#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:53:07 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179133 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/95/4309574.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_4309574
loop_
_publ_author_name
'Erwin Reisner'
'Vladimir B. Arion'
'Anna Eichinger'
'Norbert Kandler'
'Gerald Giester'
'Armando J.L. Pombeiro'
'Bernhard K. Keppler'
_publ_section_title
;
Tuning of Redox Properties for the Design of Ruthenium Anticancer Drugs:
Part 2. Syntheses, Crystal Structures, and Electrochemistry of Potentially
Antitumor [RuIII/IICl6-n(Azole)n]z (n= 3, 4, 6) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6704
_journal_page_last               6716
_journal_paper_doi               10.1021/ic0503737
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C21 H36 Cl3 N6 Ru'
_chemical_formula_weight         579.98
_chemical_name_systematic
; 
mer-trichlorotripyrazoloruthenium(III) 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.35(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.730(4)
_cell_length_b                   10.794(2)
_cell_length_c                   27.802(6)
_cell_measurement_temperature    120(2)
_cell_volume                     5320.6(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0191
_diffrn_reflns_av_sigmaI/netI    0.0292
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            30901
_diffrn_reflns_theta_full        30.49
_diffrn_reflns_theta_max         30.49
_diffrn_reflns_theta_min         2.39
_exptl_absorpt_coefficient_mu    0.911
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2392
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.275
_refine_diff_density_min         -1.329
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     560
_refine_ls_number_reflns         16107
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0310
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0542P)²+1.3657P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0829
_refine_ls_wR_factor_ref         0.0959
_reflns_number_gt                12904
_reflns_number_total             16107
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0503737si20050311_101757.cif
_cod_data_source_block           ERRE717
_cod_database_code               4309574
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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 0.062103(7) 0.909806(13) 0.359946(4) 0.01295(4) Uani 1 1 d . . .
Ru2 Ru -0.434659(7) 0.616779(13) 0.359133(4) 0.01336(4) Uani 1 1 d . . .
Cl1 Cl 0.01478(3) 0.71431(4) 0.382902(15) 0.01964(9) Uani 1 1 d . . .
Cl2 Cl -0.06120(2) 0.99437(4) 0.361518(14) 0.01660(8) Uani 1 1 d . . .
Cl3 Cl 0.11005(2) 1.10303(4) 0.334737(15) 0.01755(9) Uani 1 1 d . . .
Cl4 Cl -0.47455(3) 0.81231(4) 0.387160(15) 0.02042(9) Uani 1 1 d . . .
Cl5 Cl -0.55993(2) 0.53829(4) 0.362898(14) 0.01728(8) Uani 1 1 d . . .
Cl6 Cl -0.39137(2) 0.42382(4) 0.331311(15) 0.01794(9) Uani 1 1 d . . .
N1 N 0.16996(8) 0.83878(14) 0.35703(5) 0.0168(3) Uani 1 1 d . . .
C2 C 0.21976(10) 0.86718(18) 0.32338(7) 0.0205(4) Uani 1 1 d . . .
H2 H 0.2115 0.9244 0.2989 0.025 Uiso 1 1 calc R . .
N3 N 0.28365(8) 0.80242(15) 0.32931(5) 0.0201(3) Uani 1 1 d . . .
C4 C 0.27457(11) 0.7281(2) 0.36874(7) 0.0266(4) Uani 1 1 d . . .
H4 H 0.3096 0.6725 0.3813 0.032 Uiso 1 1 calc R . .
C5 C 0.20414(11) 0.75127(19) 0.38597(6) 0.0239(4) Uani 1 1 d . . .
H5 H 0.1827 0.7142 0.4128 0.029 Uiso 1 1 calc R . .
C6 C 0.34804(10) 0.80184(19) 0.29600(7) 0.0239(4) Uani 1 1 d . . .
H6A H 0.3943 0.7896 0.3142 0.029 Uiso 1 1 calc R . .
H6B H 0.3512 0.8818 0.2802 0.029 Uiso 1 1 calc R . .
C7 C 0.34142(10) 0.70135(19) 0.25817(7) 0.0229(4) Uani 1 1 d . . .
H7A H 0.3435 0.6213 0.2740 0.028 Uiso 1 1 calc R . .
H7B H 0.3845 0.7069 0.2369 0.028 Uiso 1 1 calc R . .
C8 C 0.26953(11) 0.7078(2) 0.22796(7) 0.0259(4) Uani 1 1 d . . .
H8A H 0.2266 0.6900 0.2483 0.031 Uiso 1 1 calc R . .
H8B H 0.2636 0.7913 0.2156 0.031 Uiso 1 1 calc R . .
C9 C 0.27014(14) 0.6173(2) 0.18613(8) 0.0386(6) Uani 1 1 d . . .
H9A H 0.2241 0.6251 0.1681 0.058 Uiso 1 1 calc R . .
H9B H 0.2746 0.5343 0.1982 0.058 Uiso 1 1 calc R . .
H9C H 0.3122 0.6352 0.1657 0.058 Uiso 1 1 calc R . .
N10 N 0.05055(8) 0.85794(14) 0.28834(5) 0.0156(3) Uani 1 1 d . . .
C11 C 0.03172(10) 0.92692(17) 0.25048(6) 0.0167(3) Uani 1 1 d . . .
H11 H 0.0196 1.0107 0.2518 0.020 Uiso 1 1 calc R . .
N12 N 0.03277(8) 0.85828(14) 0.20989(5) 0.0171(3) Uani 1 1 d . . .
C13 C 0.05352(10) 0.73970(17) 0.22233(6) 0.0184(3) Uani 1 1 d . . .
H13 H 0.0590 0.6725 0.2017 0.022 Uiso 1 1 calc R . .
C14 C 0.06444(10) 0.74044(17) 0.27073(6) 0.0173(3) Uani 1 1 d . . .
H14 H 0.0790 0.6725 0.2891 0.021 Uiso 1 1 calc R . .
C15 C 0.01027(11) 0.90003(18) 0.16152(6) 0.0210(4) Uani 1 1 d . . .
H15A H 0.0019 0.9888 0.1621 0.025 Uiso 1 1 calc R . .
H15B H -0.0369 0.8605 0.1526 0.025 Uiso 1 1 calc R . .
C16 C 0.06956(11) 0.87006(19) 0.12379(6) 0.0231(4) Uani 1 1 d . . .
H16A H 0.0790 0.7816 0.1242 0.028 Uiso 1 1 calc R . .
H16B H 0.0496 0.8912 0.0923 0.028 Uiso 1 1 calc R . .
C17 C 0.14380(12) 0.9376(2) 0.13121(7) 0.0301(5) Uani 1 1 d . . .
H17A H 0.1631 0.9190 0.1631 0.036 Uiso 1 1 calc R . .
H17B H 0.1349 1.0262 0.1295 0.036 Uiso 1 1 calc R . .
C18 C 0.20295(14) 0.9020(3) 0.09406(9) 0.0468(7) Uani 1 1 d . . .
H18A H 0.2487 0.9471 0.1003 0.070 Uiso 1 1 calc R . .
H18B H 0.1846 0.9219 0.0624 0.070 Uiso 1 1 calc R . .
H18C H 0.2128 0.8147 0.0961 0.070 Uiso 1 1 calc R . .
N19 N 0.07915(8) 0.95635(14) 0.43212(5) 0.0162(3) Uani 1 1 d . . .
C20 C 0.10249(11) 1.06505(18) 0.44844(6) 0.0224(4) Uani 1 1 d . . .
H20 H 0.1130 1.1331 0.4291 0.027 Uiso 1 1 calc R . .
N21 N 0.10900(9) 1.06430(16) 0.49666(5) 0.0217(3) Uani 1 1 d . . .
C22 C 0.08950(11) 0.94879(19) 0.51204(6) 0.0233(4) Uani 1 1 d . . .
H22 H 0.0890 0.9210 0.5437 0.028 Uiso 1 1 calc R . .
C23 C 0.07102(11) 0.88204(18) 0.47230(6) 0.0227(4) Uani 1 1 d . . .
H23 H 0.0554 0.7998 0.4721 0.027 Uiso 1 1 calc R . .
C24 C 0.13709(13) 1.1622(2) 0.52877(7) 0.0309(5) Uani 1 1 d . . .
H24A H 0.1810 1.1314 0.5459 0.037 Uiso 1 1 calc R . .
H24B H 0.0986 1.1804 0.5524 0.037 Uiso 1 1 calc R . .
C25 C 0.15823(13) 1.2816(2) 0.50336(8) 0.0349(5) Uani 1 1 d . . .
H25A H 0.1891 1.3313 0.5249 0.042 Uiso 1 1 calc R . .
H25B H 0.1884 1.2616 0.4754 0.042 Uiso 1 1 calc R . .
C26 C 0.09165(16) 1.3569(2) 0.48747(9) 0.0460(6) Uani 1 1 d . . .
H26A H 0.0635 1.3841 0.5153 0.055 Uiso 1 1 calc R . .
H26B H 0.0585 1.3065 0.4676 0.055 Uiso 1 1 calc R . .
C27 C 0.1190(2) 1.4720(3) 0.45817(10) 0.0735(11) Uani 1 1 d . . .
H27A H 0.0760 1.5176 0.4466 0.110 Uiso 1 1 calc R . .
H27B H 0.1485 1.4448 0.4314 0.110 Uiso 1 1 calc R . .
H27C H 0.1491 1.5243 0.4785 0.110 Uiso 1 1 calc R . .
N28 N -0.32640(8) 0.68594(14) 0.35324(5) 0.0172(3) Uani 1 1 d . . .
C29 C -0.27740(10) 0.65205(18) 0.31966(6) 0.0199(4) Uani 1 1 d . . .
H29 H -0.2853 0.5884 0.2977 0.024 Uiso 1 1 calc R . .
N30 N -0.21486(8) 0.72231(15) 0.32180(5) 0.0204(3) Uani 1 1 d . . .
C31 C -0.22377(11) 0.8054(2) 0.35851(7) 0.0251(4) Uani 1 1 d . . .
H31 H -0.1895 0.8657 0.3683 0.030 Uiso 1 1 calc R . .
C32 C -0.29282(11) 0.78248(19) 0.37778(6) 0.0240(4) Uani 1 1 d . . .
H32 H -0.3140 0.8252 0.4034 0.029 Uiso 1 1 calc R . .
C33 C -0.15163(10) 0.7200(2) 0.28770(7) 0.0246(4) Uani 1 1 d . . .
H33A H -0.1514 0.6413 0.2708 0.030 Uiso 1 1 calc R . .
H33B H -0.1044 0.7272 0.3053 0.030 Uiso 1 1 calc R . .
C34 C -0.15748(10) 0.82475(19) 0.25137(7) 0.0229(4) Uani 1 1 d . . .
H34A H -0.1151 0.8194 0.2295 0.027 Uiso 1 1 calc R . .
H34B H -0.1536 0.9031 0.2683 0.027 Uiso 1 1 calc R . .
C35 C -0.23026(11) 0.8241(2) 0.22205(7) 0.0275(4) Uani 1 1 d . . .
H35A H -0.2382 0.7419 0.2089 0.033 Uiso 1 1 calc R . .
H35B H -0.2722 0.8426 0.2431 0.033 Uiso 1 1 calc R . .
C36 C -0.22954(14) 0.9169(3) 0.18134(9) 0.0418(6) Uani 1 1 d . . .
H36A H -0.2765 0.9129 0.1641 0.063 Uiso 1 1 calc R . .
H36B H -0.1888 0.8980 0.1599 0.063 Uiso 1 1 calc R . .
H36C H -0.2228 0.9988 0.1942 0.063 Uiso 1 1 calc R . .
N37 N -0.41687(8) 0.55572(14) 0.42911(5) 0.0167(3) Uani 1 1 d . . .
C38 C -0.43692(10) 0.44385(18) 0.44408(6) 0.0203(4) Uani 1 1 d . . .
H38 H -0.4625 0.3862 0.4252 0.024 Uiso 1 1 calc R . .
N39 N -0.41564(9) 0.42444(15) 0.48977(5) 0.0211(3) Uani 1 1 d . . .
C40 C -0.37971(12) 0.52973(19) 0.50525(7) 0.0261(4) Uani 1 1 d . . .
H40 H -0.3587 0.5433 0.5355 0.031 Uiso 1 1 calc R . .
C41 C -0.38084(11) 0.61030(19) 0.46775(7) 0.0245(4) Uani 1 1 d . . .
H41 H -0.3605 0.6897 0.4681 0.029 Uiso 1 1 calc R . .
C42 C -0.42622(12) 0.30936(19) 0.51693(7) 0.0277(4) Uani 1 1 d . . .
H42A H -0.4727 0.2700 0.5065 0.033 Uiso 1 1 calc R . .
H42B H -0.4311 0.3290 0.5508 0.033 Uiso 1 1 calc R . .
C43 C -0.36076(13) 0.2187(2) 0.51035(7) 0.0308(5) Uani 1 1 d . . .
H43A H -0.3139 0.2611 0.5178 0.037 Uiso 1 1 calc R . .
H43B H -0.3663 0.1512 0.5331 0.037 Uiso 1 1 calc R . .
C44 C -0.35584(13) 0.1653(2) 0.46002(7) 0.0339(5) Uani 1 1 d . . .
H44A H -0.3487 0.2320 0.4371 0.041 Uiso 1 1 calc R . .
H44B H -0.4028 0.1238 0.4521 0.041 Uiso 1 1 calc R . .
C45 C -0.29094(16) 0.0736(3) 0.45588(9) 0.0514(7) Uani 1 1 d . . .
H45A H -0.2895 0.0409 0.4238 0.077 Uiso 1 1 calc R . .
H45B H -0.2981 0.0071 0.4783 0.077 Uiso 1 1 calc R . .
H45C H -0.2442 0.1150 0.4629 0.077 Uiso 1 1 calc R . .
N46 N -0.44922(8) 0.67424(14) 0.28848(5) 0.0162(3) Uani 1 1 d . . .
C47 C -0.47012(10) 0.60636(17) 0.25089(6) 0.0171(3) Uani 1 1 d . . .
H47 H -0.4835 0.5232 0.2524 0.021 Uiso 1 1 calc R . .
N48 N -0.46927(8) 0.67439(14) 0.21023(5) 0.0171(3) Uani 1 1 d . . .
C49 C -0.44697(10) 0.79236(17) 0.22240(6) 0.0189(3) Uani 1 1 d . . .
H49 H -0.4415 0.8594 0.2017 0.023 Uiso 1 1 calc R . .
C50 C -0.43446(10) 0.79148(17) 0.27089(6) 0.0188(3) Uani 1 1 d . . .
H50 H -0.4186 0.8589 0.2892 0.023 Uiso 1 1 calc R . .
C51 C -0.49419(10) 0.63294(19) 0.16239(6) 0.0213(4) Uani 1 1 d . . .
H51A H -0.5412 0.6739 0.1542 0.026 Uiso 1 1 calc R . .
H51B H -0.5036 0.5444 0.1633 0.026 Uiso 1 1 calc R . .
C52 C -0.43603(11) 0.66065(19) 0.12359(6) 0.0228(4) Uani 1 1 d . . .
H52A H -0.4578 0.6414 0.0924 0.027 Uiso 1 1 calc R . .
H52B H -0.4246 0.7485 0.1241 0.027 Uiso 1 1 calc R . .
C53 C -0.36315(12) 0.5882(2) 0.12974(8) 0.0317(5) Uani 1 1 d . . .
H53A H -0.3741 0.5003 0.1279 0.038 Uiso 1 1 calc R . .
H53B H -0.3422 0.6049 0.1614 0.038 Uiso 1 1 calc R . .
C54 C -0.30486(15) 0.6212(3) 0.09169(10) 0.0537(8) Uani 1 1 d . . .
H54A H -0.2600 0.5732 0.0969 0.081 Uiso 1 1 calc R . .
H54B H -0.2929 0.7078 0.0939 0.081 Uiso 1 1 calc R . .
H54C H -0.3250 0.6033 0.0603 0.081 Uiso 1 1 calc R . .
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_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 N10 87.03(6) . . ?
N1 Ru1 N19 89.91(6) . . ?
N10 Ru1 N19 176.88(6) . . ?
N1 Ru1 Cl1 90.55(5) . . ?
N10 Ru1 Cl1 89.14(4) . . ?
N19 Ru1 Cl1 90.28(4) . . ?
N1 Ru1 Cl3 88.91(5) . . ?
N10 Ru1 Cl3 89.27(4) . . ?
N19 Ru1 Cl3 91.29(4) . . ?
Cl1 Ru1 Cl3 178.344(15) . . ?
N1 Ru1 Cl2 178.55(4) . . ?
N10 Ru1 Cl2 92.06(5) . . ?
N19 Ru1 Cl2 91.02(5) . . ?
Cl1 Ru1 Cl2 90.57(2) . . ?
Cl3 Ru1 Cl2 89.95(2) . . ?
N28 Ru2 N46 85.82(6) . . ?
N28 Ru2 N37 93.05(6) . . ?
N46 Ru2 N37 178.02(6) . . ?
N28 Ru2 Cl6 89.35(5) . . ?
N46 Ru2 Cl6 89.56(4) . . ?
N37 Ru2 Cl6 88.80(5) . . ?
N28 Ru2 Cl4 89.05(5) . . ?
N46 Ru2 Cl4 90.54(4) . . ?
N37 Ru2 Cl4 91.07(4) . . ?
Cl6 Ru2 Cl4 178.389(16) . . ?
N28 Ru2 Cl5 177.94(4) . . ?
N46 Ru2 Cl5 92.14(5) . . ?
N37 Ru2 Cl5 88.98(5) . . ?
Cl6 Ru2 Cl5 90.33(2) . . ?
Cl4 Ru2 Cl5 91.27(2) . . ?
C2 N1 C5 106.13(15) . . ?
C2 N1 Ru1 124.29(12) . . ?
C5 N1 Ru1 129.50(12) . . ?
N1 C2 N3 111.02(16) . . ?
N1 C2 H2 124.5 . . ?
N3 C2 H2 124.5 . . ?
C2 N3 C4 107.50(15) . . ?
C2 N3 C6 125.60(16) . . ?
C4 N3 C6 126.56(16) . . ?
C5 C4 N3 106.62(17) . . ?
C5 C4 H4 126.7 . . ?
N3 C4 H4 126.7 . . ?
C4 C5 N1 108.72(17) . . ?
C4 C5 H5 125.6 . . ?
N1 C5 H5 125.6 . . ?
N3 C6 C7 112.46(16) . . ?
N3 C6 H6A 109.1 . . ?
C7 C6 H6A 109.1 . . ?
N3 C6 H6B 109.1 . . ?
C7 C6 H6B 109.1 . . ?
H6A C6 H6B 107.8 . . ?
C6 C7 C8 114.26(16) . . ?
C6 C7 H7A 108.7 . . ?
C8 C7 H7A 108.7 . . ?
C6 C7 H7B 108.7 . . ?
C8 C7 H7B 108.7 . . ?
H7A C7 H7B 107.6 . . ?
C9 C8 C7 112.50(18) . . ?
C9 C8 H8A 109.1 . . ?
C7 C8 H8A 109.1 . . ?
C9 C8 H8B 109.1 . . ?
C7 C8 H8B 109.1 . . ?
H8A C8 H8B 107.8 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C11 N10 C14 106.12(14) . . ?
C11 N10 Ru1 129.08(12) . . ?
C14 N10 Ru1 124.76(12) . . ?
N10 C11 N12 110.46(16) . . ?
N10 C11 H11 124.8 . . ?
N12 C11 H11 124.8 . . ?
C11 N12 C13 107.80(14) . . ?
C11 N12 C15 126.22(16) . . ?
C13 N12 C15 125.84(15) . . ?
C14 C13 N12 106.25(15) . . ?
C14 C13 H13 126.9 . . ?
N12 C13 H13 126.9 . . ?
C13 C14 N10 109.37(16) . . ?
C13 C14 H14 125.3 . . ?
N10 C14 H14 125.3 . . ?
N12 C15 C16 112.32(15) . . ?
N12 C15 H15A 109.1 . . ?
C16 C15 H15A 109.1 . . ?
N12 C15 H15B 109.1 . . ?
C16 C15 H15B 109.1 . . ?
H15A C15 H15B 107.9 . . ?
C17 C16 C15 113.93(16) . . ?
C17 C16 H16A 108.8 . . ?
C15 C16 H16A 108.8 . . ?
C17 C16 H16B 108.8 . . ?
C15 C16 H16B 108.8 . . ?
H16A C16 H16B 107.7 . . ?
C16 C17 C18 112.72(19) . . ?
C16 C17 H17A 109.0 . . ?
C18 C17 H17A 109.0 . . ?
C16 C17 H17B 109.0 . . ?
C18 C17 H17B 109.0 . . ?
H17A C17 H17B 107.8 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C20 N19 C23 105.73(15) . . ?
C20 N19 Ru1 125.85(12) . . ?
C23 N19 Ru1 128.39(13) . . ?
N19 C20 N21 111.17(17) . . ?
N19 C20 H20 124.4 . . ?
N21 C20 H20 124.4 . . ?
C20 N21 C22 107.32(16) . . ?
C20 N21 C24 128.93(17) . . ?
C22 N21 C24 123.59(16) . . ?
C23 C22 N21 106.90(16) . . ?
C23 C22 H22 126.6 . . ?
N21 C22 H22 126.6 . . ?
C22 C23 N19 108.88(17) . . ?
C22 C23 H23 125.6 . . ?
N19 C23 H23 125.6 . . ?
N21 C24 C25 114.32(16) . . ?
N21 C24 H24A 108.7 . . ?
C25 C24 H24A 108.7 . . ?
N21 C24 H24B 108.7 . . ?
C25 C24 H24B 108.7 . . ?
H24A C24 H24B 107.6 . . ?
C26 C25 C24 113.7(2) . . ?
C26 C25 H25A 108.8 . . ?
C24 C25 H25A 108.8 . . ?
C26 C25 H25B 108.8 . . ?
C24 C25 H25B 108.8 . . ?
H25A C25 H25B 107.7 . . ?
C25 C26 C27 109.8(2) . . ?
C25 C26 H26A 109.7 . . ?
C27 C26 H26A 109.7 . . ?
C25 C26 H26B 109.7 . . ?
C27 C26 H26B 109.7 . . ?
H26A C26 H26B 108.2 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C29 N28 C32 105.85(15) . . ?
C29 N28 Ru2 124.55(12) . . ?
C32 N28 Ru2 129.21(12) . . ?
N28 C29 N30 110.85(16) . . ?
N28 C29 H29 124.6 . . ?
N30 C29 H29 124.6 . . ?
C29 N30 C31 107.69(15) . . ?
C29 N30 C33 126.35(16) . . ?
C31 N30 C33 125.66(16) . . ?
C32 C31 N30 106.38(17) . . ?
C32 C31 H31 126.8 . . ?
N30 C31 H31 126.8 . . ?
C31 C32 N28 109.23(17) . . ?
C31 C32 H32 125.4 . . ?
N28 C32 H32 125.4 . . ?
N30 C33 C34 111.47(16) . . ?
N30 C33 H33A 109.3 . . ?
C34 C33 H33A 109.3 . . ?
N30 C33 H33B 109.3 . . ?
C34 C33 H33B 109.3 . . ?
H33A C33 H33B 108.0 . . ?
C33 C34 C35 114.01(16) . . ?
C33 C34 H34A 108.8 . . ?
C35 C34 H34A 108.8 . . ?
C33 C34 H34B 108.8 . . ?
C35 C34 H34B 108.8 . . ?
H34A C34 H34B 107.6 . . ?
C36 C35 C34 112.78(18) . . ?
C36 C35 H35A 109.0 . . ?
C34 C35 H35A 109.0 . . ?
C36 C35 H35B 109.0 . . ?
C34 C35 H35B 109.0 . . ?
H35A C35 H35B 107.8 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C38 N37 C41 105.55(15) . . ?
C38 N37 Ru2 122.93(12) . . ?
C41 N37 Ru2 131.42(13) . . ?
N37 C38 N39 111.45(16) . . ?
N37 C38 H38 124.3 . . ?
N39 C38 H38 124.3 . . ?
C38 N39 C40 107.20(16) . . ?
C38 N39 C42 125.78(17) . . ?
C40 N39 C42 126.96(16) . . ?
C41 C40 N39 106.57(16) . . ?
C41 C40 H40 126.7 . . ?
N39 C40 H40 126.7 . . ?
C40 C41 N37 109.23(18) . . ?
C40 C41 H41 125.4 . . ?
N37 C41 H41 125.4 . . ?
N39 C42 C43 112.37(16) . . ?
N39 C42 H42A 109.1 . . ?
C43 C42 H42A 109.1 . . ?
N39 C42 H42B 109.1 . . ?
C43 C42 H42B 109.1 . . ?
H42A C42 H42B 107.9 . . ?
C44 C43 C42 113.69(17) . . ?
C44 C43 H43A 108.8 . . ?
C42 C43 H43A 108.8 . . ?
C44 C43 H43B 108.8 . . ?
C42 C43 H43B 108.8 . . ?
H43A C43 H43B 107.7 . . ?
C43 C44 C45 111.40(19) . . ?
C43 C44 H44A 109.3 . . ?
C45 C44 H44A 109.3 . . ?
C43 C44 H44B 109.3 . . ?
C45 C44 H44B 109.3 . . ?
H44A C44 H44B 108.0 . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C44 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C47 N46 C50 106.22(14) . . ?
C47 N46 Ru2 127.81(13) . . ?
C50 N46 Ru2 125.87(12) . . ?
N46 C47 N48 110.80(16) . . ?
N46 C47 H47 124.6 . . ?
N48 C47 H47 124.6 . . ?
C47 N48 C49 107.62(15) . . ?
C47 N48 C51 126.06(16) . . ?
C49 N48 C51 126.12(15) . . ?
C50 C49 N48 106.35(16) . . ?
C50 C49 H49 126.8 . . ?
N48 C49 H49 126.8 . . ?
C49 C50 N46 109.01(16) . . ?
C49 C50 H50 125.5 . . ?
N46 C50 H50 125.5 . . ?
N48 C51 C52 112.30(15) . . ?
N48 C51 H51A 109.1 . . ?
C52 C51 H51A 109.1 . . ?
N48 C51 H51B 109.1 . . ?
C52 C51 H51B 109.1 . . ?
H51A C51 H51B 107.9 . . ?
C53 C52 C51 113.41(16) . . ?
C53 C52 H52A 108.9 . . ?
C51 C52 H52A 108.9 . . ?
C53 C52 H52B 108.9 . . ?
C51 C52 H52B 108.9 . . ?
H52A C52 H52B 107.7 . . ?
C52 C53 C54 112.4(2) . . ?
C52 C53 H53A 109.1 . . ?
C54 C53 H53A 109.1 . . ?
C52 C53 H53B 109.1 . . ?
C54 C53 H53B 109.1 . . ?
H53A C53 H53B 107.9 . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
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 2.0623(15) . ?
Ru1 N10 2.0769(14) . ?
Ru1 N19 2.0887(14) . ?
Ru1 Cl1 2.3602(6) . ?
Ru1 Cl3 2.3604(6) . ?
Ru1 Cl2 2.3696(6) . ?
Ru2 N28 2.0669(15) . ?
Ru2 N46 2.0744(15) . ?
Ru2 N37 2.0763(15) . ?
Ru2 Cl6 2.3522(6) . ?
Ru2 Cl4 2.3597(6) . ?
Ru2 Cl5 2.3800(6) . ?
N1 C2 1.326(2) . ?
N1 C5 1.379(2) . ?
C2 N3 1.340(2) . ?
C2 H2 0.9300 . ?
N3 C4 1.369(2) . ?
N3 C6 1.474(2) . ?
C4 C5 1.364(3) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C6 C7 1.515(3) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.524(3) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C9 1.519(3) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
N10 C11 1.330(2) . ?
N10 C14 1.382(2) . ?
C11 N12 1.350(2) . ?
C11 H11 0.9300 . ?
N12 C13 1.375(2) . ?
N12 C15 1.471(2) . ?
C13 C14 1.358(2) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C15 C16 1.524(3) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.518(3) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.525(3) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
N19 C20 1.323(2) . ?
N19 C23 1.383(2) . ?
C20 N21 1.345(2) . ?
C20 H20 0.9300 . ?
N21 C22 1.363(3) . ?
N21 C24 1.469(2) . ?
C22 C23 1.357(3) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 C25 1.518(3) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 C26 1.497(3) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 C27 1.565(4) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
N28 C29 1.330(2) . ?
N28 C32 1.379(2) . ?
C29 N30 1.344(2) . ?
C29 H29 0.9300 . ?
N30 C31 1.369(2) . ?
N30 C33 1.473(2) . ?
C31 C32 1.362(3) . ?
C31 H31 0.9300 . ?
C32 H32 0.9300 . ?
C33 C34 1.519(3) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 C35 1.522(3) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C35 C36 1.511(3) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
N37 C38 1.327(2) . ?
N37 C41 1.379(2) . ?
C38 N39 1.339(2) . ?
C38 H38 0.9300 . ?
N39 C40 1.371(3) . ?
N39 C42 1.466(2) . ?
C40 C41 1.358(3) . ?
C40 H40 0.9300 . ?
C41 H41 0.9300 . ?
C42 C43 1.530(3) . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C43 C44 1.516(3) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C44 C45 1.522(3) . ?
C44 H44A 0.9700 . ?
C44 H44B 0.9700 . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9600 . ?
N46 C47 1.327(2) . ?
N46 C50 1.382(2) . ?
C47 N48 1.348(2) . ?
C47 H47 0.9300 . ?
N48 C49 1.375(2) . ?
N48 C51 1.469(2) . ?
C49 C50 1.365(2) . ?
C49 H49 0.9300 . ?
C50 H50 0.9300 . ?
C51 C52 1.526(3) . ?
C51 H51A 0.9700 . ?
C51 H51B 0.9700 . ?
C52 C53 1.519(3) . ?
C52 H52A 0.9700 . ?
C52 H52B 0.9700 . ?
C53 C54 1.525(3) . ?
C53 H53A 0.9700 . ?
C53 H53B 0.9700 . ?
C54 H54A 0.9600 . ?
C54 H54B 0.9600 . ?
C54 H54C 0.9600 . ?
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
N10 Ru1 N1 C2 50.72(15) . . . . ?
N19 Ru1 N1 C2 -129.89(15) . . . . ?
Cl1 Ru1 N1 C2 139.83(15) . . . . ?
Cl3 Ru1 N1 C2 -38.60(15) . . . . ?
Cl2 Ru1 N1 C2 -0.2(19) . . . . ?
N10 Ru1 N1 C5 -125.56(16) . . . . ?
N19 Ru1 N1 C5 53.83(16) . . . . ?
Cl1 Ru1 N1 C5 -36.44(16) . . . . ?
Cl3 Ru1 N1 C5 145.12(16) . . . . ?
Cl2 Ru1 N1 C5 -176(79) . . . . ?
C5 N1 C2 N3 0.1(2) . . . . ?
Ru1 N1 C2 N3 -176.92(12) . . . . ?
N1 C2 N3 C4 0.2(2) . . . . ?
N1 C2 N3 C6 173.89(17) . . . . ?
C2 N3 C4 C5 -0.4(2) . . . . ?
C6 N3 C4 C5 -174.01(18) . . . . ?
N3 C4 C5 N1 0.4(2) . . . . ?
C2 N1 C5 C4 -0.3(2) . . . . ?
Ru1 N1 C5 C4 176.46(14) . . . . ?
C2 N3 C6 C7 -90.3(2) . . . . ?
C4 N3 C6 C7 82.2(2) . . . . ?
N3 C6 C7 C8 57.0(2) . . . . ?
C6 C7 C8 C9 171.94(18) . . . . ?
N1 Ru1 N10 C11 -124.39(15) . . . . ?
N19 Ru1 N10 C11 -135.7(10) . . . . ?
Cl1 Ru1 N10 C11 145.02(15) . . . . ?
Cl3 Ru1 N10 C11 -35.44(15) . . . . ?
Cl2 Ru1 N10 C11 54.48(15) . . . . ?
N1 Ru1 N10 C14 53.08(14) . . . . ?
N19 Ru1 N10 C14 41.8(11) . . . . ?
Cl1 Ru1 N10 C14 -37.51(13) . . . . ?
Cl3 Ru1 N10 C14 142.03(13) . . . . ?
Cl2 Ru1 N10 C14 -128.05(13) . . . . ?
C14 N10 C11 N12 0.29(19) . . . . ?
Ru1 N10 C11 N12 178.12(11) . . . . ?
N10 C11 N12 C13 -0.2(2) . . . . ?
N10 C11 N12 C15 175.58(16) . . . . ?
C11 N12 C13 C14 0.0(2) . . . . ?
C15 N12 C13 C14 -175.77(16) . . . . ?
N12 C13 C14 N10 0.1(2) . . . . ?
C11 N10 C14 C13 -0.3(2) . . . . ?
Ru1 N10 C14 C13 -178.21(12) . . . . ?
C11 N12 C15 C16 130.05(18) . . . . ?
C13 N12 C15 C16 -54.9(2) . . . . ?
N12 C15 C16 C17 -64.7(2) . . . . ?
C15 C16 C17 C18 177.80(19) . . . . ?
N1 Ru1 N19 C20 93.95(16) . . . . ?
N10 Ru1 N19 C20 105.2(11) . . . . ?
Cl1 Ru1 N19 C20 -175.50(15) . . . . ?
Cl3 Ru1 N19 C20 5.04(15) . . . . ?
Cl2 Ru1 N19 C20 -84.93(15) . . . . ?
N1 Ru1 N19 C23 -84.03(16) . . . . ?
N10 Ru1 N19 C23 -72.8(11) . . . . ?
Cl1 Ru1 N19 C23 6.52(15) . . . . ?
Cl3 Ru1 N19 C23 -172.94(15) . . . . ?
Cl2 Ru1 N19 C23 97.09(15) . . . . ?
C23 N19 C20 N21 -0.5(2) . . . . ?
Ru1 N19 C20 N21 -178.89(12) . . . . ?
N19 C20 N21 C22 0.6(2) . . . . ?
N19 C20 N21 C24 176.06(19) . . . . ?
C20 N21 C22 C23 -0.4(2) . . . . ?
C24 N21 C22 C23 -176.16(18) . . . . ?
N21 C22 C23 N19 0.1(2) . . . . ?
C20 N19 C23 C22 0.3(2) . . . . ?
Ru1 N19 C23 C22 178.59(13) . . . . ?
C20 N21 C24 C25 2.8(3) . . . . ?
C22 N21 C24 C25 177.64(19) . . . . ?
N21 C24 C25 C26 74.9(3) . . . . ?
C24 C25 C26 C27 -175.5(2) . . . . ?
N46 Ru2 N28 C29 -55.71(15) . . . . ?
N37 Ru2 N28 C29 122.66(15) . . . . ?
Cl6 Ru2 N28 C29 33.90(15) . . . . ?
Cl4 Ru2 N28 C29 -146.32(15) . . . . ?
Cl5 Ru2 N28 C29 -47.2(13) . . . . ?
N46 Ru2 N28 C32 116.07(16) . . . . ?
N37 Ru2 N28 C32 -65.56(16) . . . . ?
Cl6 Ru2 N28 C32 -154.33(16) . . . . ?
Cl4 Ru2 N28 C32 25.46(16) . . . . ?
Cl5 Ru2 N28 C32 124.6(12) . . . . ?
C32 N28 C29 N30 -0.1(2) . . . . ?
Ru2 N28 C29 N30 173.32(11) . . . . ?
N28 C29 N30 C31 0.1(2) . . . . ?
N28 C29 N30 C33 -173.84(17) . . . . ?
C29 N30 C31 C32 0.0(2) . . . . ?
C33 N30 C31 C32 173.91(18) . . . . ?
N30 C31 C32 N28 0.0(2) . . . . ?
C29 N28 C32 C31 0.0(2) . . . . ?
Ru2 N28 C32 C31 -172.93(13) . . . . ?
C29 N30 C33 C34 99.3(2) . . . . ?
C31 N30 C33 C34 -73.6(2) . . . . ?
N30 C33 C34 C35 -58.0(2) . . . . ?
C33 C34 C35 C36 -171.33(18) . . . . ?
N28 Ru2 N37 C38 -133.36(15) . . . . ?
N46 Ru2 N37 C38 -78.2(18) . . . . ?
Cl6 Ru2 N37 C38 -44.08(14) . . . . ?
Cl4 Ru2 N37 C38 137.53(14) . . . . ?
Cl5 Ru2 N37 C38 46.28(14) . . . . ?
N28 Ru2 N37 C41 42.32(17) . . . . ?
N46 Ru2 N37 C41 97.5(17) . . . . ?
Cl6 Ru2 N37 C41 131.60(17) . . . . ?
Cl4 Ru2 N37 C41 -46.79(17) . . . . ?
Cl5 Ru2 N37 C41 -138.04(17) . . . . ?
C41 N37 C38 N39 -0.1(2) . . . . ?
Ru2 N37 C38 N39 176.54(12) . . . . ?
N37 C38 N39 C40 0.0(2) . . . . ?
N37 C38 N39 C42 -177.55(16) . . . . ?
C38 N39 C40 C41 0.2(2) . . . . ?
C42 N39 C40 C41 177.64(17) . . . . ?
N39 C40 C41 N37 -0.2(2) . . . . ?
C38 N37 C41 C40 0.2(2) . . . . ?
Ru2 N37 C41 C40 -176.02(13) . . . . ?
C38 N39 C42 C43 88.0(2) . . . . ?
C40 N39 C42 C43 -89.0(2) . . . . ?
N39 C42 C43 C44 -68.2(3) . . . . ?
C42 C43 C44 C45 -178.7(2) . . . . ?
N28 Ru2 N46 C47 123.65(15) . . . . ?
N37 Ru2 N46 C47 68.4(18) . . . . ?
Cl6 Ru2 N46 C47 34.26(15) . . . . ?
Cl4 Ru2 N46 C47 -147.34(15) . . . . ?
Cl5 Ru2 N46 C47 -56.05(15) . . . . ?
N28 Ru2 N46 C50 -52.33(14) . . . . ?
N37 Ru2 N46 C50 -107.6(17) . . . . ?
Cl6 Ru2 N46 C50 -141.71(14) . . . . ?
Cl4 Ru2 N46 C50 36.68(14) . . . . ?
Cl5 Ru2 N46 C50 127.98(14) . . . . ?
C50 N46 C47 N48 0.1(2) . . . . ?
Ru2 N46 C47 N48 -176.47(11) . . . . ?
N46 C47 N48 C49 -0.3(2) . . . . ?
N46 C47 N48 C51 -175.28(15) . . . . ?
C47 N48 C49 C50 0.3(2) . . . . ?
C51 N48 C49 C50 175.32(16) . . . . ?
N48 C49 C50 N46 -0.3(2) . . . . ?
C47 N46 C50 C49 0.1(2) . . . . ?
Ru2 N46 C50 C49 176.77(12) . . . . ?
C47 N48 C51 C52 -130.63(19) . . . . ?
C49 N48 C51 C52 55.3(2) . . . . ?
N48 C51 C52 C53 65.9(2) . . . . ?
C51 C52 C53 C54 -177.8(2) . . . . ?
