#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/81/4308107.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_4308107
loop_
_publ_author_name
'Wolfgang F. Schmid'
'Stefanie Zorbas-Seifried'
'Roland O. John'
'Vladimir B. Arion'
'Michael A. Jakupec'
'Alexander Roller'
'Markus Galanski'
'Ion Chiorescu'
'Haralabos Zorbas'
'Bernhard K. Keppler'
_publ_section_title
;
The First Ruthenium-Based Paullones: Syntheses, X-ray Diffraction
Structures, and Spectroscopic and Antiproliferative Properties in Vitro
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3645
_journal_page_last               3656
_journal_paper_doi               10.1021/ic070098j
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C51.6 H55.2 Br2 Cl2 N8 O4 Ru S'
_chemical_formula_weight         1215.29
_chemical_name_systematic
; 
(OC-6-43)-Bis(9-bromo-6-(E)-[(alpha-picolyl-kappaN)imino-kappaN]-
7,12-dihydroindolo[3,2-d][1]benzazepine)chloro(dimethyl sulfoxide)
ruthenium(II) chloride 2.8ethanol 0.2water
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                106.807(2)
_cell_angle_beta                 92.525(2)
_cell_angle_gamma                108.003(2)
_cell_formula_units_Z            2
_cell_length_a                   12.4094(3)
_cell_length_b                   12.8933(3)
_cell_length_c                   18.5633(5)
_cell_measurement_temperature    100(2)
_cell_volume                     2674.83(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0399
_diffrn_reflns_av_sigmaI/netI    0.0391
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            41729
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.69
_exptl_absorpt_coefficient_mu    1.977
_exptl_absorpt_correction_T_max  0.8906
_exptl_absorpt_correction_T_min  0.5885
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1234
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.06
_refine_diff_density_max         3.310
_refine_diff_density_min         -2.372
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     660
_refine_ls_number_reflns         10496
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0454
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0776P)²+4.1046P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1310
_refine_ls_wR_factor_ref         0.1389
_reflns_number_gt                8281
_reflns_number_total             10496
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic070098jsi20070119_060104.cif
_cod_data_source_block           WOSC269
_cod_original_cell_volume        2674.82(12)
_cod_original_formula_sum        'C51.60 H55.20 Br2 Cl2 N8 O4 Ru S'
_cod_database_code               4308107
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
C47 C 0.0625(12) 0.6351(8) 0.2252(5) 0.115(5) Uani 1 1 d D . .
H47A H 0.1392 0.6344 0.2329 0.173 Uiso 0.608(19) 1 d PR A 1
H47B H 0.0273 0.6214 0.2682 0.173 Uiso 0.608(19) 1 d PR A 1
C48 C 0.0073(10) 0.5465(8) 0.1635(6) 0.045(3) Uani 0.608(19) 1 d PD A 1
H48A H 0.0456 0.5558 0.1196 0.067 Uiso 0.608(19) 1 calc PR A 1
H48B H -0.0720 0.5438 0.1541 0.067 Uiso 0.608(19) 1 calc PR A 1
H48C H 0.0078 0.4748 0.1716 0.067 Uiso 0.608(19) 1 calc PR A 1
O2 O 0.072(3) 0.7459(10) 0.2264(15) 0.076(8) Uani 0.608(19) 1 d PD A 1
H20A H 0.0081 0.7554 0.2317 0.114 Uiso 0.608(19) 1 calc PR A 1
H47C H 0.0850 0.6338 0.2755 0.114 Uiso 0.392(19) 1 d PR A 2
H47D H -0.0168 0.5993 0.2125 0.114 Uiso 0.392(19) 1 d PR A 2
C48X C 0.111(2) 0.571(2) 0.1776(11) 0.082(9) Uani 0.392(19) 1 d PD A 2
H48D H 0.0670 0.4897 0.1678 0.123 Uiso 0.392(19) 1 calc PR A 2
H48E H 0.1895 0.5878 0.2001 0.123 Uiso 0.392(19) 1 calc PR A 2
H48F H 0.1110 0.5889 0.1297 0.123 Uiso 0.392(19) 1 calc PR A 2
O2X O 0.091(3) 0.7504(9) 0.2299(17) 0.050(8) Uani 0.392(19) 1 d PD A 2
H20B H 0.0621 0.7551 0.1895 0.074 Uiso 0.392(19) 1 calc PR A 2
O3 O 0.4509(5) 0.6298(5) 0.2482(3) 0.0589(16) Uani 0.80 1 d P . .
H30A H 0.4330 0.6235 0.1959 0.088 Uiso 0.80 1 d PR . .
C49 C 0.5307(7) 0.7255(6) 0.3102(5) 0.0470(19) Uani 0.80 1 d P . .
H49A H 0.5125 0.7168 0.3599 0.056 Uiso 0.80 1 calc PR . .
H49B H 0.6103 0.7266 0.3059 0.056 Uiso 0.80 1 calc PR . .
C50 C 0.5189(9) 0.8324(7) 0.3041(6) 0.079(3) Uani 0.80 1 d P . .
H50A H 0.5560 0.8507 0.2617 0.119 Uiso 0.80 1 calc PR . .
H50B H 0.5552 0.8952 0.3515 0.119 Uiso 0.80 1 calc PR . .
H50C H 0.4375 0.8228 0.2951 0.119 Uiso 0.80 1 calc PR . .
O4 O 0.4508(4) 0.6274(4) 0.0963(3) 0.0817(17) Uani 1 1 d D . .
H40A H 0.4816 0.7012 0.1187 0.098 Uiso 0.551(6) 1 d PR B 1
H40B H 0.4077 0.6679 0.1094 0.098 Uiso 0.449(6) 1 d PR B 2
C51 C 0.3257(7) 0.5856(7) 0.0726(5) 0.0296(11) Uiso 0.551(6) 1 d PD B 1
H51A H 0.2927 0.6321 0.1118 0.035 Uiso 0.551(6) 1 calc PR B 1
H51B H 0.3116 0.6020 0.0249 0.035 Uiso 0.551(6) 1 calc PR B 1
C52 C 0.2609(7) 0.4634(7) 0.0601(5) 0.0296(11) Uiso 0.551(6) 1 d PD B 1
H52A H 0.2988 0.4153 0.0275 0.044 Uiso 0.551(6) 1 calc PR B 1
H52B H 0.1828 0.4448 0.0353 0.044 Uiso 0.551(6) 1 calc PR B 1
H52C H 0.2580 0.4489 0.1091 0.044 Uiso 0.551(6) 1 calc PR B 1
C51X C 0.5533(8) 0.6674(9) 0.0636(6) 0.0296(11) Uiso 0.449(6) 1 d PD B 2
H51C H 0.5819 0.6015 0.0520 0.035 Uiso 0.449(6) 1 calc PR B 2
H51D H 0.5229 0.6680 0.0136 0.035 Uiso 0.449(6) 1 calc PR B 2
C52X C 0.6568(8) 0.7657(9) 0.0865(6) 0.0296(11) Uiso 0.449(6) 1 d PD B 2
H52D H 0.6543 0.8174 0.0573 0.044 Uiso 0.449(6) 1 calc PR B 2
H52E H 0.7229 0.7401 0.0769 0.044 Uiso 0.449(6) 1 calc PR B 2
H52F H 0.6637 0.8065 0.1409 0.044 Uiso 0.449(6) 1 calc PR B 2
O100 O 0.623(2) 0.795(2) 0.2144(13) 0.053(6) Uiso 0.20 1 d P . .
Ru1 Ru 0.40690(3) 0.26181(3) 0.276747(19) 0.01316(10) Uani 1 1 d . . .
Br2 Br 0.24203(5) -0.32967(4) 0.40405(3) 0.03379(15) Uani 1 1 d . . .
Br1 Br 0.26100(5) -0.24690(5) -0.08591(3) 0.03890(16) Uani 1 1 d . . .
Cl1 Cl 0.38086(9) 0.44650(8) 0.34026(6) 0.0187(2) Uani 1 1 d . . .
Cl2 Cl 0.84570(16) 0.80126(12) 0.24543(8) 0.0532(4) Uani 1 1 d . . .
S1 S 0.52324(9) 0.26642(9) 0.37318(6) 0.0174(2) Uani 1 1 d . . .
O1 O 0.6411(3) 0.2731(3) 0.35812(19) 0.0253(7) Uani 1 1 d . . .
N1 N -0.0401(3) -0.0824(3) 0.1291(2) 0.0184(8) Uani 1 1 d . . .
H1 H -0.0934 -0.1162 0.1526 0.022 Uiso 1 1 calc R . .
N2 N 0.1486(3) 0.2675(3) 0.2201(2) 0.0172(7) Uani 1 1 d . . .
N3 N 0.3123(3) 0.2513(3) 0.1761(2) 0.0173(7) Uani 1 1 d . . .
N4 N 0.5317(3) 0.3598(3) 0.2283(2) 0.0196(8) Uani 1 1 d . . .
N5 N 0.1600(3) 0.1044(3) 0.5714(2) 0.0217(8) Uani 1 1 d . . .
H5 H 0.1647 0.1422 0.6199 0.026 Uiso 1 1 calc R . .
N6 N 0.2219(3) 0.2690(3) 0.4044(2) 0.0163(7) Uani 1 1 d . . .
N7 N 0.2647(3) 0.1451(3) 0.30303(19) 0.0130(7) Uani 1 1 d . . .
N8 N 0.4231(3) 0.1086(3) 0.21645(19) 0.0150(7) Uani 1 1 d . . .
C1 C 0.1616(4) -0.1974(4) -0.0196(3) 0.0249(10) Uani 1 1 d . . .
C2 C 0.0882(4) -0.2794(4) 0.0071(3) 0.0257(10) Uani 1 1 d . . .
H2 H 0.0878 -0.3565 -0.0092 0.031 Uiso 1 1 calc R . .
C3 C 0.0158(4) -0.2485(4) 0.0577(2) 0.0224(10) Uani 1 1 d . . .
H3 H -0.0348 -0.3034 0.0764 0.027 Uiso 1 1 calc R . .
C4 C 0.0198(4) -0.1356(4) 0.0797(2) 0.0183(9) Uani 1 1 d . . .
C5 C -0.0032(4) 0.0330(4) 0.1360(2) 0.0159(9) Uani 1 1 d . . .
C6 C -0.0438(4) 0.1158(4) 0.1884(2) 0.0170(9) Uani 1 1 d . . .
C7 C -0.1556(4) 0.0834(4) 0.2058(2) 0.0194(9) Uani 1 1 d . . .
H7 H -0.2059 0.0068 0.1819 0.023 Uiso 1 1 calc R . .
C8 C -0.1942(4) 0.1608(4) 0.2572(2) 0.0200(9) Uani 1 1 d . . .
H8 H -0.2703 0.1374 0.2684 0.024 Uiso 1 1 calc R . .
C9 C -0.1209(4) 0.2731(4) 0.2921(2) 0.0218(10) Uani 1 1 d . . .
H9 H -0.1473 0.3269 0.3267 0.026 Uiso 1 1 calc R . .
C10 C -0.0098(4) 0.3066(4) 0.2769(3) 0.0204(9) Uani 1 1 d . . .
H10 H 0.0398 0.3832 0.3016 0.024 Uiso 1 1 calc R . .
C11 C 0.0308(3) 0.2296(4) 0.2256(2) 0.0164(9) Uani 1 1 d . . .
C12 C 0.2038(4) 0.2344(4) 0.1608(2) 0.0171(9) Uani 1 1 d . . .
C13 C 0.3876(4) 0.2548(4) 0.1172(2) 0.0193(9) Uani 1 1 d . . .
H13A H 0.3534 0.2724 0.0749 0.023 Uiso 1 1 calc R . .
H13B H 0.3991 0.1798 0.0966 0.023 Uiso 1 1 calc R . .
C14 C 0.4995(4) 0.3478(4) 0.1549(3) 0.0204(9) Uani 1 1 d . . .
C15 C 0.5634(4) 0.4189(4) 0.1179(3) 0.0280(11) Uani 1 1 d . . .
H15 H 0.5389 0.4092 0.0665 0.034 Uiso 1 1 calc R . .
C16 C 0.6639(5) 0.5046(4) 0.1573(3) 0.0341(12) Uani 1 1 d . . .
H16 H 0.7088 0.5555 0.1334 0.041 Uiso 1 1 calc R . .
C17 C 0.6986(4) 0.5159(4) 0.2319(3) 0.0314(12) Uani 1 1 d . . .
H17 H 0.7681 0.5735 0.2594 0.038 Uiso 1 1 calc R . .
C18 C 0.6311(4) 0.4426(4) 0.2651(3) 0.0229(10) Uani 1 1 d . . .
H18 H 0.6552 0.4503 0.3162 0.027 Uiso 1 1 calc R . .
C19 C 0.1333(4) 0.1719(4) 0.0835(2) 0.0173(9) Uani 1 1 d . . .
H19A H 0.0767 0.2081 0.0742 0.021 Uiso 1 1 calc R . .
H19B H 0.1823 0.1698 0.0428 0.021 Uiso 1 1 calc R . .
C20 C 0.0755(4) 0.0538(4) 0.0881(2) 0.0163(9) Uani 1 1 d . . .
C21 C 0.0949(4) -0.0522(4) 0.0523(2) 0.0173(9) Uani 1 1 d . . .
C22 C 0.1668(4) -0.0852(4) 0.0008(2) 0.0202(9) Uani 1 1 d . . .
H22 H 0.2171 -0.0317 -0.0191 0.024 Uiso 1 1 calc R . .
C23 C 0.2074(4) -0.1967(4) 0.4594(3) 0.0242(10) Uani 1 1 d . . .
C24 C 0.2168(4) -0.1696(4) 0.5389(3) 0.0259(10) Uani 1 1 d . . .
H24 H 0.2349 -0.2189 0.5631 0.031 Uiso 1 1 calc R . .
C25 C 0.1995(4) -0.0705(4) 0.5814(3) 0.0255(10) Uani 1 1 d . . .
H25 H 0.2049 -0.0503 0.6352 0.031 Uiso 1 1 calc R . .
C26 C 0.1737(4) -0.0011(4) 0.5429(3) 0.0209(9) Uani 1 1 d . . .
C27 C 0.1378(4) 0.1406(4) 0.5116(2) 0.0181(9) Uani 1 1 d . . .
C28 C 0.1288(4) 0.2532(4) 0.5200(2) 0.0177(9) Uani 1 1 d . . .
C29 C 0.0892(4) 0.3121(4) 0.5835(3) 0.0222(10) Uani 1 1 d . . .
H29 H 0.0656 0.2766 0.6211 0.027 Uiso 1 1 calc R . .
C30 C 0.0836(4) 0.4197(4) 0.5926(3) 0.0248(10) Uani 1 1 d . . .
H30 H 0.0562 0.4576 0.6360 0.030 Uiso 1 1 calc R . .
C31 C 0.1183(4) 0.4733(4) 0.5380(3) 0.0230(10) Uani 1 1 d . . .
H31 H 0.1141 0.5476 0.5440 0.028 Uiso 1 1 calc R . .
C32 C 0.1583(4) 0.4182(4) 0.4758(3) 0.0196(9) Uani 1 1 d . . .
H32 H 0.1820 0.4552 0.4389 0.024 Uiso 1 1 calc R . .
C33 C 0.1650(3) 0.3086(3) 0.4656(2) 0.0160(8) Uani 1 1 d . . .
C34 C 0.1990(3) 0.1601(3) 0.3550(2) 0.0137(8) Uani 1 1 d . . .
C35 C 0.2348(4) 0.0283(3) 0.2488(2) 0.0155(8) Uani 1 1 d . . .
H35A H 0.1679 0.0133 0.2114 0.019 Uiso 1 1 calc R . .
H35B H 0.2131 -0.0285 0.2765 0.019 Uiso 1 1 calc R . .
C36 C 0.3333(3) 0.0135(4) 0.2075(2) 0.0157(8) Uani 1 1 d . . .
C37 C 0.3308(4) -0.0937(4) 0.1632(3) 0.0214(9) Uani 1 1 d . . .
H37 H 0.2657 -0.1597 0.1574 0.026 Uiso 1 1 calc R . .
C38 C 0.4243(4) -0.1043(4) 0.1273(3) 0.0260(10) Uani 1 1 d . . .
H38 H 0.4239 -0.1771 0.0958 0.031 Uiso 1 1 calc R . .
C39 C 0.5179(4) -0.0068(4) 0.1381(3) 0.0256(10) Uani 1 1 d . . .
H39 H 0.5835 -0.0119 0.1148 0.031 Uiso 1 1 calc R . .
C40 C 0.5155(4) 0.0979(4) 0.1830(3) 0.0201(9) Uani 1 1 d . . .
H40 H 0.5806 0.1646 0.1907 0.024 Uiso 1 1 calc R . .
C41 C 0.1003(4) 0.0690(3) 0.3687(2) 0.0168(9) Uani 1 1 d . . .
H41A H 0.0306 0.0910 0.3690 0.020 Uiso 1 1 calc R . .
H41B H 0.0846 -0.0052 0.3279 0.020 Uiso 1 1 calc R . .
C42 C 0.1323(4) 0.0579(4) 0.4441(2) 0.0174(9) Uani 1 1 d . . .
C43 C 0.1590(4) -0.0322(4) 0.4627(3) 0.0188(9) Uani 1 1 d . . .
C44 C 0.1770(4) -0.1327(4) 0.4199(3) 0.0211(9) Uani 1 1 d . . .
H44 H 0.1685 -0.1555 0.3659 0.025 Uiso 1 1 calc R . .
C45 C 0.5384(4) 0.3771(5) 0.4605(3) 0.0323(12) Uani 1 1 d . . .
H45A H 0.5907 0.3714 0.4991 0.049 Uiso 1 1 calc R . .
H45B H 0.4634 0.3686 0.4775 0.049 Uiso 1 1 calc R . .
H45C H 0.5693 0.4523 0.4530 0.049 Uiso 1 1 calc R . .
C46 C 0.4715(4) 0.1453(4) 0.4057(3) 0.0271(11) Uani 1 1 d . . .
H46A H 0.4597 0.0745 0.3636 0.041 Uiso 1 1 calc R . .
H46B H 0.3988 0.1437 0.4247 0.041 Uiso 1 1 calc R . .
H46C H 0.5277 0.1511 0.4468 0.041 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'
Br Br -0.2901 2.4595 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
C48X C47 C48 54.6(12) . . ?
C48X C47 O2 122.5(19) . . ?
C48 C47 O2 119.2(14) . . ?
C48X C47 O2X 118(2) . . ?
C48 C47 O2X 124.7(16) . . ?
C50 C49 O3 107.7(6) . . ?
C51X O4 C51 137.4(7) . . ?
C52 C51 O4 118.6(7) . . ?
C52X C51X O4 135.9(9) . . ?
N8 Ru1 N4 94.43(14) . . ?
N8 Ru1 N3 86.52(13) . . ?
N4 Ru1 N3 77.69(14) . . ?
N8 Ru1 N7 79.52(13) . . ?
N4 Ru1 N7 168.55(14) . . ?
N3 Ru1 N7 92.15(13) . . ?
N8 Ru1 S1 88.18(10) . . ?
N4 Ru1 S1 97.34(11) . . ?
N3 Ru1 S1 172.42(10) . . ?
N7 Ru1 S1 92.21(9) . . ?
N8 Ru1 Cl1 175.70(10) . . ?
N4 Ru1 Cl1 84.10(10) . . ?
N3 Ru1 Cl1 89.22(10) . . ?
N7 Ru1 Cl1 101.22(9) . . ?
S1 Ru1 Cl1 96.01(4) . . ?
O1 S1 C45 106.1(2) . . ?
O1 S1 C46 105.5(2) . . ?
C45 S1 C46 98.6(3) . . ?
O1 S1 Ru1 115.38(14) . . ?
C45 S1 Ru1 115.94(17) . . ?
C46 S1 Ru1 113.50(16) . . ?
C4 N1 C5 108.7(4) . . ?
C12 N2 C11 129.4(4) . . ?
C12 N3 C13 121.2(4) . . ?
C12 N3 Ru1 129.8(3) . . ?
C13 N3 Ru1 108.8(3) . . ?
C18 N4 C14 118.1(4) . . ?
C18 N4 Ru1 126.6(3) . . ?
C14 N4 Ru1 114.5(3) . . ?
C27 N5 C26 108.5(4) . . ?
C34 N6 C33 129.6(4) . . ?
C34 N7 C35 116.8(3) . . ?
C34 N7 Ru1 131.7(3) . . ?
C35 N7 Ru1 111.5(2) . . ?
C36 N8 C40 118.6(4) . . ?
C36 N8 Ru1 116.8(3) . . ?
C40 N8 Ru1 124.6(3) . . ?
C22 C1 C2 123.5(4) . . ?
C22 C1 Br1 119.6(4) . . ?
C2 C1 Br1 116.9(3) . . ?
C3 C2 C1 120.1(4) . . ?
C4 C3 C2 117.7(4) . . ?
N1 C4 C3 129.7(4) . . ?
N1 C4 C21 108.2(4) . . ?
C3 C4 C21 122.0(4) . . ?
C20 C5 N1 109.6(4) . . ?
C20 C5 C6 127.6(4) . . ?
N1 C5 C6 122.8(4) . . ?
C7 C6 C11 118.6(4) . . ?
C7 C6 C5 120.8(4) . . ?
C11 C6 C5 120.5(4) . . ?
C8 C7 C6 121.3(4) . . ?
C7 C8 C9 119.5(4) . . ?
C10 C9 C8 120.3(4) . . ?
C9 C10 C11 121.0(4) . . ?
C10 C11 N2 116.8(4) . . ?
C10 C11 C6 119.3(4) . . ?
N2 C11 C6 123.5(4) . . ?
N3 C12 N2 117.3(4) . . ?
N3 C12 C19 124.8(4) . . ?
N2 C12 C19 117.6(4) . . ?
N3 C13 C14 106.5(4) . . ?
N4 C14 C15 122.2(4) . . ?
N4 C14 C13 115.7(4) . . ?
C15 C14 C13 122.1(4) . . ?
C14 C15 C16 118.6(5) . . ?
C15 C16 C17 119.5(5) . . ?
C18 C17 C16 118.8(5) . . ?
N4 C18 C17 122.7(5) . . ?
C20 C19 C12 102.5(3) . . ?
C5 C20 C21 107.5(4) . . ?
C5 C20 C19 122.4(4) . . ?
C21 C20 C19 129.9(4) . . ?
C22 C21 C4 119.4(4) . . ?
C22 C21 C20 134.8(4) . . ?
C4 C21 C20 105.8(4) . . ?
C1 C22 C21 117.2(4) . . ?
C44 C23 C24 123.9(4) . . ?
C44 C23 Br2 118.6(4) . . ?
C24 C23 Br2 117.4(3) . . ?
C25 C24 C23 119.3(4) . . ?
C24 C25 C26 117.9(4) . . ?
N5 C26 C25 129.6(4) . . ?
N5 C26 C43 108.1(4) . . ?
C25 C26 C43 122.3(4) . . ?
N5 C27 C42 109.9(4) . . ?
N5 C27 C28 124.1(4) . . ?
C42 C27 C28 126.0(4) . . ?
C29 C28 C33 118.1(4) . . ?
C29 C28 C27 121.6(4) . . ?
C33 C28 C27 120.3(4) . . ?
C30 C29 C28 121.7(4) . . ?
C29 C30 C31 119.9(4) . . ?
C32 C31 C30 119.7(4) . . ?
C31 C32 C33 121.3(4) . . ?
C32 C33 C28 119.4(4) . . ?
C32 C33 N6 114.9(4) . . ?
C28 C33 N6 125.3(4) . . ?
N7 C34 N6 118.1(4) . . ?
N7 C34 C41 126.7(4) . . ?
N6 C34 C41 115.2(4) . . ?
N7 C35 C36 111.4(3) . . ?
N8 C36 C37 122.0(4) . . ?
N8 C36 C35 117.0(4) . . ?
C37 C36 C35 121.0(4) . . ?
C36 C37 C38 119.3(4) . . ?
C39 C38 C37 118.6(4) . . ?
C40 C39 C38 119.5(4) . . ?
N8 C40 C39 122.0(4) . . ?
C42 C41 C34 107.8(3) . . ?
C27 C42 C43 106.9(4) . . ?
C27 C42 C41 122.2(4) . . ?
C43 C42 C41 130.8(4) . . ?
C44 C43 C26 119.5(4) . . ?
C44 C43 C42 134.0(4) . . ?
C26 C43 C42 106.4(4) . . ?
C23 C44 C43 117.0(4) . . ?
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
C47 C48X 1.321(13) . ?
C47 C48 1.332(12) . ?
C47 O2 1.392(11) . ?
C47 O2X 1.394(11) . ?
O3 C49 1.466(9) . ?
C49 C50 1.466(11) . ?
O4 C51X 1.447(9) . ?
O4 C51 1.476(8) . ?
C51 C52 1.473(10) . ?
C51X C52X 1.439(11) . ?
Ru1 N8 2.045(3) . ?
Ru1 N4 2.091(4) . ?
Ru1 N3 2.109(4) . ?
Ru1 N7 2.116(3) . ?
Ru1 S1 2.2250(11) . ?
Ru1 Cl1 2.4597(10) . ?
Br2 C23 1.912(5) . ?
Br1 C1 1.900(5) . ?
S1 O1 1.482(3) . ?
S1 C45 1.780(5) . ?
S1 C46 1.782(5) . ?
N1 C4 1.371(6) . ?
N1 C5 1.379(6) . ?
N2 C12 1.356(5) . ?
N2 C11 1.410(5) . ?
N3 C12 1.300(5) . ?
N3 C13 1.471(5) . ?
N4 C18 1.348(6) . ?
N4 C14 1.353(6) . ?
N5 C27 1.370(6) . ?
N5 C26 1.376(6) . ?
N6 C34 1.371(5) . ?
N6 C33 1.417(5) . ?
N7 C34 1.300(5) . ?
N7 C35 1.471(5) . ?
N8 C36 1.340(5) . ?
N8 C40 1.352(5) . ?
C1 C22 1.365(7) . ?
C1 C2 1.393(7) . ?
C2 C3 1.387(7) . ?
C3 C4 1.378(6) . ?
C4 C21 1.422(6) . ?
C5 C20 1.366(6) . ?
C5 C6 1.454(6) . ?
C6 C7 1.400(6) . ?
C6 C11 1.415(6) . ?
C7 C8 1.387(6) . ?
C8 C9 1.391(7) . ?
C9 C10 1.379(6) . ?
C10 C11 1.397(6) . ?
C12 C19 1.502(6) . ?
C13 C14 1.502(6) . ?
C14 C15 1.380(6) . ?
C15 C16 1.382(7) . ?
C16 C17 1.384(8) . ?
C17 C18 1.367(7) . ?
C19 C20 1.499(6) . ?
C20 C21 1.435(6) . ?
C21 C22 1.403(6) . ?
C23 C44 1.370(6) . ?
C23 C24 1.405(7) . ?
C24 C25 1.379(7) . ?
C25 C26 1.392(6) . ?
C26 C43 1.413(6) . ?
C27 C42 1.375(6) . ?
C27 C28 1.454(6) . ?
C28 C29 1.403(6) . ?
C28 C33 1.412(6) . ?
C29 C30 1.371(6) . ?
C30 C31 1.396(7) . ?
C31 C32 1.372(6) . ?
C32 C33 1.399(6) . ?
C34 C41 1.501(6) . ?
C35 C36 1.503(6) . ?
C36 C37 1.380(6) . ?
C37 C38 1.387(6) . ?
C38 C39 1.377(7) . ?
C39 C40 1.376(6) . ?
C41 C42 1.496(6) . ?
C42 C43 1.427(6) . ?
C43 C44 1.400(6) . ?
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
C51X O4 C51 C52 110.5(10) . . . . ?
C51 O4 C51X C52X 129.5(12) . . . . ?
N8 Ru1 S1 O1 63.38(18) . . . . ?
N4 Ru1 S1 O1 -30.85(18) . . . . ?
N7 Ru1 S1 O1 142.82(18) . . . . ?
Cl1 Ru1 S1 O1 -115.65(16) . . . . ?
N8 Ru1 S1 C45 -171.7(2) . . . . ?
N4 Ru1 S1 C45 94.1(2) . . . . ?
N7 Ru1 S1 C45 -92.2(2) . . . . ?
Cl1 Ru1 S1 C45 9.3(2) . . . . ?
N8 Ru1 S1 C46 -58.6(2) . . . . ?
N4 Ru1 S1 C46 -152.8(2) . . . . ?
N7 Ru1 S1 C46 20.8(2) . . . . ?
Cl1 Ru1 S1 C46 122.4(2) . . . . ?
N8 Ru1 N3 C12 111.0(4) . . . . ?
N4 Ru1 N3 C12 -153.7(4) . . . . ?
N7 Ru1 N3 C12 31.6(4) . . . . ?
Cl1 Ru1 N3 C12 -69.6(4) . . . . ?
N8 Ru1 N3 C13 -63.3(3) . . . . ?
N4 Ru1 N3 C13 32.0(3) . . . . ?
N7 Ru1 N3 C13 -142.7(3) . . . . ?
Cl1 Ru1 N3 C13 116.1(3) . . . . ?
N8 Ru1 N4 C18 -117.6(4) . . . . ?
N3 Ru1 N4 C18 157.0(4) . . . . ?
N7 Ru1 N4 C18 -175.1(5) . . . . ?
S1 Ru1 N4 C18 -28.9(4) . . . . ?
Cl1 Ru1 N4 C18 66.5(3) . . . . ?
N8 Ru1 N4 C14 72.2(3) . . . . ?
N3 Ru1 N4 C14 -13.3(3) . . . . ?
N7 Ru1 N4 C14 14.6(8) . . . . ?
S1 Ru1 N4 C14 160.9(3) . . . . ?
Cl1 Ru1 N4 C14 -103.7(3) . . . . ?
N8 Ru1 N7 C34 165.7(4) . . . . ?
N4 Ru1 N7 C34 -135.5(6) . . . . ?
N3 Ru1 N7 C34 -108.3(4) . . . . ?
S1 Ru1 N7 C34 77.9(3) . . . . ?
Cl1 Ru1 N7 C34 -18.6(4) . . . . ?
N8 Ru1 N7 C35 -17.7(2) . . . . ?
N4 Ru1 N7 C35 41.1(8) . . . . ?
N3 Ru1 N7 C35 68.3(3) . . . . ?
S1 Ru1 N7 C35 -105.5(2) . . . . ?
Cl1 Ru1 N7 C35 158.0(2) . . . . ?
N4 Ru1 N8 C36 -157.1(3) . . . . ?
N3 Ru1 N8 C36 -79.8(3) . . . . ?
N7 Ru1 N8 C36 13.1(3) . . . . ?
S1 Ru1 N8 C36 105.7(3) . . . . ?
N4 Ru1 N8 C40 20.1(3) . . . . ?
N3 Ru1 N8 C40 97.4(3) . . . . ?
N7 Ru1 N8 C40 -169.7(3) . . . . ?
S1 Ru1 N8 C40 -77.1(3) . . . . ?
C22 C1 C2 C3 -0.4(7) . . . . ?
Br1 C1 C2 C3 177.9(3) . . . . ?
C1 C2 C3 C4 -0.1(7) . . . . ?
C5 N1 C4 C3 177.2(4) . . . . ?
C5 N1 C4 C21 -1.9(4) . . . . ?
C2 C3 C4 N1 -178.9(4) . . . . ?
C2 C3 C4 C21 0.1(6) . . . . ?
C4 N1 C5 C20 3.5(5) . . . . ?
C4 N1 C5 C6 -175.5(4) . . . . ?
C20 C5 C6 C7 148.8(4) . . . . ?
N1 C5 C6 C7 -32.4(6) . . . . ?
C20 C5 C6 C11 -34.1(6) . . . . ?
N1 C5 C6 C11 144.7(4) . . . . ?
C11 C6 C7 C8 1.2(6) . . . . ?
C5 C6 C7 C8 178.4(4) . . . . ?
C6 C7 C8 C9 0.2(6) . . . . ?
C7 C8 C9 C10 -1.2(6) . . . . ?
C8 C9 C10 C11 0.8(7) . . . . ?
C9 C10 C11 N2 -173.1(4) . . . . ?
C9 C10 C11 C6 0.5(6) . . . . ?
C12 N2 C11 C10 -153.6(4) . . . . ?
C12 N2 C11 C6 33.1(6) . . . . ?
C7 C6 C11 C10 -1.5(6) . . . . ?
C5 C6 C11 C10 -178.7(4) . . . . ?
C7 C6 C11 N2 171.7(4) . . . . ?
C5 C6 C11 N2 -5.5(6) . . . . ?
C13 N3 C12 N2 -159.7(4) . . . . ?
Ru1 N3 C12 N2 26.5(6) . . . . ?
C13 N3 C12 C19 25.9(6) . . . . ?
Ru1 N3 C12 C19 -147.8(3) . . . . ?
C11 N2 C12 N3 -157.6(4) . . . . ?
C11 N2 C12 C19 17.2(6) . . . . ?
C12 N3 C13 C14 141.2(4) . . . . ?
Ru1 N3 C13 C14 -43.9(4) . . . . ?
C18 N4 C14 C15 -1.6(6) . . . . ?
Ru1 N4 C14 C15 169.5(3) . . . . ?
C18 N4 C14 C13 -179.5(4) . . . . ?
Ru1 N4 C14 C13 -8.4(5) . . . . ?
N3 C13 C14 N4 34.9(5) . . . . ?
N3 C13 C14 C15 -143.0(4) . . . . ?
N4 C14 C15 C16 0.3(7) . . . . ?
C13 C14 C15 C16 178.1(4) . . . . ?
C14 C15 C16 C17 1.0(7) . . . . ?
C15 C16 C17 C18 -1.1(7) . . . . ?
C14 N4 C18 C17 1.5(6) . . . . ?
Ru1 N4 C18 C17 -168.4(3) . . . . ?
C16 C17 C18 N4 -0.2(7) . . . . ?
N3 C12 C19 C20 98.3(5) . . . . ?
N2 C12 C19 C20 -76.0(4) . . . . ?
N1 C5 C20 C21 -3.6(4) . . . . ?
C6 C5 C20 C21 175.3(4) . . . . ?
N1 C5 C20 C19 -178.8(4) . . . . ?
C6 C5 C20 C19 0.1(6) . . . . ?
C12 C19 C20 C5 66.0(5) . . . . ?
C12 C19 C20 C21 -108.1(5) . . . . ?
N1 C4 C21 C22 179.6(4) . . . . ?
C3 C4 C21 C22 0.4(6) . . . . ?
N1 C4 C21 C20 -0.3(4) . . . . ?
C3 C4 C21 C20 -179.5(4) . . . . ?
C5 C20 C21 C22 -177.5(4) . . . . ?
C19 C20 C21 C22 -2.8(8) . . . . ?
C5 C20 C21 C4 2.4(4) . . . . ?
C19 C20 C21 C4 177.1(4) . . . . ?
C2 C1 C22 C21 0.9(7) . . . . ?
Br1 C1 C22 C21 -177.4(3) . . . . ?
C4 C21 C22 C1 -0.9(6) . . . . ?
C20 C21 C22 C1 179.0(4) . . . . ?
C44 C23 C24 C25 -2.8(7) . . . . ?
Br2 C23 C24 C25 176.0(3) . . . . ?
C23 C24 C25 C26 -0.3(7) . . . . ?
C27 N5 C26 C25 178.6(5) . . . . ?
C27 N5 C26 C43 -0.3(5) . . . . ?
C24 C25 C26 N5 -175.3(4) . . . . ?
C24 C25 C26 C43 3.5(7) . . . . ?
C26 N5 C27 C42 2.4(5) . . . . ?
C26 N5 C27 C28 -174.2(4) . . . . ?
N5 C27 C28 C29 -30.4(7) . . . . ?
C42 C27 C28 C29 153.6(4) . . . . ?
N5 C27 C28 C33 146.7(4) . . . . ?
C42 C27 C28 C33 -29.4(7) . . . . ?
C33 C28 C29 C30 1.0(7) . . . . ?
C27 C28 C29 C30 178.1(4) . . . . ?
C28 C29 C30 C31 -0.2(7) . . . . ?
C29 C30 C31 C32 -0.4(7) . . . . ?
C30 C31 C32 C33 0.2(7) . . . . ?
C31 C32 C33 C28 0.6(6) . . . . ?
C31 C32 C33 N6 -172.0(4) . . . . ?
C29 C28 C33 C32 -1.2(6) . . . . ?
C27 C28 C33 C32 -178.3(4) . . . . ?
C29 C28 C33 N6 170.6(4) . . . . ?
C27 C28 C33 N6 -6.6(6) . . . . ?
C34 N6 C33 C32 -143.7(4) . . . . ?
C34 N6 C33 C28 44.2(6) . . . . ?
C35 N7 C34 N6 -177.4(3) . . . . ?
Ru1 N7 C34 N6 -0.9(5) . . . . ?
C35 N7 C34 C41 4.4(6) . . . . ?
Ru1 N7 C34 C41 -179.2(3) . . . . ?
C33 N6 C34 N7 -179.7(4) . . . . ?
C33 N6 C34 C41 -1.3(6) . . . . ?
C34 N7 C35 C36 -163.2(3) . . . . ?
Ru1 N7 C35 C36 19.6(4) . . . . ?
C40 N8 C36 C37 -2.3(6) . . . . ?
Ru1 N8 C36 C37 175.0(3) . . . . ?
C40 N8 C36 C35 177.0(4) . . . . ?
Ru1 N8 C36 C35 -5.6(4) . . . . ?
N7 C35 C36 N8 -9.8(5) . . . . ?
N7 C35 C36 C37 169.5(4) . . . . ?
N8 C36 C37 C38 0.7(6) . . . . ?
C35 C36 C37 C38 -178.7(4) . . . . ?
C36 C37 C38 C39 1.0(7) . . . . ?
C37 C38 C39 C40 -1.0(7) . . . . ?
C36 N8 C40 C39 2.3(6) . . . . ?
Ru1 N8 C40 C39 -174.8(3) . . . . ?
C38 C39 C40 N8 -0.6(7) . . . . ?
N7 C34 C41 C42 113.0(4) . . . . ?
N6 C34 C41 C42 -65.3(4) . . . . ?
N5 C27 C42 C43 -3.5(5) . . . . ?
C28 C27 C42 C43 173.0(4) . . . . ?
N5 C27 C42 C41 175.2(4) . . . . ?
C28 C27 C42 C41 -8.3(7) . . . . ?
C34 C41 C42 C27 72.1(5) . . . . ?
C34 C41 C42 C43 -109.6(5) . . . . ?
N5 C26 C43 C44 175.4(4) . . . . ?
C25 C26 C43 C44 -3.7(7) . . . . ?
N5 C26 C43 C42 -1.7(5) . . . . ?
C25 C26 C43 C42 179.2(4) . . . . ?
C27 C42 C43 C44 -173.4(5) . . . . ?
C41 C42 C43 C44 8.1(8) . . . . ?
C27 C42 C43 C26 3.2(5) . . . . ?
C41 C42 C43 C26 -175.4(4) . . . . ?
C24 C23 C44 C43 2.6(7) . . . . ?
Br2 C23 C44 C43 -176.2(3) . . . . ?
C26 C43 C44 C23 0.6(6) . . . . ?
C42 C43 C44 C23 176.8(5) . . . . ?
