#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:08:31 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179095 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/57/4305722.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_4305722
loop_
_publ_author_name
'Iryna Stepanenko'
'Artem A. Krokhin'
'Roland O. John'
'Alexander Roller'
'Vladimir B. Arion'
'Michael A. Jakupec'
'Bernhard K. Keppler'
_publ_section_title
;
Synthesis, Structure, Spectroscopic Properties, and Antiproliferative
Activity In Vitro of Novel Osmium(III) Complexes with Azole Heterocycles
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7338
_journal_page_last               7347
_journal_paper_doi               10.1021/ic8006958
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C12 H16 Cl3 N8 Os'
_chemical_formula_weight         568.88
_chemical_name_systematic
; 
trans-[Dichloridotetrakis(pyrazole)ruthenium(III)]chloride 
;
_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                102.690(2)
_cell_angle_beta                 90.8860(10)
_cell_angle_gamma                110.743(2)
_cell_formula_units_Z            2
_cell_length_a                   7.9101(2)
_cell_length_b                   8.4109(2)
_cell_length_c                   14.6494(4)
_cell_measurement_reflns_used    1873
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.92
_cell_measurement_theta_min      2.81
_cell_volume                     884.54(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_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  0.0330
_diffrn_reflns_av_sigmaI/netI    0.0159
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            46148
_diffrn_reflns_theta_full        30.08
_diffrn_reflns_theta_max         30.08
_diffrn_reflns_theta_min         2.67
_exptl_absorpt_coefficient_mu    7.674
_exptl_absorpt_correction_T_max  0.4595
_exptl_absorpt_correction_T_min  0.2500
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.136
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             542
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.641
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         5180
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0162
_refine_ls_R_factor_gt           0.0129
_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)+(0.0125P)²+0.6463P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0296
_refine_ls_wR_factor_ref         0.0306
_reflns_number_gt                4609
_reflns_number_total             5180
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8006958-file002_4.cif
_cod_data_source_block           arkr146z
_cod_database_code               4305722
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
Os1 Os 0.5000 0.5000 0.5000 0.00812(2) Uani 1 2 d S . .
Os2 Os 0.0000 0.5000 0.0000 0.00859(2) Uani 1 2 d S . .
Cl1 Cl 0.18397(5) 0.33391(5) 0.48601(3) 0.01251(7) Uani 1 1 d . . .
Cl2 Cl -0.16286(5) 0.68704(5) 0.04401(3) 0.01277(7) Uani 1 1 d . . .
Cl3 Cl 0.02432(6) 0.90857(6) 0.29688(3) 0.01705(8) Uani 1 1 d . . .
N1 N 0.54765(19) 0.27004(18) 0.45716(9) 0.0110(3) Uani 1 1 d . . .
N2 N 0.4258(2) 0.11825(18) 0.40335(10) 0.0129(3) Uani 1 1 d . . .
H2 H 0.3127 0.1019 0.3861 0.015 Uiso 1 1 calc R . .
C3 C 0.5008(3) -0.0035(2) 0.38002(12) 0.0162(3) Uani 1 1 d . . .
H3 H 0.4416 -0.1198 0.3432 0.019 Uiso 1 1 calc R . .
C4 C 0.6791(2) 0.0704(2) 0.41903(13) 0.0168(3) Uani 1 1 d . . .
H4 H 0.7670 0.0168 0.4145 0.020 Uiso 1 1 calc R . .
C5 C 0.7024(2) 0.2403(2) 0.46643(12) 0.0141(3) Uani 1 1 d . . .
H5 H 0.8125 0.3238 0.5007 0.017 Uiso 1 1 calc R . .
N6 N 0.48373(19) 0.51327(19) 0.36122(10) 0.0111(3) Uani 1 1 d . . .
N7 N 0.61213(19) 0.63396(19) 0.32572(10) 0.0122(3) Uani 1 1 d . . .
H7 H 0.7118 0.7139 0.3584 0.015 Uiso 1 1 calc R . .
C8 C 0.5669(2) 0.6151(3) 0.23433(12) 0.0169(3) Uani 1 1 d . . .
H8 H 0.6362 0.6836 0.1947 0.020 Uiso 1 1 calc R . .
C9 C 0.4030(2) 0.4793(3) 0.20840(12) 0.0188(4) Uani 1 1 d . . .
H9 H 0.3356 0.4357 0.1482 0.023 Uiso 1 1 calc R . .
C10 C 0.3559(2) 0.4184(2) 0.28948(12) 0.0165(3) Uani 1 1 d . . .
H10 H 0.2485 0.3234 0.2931 0.020 Uiso 1 1 calc R . .
N11 N -0.04112(19) 0.41871(18) 0.12409(10) 0.0110(3) Uani 1 1 d . . .
N12 N -0.0537(2) 0.51570(19) 0.20901(10) 0.0136(3) Uani 1 1 d . . .
H12 H -0.0396 0.6271 0.2204 0.016 Uiso 1 1 calc R . .
C13 C -0.0903(2) 0.4199(2) 0.27346(12) 0.0166(3) Uani 1 1 d . . .
H13 H -0.1057 0.4597 0.3375 0.020 Uiso 1 1 calc R . .
C14 C -0.1015(2) 0.2531(2) 0.22956(12) 0.0156(3) Uani 1 1 d . . .
H14 H -0.1258 0.1555 0.2567 0.019 Uiso 1 1 calc R . .
C15 C -0.0694(2) 0.2588(2) 0.13700(12) 0.0134(3) Uani 1 1 d . . .
H15 H -0.0679 0.1624 0.0894 0.016 Uiso 1 1 calc R . .
N16 N 0.23828(18) 0.70756(18) 0.05692(10) 0.0111(3) Uani 1 1 d . . .
N17 N 0.2535(2) 0.85137(19) 0.12456(10) 0.0159(3) Uani 1 1 d . . .
H17 H 0.1622 0.8686 0.1531 0.019 Uiso 1 1 calc R . .
C18 C 0.4271(2) 0.9648(2) 0.14251(13) 0.0173(3) Uani 1 1 d . . .
H18 H 0.4712 1.0745 0.1873 0.021 Uiso 1 1 calc R . .
C19 C 0.5282(2) 0.8925(2) 0.08409(13) 0.0179(3) Uani 1 1 d . . .
H19 H 0.6553 0.9413 0.0802 0.021 Uiso 1 1 calc R . .
C20 C 0.4066(2) 0.7335(2) 0.03206(13) 0.0146(3) Uani 1 1 d . . .
H20 H 0.4379 0.6538 -0.0148 0.017 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'
Os Os -1.2165 7.6030 '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
N6 Os1 N6 180.000(1) . 2_666 ?
N6 Os1 N1 90.95(5) . 2_666 ?
N6 Os1 N1 89.05(5) 2_666 2_666 ?
N6 Os1 N1 89.05(5) . . ?
N6 Os1 N1 90.95(5) 2_666 . ?
N1 Os1 N1 180.0 2_666 . ?
N6 Os1 Cl1 90.94(4) . . ?
N6 Os1 Cl1 89.06(4) 2_666 . ?
N1 Os1 Cl1 90.70(4) 2_666 . ?
N1 Os1 Cl1 89.30(4) . . ?
N6 Os1 Cl1 89.06(4) . 2_666 ?
N6 Os1 Cl1 90.94(4) 2_666 2_666 ?
N1 Os1 Cl1 89.30(4) 2_666 2_666 ?
N1 Os1 Cl1 90.70(4) . 2_666 ?
Cl1 Os1 Cl1 180.0 . 2_666 ?
N16 Os2 N16 180.00(8) 2_565 . ?
N16 Os2 N11 86.60(5) 2_565 . ?
N16 Os2 N11 93.40(5) . . ?
N16 Os2 N11 93.40(5) 2_565 2_565 ?
N16 Os2 N11 86.60(5) . 2_565 ?
N11 Os2 N11 180.00(8) . 2_565 ?
N16 Os2 Cl2 90.76(4) 2_565 . ?
N16 Os2 Cl2 89.24(4) . . ?
N11 Os2 Cl2 91.26(4) . . ?
N11 Os2 Cl2 88.74(4) 2_565 . ?
N16 Os2 Cl2 89.24(4) 2_565 2_565 ?
N16 Os2 Cl2 90.76(4) . 2_565 ?
N11 Os2 Cl2 88.74(4) . 2_565 ?
N11 Os2 Cl2 91.26(4) 2_565 2_565 ?
Cl2 Os2 Cl2 180.0 . 2_565 ?
C5 N1 N2 105.49(14) . . ?
C5 N1 Os1 129.52(12) . . ?
N2 N1 Os1 124.67(11) . . ?
C3 N2 N1 111.00(14) . . ?
C3 N2 H2 124.5 . . ?
N1 N2 H2 124.5 . . ?
N2 C3 C4 107.73(16) . . ?
N2 C3 H3 126.1 . . ?
C4 C3 H3 126.1 . . ?
C3 C4 C5 105.12(15) . . ?
C3 C4 H4 127.4 . . ?
C5 C4 H4 127.4 . . ?
N1 C5 C4 110.66(16) . . ?
N1 C5 H5 124.7 . . ?
C4 C5 H5 124.7 . . ?
C10 N6 N7 105.55(13) . . ?
C10 N6 Os1 131.12(12) . . ?
N7 N6 Os1 123.32(11) . . ?
C8 N7 N6 111.09(14) . . ?
C8 N7 H7 124.5 . . ?
N6 N7 H7 124.5 . . ?
N7 C8 C9 107.70(15) . . ?
N7 C8 H8 126.2 . . ?
C9 C8 H8 126.2 . . ?
C8 C9 C10 105.36(16) . . ?
C8 C9 H9 127.3 . . ?
C10 C9 H9 127.3 . . ?
N6 C10 C9 110.29(16) . . ?
N6 C10 H10 124.9 . . ?
C9 C10 H10 124.9 . . ?
C15 N11 N12 105.45(13) . . ?
C15 N11 Os2 127.81(11) . . ?
N12 N11 Os2 126.67(11) . . ?
C13 N12 N11 111.25(14) . . ?
C13 N12 H12 124.4 . . ?
N11 N12 H12 124.4 . . ?
N12 C13 C14 107.44(15) . . ?
N12 C13 H13 126.3 . . ?
C14 C13 H13 126.3 . . ?
C13 C14 C15 105.07(15) . . ?
C13 C14 H14 127.5 . . ?
C15 C14 H14 127.5 . . ?
N11 C15 C14 110.79(15) . . ?
N11 C15 H15 124.6 . . ?
C14 C15 H15 124.6 . . ?
C20 N16 N17 105.61(14) . . ?
C20 N16 Os2 128.10(12) . . ?
N17 N16 Os2 126.20(11) . . ?
C18 N17 N16 110.97(15) . . ?
C18 N17 H17 124.5 . . ?
N16 N17 H17 124.5 . . ?
N17 C18 C19 107.24(16) . . ?
N17 C18 H18 126.4 . . ?
C19 C18 H18 126.4 . . ?
C18 C19 C20 105.65(16) . . ?
C18 C19 H19 127.2 . . ?
C20 C19 H19 127.2 . . ?
N16 C20 C19 110.53(16) . . ?
N16 C20 H20 124.7 . . ?
C19 C20 H20 124.7 . . ?
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
Os1 N6 2.0649(13) . ?
Os1 N6 2.0649(13) 2_666 ?
Os1 N1 2.0657(14) 2_666 ?
Os1 N1 2.0657(14) . ?
Os1 Cl1 2.3722(4) . ?
Os1 Cl1 2.3722(4) 2_666 ?
Os2 N16 2.0680(14) 2_565 ?
Os2 N16 2.0680(14) . ?
Os2 N11 2.0699(14) . ?
Os2 N11 2.0699(14) 2_565 ?
Os2 Cl2 2.3591(4) . ?
Os2 Cl2 2.3591(4) 2_565 ?
N1 C5 1.344(2) . ?
N1 N2 1.3576(19) . ?
N2 C3 1.342(2) . ?
N2 H2 0.8800 . ?
C3 C4 1.378(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.390(2) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
N6 C10 1.338(2) . ?
N6 N7 1.3603(19) . ?
N7 C8 1.340(2) . ?
N7 H7 0.8800 . ?
C8 C9 1.369(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.399(2) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
N11 C15 1.339(2) . ?
N11 N12 1.3558(19) . ?
N12 C13 1.342(2) . ?
N12 H12 0.8800 . ?
C13 C14 1.380(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.391(2) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
N16 C20 1.340(2) . ?
N16 N17 1.351(2) . ?
N17 C18 1.348(2) . ?
N17 H17 0.8800 . ?
C18 C19 1.371(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.383(2) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
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
N6 Os1 N1 C5 107.04(15) . . . . ?
N6 Os1 N1 C5 -72.96(15) 2_666 . . . ?
Cl1 Os1 N1 C5 -162.01(14) . . . . ?
Cl1 Os1 N1 C5 17.99(14) 2_666 . . . ?
N6 Os1 N1 N2 -65.53(12) . . . . ?
N6 Os1 N1 N2 114.47(12) 2_666 . . . ?
Cl1 Os1 N1 N2 25.42(12) . . . . ?
Cl1 Os1 N1 N2 -154.58(12) 2_666 . . . ?
C5 N1 N2 C3 0.41(18) . . . . ?
Os1 N1 N2 C3 174.47(11) . . . . ?
N1 N2 C3 C4 -0.50(19) . . . . ?
N2 C3 C4 C5 0.38(19) . . . . ?
N2 N1 C5 C4 -0.16(18) . . . . ?
Os1 N1 C5 C4 -173.82(11) . . . . ?
C3 C4 C5 N1 -0.1(2) . . . . ?
N1 Os1 N6 C10 -108.02(16) 2_666 . . . ?
N1 Os1 N6 C10 71.98(16) . . . . ?
Cl1 Os1 N6 C10 -17.31(15) . . . . ?
Cl1 Os1 N6 C10 162.69(15) 2_666 . . . ?
N1 Os1 N6 N7 70.40(13) 2_666 . . . ?
N1 Os1 N6 N7 -109.60(13) . . . . ?
Cl1 Os1 N6 N7 161.11(12) . . . . ?
Cl1 Os1 N6 N7 -18.89(12) 2_666 . . . ?
C10 N6 N7 C8 -0.32(19) . . . . ?
Os1 N6 N7 C8 -179.08(11) . . . . ?
N6 N7 C8 C9 0.7(2) . . . . ?
N7 C8 C9 C10 -0.7(2) . . . . ?
N7 N6 C10 C9 -0.14(19) . . . . ?
Os1 N6 C10 C9 178.49(12) . . . . ?
C8 C9 C10 N6 0.5(2) . . . . ?
N16 Os2 N11 C15 53.35(14) 2_565 . . . ?
N16 Os2 N11 C15 -126.65(14) . . . . ?
Cl2 Os2 N11 C15 144.04(14) . . . . ?
Cl2 Os2 N11 C15 -35.96(14) 2_565 . . . ?
N16 Os2 N11 N12 -123.20(13) 2_565 . . . ?
N16 Os2 N11 N12 56.80(13) . . . . ?
Cl2 Os2 N11 N12 -32.52(13) . . . . ?
Cl2 Os2 N11 N12 147.48(13) 2_565 . . . ?
C15 N11 N12 C13 -0.52(19) . . . . ?
Os2 N11 N12 C13 176.66(12) . . . . ?
N11 N12 C13 C14 0.3(2) . . . . ?
N12 C13 C14 C15 0.0(2) . . . . ?
N12 N11 C15 C14 0.50(19) . . . . ?
Os2 N11 C15 C14 -176.63(11) . . . . ?
C13 C14 C15 N11 -0.3(2) . . . . ?
N11 Os2 N16 C20 116.61(15) . . . . ?
N11 Os2 N16 C20 -63.39(15) 2_565 . . . ?
Cl2 Os2 N16 C20 -152.17(14) . . . . ?
Cl2 Os2 N16 C20 27.83(14) 2_565 . . . ?
N11 Os2 N16 N17 -67.31(14) . . . . ?
N11 Os2 N16 N17 112.69(14) 2_565 . . . ?
Cl2 Os2 N16 N17 23.90(13) . . . . ?
Cl2 Os2 N16 N17 -156.10(13) 2_565 . . . ?
C20 N16 N17 C18 -0.42(19) . . . . ?
Os2 N16 N17 C18 -177.21(11) . . . . ?
N16 N17 C18 C19 0.3(2) . . . . ?
N17 C18 C19 C20 0.0(2) . . . . ?
N17 N16 C20 C19 0.39(19) . . . . ?
Os2 N16 C20 C19 177.10(12) . . . . ?
C18 C19 C20 N16 -0.2(2) . . . . ?
