#------------------------------------------------------------------------------
#$Date: 2018-01-26 09:51:48 +0200 (Fri, 26 Jan 2018) $
#$Revision: 205694 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/10/81/2108192.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2108192
loop_
_publ_author_name
'Ridgway, Benjamin M.'
'Foi, Ana'
'Corrêa, Rodrigo S.'
'Bikiel, Damian E.'
'Ellena, Javier'
'Doctorovich, Fabio'
'Di Salvo, Florencia'
_publ_section_title
;
 Conformational and structural diversity of iridium dimethyl sulfoxide
 complexes
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              1032
_journal_page_last               1042
_journal_paper_doi               10.1107/S2052520617011490
_journal_volume                  73
_journal_year                    2017
_chemical_formula_moiety         'C4 H12 Cl4 Ir K O2 S2'
_chemical_formula_sum            'C4 H12 Cl4 Ir K O2 S2'
_chemical_formula_weight         529.36
_chemical_name_common
'Potassium tetrachlorobis(dimethylsulfoxide)iridate(III)'
_chemical_name_systematic
'Potassium tetrachlorobis(dimethylsulfoxide)iridate(III)'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 91.425(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9902(7)
_cell_length_b                   15.1990(14)
_cell_length_c                   10.7569(9)
_cell_measurement_reflns_used    2542
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.8748
_cell_measurement_theta_min      3.5038
_cell_volume                     1469.4(2)
_computing_cell_refinement
;
'Scalepack (Otwinowski & Minor 1997)'
;
_computing_data_collection
;
COLLECT (Enraf-Nonius, 1997-2004)
;
_computing_data_reduction
;
'DENZO and SCALEPACK (Otwinowski & Minor 1997)'
;
_computing_molecular_graphics
;
C.B. Hubschle, G.M. Scheldrick, and B. Dittrich
Shelxle: a Qt graphical user interface for SHELXL
J. Appl. Cryst., 44 (2011) 1281--1284
;
_computing_publication_material
;
The PyMol Molecular Graphics System, Version #, Schrodinger, LLC.
Version 1.7.2.1
;
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.1158
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  Gemini
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1328
_diffrn_reflns_av_unetI/netI     0.1296
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            8941
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         3.511
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    10.357
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.27081
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.393
_exptl_crystal_description       needle
_exptl_crystal_F_000             992
_exptl_crystal_recrystallization_method
;
'Crystallized from DMSO solution of title compound and 
 subjected to heating.'
;
_exptl_crystal_size_max          0.143
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         2.935
_refine_diff_density_min         -2.382
_refine_diff_density_rms         0.316
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     131
_refine_ls_number_reflns         2582
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1127
_refine_ls_R_factor_gt           0.0720
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0647P)²+13.5359P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1577
_refine_ls_wR_factor_ref         0.1829
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1704
_reflns_number_total             2582
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            lo5014sup1.cif
_cod_data_source_block           2
_cod_database_code               2108192
_shelx_shelxl_version_number     2016/6
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.319
_shelx_estimated_absorpt_t_max   0.625
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_disorder_assembly
_atom_site_disorder_group
Ir1 Ir 0.28570(8) 0.61353(5) 0.26792(7) 0.0329(3) Uani 1 1 d . . A 1
K1 K 0.5409(6) 0.6218(3) 0.5981(5) 0.0606(14) Uani 1 1 d . . A 1
Cl1 Cl 0.2611(7) 0.4819(4) 0.1571(6) 0.0665(18) Uani 1 1 d . . A 1
Cl2 Cl 0.5394(6) 0.5752(4) 0.3036(6) 0.0607(16) Uani 1 1 d . . A 1
Cl3 Cl 0.3126(7) 0.7372(4) 0.3968(6) 0.0730(19) Uani 1 1 d . . A 1
Cl4 Cl 0.2362(7) 0.5342(5) 0.4528(5) 0.0664(18) Uani 1 1 d . . A 1
S1 S 0.3560(7) 0.6945(4) 0.1060(6) 0.0652(18) Uani 1 1 d . . A 1
S2 S 0.0420(5) 0.6467(3) 0.2359(5) 0.0411(12) Uani 1 1 d . . A 1
O1 O 0.2424(19) 0.7464(11) 0.0400(14) 0.074(5) Uani 1 1 d . . A 1
O2 O -0.0024(16) 0.7381(9) 0.2477(13) 0.056(4) Uani 1 1 d . . A 1
C1 C 0.446(5) 0.6300(19) -0.005(3) 0.138(18) Uani 1 1 d . . A 1
H1A H 0.469098 0.665600 -0.075464 0.207 Uiso 1 1 calc R U A 1
H1B H 0.382727 0.582332 -0.030471 0.207 Uiso 1 1 calc R U A 1
H1C H 0.537007 0.606749 0.031330 0.207 Uiso 1 1 calc R U A 1
C2 C 0.502(3) 0.7701(18) 0.146(3) 0.119(13) Uani 1 1 d . . A 1
H2A H 0.551910 0.787383 0.071852 0.179 Uiso 1 1 calc R U A 1
H2B H 0.571533 0.742491 0.202441 0.179 Uiso 1 1 calc R U A 1
H2C H 0.460364 0.821192 0.184435 0.179 Uiso 1 1 calc R U A 1
C3 C -0.027(3) 0.6111(14) 0.088(2) 0.068(7) Uani 1 1 d . . A 1
H3A H -0.133272 0.608586 0.087888 0.102 Uiso 1 1 calc R U A 1
H3B H 0.012380 0.553819 0.069897 0.102 Uiso 1 1 calc R U A 1
H3C H 0.004140 0.651872 0.025037 0.102 Uiso 1 1 calc R U A 1
C4 C -0.067(3) 0.5856(18) 0.340(3) 0.093(11) Uani 1 1 d . . A 1
H4A H -0.162880 0.613232 0.346780 0.140 Uiso 1 1 calc R U A 1
H4B H -0.018358 0.583620 0.419844 0.140 Uiso 1 1 calc R U A 1
H4C H -0.080478 0.526839 0.308512 0.140 Uiso 1 1 calc R U A 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ir Ir -1.4442 7.9887 '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'
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'
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'
K K 0.2009 0.2494 '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
S1 Ir1 S2 92.9(2) . .
S1 Ir1 Cl1 95.7(3) . .
S2 Ir1 Cl1 91.9(2) . .
S1 Ir1 Cl3 89.6(3) . .
S2 Ir1 Cl3 89.8(2) . .
Cl1 Ir1 Cl3 174.4(2) . .
S1 Ir1 Cl2 88.4(2) . .
S2 Ir1 Cl2 178.52(19) . .
Cl1 Ir1 Cl2 87.2(2) . .
Cl3 Ir1 Cl2 91.0(2) . .
S1 Ir1 Cl4 173.2(2) . .
S2 Ir1 Cl4 92.27(19) . .
Cl1 Ir1 Cl4 88.6(2) . .
Cl3 Ir1 Cl4 86.0(3) . .
Cl2 Ir1 Cl4 86.5(2) . .
O2 K1 O1 70.8(4) 4_676 4_676
O2 K1 Cl4 142.7(4) 4_676 3_666
O1 K1 Cl4 94.7(4) 4_676 3_666
O2 K1 Cl2 139.1(4) 4_676 .
O1 K1 Cl2 85.7(3) 4_676 .
Cl4 K1 Cl2 69.79(18) 3_666 .
O2 K1 Cl2 119.6(4) 4_676 3_666
O1 K1 Cl2 152.1(4) 4_676 3_666
Cl4 K1 Cl2 60.92(17) 3_666 3_666
Cl2 K1 Cl2 96.92(19) . 3_666
O2 K1 Cl4 117.2(4) 4_676 .
O1 K1 Cl4 134.6(4) 4_676 .
Cl4 K1 Cl4 97.71(19) 3_666 .
Cl2 K1 Cl4 58.74(17) . .
Cl2 K1 Cl4 66.83(17) 3_666 .
O2 K1 Cl3 83.1(4) 4_676 .
O1 K1 Cl3 82.7(4) 4_676 .
Cl4 K1 Cl3 130.3(2) 3_666 .
Cl2 K1 Cl3 60.49(17) . .
Cl2 K1 Cl3 122.7(2) 3_666 .
Cl4 K1 Cl3 56.35(17) . .
O2 K1 Cl1 89.1(4) 4_676 3_666
O1 K1 Cl1 99.8(4) 4_676 3_666
Cl4 K1 Cl1 58.79(16) 3_666 3_666
Cl2 K1 Cl1 128.5(2) . 3_666
Cl2 K1 Cl1 57.14(16) 3_666 3_666
Cl4 K1 Cl1 123.9(2) . 3_666
Cl3 K1 Cl1 170.6(2) . 3_666
O2 K1 K1 160.3(4) 4_676 3_666
O1 K1 K1 127.7(4) 4_676 3_666
Cl4 K1 K1 51.16(16) 3_666 3_666
Cl2 K1 K1 48.63(15) . 3_666
Cl2 K1 K1 48.30(15) 3_666 3_666
Cl4 K1 K1 46.55(15) . 3_666
Cl3 K1 K1 92.19(19) . 3_666
Cl1 K1 K1 93.35(18) 3_666 3_666
Ir1 Cl1 K1 87.82(19) . 3_666
Ir1 Cl2 K1 94.8(2) . .
Ir1 Cl2 K1 93.3(2) . 3_666
K1 Cl2 K1 83.08(19) . 3_666
Ir1 Cl3 K1 90.8(2) . .
Ir1 Cl4 K1 95.9(2) . 3_666
Ir1 Cl4 K1 91.2(2) . .
K1 Cl4 K1 82.29(19) 3_666 .
O1 S1 C1 107.6(14) . .
O1 S1 C2 105.6(12) . .
C1 S1 C2 99.9(19) . .
O1 S1 Ir1 117.9(7) . .
C1 S1 Ir1 111.4(9) . .
C2 S1 Ir1 112.8(11) . .
O2 S2 C4 106.8(12) . .
O2 S2 C3 106.2(9) . .
C4 S2 C3 102.7(14) . .
O2 S2 Ir1 117.8(6) . .
C4 S2 Ir1 109.8(8) . .
C3 S2 Ir1 112.4(9) . .
S1 O1 K1 137.0(9) . 4_575
S2 O2 K1 131.1(8) . 4_575
S1 C1 H1A 109.5 . .
S1 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
S1 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
S1 C2 H2A 109.5 . .
S1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
S1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
S2 C3 H3A 109.5 . .
S2 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
S2 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
S2 C4 H4A 109.5 . .
S2 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
S2 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ir1 S1 2.236(6) .
Ir1 S2 2.266(5) .
Ir1 Cl1 2.337(6) .
Ir1 Cl3 2.344(6) .
Ir1 Cl2 2.376(5) .
Ir1 Cl4 2.377(5) .
K1 O2 2.703(15) 4_676
K1 O1 2.782(17) 4_676
K1 Cl4 3.161(8) 3_666
K1 Cl2 3.246(9) .
K1 Cl2 3.262(8) 3_666
K1 Cl4 3.392(8) .
K1 Cl3 3.428(8) .
K1 Cl1 3.515(8) 3_666
S1 O1 1.461(16) .
S1 C1 1.76(3) .
S1 C2 1.79(3) .
S2 O2 1.451(14) .
S2 C4 1.77(2) .
S2 C3 1.78(2) .
C1 H1A 0.9600 .
C1 H1B 0.9600 .
C1 H1C 0.9600 .
C2 H2A 0.9600 .
C2 H2B 0.9600 .
C2 H2C 0.9600 .
C3 H3A 0.9600 .
C3 H3B 0.9600 .
C3 H3C 0.9600 .
C4 H4A 0.9600 .
C4 H4B 0.9600 .
C4 H4C 0.9600 .
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_4
C1 S1 O1 K1 -175.0(17) 4_575
C2 S1 O1 K1 -69.0(19) 4_575
Ir1 S1 O1 K1 58.0(17) 4_575
C4 S2 O2 K1 -163.0(13) 4_575
C3 S2 O2 K1 -53.9(14) 4_575
Ir1 S2 O2 K1 73.1(11) 4_575

_cod_database_fobs_code 2108192
