##############################################################################
#                                                                            #
# This CIF contains the data in a paper accepted for publication in          #
# Acta Crystallographica Section E. It conforms to the requirements of       #
# Notes for Authors for Acta Crystallographica Section E, and has been       #
# peer reviewed under the auspices of the IUCr Commission on Journals.       #
#                                                                            #
# Full details of the Crystallographic Information File format               #
# are given in the paper "The Crystallographic Information File (CIF):       #
# a New Standard Archive File for Crystallography" by S. R. Hall, F. H.      #
# Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685].                  #
#                                                                            #
# The current version of the core CIF dictionary is obtainable from          #
# ftp://ftp.iucr.org/pub/cif_core.dic.                                       #
#                                                                            #
# Software is freely available for graphical display of the structure(s)     #
# in this CIF. For information consult the CIF software page                 #
# http://www.iucr.org/resources/cif/software.                                #
#                                                                            #
# This file may be used for bona fide research purposes within the           #
# scientific community so long as proper attribution is given to the journal # 
# article from which it was obtained.                                        #
#                                                                            #
##############################################################################
data_I
_database_code_depnum_ccdc_archive 'CCDC 1495966'
_journal_date_recd_electronic     2016-07-27
_journal_date_accepted     2016-08-09
_journal_name_full     'Acta Crystallographica, Section E'
_journal_year     2016
_journal_volume     72
_journal_issue      9
_journal_page_first     1305
_journal_page_last     1309
_journal_paper_category     GM
_journal_paper_doi     10.1107/S2056989016012883
_journal_coeditor_code     PK2588
_publ_contact_author_name     'Merola, J.S.'
_publ_contact_author_address
;
Department of Chemistry
Virginia Tech
Blacksburg, VA 24061
USA
;
_publ_contact_author_email     'jmerola@vt.edu'
_publ_contact_author_fax     ?
_publ_contact_author_phone     '+1 540-231-4510'
_publ_section_title
;
mer-Trichloridotris(tetrahydrothiophene-κS)iridium(III):
preparation and comparison with other
mer-trichloridotris(tetrahydrothiophene-κS)metal complexes
;
_publ_section_title_footnote     .
loop_
    _publ_author_name
    _publ_author_footnote
    _publ_author_address
    'Brown, Loren C.' .
;
Department of Chemistry
Virginia Tech
Blacksburg, VA 24061
USA
;
    'DuChane, Christine M.' .
;
Department of Chemistry
Virginia Tech
Blacksburg, VA 24061
USA
;
    'Merola, Joseph S.' .
;
Department of Chemistry
Virginia Tech
Blacksburg, VA 24061
USA
;
_publ_section_synopsis
;
The crystal structure of
mer-trichloridotris(tetrahydrothiophene-κS)iridium(III) is
reported and compared with a different form of the complex previously
reported. It is also compared with other
mer-trichloridotris(tetrahydrothiophene-κS)metal(III) complexes
of molybdenum, ruthenium and rhodium.
;
_chemical_name_systematic
;
mer-Trichloridotris(tetrahydrothiophene-κS)iridium(III)
;
_chemical_name_common     ?
_chemical_formula_moiety     'C12 H24 Cl3 Ir S3'
_chemical_formula_sum     'C12 H24 Cl3 Ir S3'
_chemical_formula_iupac     '[Ir Cl3 (C4 H8 S1)3]'
_chemical_formula_weight     563.04
_chemical_melting_point     ?
_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.
;
_space_group_crystal_system     monoclinic
_space_group_name_H-M_alt     'P 21/n'
_space_group_name_Hall     '-P 2yn'
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'
_cell_length_a     11.9160(3)
_cell_length_b     10.2528(2)
_cell_length_c     14.9434(4)
_cell_angle_alpha     90
_cell_angle_beta     107.202(3)
_cell_angle_gamma     90
_cell_volume     1744.00(7)
_cell_formula_units_Z     4
_cell_measurement_reflns_used     9679
_cell_measurement_theta_min     4.1340
_cell_measurement_theta_max     32.2080
_cell_measurement_temperature     100.2(3)
_exptl_crystal_description     cube
_exptl_crystal_colour     yellow
_exptl_crystal_size_max     0.507
_exptl_crystal_size_mid     0.431
_exptl_crystal_size_min     0.324
_exptl_crystal_density_diffrn     2.144
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     ?
_exptl_crystal_F_000     1088
loop_
    _exptl_crystal_face_index_h
    _exptl_crystal_face_index_k
    _exptl_crystal_face_index_l
    _exptl_crystal_face_perp_dist
    2 5 -2 0.2131
    -3 0 5 0.1696
    -3 -2 5 0.1778
    -1 -5 0 0.1407
    3 -1 -5 0.2348
    -3 5 -1 0.2032
    2 -5 2 0.1447
    0 -4 5 0.1785
    1 2 -5 0.3090
    4 -3 5 0.2001
    5 -3 -4 0.2190
    -5 3 -3 0.2118
    5 -1 -4 0.2339
    4 0 5 0.2256
    -5 -2 -3 0.2317
    -1 2 5 0.2105
    5 3 5 0.2147
    -5 -5 -3 0.2035
    5 1 -4 0.2363
    4 5 5 0.1759
    5 1 -5 0.2295
    2 5 2 0.1493
    4 1 -5 0.2334
    0 5 1 0.1574
_exptl_absorpt_coefficient_mu     8.459
_exptl_absorpt_correction_type     analytical
_exptl_absorpt_process_details
;
[CrysAlis PRO (Rigaku Oxford Diffraction, 2015) based on expressions
derived
by Clark & Reid (1995)]
;
_shelx_estimated_absorpt_T_min     ?
_shelx_estimated_absorpt_T_max     ?
_exptl_absorpt_correction_T_min     0.064
_exptl_absorpt_correction_T_max     0.155
_diffrn_ambient_temperature     100.2(3)
_diffrn_radiation_type     MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device_type     'Rigaku OD Xcalibur Eos Gemini ultra'
_diffrn_measurement_device     'four-circle diffractometer'
_diffrn_measurement_method     'ω scans'
_diffrn_detector_area_resol_mean     8.0061
_diffrn_reflns_number     19537
_diffrn_reflns_av_R_equivalents     0.0418
_diffrn_reflns_theta_min     3.580
_diffrn_reflns_theta_max     32.238
_diffrn_reflns_theta_full     30.500
_diffrn_measured_fraction_theta_max     0.935
_diffrn_measured_fraction_theta_full     0.998
_diffrn_reflns_limit_h_min     -13
_diffrn_reflns_limit_h_max     17
_diffrn_reflns_limit_k_min     -13
_diffrn_reflns_limit_k_max     15
_diffrn_reflns_limit_l_min     -22
_diffrn_reflns_limit_l_max     21
_refine_special_details     ?
_reflns_number_total     5773
_reflns_number_gt     5062
_reflns_threshold_expression     'I > 2σ(I)'
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all     0.0350
_refine_ls_R_factor_gt     0.0286
_refine_ls_wR_factor_gt     0.0602
_refine_ls_wR_factor_ref     0.0631
_refine_ls_goodness_of_fit_ref     1.052
_refine_ls_restrained_S_all     1.052
_refine_ls_number_reflns     5773
_refine_ls_number_parameters     172
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment     constr
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
              'w=1/[σ²(Fo²)+(0.0223P)²+0.8135P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens     geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary     ?
_refine_ls_shift/su_max     0.002
_refine_ls_shift/su_mean     0.000
_refine_diff_density_max     1.537
_refine_diff_density_min     -1.464
_refine_ls_extinction_method     none
_refine_ls_extinction_coef     .
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'
    'S' 'S' 0.1246 0.1234
                         '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'
    'Ir' 'Ir' -1.4442 7.9887
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_computing_data_collection
;
CrysAlis PRO (Rigaku Oxford Diffraction, 2015)
;
_computing_cell_refinement
;
CrysAlis PRO (Rigaku Oxford Diffraction, 2015)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku Oxford Diffraction, 2015)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_computing_structure_refinement
;
SHELXL2016 (Sheldrick, 2015b)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov et al.,  2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al.,  2009)
and Mercury (Macrae et al., 2008)
;
loop_
    _atom_site_type_symbol
    _atom_site_label
    _atom_site_fract_x
    _atom_site_fract_y
    _atom_site_fract_z
    _atom_site_U_iso_or_equiv
    _atom_site_adp_type
    _atom_site_calc_flag
    _atom_site_occupancy
    _atom_site_disorder_assembly
    _atom_site_disorder_group
    Ir Ir1 0.45092(2) 0.70407(2) 0.73222(2) 0.01133(4) Uani d 1 . .
    Cl Cl1 0.59718(7) 0.70422(8) 0.65431(6) 0.01922(17) Uani d 1 . .
    Cl Cl2 0.59716(8) 0.73216(8) 0.87865(6) 0.01887(16) Uani d 1 . .
    Cl Cl3 0.30344(7) 0.71455(8) 0.80946(6) 0.01688(16) Uani d 1 . .
    S S1 0.46678(7) 0.47667(8) 0.74921(6) 0.01509(16) Uani d 1 . .
    S S2 0.30373(7) 0.68096(8) 0.59053(6) 0.01540(16) Uani d 1 . .
    S S3 0.44035(7) 0.93361(9) 0.72529(6) 0.01636(16) Uani d 1 . .
    C C1 0.6230(3) 0.4314(4) 0.7907(3) 0.0236(8) Uani d 1 . .
    H H1A 0.6388 0.3570 0.7540 0.028 Uiso calc 1 . .
    H H1B 0.6727 0.5059 0.7837 0.028 Uiso calc 1 . .
    C C2 0.6496(3) 0.3940(4) 0.8934(3) 0.0281(9) Uani d 1 . .
    H H2A 0.7157 0.3314 0.9114 0.034 Uiso calc 1 . .
    H H2B 0.6710 0.4722 0.9337 0.034 Uiso calc 1 . .
    C C3 0.5384(4) 0.3321(4) 0.9044(3) 0.0257(8) Uani d 1 . .
    H H3A 0.5449 0.3203 0.9715 0.031 Uiso calc 1 . .
    H H3B 0.5246 0.2459 0.8732 0.031 Uiso calc 1 . .
    C C4 0.4380(3) 0.4262(4) 0.8582(3) 0.0216(7) Uani d 1 . .
    H H4A 0.4387 0.5024 0.8991 0.026 Uiso calc 1 . .
    H H4B 0.3610 0.3820 0.8448 0.026 Uiso calc 1 . .
    C C5 0.3455(3) 0.5674(4) 0.5104(3) 0.0277(9) Uani d 1 . .
    H H5A 0.3271 0.6057 0.4469 0.033 Uiso calc 1 . .
    H H5B 0.4308 0.5488 0.5331 0.033 Uiso calc 1 . .
    C C6 0.2749(3) 0.4419(4) 0.5082(3) 0.0261(8) Uani d 1 . .
    H H6A 0.2620 0.3969 0.4474 0.031 Uiso calc 1 . .
    H H6B 0.3179 0.3822 0.5588 0.031 Uiso calc 1 . .
    C C7 0.1582(3) 0.4802(4) 0.5219(3) 0.0225(8) Uani d 1 . .
    H H7A 0.1078 0.5244 0.4654 0.027 Uiso calc 1 . .
    H H7B 0.1163 0.4024 0.5348 0.027 Uiso calc 1 . .
    C C8 0.1883(3) 0.5720(4) 0.6051(3) 0.0192(7) Uani d 1 . .
    H H8A 0.2167 0.5224 0.6643 0.023 Uiso calc 1 . .
    H H8B 0.1182 0.6229 0.6065 0.023 Uiso calc 1 . .
    C C9 0.3843(3) 0.9968(4) 0.6060(2) 0.0188(7) Uani d 1 . .
    H H9A 0.3912 0.9305 0.5597 0.023 Uiso calc 1 . .
    H H9B 0.3010 1.0232 0.5920 0.023 Uiso calc 1 . .
    C C10 0.4624(3) 1.1147(4) 0.6047(3) 0.0213(7) Uani d 1 . .
    H H10A 0.4527 1.1433 0.5396 0.026 Uiso calc 1 . .
    H H10B 0.4424 1.1883 0.6400 0.026 Uiso calc 1 . .
    C C11 0.5875(3) 1.0686(4) 0.6510(3) 0.0228(8) Uani d 1 . .
    H H11A 0.6424 1.1434 0.6631 0.027 Uiso calc 1 . .
    H H11B 0.6119 1.0058 0.6099 0.027 Uiso calc 1 . .
    C C12 0.5882(3) 1.0027(4) 0.7436(3) 0.0209(7) Uani d 1 . .
    H H12A 0.6061 1.0674 0.7951 0.025 Uiso calc 1 . .
    H H12B 0.6483 0.9330 0.7598 0.025 Uiso calc 1 . .
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
    _geom_bond_atom_site_label_1
    _geom_bond_atom_site_label_2
    _geom_bond_site_symmetry_2
    _geom_bond_distance
    _geom_bond_publ_flag
    Ir1 Cl1 . 2.3648(8) ?
    Ir1 Cl2 . 2.3774(9) ?
    Ir1 Cl3 . 2.3732(8) ?
    Ir1 S1 . 2.3469(9) ?
    Ir1 S2 . 2.3279(9) ?
    Ir1 S3 . 2.3575(9) ?
    S1 C1 . 1.839(4) ?
    S1 C4 . 1.835(4) ?
    S2 C5 . 1.841(4) ?
    S2 C8 . 1.834(3) ?
    S3 C9 . 1.827(4) ?
    S3 C12 . 1.843(4) ?
    C1 H1A . 0.9900 ?
    C1 H1B . 0.9900 ?
    C1 C2 . 1.522(6) ?
    C2 H2A . 0.9900 ?
    C2 H2B . 0.9900 ?
    C2 C3 . 1.521(6) ?
    C3 H3A . 0.9900 ?
    C3 H3B . 0.9900 ?
    C3 C4 . 1.533(5) ?
    C4 H4A . 0.9900 ?
    C4 H4B . 0.9900 ?
    C5 H5A . 0.9900 ?
    C5 H5B . 0.9900 ?
    C5 C6 . 1.533(6) ?
    C6 H6A . 0.9900 ?
    C6 H6B . 0.9900 ?
    C6 C7 . 1.516(5) ?
    C7 H7A . 0.9900 ?
    C7 H7B . 0.9900 ?
    C7 C8 . 1.515(5) ?
    C8 H8A . 0.9900 ?
    C8 H8B . 0.9900 ?
    C9 H9A . 0.9900 ?
    C9 H9B . 0.9900 ?
    C9 C10 . 1.529(5) ?
    C10 H10A . 0.9900 ?
    C10 H10B . 0.9900 ?
    C10 C11 . 1.521(5) ?
    C11 H11A . 0.9900 ?
    C11 H11B . 0.9900 ?
    C11 C12 . 1.537(5) ?
    C12 H12A . 0.9900 ?
    C12 H12B . 0.9900 ?
loop_
    _geom_angle_atom_site_label_1
    _geom_angle_atom_site_label_2
    _geom_angle_atom_site_label_3
    _geom_angle_site_symmetry_1
    _geom_angle_site_symmetry_3
    _geom_angle
    _geom_angle_publ_flag
    Cl1 Ir1 Cl2 . . 90.39(3) ?
    Cl1 Ir1 Cl3 . . 177.35(3) ?
    Cl3 Ir1 Cl2 . . 89.63(3) ?
    S1 Ir1 Cl1 . . 90.37(3) ?
    S1 Ir1 Cl2 . . 90.41(3) ?
    S1 Ir1 Cl3 . . 92.28(3) ?
    S1 Ir1 S3 . . 176.44(3) ?
    S2 Ir1 Cl1 . . 91.09(3) ?
    S2 Ir1 Cl2 . . 178.15(3) ?
    S2 Ir1 Cl3 . . 88.85(3) ?
    S2 Ir1 S1 . . 90.70(3) ?
    S2 Ir1 S3 . . 92.61(3) ?
    S3 Ir1 Cl1 . . 90.88(3) ?
    S3 Ir1 Cl2 . . 86.25(3) ?
    S3 Ir1 Cl3 . . 86.47(3) ?
    C1 S1 Ir1 . . 109.15(13) ?
    C4 S1 Ir1 . . 110.23(12) ?
    C4 S1 C1 . . 93.79(17) ?
    C5 S2 Ir1 . . 112.32(13) ?
    C8 S2 Ir1 . . 110.12(13) ?
    C8 S2 C5 . . 92.79(17) ?
    C9 S3 Ir1 . . 113.33(12) ?
    C9 S3 C12 . . 93.79(16) ?
    C12 S3 Ir1 . . 109.93(12) ?
    S1 C1 H1A . . 110.3 ?
    S1 C1 H1B . . 110.3 ?
    H1A C1 H1B . . 108.6 ?
    C2 C1 S1 . . 106.9(3) ?
    C2 C1 H1A . . 110.3 ?
    C2 C1 H1B . . 110.3 ?
    C1 C2 H2A . . 110.4 ?
    C1 C2 H2B . . 110.4 ?
    H2A C2 H2B . . 108.6 ?
    C3 C2 C1 . . 106.7(3) ?
    C3 C2 H2A . . 110.4 ?
    C3 C2 H2B . . 110.4 ?
    C2 C3 H3A . . 110.5 ?
    C2 C3 H3B . . 110.5 ?
    C2 C3 C4 . . 106.1(3) ?
    H3A C3 H3B . . 108.7 ?
    C4 C3 H3A . . 110.5 ?
    C4 C3 H3B . . 110.5 ?
    S1 C4 H4A . . 110.8 ?
    S1 C4 H4B . . 110.8 ?
    C3 C4 S1 . . 104.6(2) ?
    C3 C4 H4A . . 110.8 ?
    C3 C4 H4B . . 110.8 ?
    H4A C4 H4B . . 108.9 ?
    S2 C5 H5A . . 110.3 ?
    S2 C5 H5B . . 110.3 ?
    H5A C5 H5B . . 108.6 ?
    C6 C5 S2 . . 107.0(2) ?
    C6 C5 H5A . . 110.3 ?
    C6 C5 H5B . . 110.3 ?
    C5 C6 H6A . . 110.2 ?
    C5 C6 H6B . . 110.2 ?
    H6A C6 H6B . . 108.5 ?
    C7 C6 C5 . . 107.4(3) ?
    C7 C6 H6A . . 110.2 ?
    C7 C6 H6B . . 110.2 ?
    C6 C7 H7A . . 110.6 ?
    C6 C7 H7B . . 110.6 ?
    H7A C7 H7B . . 108.8 ?
    C8 C7 C6 . . 105.5(3) ?
    C8 C7 H7A . . 110.6 ?
    C8 C7 H7B . . 110.6 ?
    S2 C8 H8A . . 110.4 ?
    S2 C8 H8B . . 110.4 ?
    C7 C8 S2 . . 106.6(2) ?
    C7 C8 H8A . . 110.4 ?
    C7 C8 H8B . . 110.4 ?
    H8A C8 H8B . . 108.6 ?
    S3 C9 H9A . . 110.9 ?
    S3 C9 H9B . . 110.9 ?
    H9A C9 H9B . . 108.9 ?
    C10 C9 S3 . . 104.2(2) ?
    C10 C9 H9A . . 110.9 ?
    C10 C9 H9B . . 110.9 ?
    C9 C10 H10A . . 110.7 ?
    C9 C10 H10B . . 110.7 ?
    H10A C10 H10B . . 108.8 ?
    C11 C10 C9 . . 105.5(3) ?
    C11 C10 H10A . . 110.7 ?
    C11 C10 H10B . . 110.7 ?
    C10 C11 H11A . . 110.4 ?
    C10 C11 H11B . . 110.4 ?
    C10 C11 C12 . . 106.8(3) ?
    H11A C11 H11B . . 108.6 ?
    C12 C11 H11A . . 110.4 ?
    C12 C11 H11B . . 110.4 ?
    S3 C12 H12A . . 110.4 ?
    S3 C12 H12B . . 110.4 ?
    C11 C12 S3 . . 106.5(2) ?
    C11 C12 H12A . . 110.4 ?
    C11 C12 H12B . . 110.4 ?
    H12A C12 H12B . . 108.6 ?
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_site_symmetry_1
    _geom_torsion_site_symmetry_2
    _geom_torsion_site_symmetry_3
    _geom_torsion_site_symmetry_4
    _geom_torsion
    _geom_torsion_publ_flag
    Ir1 S1 C1 C2 . . . . 106.1(3) ?
    Ir1 S1 C4 C3 . . . . -132.6(2) ?
    Ir1 S2 C5 C6 . . . . 106.8(2) ?
    Ir1 S2 C8 C7 . . . . -135.6(2) ?
    Ir1 S3 C9 C10 . . . . -138.6(2) ?
    Ir1 S3 C12 C11 . . . . 114.0(2) ?
    S1 C1 C2 C3 . . . . 33.0(4) ?
    S2 C5 C6 C7 . . . . 31.9(4) ?
    S3 C9 C10 C11 . . . . 46.4(3) ?
    C1 S1 C4 C3 . . . . -20.5(3) ?
    C1 C2 C3 C4 . . . . -49.8(4) ?
    C2 C3 C4 S1 . . . . 43.0(4) ?
    C4 S1 C1 C2 . . . . -6.9(3) ?
    C5 S2 C8 C7 . . . . -20.6(3) ?
    C5 C6 C7 C8 . . . . -48.0(4) ?
    C6 C7 C8 S2 . . . . 42.1(3) ?
    C8 S2 C5 C6 . . . . -6.3(3) ?
    C9 S3 C12 C11 . . . . -2.5(3) ?
    C9 C10 C11 C12 . . . . -49.9(4) ?
    C10 C11 C12 S3 . . . . 29.9(4) ?
    C12 S3 C9 C10 . . . . -25.0(3) ?
