#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:53:07 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179133 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/95/4309569.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_4309569
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            'C12 H16 Cl3 N8 Ru'
_chemical_formula_weight         479.75
_chemical_name_systematic
; 
mer-trichlorotripyrazoloruthenium(III) 
;
_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                102.90(3)
_cell_angle_beta                 90.93(3)
_cell_angle_gamma                110.60(3)
_cell_formula_units_Z            2
_cell_length_a                   7.9169(16)
_cell_length_b                   8.4136(17)
_cell_length_c                   14.658(3)
_cell_measurement_temperature    120(2)
_cell_volume                     886.0(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0215
_diffrn_reflns_av_sigmaI/netI    0.0401
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10076
_diffrn_reflns_theta_full        30.47
_diffrn_reflns_theta_max         30.47
_diffrn_reflns_theta_min         3.41
_exptl_absorpt_coefficient_mu    1.350
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.798
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             478
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.983
_refine_diff_density_min         -0.638
_refine_diff_density_rms         0.091
_refine_ls_extinction_coef       0.0038(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         5363
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0257
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0189P)²+0.2804P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0527
_refine_ls_wR_factor_ref         0.0559
_reflns_number_gt                4452
_reflns_number_total             5363
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0503737si20050311_101709_5.cif
_cod_data_source_block           AT8813
_cod_original_cell_volume        886.0(3)
_cod_database_code               4309569
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 0.5000 0.5000 0.5000 0.01086(5) Uani 1 2 d S . .
Cl1 Cl 0.18360(5) 0.33534(5) 0.48559(3) 0.01598(9) Uani 1 1 d . . .
Cl3 Cl 1.02208(6) 0.90759(6) 0.29755(3) 0.02299(10) Uani 1 1 d . . .
N1 N 0.48387(19) 0.51300(19) 0.36190(10) 0.0145(3) Uani 1 1 d . . .
N2 N 0.6126(2) 0.6320(2) 0.32655(11) 0.0160(3) Uani 1 1 d . . .
N6 N 0.54537(19) 0.26970(18) 0.45714(10) 0.0142(3) Uani 1 1 d . . .
N7 N 0.4220(2) 0.11818(19) 0.40471(10) 0.0166(3) Uani 1 1 d . . .
C3 C 0.5677(3) 0.6136(3) 0.23536(13) 0.0218(4) Uani 1 1 d . . .
C4 C 0.4041(3) 0.4784(3) 0.20923(14) 0.0245(4) Uani 1 1 d . . .
C5 C 0.3564(3) 0.4183(3) 0.28990(13) 0.0210(4) Uani 1 1 d . . .
C8 C 0.4963(3) -0.0037(2) 0.37989(13) 0.0205(4) Uani 1 1 d . . .
C9 C 0.6757(3) 0.0700(2) 0.41630(13) 0.0210(4) Uani 1 1 d . . .
C10 C 0.7006(3) 0.2398(2) 0.46441(13) 0.0182(4) Uani 1 1 d . . .
Ru2 Ru 1.0000 0.5000 0.0000 0.01244(6) Uani 1 2 d S . .
Cl2 Cl 0.83633(6) 0.68596(6) 0.04474(3) 0.01744(9) Uani 1 1 d . . .
N11 N 0.96020(19) 0.41945(19) 0.12353(10) 0.0149(3) Uani 1 1 d . . .
N12 N 0.9496(2) 0.5163(2) 0.20864(10) 0.0181(3) Uani 1 1 d . . .
N16 N 1.23723(19) 0.70714(19) 0.05778(10) 0.0154(3) Uani 1 1 d . . .
N17 N 1.2501(2) 0.8526(2) 0.12398(11) 0.0221(3) Uani 1 1 d . . .
C13 C 0.9134(3) 0.4200(3) 0.27243(13) 0.0214(4) Uani 1 1 d . . .
C14 C 0.8998(3) 0.2532(3) 0.22802(14) 0.0212(4) Uani 1 1 d . . .
C15 C 0.9313(2) 0.2588(2) 0.13586(13) 0.0187(4) Uani 1 1 d . . .
C18 C 1.4232(3) 0.9660(2) 0.14237(14) 0.0235(4) Uani 1 1 d . . .
H18 H 1.4655 1.0742 0.1857 0.028 Uiso 1 1 calc R . .
C19 C 1.5254(3) 0.8925(3) 0.08544(15) 0.0250(4) Uani 1 1 d . . .
C20 C 1.4052(3) 0.7327(3) 0.03423(14) 0.0206(4) Uani 1 1 d . . .
H2 H 0.710(3) 0.694(3) 0.3583(15) 0.023(6) Uiso 1 1 d . . .
H3 H 0.648(3) 0.682(3) 0.2003(15) 0.028(6) Uiso 1 1 d . . .
H4 H 0.337(3) 0.437(3) 0.1520(17) 0.042(7) Uiso 1 1 d . . .
H5 H 0.253(3) 0.329(3) 0.2980(14) 0.023(5) Uiso 1 1 d . . .
H7 H 0.312(3) 0.107(3) 0.3934(16) 0.030(6) Uiso 1 1 d . . .
H8 H 0.427(3) -0.117(3) 0.3432(14) 0.022(5) Uiso 1 1 d . . .
H9 H 0.763(3) 0.020(3) 0.4093(15) 0.032(6) Uiso 1 1 d . . .
H10 H 0.799(3) 0.326(2) 0.4957(13) 0.014(5) Uiso 1 1 d . . .
H12 H 0.966(3) 0.623(3) 0.2164(15) 0.030(6) Uiso 1 1 d . . .
H13 H 0.902(3) 0.472(3) 0.3364(15) 0.026(6) Uiso 1 1 d . . .
H14 H 0.880(3) 0.162(3) 0.2569(14) 0.024(5) Uiso 1 1 d . . .
H15 H 0.937(3) 0.171(2) 0.0820(14) 0.017(5) Uiso 1 1 d . . .
H17 H 1.157(3) 0.869(3) 0.1562(16) 0.039(7) Uiso 1 1 d . . .
H19 H 1.649(3) 0.939(3) 0.0853(17) 0.040(7) Uiso 1 1 d . . .
H20 H 1.423(3) 0.647(3) -0.0121(14) 0.022(5) Uiso 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
N1 Ru1 N1 180.000(1) 2_666 . ?
N1 Ru1 N6 89.14(6) 2_666 2_666 ?
N1 Ru1 N6 90.86(6) . 2_666 ?
N1 Ru1 N6 90.86(6) 2_666 . ?
N1 Ru1 N6 89.14(6) . . ?
N6 Ru1 N6 180.0 2_666 . ?
N1 Ru1 Cl1 90.86(5) 2_666 2_666 ?
N1 Ru1 Cl1 89.14(5) . 2_666 ?
N6 Ru1 Cl1 89.13(5) 2_666 2_666 ?
N6 Ru1 Cl1 90.87(5) . 2_666 ?
N1 Ru1 Cl1 89.14(5) 2_666 . ?
N1 Ru1 Cl1 90.86(5) . . ?
N6 Ru1 Cl1 90.87(5) 2_666 . ?
N6 Ru1 Cl1 89.13(5) . . ?
Cl1 Ru1 Cl1 180.0 2_666 . ?
C5 N1 N2 105.51(15) . . ?
C5 N1 Ru1 131.18(13) . . ?
N2 N1 Ru1 123.31(12) . . ?
C3 N2 N1 111.19(16) . . ?
C3 N2 H2 127.9(15) . . ?
N1 N2 H2 120.3(15) . . ?
C10 N6 N7 105.68(14) . . ?
C10 N6 Ru1 129.34(13) . . ?
N7 N6 Ru1 124.60(11) . . ?
C8 N7 N6 110.89(16) . . ?
C8 N7 H7 127.8(15) . . ?
N6 N7 H7 121.2(15) . . ?
N2 C3 C4 107.58(17) . . ?
N2 C3 H3 120.8(13) . . ?
C4 C3 H3 131.5(13) . . ?
C3 C4 C5 105.49(18) . . ?
C3 C4 H4 128.2(15) . . ?
C5 C4 H4 126.3(15) . . ?
N1 C5 C4 110.23(17) . . ?
N1 C5 H5 120.8(13) . . ?
C4 C5 H5 128.9(13) . . ?
N7 C8 C9 107.88(17) . . ?
N7 C8 H8 121.3(12) . . ?
C9 C8 H8 130.9(12) . . ?
C8 C9 C10 105.13(17) . . ?
C8 C9 H9 128.3(14) . . ?
C10 C9 H9 126.6(14) . . ?
N6 C10 C9 110.42(17) . . ?
N6 C10 H10 119.0(12) . . ?
C9 C10 H10 130.5(12) . . ?
N11 Ru2 N11 180.00(8) . 2_765 ?
N11 Ru2 N16 86.97(6) . 2_765 ?
N11 Ru2 N16 93.03(6) 2_765 2_765 ?
N11 Ru2 N16 93.03(6) . . ?
N11 Ru2 N16 86.97(6) 2_765 . ?
N16 Ru2 N16 180.00(8) 2_765 . ?
N11 Ru2 Cl2 91.09(5) . . ?
N11 Ru2 Cl2 88.91(5) 2_765 . ?
N16 Ru2 Cl2 90.66(5) 2_765 . ?
N16 Ru2 Cl2 89.34(5) . . ?
N11 Ru2 Cl2 88.91(5) . 2_765 ?
N11 Ru2 Cl2 91.09(5) 2_765 2_765 ?
N16 Ru2 Cl2 89.34(5) 2_765 2_765 ?
N16 Ru2 Cl2 90.66(5) . 2_765 ?
Cl2 Ru2 Cl2 180.0 . 2_765 ?
C15 N11 N12 105.42(14) . . ?
C15 N11 Ru2 127.65(12) . . ?
N12 N11 Ru2 126.87(11) . . ?
C13 N12 N11 111.09(15) . . ?
C13 N12 H12 128.3(15) . . ?
N11 N12 H12 120.6(15) . . ?
C20 N16 N17 105.73(15) . . ?
C20 N16 Ru2 128.29(13) . . ?
N17 N16 Ru2 125.82(12) . . ?
C18 N17 N16 110.63(16) . . ?
C18 N17 H17 123.9(15) . . ?
N16 N17 H17 125.3(15) . . ?
N12 C13 C14 107.72(17) . . ?
N12 C13 H13 120.4(12) . . ?
C14 C13 H13 131.9(12) . . ?
C13 C14 C15 105.08(17) . . ?
C13 C14 H14 125.1(13) . . ?
C15 C14 H14 129.7(13) . . ?
N11 C15 C14 110.68(17) . . ?
N11 C15 H15 117.4(11) . . ?
C14 C15 H15 131.9(11) . . ?
N17 C18 C19 107.39(17) . . ?
N17 C18 H18 126.3 . . ?
C19 C18 H18 126.3 . . ?
C18 C19 C20 105.51(18) . . ?
C18 C19 H19 126.1(15) . . ?
C20 C19 H19 128.3(15) . . ?
N16 C20 C19 110.73(17) . . ?
N16 C20 H20 118.2(13) . . ?
C19 C20 H20 131.1(13) . . ?
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 2.0557(15) 2_666 ?
Ru1 N1 2.0557(15) . ?
Ru1 N6 2.0571(15) 2_666 ?
Ru1 N6 2.0571(15) . ?
Ru1 Cl1 2.3767(9) 2_666 ?
Ru1 Cl1 2.3767(9) . ?
N1 C5 1.338(2) . ?
N1 N2 1.357(2) . ?
N2 C3 1.338(2) . ?
N2 H2 0.82(2) . ?
N6 C10 1.346(2) . ?
N6 N7 1.353(2) . ?
N7 C8 1.339(2) . ?
N7 H7 0.85(2) . ?
C3 C4 1.368(3) . ?
C3 H3 0.94(2) . ?
C4 C5 1.394(3) . ?
C4 H4 0.91(2) . ?
C5 H5 0.93(2) . ?
C8 C9 1.377(3) . ?
C8 H8 0.95(2) . ?
C9 C10 1.388(3) . ?
C9 H9 0.92(2) . ?
C10 H10 0.89(2) . ?
Ru2 N11 2.0624(15) . ?
Ru2 N11 2.0624(15) 2_765 ?
Ru2 N16 2.0659(18) 2_765 ?
Ru2 N16 2.0659(18) . ?
Ru2 Cl2 2.3565(7) . ?
Ru2 Cl2 2.3565(7) 2_765 ?
N11 C15 1.343(2) . ?
N11 N12 1.351(2) . ?
N12 C13 1.340(2) . ?
N12 H12 0.84(2) . ?
N16 C20 1.334(2) . ?
N16 N17 1.352(2) . ?
N17 C18 1.346(2) . ?
N17 H17 0.92(2) . ?
C13 C14 1.374(3) . ?
C13 H13 0.96(2) . ?
C14 C15 1.386(3) . ?
C14 H14 0.92(2) . ?
C15 H15 0.969(19) . ?
C18 C19 1.370(3) . ?
C18 H18 0.9300 . ?
C19 C20 1.379(3) . ?
C19 H19 0.92(2) . ?
C20 H20 0.92(2) . ?
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
N1 Ru1 N1 C5 101(100) 2_666 . . . ?
N6 Ru1 N1 C5 -108.50(16) 2_666 . . . ?
N6 Ru1 N1 C5 71.50(16) . . . . ?
Cl1 Ru1 N1 C5 162.39(16) 2_666 . . . ?
Cl1 Ru1 N1 C5 -17.61(16) . . . . ?
N1 Ru1 N1 N2 -80(100) 2_666 . . . ?
N6 Ru1 N1 N2 70.63(13) 2_666 . . . ?
N6 Ru1 N1 N2 -109.37(13) . . . . ?
Cl1 Ru1 N1 N2 -18.49(12) 2_666 . . . ?
Cl1 Ru1 N1 N2 161.51(12) . . . . ?
C5 N1 N2 C3 0.19(19) . . . . ?
Ru1 N1 N2 C3 -179.12(12) . . . . ?
N1 Ru1 N6 C10 -74.80(16) 2_666 . . . ?
N1 Ru1 N6 C10 105.20(16) . . . . ?
N6 Ru1 N6 C10 -78(100) 2_666 . . . ?
Cl1 Ru1 N6 C10 16.08(15) 2_666 . . . ?
Cl1 Ru1 N6 C10 -163.92(15) . . . . ?
N1 Ru1 N6 N7 113.32(13) 2_666 . . . ?
N1 Ru1 N6 N7 -66.68(13) . . . . ?
N6 Ru1 N6 N7 110(100) 2_666 . . . ?
Cl1 Ru1 N6 N7 -155.80(13) 2_666 . . . ?
Cl1 Ru1 N6 N7 24.20(13) . . . . ?
C10 N6 N7 C8 0.20(19) . . . . ?
Ru1 N6 N7 C8 173.68(12) . . . . ?
N1 N2 C3 C4 0.1(2) . . . . ?
N2 C3 C4 C5 -0.4(2) . . . . ?
N2 N1 C5 C4 -0.4(2) . . . . ?
Ru1 N1 C5 C4 178.82(13) . . . . ?
C3 C4 C5 N1 0.5(2) . . . . ?
N6 N7 C8 C9 -0.6(2) . . . . ?
N7 C8 C9 C10 0.7(2) . . . . ?
N7 N6 C10 C9 0.3(2) . . . . ?
Ru1 N6 C10 C9 -172.78(12) . . . . ?
C8 C9 C10 N6 -0.6(2) . . . . ?
N11 Ru2 N11 C15 -166(100) 2_765 . . . ?
N16 Ru2 N11 C15 52.81(15) 2_765 . . . ?
N16 Ru2 N11 C15 -127.19(15) . . . . ?
Cl2 Ru2 N11 C15 143.41(15) . . . . ?
Cl2 Ru2 N11 C15 -36.59(15) 2_765 . . . ?
N11 Ru2 N11 N12 17(100) 2_765 . . . ?
N16 Ru2 N11 N12 -123.94(14) 2_765 . . . ?
N16 Ru2 N11 N12 56.06(14) . . . . ?
Cl2 Ru2 N11 N12 -33.33(14) . . . . ?
Cl2 Ru2 N11 N12 146.67(14) 2_765 . . . ?
C15 N11 N12 C13 -0.6(2) . . . . ?
Ru2 N11 N12 C13 176.69(12) . . . . ?
N11 Ru2 N16 C20 115.80(16) . . . . ?
N11 Ru2 N16 C20 -64.20(16) 2_765 . . . ?
N16 Ru2 N16 C20 116(100) 2_765 . . . ?
Cl2 Ru2 N16 C20 -153.15(15) . . . . ?
Cl2 Ru2 N16 C20 26.85(15) 2_765 . . . ?
N11 Ru2 N16 N17 -69.38(14) . . . . ?
N11 Ru2 N16 N17 110.62(14) 2_765 . . . ?
N16 Ru2 N16 N17 -69(100) 2_765 . . . ?
Cl2 Ru2 N16 N17 21.67(14) . . . . ?
Cl2 Ru2 N16 N17 -158.33(14) 2_765 . . . ?
C20 N16 N17 C18 -0.8(2) . . . . ?
Ru2 N16 N17 C18 -176.59(12) . . . . ?
N11 N12 C13 C14 0.1(2) . . . . ?
N12 C13 C14 C15 0.4(2) . . . . ?
N12 N11 C15 C14 0.9(2) . . . . ?
Ru2 N11 C15 C14 -176.40(12) . . . . ?
C13 C14 C15 N11 -0.8(2) . . . . ?
N16 N17 C18 C19 0.7(2) . . . . ?
N17 C18 C19 C20 -0.4(2) . . . . ?
N17 N16 C20 C19 0.6(2) . . . . ?
Ru2 N16 C20 C19 176.21(13) . . . . ?
C18 C19 C20 N16 -0.1(2) . . . . ?
