#------------------------------------------------------------------------------
#$Date: 2015-10-09 09:01:57 +0300 (Fri, 09 Oct 2015) $
#$Revision: 161117 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/63/7036311.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_7036311
loop_
_publ_author_name
'Nejman, Phillip S.'
'Morton-Fernandez, Brian'
'Moulding, David J.'
'Athukorala Arachchige, Kasun S.'
'Cordes, David B.'
'Slawin, Alexandra M. Z.'
'Kilian, Petr'
'Woollins, J. Derek'
_publ_section_title
;
 Structural diversity of bimetallic rhodium and iridium half sandwich
 dithiolato complexes.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16758
_journal_page_last               16766
_journal_paper_doi               10.1039/c5dt02542g
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C33 H39 Cl11 Ir2 S2'
_chemical_formula_sum            'C33 H39 Cl11 Ir2 S2'
_chemical_formula_weight         1274.21
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-05-18
_audit_creation_method           'by CrystalStructure 4.1'
_audit_update_record
;
2015-07-29 deposited with the CCDC.
2015-08-27 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   16.8938(14)
_cell_length_b                   11.8801(9)
_cell_length_c                   21.7865(18)
_cell_measurement_reflns_used    13341
_cell_measurement_temperature    93
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      1.50
_cell_volume                     4372.6(6)
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b32'
_computing_data_collection
'CrystalClear-SM Expert 2.1 b32 (Rigaku, 2014)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b32'
_computing_molecular_graphics    'CrystalStructure 4.1'
_computing_publication_material  'CrystalStructure 4.1 (Rigaku, 2014)'
_computing_structure_refinement  'SHELXL2013 (Sheldrick, 2008)'
_computing_structure_solution    'DIRDIF99-PATTY (Gould, et al., 1999)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 5.814
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0573
_diffrn_reflns_laue_measured_fraction_full 0.997
_diffrn_reflns_laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            58051
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.343
_diffrn_reflns_theta_min         1.525
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.888
_exptl_absorpt_correction_T_max  0.709
_exptl_absorpt_correction_T_min  0.437
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.935
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2440.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         5.98
_refine_diff_density_min         -2.47
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     245
_refine_ls_number_reflns         4196
_refine_ls_number_restraints     72
_refine_ls_R_factor_all          0.0919
_refine_ls_R_factor_gt           0.0916
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.1681P)²+106.8838P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2458
_refine_ls_wR_factor_ref         0.2747
_reflns_number_gt                3832
_reflns_number_total             4196
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            c5dt02542g2.cif
_cod_data_source_block           6b
_cod_depositor_comments
'Adding full bibliography for 7036305--7036311.cif.'
_cod_database_code               7036311
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 1/2-X,1/2+Y,1/2+Z
3 +X,1/2-Y,+Z
4 1/2-X,-Y,1/2+Z
5 -X,-Y,-Z
6 -1/2+X,-1/2-Y,-1/2-Z
7 -X,-1/2+Y,-Z
8 -1/2+X,+Y,-1/2-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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Ir1 Ir 0.40409(4) 0.7500 0.48797(4) 0.0402(3) Uani 1 2 d S T P
Ir2 Ir 0.42179(5) 0.7500 0.33683(4) 0.0476(3) Uani 1 2 d S T P
Cl1 Cl 0.5201(3) 0.7500 0.4195(3) 0.0665(17) Uani 1 2 d S T P
Cl2 Cl 0.8022(5) 0.7500 0.5973(3) 0.0749(19) Uani 1 2 d S T P
Cl3 Cl 0.7158(3) 0.7500 0.4256(4) 0.0714(18) Uani 1 2 d S T P
Cl4 Cl 0.8636(3) 0.8718(5) 0.4189(3) 0.0761(14) Uani 1 1 d . . .
Cl5 Cl 0.6615(7) 0.1255(11) 0.2685(5) 0.165(4) Uani 1 1 d . U .
Cl6 Cl 0.8004(11) 0.2500 0.2682(7) 0.162(5) Uani 1 2 d S TU P
Cl7 Cl 0.4638(19) 0.2500 0.1655(13) 0.264(9) Uani 1 2 d S TU P
Cl8 Cl 0.4624(7) 0.3667(9) 0.0534(5) 0.147(3) Uani 1 1 d . U .
S1 S 0.3637(2) 0.8753(3) 0.40840(19) 0.0459(9) Uani 1 1 d . . .
C1 C 0.2600(9) 0.8570(15) 0.4028(7) 0.052(4) Uani 1 1 d . . .
C2 C 0.2162(13) 0.9532(19) 0.4005(8) 0.071(6) Uani 1 1 d . . .
H2 H 0.2426 1.0238 0.4012 0.085 Uiso 1 1 calc R U .
C3 C 0.1351(15) 0.951(3) 0.3973(11) 0.097(9) Uani 1 1 d . . .
H3 H 0.1063 1.0198 0.3963 0.116 Uiso 1 1 calc R U .
C4 C 0.0982(12) 0.858(3) 0.3956(12) 0.096(9) Uani 1 1 d . . .
H4 H 0.0420 0.8580 0.3939 0.115 Uiso 1 1 calc R U .
C5 C 0.1400(16) 0.7500 0.3963(13) 0.085(11) Uani 1 2 d S T P
C6 C 0.2210(14) 0.7500 0.4020(11) 0.057(6) Uani 1 2 d S T P
C7 C 0.3251(19) 0.7500 0.5607(17) 0.117(16) Uani 1 2 d S T P
C8 C 0.3658(18) 0.843(2) 0.5659(13) 0.097(7) Uani 1 1 d . U .
C9 C 0.4461(17) 0.809(2) 0.5734(12) 0.091(7) Uani 1 1 d . U .
C10 C 0.240(3) 0.7500 0.553(3) 0.30(7) Uani 1 2 d S T P
H10A H 0.2151 0.7742 0.5917 0.361 Uiso 0.5 1 calc R U P
H10B H 0.2221 0.6739 0.5431 0.361 Uiso 0.5 1 calc R U P
H10C H 0.2253 0.8019 0.5203 0.361 Uiso 0.5 1 calc R U P
C11 C 0.318(8) 0.959(6) 0.563(3) 0.44(8) Uani 1 1 d . . .
C12 C 0.514(7) 0.864(13) 0.5820(15) 0.63(15) Uani 1 1 d . . .
C13 C 0.364(2) 0.7500 0.2529(15) 0.083(8) Uani 1 2 d S TU P
C14 C 0.4271(14) 0.845(2) 0.2539(11) 0.082(6) Uani 1 1 d . U .
C15 C 0.4955(19) 0.796(2) 0.2621(13) 0.115(9) Uani 1 1 d . U .
C16 C 0.274(4) 0.7500 0.241(3) 0.179(12) Uani 1 2 d S TU P
C17 C 0.395(4) 0.970(6) 0.251(3) 0.232(12) Uani 1 1 d . U .
C18 C 0.575(3) 0.863(5) 0.262(2) 0.180(11) Uani 1 1 d . U .
C19 C 0.8142(12) 0.7500 0.4469(11) 0.048(5) Uani 1 2 d S T P
H19 H 0.8173 0.7500 0.4927 0.058 Uiso 1 2 calc R U P
C20 C 0.699(3) 0.2500 0.246(2) 0.104(12) Uani 1 2 d S T P
H20 H 0.6983 0.2500 0.1998 0.125 Uiso 1 2 calc R U P
C21 C 0.4994(17) 0.2500 0.0944(16) 0.087(10) Uani 1 2 d S T P
H21 H 0.5586 0.2500 0.0947 0.104 Uiso 1 2 calc R U P
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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
Cl Cl 0.1484 0.1585
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Ir Ir -1.4442 7.9887
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.1246 0.1234
;
International Tables for Crystallography
(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
C7 Ir1 C8 36.1(9) . 3_565
C7 Ir1 C8 36.1(9) . .
C8 Ir1 C8 62.4(16) 3_565 .
C7 Ir1 C9 62.8(13) . .
C8 Ir1 C9 64.6(11) 3_565 .
C8 Ir1 C9 39.2(11) . .
C7 Ir1 C9 62.8(13) . 3_565
C8 Ir1 C9 39.2(11) 3_565 3_565
C8 Ir1 C9 64.6(11) . 3_565
C9 Ir1 C9 39.0(15) . 3_565
C7 Ir1 S1 111.8(8) . .
C8 Ir1 S1 144.8(8) 3_565 .
C8 Ir1 S1 99.8(8) . .
C9 Ir1 S1 121.9(7) . .
C9 Ir1 S1 160.9(8) 3_565 .
C7 Ir1 S1 111.8(8) . 3_565
C8 Ir1 S1 99.8(8) 3_565 3_565
C8 Ir1 S1 144.8(8) . 3_565
C9 Ir1 S1 160.9(8) . 3_565
C9 Ir1 S1 121.9(7) 3_565 3_565
S1 Ir1 S1 77.24(19) . 3_565
C7 Ir1 Cl1 167.4(11) . .
C8 Ir1 Cl1 136.6(8) 3_565 .
C8 Ir1 Cl1 136.6(8) . .
C9 Ir1 Cl1 105.4(8) . .
C9 Ir1 Cl1 105.4(8) 3_565 .
S1 Ir1 Cl1 77.70(15) . .
S1 Ir1 Cl1 77.70(15) 3_565 .
C13 Ir2 C14 43.3(9) . 3_565
C13 Ir2 C14 43.3(9) . .
C14 Ir2 C14 63.7(13) 3_565 .
C13 Ir2 C15 66.4(12) . .
C14 Ir2 C15 57.2(10) 3_565 .
C14 Ir2 C15 35.8(9) . .
C13 Ir2 C15 66.4(12) . 3_565
C14 Ir2 C15 35.8(9) 3_565 3_565
C14 Ir2 C15 57.2(10) . 3_565
C15 Ir2 C15 29.5(15) . 3_565
C13 Ir2 S1 112.6(7) . 3_565
C14 Ir2 S1 104.1(7) 3_565 3_565
C14 Ir2 S1 155.2(7) . 3_565
C15 Ir2 S1 155.4(8) . 3_565
C15 Ir2 S1 126.1(8) 3_565 3_565
C13 Ir2 S1 112.6(7) . .
C14 Ir2 S1 155.2(7) 3_565 .
C14 Ir2 S1 104.1(7) . .
C15 Ir2 S1 126.1(8) . .
C15 Ir2 S1 155.4(8) 3_565 .
S1 Ir2 S1 77.87(18) 3_565 .
C13 Ir2 Cl1 165.5(10) . .
C14 Ir2 Cl1 126.5(7) 3_565 .
C14 Ir2 Cl1 126.5(7) . .
C15 Ir2 Cl1 99.6(8) . .
C15 Ir2 Cl1 99.6(8) 3_565 .
S1 Ir2 Cl1 78.28(14) 3_565 .
S1 Ir2 Cl1 78.28(14) . .
Ir1 Cl1 Ir2 84.58(17) . .
C1 S1 Ir2 106.7(6) . .
C1 S1 Ir1 104.9(6) . .
Ir2 S1 Ir1 88.17(12) . .
C2 C1 C6 119.6(17) . .
C2 C1 S1 115.9(16) . .
C6 C1 S1 124.4(13) . .
C1 C2 C3 122(2) . .
C1 C2 H2 119.0 . .
C3 C2 H2 119.0 . .
C4 C3 C2 120(2) . .
C4 C3 H3 119.8 . .
C2 C3 H3 119.8 . .
C5 C4 C3 121.7(19) . .
C5 C4 H4 119.1 . .
C3 C4 H4 119.1 . .
C4 C5 C4 122(3) . 3_565
C4 C5 C6 118.9(15) . .
C4 C5 C6 118.9(15) 3_565 .
C5 C6 C1 117.3(10) . 3_565
C5 C6 C1 117.3(10) . .
C1 C6 C1 125(2) 3_565 .
C8 C7 C8 115(4) 3_565 .
C8 C7 C10 122.3(18) 3_565 .
C8 C7 C10 122.3(18) . .
C8 C7 Ir1 74.1(17) 3_565 .
C8 C7 Ir1 74.1(17) . .
C10 C7 Ir1 124(3) . .
C7 C8 C9 106(3) . .
C7 C8 C11 117(6) . .
C9 C8 C11 136(6) . .
C7 C8 Ir1 69.8(18) . .
C9 C8 Ir1 70.0(16) . .
C11 C8 Ir1 124(3) . .
C8 C9 C12 135(8) . .
C8 C9 C9 106.1(16) . 3_565
C12 C9 C9 119(7) . 3_565
C8 C9 Ir1 70.8(16) . .
C12 C9 Ir1 125(3) . .
C9 C9 Ir1 70.5(7) 3_565 .
C7 C10 H10A 109.5 . .
C7 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C7 C10 H10C 109.4 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
C16 C13 C14 132.9(14) . .
C16 C13 C14 132.9(14) . 3_565
C14 C13 C14 93(3) . 3_565
C16 C13 Ir2 128(3) . .
C14 C13 Ir2 70.3(15) . .
C14 C13 Ir2 70.3(15) 3_565 .
C15 C14 C17 136(3) . .
C15 C14 C13 107(2) . .
C17 C14 C13 117(3) . .
C15 C14 Ir2 71.7(17) . .
C17 C14 Ir2 121(3) . .
C13 C14 Ir2 66.4(15) . .
C15 C15 C14 116.5(17) 3_565 .
C15 C15 C18 121(2) 3_565 .
C14 C15 C18 122(3) . .
C15 C15 Ir2 75.2(8) 3_565 .
C14 C15 Ir2 72.5(17) . .
C18 C15 Ir2 129(3) . .
Cl3 C19 Cl4 111.1(8) . 3_565
Cl3 C19 Cl4 111.1(8) . .
Cl4 C19 Cl4 109.0(13) 3_565 .
Cl3 C19 H19 108.5 . .
Cl4 C19 H19 108.5 3_565 .
Cl4 C19 H19 108.5 . .
Cl5 C20 Cl5 123(3) 3 .
Cl5 C20 Cl6 106.4(18) 3 .
Cl5 C20 Cl6 106.4(18) . .
Cl5 C20 H20 106.8 3 .
Cl5 C20 H20 106.8 . .
Cl6 C20 H20 106.8 . .
Cl7 C21 Cl8 110.2(15) . 3
Cl7 C21 Cl8 110.2(15) . .
Cl8 C21 Cl8 103.6(17) 3 .
Cl7 C21 H21 110.9 . .
Cl8 C21 H21 110.9 3 .
Cl8 C21 H21 110.9 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ir1 C7 2.07(3) .
Ir1 C8 2.12(3) 3_565
Ir1 C8 2.12(3) .
Ir1 C9 2.11(3) .
Ir1 C9 2.11(3) 3_565
Ir1 S1 2.384(4) .
Ir1 S1 2.384(4) 3_565
Ir1 Cl1 2.464(6) .
Ir2 C13 2.07(3) .
Ir2 C14 2.13(2) 3_565
Ir2 C14 2.13(2) .
Ir2 C15 2.12(3) .
Ir2 C15 2.12(3) 3_565
Ir2 S1 2.368(4) 3_565
Ir2 S1 2.368(4) .
Ir2 Cl1 2.450(6) .
Cl3 C19 1.73(2) .
Cl4 C19 1.777(14) .
Cl5 C20 1.68(2) .
Cl6 C20 1.78(5) .
Cl7 C21 1.66(4) .
Cl8 C21 1.76(2) .
S1 C1 1.771(17) .
C1 C2 1.36(2) .
C1 C6 1.43(2) .
C2 C3 1.37(3) .
C2 H2 0.9500 .
C3 C4 1.27(4) .
C3 H3 0.9500 .
C4 C5 1.46(3) .
C4 H4 0.9500 .
C5 C4 1.46(3) 3_565
C5 C6 1.37(4) .
C6 C1 1.43(2) 3_565
C7 C8 1.30(3) 3_565
C7 C8 1.30(3) .
C7 C10 1.45(6) .
C8 C9 1.42(4) .
C8 C11 1.60(6) .
C9 C12 1.33(11) .
C9 C9 1.41(5) 3_565
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C13 C16 1.55(8) .
C13 C14 1.55(3) .
C13 C14 1.55(3) 3_565
C14 C15 1.31(4) .
C14 C17 1.58(7) .
C15 C15 1.08(6) 3_565
C15 C18 1.57(5) .
C19 Cl4 1.777(14) 3_565
C19 H19 1.0000 .
C20 Cl5 1.68(2) 3
C20 H20 1.0000 .
C21 Cl8 1.76(2) 3
C21 H21 1.0000 .
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_4
Ir2 S1 C1 C2 -134.4(13) . .
Ir1 S1 C1 C2 133.0(13) . .
Ir2 S1 C1 C6 47.1(17) . .
Ir1 S1 C1 C6 -45.5(17) . .
C6 C1 C2 C3 0(3) . .
S1 C1 C2 C3 -178.8(16) . .
C1 C2 C3 C4 -1(4) . .
C2 C3 C4 C5 -1(4) . .
C3 C4 C5 C4 178.8(19) . 3_565
C3 C4 C5 C6 3(4) . .
C4 C5 C6 C1 180(2) . 3_565
C4 C5 C6 C1 4(4) 3_565 3_565
C4 C5 C6 C1 -4(4) . .
C4 C5 C6 C1 -180(2) 3_565 .
C2 C1 C6 C5 3(3) . .
S1 C1 C6 C5 -178.9(18) . .
C2 C1 C6 C1 178.5(16) . 3_565
S1 C1 C6 C1 -3(3) . 3_565
C8 C7 C8 C9 2(5) 3_565 .
C10 C7 C8 C9 179(4) . .
Ir1 C7 C8 C9 -61(2) . .
C8 C7 C8 C11 -178(3) 3_565 .
C10 C7 C8 C11 -1(6) . .
Ir1 C7 C8 C11 119(4) . .
C8 C7 C8 Ir1 63(3) 3_565 .
C10 C7 C8 Ir1 -120(4) . .
C7 C8 C9 C12 -178(4) . .
C11 C8 C9 C12 2(7) . .
Ir1 C8 C9 C12 121(4) . .
C7 C8 C9 C9 -1(3) . 3_565
C11 C8 C9 C9 179(5) . 3_565
Ir1 C8 C9 C9 -62.1(7) . 3_565
C7 C8 C9 Ir1 61(2) . .
C11 C8 C9 Ir1 -119(5) . .
C16 C13 C14 C15 -175(5) . .
C14 C13 C14 C15 -7(3) 3_565 .
Ir2 C13 C14 C15 61(2) . .
C16 C13 C14 C17 10(6) . .
C14 C13 C14 C17 178(3) 3_565 .
Ir2 C13 C14 C17 -114(3) . .
C16 C13 C14 Ir2 124(5) . .
C14 C13 C14 Ir2 -67.8(16) 3_565 .
C17 C14 C15 C15 178(4) . 3_565
C13 C14 C15 C15 5(2) . 3_565
Ir2 C14 C15 C15 62.9(9) . 3_565
C17 C14 C15 C18 -10(6) . .
C13 C14 C15 C18 177(3) . .
Ir2 C14 C15 C18 -126(3) . .
C17 C14 C15 Ir2 116(5) . .
C13 C14 C15 Ir2 -57.4(18) . .
