#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:06:12 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179093 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/55/4305503.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_4305503
loop_
_publ_author_name
'Berta Cebrián-Losantos'
'Erwin Reisner'
'Christian R. Kowol'
'Alexander Roller'
'Sergiu Shova'
'Vladimir B. Arion'
'Bernhard K. Keppler'
_publ_section_title
;
Synthesis and Reactivity of the Aquation Product of the Antitumor
Complex trans-[RuIIICl4(indazole)2]-
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6513
_journal_page_last               6523
_journal_paper_doi               10.1021/ic800506g
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C20 H21 Cl3 N7 Ru'
_chemical_formula_weight         566.86
_chemical_name_systematic
; 
trans,trans-[Dichlorido-bis(1-(1H-indazol-1-yl)ethanimine)ruthenium(III)] 
acetonitrile solvate
;
_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                102.157(6)
_cell_angle_beta                 106.752(7)
_cell_angle_gamma                95.512(6)
_cell_formula_units_Z            2
_cell_length_a                   9.1416(8)
_cell_length_b                   10.5096(7)
_cell_length_c                   13.0426(12)
_cell_measurement_temperature    100(2)
_cell_volume                     1156.41(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0740
_diffrn_reflns_av_sigmaI/netI    0.0669
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            20055
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.43
_exptl_absorpt_coefficient_mu    1.047
_exptl_absorpt_correction_T_max  0.9896
_exptl_absorpt_correction_T_min  0.8179
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    1.628
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             570
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.739
_refine_diff_density_min         -0.544
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         4734
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0370
_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)+(0.0350P)²+0.5580P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0721
_refine_ls_wR_factor_ref         0.0852
_reflns_number_gt                3280
_reflns_number_total             4734
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800506g-file001_4.cif
_cod_data_source_block           BEC244
_cod_original_cell_volume        1156.41(17)
_cod_database_code               4305503
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
Ru1 Ru 0.36499(4) 0.28777(3) 0.69837(3) 0.01546(10) Uani 1 1 d . . .
Cl1 Cl 0.27787(12) 0.16623(9) 0.51257(8) 0.0203(2) Uani 1 1 d . . .
Cl2 Cl 0.44418(13) 0.40902(10) 0.87907(8) 0.0268(3) Uani 1 1 d . . .
N1 N 0.3494(4) 0.0577(3) 0.7858(3) 0.0174(7) Uani 1 1 d . . .
N2 N 0.4507(4) 0.1343(3) 0.7528(3) 0.0178(7) Uani 1 1 d . . .
N3 N 0.1818(4) 0.1920(3) 0.7277(3) 0.0202(8) Uani 1 1 d . . .
H3 H 0.0907 0.2175 0.7111 0.024 Uiso 1 1 calc R . .
N4 N 0.3968(4) 0.5357(3) 0.6374(3) 0.0168(7) Uani 1 1 d . . .
N5 N 0.2862(4) 0.4492(3) 0.6545(3) 0.0166(7) Uani 1 1 d . . .
N6 N 0.5540(4) 0.3859(3) 0.6774(3) 0.0219(8) Uani 1 1 d . . .
H6 H 0.6399 0.3525 0.6840 0.026 Uiso 1 1 calc R . .
C1 C 0.5837(5) 0.0916(4) 0.7752(3) 0.0197(9) Uani 1 1 d . . .
H1 H 0.6727 0.1266 0.7601 0.024 Uiso 1 1 calc R . .
C2 C 0.5744(5) -0.0152(4) 0.8257(3) 0.0208(9) Uani 1 1 d . . .
C3 C 0.6819(5) -0.0950(4) 0.8652(4) 0.0255(10) Uani 1 1 d . . .
H3A H 0.7847 -0.0813 0.8624 0.031 Uiso 1 1 calc R . .
C4 C 0.6322(5) -0.1932(4) 0.9080(4) 0.0282(10) Uani 1 1 d . . .
H4 H 0.7017 -0.2490 0.9349 0.034 Uiso 1 1 calc R . .
C5 C 0.4814(5) -0.2124(4) 0.9125(4) 0.0290(10) Uani 1 1 d . . .
H5 H 0.4511 -0.2815 0.9427 0.035 Uiso 1 1 calc R . .
C6 C 0.3742(5) -0.1347(4) 0.8749(3) 0.0249(10) Uani 1 1 d . . .
H6A H 0.2717 -0.1486 0.8784 0.030 Uiso 1 1 calc R . .
C7 C 0.4248(5) -0.0349(4) 0.8316(3) 0.0178(9) Uani 1 1 d . . .
C8 C 0.2032(5) 0.0935(4) 0.7711(3) 0.0193(9) Uani 1 1 d . . .
C9 C 0.0878(5) 0.0215(4) 0.8066(4) 0.0258(10) Uani 1 1 d . . .
H9A H -0.0069 0.0607 0.7923 0.039 Uiso 1 1 calc R . .
H9B H 0.1299 0.0274 0.8859 0.039 Uiso 1 1 calc R . .
H9C H 0.0636 -0.0713 0.7653 0.039 Uiso 1 1 calc R . .
C10 C 0.1598(4) 0.5011(4) 0.6421(3) 0.0168(8) Uani 1 1 d . . .
H10 H 0.0677 0.4631 0.6518 0.020 Uiso 1 1 calc R . .
C11 C 0.1797(5) 0.6231(4) 0.6117(3) 0.0168(8) Uani 1 1 d . . .
C12 C 0.0814(5) 0.7141(4) 0.5853(3) 0.0213(9) Uani 1 1 d . . .
H12 H -0.0212 0.7032 0.5890 0.026 Uiso 1 1 calc R . .
C13 C 0.1398(5) 0.8202(4) 0.5539(3) 0.0256(10) Uani 1 1 d . . .
H13 H 0.0754 0.8826 0.5339 0.031 Uiso 1 1 calc R . .
C14 C 0.2919(5) 0.8378(4) 0.5508(3) 0.0240(10) Uani 1 1 d . . .
H14 H 0.3277 0.9122 0.5287 0.029 Uiso 1 1 calc R . .
C15 C 0.3922(5) 0.7511(4) 0.5788(3) 0.0205(9) Uani 1 1 d . . .
H15 H 0.4960 0.7647 0.5778 0.025 Uiso 1 1 calc R . .
C16 C 0.3324(5) 0.6428(4) 0.6086(3) 0.0172(8) Uani 1 1 d . . .
C17 C 0.5429(5) 0.4978(4) 0.6542(3) 0.0191(9) Uani 1 1 d . . .
C18 C 0.6734(5) 0.5899(4) 0.6475(4) 0.0243(10) Uani 1 1 d . . .
H18A H 0.7676 0.5500 0.6612 0.036 Uiso 1 1 calc R . .
H18B H 0.6914 0.6735 0.7031 0.036 Uiso 1 1 calc R . .
H18C H 0.6468 0.6064 0.5736 0.036 Uiso 1 1 calc R . .
Cl3 Cl 0.88726(12) 0.31652(10) 0.74307(9) 0.0285(3) Uani 1 1 d . . .
N7 N 0.0013(7) 0.7544(7) 0.9056(7) 0.121(3) Uani 1 1 d . . .
C20 C 0.1523(6) 0.5773(5) 0.9722(5) 0.0503(15) Uani 1 1 d . . .
H20D H 0.0945 0.4901 0.9281 0.075 Uiso 1 1 calc R . .
H20E H 0.1644 0.5843 1.0504 0.075 Uiso 1 1 calc R . .
H20F H 0.2547 0.5891 0.9625 0.075 Uiso 1 1 calc R . .
C19 C 0.0688(7) 0.6781(7) 0.9363(6) 0.0635(19) Uani 1 1 d . . .
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
N2 Ru1 N5 176.10(14) . . ?
N2 Ru1 N6 101.86(13) . . ?
N5 Ru1 N6 77.46(13) . . ?
N2 Ru1 N3 76.98(13) . . ?
N5 Ru1 N3 103.52(13) . . ?
N6 Ru1 N3 177.12(14) . . ?
N2 Ru1 Cl2 88.40(10) . . ?
N5 Ru1 Cl2 87.75(9) . . ?
N6 Ru1 Cl2 89.00(10) . . ?
N3 Ru1 Cl2 88.33(10) . . ?
N2 Ru1 Cl1 92.80(10) . . ?
N5 Ru1 Cl1 91.07(9) . . ?
N6 Ru1 Cl1 91.70(10) . . ?
N3 Ru1 Cl1 90.99(10) . . ?
Cl2 Ru1 Cl1 178.46(5) . . ?
C7 N1 N2 109.3(3) . . ?
C7 N1 C8 135.2(3) . . ?
N2 N1 C8 115.4(3) . . ?
C1 N2 N1 108.2(3) . . ?
C1 N2 Ru1 137.3(3) . . ?
N1 N2 Ru1 114.2(2) . . ?
C8 N3 Ru1 118.1(3) . . ?
C16 N4 N5 109.6(3) . . ?
C16 N4 C17 135.4(3) . . ?
N5 N4 C17 115.0(3) . . ?
C10 N5 N4 107.9(3) . . ?
C10 N5 Ru1 138.1(3) . . ?
N4 N5 Ru1 114.0(2) . . ?
C17 N6 Ru1 117.6(3) . . ?
N2 C1 C2 109.7(3) . . ?
C7 C2 C3 120.9(4) . . ?
C7 C2 C1 106.3(3) . . ?
C3 C2 C1 132.8(4) . . ?
C4 C3 C2 117.4(4) . . ?
C3 C4 C5 121.2(4) . . ?
C6 C5 C4 122.5(4) . . ?
C5 C6 C7 116.4(4) . . ?
N1 C7 C2 106.6(3) . . ?
N1 C7 C6 131.7(4) . . ?
C2 C7 C6 121.8(4) . . ?
N3 C8 N1 115.0(3) . . ?
N3 C8 C9 124.9(4) . . ?
N1 C8 C9 120.1(3) . . ?
N5 C10 C11 110.4(3) . . ?
C12 C11 C16 120.6(3) . . ?
C12 C11 C10 133.6(4) . . ?
C16 C11 C10 105.8(3) . . ?
C13 C12 C11 117.2(4) . . ?
C12 C13 C14 121.4(4) . . ?
C15 C14 C13 122.5(4) . . ?
C14 C15 C16 116.1(4) . . ?
N4 C16 C15 131.6(4) . . ?
N4 C16 C11 106.2(3) . . ?
C15 C16 C11 122.2(3) . . ?
N6 C17 N4 115.9(4) . . ?
N6 C17 C18 125.1(4) . . ?
N4 C17 C18 119.0(3) . . ?
N7 C19 C20 178.1(9) . . ?
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 N2 2.031(3) . ?
Ru1 N5 2.032(3) . ?
Ru1 N6 2.043(3) . ?
Ru1 N3 2.043(3) . ?
Ru1 Cl2 2.2971(11) . ?
Ru1 Cl1 2.3509(11) . ?
N1 C7 1.383(5) . ?
N1 N2 1.387(4) . ?
N1 C8 1.395(5) . ?
N2 C1 1.311(5) . ?
N3 C8 1.285(5) . ?
N4 C16 1.390(4) . ?
N4 N5 1.393(4) . ?
N4 C17 1.400(5) . ?
N5 C10 1.307(5) . ?
N6 C17 1.281(5) . ?
C1 C2 1.424(5) . ?
C2 C7 1.390(6) . ?
C2 C3 1.408(5) . ?
C3 C4 1.371(6) . ?
C4 C5 1.394(6) . ?
C5 C6 1.384(6) . ?
C6 C7 1.393(5) . ?
C8 C9 1.475(5) . ?
C10 C11 1.430(5) . ?
C11 C12 1.402(5) . ?
C11 C16 1.405(5) . ?
C12 C13 1.379(5) . ?
C13 C14 1.398(6) . ?
C14 C15 1.383(5) . ?
C15 C16 1.392(5) . ?
C17 C18 1.498(5) . ?
N7 C19 1.128(7) . ?
C20 C19 1.443(7) . ?
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
C7 N1 N2 C1 0.7(4) . . . . ?
C8 N1 N2 C1 177.9(3) . . . . ?
C7 N1 N2 Ru1 -173.9(2) . . . . ?
C8 N1 N2 Ru1 3.2(4) . . . . ?
N6 Ru1 N2 C1 0.8(4) . . . . ?
N3 Ru1 N2 C1 -176.5(4) . . . . ?
Cl2 Ru1 N2 C1 -87.9(4) . . . . ?
Cl1 Ru1 N2 C1 93.1(4) . . . . ?
N6 Ru1 N2 N1 173.2(2) . . . . ?
N3 Ru1 N2 N1 -4.1(2) . . . . ?
Cl2 Ru1 N2 N1 84.6(2) . . . . ?
Cl1 Ru1 N2 N1 -94.5(2) . . . . ?
N2 Ru1 N3 C8 4.8(3) . . . . ?
N5 Ru1 N3 C8 -171.2(3) . . . . ?
Cl2 Ru1 N3 C8 -83.9(3) . . . . ?
Cl1 Ru1 N3 C8 97.4(3) . . . . ?
C16 N4 N5 C10 -2.6(4) . . . . ?
C17 N4 N5 C10 176.4(3) . . . . ?
C16 N4 N5 Ru1 -179.6(2) . . . . ?
C17 N4 N5 Ru1 -0.7(4) . . . . ?
N6 Ru1 N5 C10 -177.1(4) . . . . ?
N3 Ru1 N5 C10 0.1(4) . . . . ?
Cl2 Ru1 N5 C10 -87.6(4) . . . . ?
Cl1 Ru1 N5 C10 91.4(4) . . . . ?
N6 Ru1 N5 N4 -1.3(2) . . . . ?
N3 Ru1 N5 N4 175.9(2) . . . . ?
Cl2 Ru1 N5 N4 88.2(2) . . . . ?
Cl1 Ru1 N5 N4 -92.8(2) . . . . ?
N2 Ru1 N6 C17 -172.6(3) . . . . ?
N5 Ru1 N6 C17 3.4(3) . . . . ?
Cl2 Ru1 N6 C17 -84.5(3) . . . . ?
Cl1 Ru1 N6 C17 94.1(3) . . . . ?
N1 N2 C1 C2 -0.7(4) . . . . ?
Ru1 N2 C1 C2 172.1(3) . . . . ?
N2 C1 C2 C7 0.4(5) . . . . ?
N2 C1 C2 C3 180.0(4) . . . . ?
C7 C2 C3 C4 0.9(6) . . . . ?
C1 C2 C3 C4 -178.6(4) . . . . ?
C2 C3 C4 C5 -0.4(7) . . . . ?
C3 C4 C5 C6 -0.1(7) . . . . ?
C4 C5 C6 C7 0.0(7) . . . . ?
N2 N1 C7 C2 -0.5(4) . . . . ?
C8 N1 C7 C2 -176.8(4) . . . . ?
N2 N1 C7 C6 -178.9(4) . . . . ?
C8 N1 C7 C6 4.8(8) . . . . ?
C3 C2 C7 N1 -179.6(4) . . . . ?
C1 C2 C7 N1 0.1(4) . . . . ?
C3 C2 C7 C6 -1.0(6) . . . . ?
C1 C2 C7 C6 178.6(4) . . . . ?
C5 C6 C7 N1 178.7(4) . . . . ?
C5 C6 C7 C2 0.5(6) . . . . ?
Ru1 N3 C8 N1 -4.5(5) . . . . ?
Ru1 N3 C8 C9 174.2(3) . . . . ?
C7 N1 C8 N3 176.9(4) . . . . ?
N2 N1 C8 N3 0.7(5) . . . . ?
C7 N1 C8 C9 -1.9(7) . . . . ?
N2 N1 C8 C9 -178.0(3) . . . . ?
N4 N5 C10 C11 2.2(4) . . . . ?
Ru1 N5 C10 C11 178.2(3) . . . . ?
N5 C10 C11 C12 177.5(4) . . . . ?
N5 C10 C11 C16 -1.0(4) . . . . ?
C16 C11 C12 C13 1.6(6) . . . . ?
C10 C11 C12 C13 -176.7(4) . . . . ?
C11 C12 C13 C14 -1.4(6) . . . . ?
C12 C13 C14 C15 0.0(7) . . . . ?
C13 C14 C15 C16 1.2(6) . . . . ?
N5 N4 C16 C15 -176.8(4) . . . . ?
C17 N4 C16 C15 4.6(8) . . . . ?
N5 N4 C16 C11 1.9(4) . . . . ?
C17 N4 C16 C11 -176.8(4) . . . . ?
C14 C15 C16 N4 177.6(4) . . . . ?
C14 C15 C16 C11 -0.9(6) . . . . ?
C12 C11 C16 N4 -179.3(4) . . . . ?
C10 C11 C16 N4 -0.6(4) . . . . ?
C12 C11 C16 C15 -0.5(6) . . . . ?
C10 C11 C16 C15 178.2(4) . . . . ?
Ru1 N6 C17 N4 -4.8(5) . . . . ?
Ru1 N6 C17 C18 173.4(3) . . . . ?
C16 N4 C17 N6 -177.8(4) . . . . ?
N5 N4 C17 N6 3.6(5) . . . . ?
C16 N4 C17 C18 3.9(7) . . . . ?
N5 N4 C17 C18 -174.8(3) . . . . ?
