#------------------------------------------------------------------------------
#$Date: 2018-12-01 01:15:33 +0200 (Sat, 01 Dec 2018) $
#$Revision: 212256 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/26/7122668.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7122668
loop_
_publ_author_name
'Toda, Tatsuro'
'Suzuki, Satoshi'
'Kuwata, Shigeki'
_publ_section_title
;
 Metallo-supramolecular assembly of protic pincer-type complexes:
 encapsulation of dinitrogen and carbon disulfide into
 multiproton-responsive diruthenium cage
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C8CC08384C
_journal_year                    2018
_chemical_formula_moiety         'C108 H112 N10 P4 Ru2, 2(H2 O), 1.5(C7 H8)'
_chemical_formula_sum            'C118.5 H128 N10 O2 P4 Ru2'
_chemical_formula_weight         2050.42
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2018-11-23 deposited with the CCDC.
2018-11-30 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                120.0000
_cell_formula_units_Z            9
_cell_length_a                   47.685(5)
_cell_length_b                   47.685(5)
_cell_length_c                   12.1985(16)
_cell_measurement_reflns_used    12862
_cell_measurement_temperature    93
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.08
_cell_volume                     24022(5)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.2.5'
_computing_publication_material  'CrystalStructure 4.2.5 (Rigaku, 2017)'
_computing_structure_refinement  'SHELXL Version 2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0706
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       61
_diffrn_reflns_limit_h_min       -61
_diffrn_reflns_limit_k_max       61
_diffrn_reflns_limit_k_min       -61
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            88358
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.374
_diffrn_reflns_theta_min         3.081
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.398
_exptl_absorpt_correction_T_max  0.961
_exptl_absorpt_correction_T_min  0.738
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             9657.00
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Toluene'
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.100
_refine_diff_density_max         4.36
_refine_diff_density_min         -0.94
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     533
_refine_ls_number_reflns         11981
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0649
_refine_ls_shift/su_max          0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.1209P)²+57.3279P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1800
_refine_ls_wR_factor_ref         0.1914
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9852
_reflns_number_total             11981
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            c8cc08384c2.cif
_cod_data_source_block           compound3-2H2O-C7H8
_cod_original_cell_volume        24021(5)
_cod_database_code               7122668
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'
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 0.51456(2) 0.45485(2) 0.44111(2) 0.01844(11) Uani 1 1 d . . . . .
P1 P 0.54153(2) 0.48462(2) 0.27847(7) 0.01949(18) Uani 1 1 d . . . . .
P2 P 0.51290(2) 0.57582(2) 0.39881(7) 0.02136(19) Uani 1 1 d . . . . .
O1 O 0.56567(8) 0.54048(7) 0.6003(3) 0.0445(8) Uani 1 1 d . . . . .
N1 N 0.57577(7) 0.49069(7) 0.6134(2) 0.0248(6) Uani 1 1 d . . . . .
H1 H 0.5716 0.5054 0.6401 0.030 Uiso 1 1 calc R U . . .
N2 N 0.55726(6) 0.46779(6) 0.5367(2) 0.0223(6) Uani 1 1 d . . . . .
N3 N 0.45286(7) 0.42648(7) 0.2734(2) 0.0260(6) Uani 1 1 d . . . . .
N4 N 0.47793(6) 0.42514(6) 0.3249(2) 0.0217(6) Uani 1 1 d . . . . .
N5 N 0.50297(6) 0.49045(6) 0.4873(2) 0.0210(5) Uani 1 1 d . . . . .
C1 C 0.60162(8) 0.48737(9) 0.6423(3) 0.0269(7) Uani 1 1 d . . . . .
C2 C 0.59951(8) 0.46130(9) 0.5844(3) 0.0271(7) Uani 1 1 d . . . . .
H2 H 0.6141 0.4532 0.5879 0.033 Uiso 1 1 calc R U . . .
C3 C 0.57140(8) 0.44929(8) 0.5193(3) 0.0234(7) Uani 1 1 d . . . . .
C4 C 0.52626(8) 0.42096(8) 0.4000(3) 0.0220(6) Uani 1 1 d . . . . .
C5 C 0.55399(8) 0.42220(8) 0.4433(3) 0.0230(7) Uani 1 1 d . . . . .
C6 C 0.56143(8) 0.39793(8) 0.4179(3) 0.0267(7) Uani 1 1 d . . . . .
H3 H 0.5801 0.3988 0.4492 0.032 Uiso 1 1 calc R U . . .
C7 C 0.54159(9) 0.37231(8) 0.3464(3) 0.0290(8) Uani 1 1 d . . . . .
C8 C 0.51426(9) 0.37178(8) 0.3014(3) 0.0275(7) Uani 1 1 d . . . . .
H4 H 0.5009 0.3549 0.2521 0.033 Uiso 1 1 calc R U . . .
C9 C 0.50628(8) 0.39561(8) 0.3279(3) 0.0237(7) Uani 1 1 d . . . . .
C10 C 0.47915(8) 0.39869(8) 0.2878(3) 0.0240(7) Uani 1 1 d . . . . .
C11 C 0.45399(9) 0.38218(8) 0.2099(3) 0.0284(8) Uani 1 1 d . . . . .
H5 H 0.4488 0.3630 0.1706 0.034 Uiso 1 1 calc R U . . .
C12 C 0.43842(8) 0.40059(8) 0.2042(3) 0.0271(7) Uani 1 1 d . . . . .
C13 C 0.62642(9) 0.50942(10) 0.7277(3) 0.0343(8) Uani 1 1 d . . . . .
C14 C 0.64036(17) 0.54559(16) 0.6946(6) 0.0766(17) Uiso 1 1 d . . . . .
H6 H 0.6228 0.5506 0.6923 0.115 Uiso 1 1 calc R U . . .
H7 H 0.6566 0.5596 0.7486 0.115 Uiso 1 1 calc R U . . .
H8 H 0.6505 0.5493 0.6221 0.115 Uiso 1 1 calc R U . . .
C15 C 0.61044(16) 0.50315(16) 0.8406(5) 0.0718(16) Uiso 1 1 d . . . . .
H9 H 0.5919 0.5067 0.8372 0.108 Uiso 1 1 calc R U . . .
H10 H 0.6030 0.4807 0.8626 0.108 Uiso 1 1 calc R U . . .
H11 H 0.6262 0.5180 0.8942 0.108 Uiso 1 1 calc R U . . .
C16 C 0.65519(14) 0.50425(14) 0.7288(5) 0.0639(14) Uiso 1 1 d . . . . .
H12 H 0.6649 0.5084 0.6556 0.096 Uiso 1 1 calc R U . . .
H13 H 0.6713 0.5191 0.7816 0.096 Uiso 1 1 calc R U . . .
H14 H 0.6481 0.4819 0.7500 0.096 Uiso 1 1 calc R U . . .
C17 C 0.40919(10) 0.39457(10) 0.1354(4) 0.0392(10) Uani 1 1 d . . . . .
C18 C 0.41553(18) 0.42380(17) 0.0725(6) 0.0812(18) Uiso 1 1 d . . . . .
H15 H 0.3963 0.4191 0.0295 0.122 Uiso 1 1 calc R U . . .
H16 H 0.4205 0.4416 0.1234 0.122 Uiso 1 1 calc R U . . .
H17 H 0.4339 0.4300 0.0232 0.122 Uiso 1 1 calc R U . . .
C19 C 0.38003(17) 0.38546(18) 0.2153(6) 0.0823(19) Uiso 1 1 d . . . . .
H18 H 0.3755 0.3662 0.2575 0.123 Uiso 1 1 calc R U . . .
H19 H 0.3855 0.4035 0.2655 0.123 Uiso 1 1 calc R U . . .
H20 H 0.3608 0.3810 0.1726 0.123 Uiso 1 1 calc R U . . .
C20 C 0.39840(15) 0.36489(15) 0.0620(5) 0.0677(15) Uiso 1 1 d . . . . .
H21 H 0.3945 0.3463 0.1071 0.102 Uiso 1 1 calc R U . . .
H22 H 0.3784 0.3601 0.0238 0.102 Uiso 1 1 calc R U . . .
H23 H 0.4154 0.3693 0.0081 0.102 Uiso 1 1 calc R U . . .
C21 C 0.54871(10) 0.34507(9) 0.3182(4) 0.0359(9) Uani 1 1 d . . . . .
C22 C 0.57921(12) 0.34907(12) 0.3786(5) 0.0576(14) Uani 1 1 d . . . . .
H24 H 0.5828 0.3312 0.3583 0.086 Uiso 1 1 calc R U . . .
H25 H 0.5981 0.3697 0.3576 0.086 Uiso 1 1 calc R U . . .
H26 H 0.5759 0.3488 0.4580 0.086 Uiso 1 1 calc R U . . .
C23 C 0.55450(13) 0.34501(12) 0.1927(4) 0.0520(12) Uani 1 1 d . . . . .
H27 H 0.5590 0.3276 0.1750 0.078 Uiso 1 1 calc R U . . .
H28 H 0.5351 0.3415 0.1531 0.078 Uiso 1 1 calc R U . . .
H29 H 0.5730 0.3659 0.1711 0.078 Uiso 1 1 calc R U . . .
C24 C 0.51972(12) 0.31220(10) 0.3531(4) 0.0478(11) Uani 1 1 d . . . . .
H30 H 0.5243 0.2948 0.3352 0.072 Uiso 1 1 calc R U . . .
H31 H 0.5163 0.3123 0.4323 0.072 Uiso 1 1 calc R U . . .
H32 H 0.5002 0.3086 0.3141 0.072 Uiso 1 1 calc R U . . .
C25 C 0.58350(7) 0.51929(7) 0.2801(2) 0.0238(7) Uani 1 1 d D . . . .
C26 C 0.60520(12) 0.51989(14) 0.3588(4) 0.0240(14) Uiso 0.5 1 d D . P A 1
H33 H 0.5979 0.5031 0.4117 0.029 Uiso 0.5 1 calc R U P A 1
C27 C 0.63735(13) 0.54495(14) 0.3604(5) 0.0283(15) Uiso 0.5 1 d D . P A 1
H34 H 0.6519 0.5452 0.4141 0.034 Uiso 0.5 1 calc R U P A 1
C28 C 0.6478(2) 0.56948(18) 0.2827(5) 0.031(3) Uiso 0.5 1 d D . P A 1
H35 H 0.6697 0.5866 0.2829 0.038 Uiso 0.5 1 calc R U P A 1
C29 C 0.62627(14) 0.56897(16) 0.2046(6) 0.0327(18) Uiso 0.5 1 d D . P A 1
H36 H 0.6336 0.5859 0.1520 0.039 Uiso 0.5 1 calc R U P A 1
C30 C 0.59420(14) 0.54401(12) 0.2026(4) 0.0263(15) Uiso 0.5 1 d D . P A 1
H37 H 0.5797 0.5438 0.1489 0.032 Uiso 0.5 1 calc R U P A 1
C55 C 0.60151(14) 0.52962(14) 0.3758(5) 0.0347(17) Uiso 0.5 1 d D . P A 2
H57 H 0.5927 0.5187 0.4431 0.042 Uiso 0.5 1 calc R U P A 2
C56 C 0.63276(16) 0.55629(16) 0.3715(7) 0.044(2) Uiso 0.5 1 d D . P A 2
H58 H 0.6452 0.5634 0.4369 0.053 Uiso 0.5 1 calc R U P A 2
C57 C 0.6462(2) 0.5727(2) 0.2740(6) 0.042(3) Uiso 0.5 1 d D . P A 2
H59 H 0.6675 0.5908 0.2729 0.051 Uiso 0.5 1 calc R U P A 2
C58 C 0.62800(14) 0.56216(15) 0.1781(6) 0.0307(17) Uiso 0.5 1 d D . P A 2
H60 H 0.6369 0.5731 0.1108 0.037 Uiso 0.5 1 calc R U P A 2
C59 C 0.59672(14) 0.53557(13) 0.1809(4) 0.0266(15) Uiso 0.5 1 d D . P A 2
H61 H 0.5843 0.5284 0.1155 0.032 Uiso 0.5 1 calc R U P A 2
C31 C 0.54495(8) 0.46029(8) 0.1666(3) 0.0241(7) Uani 1 1 d . . . . .
C32 C 0.51897(9) 0.43946(8) 0.0985(3) 0.0285(7) Uani 1 1 d . . . . .
H38 H 0.4990 0.4393 0.1029 0.034 Uiso 1 1 calc R U . . .
C33 C 0.52234(10) 0.41886(9) 0.0241(3) 0.0360(9) Uani 1 1 d . . . . .
H39 H 0.5048 0.4053 -0.0229 0.043 Uiso 1 1 calc R U . . .
C34 C 0.55074(11) 0.41812(10) 0.0188(3) 0.0413(10) Uani 1 1 d . . . . .
H40 H 0.5528 0.4040 -0.0314 0.050 Uiso 1 1 calc R U . . .
C35 C 0.57646(11) 0.43797(11) 0.0868(4) 0.0436(10) Uani 1 1 d . . . . .
H41 H 0.5960 0.4372 0.0834 0.052 Uiso 1 1 calc R U . . .
C36 C 0.57376(9) 0.45905(10) 0.1602(3) 0.0341(8) Uani 1 1 d . . . . .
H42 H 0.5915 0.4726 0.2062 0.041 Uiso 1 1 calc R U . . .
C37 C 0.52025(7) 0.50577(8) 0.2287(3) 0.0203(6) Uani 1 1 d . . . . .
C38 C 0.52550(8) 0.53218(8) 0.2955(3) 0.0222(7) Uani 1 1 d . . . . .
H43 H 0.5419 0.5397 0.3500 0.027 Uiso 1 1 calc R U . . .
C39 C 0.50723(8) 0.54771(8) 0.2842(3) 0.0222(6) Uani 1 1 d . . . . .
C40 C 0.48457(8) 0.53756(9) 0.1987(3) 0.0259(7) Uani 1 1 d . . . . .
H44 H 0.4720 0.5477 0.1887 0.031 Uiso 1 1 calc R U . . .
C41 C 0.48029(9) 0.51281(9) 0.1283(3) 0.0272(7) Uani 1 1 d . . . . .
H45 H 0.4656 0.5070 0.0686 0.033 Uiso 1 1 calc R U . . .
C42 C 0.49733(8) 0.49626(8) 0.1442(3) 0.0253(7) Uani 1 1 d . . . . .
H46 H 0.4934 0.4786 0.0979 0.030 Uiso 1 1 calc R U . . .
C43 C 0.50040(9) 0.60507(8) 0.3569(3) 0.0267(7) Uani 1 1 d . . . . .
C44 C 0.51879(10) 0.63654(9) 0.4008(3) 0.0359(9) Uani 1 1 d . . . . .
H47 H 0.5385 0.6426 0.4381 0.043 Uiso 1 1 calc R U . . .
C45 C 0.50790(12) 0.65872(10) 0.3892(4) 0.0442(11) Uani 1 1 d . . . . .
H48 H 0.5200 0.6797 0.4207 0.053 Uiso 1 1 calc R U . . .
C46 C 0.47981(13) 0.65049(11) 0.3328(4) 0.0466(11) Uani 1 1 d . . . . .
H49 H 0.4729 0.6659 0.3238 0.056 Uiso 1 1 calc R U . . .
C47 C 0.46168(12) 0.61964(11) 0.2891(3) 0.0429(10) Uani 1 1 d . . . . .
H50 H 0.4423 0.6140 0.2504 0.051 Uiso 1 1 calc R U . . .
C48 C 0.47143(10) 0.59680(10) 0.3011(3) 0.0338(8) Uani 1 1 d . . . . .
H51 H 0.4586 0.5757 0.2716 0.041 Uiso 1 1 calc R U . . .
C49 C 0.55741(8) 0.60153(8) 0.3891(3) 0.0273(7) Uani 1 1 d . . . . .
C50 C 0.57779(9) 0.60994(9) 0.4815(3) 0.0315(8) Uani 1 1 d . . . . .
H52 H 0.5687 0.6030 0.5525 0.038 Uiso 1 1 calc R U . . .
C51 C 0.61137(10) 0.62854(10) 0.4685(4) 0.0414(10) Uani 1 1 d . . . . .
H53 H 0.6251 0.6340 0.5306 0.050 Uiso 1 1 calc R U . . .
C52 C 0.62471(10) 0.63905(10) 0.3647(4) 0.0464(11) Uani 1 1 d . . . . .
H54 H 0.6475 0.6516 0.3562 0.056 Uiso 1 1 calc R U . . .
C53 C 0.60461(12) 0.63116(11) 0.2732(4) 0.0527(13) Uani 1 1 d . . . . .
H55 H 0.6138 0.6385 0.2026 0.063 Uiso 1 1 calc R U . . .
C54 C 0.57142(11) 0.61282(10) 0.2843(4) 0.0449(11) Uani 1 1 d . . . . .
H56 H 0.5579 0.6077 0.2216 0.054 Uiso 1 1 calc R U . . .
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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
P P 0.1023 0.0942
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Ru Ru -1.2594 0.8363
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
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
C4 Ru1 N5 178.69(12) . .
C4 Ru1 N4 76.51(12) . .
N5 Ru1 N4 104.72(10) . .
C4 Ru1 N2 76.32(12) . .
N5 Ru1 N2 102.45(10) . .
N4 Ru1 N2 152.83(11) . .
C4 Ru1 P2 89.95(9) . 10_666
N5 Ru1 P2 89.45(8) . 10_666
N4 Ru1 P2 96.86(8) . 10_666
N2 Ru1 P2 83.31(8) . 10_666
C4 Ru1 P1 89.28(9) . .
N5 Ru1 P1 91.34(8) . .
N4 Ru1 P1 82.14(8) . .
N2 Ru1 P1 97.33(8) . .
P2 Ru1 P1 178.85(3) 10_666 .
C31 P1 C25 99.94(15) . .
C31 P1 C37 110.09(15) . .
C25 P1 C37 99.14(14) . .
C31 P1 Ru1 115.29(11) . .
C25 P1 Ru1 122.60(10) . .
C37 P1 Ru1 108.33(10) . .
C43 P2 C49 100.29(16) . .
C43 P2 C39 110.58(16) . .
C49 P2 C39 97.74(16) . .
C43 P2 Ru1 113.78(11) . 10_666
C49 P2 Ru1 123.51(12) . 10_666
C39 P2 Ru1 109.52(10) . 10_666
C1 N1 N2 110.0(3) . .
C1 N1 H1 125.0 . .
N2 N1 H1 125.0 . .
C3 N2 N1 106.9(3) . .
C3 N2 Ru1 115.6(2) . .
N1 N2 Ru1 137.5(2) . .
C12 N3 N4 107.3(3) . .
C10 N4 N3 109.2(3) . .
C10 N4 Ru1 115.6(2) . .
N3 N4 Ru1 135.2(2) . .
N5 N5 Ru1 179.3(4) 10_666 .
N1 C1 C2 107.9(3) . .
N1 C1 C13 121.9(3) . .
C2 C1 C13 130.2(3) . .
C1 C2 C3 106.2(3) . .
C1 C2 H2 126.9 . .
C3 C2 H2 126.9 . .
N2 C3 C2 109.0(3) . .
N2 C3 C5 115.0(3) . .
C2 C3 C5 136.0(3) . .
C5 C4 C9 119.4(3) . .
C5 C4 Ru1 120.4(2) . .
C9 C4 Ru1 120.1(2) . .
C4 C5 C6 120.3(3) . .
C4 C5 C3 112.5(3) . .
C6 C5 C3 127.0(3) . .
C5 C6 C7 120.9(3) . .
C5 C6 H3 119.5 . .
C7 C6 H3 119.5 . .
C8 C7 C6 118.1(3) . .
C8 C7 C21 119.6(3) . .
C6 C7 C21 122.3(3) . .
C7 C8 C9 121.4(3) . .
C7 C8 H4 119.3 . .
C9 C8 H4 119.3 . .
C8 C9 C4 119.8(3) . .
C8 C9 C10 128.1(3) . .
C4 C9 C10 112.1(3) . .
N4 C10 C11 108.6(3) . .
N4 C10 C9 115.5(3) . .
C11 C10 C9 135.7(3) . .
C12 C11 C10 104.5(3) . .
C12 C11 H5 127.7 . .
C10 C11 H5 127.7 . .
N3 C12 C11 110.4(3) . .
N3 C12 C17 120.7(3) . .
C11 C12 C17 128.9(3) . .
C16 C13 C15 111.4(4) . .
C16 C13 C1 110.3(4) . .
C15 C13 C1 109.9(4) . .
C16 C13 C14 105.3(4) . .
C15 C13 C14 110.2(4) . .
C1 C13 C14 109.8(4) . .
C13 C14 H6 109.5 . .
C13 C14 H7 109.5 . .
H6 C14 H7 109.5 . .
C13 C14 H8 109.5 . .
H6 C14 H8 109.5 . .
H7 C14 H8 109.5 . .
C13 C15 H9 109.5 . .
C13 C15 H10 109.5 . .
H9 C15 H10 109.5 . .
C13 C15 H11 109.5 . .
H9 C15 H11 109.5 . .
H10 C15 H11 109.5 . .
C13 C16 H12 109.5 . .
C13 C16 H13 109.5 . .
H12 C16 H13 109.5 . .
C13 C16 H14 109.5 . .
H12 C16 H14 109.5 . .
H13 C16 H14 109.5 . .
C18 C17 C12 111.7(4) . .
C18 C17 C20 112.5(5) . .
C12 C17 C20 110.4(4) . .
C18 C17 C19 108.5(5) . .
C12 C17 C19 108.1(4) . .
C20 C17 C19 105.4(4) . .
C17 C18 H15 109.5 . .
C17 C18 H16 109.5 . .
H15 C18 H16 109.5 . .
C17 C18 H17 109.5 . .
H15 C18 H17 109.5 . .
H16 C18 H17 109.5 . .
C17 C19 H18 109.5 . .
C17 C19 H19 109.5 . .
H18 C19 H19 109.5 . .
C17 C19 H20 109.5 . .
H18 C19 H20 109.5 . .
H19 C19 H20 109.5 . .
C17 C20 H21 109.5 . .
C17 C20 H22 109.5 . .
H21 C20 H22 109.5 . .
C17 C20 H23 109.5 . .
H21 C20 H23 109.5 . .
H22 C20 H23 109.5 . .
C7 C21 C24 109.4(3) . .
C7 C21 C22 112.3(3) . .
C24 C21 C22 107.6(4) . .
C7 C21 C23 109.6(3) . .
C24 C21 C23 109.8(4) . .
C22 C21 C23 108.1(4) . .
C21 C22 H24 109.5 . .
C21 C22 H25 109.5 . .
H24 C22 H25 109.5 . .
C21 C22 H26 109.5 . .
H24 C22 H26 109.5 . .
H25 C22 H26 109.5 . .
C21 C23 H27 109.5 . .
C21 C23 H28 109.5 . .
H27 C23 H28 109.5 . .
C21 C23 H29 109.5 . .
H27 C23 H29 109.5 . .
H28 C23 H29 109.5 . .
C21 C24 H30 109.5 . .
C21 C24 H31 109.5 . .
H30 C24 H31 109.5 . .
C21 C24 H32 109.5 . .
H30 C24 H32 109.5 . .
H31 C24 H32 109.5 . .
C30 C25 C26 119.6(4) . .
C55 C25 C59 120.1(4) . .
C55 C25 P1 121.8(3) . .
C30 C25 P1 121.6(3) . .
C26 C25 P1 118.8(3) . .
C59 C25 P1 118.0(3) . .
C27 C26 C25 120.7(5) . .
C27 C26 H33 119.6 . .
C25 C26 H33 119.6 . .
C28 C27 C26 119.3(7) . .
C28 C27 H34 120.3 . .
C26 C27 H34 120.3 . .
C27 C28 C29 120.0(8) . .
C27 C28 H35 120.0 . .
C29 C28 H35 120.0 . .
C30 C29 C28 120.8(7) . .
C30 C29 H36 119.6 . .
C28 C29 H36 119.6 . .
C29 C30 C25 119.5(6) . .
C29 C30 H37 120.2 . .
C25 C30 H37 120.2 . .
C25 C55 C56 118.8(6) . .
C25 C55 H57 120.6 . .
C56 C55 H57 120.6 . .
C57 C56 C55 121.7(8) . .
C57 C56 H58 119.1 . .
C55 C56 H58 119.1 . .
C56 C57 C58 119.1(9) . .
C56 C57 H59 120.4 . .
C58 C57 H59 120.4 . .
C57 C58 C59 119.9(8) . .
C57 C58 H60 120.1 . .
C59 C58 H60 120.1 . .
C58 C59 C25 120.3(6) . .
C58 C59 H61 119.9 . .
C25 C59 H61 119.9 . .
C36 C31 C32 118.1(3) . .
C36 C31 P1 117.5(3) . .
C32 C31 P1 123.7(3) . .
C33 C32 C31 120.4(4) . .
C33 C32 H38 119.8 . .
C31 C32 H38 119.8 . .
C34 C33 C32 120.5(4) . .
C34 C33 H39 119.8 . .
C32 C33 H39 119.8 . .
C33 C34 C35 120.0(4) . .
C33 C34 H40 120.0 . .
C35 C34 H40 120.0 . .
C34 C35 C36 120.3(4) . .
C34 C35 H41 119.8 . .
C36 C35 H41 119.8 . .
C35 C36 C31 120.5(4) . .
C35 C36 H42 119.7 . .
C31 C36 H42 119.7 . .
C42 C37 C38 118.3(3) . .
C42 C37 P1 127.9(3) . .
C38 C37 P1 113.3(2) . .
C39 C38 C37 122.2(3) . .
C39 C38 H43 118.9 . .
C37 C38 H43 118.9 . .
C40 C39 C38 117.7(3) . .
C40 C39 P2 128.1(3) . .
C38 C39 P2 113.6(2) . .
C41 C40 C39 120.9(3) . .
C41 C40 H44 119.5 . .
C39 C40 H44 119.5 . .
C40 C41 C42 120.8(3) . .
C40 C41 H45 119.6 . .
C42 C41 H45 119.6 . .
C41 C42 C37 119.9(3) . .
C41 C42 H46 120.1 . .
C37 C42 H46 120.1 . .
C48 C43 C44 118.9(3) . .
C48 C43 P2 124.4(3) . .
C44 C43 P2 115.8(3) . .
C45 C44 C43 119.8(4) . .
C45 C44 H47 120.1 . .
C43 C44 H47 120.1 . .
C46 C45 C44 120.7(4) . .
C46 C45 H48 119.6 . .
C44 C45 H48 119.6 . .
C45 C46 C47 119.7(4) . .
C45 C46 H49 120.1 . .
C47 C46 H49 120.1 . .
C46 C47 C48 121.1(4) . .
C46 C47 H50 119.5 . .
C48 C47 H50 119.5 . .
C47 C48 C43 119.8(4) . .
C47 C48 H51 120.1 . .
C43 C48 H51 120.1 . .
C50 C49 C54 119.1(3) . .
C50 C49 P2 122.5(3) . .
C54 C49 P2 118.4(3) . .
C51 C50 C49 119.8(4) . .
C51 C50 H52 120.1 . .
C49 C50 H52 120.1 . .
C52 C51 C50 120.2(4) . .
C52 C51 H53 119.9 . .
C50 C51 H53 119.9 . .
C51 C52 C53 120.1(4) . .
C51 C52 H54 119.9 . .
C53 C52 H54 119.9 . .
C54 C53 C52 120.5(4) . .
C54 C53 H55 119.7 . .
C52 C53 H55 119.7 . .
C53 C54 C49 120.2(4) . .
C53 C54 H56 119.9 . .
C49 C54 H56 119.9 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ru1 C4 2.019(3) .
Ru1 N5 2.108(3) .
Ru1 N4 2.143(3) .
Ru1 N2 2.152(3) .
Ru1 P2 2.3981(9) 10_666
Ru1 P1 2.4042(9) .
P1 C31 1.851(4) .
P1 C25 1.852(3) .
P1 C37 1.854(3) .
P2 C43 1.842(3) .
P2 C49 1.849(4) .
P2 C39 1.861(4) .
P2 Ru1 2.3982(9) 10_666
N1 C1 1.365(4) .
N1 N2 1.372(4) .
N1 H1 0.8800 .
N2 C3 1.368(4) .
N3 C12 1.364(4) .
N3 N4 1.380(4) .
N4 C10 1.369(4) .
N5 N5 1.124(5) 10_666
C1 C2 1.389(5) .
C1 C13 1.532(5) .
C2 C3 1.410(5) .
C2 H2 0.9500 .
C3 C5 1.464(5) .
C4 C5 1.398(5) .
C4 C9 1.411(5) .
C5 C6 1.404(5) .
C6 C7 1.412(5) .
C6 H3 0.9500 .
C7 C8 1.403(5) .
C7 C21 1.537(5) .
C8 C9 1.405(5) .
C8 H4 0.9500 .
C9 C10 1.457(5) .
C10 C11 1.420(5) .
C11 C12 1.407(5) .
C11 H5 0.9500 .
C12 C17 1.526(5) .
C13 C16 1.510(7) .
C13 C15 1.529(7) .
C13 C14 1.560(7) .
C14 H6 0.9800 .
C14 H7 0.9800 .
C14 H8 0.9800 .
C15 H9 0.9800 .
C15 H10 0.9800 .
C15 H11 0.9800 .
C16 H12 0.9800 .
C16 H13 0.9800 .
C16 H14 0.9800 .
C17 C18 1.484(8) .
C17 C20 1.530(7) .
C17 C19 1.571(8) .
C18 H15 0.9800 .
C18 H16 0.9800 .
C18 H17 0.9800 .
C19 H18 0.9800 .
C19 H19 0.9800 .
C19 H20 0.9800 .
C20 H21 0.9800 .
C20 H22 0.9800 .
C20 H23 0.9800 .
C21 C24 1.544(6) .
C21 C22 1.555(6) .
C21 C23 1.556(6) .
C22 H24 0.9800 .
C22 H25 0.9800 .
C22 H26 0.9800 .
C23 H27 0.9800 .
C23 H28 0.9800 .
C23 H29 0.9800 .
C24 H30 0.9800 .
C24 H31 0.9800 .
C24 H32 0.9800 .
C25 C55 1.386(4) .
C25 C30 1.393(4) .
C25 C26 1.402(4) .
C25 C59 1.405(4) .
C26 C27 1.395(5) .
C26 H33 0.9500 .
C27 C28 1.390(5) .
C27 H34 0.9500 .
C28 C29 1.393(5) .
C28 H35 0.9500 .
C29 C30 1.391(5) .
C29 H36 0.9500 .
C30 H37 0.9500 .
C55 C56 1.395(5) .
C55 H57 0.9500 .
C56 C57 1.392(5) .
C56 H58 0.9500 .
C57 C58 1.392(5) .
C57 H59 0.9500 .
C58 C59 1.394(5) .
C58 H60 0.9500 .
C59 H61 0.9500 .
C31 C36 1.406(5) .
C31 C32 1.408(5) .
C32 C33 1.404(5) .
C32 H38 0.9500 .
C33 C34 1.374(6) .
C33 H39 0.9500 .
C34 C35 1.388(6) .
C34 H40 0.9500 .
C35 C36 1.400(6) .
C35 H41 0.9500 .
C36 H42 0.9500 .
C37 C42 1.403(5) .
C37 C38 1.414(5) .
C38 C39 1.404(5) .
C38 H43 0.9500 .
C39 C40 1.402(5) .
C40 C41 1.390(5) .
C40 H44 0.9500 .
C41 C42 1.401(5) .
C41 H45 0.9500 .
C42 H46 0.9500 .
C43 C48 1.408(5) .
C43 C44 1.411(5) .
C44 C45 1.399(6) .
C44 H47 0.9500 .
C45 C46 1.377(7) .
C45 H48 0.9500 .
C46 C47 1.387(7) .
C46 H49 0.9500 .
C47 C48 1.389(5) .
C47 H50 0.9500 .
C48 H51 0.9500 .
C49 C50 1.410(5) .
C49 C54 1.418(5) .
C50 C51 1.398(5) .
C50 H52 0.9500 .
C51 C52 1.393(6) .
C51 H53 0.9500 .
C52 C53 1.394(7) .
C52 H54 0.9500 .
C53 C54 1.380(6) .
C53 H55 0.9500 .
C54 H56 0.9500 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N1 H1 O1 2.653(6) 0.880 1.895 143.2 no
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
C1 N1 N2 C3 1.5(4) .
C1 N1 N2 Ru1 -177.5(3) .
C12 N3 N4 C10 0.2(4) .
C12 N3 N4 Ru1 178.0(2) .
N2 N1 C1 C2 -1.1(4) .
N2 N1 C1 C13 -179.3(3) .
N1 C1 C2 C3 0.3(4) .
C13 C1 C2 C3 178.3(4) .
N1 N2 C3 C2 -1.3(4) .
Ru1 N2 C3 C2 178.0(2) .
N1 N2 C3 C5 176.9(3) .
Ru1 N2 C3 C5 -3.8(4) .
C1 C2 C3 N2 0.6(4) .
C1 C2 C3 C5 -177.1(4) .
C9 C4 C5 C6 -1.9(5) .
Ru1 C4 C5 C6 177.6(3) .
C9 C4 C5 C3 -178.1(3) .
Ru1 C4 C5 C3 1.3(4) .
N2 C3 C5 C4 1.7(4) .
C2 C3 C5 C4 179.3(4) .
N2 C3 C5 C6 -174.2(3) .
C2 C3 C5 C6 3.3(7) .
C4 C5 C6 C7 1.5(5) .
C3 C5 C6 C7 177.2(3) .
C5 C6 C7 C8 0.0(5) .
C5 C6 C7 C21 -179.0(3) .
C6 C7 C8 C9 -1.2(5) .
C21 C7 C8 C9 177.9(3) .
C7 C8 C9 C4 0.8(5) .
C7 C8 C9 C10 179.3(3) .
C5 C4 C9 C8 0.7(5) .
Ru1 C4 C9 C8 -178.7(3) .
C5 C4 C9 C10 -178.0(3) .
Ru1 C4 C9 C10 2.5(4) .
N3 N4 C10 C11 -0.3(4) .
Ru1 N4 C10 C11 -178.5(2) .
N3 N4 C10 C9 174.9(3) .
Ru1 N4 C10 C9 -3.4(4) .
C8 C9 C10 N4 -177.9(3) .
C4 C9 C10 N4 0.7(4) .
C8 C9 C10 C11 -4.5(7) .
C4 C9 C10 C11 174.1(4) .
N4 C10 C11 C12 0.2(4) .
C9 C10 C11 C12 -173.5(4) .
N4 N3 C12 C11 -0.1(4) .
N4 N3 C12 C17 179.0(3) .
C10 C11 C12 N3 -0.1(4) .
C10 C11 C12 C17 -179.1(4) .
N1 C1 C13 C16 -170.1(4) .
C2 C1 C13 C16 12.2(6) .
N1 C1 C13 C15 66.7(5) .
C2 C1 C13 C15 -111.0(5) .
N1 C1 C13 C14 -54.6(5) .
C2 C1 C13 C14 127.7(5) .
N3 C12 C17 C18 51.9(6) .
C11 C12 C17 C18 -129.2(5) .
N3 C12 C17 C20 177.9(4) .
C11 C12 C17 C20 -3.2(6) .
N3 C12 C17 C19 -67.3(5) .
C11 C12 C17 C19 111.6(5) .
C8 C7 C21 C24 -58.6(5) .
C6 C7 C21 C24 120.4(4) .
C8 C7 C21 C22 -178.0(4) .
C6 C7 C21 C22 1.0(5) .
C8 C7 C21 C23 61.9(5) .
C6 C7 C21 C23 -119.1(4) .
C31 P1 C25 C55 -128.4(3) .
C37 P1 C25 C55 119.2(3) .
Ru1 P1 C25 C55 0.4(3) .
C31 P1 C25 C30 78.3(3) .
C37 P1 C25 C30 -34.1(3) .
Ru1 P1 C25 C30 -152.8(3) .
C31 P1 C25 C26 -99.3(3) .
C37 P1 C25 C26 148.3(3) .
Ru1 P1 C25 C26 29.5(3) .
C31 P1 C25 C59 52.8(3) .
C37 P1 C25 C59 -59.6(3) .
Ru1 P1 C25 C59 -178.4(2) .
C30 C25 C26 C27 -0.03(14) .
P1 C25 C26 C27 177.7(2) .
C25 C26 C27 C28 -0.11(14) .
C26 C27 C28 C29 0.3(3) .
C27 C28 C29 C30 -0.4(4) .
C28 C29 C30 C25 0.3(4) .
C26 C25 C30 C29 0.0(3) .
P1 C25 C30 C29 -177.7(3) .
C59 C25 C55 C56 -0.01(14) .
P1 C25 C55 C56 -178.8(3) .
C25 C55 C56 C57 0.04(14) .
C55 C56 C57 C58 -0.1(3) .
C56 C57 C58 C59 0.2(4) .
C57 C58 C59 C25 -0.2(4) .
C55 C25 C59 C58 0.1(3) .
P1 C25 C59 C58 178.9(3) .
C25 P1 C31 C36 38.5(3) .
C37 P1 C31 C36 142.2(3) .
Ru1 P1 C31 C36 -94.9(3) .
C25 P1 C31 C32 -151.1(3) .
C37 P1 C31 C32 -47.4(3) .
Ru1 P1 C31 C32 75.4(3) .
C36 C31 C32 C33 -2.0(5) .
P1 C31 C32 C33 -172.3(3) .
C31 C32 C33 C34 1.7(6) .
C32 C33 C34 C35 -0.4(6) .
C33 C34 C35 C36 -0.6(7) .
C34 C35 C36 C31 0.3(7) .
C32 C31 C36 C35 1.0(6) .
P1 C31 C36 C35 171.9(3) .
C31 P1 C37 C42 27.5(3) .
C25 P1 C37 C42 131.7(3) .
Ru1 P1 C37 C42 -99.4(3) .
C31 P1 C37 C38 -161.1(2) .
C25 P1 C37 C38 -56.9(3) .
Ru1 P1 C37 C38 72.0(2) .
C42 C37 C38 C39 3.9(5) .
P1 C37 C38 C39 -168.3(2) .
C37 C38 C39 C40 -4.1(5) .
C37 C38 C39 P2 168.2(2) .
C43 P2 C39 C40 -28.6(4) .
C49 P2 C39 C40 -132.7(3) .
Ru1 P2 C39 C40 97.6(3) 10_666
C43 P2 C39 C38 160.1(2) .
C49 P2 C39 C38 56.0(3) .
Ru1 P2 C39 C38 -73.7(2) 10_666
C38 C39 C40 C41 0.4(5) .
P2 C39 C40 C41 -170.5(3) .
C39 C40 C41 C42 3.2(5) .
C40 C41 C42 C37 -3.3(5) .
C38 C37 C42 C41 -0.2(5) .
P1 C37 C42 C41 170.8(3) .
C49 P2 C43 C48 148.7(3) .
C39 P2 C43 C48 46.4(3) .
Ru1 P2 C43 C48 -77.4(3) 10_666
C49 P2 C43 C44 -42.3(3) .
C39 P2 C43 C44 -144.6(3) .
Ru1 P2 C43 C44 91.6(3) 10_666
C48 C43 C44 C45 0.6(6) .
P2 C43 C44 C45 -169.0(3) .
C43 C44 C45 C46 -1.8(6) .
C44 C45 C46 C47 1.6(6) .
C45 C46 C47 C48 -0.2(7) .
C46 C47 C48 C43 -0.9(6) .
C44 C43 C48 C47 0.7(5) .
P2 C43 C48 C47 169.4(3) .
C43 P2 C49 C50 114.8(3) .
C39 P2 C49 C50 -132.5(3) .
Ru1 P2 C49 C50 -12.9(4) 10_666
C43 P2 C49 C54 -65.9(3) .
C39 P2 C49 C54 46.8(3) .
Ru1 P2 C49 C54 166.4(3) 10_666
C54 C49 C50 C51 -1.5(6) .
P2 C49 C50 C51 177.8(3) .
C49 C50 C51 C52 0.7(6) .
C50 C51 C52 C53 0.2(7) .
C51 C52 C53 C54 -0.2(8) .
C52 C53 C54 C49 -0.6(7) .
C50 C49 C54 C53 1.5(6) .
P2 C49 C54 C53 -177.8(4) .
