#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:06:12 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179093 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/55/4305504.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_4305504
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            'C16 H20 Cl3 N4 O2 Ru'
_chemical_formula_weight         507.78
_chemical_name_systematic
; 
mer,trans-[Trichloridobis(indazole)methanolruthenium(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                 99.626(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.1718(3)
_cell_length_b                   12.0086(5)
_cell_length_c                   21.2128(8)
_cell_measurement_temperature    296(2)
_cell_volume                     2052.34(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(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  0.0788
_diffrn_reflns_av_sigmaI/netI    0.0373
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            36740
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.53
_exptl_absorpt_coefficient_mu    1.172
_exptl_absorpt_correction_T_max  0.8721
_exptl_absorpt_correction_T_min  0.7503
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1020
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.515
_refine_diff_density_min         -0.497
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         3612
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0371
_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)+(0.0425P)²+1.5629P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0846
_refine_ls_wR_factor_ref         0.0970
_reflns_number_gt                2573
_reflns_number_total             3612
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800506g-file001_5.cif
_cod_data_source_block           BECE310
_cod_database_code               4305504
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 0.77713(4) 0.30956(3) 0.042410(16) 0.04888(14) Uani 1 1 d . . .
Cl1 Cl 0.73405(14) 0.49374(9) 0.00540(5) 0.0524(3) Uani 1 1 d . . .
Cl2 Cl 1.03194(14) 0.35767(11) 0.10127(5) 0.0595(3) Uani 1 1 d . . .
Cl3 Cl 0.80038(19) 0.12527(11) 0.07622(7) 0.0788(4) Uani 1 1 d . . .
N1 N 0.8907(4) 0.2732(3) -0.03618(17) 0.0530(9) Uani 1 1 d . . .
N3 N 0.6675(4) 0.3513(3) 0.11945(16) 0.0521(9) Uani 1 1 d . . .
N4 N 0.5434(5) 0.4264(3) 0.11494(16) 0.0595(10) Uani 1 1 d . . .
H4 H 0.4955 0.4561 0.0798 0.071 Uiso 1 1 calc R . .
C7 C 1.0079(6) 0.3142(4) -0.1211(2) 0.0585(12) Uani 1 1 d . . .
C2 C 0.9954(6) 0.1996(4) -0.1178(2) 0.0603(13) Uani 1 1 d . . .
C1 C 0.9224(6) 0.1789(4) -0.0634(2) 0.0634(13) Uani 1 1 d . . .
H1 H 0.8997 0.1086 -0.0487 0.076 Uiso 1 1 calc R . .
N2 N 0.9427(5) 0.3556(3) -0.07135(18) 0.0604(10) Uani 1 1 d . . .
H2 H 0.9354 0.4254 -0.0632 0.072 Uiso 1 1 calc R . .
C5 C 1.1215(8) 0.3030(6) -0.2150(3) 0.090(2) Uani 1 1 d . . .
H5 H 1.1630 0.3360 -0.2487 0.108 Uiso 1 1 calc R . .
C14 C 0.5042(6) 0.4487(4) 0.1728(2) 0.0535(11) Uani 1 1 d . . .
C9 C 0.6065(5) 0.3841(4) 0.2164(2) 0.0592(13) Uani 1 1 d . . .
C8 C 0.7060(6) 0.3250(4) 0.1804(2) 0.0615(13) Uani 1 1 d . . .
H8 H 0.7878 0.2742 0.1971 0.074 Uiso 1 1 calc R . .
C4 C 1.1109(8) 0.1881(6) -0.2128(3) 0.090(2) Uani 1 1 d . . .
H4A H 1.1466 0.1464 -0.2449 0.108 Uiso 1 1 calc R . .
C13 C 0.3873(7) 0.5215(5) 0.1908(2) 0.0717(14) Uani 1 1 d . . .
H13 H 0.3180 0.5637 0.1607 0.086 Uiso 1 1 calc R . .
C12 C 0.3789(7) 0.5283(5) 0.2542(3) 0.0802(16) Uani 1 1 d . . .
H12 H 0.3045 0.5775 0.2681 0.096 Uiso 1 1 calc R . .
C11 C 0.4805(8) 0.4625(6) 0.2984(3) 0.0873(19) Uani 1 1 d . . .
H11 H 0.4700 0.4677 0.3413 0.105 Uiso 1 1 calc R . .
C10 C 0.5930(7) 0.3919(6) 0.2817(2) 0.088(2) Uani 1 1 d . . .
H10 H 0.6602 0.3492 0.3123 0.106 Uiso 1 1 calc R . .
C3 C 1.0506(7) 0.1348(5) -0.1657(3) 0.0831(17) Uani 1 1 d . . .
H3 H 1.0455 0.0575 -0.1647 0.100 Uiso 1 1 calc R . .
C6 C 1.0730(7) 0.3696(5) -0.1694(2) 0.0793(16) Uani 1 1 d . . .
H6 H 1.0827 0.4467 -0.1703 0.095 Uiso 1 1 calc R . .
O1 O 0.5443(4) 0.2739(3) -0.00676(16) 0.0665(10) Uani 1 1 d . . .
H1A H 0.470(6) 0.261(4) 0.015(2) 0.071(17) Uiso 1 1 d . . .
C15 C 0.4941(7) 0.2493(7) -0.0704(3) 0.110(2) Uani 1 1 d . . .
H15A H 0.5666 0.2852 -0.0953 0.165 Uiso 1 1 calc R . .
H15B H 0.3826 0.2752 -0.0838 0.165 Uiso 1 1 calc R . .
H15C H 0.4981 0.1702 -0.0765 0.165 Uiso 1 1 calc R . .
O2 O 0.2949(7) 0.2246(4) 0.0418(3) 0.0735(18) Uiso 0.762(13) 1 d PD A 1
H20 H 0.2648 0.2928 0.0536 0.088 Uiso 0.762(13) 1 d PRD A 1
C16 C 0.2910(13) 0.1222(8) 0.0799(6) 0.127(4) Uiso 0.762(13) 1 d PD A 1
H16A H 0.3428 0.1361 0.1232 0.190 Uiso 0.762(13) 1 calc PR A 1
H16B H 0.3498 0.0640 0.0621 0.190 Uiso 0.762(13) 1 calc PR A 1
H16C H 0.1780 0.0998 0.0792 0.190 Uiso 0.762(13) 1 calc PR A 1
O2X O 0.333(2) 0.2098(14) 0.0712(10) 0.076(6) Uiso 0.238(13) 1 d PD A 2
H20X H 0.3297 0.1897 0.1128 0.092 Uiso 0.238(13) 1 d PRD A 2
C16X C 0.267(3) 0.1043(15) 0.0369(10) 0.073(8) Uiso 0.238(13) 1 d PD A 2
H16D H 0.2068 0.1228 -0.0046 0.110 Uiso 0.238(13) 1 calc PR A 2
H16E H 0.1934 0.0675 0.0612 0.110 Uiso 0.238(13) 1 calc PR A 2
H16F H 0.3572 0.0557 0.0325 0.110 Uiso 0.238(13) 1 calc PR A 2
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'
O O 0.0106 0.0060 '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
N3 Ru1 O1 87.99(14) . . ?
N3 Ru1 N1 177.93(15) . . ?
O1 Ru1 N1 92.78(14) . . ?
N3 Ru1 Cl2 88.99(10) . . ?
O1 Ru1 Cl2 176.53(11) . . ?
N1 Ru1 Cl2 90.18(10) . . ?
N3 Ru1 Cl3 90.63(11) . . ?
O1 Ru1 Cl3 88.80(12) . . ?
N1 Ru1 Cl3 91.31(11) . . ?
Cl2 Ru1 Cl3 92.95(5) . . ?
N3 Ru1 Cl1 88.58(11) . . ?
O1 Ru1 Cl1 87.28(11) . . ?
N1 Ru1 Cl1 89.54(11) . . ?
Cl2 Ru1 Cl1 90.93(4) . . ?
Cl3 Ru1 Cl1 176.02(5) . . ?
C1 N1 N2 106.6(4) . . ?
C1 N1 Ru1 132.7(3) . . ?
N2 N1 Ru1 120.7(3) . . ?
C8 N3 N4 106.5(4) . . ?
C8 N3 Ru1 131.2(3) . . ?
N4 N3 Ru1 122.0(3) . . ?
C14 N4 N3 111.0(3) . . ?
N2 C7 C2 106.5(4) . . ?
N2 C7 C6 130.1(5) . . ?
C2 C7 C6 123.5(5) . . ?
C7 C2 C1 105.2(4) . . ?
C7 C2 C3 118.5(5) . . ?
C1 C2 C3 136.3(5) . . ?
N1 C1 C2 110.5(5) . . ?
N1 N2 C7 111.3(4) . . ?
C6 C5 C4 122.2(6) . . ?
N4 C14 C9 106.9(4) . . ?
N4 C14 C13 130.7(4) . . ?
C9 C14 C13 122.4(4) . . ?
C14 C9 C8 105.2(4) . . ?
C14 C9 C10 119.0(5) . . ?
C8 C9 C10 135.9(5) . . ?
N3 C8 C9 110.4(4) . . ?
C3 C4 C5 122.1(5) . . ?
C12 C13 C14 117.2(5) . . ?
C13 C12 C11 120.6(5) . . ?
C10 C11 C12 122.7(5) . . ?
C11 C10 C9 118.1(5) . . ?
C4 C3 C2 118.2(6) . . ?
C5 C6 C7 115.6(6) . . ?
C15 O1 Ru1 129.9(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
Ru1 N3 2.053(4) . ?
Ru1 O1 2.056(3) . ?
Ru1 N1 2.085(4) . ?
Ru1 Cl2 2.3149(12) . ?
Ru1 Cl3 2.3243(13) . ?
Ru1 Cl1 2.3537(11) . ?
N1 C1 1.315(6) . ?
N1 N2 1.351(5) . ?
N3 C8 1.317(5) . ?
N3 N4 1.348(5) . ?
N4 C14 1.347(5) . ?
C7 N2 1.355(6) . ?
C7 C2 1.383(7) . ?
C7 C6 1.397(7) . ?
C2 C1 1.407(7) . ?
C2 C3 1.412(7) . ?
C5 C6 1.364(8) . ?
C5 C4 1.384(8) . ?
C14 C9 1.377(6) . ?
C14 C13 1.394(7) . ?
C9 C8 1.400(7) . ?
C9 C10 1.411(6) . ?
C4 C3 1.348(9) . ?
C13 C12 1.361(7) . ?
C12 C11 1.390(8) . ?
C11 C10 1.342(8) . ?
O1 C15 1.376(6) . ?
O2 C16 1.475(8) . ?
O2X C16X 1.516(11) . ?
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
O1 Ru1 N1 C1 -74.1(4) . . . . ?
Cl2 Ru1 N1 C1 107.7(4) . . . . ?
Cl3 Ru1 N1 C1 14.8(4) . . . . ?
Cl1 Ru1 N1 C1 -161.3(4) . . . . ?
O1 Ru1 N1 N2 103.3(3) . . . . ?
Cl2 Ru1 N1 N2 -74.9(3) . . . . ?
Cl3 Ru1 N1 N2 -167.8(3) . . . . ?
Cl1 Ru1 N1 N2 16.1(3) . . . . ?
O1 Ru1 N3 C8 133.7(4) . . . . ?
Cl2 Ru1 N3 C8 -48.0(4) . . . . ?
Cl3 Ru1 N3 C8 44.9(4) . . . . ?
Cl1 Ru1 N3 C8 -139.0(4) . . . . ?
O1 Ru1 N3 N4 -53.9(3) . . . . ?
Cl2 Ru1 N3 N4 124.4(3) . . . . ?
Cl3 Ru1 N3 N4 -142.7(3) . . . . ?
Cl1 Ru1 N3 N4 33.4(3) . . . . ?
C8 N3 N4 C14 0.7(5) . . . . ?
Ru1 N3 N4 C14 -173.3(3) . . . . ?
N2 C7 C2 C1 -0.8(5) . . . . ?
C6 C7 C2 C1 -179.3(5) . . . . ?
N2 C7 C2 C3 178.2(4) . . . . ?
C6 C7 C2 C3 -0.2(7) . . . . ?
N2 N1 C1 C2 -0.5(5) . . . . ?
Ru1 N1 C1 C2 177.2(3) . . . . ?
C7 C2 C1 N1 0.8(5) . . . . ?
C3 C2 C1 N1 -178.0(5) . . . . ?
C1 N1 N2 C7 0.0(5) . . . . ?
Ru1 N1 N2 C7 -178.0(3) . . . . ?
C2 C7 N2 N1 0.5(5) . . . . ?
C6 C7 N2 N1 178.9(5) . . . . ?
N3 N4 C14 C9 -0.7(5) . . . . ?
N3 N4 C14 C13 178.7(5) . . . . ?
N4 C14 C9 C8 0.4(5) . . . . ?
C13 C14 C9 C8 -179.0(5) . . . . ?
N4 C14 C9 C10 179.4(5) . . . . ?
C13 C14 C9 C10 -0.1(8) . . . . ?
N4 N3 C8 C9 -0.4(5) . . . . ?
Ru1 N3 C8 C9 172.9(3) . . . . ?
C14 C9 C8 N3 0.0(6) . . . . ?
C10 C9 C8 N3 -178.7(6) . . . . ?
C6 C5 C4 C3 0.6(10) . . . . ?
N4 C14 C13 C12 -178.3(5) . . . . ?
C9 C14 C13 C12 1.0(8) . . . . ?
C14 C13 C12 C11 -1.7(9) . . . . ?
C13 C12 C11 C10 1.6(10) . . . . ?
C12 C11 C10 C9 -0.6(10) . . . . ?
C14 C9 C10 C11 -0.2(9) . . . . ?
C8 C9 C10 C11 178.4(6) . . . . ?
C5 C4 C3 C2 0.7(9) . . . . ?
C7 C2 C3 C4 -0.8(8) . . . . ?
C1 C2 C3 C4 177.8(6) . . . . ?
C4 C5 C6 C7 -1.6(9) . . . . ?
N2 C7 C6 C5 -176.7(5) . . . . ?
C2 C7 C6 C5 1.5(8) . . . . ?
N3 Ru1 O1 C15 171.3(6) . . . . ?
N1 Ru1 O1 C15 -6.8(6) . . . . ?
Cl3 Ru1 O1 C15 -98.0(6) . . . . ?
Cl1 Ru1 O1 C15 82.6(6) . . . . ?
