3. Others
 Fixed Sof: Cl2(0.16667) O2(0.5) O1(0.333)
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
Ru Ru 0.6250 0.1250 0.3750 0.0361(3) Uani 1 6 d S T P . .
N1 N 0.55942(18) 0.16658(19) 0.43350(18) 0.0392(9) Uani 1 1 d . . . . .
N2 N 0.3697(3) 0.3604(5) 0.6301(3) 0.089(2) Uani 1 1 d . U . . .
C1 C 0.5243(2) 0.2147(2) 0.4088(2) 0.0390(10) Uani 1 1 d . . . . .
C2 C 0.4846(3) 0.2512(2) 0.4448(2) 0.0415(11) Uani 1 1 d . . . . .
H2 H 0.4617 0.2850 0.4258 0.050 Uiso 1 1 calc R . . . .
C3 C 0.4779(2) 0.2387(3) 0.5102(3) 0.0470(12) Uani 1 1 d . . . . .
C4 C 0.5116(3) 0.1875(3) 0.5331(3) 0.0507(13) Uani 1 1 d . . . . .
H4 H 0.5072 0.1761 0.5765 0.061 Uiso 1 1 calc R . . . .
C5 C 0.5513(3) 0.1526(3) 0.4952(3) 0.0451(12) Uani 1 1 d . . . . .
H5 H 0.5735 0.1176 0.5129 0.054 Uiso 1 1 calc R . . . .
C6 C 0.3946(4) 0.3797(5) 0.5777(4) 0.085(3) Uani 1 1 d . U . . .
H6 H 0.3884 0.4229 0.5668 0.101 Uiso 1 1 calc R . . . .
C7 C 0.4289(3) 0.3439(3) 0.5367(3) 0.0622(17) Uani 1 1 d . U . . .
H7 H 0.4459 0.3618 0.4991 0.075 Uiso 1 1 calc R . . . .
C8 C 0.4386(3) 0.2793(3) 0.5513(3) 0.0583(16) Uani 1 1 d . . . . .
C9 C 0.4112(3) 0.2582(4) 0.6060(3) 0.0679(19) Uani 1 1 d . U . . .
H9 H 0.4154 0.2150 0.6181 0.081 Uiso 1 1 calc R . . . .
C10 C 0.3778(4) 0.2994(5) 0.6433(3) 0.083(2) Uani 1 1 d . U . . .
H10 H 0.3593 0.2833 0.6811 0.099 Uiso 1 1 calc R . . . .
Cl2 Cl 0.4897(10) 0.3806(7) 0.7558(8) 0.080(5) Uani 0.1667 1 d . . . A 1
O2 O 0.4864(5) 0.4031(7) 0.7379(6) 0.061(3) Uani 0.5 1 d . . . B 2
O1 O 0.4437(9) 0.3793(8) 0.7978(7) 0.079(4) Uani 0.333 1 d . . . C 3
Cl1 Cl 0.3750 0.3750 0.3750 0.0571(8) Uani 1 6 d S T 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
Ru N1 2.052(4) . ?
Ru N1 2.052(4) 14 ?
Ru N1 2.052(4) 11_556 ?
Ru N1 2.052(4) 8_645 ?
Ru N1 2.052(4) 22_554 ?
Ru N1 2.052(4) 18_645 ?
N1 C1 1.361(6) . ?
N1 C5 1.346(7) . ?
N2 C6 1.291(12) . ?
N2 C10 1.330(13) . ?
C1 C1 1.465(10) 14 ?
C1 C2 1.369(7) . ?
C2 H2 0.9500 . ?
C2 C3 1.413(8) . ?
C3 C4 1.382(8) . ?
C3 C8 1.475(8) . ?
C4 H4 0.9500 . ?
C4 C5 1.374(8) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C6 C7 1.358(9) . ?
C7 H7 0.9500 . ?
C7 C8 1.412(10) . ?
C8 C9 1.366(10) . ?
C9 H9 0.9500 . ?
C9 C10 1.369(11) . ?
C10 H10 0.9500 . ?

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 Ru N1 86.6(2) . 18_645 ?
N1 Ru N1 77.6(2) 8_645 22_554 ?
N1 Ru N1 98.05(15) 18_645 22_554 ?
N1 Ru N1 98.05(15) 18_645 14 ?
N1 Ru N1 98.05(15) . 11_556 ?
N1 Ru N1 86.6(2) 22_554 11_556 ?
N1 Ru N1 86.6(2) 8_645 14 ?
N1 Ru N1 174.1(2) 11_556 14 ?
N1 Ru N1 174.1(2) 18_645 8_645 ?
N1 Ru N1 98.05(15) 22_554 14 ?
N1 Ru N1 77.6(2) 18_645 11_556 ?
N1 Ru N1 98.05(15) 8_645 11_556 ?
N1 Ru N1 174.1(2) . 22_554 ?
N1 Ru N1 77.6(2) . 14 ?
N1 Ru N1 98.05(15) . 8_645 ?
C1 N1 Ru 117.1(3) . . ?
C5 N1 Ru 125.0(3) . . ?
C5 N1 C1 117.7(4) . . ?
C6 N2 C10 115.6(6) . . ?
N1 C1 C1 113.9(3) . 14 ?
N1 C1 C2 122.8(4) . . ?
C2 C1 C1 123.2(3) . 14 ?
C1 C2 H2 120.1 . . ?
C1 C2 C3 119.9(5) . . ?
C3 C2 H2 120.1 . . ?
C2 C3 C8 121.5(5) . . ?
C4 C3 C2 115.9(5) . . ?
C4 C3 C8 122.6(5) . . ?
C3 C4 H4 119.0 . . ?
C5 C4 C3 122.0(5) . . ?
C5 C4 H4 119.0 . . ?
N1 C5 C4 121.6(5) . . ?
N1 C5 H5 119.2 . . ?
C4 C5 H5 119.2 . . ?
N2 C6 H6 117.0 . . ?
N2 C6 C7 126.1(9) . . ?
C7 C6 H6 117.0 . . ?
C6 C7 H7 120.8 . . ?
C6 C7 C8 118.3(8) . . ?
C8 C7 H7 120.8 . . ?
C7 C8 C3 120.9(6) . . ?
C9 C8 C3 123.0(6) . . ?
C9 C8 C7 116.0(6) . . ?
C8 C9 H9 120.1 . . ?
C8 C9 C10 119.8(8) . . ?
C10 C9 H9 120.1 . . ?
N2 C10 C9 124.2(8) . . ?
N2 C10 H10 117.9 . . ?
C9 C10 H10 117.9 . . ?

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
Ru N1 C1 C1 5.2(7) . . . 14 ?
Ru N1 C1 C2 -171.9(4) . . . . ?
Ru N1 C5 C4 172.2(4) . . . . ?
N1 C1 C2 C3 -1.4(8) . . . . ?
N2 C6 C7 C8 0.4(11) . . . . ?
C1 N1 C5 C4 -3.5(8) . . . . ?
C1 C1 C2 C3 -178.2(6) 14 . . . ?
C1 C2 C3 C4 -2.0(8) . . . . ?
C1 C2 C3 C8 176.3(5) . . . . ?
C2 C3 C4 C5 2.6(9) . . . . ?
C2 C3 C8 C7 -27.7(9) . . . . ?
C2 C3 C8 C9 154.5(6) . . . . ?
C3 C4 C5 N1 0.2(9) . . . . ?
C3 C8 C9 C10 176.9(6) . . . . ?
C4 C3 C8 C7 150.5(6) . . . . ?
C4 C3 C8 C9 -27.3(10) . . . . ?
C5 N1 C1 C1 -178.8(5) . . . 14 ?
C5 N1 C1 C2 4.2(8) . . . . ?
C6 N2 C10 C9 1.4(12) . . . . ?
C6 C7 C8 C3 -177.1(6) . . . . ?
C6 C7 C8 C9 0.9(10) . . . . ?
C7 C8 C9 C10 -1.1(10) . . . . ?
C8 C3 C4 C5 -175.7(6) . . . . ?
C8 C9 C10 N2 -0.1(12) . . . . ?
C10 N2 C6 C7 -1.5(12) . . . . ?
_olex2_submission_special_instructions 'No special instructions were received'
_platon_squeeze_details          ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.089 0.117 0.120 3992 1303 ' '

_platon_squeeze_void_probe_radius 1.20

_vrf_PLAT042_dane33_0m           
;
PROBLEM: ...
RESPONSE: The data quality of the crystal was limited due to
presence of strong solvent disorder and by the decomposition
of the crystal due to the desolvatation of the cocrystalised
water solvent molecule.
;
_vrf_PLAT094_dane33_0m           
;
PROBLEM: Ratio of Maximum / Minimum Residual Density .... 2.06 Report
RESPONSE: The high ratio comes form the remaining electron density around 
the  heavy metal (0.8) and the remaining electron density near carbon double
bonds (0.2). Note that the disordered solvent of this structure were modeled
 with SQUEEZE algorithm from the PLATON software. 
;
_vrf_PLAT250_dane33_0m           
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.1 Note
RESPONSE:
This is due to the pendant pyridyl group showing increased thermal motion in 
the plane of the pyridyl ring.
;
_vrf_PLAT304_dane33_0m           
;
PROBLEM: Non-Integer Number of Atoms

RESPONSE:  1/6 atom on a (322) local symmetry (6-fold), and a group
 of disordered atoms in the same vicinity totalizing an occupancy of 1. 
;
_vrf_PLAT311_dane33_0m           
;
PROBLEM:Isolated Disordered Oxygen Atom (No H?s ?)

RESPONSE:  No potential H-bond acceptor present to define the protons, 
see _publ_section_exptl_refinement for details.
;
_vrf_PLAT342_dane33_0m           
;
PROBLEM: Low Bond Precision on C-C Bonds ............... 0.0088 Ang.
RESPONSE: The data quality of the crystal was limited due to
presence of strong solvent disorder and by the decomposition
of the crystal due to the desolvatation of the cocrystalised
water solvent molecule.
;
_vrf_PLAT606_dane33_0m           
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure

RESPONSE: Disordered solvent molecules in channels were removed
by applying SQUEEZE see _publ_section_exptl_refinement for details.
;
_vrf_PLAT910_dane33_0m           
;
PROBLEM:Missing # of FCF Reflection(s) Below Th(Min) ....

RESPONSE: See PLAT913
;
_vrf_PLAT911_dane33_0m           
;
PROBLEM: Missing # FCF Refl Between THmin & STh/L= 0.600 5

RESPONSE: These are omitted reflections where |Error/esd| > 10. 
;
_vrf_PLAT913_dane33_0m           
;
PROBLEM:Missing # of Very Strong Reflections in FCF ....

RESPONSE: Reflection 0 1 1 saturated the detector, 
leading to a (Iobs-Icalc)/Iobs(sigma)<-100 and was thus removed. 
;

