# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2015

data_global


#==============================================================================
#                          1. SUBMISSION DETAILS
#==============================================================================



_publ_contact_author_name   'Warren, Piers'

_publ_contact_author_address
;
      Department of Chemistry
      University of Calgary
      2500 University Dr. NW
      Calgary, Alberta  T2N 1N4
;


_publ_contact_author_phone        '403-220-5746'
_publ_contact_author_fax          '403-289-9488'
_publ_contact_author_email        'wpiers@ucalgary.ca'



#==============================================================================
#                   2. PROCESSING SUMMARY (IUCr Office Use Only)
#==============================================================================


_journal_date_recd_electronic     ?

_journal_date_to_coeditor         ?
_journal_date_from_coeditor       ?
_journal_date_accepted            ?

_journal_date_printers_first      ?
_journal_date_printers_final      ?
_journal_date_proofs_out          ?
_journal_date_proofs_in           ?

_journal_coeditor_name            ?
_journal_coeditor_code            ?
_journal_coeditor_notes
; ?
;

_journal_techeditor_code          ?
_journal_techeditor_notes
; ?
;

_journal_coden_ASTM               ?
_journal_name_full                ?
_journal_year                     ?
_journal_volume                   ?
_journal_issue                    ?
_journal_page_first               ?
_journal_page_last                ?

_journal_suppl_publ_number        ?
_journal_suppl_publ_pages         ?

#==============================================================================
#                        3. TITLE AND AUTHOR LIST
#==============================================================================


_publ_section_title
;
Structures of IrPCPS2 complexes 
;

# The loop structure below should contain the names and addresses of all
# authors, in the required order of publication. Repeat as necessary.

loop_
    _publ_author_name
    _publ_author_address
      'Lauren, Doyle'
;
     
      Department of Chemistry
      University of Calgary
      2500 University Dr. NW
      Calgary, Alberta  T2N 1N4
;
      'Denis, Spasyuk'
;
     
      Department of Chemistry
      University of Calgary
      2500 University Dr. NW
      Calgary, Alberta  T2N 1N4
;
      'Warren, Piers'
;
      
       Department of Chemistry
       University of Calgary
       2500 University Dr. NW
       Calgary, Alberta  T2N 1N4

;

  
#==============================================================================
#                              4. TEXT
#==============================================================================

_publ_requested_journal
;
 Organometallics
;
_publ_section_abstract
;
 Here should be written a short abstract
;


_publ_section_comment
;
 Here should be written the text  of the article
;





_publ_section_exptl_prep
;
 Small details about the preparation of the compound.
;




_publ_section_exptl_refinement
;

All non-H atoms were refined by full-matrix least-squares
with anisotropic displacement parameters. The H atoms were 
generated geometrically (C-H 0.93 to 0.98, N-H 0.86 and O-H 0.82Å)
and were included in the refinement in the riding model approximation; 
their temperature factors were set to 1.5 times those of the 
equivalent isotropic temperature factors of the parent site (methyl) 
and 1.2 times for others. 
A final verification of possible voids was performed using the VOID routine 
of the PLATON program (Spek, 2011). 
;



_publ_section_figure_captions
;
Fig 1 Ortep view of the title compound.
      Thermal ellipsoids are shown at 50% probability levels.
;



_publ_section_table_legends
;
Table 1.  Selected geometric parameters (Å, °) for the title compound.
;


_publ_section_references
;
 Bruker (1997). SHELXTL (1997). Release 5.10; The Complete Software Package 
 for Single Crystal Structure Determination.  Bruker AXS Inc.,
 Madison, USA.

 Bruker (1999a). SAINT Release 6.06. Integration Software for Single Crystal 
 Data. Bruker AXS Inc., Madison, USA.

 Bruker (1999b). SMART Release 5.059; Bruker Molecular Analysis Research Tool,
 Bruker AXS Inc., Madison, USA.

 Flack, H. D. (1983). Acta Cryst. A39, 876-881.

 Flack, H. D. and Schwarzenbach, D. (1988). Acta Cryst. A44, 499-506.

 Sheldrick, G. M. (1986). SHELXS86. Program for Crystal Structure
 solution. University of Göttingen, Germany.

 Sheldrick, G. M. (1996). SADABS, Bruker Area Detector Absorption Corrections.
 Bruker AXS Inc., Madison, USA.

 Sheldrick, G. M. (1997a). SHELXS97. Program for Crystal Structure
 solution. University of Göttingen, Germany.

 Sheldrick, G. M. (1997b). SHELXL97. Program for crystal structure
 refinement. University of Göttingen, Germany.

 Spek, A. L. (2000). PLATON,  2000 version; Molecular Geometry Program,
 University of Utrecht, Utrecht, Holland.
;
_publ_section_acknowledgements
;
We are grateful to the Natural Sciences and Engineering Research
Council of Canada. 
; 

data_3_OH
 
_audit_creation_method            SHELXL-2013
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety         'C29 H37 Ir O P2 S2'
_chemical_formula_sum
 'C29 H37 Ir O P2 S2' 
_chemical_formula_weight          719.84

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'
 'Ir'  'Ir'  -1.4442   7.9887
 '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'
 'P'  'P'   0.1023   0.0942
 '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'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            14
_space_group_name_H-M_alt         'P 21/c'
_space_group_name_Hall            '-P 2ybc'
 
_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.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y-1/2, z-1/2'
 
_cell_length_a                    13.5212(3)
_cell_length_b                    15.0131(4)
_cell_length_c                    16.0250(2)
_cell_angle_alpha                 90
_cell_angle_beta                  116.7160(10)
_cell_angle_gamma                 90
_cell_volume                      2905.73(11)
_cell_formula_units_Z             4
_cell_measurement_temperature     173(2)
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min       ?
_cell_measurement_theta_max       ?
 
_exptl_crystal_description       'Rhombohedral'
_exptl_crystal_colour            'Black'
_exptl_crystal_density_meas      '?'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn     1.645          
_exptl_crystal_F_000              1432
_exptl_transmission_factor_min    ?                                             
_exptl_transmission_factor_max    ?                                             
_exptl_crystal_size_max           0.08
_exptl_crystal_size_mid           0.06
_exptl_crystal_size_min           0.04
_exptl_absorpt_coefficient_mu     4.869
_shelx_estimated_absorpt_T_min    0.697
_shelx_estimated_absorpt_T_max    0.829
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.6967
_exptl_absorpt_correction_T_max   0.8291
_exptl_absorpt_process_details    'Sadabs (Sheldrick, 1996)'
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       173(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    ?                       
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number             18604
_diffrn_reflns_av_unetI/netI      0.0272
_diffrn_reflns_av_R_equivalents   0.0403
_diffrn_reflns_limit_h_min        -16
_diffrn_reflns_limit_h_max        16
_diffrn_reflns_limit_k_min        -17
_diffrn_reflns_limit_k_max        17
_diffrn_reflns_limit_l_min        -19
_diffrn_reflns_limit_l_max        19
_diffrn_reflns_theta_min          1.966
_diffrn_reflns_theta_max          24.999
_diffrn_reflns_theta_full         25.000
_diffrn_measured_fraction_theta_max   0.991
_diffrn_measured_fraction_theta_full  0.991
_diffrn_reflns_Laue_measured_fraction_max    0.991
_diffrn_reflns_Laue_measured_fraction_full   0.991
_diffrn_reflns_point_group_measured_fraction_max   0.991
_diffrn_reflns_point_group_measured_fraction_full  0.991
_reflns_number_total              5061
_reflns_number_gt                 4476
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection      'Bruker APEX2'
_computing_cell_refinement      'Bruker SAINT'
_computing_data_reduction       'Bruker SAINT'
_computing_structure_solution   'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics   'Bruker SHELXTL'
_computing_publication_material 'LinXTL v.  5.3.7'
 
_refine_special_details
;
 ?
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0230P)²+12.3043P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    mixed
_refine_ls_hydrogen_treatment     mixed
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          5061
_refine_ls_number_parameters      320
_refine_ls_number_restraints      2
_refine_ls_R_factor_all           0.0348
_refine_ls_R_factor_gt            0.0276
_refine_ls_wR_factor_ref          0.0682
_refine_ls_wR_factor_gt           0.0632
_refine_ls_goodness_of_fit_ref    1.044
_refine_ls_restrained_S_all       1.043
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
 
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
 _atom_site_disorder_assembly
 _atom_site_disorder_group
C1 C 0.1747(4) 0.4000(3) 0.1614(3) 0.0265(10) Uani 1 1 d . . . . .
C2 C 0.0857(4) 0.3341(3) 0.1401(3) 0.0260(10) Uani 1 1 d . . . . .
C3 C 0.0785(4) 0.2837(3) 0.2072(3) 0.0268(10) Uani 1 1 d . . . . .
C4 C -0.0094(4) 0.2205(3) 0.1730(3) 0.0279(10) Uani 1 1 d . . . . .
C5 C -0.0408(4) 0.1563(4) 0.2188(4) 0.0389(13) Uani 1 1 d . . . . .
H5 H -0.0011 0.1507 0.2848 0.047 Uiso 1 1 calc R U . . .
C6 C -0.1281(5) 0.1012(4) 0.1701(4) 0.0411(13) Uani 1 1 d . . . . .
H6 H -0.1481 0.0571 0.2023 0.049 Uiso 1 1 calc R U . . .
C7 C -0.1883(5) 0.1090(4) 0.0732(4) 0.0430(14) Uani 1 1 d . . . . .
H7 H -0.2491 0.0701 0.0404 0.052 Uiso 1 1 calc R U . . .
C8 C -0.1615(4) 0.1714(4) 0.0248(4) 0.0387(13) Uani 1 1 d . . . . .
H8 H -0.2030 0.1768 -0.0410 0.046 Uiso 1 1 calc R U . . .
C9 C -0.0713(4) 0.2270(3) 0.0752(3) 0.0292(11) Uani 1 1 d . . . . .
C10 C 0.1880(4) 0.4471(3) 0.0878(3) 0.0245(10) Uani 1 1 d . . . . .
C11 C 0.2767(4) 0.5019(3) 0.1077(3) 0.0293(11) Uani 1 1 d . . . . .
C12 C 0.2779(4) 0.5403(4) 0.0271(3) 0.0324(11) Uani 1 1 d . . . . .
C13 C 0.3533(5) 0.5995(4) 0.0196(4) 0.0496(16) Uani 1 1 d . . . . .
H13 H 0.4162 0.6189 0.0741 0.060 Uiso 1 1 calc R U . . .
C14 C 0.3361(5) 0.6293(5) -0.0662(4) 0.063(2) Uani 1 1 d . . . . .
H14 H 0.3870 0.6703 -0.0708 0.076 Uiso 1 1 calc R U . . .
C15 C 0.2450(5) 0.6007(5) -0.1479(4) 0.0573(18) Uani 1 1 d . . . . .
H15 H 0.2354 0.6211 -0.2072 0.069 Uiso 1 1 calc R U . . .
C16 C 0.1698(5) 0.5434(4) -0.1418(4) 0.0403(13) Uani 1 1 d . . . . .
H16 H 0.1073 0.5240 -0.1966 0.048 Uiso 1 1 calc R U . . .
C17 C 0.1864(4) 0.5144(3) -0.0550(3) 0.0299(11) Uani 1 1 d . . . . .
C18 C 0.2615(4) 0.1925(3) 0.3464(3) 0.0337(11) Uani 1 1 d . . . . .
H18 H 0.2080 0.1475 0.3482 0.040 Uiso 1 1 calc R U . . .
C19 C 0.2903(6) 0.1654(5) 0.2702(5) 0.068(2) Uani 1 1 d . . . . .
H19A H 0.2236 0.1668 0.2102 0.101 Uiso 1 1 calc R U . . .
H19B H 0.3209 0.1050 0.2823 0.101 Uiso 1 1 calc R U . . .
H19C H 0.3455 0.2067 0.2684 0.101 Uiso 1 1 calc R U . . .
C20 C 0.3620(6) 0.1908(6) 0.4403(5) 0.084(3) Uani 1 1 d . . . . .
H20A H 0.3406 0.2079 0.4890 0.126 Uiso 1 1 calc R U . . .
H20B H 0.4175 0.2327 0.4402 0.126 Uiso 1 1 calc R U . . .
H20C H 0.3933 0.1305 0.4529 0.126 Uiso 1 1 calc R U . . .
C21 C 0.1309(4) 0.3093(3) 0.4038(3) 0.0316(11) Uani 1 1 d . . . . .
H21 H 0.1098 0.2480 0.4142 0.038 Uiso 1 1 calc R U . . .
C22 C 0.2138(5) 0.3467(5) 0.4983(4) 0.0560(17) Uani 1 1 d . . . . .
H22A H 0.2807 0.3097 0.5237 0.084 Uiso 1 1 calc R U . . .
H22B H 0.1806 0.3464 0.5415 0.084 Uiso 1 1 calc R U . . .
H22C H 0.2333 0.4078 0.4902 0.084 Uiso 1 1 calc R U . . .
C23 C 0.0273(5) 0.3667(4) 0.3651(4) 0.0485(15) Uani 1 1 d . . . . .
H23A H -0.0266 0.3425 0.3049 0.073 Uiso 1 1 calc R U . . .
H23B H 0.0466 0.4277 0.3563 0.073 Uiso 1 1 calc R U . . .
H23C H -0.0049 0.3669 0.4090 0.073 Uiso 1 1 calc R U . . .
C24 C 0.5015(4) 0.4675(4) 0.2391(4) 0.0391(13) Uani 1 1 d . . . . .
H24 H 0.5210 0.5049 0.1971 0.047 Uiso 1 1 calc R U . . .
C25 C 0.5948(5) 0.4735(5) 0.3361(4) 0.0611(19) Uani 1 1 d . . . . .
H25A H 0.6035 0.5354 0.3576 0.092 Uiso 1 1 calc R U . . .
H25B H 0.6635 0.4531 0.3358 0.092 Uiso 1 1 calc R U . . .
H25C H 0.5783 0.4359 0.3783 0.092 Uiso 1 1 calc R U . . .
C26 C 0.4879(5) 0.3717(5) 0.2046(5) 0.067(2) Uani 1 1 d . . . . .
H26A H 0.4274 0.3684 0.1410 0.100 Uiso 1 1 calc R U . . .
H26B H 0.4708 0.3335 0.2460 0.100 Uiso 1 1 calc R U . . .
H26C H 0.5568 0.3515 0.2045 0.100 Uiso 1 1 calc R U . . .
C27 C 0.3909(4) 0.6287(3) 0.2574(4) 0.0371(12) Uani 1 1 d . . . . .
H27 H 0.4479 0.6503 0.2385 0.045 Uiso 1 1 calc R U . . .
C28 C 0.4341(5) 0.6438(4) 0.3615(4) 0.0491(15) Uani 1 1 d . . . . .
H28A H 0.5029 0.6103 0.3955 0.074 Uiso 1 1 calc R U . . .
H28B H 0.3788 0.6236 0.3811 0.074 Uiso 1 1 calc R U . . .
H28C H 0.4485 0.7075 0.3753 0.074 Uiso 1 1 calc R U . . .
C29 C 0.2842(5) 0.6806(4) 0.2022(4) 0.0533(16) Uani 1 1 d . . . . .
H29A H 0.2584 0.6703 0.1352 0.080 Uiso 1 1 calc R U . . .
H29B H 0.2982 0.7443 0.2156 0.080 Uiso 1 1 calc R U . . .
H29C H 0.2276 0.6606 0.2203 0.080 Uiso 1 1 calc R U . . .
Ir1 Ir 0.28328(2) 0.41538(2) 0.29114(2) 0.02468(7) Uani 1 1 d . . . . .
O1 O 0.3855(4) 0.4354(3) 0.4266(3) 0.0563(12) Uani 1 1 d D . . . .
P1 P 0.19098(10) 0.30157(9) 0.32118(8) 0.0267(3) Uani 1 1 d . . . . .
P2 P 0.36864(10) 0.50785(8) 0.23071(8) 0.0273(3) Uani 1 1 d D . . . .
S1 S -0.01967(10) 0.30849(8) 0.02930(8) 0.0301(3) Uani 1 1 d . . . . .
S2 S 0.10169(10) 0.44280(8) -0.03150(8) 0.0288(3) Uani 1 1 d . . . . .
H1O H 0.435(6) 0.473(5) 0.4337(15) 0.14(4) Uiso 1 1 d D . . . .
 
 
_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_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
C1 C10 1.453(7) . ?
C1 C2 1.474(6) . ?
C1 Ir1 1.946(5) . ?
C2 C3 1.355(6) . ?
C2 S1 1.748(5) . ?
C3 C4 1.423(7) . ?
C3 P1 1.795(5) . ?
C4 C5 1.389(7) . ?
C4 C9 1.409(7) . ?
C5 C6 1.363(7) . ?
C5 H5 0.9500 . ?
C6 C7 1.396(8) . ?
C6 H6 0.9500 . ?
C7 C8 1.365(8) . ?
C7 H7 0.9500 . ?
C8 C9 1.398(7) . ?
C8 H8 0.9500 . ?
C9 S1 1.728(5) . ?
C10 C11 1.369(7) . ?
C10 S2 1.737(5) . ?
C11 C12 1.421(7) . ?
C11 P2 1.799(5) . ?
C12 C17 1.396(7) . ?
C12 C13 1.398(7) . ?
C13 C14 1.363(8) . ?
C13 H13 0.9500 . ?
C14 C15 1.402(9) . ?
C14 H14 0.9500 . ?
C15 C16 1.367(8) . ?
C15 H15 0.9500 . ?
C16 C17 1.378(7) . ?
C16 H16 0.9500 . ?
C17 S2 1.730(5) . ?
C18 C19 1.495(8) . ?
C18 C20 1.508(8) . ?
C18 P1 1.845(5) . ?
C18 H18 1.0000 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C23 1.519(7) . ?
C21 C22 1.528(7) . ?
C21 P1 1.843(5) . ?
C21 H21 1.0000 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C25 1.501(8) . ?
C24 C26 1.522(9) . ?
C24 P2 1.842(5) . ?
C24 H24 1.0000 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28 1.518(7) . ?
C27 C29 1.524(8) . ?
C27 P2 1.856(5) . ?
C27 H27 1.0000 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
Ir1 O1 2.003(4) . ?
Ir1 P2 2.2808(13) . ?
Ir1 P1 2.2911(13) . ?
O1 H1O 0.85(2) . ?
 
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
C10 C1 C2 121.6(4) . . ?
C10 C1 Ir1 120.0(3) . . ?
C2 C1 Ir1 118.2(3) . . ?
C3 C2 C1 122.2(4) . . ?
C3 C2 S1 111.5(4) . . ?
C1 C2 S1 126.2(4) . . ?
C2 C3 C4 114.3(4) . . ?
C2 C3 P1 113.2(4) . . ?
C4 C3 P1 132.1(4) . . ?
C5 C4 C9 117.8(4) . . ?
C5 C4 C3 131.2(5) . . ?
C9 C4 C3 111.0(4) . . ?
C6 C5 C4 120.7(5) . . ?
C6 C5 H5 119.7 . . ?
C4 C5 H5 119.7 . . ?
C5 C6 C7 120.5(5) . . ?
C5 C6 H6 119.7 . . ?
C7 C6 H6 119.7 . . ?
C8 C7 C6 121.2(5) . . ?
C8 C7 H7 119.4 . . ?
C6 C7 H7 119.4 . . ?
C7 C8 C9 117.9(5) . . ?
C7 C8 H8 121.1 . . ?
C9 C8 H8 121.1 . . ?
C8 C9 C4 121.9(5) . . ?
C8 C9 S1 126.3(4) . . ?
C4 C9 S1 111.8(3) . . ?
C11 C10 C1 121.3(4) . . ?
C11 C10 S2 111.3(3) . . ?
C1 C10 S2 127.5(4) . . ?
C10 C11 C12 113.6(4) . . ?
C10 C11 P2 112.7(4) . . ?
C12 C11 P2 133.7(4) . . ?
C17 C12 C13 117.9(5) . . ?
C17 C12 C11 112.0(4) . . ?
C13 C12 C11 130.0(5) . . ?
C14 C13 C12 119.7(5) . . ?
C14 C13 H13 120.1 . . ?
C12 C13 H13 120.1 . . ?
C13 C14 C15 121.3(6) . . ?
C13 C14 H14 119.3 . . ?
C15 C14 H14 119.3 . . ?
C16 C15 C14 119.8(5) . . ?
C16 C15 H15 120.1 . . ?
C14 C15 H15 120.1 . . ?
C15 C16 C17 118.9(5) . . ?
C15 C16 H16 120.6 . . ?
C17 C16 H16 120.6 . . ?
C16 C17 C12 122.4(5) . . ?
C16 C17 S2 126.4(4) . . ?
C12 C17 S2 111.2(4) . . ?
C19 C18 C20 111.2(5) . . ?
C19 C18 P1 111.2(4) . . ?
C20 C18 P1 112.3(4) . . ?
C19 C18 H18 107.3 . . ?
C20 C18 H18 107.3 . . ?
P1 C18 H18 107.3 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C23 C21 C22 109.2(5) . . ?
C23 C21 P1 111.4(3) . . ?
C22 C21 P1 111.8(4) . . ?
C23 C21 H21 108.1 . . ?
C22 C21 H21 108.1 . . ?
P1 C21 H21 108.1 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C25 C24 C26 110.0(5) . . ?
C25 C24 P2 113.2(4) . . ?
C26 C24 P2 109.3(4) . . ?
C25 C24 H24 108.1 . . ?
C26 C24 H24 108.1 . . ?
P2 C24 H24 108.1 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C28 C27 C29 110.9(5) . . ?
C28 C27 P2 110.0(4) . . ?
C29 C27 P2 110.7(4) . . ?
C28 C27 H27 108.4 . . ?
C29 C27 H27 108.4 . . ?
P2 C27 H27 108.4 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C1 Ir1 O1 175.5(2) . . ?
C1 Ir1 P2 84.34(14) . . ?
O1 Ir1 P2 97.71(13) . . ?
C1 Ir1 P1 85.14(14) . . ?
O1 Ir1 P1 93.44(13) . . ?
P2 Ir1 P1 166.07(5) . . ?
Ir1 O1 H1O 111.5(15) . . ?
C3 P1 C21 107.2(2) . . ?
C3 P1 C18 102.0(2) . . ?
C21 P1 C18 104.5(2) . . ?
C3 P1 Ir1 100.98(16) . . ?
C21 P1 Ir1 124.17(18) . . ?
C18 P1 Ir1 115.53(17) . . ?
C11 P2 C24 103.6(2) . . ?
C11 P2 C27 105.1(2) . . ?
C24 P2 C27 104.6(3) . . ?
C11 P2 Ir1 101.70(16) . . ?
C24 P2 Ir1 115.56(19) . . ?
C27 P2 Ir1 123.88(19) . . ?
C9 S1 C2 91.4(2) . . ?
C17 S2 C10 91.9(2) . . ?
 
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
C10 C1 C2 C3 173.6(5) . . . . ?
Ir1 C1 C2 C3 -1.1(6) . . . . ?
C10 C1 C2 S1 -4.7(7) . . . . ?
Ir1 C1 C2 S1 -179.5(3) . . . . ?
C1 C2 C3 C4 -176.8(4) . . . . ?
S1 C2 C3 C4 1.8(6) . . . . ?
C1 C2 C3 P1 -3.0(6) . . . . ?
S1 C2 C3 P1 175.6(2) . . . . ?
C2 C3 C4 C5 177.7(5) . . . . ?
P1 C3 C4 C5 5.4(9) . . . . ?
C2 C3 C4 C9 -1.4(6) . . . . ?
P1 C3 C4 C9 -173.7(4) . . . . ?
C9 C4 C5 C6 0.5(8) . . . . ?
C3 C4 C5 C6 -178.6(5) . . . . ?
C4 C5 C6 C7 -0.7(9) . . . . ?
C5 C6 C7 C8 0.2(9) . . . . ?
C6 C7 C8 C9 0.4(9) . . . . ?
C7 C8 C9 C4 -0.6(8) . . . . ?
C7 C8 C9 S1 178.2(4) . . . . ?
C5 C4 C9 C8 0.1(8) . . . . ?
C3 C4 C9 C8 179.4(5) . . . . ?
C5 C4 C9 S1 -178.9(4) . . . . ?
C3 C4 C9 S1 0.4(5) . . . . ?
C2 C1 C10 C11 -173.9(4) . . . . ?
Ir1 C1 C10 C11 0.8(6) . . . . ?
C2 C1 C10 S2 5.2(7) . . . . ?
Ir1 C1 C10 S2 179.9(3) . . . . ?
C1 C10 C11 C12 178.2(4) . . . . ?
S2 C10 C11 C12 -1.0(6) . . . . ?
C1 C10 C11 P2 -0.5(6) . . . . ?
S2 C10 C11 P2 -179.7(2) . . . . ?
C10 C11 C12 C17 1.0(7) . . . . ?
P2 C11 C12 C17 179.4(4) . . . . ?
C10 C11 C12 C13 179.2(6) . . . . ?
P2 C11 C12 C13 -2.5(10) . . . . ?
C17 C12 C13 C14 -0.5(10) . . . . ?
C11 C12 C13 C14 -178.5(6) . . . . ?
C12 C13 C14 C15 -1.0(12) . . . . ?
C13 C14 C15 C16 1.6(12) . . . . ?
C14 C15 C16 C17 -0.6(10) . . . . ?
C15 C16 C17 C12 -0.9(9) . . . . ?
C15 C16 C17 S2 179.6(5) . . . . ?
C13 C12 C17 C16 1.5(8) . . . . ?
C11 C12 C17 C16 179.9(5) . . . . ?
C13 C12 C17 S2 -178.9(5) . . . . ?
C11 C12 C17 S2 -0.6(6) . . . . ?
C2 C3 P1 C21 136.0(4) . . . . ?
C4 C3 P1 C21 -51.6(5) . . . . ?
C2 C3 P1 C18 -114.6(4) . . . . ?
C4 C3 P1 C18 57.8(5) . . . . ?
C2 C3 P1 Ir1 4.8(4) . . . . ?
C4 C3 P1 Ir1 177.2(4) . . . . ?
C23 C21 P1 C3 -43.7(5) . . . . ?
C22 C21 P1 C3 -166.2(4) . . . . ?
C23 C21 P1 C18 -151.4(4) . . . . ?
C22 C21 P1 C18 86.1(4) . . . . ?
C23 C21 P1 Ir1 73.0(4) . . . . ?
C22 C21 P1 Ir1 -49.4(5) . . . . ?
C19 C18 P1 C3 54.2(5) . . . . ?
C20 C18 P1 C3 179.5(5) . . . . ?
C19 C18 P1 C21 165.7(5) . . . . ?
C20 C18 P1 C21 -69.0(5) . . . . ?
C19 C18 P1 Ir1 -54.3(5) . . . . ?
C20 C18 P1 Ir1 71.0(5) . . . . ?
C10 C11 P2 C24 120.3(4) . . . . ?
C12 C11 P2 C24 -58.1(6) . . . . ?
C10 C11 P2 C27 -130.1(4) . . . . ?
C12 C11 P2 C27 51.5(6) . . . . ?
C10 C11 P2 Ir1 0.1(4) . . . . ?
C12 C11 P2 Ir1 -178.3(5) . . . . ?
C25 C24 P2 C11 175.3(5) . . . . ?
C26 C24 P2 C11 -61.8(5) . . . . ?
C25 C24 P2 C27 65.4(5) . . . . ?
C26 C24 P2 C27 -171.7(4) . . . . ?
C25 C24 P2 Ir1 -74.4(5) . . . . ?
C26 C24 P2 Ir1 48.5(5) . . . . ?
C28 C27 P2 C11 161.1(4) . . . . ?
C29 C27 P2 C11 38.2(5) . . . . ?
C28 C27 P2 C24 -90.1(4) . . . . ?
C29 C27 P2 C24 146.9(4) . . . . ?
C28 C27 P2 Ir1 45.3(5) . . . . ?
C29 C27 P2 Ir1 -77.6(4) . . . . ?
C8 C9 S1 C2 -178.5(5) . . . . ?
C4 C9 S1 C2 0.5(4) . . . . ?
C3 C2 S1 C9 -1.3(4) . . . . ?
C1 C2 S1 C9 177.2(4) . . . . ?
C16 C17 S2 C10 179.5(5) . . . . ?
C12 C17 S2 C10 0.0(4) . . . . ?
C11 C10 S2 C17 0.6(4) . . . . ?
C1 C10 S2 C17 -178.6(4) . . . . ?
 
loop_
 _geom_hbond_atom_site_label_D 
 _geom_hbond_atom_site_label_H 
 _geom_hbond_atom_site_label_A 
 _geom_hbond_distance_DH 
 _geom_hbond_distance_HA 
 _geom_hbond_distance_DA 
 _geom_hbond_angle_DHA 
 _geom_hbond_site_symmetry_A 
C28 H28A O1  0.98 2.65 3.383(7) 132.1 3_666
C21 H21 S2  1.00 3.01 3.991(5) 167.1 4_566
 
_refine_diff_density_max    1.216
_refine_diff_density_min   -0.659
_refine_diff_density_rms    0.107

_shelxl_version_number 2013-4



#===END
 
data_1_OH
 
_audit_creation_method            SHELXL-2013
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety         '2(C29 H36 Ir O2 P2 S2), C7 H8'
_chemical_formula_sum
 'C65 H80 Ir2 O4 P4 S4' 
_chemical_formula_weight          1561.81

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0181   0.0091
 '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'
 'O'  'O'   0.0492   0.0322
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'P'  'P'   0.2955   0.4335
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'S'  'S'   0.3331   0.5567
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Ir'  'Ir'  -4.7710   6.5667
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       triclinic
_space_group_IT_number            2
_space_group_name_H-M_alt         'P -1'
_space_group_name_Hall            '-P 1'
 
_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.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, -z'
 
_cell_length_a                    12.8155(7)
_cell_length_b                    14.1374(8)
_cell_length_c                    19.4358(11)
_cell_angle_alpha                 105.409(2)
_cell_angle_beta                  103.594(2)
_cell_angle_gamma                 93.729(2)
_cell_volume                      3269.0(3)
_cell_formula_units_Z             2
_cell_measurement_temperature     173(2)
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min       ?
_cell_measurement_theta_max       ?
 
_exptl_crystal_description       'plate'
_exptl_crystal_colour            'Orange'
_exptl_crystal_density_meas      '?'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn     1.587          
_exptl_crystal_F_000              1560
_exptl_transmission_factor_min    ?                                             
_exptl_transmission_factor_max    ?                                             
_exptl_crystal_size_max           0.25
_exptl_crystal_size_mid           0.150
_exptl_crystal_size_min           0.110
_exptl_absorpt_coefficient_mu     10.236
_shelx_estimated_absorpt_T_min    0.184
_shelx_estimated_absorpt_T_max    0.399
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.552
_exptl_absorpt_correction_T_max   0.753
_exptl_absorpt_process_details    'Sadabs (Sheldrick, 1996)'
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       173(2)
_diffrn_radiation_wavelength      1.54178
_diffrn_radiation_type            CuK\a
_diffrn_source                    ?                       
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number             40418
_diffrn_reflns_av_unetI/netI      0.0491
_diffrn_reflns_av_R_equivalents   0.0585
_diffrn_reflns_limit_h_min        -15
_diffrn_reflns_limit_h_max        15
_diffrn_reflns_limit_k_min        -16
_diffrn_reflns_limit_k_max        16
_diffrn_reflns_limit_l_min        -23
_diffrn_reflns_limit_l_max        21
_diffrn_reflns_theta_min          2.444
_diffrn_reflns_theta_max          67.493
_diffrn_reflns_theta_full         67.500
_diffrn_measured_fraction_theta_max   0.969
_diffrn_measured_fraction_theta_full  0.969
_diffrn_reflns_Laue_measured_fraction_max    0.969
_diffrn_reflns_Laue_measured_fraction_full   0.969
_diffrn_reflns_point_group_measured_fraction_max   0.969
_diffrn_reflns_point_group_measured_fraction_full  0.969
_reflns_number_total              11415
_reflns_number_gt                 10577
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection      'Bruker APEX2'
_computing_cell_refinement      'Bruker SAINT'
_computing_data_reduction       'Bruker SAINT'  
_computing_structure_solution   'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics   'Bruker SHELXTL'
_computing_publication_material 'LinXTL v.  5.3.8'
 
_refine_special_details
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0505P)²+3.0386P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          11415
_refine_ls_number_parameters      730
_refine_ls_number_restraints      729
_refine_ls_R_factor_all           0.0382
_refine_ls_R_factor_gt            0.0356
_refine_ls_wR_factor_ref          0.0917
_refine_ls_wR_factor_gt           0.0894
_refine_ls_goodness_of_fit_ref    1.031
_refine_ls_restrained_S_all       1.005
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
 
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
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Ir1 Ir 0.51567(2) 0.27853(2) 0.19883(2) 0.02722(6) Uani 1 1 d . U . . .
Ir2 Ir 0.95616(2) 0.10438(2) 0.67338(2) 0.03069(6) Uani 1 1 d . U . . .
S1 S 0.72020(7) 0.10282(7) 0.05010(5) 0.02863(18) Uani 1 1 d . U . . .
S2 S 0.56087(7) -0.04521(6) 0.08177(5) 0.02796(18) Uani 1 1 d . U . . .
S3 S 1.00341(8) 0.38905(7) 0.87174(5) 0.0320(2) Uani 1 1 d . U . . .
S4 S 0.79129(9) 0.38723(8) 0.75519(6) 0.0415(2) Uani 1 1 d . U . . .
P1 P 0.66558(8) 0.37221(7) 0.19208(6) 0.02834(19) Uani 1 1 d . U . . .
P2 P 0.39420(7) 0.15729(7) 0.20839(5) 0.02639(18) Uani 1 1 d . U . . .
P3 P 1.09990(8) 0.11169(7) 0.77383(5) 0.0303(2) Uani 1 1 d . U . . .
P4 P 0.82550(8) 0.13969(7) 0.58364(5) 0.0302(2) Uani 1 1 d . U . . .
O1 O 0.4773(2) 0.2077(2) 0.08568(15) 0.0302(5) Uani 1 1 d . U . . .
O2 O 0.5277(3) 0.3659(2) 0.2989(2) 0.0478(8) Uani 1 1 d . U . . .
O3 O 0.8617(2) 0.1356(2) 0.74740(15) 0.0330(6) Uani 1 1 d . U . . .
O4 O 1.0319(3) 0.0373(3) 0.6004(2) 0.0577(10) Uani 1 1 d . U . . .
C1 C 0.5565(3) 0.1646(3) 0.1212(2) 0.0271(7) Uani 1 1 d . U . . .
C2 C 0.6651(3) 0.1875(3) 0.1092(2) 0.0270(7) Uani 1 1 d . U . . .
C3 C 0.7227(3) 0.2798(3) 0.1331(2) 0.0298(8) Uani 1 1 d . U . . .
C4 C 0.8144(3) 0.2850(3) 0.1027(2) 0.0308(8) Uani 1 1 d . U . . .
C5 C 0.8922(4) 0.3660(3) 0.1117(3) 0.0391(9) Uani 1 1 d . U . . .
H5 H 0.8877 0.4298 0.1417 0.047 Uiso 1 1 calc R U . . .
C6 C 0.9739(4) 0.3525(3) 0.0772(3) 0.0446(10) Uani 1 1 d . U . . .
H6 H 1.0267 0.4071 0.0846 0.053 Uiso 1 1 calc R U . . .
C7 C 0.9811(4) 0.2597(3) 0.0311(3) 0.0404(9) Uani 1 1 d . U . . .
H7 H 1.0380 0.2523 0.0072 0.049 Uiso 1 1 calc R U . . .
C8 C 0.9058(4) 0.1787(3) 0.0204(2) 0.0354(9) Uani 1 1 d . U . . .
H8 H 0.9101 0.1154 -0.0108 0.042 Uiso 1 1 calc R U . . .
C9 C 0.8234(3) 0.1926(3) 0.0566(2) 0.0301(8) Uani 1 1 d . U . . .
C10 C 0.5179(3) 0.0641(3) 0.1255(2) 0.0263(7) Uani 1 1 d . U . . .
C11 C 0.4380(3) 0.0470(3) 0.1573(2) 0.0266(7) Uani 1 1 d . U . . .
C12 C 0.4061(3) -0.0573(3) 0.1468(2) 0.0316(8) Uani 1 1 d . U . . .
C13 C 0.3240(4) -0.1036(3) 0.1673(2) 0.0378(9) Uani 1 1 d . U . . .
H13 H 0.2801 -0.0655 0.1940 0.045 Uiso 1 1 calc R U . . .
C14 C 0.3074(4) -0.2056(3) 0.1485(3) 0.0475(11) Uani 1 1 d . U . . .
H14 H 0.2504 -0.2374 0.1615 0.057 Uiso 1 1 calc R U . . .
C15 C 0.3726(5) -0.2634(3) 0.1105(3) 0.0510(12) Uani 1 1 d . U . . .
H15 H 0.3607 -0.3335 0.0994 0.061 Uiso 1 1 calc R U . . .
C16 C 0.4535(4) -0.2193(3) 0.0892(3) 0.0418(10) Uani 1 1 d . U . . .
H16 H 0.4973 -0.2581 0.0629 0.050 Uiso 1 1 calc R U . . .
C17 C 0.4698(3) -0.1157(3) 0.1073(2) 0.0304(8) Uani 1 1 d . U . . .
C18 C 0.6514(4) 0.4783(3) 0.1527(3) 0.0368(9) Uani 1 1 d . U . . .
H18 H 0.7247 0.5165 0.1632 0.044 Uiso 1 1 calc R U . . .
C19 C 0.6027(4) 0.4422(4) 0.0696(3) 0.0481(11) Uani 1 1 d . U . . .
H19A H 0.5307 0.4047 0.0588 0.072 Uiso 1 1 calc R U . . .
H19B H 0.6496 0.3993 0.0465 0.072 Uiso 1 1 calc R U . . .
H19C H 0.5962 0.4991 0.0498 0.072 Uiso 1 1 calc R U . . .
C20 C 0.5808(5) 0.5448(4) 0.1916(3) 0.0529(12) Uani 1 1 d . U . . .
H20A H 0.5757 0.6038 0.1742 0.079 Uiso 1 1 calc R U . . .
H20B H 0.6132 0.5648 0.2451 0.079 Uiso 1 1 calc R U . . .
H20C H 0.5082 0.5086 0.1804 0.079 Uiso 1 1 calc R U . . .
C21 C 0.7628(4) 0.4208(3) 0.2840(3) 0.0395(9) Uani 1 1 d . U . . .
H21 H 0.7202 0.4566 0.3173 0.047 Uiso 1 1 calc R U . . .
C22 C 0.7987(5) 0.3367(4) 0.3142(3) 0.0556(13) Uani 1 1 d . U . . .
H22A H 0.8459 0.3015 0.2862 0.083 Uiso 1 1 calc R U . . .
H22B H 0.7350 0.2909 0.3095 0.083 Uiso 1 1 calc R U . . .
H22C H 0.8384 0.3633 0.3664 0.083 Uiso 1 1 calc R U . . .
C23 C 0.8601(5) 0.4967(4) 0.2926(3) 0.0637(16) Uani 1 1 d . U . . .
H23A H 0.9062 0.5143 0.3434 0.096 Uiso 1 1 calc R U . . .
H23B H 0.8340 0.5563 0.2820 0.096 Uiso 1 1 calc R U . . .
H23C H 0.9021 0.4679 0.2580 0.096 Uiso 1 1 calc R U . . .
C24 C 0.2465(3) 0.1507(3) 0.1699(2) 0.0335(8) Uani 1 1 d . U . . .
H24 H 0.2077 0.1089 0.1928 0.040 Uiso 1 1 calc R U . . .
C25 C 0.2133(4) 0.2548(4) 0.1890(3) 0.0470(11) Uani 1 1 d . U . . .
H25A H 0.2404 0.2930 0.1599 0.070 Uiso 1 1 calc R U . . .
H25B H 0.2441 0.2881 0.2418 0.070 Uiso 1 1 calc R U . . .
H25C H 0.1341 0.2498 0.1773 0.070 Uiso 1 1 calc R U . . .
C26 C 0.2152(3) 0.1033(3) 0.0863(2) 0.0381(9) Uani 1 1 d . U . . .
H26A H 0.1378 0.1048 0.0663 0.057 Uiso 1 1 calc R U . . .
H26B H 0.2299 0.0344 0.0754 0.057 Uiso 1 1 calc R U . . .
H26C H 0.2576 0.1401 0.0636 0.057 Uiso 1 1 calc R U . . .
C27 C 0.4072(4) 0.1368(3) 0.3003(2) 0.0357(9) Uani 1 1 d . U . . .
H27 H 0.3715 0.0679 0.2913 0.043 Uiso 1 1 calc R U . . .
C28 C 0.3507(4) 0.2062(4) 0.3491(3) 0.0463(11) Uani 1 1 d . U . . .
H28A H 0.3647 0.1942 0.3977 0.069 Uiso 1 1 calc R U . . .
H28B H 0.2725 0.1942 0.3260 0.069 Uiso 1 1 calc R U . . .
H28C H 0.3784 0.2750 0.3551 0.069 Uiso 1 1 calc R U . . .
C29 C 0.5269(4) 0.1405(4) 0.3386(3) 0.0471(11) Uani 1 1 d . U . . .
H29A H 0.5641 0.2079 0.3506 0.071 Uiso 1 1 calc R U . . .
H29B H 0.5602 0.0945 0.3056 0.071 Uiso 1 1 calc R U . . .
H29C H 0.5330 0.1216 0.3843 0.071 Uiso 1 1 calc R U . . .
C30 C 0.9115(3) 0.2223(3) 0.7457(2) 0.0305(8) Uani 1 1 d . U . . .
C31 C 1.0020(3) 0.2725(3) 0.8122(2) 0.0303(8) Uani 1 1 d . U . . .
C32 C 1.0898(3) 0.2284(3) 0.8372(2) 0.0294(7) Uani 1 1 d . U . . .
C33 C 1.1584(3) 0.2866(3) 0.9079(2) 0.0295(7) Uani 1 1 d . U . . .
C34 C 1.2508(3) 0.2645(3) 0.9540(2) 0.0329(8) Uani 1 1 d . U . . .
H34 H 1.2781 0.2036 0.9387 0.040 Uiso 1 1 calc R U . . .
C35 C 1.3007(3) 0.3318(3) 1.0213(2) 0.0369(9) Uani 1 1 d . U . . .
H35 H 1.3613 0.3159 1.0529 0.044 Uiso 1 1 calc R U . . .
C36 C 1.2644(4) 0.4231(3) 1.0442(2) 0.0375(9) Uani 1 1 d . U . . .
H36 H 1.3013 0.4687 1.0906 0.045 Uiso 1 1 calc R U . . .
C37 C 1.1746(3) 0.4480(3) 1.0000(2) 0.0338(8) Uani 1 1 d . U . . .
H37 H 1.1498 0.5102 1.0149 0.041 Uiso 1 1 calc R U . . .
C38 C 1.1227(3) 0.3785(3) 0.9330(2) 0.0298(7) Uani 1 1 d . U . . .
C39 C 0.8354(3) 0.2806(3) 0.7083(2) 0.0320(8) Uani 1 1 d . U . . .
C40 C 0.7792(3) 0.2475(3) 0.6353(2) 0.0322(8) Uani 1 1 d . U . . .
C41 C 0.6945(4) 0.3056(3) 0.6154(2) 0.0385(9) Uani 1 1 d . U . . .
C42 C 0.6178(4) 0.2941(4) 0.5481(3) 0.0502(12) Uani 1 1 d . U . . .
H42 H 0.6161 0.2404 0.5062 0.060 Uiso 1 1 calc R U . . .
C43 C 0.5449(5) 0.3610(5) 0.5428(3) 0.0662(18) Uani 1 1 d . U . . .
H43 H 0.4927 0.3524 0.4972 0.079 Uiso 1 1 calc R U . . .
C44 C 0.5463(5) 0.4408(5) 0.6032(3) 0.0692(19) Uani 1 1 d . U . . .
H44 H 0.4961 0.4867 0.5983 0.083 Uiso 1 1 calc R U . . .
C45 C 0.6200(5) 0.4536(4) 0.6701(3) 0.0571(14) Uani 1 1 d . U . . .
H45 H 0.6207 0.5075 0.7117 0.069 Uiso 1 1 calc R U . . .
C46 C 0.6934(4) 0.3861(4) 0.6757(3) 0.0432(10) Uani 1 1 d . U . . .
C47 C 1.1013(4) 0.0169(3) 0.8239(2) 0.0368(9) Uani 1 1 d . U . . .
H47 H 1.1775 0.0178 0.8523 0.044 Uiso 1 1 calc R U . . .
C48 C 1.0618(6) -0.0857(4) 0.7674(3) 0.0607(15) Uani 1 1 d . U . . .
H48A H 1.0652 -0.1365 0.7934 0.091 Uiso 1 1 calc R U . . .
H48B H 1.1081 -0.0983 0.7332 0.091 Uiso 1 1 calc R U . . .
H48C H 0.9868 -0.0877 0.7395 0.091 Uiso 1 1 calc R U . . .
C49 C 1.0309(4) 0.0374(3) 0.8779(3) 0.0453(10) Uani 1 1 d . U . . .
H49A H 0.9582 0.0455 0.8519 0.068 Uiso 1 1 calc R U . . .
H49B H 1.0632 0.0982 0.9179 0.068 Uiso 1 1 calc R U . . .
H49C H 1.0261 -0.0182 0.8987 0.068 Uiso 1 1 calc R U . . .
C50 C 1.2392(4) 0.1309(4) 0.7638(3) 0.0404(9) Uani 1 1 d . U . . .
H50 H 1.2892 0.1564 0.8147 0.048 Uiso 1 1 calc R U . . .
C51 C 1.2760(5) 0.0362(4) 0.7248(3) 0.0578(14) Uani 1 1 d . U . . .
H51A H 1.2266 0.0078 0.6754 0.087 Uiso 1 1 calc R U . . .
H51B H 1.2757 -0.0113 0.7535 0.087 Uiso 1 1 calc R U . . .
H51C H 1.3495 0.0509 0.7204 0.087 Uiso 1 1 calc R U . . .
C52 C 1.2470(5) 0.2104(4) 0.7249(4) 0.0579(13) Uani 1 1 d . U . . .
H52A H 1.3232 0.2302 0.7284 0.087 Uiso 1 1 calc R U . . .
H52B H 1.2161 0.2680 0.7486 0.087 Uiso 1 1 calc R U . . .
H52C H 1.2068 0.1841 0.6728 0.087 Uiso 1 1 calc R U . . .
C53 C 0.7031(4) 0.0501(3) 0.5310(3) 0.0434(10) Uani 1 1 d . U . . .
H53 H 0.6575 0.0780 0.4940 0.052 Uiso 1 1 calc R U . . .
C54 C 0.7377(6) -0.0457(4) 0.4904(3) 0.0664(16) Uani 1 1 d . U . . .
H54A H 0.7822 -0.0736 0.5265 0.100 Uiso 1 1 calc R U . . .
H54B H 0.7799 -0.0317 0.4574 0.100 Uiso 1 1 calc R U . . .
H54C H 0.6732 -0.0933 0.4613 0.100 Uiso 1 1 calc R U . . .
C55 C 0.6385(5) 0.0327(5) 0.5844(4) 0.0689(16) Uani 1 1 d . U . . .
H55A H 0.5771 -0.0194 0.5576 0.103 Uiso 1 1 calc R U . . .
H55B H 0.6114 0.0941 0.6057 0.103 Uiso 1 1 calc R U . . .
H55C H 0.6853 0.0124 0.6240 0.103 Uiso 1 1 calc R U . . .
C56 C 0.8866(4) 0.1783(4) 0.5166(3) 0.0426(10) Uani 1 1 d . U . . .
H56 H 0.9282 0.1244 0.4973 0.051 Uiso 1 1 calc R U . . .
C57 C 0.8087(5) 0.1942(4) 0.4493(3) 0.0529(12) Uani 1 1 d . U . . .
H57A H 0.7766 0.2548 0.4647 0.079 Uiso 1 1 calc R U . . .
H57B H 0.7512 0.1375 0.4272 0.079 Uiso 1 1 calc R U . . .
H57C H 0.8482 0.2004 0.4129 0.079 Uiso 1 1 calc R U . . .
C58 C 0.9690(5) 0.2701(5) 0.5582(4) 0.0648(16) Uani 1 1 d . U . . .
H58A H 1.0093 0.2864 0.5249 0.097 Uiso 1 1 calc R U . . .
H58B H 1.0195 0.2572 0.6001 0.097 Uiso 1 1 calc R U . . .
H58C H 0.9313 0.3258 0.5765 0.097 Uiso 1 1 calc R U . . .
C59 C 0.7379(8) 0.6817(6) 0.4337(5) 0.097(3) Uani 1 1 d . U . . .
H59A H 0.7388 0.6308 0.3885 0.145 Uiso 1 1 calc R U . . .
H59B H 0.7830 0.7426 0.4378 0.145 Uiso 1 1 calc R U . . .
H59C H 0.6633 0.6949 0.4319 0.145 Uiso 1 1 calc R U . . .
C60 C 0.7809(6) 0.6464(5) 0.4986(4) 0.0683(15) Uani 1 1 d . U . . .
C61 C 0.7555(6) 0.5506(6) 0.4962(5) 0.0811(19) Uani 1 1 d . U . . .
H61 H 0.7091 0.5067 0.4521 0.097 Uiso 1 1 calc R U . . .
C62 C 0.7948(7) 0.5144(7) 0.5557(5) 0.094(2) Uani 1 1 d . U . . .
H62 H 0.7750 0.4474 0.5531 0.113 Uiso 1 1 calc R U . . .
C63 C 0.8653(7) 0.5808(7) 0.6205(5) 0.092(2) Uani 1 1 d . U . . .
H63 H 0.8944 0.5577 0.6617 0.110 Uiso 1 1 calc R U . . .
C64 C 0.8914(6) 0.6752(7) 0.6242(5) 0.0838(19) Uani 1 1 d . U . . .
H64 H 0.9376 0.7192 0.6683 0.101 Uiso 1 1 calc R U . . .
C65 C 0.8512(6) 0.7092(6) 0.5639(4) 0.0758(17) Uani 1 1 d . U . . .
H65 H 0.8716 0.7763 0.5668 0.091 Uiso 1 1 calc R U . . .
 
 
_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_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
Ir1 O2 1.971(3) . ?
Ir1 C1 2.081(4) . ?
Ir1 O1 2.083(3) . ?
Ir1 P1 2.3112(10) . ?
Ir1 P2 2.3139(9) . ?
Ir2 O4 1.977(3) . ?
Ir2 O3 2.069(3) . ?
Ir2 C30 2.083(4) . ?
Ir2 P4 2.3008(10) . ?
Ir2 P3 2.3223(10) . ?
S1 C9 1.730(4) . ?
S1 C2 1.735(4) . ?
S2 C17 1.727(4) . ?
S2 C10 1.745(4) . ?
S3 C31 1.740(4) . ?
S3 C38 1.745(4) . ?
S4 C46 1.741(5) . ?
S4 C39 1.745(4) . ?
P1 C3 1.811(4) . ?
P1 C21 1.846(5) . ?
P1 C18 1.858(4) . ?
P2 C11 1.813(4) . ?
P2 C24 1.851(4) . ?
P2 C27 1.856(4) . ?
P3 C32 1.811(4) . ?
P3 C50 1.851(5) . ?
P3 C47 1.852(4) . ?
P4 C40 1.808(4) . ?
P4 C53 1.847(5) . ?
P4 C56 1.848(5) . ?
O1 C1 1.361(5) . ?
O3 C30 1.357(5) . ?
C1 C2 1.495(5) . ?
C1 C10 1.504(5) . ?
C2 C3 1.362(5) . ?
C3 C4 1.439(6) . ?
C4 C9 1.404(6) . ?
C4 C5 1.413(6) . ?
C5 C6 1.367(7) . ?
C5 H5 0.9500 . ?
C6 C7 1.401(7) . ?
C6 H6 0.9500 . ?
C7 C8 1.386(6) . ?
C7 H7 0.9500 . ?
C8 C9 1.397(6) . ?
C8 H8 0.9500 . ?
C10 C11 1.354(6) . ?
C11 C12 1.451(5) . ?
C12 C13 1.393(6) . ?
C12 C17 1.409(6) . ?
C13 C14 1.378(6) . ?
C13 H13 0.9500 . ?
C14 C15 1.404(7) . ?
C14 H14 0.9500 . ?
C15 C16 1.376(7) . ?
C15 H15 0.9500 . ?
C16 C17 1.402(6) . ?
C16 H16 0.9500 . ?
C18 C19 1.519(7) . ?
C18 C20 1.525(7) . ?
C18 H18 1.0000 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.511(7) . ?
C21 C23 1.539(7) . ?
C21 H21 1.0000 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C26 1.526(6) . ?
C24 C25 1.533(6) . ?
C24 H24 1.0000 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28 1.520(6) . ?
C27 C29 1.530(6) . ?
C27 H27 1.0000 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 C31 1.490(6) . ?
C30 C39 1.499(5) . ?
C31 C32 1.373(6) . ?
C32 C33 1.440(6) . ?
C33 C38 1.408(6) . ?
C33 C34 1.416(6) . ?
C34 C35 1.375(6) . ?
C34 H34 0.9500 . ?
C35 C36 1.397(6) . ?
C35 H35 0.9500 . ?
C36 C37 1.391(6) . ?
C36 H36 0.9500 . ?
C37 C38 1.389(6) . ?
C37 H37 0.9500 . ?
C39 C40 1.369(6) . ?
C40 C41 1.445(6) . ?
C41 C42 1.403(6) . ?
C41 C46 1.403(6) . ?
C42 C43 1.378(7) . ?
C42 H42 0.9500 . ?
C43 C44 1.391(8) . ?
C43 H43 0.9500 . ?
C44 C45 1.374(7) . ?
C44 H44 0.9500 . ?
C45 C46 1.391(6) . ?
C45 H45 0.9500 . ?
C47 C49 1.522(7) . ?
C47 C48 1.538(6) . ?
C47 H47 1.0000 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C50 C51 1.516(7) . ?
C50 C52 1.522(7) . ?
C50 H50 1.0000 . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 C54 1.525(7) . ?
C53 C55 1.528(8) . ?
C53 H53 1.0000 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C56 C58 1.522(8) . ?
C56 C57 1.525(6) . ?
C56 H56 1.0000 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C59 C60 1.479(10) . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C60 C61 1.358(10) . ?
C60 C65 1.404(10) . ?
C61 C62 1.388(11) . ?
C61 H61 0.9500 . ?
C62 C63 1.418(12) . ?
C62 H62 0.9500 . ?
C63 C64 1.334(12) . ?
C63 H63 0.9500 . ?
C64 C65 1.384(11) . ?
C64 H64 0.9500 . ?
C65 H65 0.9500 . ?
 
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
O2 Ir1 C1 155.16(15) . . ?
O2 Ir1 O1 166.65(13) . . ?
C1 Ir1 O1 38.14(12) . . ?
O2 Ir1 P1 90.07(11) . . ?
C1 Ir1 P1 85.26(11) . . ?
O1 Ir1 P1 91.17(8) . . ?
O2 Ir1 P2 94.07(10) . . ?
C1 Ir1 P2 85.48(11) . . ?
O1 Ir1 P2 87.84(8) . . ?
P1 Ir1 P2 166.22(3) . . ?
O4 Ir2 O3 164.48(16) . . ?
O4 Ir2 C30 157.35(18) . . ?
O3 Ir2 C30 38.15(14) . . ?
O4 Ir2 P4 92.14(11) . . ?
O3 Ir2 P4 91.09(8) . . ?
C30 Ir2 P4 84.66(11) . . ?
O4 Ir2 P3 93.42(11) . . ?
O3 Ir2 P3 87.09(8) . . ?
C30 Ir2 P3 85.08(11) . . ?
P4 Ir2 P3 165.55(4) . . ?
C9 S1 C2 91.49(19) . . ?
C17 S2 C10 91.43(19) . . ?
C31 S3 C38 91.91(19) . . ?
C46 S4 C39 91.6(2) . . ?
C3 P1 C21 109.3(2) . . ?
C3 P1 C18 107.8(2) . . ?
C21 P1 C18 106.1(2) . . ?
C3 P1 Ir1 101.38(13) . . ?
C21 P1 Ir1 110.61(16) . . ?
C18 P1 Ir1 121.27(15) . . ?
C11 P2 C24 108.08(18) . . ?
C11 P2 C27 102.58(18) . . ?
C24 P2 C27 104.32(19) . . ?
C11 P2 Ir1 100.38(13) . . ?
C24 P2 Ir1 121.21(14) . . ?
C27 P2 Ir1 118.26(14) . . ?
C32 P3 C50 102.7(2) . . ?
C32 P3 C47 107.19(19) . . ?
C50 P3 C47 105.4(2) . . ?
C32 P3 Ir2 100.64(13) . . ?
C50 P3 Ir2 118.07(15) . . ?
C47 P3 Ir2 120.68(15) . . ?
C40 P4 C53 106.4(2) . . ?
C40 P4 C56 107.1(2) . . ?
C53 P4 C56 107.9(2) . . ?
C40 P4 Ir2 102.71(13) . . ?
C53 P4 Ir2 121.08(15) . . ?
C56 P4 Ir2 110.69(16) . . ?
C1 O1 Ir1 70.9(2) . . ?
C30 O3 Ir2 71.5(2) . . ?
O1 C1 C2 113.8(3) . . ?
O1 C1 C10 113.9(3) . . ?
C2 C1 C10 121.6(3) . . ?
O1 C1 Ir1 71.0(2) . . ?
C2 C1 Ir1 113.6(3) . . ?
C10 C1 Ir1 112.2(3) . . ?
C3 C2 C1 124.0(3) . . ?
C3 C2 S1 112.6(3) . . ?
C1 C2 S1 122.6(3) . . ?
C2 C3 C4 112.7(4) . . ?
C2 C3 P1 114.4(3) . . ?
C4 C3 P1 132.9(3) . . ?
C9 C4 C5 117.7(4) . . ?
C9 C4 C3 111.6(3) . . ?
C5 C4 C3 130.7(4) . . ?
C6 C5 C4 120.1(4) . . ?
C6 C5 H5 119.9 . . ?
C4 C5 H5 119.9 . . ?
C5 C6 C7 121.3(4) . . ?
C5 C6 H6 119.4 . . ?
C7 C6 H6 119.4 . . ?
C8 C7 C6 120.3(4) . . ?
C8 C7 H7 119.8 . . ?
C6 C7 H7 119.8 . . ?
C7 C8 C9 118.1(4) . . ?
C7 C8 H8 120.9 . . ?
C9 C8 H8 120.9 . . ?
C8 C9 C4 122.4(4) . . ?
C8 C9 S1 126.0(3) . . ?
C4 C9 S1 111.6(3) . . ?
C11 C10 C1 123.7(3) . . ?
C11 C10 S2 112.2(3) . . ?
C1 C10 S2 123.8(3) . . ?
C10 C11 C12 113.6(3) . . ?
C10 C11 P2 114.9(3) . . ?
C12 C11 P2 131.5(3) . . ?
C13 C12 C17 119.3(4) . . ?
C13 C12 C11 130.2(4) . . ?
C17 C12 C11 110.5(4) . . ?
C14 C13 C12 119.1(4) . . ?
C14 C13 H13 120.5 . . ?
C12 C13 H13 120.5 . . ?
C13 C14 C15 121.5(4) . . ?
C13 C14 H14 119.2 . . ?
C15 C14 H14 119.2 . . ?
C16 C15 C14 120.4(4) . . ?
C16 C15 H15 119.8 . . ?
C14 C15 H15 119.8 . . ?
C15 C16 C17 118.3(4) . . ?
C15 C16 H16 120.8 . . ?
C17 C16 H16 120.8 . . ?
C16 C17 C12 121.4(4) . . ?
C16 C17 S2 126.2(3) . . ?
C12 C17 S2 112.3(3) . . ?
C19 C18 C20 111.7(4) . . ?
C19 C18 P1 110.7(3) . . ?
C20 C18 P1 107.6(3) . . ?
C19 C18 H18 109.0 . . ?
C20 C18 H18 109.0 . . ?
P1 C18 H18 109.0 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 C23 111.3(4) . . ?
C22 C21 P1 110.4(3) . . ?
C23 C21 P1 118.0(4) . . ?
C22 C21 H21 105.4 . . ?
C23 C21 H21 105.4 . . ?
P1 C21 H21 105.4 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C26 C24 C25 110.6(4) . . ?
C26 C24 P2 110.4(3) . . ?
C25 C24 P2 109.8(3) . . ?
C26 C24 H24 108.6 . . ?
C25 C24 H24 108.6 . . ?
P2 C24 H24 108.6 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C28 C27 C29 112.0(4) . . ?
C28 C27 P2 113.8(3) . . ?
C29 C27 P2 109.7(3) . . ?
C28 C27 H27 107.0 . . ?
C29 C27 H27 107.0 . . ?
P2 C27 H27 107.0 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
O3 C30 C31 114.7(3) . . ?
O3 C30 C39 113.2(3) . . ?
C31 C30 C39 121.1(3) . . ?
O3 C30 Ir2 70.4(2) . . ?
C31 C30 Ir2 112.5(3) . . ?
C39 C30 Ir2 114.3(3) . . ?
C32 C31 C30 123.7(4) . . ?
C32 C31 S3 111.9(3) . . ?
C30 C31 S3 124.1(3) . . ?
C31 C32 C33 113.2(3) . . ?
C31 C32 P3 114.2(3) . . ?
C33 C32 P3 132.6(3) . . ?
C38 C33 C34 117.8(4) . . ?
C38 C33 C32 111.8(3) . . ?
C34 C33 C32 130.4(4) . . ?
C35 C34 C33 119.4(4) . . ?
C35 C34 H34 120.3 . . ?
C33 C34 H34 120.3 . . ?
C34 C35 C36 121.5(4) . . ?
C34 C35 H35 119.2 . . ?
C36 C35 H35 119.2 . . ?
C37 C36 C35 120.8(4) . . ?
C37 C36 H36 119.6 . . ?
C35 C36 H36 119.6 . . ?
C38 C37 C36 117.5(4) . . ?
C38 C37 H37 121.3 . . ?
C36 C37 H37 121.3 . . ?
C37 C38 C33 123.1(4) . . ?
C37 C38 S3 125.8(3) . . ?
C33 C38 S3 111.1(3) . . ?
C40 C39 C30 123.4(4) . . ?
C40 C39 S4 111.9(3) . . ?
C30 C39 S4 123.9(3) . . ?
C39 C40 C41 113.4(4) . . ?
C39 C40 P4 113.5(3) . . ?
C41 C40 P4 133.2(3) . . ?
C42 C41 C46 117.9(4) . . ?
C42 C41 C40 130.9(4) . . ?
C46 C41 C40 111.3(4) . . ?
C43 C42 C41 119.9(5) . . ?
C43 C42 H42 120.1 . . ?
C41 C42 H42 120.1 . . ?
C42 C43 C44 121.1(5) . . ?
C42 C43 H43 119.4 . . ?
C44 C43 H43 119.4 . . ?
C45 C44 C43 120.3(5) . . ?
C45 C44 H44 119.8 . . ?
C43 C44 H44 119.8 . . ?
C44 C45 C46 118.7(5) . . ?
C44 C45 H45 120.6 . . ?
C46 C45 H45 120.6 . . ?
C45 C46 C41 122.1(4) . . ?
C45 C46 S4 126.1(4) . . ?
C41 C46 S4 111.8(3) . . ?
C49 C47 C48 110.2(4) . . ?
C49 C47 P3 111.6(3) . . ?
C48 C47 P3 109.0(3) . . ?
C49 C47 H47 108.6 . . ?
C48 C47 H47 108.6 . . ?
P3 C47 H47 108.6 . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C47 C49 H49A 109.5 . . ?
C47 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C47 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C51 C50 C52 111.6(4) . . ?
C51 C50 P3 113.0(4) . . ?
C52 C50 P3 109.3(3) . . ?
C51 C50 H50 107.5 . . ?
C52 C50 H50 107.5 . . ?
P3 C50 H50 107.5 . . ?
C50 C51 H51A 109.5 . . ?
C50 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C50 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C50 C52 H52A 109.5 . . ?
C50 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C50 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C54 C53 C55 111.6(5) . . ?
C54 C53 P4 108.8(4) . . ?
C55 C53 P4 109.1(4) . . ?
C54 C53 H53 109.1 . . ?
C55 C53 H53 109.1 . . ?
P4 C53 H53 109.1 . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C53 C55 H55A 109.5 . . ?
C53 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C53 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C58 C56 C57 111.1(4) . . ?
C58 C56 P4 108.3(3) . . ?
C57 C56 P4 116.8(4) . . ?
C58 C56 H56 106.7 . . ?
C57 C56 H56 106.7 . . ?
P4 C56 H56 106.7 . . ?
C56 C57 H57A 109.5 . . ?
C56 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
C56 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C56 C58 H58A 109.5 . . ?
C56 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
C56 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C60 C59 H59A 109.5 . . ?
C60 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
C60 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C61 C60 C65 117.6(7) . . ?
C61 C60 C59 120.7(7) . . ?
C65 C60 C59 121.7(7) . . ?
C60 C61 C62 122.4(8) . . ?
C60 C61 H61 118.8 . . ?
C62 C61 H61 118.8 . . ?
C61 C62 C63 117.9(8) . . ?
C61 C62 H62 121.1 . . ?
C63 C62 H62 121.1 . . ?
C64 C63 C62 120.7(9) . . ?
C64 C63 H63 119.6 . . ?
C62 C63 H63 119.6 . . ?
C63 C64 C65 120.2(8) . . ?
C63 C64 H64 119.9 . . ?
C65 C64 H64 119.9 . . ?
C64 C65 C60 121.1(8) . . ?
C64 C65 H65 119.4 . . ?
C60 C65 H65 119.4 . . ?
 
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
Ir1 O1 C1 C2 -108.1(3) . . . . ?
Ir1 O1 C1 C10 106.5(3) . . . . ?
O1 C1 C2 C3 65.0(5) . . . . ?
C10 C1 C2 C3 -152.7(4) . . . . ?
Ir1 C1 C2 C3 -13.8(5) . . . . ?
O1 C1 C2 S1 -103.9(3) . . . . ?
C10 C1 C2 S1 38.4(5) . . . . ?
Ir1 C1 C2 S1 177.33(19) . . . . ?
C9 S1 C2 C3 -0.2(3) . . . . ?
C9 S1 C2 C1 169.8(3) . . . . ?
C1 C2 C3 C4 -169.1(3) . . . . ?
S1 C2 C3 C4 0.8(4) . . . . ?
C1 C2 C3 P1 7.8(5) . . . . ?
S1 C2 C3 P1 177.69(19) . . . . ?
C21 P1 C3 C2 118.0(3) . . . . ?
C18 P1 C3 C2 -127.2(3) . . . . ?
Ir1 P1 C3 C2 1.2(3) . . . . ?
C21 P1 C3 C4 -65.9(4) . . . . ?
C18 P1 C3 C4 49.0(4) . . . . ?
Ir1 P1 C3 C4 177.3(4) . . . . ?
C2 C3 C4 C9 -1.0(5) . . . . ?
P1 C3 C4 C9 -177.2(3) . . . . ?
C2 C3 C4 C5 178.2(4) . . . . ?
P1 C3 C4 C5 2.0(7) . . . . ?
C9 C4 C5 C6 -1.3(7) . . . . ?
C3 C4 C5 C6 179.5(4) . . . . ?
C4 C5 C6 C7 1.6(8) . . . . ?
C5 C6 C7 C8 -0.9(8) . . . . ?
C6 C7 C8 C9 0.0(7) . . . . ?
C7 C8 C9 C4 0.2(6) . . . . ?
C7 C8 C9 S1 179.0(3) . . . . ?
C5 C4 C9 C8 0.4(6) . . . . ?
C3 C4 C9 C8 179.8(4) . . . . ?
C5 C4 C9 S1 -178.5(3) . . . . ?
C3 C4 C9 S1 0.8(4) . . . . ?
C2 S1 C9 C8 -179.3(4) . . . . ?
C2 S1 C9 C4 -0.3(3) . . . . ?
O1 C1 C10 C11 -58.2(5) . . . . ?
C2 C1 C10 C11 159.5(4) . . . . ?
Ir1 C1 C10 C11 20.1(5) . . . . ?
O1 C1 C10 S2 114.9(3) . . . . ?
C2 C1 C10 S2 -27.4(5) . . . . ?
Ir1 C1 C10 S2 -166.83(19) . . . . ?
C17 S2 C10 C11 -0.3(3) . . . . ?
C17 S2 C10 C1 -174.1(3) . . . . ?
C1 C10 C11 C12 172.9(3) . . . . ?
S2 C10 C11 C12 -0.9(4) . . . . ?
C1 C10 C11 P2 -9.5(5) . . . . ?
S2 C10 C11 P2 176.66(18) . . . . ?
C24 P2 C11 C10 123.6(3) . . . . ?
C27 P2 C11 C10 -126.6(3) . . . . ?
Ir1 P2 C11 C10 -4.3(3) . . . . ?
C24 P2 C11 C12 -59.5(4) . . . . ?
C27 P2 C11 C12 50.4(4) . . . . ?
Ir1 P2 C11 C12 172.7(4) . . . . ?
C10 C11 C12 C13 -176.0(4) . . . . ?
P2 C11 C12 C13 7.1(7) . . . . ?
C10 C11 C12 C17 1.9(5) . . . . ?
P2 C11 C12 C17 -175.1(3) . . . . ?
C17 C12 C13 C14 0.1(7) . . . . ?
C11 C12 C13 C14 177.7(5) . . . . ?
C12 C13 C14 C15 1.3(8) . . . . ?
C13 C14 C15 C16 -1.8(9) . . . . ?
C14 C15 C16 C17 0.8(8) . . . . ?
C15 C16 C17 C12 0.6(7) . . . . ?
C15 C16 C17 S2 -176.1(4) . . . . ?
C13 C12 C17 C16 -1.1(6) . . . . ?
C11 C12 C17 C16 -179.1(4) . . . . ?
C13 C12 C17 S2 176.1(3) . . . . ?
C11 C12 C17 S2 -2.0(4) . . . . ?
C10 S2 C17 C16 178.3(4) . . . . ?
C10 S2 C17 C12 1.4(3) . . . . ?
C3 P1 C18 C19 45.3(4) . . . . ?
C21 P1 C18 C19 162.2(3) . . . . ?
Ir1 P1 C18 C19 -70.7(4) . . . . ?
C3 P1 C18 C20 167.5(3) . . . . ?
C21 P1 C18 C20 -75.6(4) . . . . ?
Ir1 P1 C18 C20 51.6(4) . . . . ?
C3 P1 C21 C22 -52.0(4) . . . . ?
C18 P1 C21 C22 -167.9(4) . . . . ?
Ir1 P1 C21 C22 58.8(4) . . . . ?
C3 P1 C21 C23 77.6(4) . . . . ?
C18 P1 C21 C23 -38.4(5) . . . . ?
Ir1 P1 C21 C23 -171.6(4) . . . . ?
C11 P2 C24 C26 -36.2(3) . . . . ?
C27 P2 C24 C26 -144.9(3) . . . . ?
Ir1 P2 C24 C26 78.6(3) . . . . ?
C11 P2 C24 C25 -158.5(3) . . . . ?
C27 P2 C24 C25 92.8(3) . . . . ?
Ir1 P2 C24 C25 -43.7(4) . . . . ?
C11 P2 C27 C28 -166.2(3) . . . . ?
C24 P2 C27 C28 -53.6(4) . . . . ?
Ir1 P2 C27 C28 84.5(4) . . . . ?
C11 P2 C27 C29 67.4(3) . . . . ?
C24 P2 C27 C29 -179.9(3) . . . . ?
Ir1 P2 C27 C29 -41.8(4) . . . . ?
Ir2 O3 C30 C31 -106.4(3) . . . . ?
Ir2 O3 C30 C39 108.9(3) . . . . ?
O3 C30 C31 C32 56.0(5) . . . . ?
C39 C30 C31 C32 -162.3(4) . . . . ?
Ir2 C30 C31 C32 -21.8(5) . . . . ?
O3 C30 C31 S3 -118.0(4) . . . . ?
C39 C30 C31 S3 23.7(6) . . . . ?
Ir2 C30 C31 S3 164.2(2) . . . . ?
C38 S3 C31 C32 -1.2(3) . . . . ?
C38 S3 C31 C30 173.4(4) . . . . ?
C30 C31 C32 C33 -171.8(4) . . . . ?
S3 C31 C32 C33 2.9(5) . . . . ?
C30 C31 C32 P3 10.6(5) . . . . ?
S3 C31 C32 P3 -174.8(2) . . . . ?
C50 P3 C32 C31 126.6(3) . . . . ?
C47 P3 C32 C31 -122.6(3) . . . . ?
Ir2 P3 C32 C31 4.4(3) . . . . ?
C50 P3 C32 C33 -50.5(4) . . . . ?
C47 P3 C32 C33 60.3(4) . . . . ?
Ir2 P3 C32 C33 -172.7(4) . . . . ?
C31 C32 C33 C38 -3.5(5) . . . . ?
P3 C32 C33 C38 173.6(3) . . . . ?
C31 C32 C33 C34 175.1(4) . . . . ?
P3 C32 C33 C34 -7.9(7) . . . . ?
C38 C33 C34 C35 1.0(6) . . . . ?
C32 C33 C34 C35 -177.5(4) . . . . ?
C33 C34 C35 C36 -2.0(7) . . . . ?
C34 C35 C36 C37 1.2(7) . . . . ?
C35 C36 C37 C38 0.6(7) . . . . ?
C36 C37 C38 C33 -1.7(6) . . . . ?
C36 C37 C38 S3 175.0(3) . . . . ?
C34 C33 C38 C37 0.9(6) . . . . ?
C32 C33 C38 C37 179.7(4) . . . . ?
C34 C33 C38 S3 -176.2(3) . . . . ?
C32 C33 C38 S3 2.5(4) . . . . ?
C31 S3 C38 C37 -177.8(4) . . . . ?
C31 S3 C38 C33 -0.8(3) . . . . ?
O3 C30 C39 C40 -63.1(6) . . . . ?
C31 C30 C39 C40 154.7(4) . . . . ?
Ir2 C30 C39 C40 14.9(6) . . . . ?
O3 C30 C39 S4 105.9(4) . . . . ?
C31 C30 C39 S4 -36.3(6) . . . . ?
Ir2 C30 C39 S4 -176.1(2) . . . . ?
C46 S4 C39 C40 1.2(4) . . . . ?
C46 S4 C39 C30 -168.9(4) . . . . ?
C30 C39 C40 C41 167.6(4) . . . . ?
S4 C39 C40 C41 -2.5(5) . . . . ?
C30 C39 C40 P4 -12.0(6) . . . . ?
S4 C39 C40 P4 177.8(2) . . . . ?
C53 P4 C40 C39 131.8(3) . . . . ?
C56 P4 C40 C39 -113.0(4) . . . . ?
Ir2 P4 C40 C39 3.6(4) . . . . ?
C53 P4 C40 C41 -47.7(5) . . . . ?
C56 P4 C40 C41 67.5(5) . . . . ?
Ir2 P4 C40 C41 -175.9(4) . . . . ?
C39 C40 C41 C42 -177.6(5) . . . . ?
P4 C40 C41 C42 1.9(9) . . . . ?
C39 C40 C41 C46 2.9(6) . . . . ?
P4 C40 C41 C46 -177.6(4) . . . . ?
C46 C41 C42 C43 0.1(9) . . . . ?
C40 C41 C42 C43 -179.4(6) . . . . ?
C41 C42 C43 C44 0.6(11) . . . . ?
C42 C43 C44 C45 -1.0(13) . . . . ?
C43 C44 C45 C46 0.8(12) . . . . ?
C44 C45 C46 C41 -0.1(10) . . . . ?
C44 C45 C46 S4 -178.7(6) . . . . ?
C42 C41 C46 C45 -0.4(8) . . . . ?
C40 C41 C46 C45 179.2(5) . . . . ?
C42 C41 C46 S4 178.5(4) . . . . ?
C40 C41 C46 S4 -2.0(6) . . . . ?
C39 S4 C46 C45 179.3(6) . . . . ?
C39 S4 C46 C41 0.5(4) . . . . ?
C32 P3 C47 C49 34.2(4) . . . . ?
C50 P3 C47 C49 143.1(3) . . . . ?
Ir2 P3 C47 C49 -79.9(3) . . . . ?
C32 P3 C47 C48 156.2(4) . . . . ?
C50 P3 C47 C48 -94.8(4) . . . . ?
Ir2 P3 C47 C48 42.1(4) . . . . ?
C32 P3 C50 C51 168.8(4) . . . . ?
C47 P3 C50 C51 56.6(4) . . . . ?
Ir2 P3 C50 C51 -81.7(4) . . . . ?
C32 P3 C50 C52 -66.3(4) . . . . ?
C47 P3 C50 C52 -178.4(4) . . . . ?
Ir2 P3 C50 C52 43.3(4) . . . . ?
C40 P4 C53 C54 -176.0(4) . . . . ?
C56 P4 C53 C54 69.3(4) . . . . ?
Ir2 P4 C53 C54 -59.6(4) . . . . ?
C40 P4 C53 C55 -54.0(4) . . . . ?
C56 P4 C53 C55 -168.7(4) . . . . ?
Ir2 P4 C53 C55 62.4(4) . . . . ?
C40 P4 C56 C58 51.5(4) . . . . ?
C53 P4 C56 C58 165.7(4) . . . . ?
Ir2 P4 C56 C58 -59.7(4) . . . . ?
C40 P4 C56 C57 -74.8(4) . . . . ?
C53 P4 C56 C57 39.4(4) . . . . ?
Ir2 P4 C56 C57 174.0(3) . . . . ?
C65 C60 C61 C62 1.1(12) . . . . ?
C59 C60 C61 C62 179.6(8) . . . . ?
C60 C61 C62 C63 -1.0(14) . . . . ?
C61 C62 C63 C64 1.1(14) . . . . ?
C62 C63 C64 C65 -1.3(13) . . . . ?
C63 C64 C65 C60 1.4(11) . . . . ?
C61 C60 C65 C64 -1.3(10) . . . . ?
C59 C60 C65 C64 -179.7(7) . . . . ?
 
_refine_diff_density_max    2.780
_refine_diff_density_min   -1.149
_refine_diff_density_rms    0.126

_shelxl_version_number 2013-4



#===END

data_1_Br
 
_audit_creation_method            SHELXL-2014/6
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety         'C29 H36 Br Ir O P2 S2, C7 H8 '
_chemical_formula_sum
 'C36 H44 Br Ir O P2 S2' 
_chemical_formula_weight          890.88

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0181   0.0091
 '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'
 'O'  'O'   0.0492   0.0322
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'P'  'P'   0.2955   0.4335
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'S'  'S'   0.3331   0.5567
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Br'  'Br'  -0.6763   1.2805
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Ir'  'Ir'  -4.7710   6.5667
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            14
_space_group_name_H-M_alt         'P 21/n'
_space_group_name_Hall            '-P 2yn'
 
_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.
;
 
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                    14.5417(3)
_cell_length_b                    11.2071(2)
_cell_length_c                    22.7055(5)
_cell_angle_alpha                 90
_cell_angle_beta                  106.9590(10)
_cell_angle_gamma                 90
_cell_volume                      3539.41(13)
_cell_formula_units_Z             4
_cell_measurement_temperature     173(2)
_cell_measurement_reflns_used      9099
_cell_measurement_theta_min        3.23
_cell_measurement_theta_max       71.91
 
_exptl_crystal_description       'block'
_exptl_crystal_colour            'Red'
_exptl_crystal_density_meas      '?'

_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn     1.672          
_exptl_crystal_F_000              1768
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.20
_exptl_crystal_size_mid           0.20
_exptl_crystal_size_min           0.20
_exptl_absorpt_coefficient_mu     10.789
_shelx_estimated_absorpt_T_min    0.221
_shelx_estimated_absorpt_T_max    0.221
_exptl_absorpt_correction_type    multi-scan

_exptl_absorpt_correction_T_min   0.3974
_exptl_absorpt_correction_T_max   0.5230
_exptl_absorpt_process_details    'Sadabs (Sheldrick, 1996)'

_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       173(2)
_diffrn_radiation_wavelength      1.54178
_diffrn_radiation_type            CuK\a
_diffrn_source                    ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number             36978
_diffrn_reflns_av_unetI/netI      0.0174
_diffrn_reflns_av_R_equivalents   0.0294
_diffrn_reflns_limit_h_min        -17
_diffrn_reflns_limit_h_max        17
_diffrn_reflns_limit_k_min        -13
_diffrn_reflns_limit_k_max        13
_diffrn_reflns_limit_l_min        -27
_diffrn_reflns_limit_l_max        27
_diffrn_reflns_theta_min          3.235
_diffrn_reflns_theta_max          67.490
_diffrn_reflns_theta_full         67.500
_diffrn_measured_fraction_theta_max   1.000
_diffrn_measured_fraction_theta_full  1.000
_diffrn_reflns_Laue_measured_fraction_max    1.000
_diffrn_reflns_Laue_measured_fraction_full   1.000
_diffrn_reflns_point_group_measured_fraction_max   1.000
_diffrn_reflns_point_group_measured_fraction_full  1.000
_reflns_number_total              6367
_reflns_number_gt                 6097
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material 'LinXTL v.  5.3.1'
_refine_special_details           ?
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0287P)²+2.3500P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          6367
_refine_ls_number_parameters      397
_refine_ls_number_restraints      387
_refine_ls_R_factor_all           0.0214
_refine_ls_R_factor_gt            0.0201
_refine_ls_wR_factor_ref          0.0497
_refine_ls_wR_factor_gt           0.0491
_refine_ls_goodness_of_fit_ref    1.073
_refine_ls_restrained_S_all       1.053
_refine_ls_shift/su_max           0.006
_refine_ls_shift/su_mean          0.000
 
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
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Br1 Br 0.85152(2) 0.04754(3) 0.60979(2) 0.02698(7) Uani 1 1 d . U . . .
C1 C 0.62394(17) 0.3015(2) 0.50758(11) 0.0159(5) Uani 1 1 d . U . . .
C2 C 0.53809(17) 0.2957(2) 0.53143(12) 0.0167(5) Uani 1 1 d . U . . .
C3 C 0.54389(17) 0.2634(2) 0.59016(11) 0.0163(5) Uani 1 1 d . U . . .
C4 C 0.45782(18) 0.2926(2) 0.60716(12) 0.0186(5) Uani 1 1 d . U . . .
C5 C 0.38699(18) 0.3408(2) 0.55722(12) 0.0209(5) Uani 1 1 d . U . . .
C6 C 0.2965(2) 0.3759(3) 0.56122(14) 0.0301(6) Uani 1 1 d . U . . .
H6 H 0.2487 0.4060 0.5263 0.036 Uiso 1 1 calc R U . . .
C7 C 0.2793(2) 0.3653(3) 0.61776(15) 0.0343(7) Uani 1 1 d . U . . .
H7 H 0.2184 0.3874 0.6219 0.041 Uiso 1 1 calc R U . . .
C8 C 0.3510(2) 0.3221(3) 0.66908(14) 0.0289(6) Uani 1 1 d . U . . .
H8 H 0.3387 0.3186 0.7079 0.035 Uiso 1 1 calc R U . . .
C9 C 0.4383(2) 0.2850(2) 0.66425(13) 0.0236(5) Uani 1 1 d . U . . .
H9 H 0.4855 0.2543 0.6993 0.028 Uiso 1 1 calc R U . . .
C10 C 0.69389(19) 0.2685(2) 0.70814(12) 0.0226(5) Uani 1 1 d . U . . .
H10 H 0.6484 0.2434 0.7314 0.027 Uiso 1 1 calc R U . . .
C11 C 0.6884(2) 0.4036(3) 0.70105(14) 0.0354(7) Uani 1 1 d . U . . .
H11A H 0.7088 0.4410 0.7418 0.053 Uiso 1 1 calc R U . . .
H11B H 0.6221 0.4272 0.6798 0.053 Uiso 1 1 calc R U . . .
H11C H 0.7307 0.4297 0.6770 0.053 Uiso 1 1 calc R U . . .
C12 C 0.7951(2) 0.2285(3) 0.74440(14) 0.0330(7) Uani 1 1 d . U . . .
H12A H 0.8412 0.2560 0.7234 0.050 Uiso 1 1 calc R U . . .
H12B H 0.7971 0.1412 0.7472 0.050 Uiso 1 1 calc R U . . .
H12C H 0.8118 0.2626 0.7859 0.050 Uiso 1 1 calc R U . . .
C13 C 0.63031(18) 0.0381(2) 0.64617(12) 0.0217(5) Uani 1 1 d . U . . .
H13 H 0.6935 -0.0025 0.6643 0.026 Uiso 1 1 calc R U . . .
C14 C 0.5714(2) 0.0198(3) 0.69119(14) 0.0297(6) Uani 1 1 d . U . . .
H14A H 0.5083 0.0576 0.6748 0.045 Uiso 1 1 calc R U . . .
H14B H 0.6052 0.0558 0.7309 0.045 Uiso 1 1 calc R U . . .
H14C H 0.5630 -0.0658 0.6967 0.045 Uiso 1 1 calc R U . . .
C15 C 0.5826(2) -0.0234(3) 0.58499(14) 0.0334(7) Uani 1 1 d . U . . .
H15A H 0.5699 -0.1071 0.5924 0.050 Uiso 1 1 calc R U . . .
H15B H 0.6253 -0.0194 0.5587 0.050 Uiso 1 1 calc R U . . .
H15C H 0.5218 0.0168 0.5645 0.050 Uiso 1 1 calc R U . . .
C16 C 0.61435(17) 0.3002(2) 0.44007(11) 0.0169(5) Uani 1 1 d . U . . .
C17 C 0.68719(17) 0.2691(2) 0.41629(12) 0.0178(5) Uani 1 1 d . U . . .
C18 C 0.66731(18) 0.3024(2) 0.35212(12) 0.0203(5) Uani 1 1 d . U . . .
C19 C 0.57606(18) 0.3541(2) 0.32941(12) 0.0203(5) Uani 1 1 d . U . . .
C20 C 0.53993(18) 0.3942(3) 0.26859(12) 0.0248(6) Uani 1 1 d . U . . .
H20 H 0.4770 0.4265 0.2539 0.030 Uiso 1 1 calc R U . . .
C21 C 0.5978(2) 0.3854(3) 0.23098(13) 0.0309(6) Uani 1 1 d . U . . .
H21 H 0.5750 0.4125 0.1896 0.037 Uiso 1 1 calc R U . . .
C22 C 0.6903(2) 0.3369(3) 0.25268(14) 0.0329(7) Uani 1 1 d . U . . .
H22 H 0.7300 0.3332 0.2261 0.039 Uiso 1 1 calc R U . . .
C23 C 0.7249(2) 0.2944(3) 0.31218(13) 0.0281(6) Uani 1 1 d . U . . .
H23 H 0.7872 0.2599 0.3260 0.034 Uiso 1 1 calc R U . . .
C24 C 0.89958(18) 0.2651(3) 0.46233(13) 0.0237(5) Uani 1 1 d . U . . .
H24 H 0.9041 0.2439 0.4205 0.028 Uiso 1 1 calc R U . . .
C25 C 0.8949(2) 0.4006(3) 0.46634(15) 0.0357(7) Uani 1 1 d . U . . .
H25A H 0.8917 0.4235 0.5074 0.053 Uiso 1 1 calc R U . . .
H25B H 0.8375 0.4298 0.4351 0.053 Uiso 1 1 calc R U . . .
H25C H 0.9524 0.4356 0.4591 0.053 Uiso 1 1 calc R U . . .
C26 C 0.9877(2) 0.2138(3) 0.51003(17) 0.0441(9) Uani 1 1 d . U . . .
H26A H 1.0461 0.2493 0.5043 0.066 Uiso 1 1 calc R U . . .
H26B H 0.9895 0.1271 0.5049 0.066 Uiso 1 1 calc R U . . .
H26C H 0.9842 0.2321 0.5515 0.066 Uiso 1 1 calc R U . . .
C27 C 0.7918(2) 0.0404(2) 0.44658(12) 0.0243(5) Uani 1 1 d . U . . .
H27 H 0.8365 -0.0030 0.4819 0.029 Uiso 1 1 calc R U . . .
C28 C 0.6930(2) -0.0165(3) 0.43587(17) 0.0417(8) Uani 1 1 d . U . . .
H28A H 0.6481 0.0180 0.3989 0.063 Uiso 1 1 calc R U . . .
H28B H 0.6696 -0.0014 0.4715 0.063 Uiso 1 1 calc R U . . .
H28C H 0.6978 -0.1027 0.4303 0.063 Uiso 1 1 calc R U . . .
C29 C 0.8282(3) 0.0186(3) 0.39077(15) 0.0390(7) Uani 1 1 d . U . . .
H29A H 0.8314 -0.0674 0.3839 0.059 Uiso 1 1 calc R U . . .
H29B H 0.8924 0.0535 0.3984 0.059 Uiso 1 1 calc R U . . .
H29C H 0.7842 0.0558 0.3543 0.059 Uiso 1 1 calc R U . . .
C30 C 0.9897(3) 0.5288(3) 0.66850(16) 0.0438(8) Uani 1 1 d . U . . .
C31 C 0.8965(3) 0.5035(3) 0.63402(15) 0.0429(8) Uani 1 1 d . U . . .
H31 H 0.8778 0.4229 0.6243 0.051 Uiso 1 1 calc R U . . .
C32 C 0.8304(3) 0.5939(4) 0.61359(17) 0.0525(9) Uani 1 1 d . U . . .
H32 H 0.7664 0.5749 0.5906 0.063 Uiso 1 1 calc R U . . .
C33 C 0.8562(3) 0.7100(4) 0.62612(19) 0.0535(10) Uani 1 1 d . U . . .
H33 H 0.8106 0.7718 0.6114 0.064 Uiso 1 1 calc R U . . .
C34 C 0.9490(3) 0.7375(3) 0.66037(18) 0.0488(9) Uani 1 1 d . U . . .
H34 H 0.9673 0.8184 0.6692 0.059 Uiso 1 1 calc R U . . .
C35 C 1.0142(2) 0.6485(4) 0.68145(15) 0.0434(8) Uani 1 1 d . U . . .
H35 H 1.0776 0.6682 0.7054 0.052 Uiso 1 1 calc R U . . .
C36 C 1.0615(4) 0.4316(5) 0.6932(2) 0.0766(15) Uani 1 1 d . U . . .
H36A H 1.1256 0.4587 0.6932 0.115 Uiso 1 1 calc R U . . .
H36B H 1.0438 0.3606 0.6671 0.115 Uiso 1 1 calc R U . . .
H36C H 1.0620 0.4120 0.7353 0.115 Uiso 1 1 calc R U . . .
Ir1 Ir 0.74391(2) 0.20946(2) 0.56136(2) 0.01417(4) Uani 1 1 d . U . . .
O1 O 0.69223(12) 0.37878(15) 0.53921(8) 0.0176(3) Uani 1 1 d . U . . .
P1 P 0.65698(4) 0.19558(5) 0.63213(3) 0.01541(12) Uani 1 1 d . U . . .
P2 P 0.78872(4) 0.19737(5) 0.47134(3) 0.01588(12) Uani 1 1 d . U . . .
S1 S 0.42636(4) 0.35503(6) 0.49231(3) 0.02199(13) Uani 1 1 d . U . . .
S2 S 0.51724(4) 0.36421(6) 0.38563(3) 0.02043(12) Uani 1 1 d . U . . .
 
 
_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_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
Br1 Ir1 2.4387(3) . ?
C1 O1 1.355(3) . ?
C1 C16 1.498(3) . ?
C1 C2 1.500(3) . ?
C1 Ir1 2.087(2) . ?
C2 C3 1.360(4) . ?
C2 S1 1.740(2) . ?
C3 C4 1.451(3) . ?
C3 P1 1.810(2) . ?
C4 C5 1.399(4) . ?
C4 C9 1.408(4) . ?
C5 C6 1.402(4) . ?
C5 S1 1.737(3) . ?
C6 C7 1.383(4) . ?
C6 H6 0.9500 . ?
C7 C8 1.403(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.371(4) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 C11 1.523(4) . ?
C10 C12 1.529(4) . ?
C10 P1 1.842(3) . ?
C10 H10 1.0000 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.527(4) . ?
C13 C15 1.524(4) . ?
C13 P1 1.855(3) . ?
C13 H13 1.0000 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.367(4) . ?
C16 S2 1.737(2) . ?
C17 C18 1.449(3) . ?
C17 P2 1.820(3) . ?
C18 C19 1.401(4) . ?
C18 C23 1.405(4) . ?
C19 C20 1.400(4) . ?
C19 S2 1.735(2) . ?
C20 C21 1.366(4) . ?
C20 H20 0.9500 . ?
C21 C22 1.401(4) . ?
C21 H21 0.9500 . ?
C22 C23 1.382(4) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 C25 1.524(4) . ?
C24 C26 1.529(4) . ?
C24 P2 1.846(3) . ?
C24 H24 1.0000 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28 1.525(4) . ?
C27 C29 1.529(4) . ?
C27 P2 1.851(3) . ?
C27 H27 1.0000 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 C31 1.382(5) . ?
C30 C35 1.397(5) . ?
C30 C36 1.500(6) . ?
C31 C32 1.380(6) . ?
C31 H31 0.9500 . ?
C32 C33 1.361(6) . ?
C32 H32 0.9500 . ?
C33 C34 1.381(6) . ?
C33 H33 0.9500 . ?
C34 C35 1.364(6) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
Ir1 O1 2.0489(17) . ?
Ir1 P1 2.3214(6) . ?
Ir1 P2 2.3234(6) . ?
 
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
O1 C1 C16 112.6(2) . . ?
O1 C1 C2 113.3(2) . . ?
C16 C1 C2 122.0(2) . . ?
O1 C1 Ir1 69.36(12) . . ?
C16 C1 Ir1 113.96(16) . . ?
C2 C1 Ir1 114.14(16) . . ?
C3 C2 C1 123.0(2) . . ?
C3 C2 S1 112.56(18) . . ?
C1 C2 S1 123.40(18) . . ?
C2 C3 C4 112.9(2) . . ?
C2 C3 P1 114.51(18) . . ?
C4 C3 P1 132.56(19) . . ?
C5 C4 C9 118.1(2) . . ?
C5 C4 C3 111.1(2) . . ?
C9 C4 C3 130.7(2) . . ?
C4 C5 C6 122.6(2) . . ?
C4 C5 S1 112.10(19) . . ?
C6 C5 S1 125.2(2) . . ?
C7 C6 C5 117.6(3) . . ?
C7 C6 H6 121.2 . . ?
C5 C6 H6 121.2 . . ?
C6 C7 C8 120.6(3) . . ?
C6 C7 H7 119.7 . . ?
C8 C7 H7 119.7 . . ?
C9 C8 C7 121.3(3) . . ?
C9 C8 H8 119.4 . . ?
C7 C8 H8 119.4 . . ?
C8 C9 C4 119.7(3) . . ?
C8 C9 H9 120.2 . . ?
C4 C9 H9 120.2 . . ?
C11 C10 C12 111.2(2) . . ?
C11 C10 P1 110.50(19) . . ?
C12 C10 P1 110.25(19) . . ?
C11 C10 H10 108.3 . . ?
C12 C10 H10 108.3 . . ?
P1 C10 H10 108.3 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 C15 110.8(2) . . ?
C14 C13 P1 115.41(19) . . ?
C15 C13 P1 109.61(18) . . ?
C14 C13 H13 106.9 . . ?
C15 C13 H13 106.9 . . ?
P1 C13 H13 106.9 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 C1 123.7(2) . . ?
C17 C16 S2 112.77(19) . . ?
C1 C16 S2 122.51(18) . . ?
C16 C17 C18 112.4(2) . . ?
C16 C17 P2 114.09(19) . . ?
C18 C17 P2 133.49(19) . . ?
C19 C18 C23 117.9(2) . . ?
C19 C18 C17 111.5(2) . . ?
C23 C18 C17 130.6(2) . . ?
C18 C19 C20 122.6(2) . . ?
C18 C19 S2 111.92(19) . . ?
C20 C19 S2 125.5(2) . . ?
C21 C20 C19 118.1(2) . . ?
C21 C20 H20 120.9 . . ?
C19 C20 H20 120.9 . . ?
C20 C21 C22 120.8(3) . . ?
C20 C21 H21 119.6 . . ?
C22 C21 H21 119.6 . . ?
C23 C22 C21 121.0(3) . . ?
C23 C22 H22 119.5 . . ?
C21 C22 H22 119.5 . . ?
C22 C23 C18 119.6(3) . . ?
C22 C23 H23 120.2 . . ?
C18 C23 H23 120.2 . . ?
C25 C24 C26 112.0(3) . . ?
C25 C24 P2 110.32(19) . . ?
C26 C24 P2 110.2(2) . . ?
C25 C24 H24 108.0 . . ?
C26 C24 H24 108.0 . . ?
P2 C24 H24 108.0 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C28 C27 C29 109.8(2) . . ?
C28 C27 P2 109.9(2) . . ?
C29 C27 P2 116.6(2) . . ?
C28 C27 H27 106.6 . . ?
C29 C27 H27 106.6 . . ?
P2 C27 H27 106.6 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C31 C30 C35 117.7(4) . . ?
C31 C30 C36 121.5(4) . . ?
C35 C30 C36 120.8(4) . . ?
C32 C31 C30 120.7(3) . . ?
C32 C31 H31 119.6 . . ?
C30 C31 H31 119.6 . . ?
C33 C32 C31 120.6(4) . . ?
C33 C32 H32 119.7 . . ?
C31 C32 H32 119.7 . . ?
C32 C33 C34 119.7(4) . . ?
C32 C33 H33 120.1 . . ?
C34 C33 H33 120.1 . . ?
C35 C34 C33 119.9(4) . . ?
C35 C34 H34 120.0 . . ?
C33 C34 H34 120.0 . . ?
C34 C35 C30 121.3(3) . . ?
C34 C35 H35 119.3 . . ?
C30 C35 H35 119.3 . . ?
C30 C36 H36A 109.5 . . ?
C30 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C30 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
O1 Ir1 C1 38.23(8) . . ?
O1 Ir1 P1 89.84(5) . . ?
C1 Ir1 P1 84.67(7) . . ?
O1 Ir1 P2 90.86(5) . . ?
C1 Ir1 P2 85.13(7) . . ?
P1 Ir1 P2 162.57(2) . . ?
O1 Ir1 Br1 160.23(5) . . ?
C1 Ir1 Br1 161.54(7) . . ?
P1 Ir1 Br1 92.599(16) . . ?
P2 Ir1 Br1 92.614(16) . . ?
C1 O1 Ir1 72.42(12) . . ?
C3 P1 C10 106.17(12) . . ?
C3 P1 C13 106.67(12) . . ?
C10 P1 C13 106.23(12) . . ?
C3 P1 Ir1 101.65(8) . . ?
C10 P1 Ir1 123.37(9) . . ?
C13 P1 Ir1 111.48(8) . . ?
C17 P2 C24 107.57(12) . . ?
C17 P2 C27 107.33(12) . . ?
C24 P2 C27 104.95(13) . . ?
C17 P2 Ir1 101.47(8) . . ?
C24 P2 Ir1 123.46(9) . . ?
C27 P2 Ir1 111.12(9) . . ?
C5 S1 C2 91.23(12) . . ?
C19 S2 C16 91.36(12) . . ?
 
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 C1 C2 C3 -59.5(3) . . . . ?
C16 C1 C2 C3 160.9(2) . . . . ?
Ir1 C1 C2 C3 17.3(3) . . . . ?
O1 C1 C2 S1 108.2(2) . . . . ?
C16 C1 C2 S1 -31.4(3) . . . . ?
Ir1 C1 C2 S1 -174.95(13) . . . . ?
C1 C2 C3 C4 165.5(2) . . . . ?
S1 C2 C3 C4 -3.4(3) . . . . ?
C1 C2 C3 P1 -13.5(3) . . . . ?
S1 C2 C3 P1 177.65(12) . . . . ?
C2 C3 C4 C5 3.6(3) . . . . ?
P1 C3 C4 C5 -177.7(2) . . . . ?
C2 C3 C4 C9 -173.1(3) . . . . ?
P1 C3 C4 C9 5.6(4) . . . . ?
C9 C4 C5 C6 -3.2(4) . . . . ?
C3 C4 C5 C6 179.6(3) . . . . ?
C9 C4 C5 S1 174.98(19) . . . . ?
C3 C4 C5 S1 -2.2(3) . . . . ?
C4 C5 C6 C7 2.1(5) . . . . ?
S1 C5 C6 C7 -175.8(2) . . . . ?
C5 C6 C7 C8 0.8(5) . . . . ?
C6 C7 C8 C9 -2.6(5) . . . . ?
C7 C8 C9 C4 1.4(4) . . . . ?
C5 C4 C9 C8 1.3(4) . . . . ?
C3 C4 C9 C8 177.9(3) . . . . ?
O1 C1 C16 C17 60.9(3) . . . . ?
C2 C1 C16 C17 -159.3(2) . . . . ?
Ir1 C1 C16 C17 -15.6(3) . . . . ?
O1 C1 C16 S2 -106.8(2) . . . . ?
C2 C1 C16 S2 33.0(3) . . . . ?
Ir1 C1 C16 S2 176.70(13) . . . . ?
C1 C16 C17 C18 -166.0(2) . . . . ?
S2 C16 C17 C18 2.7(3) . . . . ?
C1 C16 C17 P2 13.1(3) . . . . ?
S2 C16 C17 P2 -178.15(12) . . . . ?
C16 C17 C18 C19 -2.4(3) . . . . ?
P2 C17 C18 C19 178.6(2) . . . . ?
C16 C17 C18 C23 175.1(3) . . . . ?
P2 C17 C18 C23 -3.8(5) . . . . ?
C23 C18 C19 C20 2.0(4) . . . . ?
C17 C18 C19 C20 179.9(2) . . . . ?
C23 C18 C19 S2 -176.8(2) . . . . ?
C17 C18 C19 S2 1.1(3) . . . . ?
C18 C19 C20 C21 -2.1(4) . . . . ?
S2 C19 C20 C21 176.5(2) . . . . ?
C19 C20 C21 C22 0.4(5) . . . . ?
C20 C21 C22 C23 1.4(5) . . . . ?
C21 C22 C23 C18 -1.5(5) . . . . ?
C19 C18 C23 C22 -0.1(4) . . . . ?
C17 C18 C23 C22 -177.5(3) . . . . ?
C35 C30 C31 C32 -0.3(5) . . . . ?
C36 C30 C31 C32 177.6(4) . . . . ?
C30 C31 C32 C33 1.1(6) . . . . ?
C31 C32 C33 C34 -0.9(6) . . . . ?
C32 C33 C34 C35 0.0(6) . . . . ?
C33 C34 C35 C30 0.8(6) . . . . ?
C31 C30 C35 C34 -0.6(5) . . . . ?
C36 C30 C35 C34 -178.6(4) . . . . ?
C16 C1 O1 Ir1 -108.27(18) . . . . ?
C2 C1 O1 Ir1 108.28(19) . . . . ?
C2 C3 P1 C10 133.6(2) . . . . ?
C4 C3 P1 C10 -45.1(3) . . . . ?
C2 C3 P1 C13 -113.4(2) . . . . ?
C4 C3 P1 C13 67.9(3) . . . . ?
C2 C3 P1 Ir1 3.5(2) . . . . ?
C4 C3 P1 Ir1 -175.2(2) . . . . ?
C11 C10 P1 C3 -49.6(2) . . . . ?
C12 C10 P1 C3 -172.9(2) . . . . ?
C11 C10 P1 C13 -162.9(2) . . . . ?
C12 C10 P1 C13 73.8(2) . . . . ?
C11 C10 P1 Ir1 66.7(2) . . . . ?
C12 C10 P1 Ir1 -56.6(2) . . . . ?
C14 C13 P1 C3 -68.7(2) . . . . ?
C15 C13 P1 C3 57.2(2) . . . . ?
C14 C13 P1 C10 44.3(2) . . . . ?
C15 C13 P1 C10 170.18(19) . . . . ?
C14 C13 P1 Ir1 -178.80(18) . . . . ?
C15 C13 P1 Ir1 -52.9(2) . . . . ?
C16 C17 P2 C24 -135.2(2) . . . . ?
C18 C17 P2 C24 43.7(3) . . . . ?
C16 C17 P2 C27 112.3(2) . . . . ?
C18 C17 P2 C27 -68.8(3) . . . . ?
C16 C17 P2 Ir1 -4.4(2) . . . . ?
C18 C17 P2 Ir1 174.5(2) . . . . ?
C25 C24 P2 C17 52.4(2) . . . . ?
C26 C24 P2 C17 176.7(2) . . . . ?
C25 C24 P2 C27 166.5(2) . . . . ?
C26 C24 P2 C27 -69.3(2) . . . . ?
C25 C24 P2 Ir1 -65.0(2) . . . . ?
C26 C24 P2 Ir1 59.3(3) . . . . ?
C28 C27 P2 C17 -51.1(2) . . . . ?
C29 C27 P2 C17 74.8(2) . . . . ?
C28 C27 P2 C24 -165.3(2) . . . . ?
C29 C27 P2 C24 -39.5(3) . . . . ?
C28 C27 P2 Ir1 59.1(2) . . . . ?
C29 C27 P2 Ir1 -175.1(2) . . . . ?
C4 C5 S1 C2 0.3(2) . . . . ?
C6 C5 S1 C2 178.4(3) . . . . ?
C3 C2 S1 C5 1.8(2) . . . . ?
C1 C2 S1 C5 -167.0(2) . . . . ?
C18 C19 S2 C16 0.3(2) . . . . ?
C20 C19 S2 C16 -178.4(3) . . . . ?
C17 C16 S2 C19 -1.8(2) . . . . ?
C1 C16 S2 C19 167.1(2) . . . . ?
 
_refine_diff_density_max    0.439
_refine_diff_density_min   -0.849
_refine_diff_density_rms    0.089

_shelxl_version_number 2014/6



#===END

data_7_Cl3
 
_audit_creation_method            SHELXL-2013
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety         'C29 H36 Cl3 Ir P2 S2, C7 H8'
_chemical_formula_sum
 'C36 H44 Cl3 Ir P2 S2' 
_chemical_formula_weight          901.32

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'
 'Ir'  'Ir'  -1.4442   7.9887
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'P'  'P'   0.1023   0.0942
 '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'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            14
_space_group_name_H-M_alt         'P 21/c'
_space_group_name_Hall            '-P 2ybc'
 
_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.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y-1/2, z-1/2'
 
_cell_length_a                    12.4862(3)
_cell_length_b                    13.6671(5)
_cell_length_c                    23.6020(6)
_cell_angle_alpha                 90
_cell_angle_beta                  118.383(2)
_cell_angle_gamma                 90
_cell_volume                      3543.51(19)
_cell_formula_units_Z             4
_cell_measurement_temperature     173(2)
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min       ?
_cell_measurement_theta_max       ?
 
_exptl_crystal_description       'block'
_exptl_crystal_colour            'Red'
_exptl_crystal_density_meas      '?'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn     1.689          
_exptl_crystal_F_000              1800
_exptl_transmission_factor_min    ?                                             
_exptl_transmission_factor_max    ?                                             
_exptl_crystal_size_max           0.04
_exptl_crystal_size_mid           0.04
_exptl_crystal_size_min           0.02
_exptl_absorpt_coefficient_mu     4.229
_shelx_estimated_absorpt_T_min    0.849
_shelx_estimated_absorpt_T_max    0.920
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.8491
_exptl_absorpt_correction_T_max   0.9202
_exptl_absorpt_process_details    'Sadabs (Sheldrick, 1996)'
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       173(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    ?                       
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number             20857
_diffrn_reflns_av_unetI/netI      0.0543
_diffrn_reflns_av_R_equivalents   0.0775
_diffrn_reflns_limit_h_min        -14
_diffrn_reflns_limit_h_max        14
_diffrn_reflns_limit_k_min        -16
_diffrn_reflns_limit_k_max        16
_diffrn_reflns_limit_l_min        -28
_diffrn_reflns_limit_l_max        27
_diffrn_reflns_theta_min          2.379
_diffrn_reflns_theta_max          24.998
_diffrn_reflns_theta_full         25.000
_diffrn_measured_fraction_theta_max   0.991
_diffrn_measured_fraction_theta_full  0.991
_diffrn_reflns_Laue_measured_fraction_max    0.991
_diffrn_reflns_Laue_measured_fraction_full   0.991
_diffrn_reflns_point_group_measured_fraction_max   0.991
_diffrn_reflns_point_group_measured_fraction_full  0.991
_reflns_number_total              6180
_reflns_number_gt                 5119
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection      'Bruker APEX2'
_computing_cell_refinement      'Bruker SAINT'
_computing_data_reduction       'Bruker SAINT'  
_computing_structure_solution   'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics   'Bruker SHELXTL'
_computing_publication_material 'LinXTL v.  5.3.8'
 
_refine_special_details
;
 ?
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0740P)²+16.2535P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          6180
_refine_ls_number_parameters      425
_refine_ls_number_restraints      570
_refine_ls_R_factor_all           0.0757
_refine_ls_R_factor_gt            0.0552
_refine_ls_wR_factor_ref          0.1511
_refine_ls_wR_factor_gt           0.1355
_refine_ls_goodness_of_fit_ref    1.132
_refine_ls_restrained_S_all       1.091
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
 
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
 _atom_site_disorder_assembly
 _atom_site_disorder_group
C1 C 0.1353(7) 0.1475(6) 0.6257(4) 0.0267(16) Uani 1 1 d . U . A 1
C2 C 0.1856(8) 0.2085(7) 0.5936(4) 0.0312(18) Uani 1 1 d . U . A 1
C3 C 0.2884(8) 0.2647(7) 0.6278(4) 0.0330(19) Uani 1 1 d . U . A 1
C4 C 0.3221(9) 0.3210(7) 0.5879(4) 0.038(2) Uani 1 1 d . U . A 1
C5 C 0.4186(10) 0.3857(8) 0.6040(5) 0.047(2) Uani 1 1 d . U . A 1
H5 H 0.4737 0.3993 0.6479 0.057 Uiso 1 1 calc R U . A 1
C6 C 0.4330(11) 0.4294(8) 0.5559(5) 0.053(3) Uani 1 1 d . U . A 1
H6 H 0.4964 0.4759 0.5669 0.063 Uiso 1 1 calc R U . A 1
C7 C 0.3586(11) 0.4080(9) 0.4926(5) 0.060(3) Uani 1 1 d . U . A 1
H7 H 0.3741 0.4376 0.4608 0.071 Uiso 1 1 calc R U . A 1
C8 C 0.2629(11) 0.3455(8) 0.4736(5) 0.051(3) Uani 1 1 d . U . A 1
H8 H 0.2110 0.3317 0.4294 0.061 Uiso 1 1 calc R U . A 1
C9 C 0.2439(9) 0.3020(8) 0.5221(4) 0.041(2) Uani 1 1 d . U . A 1
C10 C 0.0208(8) 0.0985(7) 0.5896(4) 0.0333(18) Uani 1 1 d . U . A 1
C11 C -0.0230(8) 0.0357(7) 0.6206(4) 0.0345(19) Uani 1 1 d . U . A 1
C12 C -0.1396(8) -0.0031(8) 0.5782(5) 0.041(2) Uani 1 1 d . U . A 1
C13 C -0.2141(9) -0.0675(9) 0.5899(5) 0.052(3) Uani 1 1 d . U . A 1
H13 H -0.1858 -0.0946 0.6317 0.062 Uiso 1 1 calc R U . A 1
C14 C -0.3254(11) -0.0917(11) 0.5425(6) 0.069(3) Uani 1 1 d . U . A 1
H14 H -0.3762 -0.1338 0.5514 0.083 Uiso 1 1 calc R U . A 1
C15 C -0.3665(10) -0.0551(10) 0.4804(6) 0.063(3) Uani 1 1 d . U . A 1
H15 H -0.4454 -0.0729 0.4476 0.076 Uiso 1 1 calc R U . A 1
C16 C -0.2975(9) 0.0053(9) 0.4651(5) 0.055(3) Uani 1 1 d . U . A 1
H16 H -0.3254 0.0285 0.4224 0.065 Uiso 1 1 calc R U . A 1
C17 C -0.1834(8) 0.0315(8) 0.5151(5) 0.042(2) Uani 1 1 d . U . A 1
C18 C 0.3648(9) 0.3778(7) 0.7432(5) 0.041(2) Uani 1 1 d . U . A 1
H18 H 0.4372 0.4094 0.7433 0.049 Uiso 1 1 calc R U . A 1
C19 C 0.3878(10) 0.3800(8) 0.8130(5) 0.048(3) Uani 1 1 d . U . A 1
H19A H 0.4590 0.3397 0.8399 0.071 Uiso 1 1 calc R U . A 1
H19B H 0.3164 0.3542 0.8150 0.071 Uiso 1 1 calc R U . A 1
H19C H 0.4026 0.4476 0.8289 0.071 Uiso 1 1 calc R U . A 1
C20 C 0.2554(10) 0.4401(8) 0.6998(5) 0.051(3) Uani 1 1 d . U . A 1
H20A H 0.2435 0.4381 0.6557 0.076 Uiso 1 1 calc R U . A 1
H20B H 0.2696 0.5079 0.7153 0.076 Uiso 1 1 calc R U . A 1
H20C H 0.1826 0.4147 0.7005 0.076 Uiso 1 1 calc R U . A 1
C21 C 0.5201(9) 0.2263(9) 0.7387(5) 0.054(3) Uani 1 1 d . U . A 1
H21 H 0.5568 0.2919 0.7402 0.065 Uiso 1 1 calc R U . A 1
C22 C 0.5863(11) 0.1898(11) 0.8049(6) 0.075(4) Uani 1 1 d . U . A 1
H22A H 0.5688 0.2316 0.8332 0.113 Uiso 1 1 calc R U . A 1
H22B H 0.6739 0.1907 0.8191 0.113 Uiso 1 1 calc R U . A 1
H22C H 0.5604 0.1227 0.8066 0.113 Uiso 1 1 calc R U . A 1
C23 C 0.5413(9) 0.1686(8) 0.6904(5) 0.049(3) Uani 1 1 d . U . A 1
H23A H 0.4954 0.1984 0.6477 0.074 Uiso 1 1 calc R U . A 1
H23B H 0.5140 0.1011 0.6891 0.074 Uiso 1 1 calc R U . A 1
H23C H 0.6283 0.1690 0.7031 0.074 Uiso 1 1 calc R U . A 1
C24 C -0.0175(8) 0.0295(8) 0.7459(5) 0.039(2) Uani 1 1 d . U . A 1
H24 H -0.0548 -0.0362 0.7431 0.047 Uiso 1 1 calc R U . A 1
C25 C 0.0597(9) 0.0527(9) 0.8178(5) 0.050(3) Uani 1 1 d . U . A 1
H25A H 0.1261 0.0052 0.8376 0.075 Uiso 1 1 calc R U . A 1
H25B H 0.0085 0.0491 0.8389 0.075 Uiso 1 1 calc R U . A 1
H25C H 0.0936 0.1188 0.8229 0.075 Uiso 1 1 calc R U . A 1
C26 C -0.1209(9) 0.1008(8) 0.7143(5) 0.044(2) Uani 1 1 d . U . A 1
H26A H -0.1695 0.0843 0.6686 0.066 Uiso 1 1 calc R U . A 1
H26B H -0.0884 0.1672 0.7184 0.066 Uiso 1 1 calc R U . A 1
H26C H -0.1723 0.0974 0.7353 0.066 Uiso 1 1 calc R U . A 1
C30 C 0.7165(11) 0.2894(8) 0.5315(6) 0.079(3) Uani 1 1 d D U . B 1
C31 C 0.8333(11) 0.3017(7) 0.5776(6) 0.077(3) Uani 1 1 d D U . B 1
H31 H 0.8604 0.2724 0.6187 0.092 Uiso 1 1 calc R U . B 1
C32 C 0.9125(12) 0.3552(8) 0.5658(6) 0.088(3) Uani 1 1 d D U . B 1
H32 H 0.9943 0.3631 0.5987 0.106 Uiso 1 1 calc R U . B 1
C33 C 0.8752(12) 0.3976(9) 0.5074(6) 0.097(3) Uani 1 1 d D U . B 1
H33 H 0.9303 0.4352 0.4991 0.116 Uiso 1 1 calc R U . B 1
C34 C 0.7578(12) 0.3853(9) 0.4608(7) 0.099(3) Uani 1 1 d D U . B 1
H34 H 0.7312 0.4145 0.4198 0.119 Uiso 1 1 calc R U . B 1
C35 C 0.6778(12) 0.3318(8) 0.4722(7) 0.087(3) Uani 1 1 d D U . B 1
H35 H 0.5960 0.3239 0.4394 0.104 Uiso 1 1 calc R U . B 1
C36 C 0.6332(14) 0.2311(12) 0.5436(8) 0.099(5) Uani 1 1 d . U . B 1
H36A H 0.5530 0.2310 0.5052 0.148 Uiso 1 1 calc R U . B 1
H36B H 0.6261 0.2590 0.5800 0.148 Uiso 1 1 calc R U . B 1
H36C H 0.6638 0.1639 0.5539 0.148 Uiso 1 1 calc R U . B 1
Ir1 Ir 0.22707(3) 0.13412(3) 0.71866(2) 0.02910(14) Uani 1 1 d . U . A 1
P1 P 0.3578(2) 0.25243(19) 0.71322(11) 0.0330(5) Uani 1 1 d . U . A 1
P2 P 0.0782(2) 0.01832(18) 0.70539(11) 0.0323(5) Uani 1 1 d . U . A 1
S1 S 0.1274(2) 0.2223(2) 0.51080(11) 0.0418(6) Uani 1 1 d . U . A 1
S2 S -0.0816(2) 0.10954(19) 0.50858(11) 0.0398(6) Uani 1 1 d . U . A 1
Cl1 Cl 0.1097(2) 0.25485(17) 0.73431(11) 0.0388(5) Uani 1 1 d . U . A 1
Cl2 Cl 0.3459(2) 0.1173(2) 0.83475(11) 0.0462(6) Uani 1 1 d . U . A 1
Cl3 Cl 0.3488(2) 0.01190(19) 0.70751(12) 0.0420(6) Uani 1 1 d . U . A 1
C27A C 0.126(3) -0.108(2) 0.7044(13) 0.036(3) Uani 0.413(17) 1 d . U P A 1
H27A H 0.1797 -0.1065 0.6836 0.043 Uiso 0.413(17) 1 calc R U P A 1
C29A C 0.207(3) -0.142(3) 0.7743(16) 0.039(5) Uani 0.413(17) 1 d . U P A 1
H29A H 0.1860 -0.1058 0.8033 0.059 Uiso 0.413(17) 1 calc R U P A 1
H29B H 0.2929 -0.1309 0.7864 0.059 Uiso 0.413(17) 1 calc R U P A 1
H29C H 0.1943 -0.2125 0.7777 0.059 Uiso 0.413(17) 1 calc R U P A 1
C28A C 0.033(2) -0.1810(17) 0.6697(11) 0.037(4) Uani 0.413(17) 1 d . U P A 1
H28A H 0.0710 -0.2459 0.6774 0.056 Uiso 0.413(17) 1 calc R U P A 1
H28B H -0.0060 -0.1663 0.6235 0.056 Uiso 0.413(17) 1 calc R U P A 1
H28C H -0.0274 -0.1798 0.6847 0.056 Uiso 0.413(17) 1 calc R U P A 1
C27B C 0.1153(19) -0.1160(14) 0.7225(10) 0.036(3) Uani 0.587(17) 1 d . U P A 2
H27B H 0.0458 -0.1473 0.7255 0.043 Uiso 0.587(17) 1 calc R U P A 2
C29B C 0.228(2) -0.1262(18) 0.7886(11) 0.039(4) Uani 0.587(17) 1 d . U P A 2
H29D H 0.2847 -0.1729 0.7857 0.058 Uiso 0.587(17) 1 calc R U P A 2
H29E H 0.2035 -0.1499 0.8199 0.058 Uiso 0.587(17) 1 calc R U P A 2
H29F H 0.2678 -0.0624 0.8024 0.058 Uiso 0.587(17) 1 calc R U P A 2
C28B C 0.1255(16) -0.1659(12) 0.6663(8) 0.040(4) Uani 0.587(17) 1 d . U P A 2
H28D H 0.1968 -0.1404 0.6642 0.061 Uiso 0.587(17) 1 calc R U P A 2
H28E H 0.0520 -0.1522 0.6257 0.061 Uiso 0.587(17) 1 calc R U P A 2
H28F H 0.1341 -0.2368 0.6735 0.061 Uiso 0.587(17) 1 calc R U P A 2
 
 
_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_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
C1 C10 1.435(12) . ?
C1 C2 1.455(12) . ?
C1 Ir1 1.941(8) . ?
C2 C3 1.380(12) . ?
C2 S1 1.742(9) . ?
C3 C4 1.426(12) . ?
C3 P1 1.784(9) . ?
C4 C5 1.393(14) . ?
C4 C9 1.411(13) . ?
C5 C6 1.369(14) . ?
C5 H5 0.9500 . ?
C6 C7 1.365(15) . ?
C6 H6 0.9500 . ?
C7 C8 1.359(16) . ?
C7 H7 0.9500 . ?
C8 C9 1.405(13) . ?
C8 H8 0.9500 . ?
C9 S1 1.734(10) . ?
C10 C11 1.396(13) . ?
C10 S2 1.730(9) . ?
C11 C12 1.420(12) . ?
C11 P2 1.804(9) . ?
C12 C13 1.400(14) . ?
C12 C17 1.402(14) . ?
C13 C14 1.347(14) . ?
C13 H13 0.9500 . ?
C14 C15 1.397(18) . ?
C14 H14 0.9500 . ?
C15 C16 1.360(16) . ?
C15 H15 0.9500 . ?
C16 C17 1.397(13) . ?
C16 H16 0.9500 . ?
C17 S2 1.721(10) . ?
C18 C20 1.520(14) . ?
C18 C19 1.533(13) . ?
C18 P1 1.839(10) . ?
C18 H18 1.0000 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.463(16) . ?
C21 C23 1.510(15) . ?
C21 P1 1.854(10) . ?
C21 H21 1.0000 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C26 1.502(14) . ?
C24 C25 1.536(13) . ?
C24 P2 1.857(9) . ?
C24 H24 1.0000 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C30 C31 1.353(12) . ?
C30 C35 1.371(12) . ?
C30 C36 1.444(19) . ?
C31 C32 1.360(12) . ?
C31 H31 0.9500 . ?
C32 C33 1.358(13) . ?
C32 H32 0.9500 . ?
C33 C34 1.361(12) . ?
C33 H33 0.9500 . ?
C34 C35 1.364(13) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
Ir1 P1 2.344(2) . ?
Ir1 P2 2.346(2) . ?
Ir1 Cl1 2.350(2) . ?
Ir1 Cl3 2.355(2) . ?
Ir1 Cl2 2.428(2) . ?
P2 C27A 1.84(3) . ?
P2 C27B 1.89(2) . ?
C27A C28A 1.45(4) . ?
C27A C29A 1.54(4) . ?
C27A H27A 1.0000 . ?
C29A H29A 0.9800 . ?
C29A H29B 0.9800 . ?
C29A H29C 0.9800 . ?
C28A H28A 0.9800 . ?
C28A H28B 0.9800 . ?
C28A H28C 0.9800 . ?
C27B C29B 1.53(3) . ?
C27B C28B 1.55(3) . ?
C27B H27B 1.0000 . ?
C29B H29D 0.9800 . ?
C29B H29E 0.9800 . ?
C29B H29F 0.9800 . ?
C28B H28D 0.9800 . ?
C28B H28E 0.9800 . ?
C28B H28F 0.9800 . ?
 
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
C10 C1 C2 120.9(8) . . ?
C10 C1 Ir1 120.9(6) . . ?
C2 C1 Ir1 118.2(6) . . ?
C3 C2 C1 121.8(8) . . ?
C3 C2 S1 111.8(7) . . ?
C1 C2 S1 126.4(7) . . ?
C2 C3 C4 113.5(8) . . ?
C2 C3 P1 115.1(7) . . ?
C4 C3 P1 131.3(7) . . ?
C5 C4 C9 118.3(9) . . ?
C5 C4 C3 130.5(9) . . ?
C9 C4 C3 111.2(9) . . ?
C6 C5 C4 119.2(10) . . ?
C6 C5 H5 120.4 . . ?
C4 C5 H5 120.4 . . ?
C7 C6 C5 121.7(11) . . ?
C7 C6 H6 119.2 . . ?
C5 C6 H6 119.2 . . ?
C8 C7 C6 122.0(10) . . ?
C8 C7 H7 119.0 . . ?
C6 C7 H7 119.0 . . ?
C7 C8 C9 117.3(10) . . ?
C7 C8 H8 121.3 . . ?
C9 C8 H8 121.3 . . ?
C8 C9 C4 121.5(10) . . ?
C8 C9 S1 126.5(8) . . ?
C4 C9 S1 112.0(7) . . ?
C11 C10 C1 120.2(8) . . ?
C11 C10 S2 111.4(7) . . ?
C1 C10 S2 128.3(7) . . ?
C10 C11 C12 112.7(8) . . ?
C10 C11 P2 114.8(7) . . ?
C12 C11 P2 132.4(8) . . ?
C13 C12 C17 117.4(9) . . ?
C13 C12 C11 130.6(10) . . ?
C17 C12 C11 111.9(9) . . ?
C14 C13 C12 120.8(12) . . ?
C14 C13 H13 119.6 . . ?
C12 C13 H13 119.6 . . ?
C13 C14 C15 120.2(12) . . ?
C13 C14 H14 119.9 . . ?
C15 C14 H14 119.9 . . ?
C16 C15 C14 122.2(10) . . ?
C16 C15 H15 118.9 . . ?
C14 C15 H15 118.9 . . ?
C15 C16 C17 116.9(11) . . ?
C15 C16 H16 121.6 . . ?
C17 C16 H16 121.6 . . ?
C16 C17 C12 122.5(10) . . ?
C16 C17 S2 125.6(9) . . ?
C12 C17 S2 111.9(7) . . ?
C20 C18 C19 111.2(9) . . ?
C20 C18 P1 113.6(7) . . ?
C19 C18 P1 112.5(7) . . ?
C20 C18 H18 106.3 . . ?
C19 C18 H18 106.3 . . ?
P1 C18 H18 106.3 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 C23 114.5(11) . . ?
C22 C21 P1 112.8(8) . . ?
C23 C21 P1 114.4(8) . . ?
C22 C21 H21 104.6 . . ?
C23 C21 H21 104.6 . . ?
P1 C21 H21 104.6 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C26 C24 C25 110.7(8) . . ?
C26 C24 P2 114.2(7) . . ?
C25 C24 P2 111.6(7) . . ?
C26 C24 H24 106.6 . . ?
C25 C24 H24 106.6 . . ?
P2 C24 H24 106.6 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C31 C30 C35 119.4(12) . . ?
C31 C30 C36 120.8(13) . . ?
C35 C30 C36 119.9(12) . . ?
C30 C31 C32 120.8(10) . . ?
C30 C31 H31 119.6 . . ?
C32 C31 H31 119.6 . . ?
C33 C32 C31 120.3(9) . . ?
C33 C32 H32 119.8 . . ?
C31 C32 H32 119.8 . . ?
C32 C33 C34 119.0(10) . . ?
C32 C33 H33 120.5 . . ?
C34 C33 H33 120.5 . . ?
C33 C34 C35 121.0(11) . . ?
C33 C34 H34 119.5 . . ?
C35 C34 H34 119.5 . . ?
C34 C35 C30 119.4(12) . . ?
C34 C35 H35 120.3 . . ?
C30 C35 H35 120.3 . . ?
C30 C36 H36A 109.5 . . ?
C30 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C30 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C1 Ir1 P1 85.7(3) . . ?
C1 Ir1 P2 84.7(3) . . ?
P1 Ir1 P2 170.45(8) . . ?
C1 Ir1 Cl1 92.0(2) . . ?
P1 Ir1 Cl1 91.52(9) . . ?
P2 Ir1 Cl1 88.91(8) . . ?
C1 Ir1 Cl3 90.4(2) . . ?
P1 Ir1 Cl3 88.87(9) . . ?
P2 Ir1 Cl3 91.09(9) . . ?
Cl1 Ir1 Cl3 177.67(8) . . ?
C1 Ir1 Cl2 178.8(2) . . ?
P1 Ir1 Cl2 93.40(8) . . ?
P2 Ir1 Cl2 96.14(8) . . ?
Cl1 Ir1 Cl2 88.92(9) . . ?
Cl3 Ir1 Cl2 88.76(9) . . ?
C3 P1 C18 104.8(5) . . ?
C3 P1 C21 104.7(5) . . ?
C18 P1 C21 102.1(5) . . ?
C3 P1 Ir1 98.6(3) . . ?
C18 P1 Ir1 121.9(3) . . ?
C21 P1 Ir1 122.1(4) . . ?
C11 P2 C27A 99.8(9) . . ?
C11 P2 C24 106.1(4) . . ?
C27A P2 C24 112.2(10) . . ?
C11 P2 Ir1 98.7(3) . . ?
C27A P2 Ir1 113.3(9) . . ?
C24 P2 Ir1 122.6(3) . . ?
C9 S1 C2 91.4(4) . . ?
C17 S2 C10 92.0(5) . . ?
C28A C27A C29A 110(3) . . ?
C28A C27A P2 118(2) . . ?
C29A C27A P2 109(2) . . ?
C28A C27A H27A 106.3 . . ?
C29A C27A H27A 106.3 . . ?
P2 C27A H27A 106.3 . . ?
C27A C29A H29A 109.5 . . ?
C27A C29A H29B 109.5 . . ?
H29A C29A H29B 109.5 . . ?
C27A C29A H29C 109.5 . . ?
H29A C29A H29C 109.5 . . ?
H29B C29A H29C 109.5 . . ?
C27A C28A H28A 109.5 . . ?
C27A C28A H28B 109.5 . . ?
H28A C28A H28B 109.5 . . ?
C27A C28A H28C 109.5 . . ?
H28A C28A H28C 109.5 . . ?
H28B C28A H28C 109.5 . . ?
C29B C27B C28B 115.0(17) . . ?
C29B C27B H27B 107.3 . . ?
C28B C27B H27B 107.3 . . ?
C27B C29B H29D 109.5 . . ?
C27B C29B H29E 109.5 . . ?
H29D C29B H29E 109.5 . . ?
C27B C29B H29F 109.5 . . ?
H29D C29B H29F 109.5 . . ?
H29E C29B H29F 109.5 . . ?
C27B C28B H28D 109.5 . . ?
C27B C28B H28E 109.5 . . ?
H28D C28B H28E 109.5 . . ?
C27B C28B H28F 109.5 . . ?
H28D C28B H28F 109.5 . . ?
H28E C28B H28F 109.5 . . ?
 
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
C10 C1 C2 C3 172.7(8) . . . . ?
Ir1 C1 C2 C3 -7.3(11) . . . . ?
C10 C1 C2 S1 -6.4(12) . . . . ?
Ir1 C1 C2 S1 173.6(5) . . . . ?
C1 C2 C3 C4 -178.8(8) . . . . ?
S1 C2 C3 C4 0.5(11) . . . . ?
C1 C2 C3 P1 2.8(12) . . . . ?
S1 C2 C3 P1 -178.0(5) . . . . ?
C2 C3 C4 C5 179.9(10) . . . . ?
P1 C3 C4 C5 -2.0(17) . . . . ?
C2 C3 C4 C9 -2.5(12) . . . . ?
P1 C3 C4 C9 175.6(8) . . . . ?
C9 C4 C5 C6 1.0(16) . . . . ?
C3 C4 C5 C6 178.4(10) . . . . ?
C4 C5 C6 C7 -3.0(18) . . . . ?
C5 C6 C7 C8 3(2) . . . . ?
C6 C7 C8 C9 -0.9(19) . . . . ?
C7 C8 C9 C4 -1.1(17) . . . . ?
C7 C8 C9 S1 178.5(9) . . . . ?
C5 C4 C9 C8 1.0(16) . . . . ?
C3 C4 C9 C8 -176.9(10) . . . . ?
C5 C4 C9 S1 -178.6(8) . . . . ?
C3 C4 C9 S1 3.5(11) . . . . ?
C2 C1 C10 C11 176.3(8) . . . . ?
Ir1 C1 C10 C11 -3.7(12) . . . . ?
C2 C1 C10 S2 -6.8(13) . . . . ?
Ir1 C1 C10 S2 173.2(5) . . . . ?
C1 C10 C11 C12 177.4(8) . . . . ?
S2 C10 C11 C12 0.0(10) . . . . ?
C1 C10 C11 P2 -3.2(11) . . . . ?
S2 C10 C11 P2 179.4(5) . . . . ?
C10 C11 C12 C13 -179.9(10) . . . . ?
P2 C11 C12 C13 0.8(17) . . . . ?
C10 C11 C12 C17 -0.3(12) . . . . ?
P2 C11 C12 C17 -179.6(8) . . . . ?
C17 C12 C13 C14 -2.7(16) . . . . ?
C11 C12 C13 C14 177.0(11) . . . . ?
C12 C13 C14 C15 2.1(19) . . . . ?
C13 C14 C15 C16 0(2) . . . . ?
C14 C15 C16 C17 -1.6(18) . . . . ?
C15 C16 C17 C12 0.9(16) . . . . ?
C15 C16 C17 S2 -177.9(9) . . . . ?
C13 C12 C17 C16 1.1(15) . . . . ?
C11 C12 C17 C16 -178.6(9) . . . . ?
C13 C12 C17 S2 -179.9(8) . . . . ?
C11 C12 C17 S2 0.4(11) . . . . ?
C36 C30 C31 C32 178.9(11) . . . . ?
C31 C32 C33 C34 -0.2(5) . . . . ?
C32 C33 C34 C35 0.2(7) . . . . ?
C33 C34 C35 C30 -0.2(7) . . . . ?
C31 C30 C35 C34 0.1(5) . . . . ?
C36 C30 C35 C34 -178.9(11) . . . . ?
C2 C3 P1 C18 -124.5(7) . . . . ?
C4 C3 P1 C18 57.4(10) . . . . ?
C2 C3 P1 C21 128.4(8) . . . . ?
C4 C3 P1 C21 -49.7(11) . . . . ?
C2 C3 P1 Ir1 1.9(7) . . . . ?
C4 C3 P1 Ir1 -176.2(9) . . . . ?
C20 C18 P1 C3 36.3(8) . . . . ?
C19 C18 P1 C3 163.7(7) . . . . ?
C20 C18 P1 C21 145.3(8) . . . . ?
C19 C18 P1 C21 -87.3(8) . . . . ?
C20 C18 P1 Ir1 -74.0(8) . . . . ?
C19 C18 P1 Ir1 53.4(8) . . . . ?
C22 C21 P1 C3 -165.6(9) . . . . ?
C23 C21 P1 C3 -32.4(10) . . . . ?
C22 C21 P1 C18 85.3(10) . . . . ?
C23 C21 P1 C18 -141.5(9) . . . . ?
C22 C21 P1 Ir1 -55.3(11) . . . . ?
C23 C21 P1 Ir1 77.9(9) . . . . ?
C10 C11 P2 C27A -108.9(12) . . . . ?
C12 C11 P2 C27A 70.4(13) . . . . ?
C10 C11 P2 C24 134.4(7) . . . . ?
C12 C11 P2 C24 -46.3(10) . . . . ?
C10 C11 P2 C27B -121.8(10) . . . . ?
C12 C11 P2 C27B 57.5(12) . . . . ?
C10 C11 P2 Ir1 6.7(7) . . . . ?
C12 C11 P2 Ir1 -174.0(9) . . . . ?
C26 C24 P2 C11 -33.3(8) . . . . ?
C25 C24 P2 C11 -159.7(7) . . . . ?
C26 C24 P2 C27A -141.3(12) . . . . ?
C25 C24 P2 C27A 92.2(12) . . . . ?
C26 C24 P2 C27B -146.1(9) . . . . ?
C25 C24 P2 C27B 87.4(10) . . . . ?
C26 C24 P2 Ir1 78.6(7) . . . . ?
C25 C24 P2 Ir1 -47.9(9) . . . . ?
C8 C9 S1 C2 177.6(10) . . . . ?
C4 C9 S1 C2 -2.7(8) . . . . ?
C3 C2 S1 C9 1.3(8) . . . . ?
C1 C2 S1 C9 -179.5(8) . . . . ?
C16 C17 S2 C10 178.6(9) . . . . ?
C12 C17 S2 C10 -0.3(8) . . . . ?
C11 C10 S2 C17 0.2(7) . . . . ?
C1 C10 S2 C17 -176.9(8) . . . . ?
C11 P2 C27A C28A -49(2) . . . . ?
C24 P2 C27A C28A 63(2) . . . . ?
C27B P2 C27A C28A 81(5) . . . . ?
Ir1 P2 C27A C28A -153.0(18) . . . . ?
C11 P2 C27A C29A -175(2) . . . . ?
C24 P2 C27A C29A -63(2) . . . . ?
C27B P2 C27A C29A -46(4) . . . . ?
Ir1 P2 C27A C29A 81(2) . . . . ?
C11 P2 C27B C29B 163.2(15) . . . . ?
C27A P2 C27B C29B 110(6) . . . . ?
C24 P2 C27B C29B -86.9(16) . . . . ?
Ir1 P2 C27B C29B 48.8(17) . . . . ?
C11 P2 C27B C28B 35.9(15) . . . . ?
C27A P2 C27B C28B -18(4) . . . . ?
C24 P2 C27B C28B 145.9(13) . . . . ?
Ir1 P2 C27B C28B -78.4(14) . . . . ?
 
_refine_diff_density_max    1.332
_refine_diff_density_min   -0.798
_refine_diff_density_rms    0.241

_shelxl_version_number 2013-4



#===END
 
data_7_OTf2Cl
 
_audit_creation_method            SHELXL-2013
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety         'C31 H36 Cl F6 Ir O6 P2 S4'
_chemical_formula_sum
 'C31 H36 Cl F6 Ir O6 P2 S4' 
_chemical_formula_weight          1036.43

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0181   0.0091
 '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'
 'O'  'O'   0.0492   0.0322
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'F'  'F'   0.0727   0.0534
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'P'  'P'   0.2955   0.4335
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'S'  'S'   0.3331   0.5567
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Ir'  'Ir'  -4.7710   6.5667
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Cl'  'Cl'   0.3639   0.7018
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            15
_space_group_name_H-M_alt         'C 2/c'
_space_group_name_Hall            '-C 2yc'
 
_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.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x, y, -z+1/2'
 'x+1/2, y+1/2, z'
 '-x+1/2, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y, z-1/2'
 '-x+1/2, -y+1/2, -z'
 'x+1/2, -y+1/2, z-1/2'
 
_cell_length_a                    29.3975(5)
_cell_length_b                    17.9182(3)
_cell_length_c                    23.5916(6)
_cell_angle_alpha                 90
_cell_angle_beta                  122.6490(10)
_cell_angle_gamma                 90
_cell_volume                      10463.3(4)
_cell_formula_units_Z             8
_cell_measurement_temperature     173(2)
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min       ?
_cell_measurement_theta_max       ?
 
_exptl_crystal_description       'Plate'
_exptl_crystal_colour            'Green'
_exptl_crystal_density_meas      '?'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn     1.316          
_exptl_crystal_F_000              4096
_exptl_transmission_factor_min    ?                                             
_exptl_transmission_factor_max    ?                                             
_exptl_crystal_size_max           0.15
_exptl_crystal_size_mid           0.1
_exptl_crystal_size_min           0.1
_exptl_absorpt_coefficient_mu     7.944
_shelx_estimated_absorpt_T_min    0.382
_shelx_estimated_absorpt_T_max    0.504
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.3820
_exptl_absorpt_correction_T_max   0.5038
_exptl_absorpt_process_details    'Sadabs (Sheldrick, 1996)'
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       173(2)
_diffrn_radiation_wavelength      1.54178
_diffrn_radiation_type            CuK\a
_diffrn_source                    ?                       
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number             40850
_diffrn_reflns_av_unetI/netI      0.0368
_diffrn_reflns_av_R_equivalents   0.0486
_diffrn_reflns_limit_h_min        -34
_diffrn_reflns_limit_h_max        33
_diffrn_reflns_limit_k_min        -21
_diffrn_reflns_limit_k_max        21
_diffrn_reflns_limit_l_min        -27
_diffrn_reflns_limit_l_max        28
_diffrn_reflns_theta_min          3.045
_diffrn_reflns_theta_max          66.500
_diffrn_reflns_theta_full         66.500
_diffrn_measured_fraction_theta_max   0.988
_diffrn_measured_fraction_theta_full  0.988
_diffrn_reflns_Laue_measured_fraction_max    0.988
_diffrn_reflns_Laue_measured_fraction_full   0.988
_diffrn_reflns_point_group_measured_fraction_max   0.988
_diffrn_reflns_point_group_measured_fraction_full  0.988
_reflns_number_total              9117
_reflns_number_gt                 7468
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection      'Bruker APEX2'
_computing_cell_refinement      'Bruker SAINT'
_computing_data_reduction       'Bruker SAINT' 
_computing_structure_solution   'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics   'Bruker SHELXTL'
_computing_publication_material 'LinXTL v.  5.3.8'
 
_refine_special_details
;
 ?
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0688P)²+167.4662P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          9117
_refine_ls_number_parameters      468
_refine_ls_number_restraints      474
_refine_ls_R_factor_all           0.0635
_refine_ls_R_factor_gt            0.0498
_refine_ls_wR_factor_ref          0.1443
_refine_ls_wR_factor_gt           0.1303
_refine_ls_goodness_of_fit_ref    1.020
_refine_ls_restrained_S_all       1.004
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
 
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
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Ir1 Ir 0.82117(2) 0.27803(2) 0.39496(2) 0.02468(11) Uani 1 1 d . U . . .
Cl1 Cl 0.77752(7) 0.33132(9) 0.44185(9) 0.0345(4) Uani 1 1 d . U . . .
S1 S 0.96708(7) 0.41400(10) 0.55330(9) 0.0365(4) Uani 1 1 d . U . . .
S2 S 1.00041(7) 0.24777(10) 0.55243(10) 0.0363(4) Uani 1 1 d . U . . .
S3 S 0.70631(7) 0.21567(10) 0.24300(9) 0.0348(4) Uani 1 1 d . U . . .
S4 S 0.89978(7) 0.21015(10) 0.34538(9) 0.0341(4) Uani 1 1 d . U . . .
P1 P 0.82098(7) 0.40122(9) 0.35708(9) 0.0276(4) Uani 1 1 d . U . . .
P2 P 0.83917(6) 0.16859(9) 0.46070(9) 0.0268(3) Uani 1 1 d . U . . .
F1 F 0.60460(19) 0.1797(4) 0.1785(3) 0.0686(16) Uani 1 1 d . U . . .
F2 F 0.6249(2) 0.2762(3) 0.2420(3) 0.0634(14) Uani 1 1 d . U . . .
F3 F 0.64511(19) 0.1662(3) 0.2850(3) 0.0576(13) Uani 1 1 d . U . . .
F4 F 0.8480(3) 0.2322(5) 0.2158(3) 0.096(2) Uani 1 1 d . U . . .
F5 F 0.8461(3) 0.1206(4) 0.2431(3) 0.0872(19) Uani 1 1 d . U . . .
F6 F 0.9180(3) 0.1651(4) 0.2556(4) 0.091(2) Uani 1 1 d . U . . .
O1 O 0.74018(19) 0.2461(3) 0.3107(3) 0.0380(11) Uani 1 1 d . U . . .
O2 O 0.6952(3) 0.2660(4) 0.1903(3) 0.0571(16) Uani 1 1 d . U . . .
O3 O 0.7190(2) 0.1409(3) 0.2359(3) 0.0450(13) Uani 1 1 d . U . . .
O4 O 0.8470(2) 0.2248(3) 0.3366(3) 0.0343(11) Uani 1 1 d . U . . .
O5 O 0.9312(2) 0.2758(3) 0.3575(3) 0.0506(14) Uani 1 1 d . U . . .
O6 O 0.9271(2) 0.1462(3) 0.3855(3) 0.0474(13) Uani 1 1 d . U . . .
C1 C 0.8940(2) 0.3035(4) 0.4678(3) 0.0269(13) Uani 1 1 d . U . . .
C2 C 0.9096(3) 0.3797(4) 0.4803(3) 0.0310(14) Uani 1 1 d . U . . .
C3 C 0.8790(3) 0.4361(4) 0.4359(4) 0.0297(13) Uani 1 1 d . U . . .
C4 C 0.9006(3) 0.5090(4) 0.4600(4) 0.0329(14) Uani 1 1 d . U . . .
C5 C 0.8808(3) 0.5797(4) 0.4305(4) 0.0391(16) Uani 1 1 d . U . . .
H5 H 0.8491 0.5839 0.3867 0.047 Uiso 1 1 calc R U . . .
C6 C 0.9083(3) 0.6422(4) 0.4663(5) 0.0454(18) Uani 1 1 d . U . . .
H6 H 0.8949 0.6899 0.4468 0.054 Uiso 1 1 calc R U . . .
C7 C 0.9553(3) 0.6378(4) 0.5304(5) 0.0472(19) Uani 1 1 d . U . . .
H7 H 0.9730 0.6823 0.5539 0.057 Uiso 1 1 calc R U . . .
C8 C 0.9766(3) 0.5689(4) 0.5603(4) 0.0444(18) Uani 1 1 d . U . . .
H8 H 1.0089 0.5655 0.6036 0.053 Uiso 1 1 calc R U . . .
C9 C 0.9489(3) 0.5051(4) 0.5246(4) 0.0369(15) Uani 1 1 d . U . . .
C10 C 0.9302(3) 0.2424(4) 0.5042(4) 0.0297(13) Uani 1 1 d . U . . .
C11 C 0.9119(3) 0.1705(4) 0.5018(3) 0.0264(13) Uani 1 1 d . U . . .
C12 C 0.9543(3) 0.1182(4) 0.5381(4) 0.0314(14) Uani 1 1 d . U . . .
C13 C 0.9526(3) 0.0402(4) 0.5445(4) 0.0380(16) Uani 1 1 d . U . . .
H13 H 0.9189 0.0149 0.5233 0.046 Uiso 1 1 calc R U . . .
C14 C 1.0000(3) 0.0008(5) 0.5814(4) 0.0429(17) Uani 1 1 d . U . . .
H14 H 0.9989 -0.0516 0.5868 0.051 Uiso 1 1 calc R U . . .
C15 C 1.0497(3) 0.0373(5) 0.6110(4) 0.0443(18) Uani 1 1 d . U . . .
H15 H 1.0820 0.0090 0.6357 0.053 Uiso 1 1 calc R U . . .
C16 C 1.0530(3) 0.1123(5) 0.6054(4) 0.0415(17) Uani 1 1 d . U . . .
H16 H 1.0871 0.1365 0.6264 0.050 Uiso 1 1 calc R U . . .
C17 C 1.0053(3) 0.1529(4) 0.5681(4) 0.0345(15) Uani 1 1 d . U . . .
C18 C 0.7629(3) 0.4662(4) 0.3261(4) 0.0354(15) Uani 1 1 d . U . . .
H18 H 0.7672 0.5056 0.2993 0.042 Uiso 1 1 calc R U . . .
C19 C 0.7600(3) 0.5072(4) 0.3819(4) 0.0382(16) Uani 1 1 d . U . . .
H19A H 0.7368 0.5512 0.3627 0.057 Uiso 1 1 calc R U . . .
H19B H 0.7964 0.5228 0.4177 0.057 Uiso 1 1 calc R U . . .
H19C H 0.7451 0.4735 0.4006 0.057 Uiso 1 1 calc R U . . .
C20 C 0.7099(3) 0.4272(4) 0.2785(4) 0.0423(18) Uani 1 1 d . U . . .
H20A H 0.7036 0.3887 0.3030 0.063 Uiso 1 1 calc R U . . .
H20B H 0.7114 0.4040 0.2419 0.063 Uiso 1 1 calc R U . . .
H20C H 0.6804 0.4637 0.2597 0.063 Uiso 1 1 calc R U . . .
C21 C 0.8429(3) 0.4093(4) 0.2971(4) 0.0357(15) Uani 1 1 d . U . . .
H21 H 0.8732 0.3729 0.3122 0.043 Uiso 1 1 calc R U . . .
C22 C 0.7971(4) 0.3844(5) 0.2263(4) 0.049(2) Uani 1 1 d . U . . .
H22A H 0.7664 0.4185 0.2096 0.074 Uiso 1 1 calc R U . . .
H22B H 0.7858 0.3336 0.2287 0.074 Uiso 1 1 calc R U . . .
H22C H 0.8101 0.3851 0.1958 0.074 Uiso 1 1 calc R U . . .
C23 C 0.8648(4) 0.4856(4) 0.2949(4) 0.0456(19) Uani 1 1 d . U . . .
H23A H 0.8755 0.4847 0.2622 0.068 Uiso 1 1 calc R U . . .
H23B H 0.8962 0.4977 0.3396 0.068 Uiso 1 1 calc R U . . .
H23C H 0.8366 0.5234 0.2816 0.068 Uiso 1 1 calc R U . . .
C24 C 0.8303(3) 0.1780(4) 0.5325(4) 0.0359(15) Uani 1 1 d . U . . .
H24 H 0.7917 0.1915 0.5134 0.043 Uiso 1 1 calc R U . . .
C25 C 0.8411(4) 0.1053(5) 0.5716(4) 0.048(2) Uani 1 1 d . U . . .
H25A H 0.8780 0.0886 0.5887 0.072 Uiso 1 1 calc R U . . .
H25B H 0.8154 0.0671 0.5417 0.072 Uiso 1 1 calc R U . . .
H25C H 0.8366 0.1137 0.6094 0.072 Uiso 1 1 calc R U . . .
C26 C 0.8648(4) 0.2404(5) 0.5809(4) 0.0485(19) Uani 1 1 d . U . . .
H26A H 0.8565 0.2459 0.6157 0.073 Uiso 1 1 calc R U . . .
H26B H 0.8569 0.2874 0.5559 0.073 Uiso 1 1 calc R U . . .
H26C H 0.9031 0.2281 0.6020 0.073 Uiso 1 1 calc R U . . .
C27 C 0.8128(3) 0.0757(4) 0.4259(4) 0.0365(15) Uani 1 1 d . U . . .
H27 H 0.8309 0.0389 0.4637 0.044 Uiso 1 1 calc R U . . .
C28 C 0.7522(3) 0.0732(5) 0.3977(5) 0.0463(19) Uani 1 1 d . U . . .
H28A H 0.7331 0.1063 0.3586 0.070 Uiso 1 1 calc R U . . .
H28B H 0.7457 0.0896 0.4324 0.070 Uiso 1 1 calc R U . . .
H28C H 0.7389 0.0220 0.3841 0.070 Uiso 1 1 calc R U . . .
C29 C 0.8244(3) 0.0529(5) 0.3733(5) 0.0466(18) Uani 1 1 d . U . . .
H29A H 0.8147 0.0004 0.3614 0.070 Uiso 1 1 calc R U . . .
H29B H 0.8630 0.0596 0.3913 0.070 Uiso 1 1 calc R U . . .
H29C H 0.8032 0.0840 0.3331 0.070 Uiso 1 1 calc R U . . .
C30 C 0.6418(3) 0.2096(5) 0.2368(4) 0.0424(16) Uani 1 1 d . U . . .
C31 C 0.8758(4) 0.1806(6) 0.2592(5) 0.059(2) Uani 1 1 d . U . . .
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1 -0.007  0.139  0.243      1915       778 ' '
   2 -0.011 -0.155  0.739      1915       777 ' '
_platon_squeeze_details
;PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure   ! 
RESPONSE: During the 
refinement of the structure, electron density peaks were located 
that were believed to be highly disordered 
solvent molecules (possibly toluene and pentane). Attempts 
made to model the solvent molecule were not successful. 
The SQUEEZE option in PLATON (Spek, 2009) indicated there was a 
large solvent cavity 3832.7 Ang^3. In the final cycles of refinement, 
this contribution (1555) to the 
electron density was removed from the observed data. The 
density, the F(000) value, the molecular weight and the formula are 
given without taking into account the results obtained with the 
SQUEEZE option PLATON (Spek, 2009). Similar treatments of disordered 
solvent molecules were carried out by Stähler et al. (2001), 
Cox et al. (2003), Mohamed et al. (2003) and Athimoolam et al. (2005). 
References: 
  
Spek, A. L. (2009). Acta Cryst. D65, 148--155.
  
Athimoolam, S., Kumar, J., Ramakrishnan, V. & Rajaram, R.K. (2005). 
Acta Cryst. E61, m2014-m2017. 
  
Cox, J.P., Kumarasammy, Y., Nahar, L., Sarkar D.S. & Shoeb, M. 
(2003). Acta Cryst. E59, o975-o977. 
  
Mohamed, A.A., Krause Bauer, A.J., Bruce, E.A. & Bruce M.R.M. 
(2003). Acta Cryst. C59, m84-m86. 
  
Stahler, R., Nather, C. & Bensch, W. (2001). Acta Cryst. 
C57, 26-27.
;
 
 
_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_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
Ir1 C1 1.943(6) . ?
Ir1 O4 2.123(5) . ?
Ir1 O1 2.200(5) . ?
Ir1 Cl1 2.3051(16) . ?
Ir1 P2 2.3758(16) . ?
Ir1 P1 2.3803(17) . ?
S1 C9 1.737(8) . ?
S1 C2 1.750(7) . ?
S2 C17 1.729(8) . ?
S2 C10 1.740(7) . ?
S3 O2 1.424(6) . ?
S3 O3 1.425(6) . ?
S3 O1 1.458(5) . ?
S3 C30 1.826(8) . ?
S4 O6 1.427(6) . ?
S4 O5 1.427(6) . ?
S4 O4 1.474(5) . ?
S4 C31 1.834(9) . ?
P1 C3 1.826(7) . ?
P1 C21 1.851(7) . ?
P1 C18 1.860(7) . ?
P2 C11 1.810(7) . ?
P2 C27 1.833(7) . ?
P2 C24 1.856(7) . ?
F1 C30 1.323(9) . ?
F2 C30 1.324(9) . ?
F3 C30 1.336(10) . ?
F4 C31 1.292(12) . ?
F5 C31 1.307(12) . ?
F6 C31 1.318(12) . ?
C1 C2 1.420(10) . ?
C1 C10 1.442(9) . ?
C2 C3 1.382(10) . ?
C3 C4 1.430(10) . ?
C4 C5 1.410(10) . ?
C4 C9 1.418(10) . ?
C5 C6 1.374(11) . ?
C5 H5 0.9500 . ?
C6 C7 1.396(12) . ?
C6 H6 0.9500 . ?
C7 C8 1.391(12) . ?
C7 H7 0.9500 . ?
C8 C9 1.392(10) . ?
C8 H8 0.9500 . ?
C10 C11 1.385(10) . ?
C11 C12 1.419(9) . ?
C12 C13 1.410(10) . ?
C12 C17 1.412(10) . ?
C13 C14 1.373(10) . ?
C13 H13 0.9500 . ?
C14 C15 1.396(12) . ?
C14 H14 0.9500 . ?
C15 C16 1.360(12) . ?
C15 H15 0.9500 . ?
C16 C17 1.391(10) . ?
C16 H16 0.9500 . ?
C18 C20 1.513(10) . ?
C18 C19 1.548(11) . ?
C18 H18 1.0000 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C23 1.523(11) . ?
C21 C22 1.540(11) . ?
C21 H21 1.0000 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C25 1.526(11) . ?
C24 C26 1.527(12) . ?
C24 H24 1.0000 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C29 1.511(12) . ?
C27 C28 1.529(10) . ?
C27 H27 1.0000 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
 
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
C1 Ir1 O4 94.0(2) . . ?
C1 Ir1 O1 177.6(2) . . ?
O4 Ir1 O1 83.6(2) . . ?
C1 Ir1 Cl1 96.4(2) . . ?
O4 Ir1 Cl1 169.57(14) . . ?
O1 Ir1 Cl1 85.97(15) . . ?
C1 Ir1 P2 82.3(2) . . ?
O4 Ir1 P2 91.19(14) . . ?
O1 Ir1 P2 97.24(14) . . ?
Cl1 Ir1 P2 90.82(6) . . ?
C1 Ir1 P1 83.8(2) . . ?
O4 Ir1 P1 95.88(14) . . ?
O1 Ir1 P1 96.90(14) . . ?
Cl1 Ir1 P1 84.65(6) . . ?
P2 Ir1 P1 164.80(6) . . ?
C9 S1 C2 90.9(3) . . ?
C17 S2 C10 91.1(3) . . ?
O2 S3 O3 116.3(4) . . ?
O2 S3 O1 114.8(4) . . ?
O3 S3 O1 114.4(3) . . ?
O2 S3 C30 103.2(4) . . ?
O3 S3 C30 105.2(4) . . ?
O1 S3 C30 100.1(3) . . ?
O6 S4 O5 117.3(4) . . ?
O6 S4 O4 114.1(3) . . ?
O5 S4 O4 113.6(3) . . ?
O6 S4 C31 104.2(4) . . ?
O5 S4 C31 106.3(5) . . ?
O4 S4 C31 98.7(4) . . ?
C3 P1 C21 103.4(3) . . ?
C3 P1 C18 109.9(3) . . ?
C21 P1 C18 106.0(3) . . ?
C3 P1 Ir1 97.1(2) . . ?
C21 P1 Ir1 115.4(2) . . ?
C18 P1 Ir1 123.0(2) . . ?
C11 P2 C27 110.5(3) . . ?
C11 P2 C24 102.5(3) . . ?
C27 P2 C24 104.9(4) . . ?
C11 P2 Ir1 96.7(2) . . ?
C27 P2 Ir1 124.4(3) . . ?
C24 P2 Ir1 115.4(2) . . ?
S3 O1 Ir1 148.6(3) . . ?
S4 O4 Ir1 135.0(3) . . ?
C2 C1 C10 123.7(6) . . ?
C2 C1 Ir1 119.1(5) . . ?
C10 C1 Ir1 117.1(5) . . ?
C3 C2 C1 122.8(6) . . ?
C3 C2 S1 112.2(5) . . ?
C1 C2 S1 125.0(5) . . ?
C2 C3 C4 113.5(6) . . ?
C2 C3 P1 112.9(5) . . ?
C4 C3 P1 133.5(5) . . ?
C5 C4 C9 118.9(7) . . ?
C5 C4 C3 130.3(7) . . ?
C9 C4 C3 110.8(6) . . ?
C6 C5 C4 118.7(7) . . ?
C6 C5 H5 120.7 . . ?
C4 C5 H5 120.7 . . ?
C5 C6 C7 122.1(8) . . ?
C5 C6 H6 119.0 . . ?
C7 C6 H6 119.0 . . ?
C8 C7 C6 120.6(7) . . ?
C8 C7 H7 119.7 . . ?
C6 C7 H7 119.7 . . ?
C7 C8 C9 117.8(8) . . ?
C7 C8 H8 121.1 . . ?
C9 C8 H8 121.1 . . ?
C8 C9 C4 121.9(7) . . ?
C8 C9 S1 125.4(6) . . ?
C4 C9 S1 112.6(5) . . ?
C11 C10 C1 122.4(6) . . ?
C11 C10 S2 112.0(5) . . ?
C1 C10 S2 125.5(5) . . ?
C10 C11 C12 113.3(6) . . ?
C10 C11 P2 111.1(5) . . ?
C12 C11 P2 135.2(5) . . ?
C13 C12 C17 118.1(6) . . ?
C13 C12 C11 130.6(7) . . ?
C17 C12 C11 111.2(6) . . ?
C14 C13 C12 119.8(7) . . ?
C14 C13 H13 120.1 . . ?
C12 C13 H13 120.1 . . ?
C13 C14 C15 120.3(7) . . ?
C13 C14 H14 119.8 . . ?
C15 C14 H14 119.8 . . ?
C16 C15 C14 121.7(7) . . ?
C16 C15 H15 119.1 . . ?
C14 C15 H15 119.1 . . ?
C15 C16 C17 118.5(8) . . ?
C15 C16 H16 120.8 . . ?
C17 C16 H16 120.8 . . ?
C16 C17 C12 121.5(7) . . ?
C16 C17 S2 126.0(6) . . ?
C12 C17 S2 112.5(5) . . ?
C20 C18 C19 110.1(6) . . ?
C20 C18 P1 111.2(5) . . ?
C19 C18 P1 115.0(5) . . ?
C20 C18 H18 106.7 . . ?
C19 C18 H18 106.7 . . ?
P1 C18 H18 106.7 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C23 C21 C22 111.2(6) . . ?
C23 C21 P1 115.0(5) . . ?
C22 C21 P1 110.2(5) . . ?
C23 C21 H21 106.7 . . ?
C22 C21 H21 106.7 . . ?
P1 C21 H21 106.7 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C25 C24 C26 109.7(7) . . ?
C25 C24 P2 112.8(5) . . ?
C26 C24 P2 112.6(5) . . ?
C25 C24 H24 107.1 . . ?
C26 C24 H24 107.1 . . ?
P2 C24 H24 107.1 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C29 C27 C28 111.3(7) . . ?
C29 C27 P2 112.6(5) . . ?
C28 C27 P2 109.5(5) . . ?
C29 C27 H27 107.8 . . ?
C28 C27 H27 107.8 . . ?
P2 C27 H27 107.8 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
F1 C30 F2 108.7(7) . . ?
F1 C30 F3 106.9(7) . . ?
F2 C30 F3 107.8(7) . . ?
F1 C30 S3 110.3(6) . . ?
F2 C30 S3 111.3(6) . . ?
F3 C30 S3 111.8(5) . . ?
F4 C31 F5 108.7(9) . . ?
F4 C31 F6 108.3(9) . . ?
F5 C31 F6 108.3(8) . . ?
F4 C31 S4 111.8(7) . . ?
F5 C31 S4 110.9(7) . . ?
F6 C31 S4 108.7(7) . . ?
 
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
O2 S3 O1 Ir1 -76.8(7) . . . . ?
O3 S3 O1 Ir1 61.5(7) . . . . ?
C30 S3 O1 Ir1 173.4(6) . . . . ?
O6 S4 O4 Ir1 82.1(5) . . . . ?
O5 S4 O4 Ir1 -55.9(5) . . . . ?
C31 S4 O4 Ir1 -168.0(5) . . . . ?
C10 C1 C2 C3 164.7(7) . . . . ?
Ir1 C1 C2 C3 -12.1(9) . . . . ?
C10 C1 C2 S1 -17.8(10) . . . . ?
Ir1 C1 C2 S1 165.4(4) . . . . ?
C9 S1 C2 C3 1.4(6) . . . . ?
C9 S1 C2 C1 -176.4(7) . . . . ?
C1 C2 C3 C4 176.7(6) . . . . ?
S1 C2 C3 C4 -1.1(8) . . . . ?
C1 C2 C3 P1 -5.7(9) . . . . ?
S1 C2 C3 P1 176.5(4) . . . . ?
C21 P1 C3 C2 -102.5(6) . . . . ?
C18 P1 C3 C2 144.7(5) . . . . ?
Ir1 P1 C3 C2 15.8(5) . . . . ?
C21 P1 C3 C4 74.5(8) . . . . ?
C18 P1 C3 C4 -38.3(8) . . . . ?
Ir1 P1 C3 C4 -167.2(7) . . . . ?
C2 C3 C4 C5 -178.6(8) . . . . ?
P1 C3 C4 C5 4.4(13) . . . . ?
C2 C3 C4 C9 0.1(9) . . . . ?
P1 C3 C4 C9 -176.8(6) . . . . ?
C9 C4 C5 C6 -1.9(11) . . . . ?
C3 C4 C5 C6 176.8(8) . . . . ?
C4 C5 C6 C7 0.7(13) . . . . ?
C5 C6 C7 C8 0.8(14) . . . . ?
C6 C7 C8 C9 -1.1(13) . . . . ?
C7 C8 C9 C4 -0.1(12) . . . . ?
C7 C8 C9 S1 -178.1(7) . . . . ?
C5 C4 C9 C8 1.6(12) . . . . ?
C3 C4 C9 C8 -177.3(7) . . . . ?
C5 C4 C9 S1 179.8(6) . . . . ?
C3 C4 C9 S1 0.9(8) . . . . ?
C2 S1 C9 C8 176.9(8) . . . . ?
C2 S1 C9 C4 -1.3(6) . . . . ?
C2 C1 C10 C11 165.6(7) . . . . ?
Ir1 C1 C10 C11 -17.6(9) . . . . ?
C2 C1 C10 S2 -17.3(10) . . . . ?
Ir1 C1 C10 S2 159.5(4) . . . . ?
C17 S2 C10 C11 1.1(6) . . . . ?
C17 S2 C10 C1 -176.2(7) . . . . ?
C1 C10 C11 C12 176.6(6) . . . . ?
S2 C10 C11 C12 -0.8(8) . . . . ?
C1 C10 C11 P2 -10.0(9) . . . . ?
S2 C10 C11 P2 172.6(3) . . . . ?
C27 P2 C11 C10 156.0(5) . . . . ?
C24 P2 C11 C10 -92.7(5) . . . . ?
Ir1 P2 C11 C10 25.3(5) . . . . ?
C27 P2 C11 C12 -32.7(8) . . . . ?
C24 P2 C11 C12 78.7(8) . . . . ?
Ir1 P2 C11 C12 -163.3(7) . . . . ?
C10 C11 C12 C13 -175.7(7) . . . . ?
P2 C11 C12 C13 13.0(13) . . . . ?
C10 C11 C12 C17 0.0(9) . . . . ?
P2 C11 C12 C17 -171.3(6) . . . . ?
C17 C12 C13 C14 2.5(11) . . . . ?
C11 C12 C13 C14 178.0(7) . . . . ?
C12 C13 C14 C15 -1.8(12) . . . . ?
C13 C14 C15 C16 1.1(13) . . . . ?
C14 C15 C16 C17 -1.1(13) . . . . ?
C15 C16 C17 C12 1.8(12) . . . . ?
C15 C16 C17 S2 -177.9(7) . . . . ?
C13 C12 C17 C16 -2.6(11) . . . . ?
C11 C12 C17 C16 -178.9(7) . . . . ?
C13 C12 C17 S2 177.2(6) . . . . ?
C11 C12 C17 S2 0.8(8) . . . . ?
C10 S2 C17 C16 178.6(7) . . . . ?
C10 S2 C17 C12 -1.1(6) . . . . ?
C3 P1 C18 C20 -158.1(6) . . . . ?
C21 P1 C18 C20 90.8(6) . . . . ?
Ir1 P1 C18 C20 -45.0(7) . . . . ?
C3 P1 C18 C19 -32.1(6) . . . . ?
C21 P1 C18 C19 -143.2(5) . . . . ?
Ir1 P1 C18 C19 81.0(6) . . . . ?
C3 P1 C21 C23 -51.3(6) . . . . ?
C18 P1 C21 C23 64.3(6) . . . . ?
Ir1 P1 C21 C23 -156.0(5) . . . . ?
C3 P1 C21 C22 -178.0(5) . . . . ?
C18 P1 C21 C22 -62.3(6) . . . . ?
Ir1 P1 C21 C22 77.3(6) . . . . ?
C11 P2 C24 C25 -77.7(6) . . . . ?
C27 P2 C24 C25 37.7(6) . . . . ?
Ir1 P2 C24 C25 178.5(5) . . . . ?
C11 P2 C24 C26 47.1(6) . . . . ?
C27 P2 C24 C26 162.5(5) . . . . ?
Ir1 P2 C24 C26 -56.7(6) . . . . ?
C11 P2 C27 C29 -61.3(6) . . . . ?
C24 P2 C27 C29 -171.1(5) . . . . ?
Ir1 P2 C27 C29 52.7(6) . . . . ?
C11 P2 C27 C28 174.4(5) . . . . ?
C24 P2 C27 C28 64.6(6) . . . . ?
Ir1 P2 C27 C28 -71.6(6) . . . . ?
O2 S3 C30 F1 63.8(7) . . . . ?
O3 S3 C30 F1 -58.6(7) . . . . ?
O1 S3 C30 F1 -177.5(6) . . . . ?
O2 S3 C30 F2 -57.0(7) . . . . ?
O3 S3 C30 F2 -179.4(6) . . . . ?
O1 S3 C30 F2 61.8(6) . . . . ?
O2 S3 C30 F3 -177.5(6) . . . . ?
O3 S3 C30 F3 60.1(6) . . . . ?
O1 S3 C30 F3 -58.8(6) . . . . ?
O6 S4 C31 F4 177.5(8) . . . . ?
O5 S4 C31 F4 -58.1(9) . . . . ?
O4 S4 C31 F4 59.7(9) . . . . ?
O6 S4 C31 F5 56.0(8) . . . . ?
O5 S4 C31 F5 -179.6(7) . . . . ?
O4 S4 C31 F5 -61.8(8) . . . . ?
O6 S4 C31 F6 -63.0(8) . . . . ?
O5 S4 C31 F6 61.5(8) . . . . ?
O4 S4 C31 F6 179.3(7) . . . . ?
 
_refine_diff_density_max    2.243
_refine_diff_density_min   -0.725
_refine_diff_density_rms    0.167

_shelxl_version_number 2013-4



#===END

data_8
 
_audit_creation_method            SHELXL-2013
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety         'C30 H38 Cl F3 Ir O4 P2 S3, C O3 S, 3(F)'
_chemical_formula_sum
 'C31 H38 Cl F6 Ir O7 P2 S4' 
_chemical_formula_weight          1054.44

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0181   0.0091
 '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'
 'Cl'  'Cl'   0.3639   0.7018
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'F'  'F'   0.0727   0.0534
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Ir'  'Ir'  -4.7710   6.5667
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0492   0.0322
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'P'  'P'   0.2955   0.4335
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'S'  'S'   0.3331   0.5567
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            15
_space_group_name_H-M_alt         'C 2/c'
_space_group_name_Hall            '-C 2yc'
 
_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.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x, y, -z+1/2'
 'x+1/2, y+1/2, z'
 '-x+1/2, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y, z-1/2'
 '-x+1/2, -y+1/2, -z'
 'x+1/2, -y+1/2, z-1/2'
 
_cell_length_a                    27.4764(5)
_cell_length_b                    20.4688(4)
_cell_length_c                    18.4422(4)
_cell_angle_alpha                 90
_cell_angle_beta                  112.8740(10)
_cell_angle_gamma                 90
_cell_volume                      9556.4(3)
_cell_formula_units_Z             8
_cell_measurement_temperature     173(2)
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min       ?
_cell_measurement_theta_max       ?
 
_exptl_crystal_description       'needles'
_exptl_crystal_colour            'Purple'
_exptl_crystal_density_meas      '?'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn     1.466          
_exptl_crystal_F_000              4176
_exptl_transmission_factor_min    ?                                             
_exptl_transmission_factor_max    ?                                             
_exptl_crystal_size_max           0.18
_exptl_crystal_size_mid           0.09
_exptl_crystal_size_min           0.09
_exptl_absorpt_coefficient_mu     8.724
_shelx_estimated_absorpt_T_min    ? 
_shelx_estimated_absorpt_T_max    ? 
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.4746
_exptl_absorpt_correction_T_max   0.7531
_exptl_absorpt_process_details    'Sadabs (Sheldrick, 1996)'
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       173(2)
_diffrn_radiation_wavelength      1.54178
_diffrn_radiation_type            CuK\a
_diffrn_source                    ?                       
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number             33628
_diffrn_reflns_av_unetI/netI      0.0315
_diffrn_reflns_av_R_equivalents   0.0398
_diffrn_reflns_limit_h_min        -33
_diffrn_reflns_limit_h_max        32
_diffrn_reflns_limit_k_min        -23
_diffrn_reflns_limit_k_max        24
_diffrn_reflns_limit_l_min        -22
_diffrn_reflns_limit_l_max        21
_diffrn_reflns_theta_min          3.308
_diffrn_reflns_theta_max          68.419
_diffrn_reflns_theta_full         67.679
_diffrn_measured_fraction_theta_max   0.982
_diffrn_measured_fraction_theta_full  0.983
_diffrn_reflns_Laue_measured_fraction_max    0.982
_diffrn_reflns_Laue_measured_fraction_full   0.983
_diffrn_reflns_point_group_measured_fraction_max   0.982
_diffrn_reflns_point_group_measured_fraction_full  0.983
_reflns_number_total              8633
_reflns_number_gt                 7652
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection      'Bruker APEX2'
_computing_cell_refinement      'Bruker SAINT'
_computing_data_reduction       'Bruker SAINT' 
_computing_structure_solution   'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics   'Bruker SHELXTL'
_computing_publication_material 'LinXTL v.  5.3.7'
 
_refine_special_details
;
 ?
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0637P)²+27.0634P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    mixed
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          8633
_refine_ls_number_parameters      525
_refine_ls_number_restraints      150
_refine_ls_R_factor_all           0.0437
_refine_ls_R_factor_gt            0.0391
_refine_ls_wR_factor_ref          0.1089
_refine_ls_wR_factor_gt           0.1051
_refine_ls_goodness_of_fit_ref    1.037
_refine_ls_restrained_S_all       1.070
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
 
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
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Ir1 Ir 0.88929(2) 0.17338(2) 0.52431(2) 0.03709(8) Uani 1 1 d . . . . .
Cl1 Cl 0.96445(5) 0.16550(7) 0.63928(7) 0.0545(3) Uani 1 1 d . . . . .
S1 S 0.99083(4) 0.11758(6) 0.38497(7) 0.0440(3) Uani 1 1 d . . . . .
S2 S 0.93689(4) -0.00196(6) 0.40749(7) 0.0431(2) Uani 1 1 d . . . . .
S3 S 0.81058(4) 0.24699(6) 0.61238(7) 0.0436(3) Uani 1 1 d . . . . .
P1 P 0.92572(5) 0.26522(6) 0.48591(8) 0.0469(3) Uani 1 1 d . . . . .
P2 P 0.85653(4) 0.07258(6) 0.54896(7) 0.0396(2) Uani 1 1 d . . . . .
F1 F 0.8144(2) 0.2894(3) 0.7464(3) 0.125(2) Uani 1 1 d . U . . .
F2 F 0.87082(18) 0.33432(19) 0.7103(2) 0.0770(11) Uani 1 1 d . U . . .
F3 F 0.8836(2) 0.2362(2) 0.7528(2) 0.1058(16) Uani 1 1 d . U . . .
O1 O 0.81991(12) 0.18884(16) 0.42439(19) 0.0421(7) Uani 1 1 d . . . . .
H1 H 0.8202 0.1697 0.3804 0.063 Uiso 1 1 d R U . . .
H2 H 0.7892 0.1912 0.4243 0.063 Uiso 1 1 d R U . . .
O2 O 0.85255(14) 0.23814(18) 0.5833(2) 0.0513(8) Uani 1 1 d . . . . .
O3 O 0.78594(15) 0.1885(2) 0.6225(2) 0.0578(9) Uani 1 1 d . . . . .
O4 O 0.77609(14) 0.29999(19) 0.5737(2) 0.0534(9) Uani 1 1 d . . . . .
C1 C 0.92236(16) 0.1216(2) 0.4665(2) 0.0363(9) Uani 1 1 d . . . . .
C2 C 0.95574(17) 0.1553(2) 0.4349(3) 0.0406(10) Uani 1 1 d . . . . .
C3 C 0.96409(18) 0.2222(3) 0.4403(3) 0.0454(11) Uani 1 1 d . . . . .
C4 C 0.9997(2) 0.2437(3) 0.4061(3) 0.0516(12) Uani 1 1 d . . . . .
C5 C 1.0192(3) 0.3062(3) 0.4028(5) 0.0751(19) Uani 1 1 d . . . . .
H5B H 1.0083 0.3423 0.4252 0.090 Uiso 1 1 calc R U . . .
C6 C 1.0541(3) 0.3153(4) 0.3671(5) 0.084(2) Uani 1 1 d . . . . .
H6B H 1.0675 0.3577 0.3653 0.101 Uiso 1 1 calc R U . . .
C7 C 1.0703(3) 0.2623(4) 0.3331(5) 0.079(2) Uani 1 1 d . . . . .
H7B H 1.0935 0.2700 0.3071 0.094 Uiso 1 1 calc R U . . .
C8 C 1.0532(2) 0.1999(3) 0.3369(3) 0.0557(13) Uani 1 1 d . . . . .
H8A H 1.0653 0.1640 0.3158 0.067 Uiso 1 1 calc R U . . .
C9 C 1.0173(2) 0.1913(3) 0.3727(3) 0.0487(11) Uani 1 1 d . . . . .
C10 C 0.91238(17) 0.0522(2) 0.4585(3) 0.0391(9) Uani 1 1 d . . . . .
C11 C 0.88212(18) 0.0205(2) 0.4918(3) 0.0406(10) Uani 1 1 d . . . . .
C12 C 0.87754(19) -0.0481(2) 0.4778(3) 0.0437(10) Uani 1 1 d . . . . .
C13 C 0.8511(2) -0.0959(3) 0.5027(3) 0.0565(13) Uani 1 1 d . . . . .
H13A H 0.8327 -0.0845 0.5351 0.068 Uiso 1 1 calc R U . . .
C14 C 0.8521(3) -0.1593(3) 0.4798(4) 0.0591(14) Uani 1 1 d . . . . .
H14A H 0.8336 -0.1917 0.4958 0.071 Uiso 1 1 calc R U . . .
C15 C 0.8799(3) -0.1773(3) 0.4333(3) 0.0569(13) Uani 1 1 d . . . . .
H15A H 0.8798 -0.2218 0.4184 0.068 Uiso 1 1 calc R U . . .
C16 C 0.9070(2) -0.1323(2) 0.4087(3) 0.0489(11) Uani 1 1 d . . . . .
H16A H 0.9261 -0.1447 0.3775 0.059 Uiso 1 1 calc R U . . .
C17 C 0.90568(19) -0.0674(2) 0.4312(3) 0.0436(10) Uani 1 1 d . . . . .
C18 C 0.8751(2) 0.3124(3) 0.4035(4) 0.0572(13) Uani 1 1 d . . . . .
H18A H 0.8508 0.2792 0.3678 0.069 Uiso 1 1 calc R U . . .
C19 C 0.8954(3) 0.3528(4) 0.3531(5) 0.0787(19) Uani 1 1 d . . . . .
H19A H 0.8656 0.3718 0.3095 0.118 Uiso 1 1 calc R U . . .
H19B H 0.9160 0.3250 0.3322 0.118 Uiso 1 1 calc R U . . .
H19C H 0.9180 0.3878 0.3849 0.118 Uiso 1 1 calc R U . . .
C20 C 0.8414(3) 0.3537(3) 0.4363(4) 0.0700(17) Uani 1 1 d . . . . .
H20A H 0.8123 0.3741 0.3926 0.105 Uiso 1 1 calc R U . . .
H20B H 0.8634 0.3878 0.4710 0.105 Uiso 1 1 calc R U . . .
H20C H 0.8270 0.3256 0.4661 0.105 Uiso 1 1 calc R U . . .
C21 C 0.9678(3) 0.3267(3) 0.5549(4) 0.0650(16) Uani 1 1 d . . . . .
H21A H 0.9673 0.3673 0.5245 0.078 Uiso 1 1 calc R U . . .
C22 C 1.0254(3) 0.3044(4) 0.5958(5) 0.084(2) Uani 1 1 d . . . . .
H22A H 1.0452 0.3366 0.6356 0.126 Uiso 1 1 calc R U . . .
H22B H 1.0413 0.3002 0.5567 0.126 Uiso 1 1 calc R U . . .
H22C H 1.0265 0.2620 0.6211 0.126 Uiso 1 1 calc R U . . .
C23 C 0.9466(3) 0.3436(4) 0.6181(4) 0.079(2) Uani 1 1 d . . . . .
H23A H 0.9701 0.3754 0.6549 0.118 Uiso 1 1 calc R U . . .
H23B H 0.9450 0.3039 0.6467 0.118 Uiso 1 1 calc R U . . .
H23C H 0.9111 0.3623 0.5931 0.118 Uiso 1 1 calc R U . . .
C24 C 0.78337(19) 0.0662(3) 0.5055(3) 0.0493(12) Uani 1 1 d . . . . .
H24A H 0.7698 0.1115 0.5052 0.059 Uiso 1 1 calc R U . . .
C25 C 0.7622(2) 0.0444(3) 0.4200(3) 0.0618(14) Uani 1 1 d . . . . .
H25A H 0.7246 0.0551 0.3948 0.093 Uiso 1 1 calc R U . . .
H25B H 0.7670 -0.0029 0.4175 0.093 Uiso 1 1 calc R U . . .
H25C H 0.7815 0.0669 0.3925 0.093 Uiso 1 1 calc R U . . .
C26 C 0.7584(2) 0.0242(3) 0.5514(4) 0.0645(15) Uani 1 1 d . . . . .
H26A H 0.7199 0.0292 0.5279 0.097 Uiso 1 1 calc R U . . .
H26B H 0.7718 0.0385 0.6064 0.097 Uiso 1 1 calc R U . . .
H26C H 0.7676 -0.0218 0.5490 0.097 Uiso 1 1 calc R U . . .
C27 C 0.8801(2) 0.0332(3) 0.6471(3) 0.0537(13) Uani 1 1 d . . . . .
H27A H 0.8559 -0.0043 0.6431 0.064 Uiso 1 1 calc R U . . .
C28 C 0.9363(3) 0.0050(3) 0.6739(3) 0.0668(16) Uani 1 1 d . . . . .
H28A H 0.9455 -0.0170 0.7246 0.100 Uiso 1 1 calc R U . . .
H28B H 0.9614 0.0406 0.6793 0.100 Uiso 1 1 calc R U . . .
H28C H 0.9378 -0.0264 0.6347 0.100 Uiso 1 1 calc R U . . .
C29 C 0.8760(3) 0.0796(3) 0.7088(3) 0.0656(17) Uani 1 1 d . . . . .
H29A H 0.8805 0.0550 0.7566 0.098 Uiso 1 1 calc R U . . .
H29B H 0.8412 0.1006 0.6884 0.098 Uiso 1 1 calc R U . . .
H29C H 0.9035 0.1130 0.7211 0.098 Uiso 1 1 calc R U . . .
C30 C 0.8468(3) 0.2789(4) 0.7111(3) 0.0660(16) Uani 1 1 d . . . . .
S4 S 0.67033(6) 0.34882(8) 0.76328(9) 0.0609(3) Uani 1 1 d D . . . .
O5 O 0.6904(2) 0.3698(2) 0.7053(3) 0.0769(13) Uani 1 1 d . U . . .
O7 O 0.6308(2) 0.2998(3) 0.7343(3) 0.0853(14) Uani 1 1 d . U . . .
C31A C 0.7226(5) 0.3052(7) 0.8354(7) 0.104(4) Uani 0.77(3) 1 d D U P A 1
C31B C 0.7271(11) 0.3343(12) 0.8381(19) 0.100(5) Uani 0.23(3) 1 d D U P A 2
F6A F 0.7360(3) 0.2534(5) 0.8026(5) 0.131(3) Uani 0.693(8) 1 d D U P A 1
F5A F 0.7624(4) 0.3543(7) 0.8642(6) 0.150(3) Uani 0.693(8) 1 d D U P A 1
F4A F 0.7092(5) 0.2853(6) 0.8953(6) 0.134(3) Uani 0.693(8) 1 d D U P A 1
F4B F 0.7221(11) 0.3281(13) 0.9064(11) 0.138(3) Uani 0.307(8) 1 d D U P A 2
F5B F 0.7719(6) 0.3020(13) 0.8588(11) 0.114(3) Uani 0.307(8) 1 d D U P A 2
F6B F 0.7088(11) 0.2532(11) 0.8693(15) 0.141(4) Uani 0.307(8) 1 d D U P A 2
O6A O 0.6477(9) 0.3989(9) 0.7976(13) 0.088(4) Uani 0.57(3) 1 d . U P A 1
O6B O 0.6743(13) 0.3938(14) 0.8198(16) 0.097(5) Uani 0.43(3) 1 d . U P A 2
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.000  0.500 -0.009      1293       341 ' '
   2  0.500  1.000  0.068      1293       341 ' '
_platon_squeeze_details
;PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure   ! 
RESPONSE: During the 
refinement of the structure, electron density peaks were located 
that were believed to be highly disordered 
solvent molecules (possibly methylene chloride). Attempts 
made to model the solvent molecule were not successful. 
The SQUEEZE option in PLATON (Spek, 2009) indicated there was a 
large solvent cavity 2593.8 Ang^3. In the final cycles of refinement, 
this contribution (681) to the 
electron density was removed from the observed data. The 
density, the F(000) value, the molecular weight and the formula are 
given without taking into account the results obtained with the 
SQUEEZE option PLATON (Spek, 2009). Similar treatments of disordered 
solvent molecules were carried out by Stähler et al. (2001), 
Cox et al. (2003), Mohamed et al. (2003) and Athimoolam et al. (2005). 
References: 
  
Spek, A. L. (2009). Acta Cryst. D65, 148--155.
  
Athimoolam, S., Kumar, J., Ramakrishnan, V. & Rajaram, R.K. (2005). 
Acta Cryst. E61, m2014-m2017. 
  
Cox, J.P., Kumarasammy, Y., Nahar, L., Sarkar D.S. & Shoeb, M. 
(2003). Acta Cryst. E59, o975-o977. 
  
Mohamed, A.A., Krause Bauer, A.J., Bruce, E.A. & Bruce M.R.M. 
(2003). Acta Cryst. C59, m84-m86. 
  
Stahler, R., Nather, C. & Bensch, W. (2001). Acta Cryst. 
C57, 26-27.
;
 
 
_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_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
Ir1 C1 1.960(4) . ?
Ir1 O1 2.097(3) . ?
Ir1 O2 2.194(3) . ?
Ir1 Cl1 2.3200(12) . ?
Ir1 P1 2.3640(13) . ?
Ir1 P2 2.3648(12) . ?
S1 C9 1.728(6) . ?
S1 C2 1.751(4) . ?
S2 C17 1.735(5) . ?
S2 C10 1.749(4) . ?
S3 O3 1.423(4) . ?
S3 O4 1.435(4) . ?
S3 O2 1.459(3) . ?
S3 C30 1.823(6) . ?
P1 C3 1.813(5) . ?
P1 C21 1.843(6) . ?
P1 C18 1.879(6) . ?
P2 C11 1.821(4) . ?
P2 C27 1.853(5) . ?
P2 C24 1.857(5) . ?
F1 C30 1.310(7) . ?
F2 C30 1.315(8) . ?
F3 C30 1.331(8) . ?
O1 H1 0.9040 . ?
O1 H2 0.8441 . ?
C1 C2 1.439(7) . ?
C1 C10 1.442(7) . ?
C2 C3 1.385(7) . ?
C3 C4 1.423(7) . ?
C4 C5 1.397(9) . ?
C4 C9 1.413(7) . ?
C5 C6 1.371(9) . ?
C5 H5B 0.9500 . ?
C6 C7 1.408(10) . ?
C6 H6B 0.9500 . ?
C7 C8 1.372(9) . ?
C7 H7B 0.9500 . ?
C8 C9 1.395(7) . ?
C8 H8A 0.9500 . ?
C10 C11 1.374(7) . ?
C11 C12 1.424(7) . ?
C12 C13 1.398(7) . ?
C12 C17 1.418(6) . ?
C13 C14 1.368(8) . ?
C13 H13A 0.9500 . ?
C14 C15 1.402(8) . ?
C14 H14A 0.9500 . ?
C15 C16 1.370(8) . ?
C15 H15A 0.9500 . ?
C16 C17 1.397(7) . ?
C16 H16A 0.9500 . ?
C18 C19 1.504(9) . ?
C18 C20 1.542(8) . ?
C18 H18A 1.0000 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.533(9) . ?
C21 C23 1.533(9) . ?
C21 H21A 1.0000 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C25 1.521(8) . ?
C24 C26 1.541(7) . ?
C24 H24A 1.0000 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C29 1.520(7) . ?
C27 C28 1.537(7) . ?
C27 H27A 1.0000 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
S4 O6B 1.36(2) . ?
S4 O7 1.422(5) . ?
S4 O5 1.446(4) . ?
S4 O6A 1.464(16) . ?
S4 C31B 1.66(2) . ?
S4 C31A 1.773(15) . ?
C31A F6A 1.342(12) . ?
C31A F4A 1.357(12) . ?
C31A F5A 1.426(12) . ?
C31B F5B 1.32(3) . ?
C31B F4B 1.32(5) . ?
C31B O6B 1.82(4) . ?
C31B F6B 1.89(3) . ?
F4B F6B 1.66(3) . ?
 
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
C1 Ir1 O1 93.37(15) . . ?
C1 Ir1 O2 175.41(17) . . ?
O1 Ir1 O2 84.75(13) . . ?
C1 Ir1 Cl1 91.34(12) . . ?
O1 Ir1 Cl1 174.64(10) . . ?
O2 Ir1 Cl1 90.36(10) . . ?
C1 Ir1 P1 85.84(14) . . ?
O1 Ir1 P1 87.87(10) . . ?
O2 Ir1 P1 89.90(10) . . ?
Cl1 Ir1 P1 89.94(5) . . ?
C1 Ir1 P2 85.65(14) . . ?
O1 Ir1 P2 90.96(10) . . ?
O2 Ir1 P2 98.56(10) . . ?
Cl1 Ir1 P2 91.93(5) . . ?
P1 Ir1 P2 171.32(4) . . ?
C9 S1 C2 91.7(2) . . ?
C17 S2 C10 91.3(2) . . ?
O3 S3 O4 116.5(2) . . ?
O3 S3 O2 115.3(2) . . ?
O4 S3 O2 112.0(2) . . ?
O3 S3 C30 105.9(3) . . ?
O4 S3 C30 103.0(3) . . ?
O2 S3 C30 102.0(3) . . ?
C3 P1 C21 109.3(3) . . ?
C3 P1 C18 104.8(2) . . ?
C21 P1 C18 106.0(3) . . ?
C3 P1 Ir1 98.22(17) . . ?
C21 P1 Ir1 124.2(2) . . ?
C18 P1 Ir1 112.61(19) . . ?
C11 P2 C27 104.0(2) . . ?
C11 P2 C24 107.8(2) . . ?
C27 P2 C24 107.5(2) . . ?
C11 P2 Ir1 97.95(16) . . ?
C27 P2 Ir1 123.5(2) . . ?
C24 P2 Ir1 114.07(16) . . ?
Ir1 O1 H1 113.7 . . ?
Ir1 O1 H2 125.2 . . ?
H1 O1 H2 112.4 . . ?
S3 O2 Ir1 147.0(2) . . ?
C2 C1 C10 123.8(4) . . ?
C2 C1 Ir1 117.6(3) . . ?
C10 C1 Ir1 118.6(3) . . ?
C3 C2 C1 124.0(4) . . ?
C3 C2 S1 111.3(3) . . ?
C1 C2 S1 124.7(4) . . ?
C2 C3 C4 113.4(4) . . ?
C2 C3 P1 113.8(3) . . ?
C4 C3 P1 132.8(4) . . ?
C5 C4 C9 118.3(5) . . ?
C5 C4 C3 130.0(5) . . ?
C9 C4 C3 111.7(5) . . ?
C6 C5 C4 119.8(6) . . ?
C6 C5 H5B 120.1 . . ?
C4 C5 H5B 120.1 . . ?
C5 C6 C7 120.7(6) . . ?
C5 C6 H6B 119.6 . . ?
C7 C6 H6B 119.6 . . ?
C8 C7 C6 121.3(5) . . ?
C8 C7 H7B 119.3 . . ?
C6 C7 H7B 119.3 . . ?
C7 C8 C9 117.5(5) . . ?
C7 C8 H8A 121.3 . . ?
C9 C8 H8A 121.3 . . ?
C8 C9 C4 122.4(5) . . ?
C8 C9 S1 125.7(4) . . ?
C4 C9 S1 111.9(4) . . ?
C11 C10 C1 122.9(4) . . ?
C11 C10 S2 111.5(4) . . ?
C1 C10 S2 125.5(3) . . ?
C10 C11 C12 114.3(4) . . ?
C10 C11 P2 114.7(4) . . ?
C12 C11 P2 130.9(4) . . ?
C13 C12 C17 118.7(5) . . ?
C13 C12 C11 130.6(5) . . ?
C17 C12 C11 110.7(4) . . ?
C14 C13 C12 119.2(5) . . ?
C14 C13 H13A 120.4 . . ?
C12 C13 H13A 120.4 . . ?
C13 C14 C15 121.3(5) . . ?
C13 C14 H14A 119.4 . . ?
C15 C14 H14A 119.4 . . ?
C16 C15 C14 121.5(5) . . ?
C16 C15 H15A 119.3 . . ?
C14 C15 H15A 119.3 . . ?
C15 C16 C17 117.4(5) . . ?
C15 C16 H16A 121.3 . . ?
C17 C16 H16A 121.3 . . ?
C16 C17 C12 121.9(5) . . ?
C16 C17 S2 125.9(4) . . ?
C12 C17 S2 112.2(4) . . ?
C19 C18 C20 111.4(5) . . ?
C19 C18 P1 116.5(5) . . ?
C20 C18 P1 109.5(4) . . ?
C19 C18 H18A 106.3 . . ?
C20 C18 H18A 106.3 . . ?
P1 C18 H18A 106.3 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 C23 108.6(6) . . ?
C22 C21 P1 112.7(4) . . ?
C23 C21 P1 110.8(4) . . ?
C22 C21 H21A 108.2 . . ?
C23 C21 H21A 108.2 . . ?
P1 C21 H21A 108.2 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C25 C24 C26 109.5(5) . . ?
C25 C24 P2 112.4(3) . . ?
C26 C24 P2 116.1(4) . . ?
C25 C24 H24A 106.0 . . ?
C26 C24 H24A 106.0 . . ?
P2 C24 H24A 106.0 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C29 C27 C28 110.6(5) . . ?
C29 C27 P2 111.1(4) . . ?
C28 C27 P2 113.8(4) . . ?
C29 C27 H27A 107.0 . . ?
C28 C27 H27A 107.0 . . ?
P2 C27 H27A 107.0 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
F1 C30 F2 107.7(6) . . ?
F1 C30 F3 109.3(6) . . ?
F2 C30 F3 107.6(6) . . ?
F1 C30 S3 110.0(5) . . ?
F2 C30 S3 112.3(4) . . ?
F3 C30 S3 109.9(5) . . ?
O6B S4 O7 125.9(13) . . ?
O6B S4 O5 115.1(13) . . ?
O7 S4 O5 112.8(3) . . ?
O7 S4 O6A 105.4(9) . . ?
O5 S4 O6A 117.4(8) . . ?
O6B S4 C31B 73.5(18) . . ?
O7 S4 C31B 121.3(9) . . ?
O5 S4 C31B 99.4(15) . . ?
O7 S4 C31A 101.8(5) . . ?
O5 S4 C31A 105.9(4) . . ?
O6A S4 C31A 112.6(11) . . ?
F6A C31A F4A 109.8(12) . . ?
F6A C31A F5A 114.8(11) . . ?
F4A C31A F5A 108.7(11) . . ?
F6A C31A S4 110.1(8) . . ?
F4A C31A S4 111.4(9) . . ?
F5A C31A S4 101.9(9) . . ?
F5B C31B F4B 96(2) . . ?
F5B C31B S4 143(3) . . ?
F4B C31B S4 113(3) . . ?
F5B C31B O6B 168(2) . . ?
F4B C31B O6B 83(3) . . ?
S4 C31B O6B 45.8(11) . . ?
F5B C31B F6B 78.4(17) . . ?
F4B C31B F6B 59.2(17) . . ?
S4 C31B F6B 97.8(15) . . ?
O6B C31B F6B 111(2) . . ?
C31B F4B F6B 77.6(14) . . ?
F4B F6B C31B 43.2(15) . . ?
S4 O6B C31B 60.8(14) . . ?
 
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
O3 S3 O2 Ir1 18.2(5) . . . . ?
O4 S3 O2 Ir1 -118.1(4) . . . . ?
C30 S3 O2 Ir1 132.4(5) . . . . ?
C10 C1 C2 C3 177.8(4) . . . . ?
Ir1 C1 C2 C3 -2.7(6) . . . . ?
C10 C1 C2 S1 -2.1(6) . . . . ?
Ir1 C1 C2 S1 177.4(2) . . . . ?
C9 S1 C2 C3 0.9(4) . . . . ?
C9 S1 C2 C1 -179.2(4) . . . . ?
C1 C2 C3 C4 178.6(4) . . . . ?
S1 C2 C3 C4 -1.4(6) . . . . ?
C1 C2 C3 P1 -3.6(6) . . . . ?
S1 C2 C3 P1 176.4(2) . . . . ?
C21 P1 C3 C2 137.1(4) . . . . ?
C18 P1 C3 C2 -109.6(4) . . . . ?
Ir1 P1 C3 C2 6.5(4) . . . . ?
C21 P1 C3 C4 -45.6(6) . . . . ?
C18 P1 C3 C4 67.6(6) . . . . ?
Ir1 P1 C3 C4 -176.3(5) . . . . ?
C2 C3 C4 C5 -177.2(7) . . . . ?
P1 C3 C4 C5 5.6(10) . . . . ?
C2 C3 C4 C9 1.4(7) . . . . ?
P1 C3 C4 C9 -175.8(4) . . . . ?
C9 C4 C5 C6 0.7(11) . . . . ?
C3 C4 C5 C6 179.2(7) . . . . ?
C4 C5 C6 C7 0.5(14) . . . . ?
C5 C6 C7 C8 -2.2(14) . . . . ?
C6 C7 C8 C9 2.6(11) . . . . ?
C7 C8 C9 C4 -1.5(9) . . . . ?
C7 C8 C9 S1 -179.4(5) . . . . ?
C5 C4 C9 C8 -0.1(9) . . . . ?
C3 C4 C9 C8 -178.9(5) . . . . ?
C5 C4 C9 S1 178.1(5) . . . . ?
C3 C4 C9 S1 -0.7(6) . . . . ?
C2 S1 C9 C8 178.1(5) . . . . ?
C2 S1 C9 C4 -0.1(4) . . . . ?
C2 C1 C10 C11 177.2(4) . . . . ?
Ir1 C1 C10 C11 -2.2(6) . . . . ?
C2 C1 C10 S2 -2.0(6) . . . . ?
Ir1 C1 C10 S2 178.5(2) . . . . ?
C17 S2 C10 C11 0.3(4) . . . . ?
C17 S2 C10 C1 179.6(4) . . . . ?
C1 C10 C11 C12 -179.3(4) . . . . ?
S2 C10 C11 C12 0.0(5) . . . . ?
C1 C10 C11 P2 -1.2(6) . . . . ?
S2 C10 C11 P2 178.1(2) . . . . ?
C27 P2 C11 C10 -124.4(4) . . . . ?
C24 P2 C11 C10 121.7(4) . . . . ?
Ir1 P2 C11 C10 3.2(3) . . . . ?
C27 P2 C11 C12 53.3(5) . . . . ?
C24 P2 C11 C12 -60.6(5) . . . . ?
Ir1 P2 C11 C12 -179.1(4) . . . . ?
C10 C11 C12 C13 179.0(5) . . . . ?
P2 C11 C12 C13 1.3(9) . . . . ?
C10 C11 C12 C17 -0.5(6) . . . . ?
P2 C11 C12 C17 -178.2(4) . . . . ?
C17 C12 C13 C14 -1.6(8) . . . . ?
C11 C12 C13 C14 179.0(5) . . . . ?
C12 C13 C14 C15 1.2(10) . . . . ?
C13 C14 C15 C16 -0.1(10) . . . . ?
C14 C15 C16 C17 -0.6(9) . . . . ?
C15 C16 C17 C12 0.2(8) . . . . ?
C15 C16 C17 S2 179.9(4) . . . . ?
C13 C12 C17 C16 0.9(8) . . . . ?
C11 C12 C17 C16 -179.5(4) . . . . ?
C13 C12 C17 S2 -178.9(4) . . . . ?
C11 C12 C17 S2 0.7(5) . . . . ?
C10 S2 C17 C16 179.6(5) . . . . ?
C10 S2 C17 C12 -0.6(4) . . . . ?
C3 P1 C18 C19 -50.0(5) . . . . ?
C21 P1 C18 C19 65.5(5) . . . . ?
Ir1 P1 C18 C19 -155.7(4) . . . . ?
C3 P1 C18 C20 -177.5(4) . . . . ?
C21 P1 C18 C20 -62.0(5) . . . . ?
Ir1 P1 C18 C20 76.8(4) . . . . ?
C3 P1 C21 C22 -34.4(6) . . . . ?
C18 P1 C21 C22 -146.8(5) . . . . ?
Ir1 P1 C21 C22 80.5(6) . . . . ?
C3 P1 C21 C23 -156.3(5) . . . . ?
C18 P1 C21 C23 91.3(6) . . . . ?
Ir1 P1 C21 C23 -41.4(6) . . . . ?
C11 P2 C24 C25 -22.9(4) . . . . ?
C27 P2 C24 C25 -134.5(4) . . . . ?
Ir1 P2 C24 C25 84.7(4) . . . . ?
C11 P2 C24 C26 104.3(4) . . . . ?
C27 P2 C24 C26 -7.3(5) . . . . ?
Ir1 P2 C24 C26 -148.1(4) . . . . ?
C11 P2 C27 C29 163.9(4) . . . . ?
C24 P2 C27 C29 -82.0(5) . . . . ?
Ir1 P2 C27 C29 54.2(5) . . . . ?
C11 P2 C27 C28 38.3(5) . . . . ?
C24 P2 C27 C28 152.5(4) . . . . ?
Ir1 P2 C27 C28 -71.4(5) . . . . ?
O3 S3 C30 F1 -58.7(6) . . . . ?
O4 S3 C30 F1 64.1(6) . . . . ?
O2 S3 C30 F1 -179.6(5) . . . . ?
O3 S3 C30 F2 -178.6(4) . . . . ?
O4 S3 C30 F2 -55.8(5) . . . . ?
O2 S3 C30 F2 60.5(5) . . . . ?
O3 S3 C30 F3 61.7(6) . . . . ?
O4 S3 C30 F3 -175.5(5) . . . . ?
O2 S3 C30 F3 -59.2(6) . . . . ?
O6B S4 C31A F6A -176.2(15) . . . . ?
O7 S4 C31A F6A 57.4(8) . . . . ?
O5 S4 C31A F6A -60.6(8) . . . . ?
O6A S4 C31A F6A 169.8(10) . . . . ?
C31B S4 C31A F6A -134(5) . . . . ?
O6B S4 C31A F4A 61.7(16) . . . . ?
O7 S4 C31A F4A -64.6(11) . . . . ?
O5 S4 C31A F4A 177.3(9) . . . . ?
O6A S4 C31A F4A 47.8(14) . . . . ?
C31B S4 C31A F4A 104(5) . . . . ?
O6B S4 C31A F5A -54.0(15) . . . . ?
O7 S4 C31A F5A 179.7(7) . . . . ?
O5 S4 C31A F5A 61.6(8) . . . . ?
O6A S4 C31A F5A -67.9(11) . . . . ?
C31B S4 C31A F5A -12(5) . . . . ?
O6B S4 C31B F5B -167(5) . . . . ?
O7 S4 C31B F5B 70(5) . . . . ?
O5 S4 C31B F5B -54(4) . . . . ?
O6A S4 C31B F5B -174(4) . . . . ?
C31A S4 C31B F5B 57(4) . . . . ?
O6B S4 C31B F4B 52(2) . . . . ?
O7 S4 C31B F4B -70(2) . . . . ?
O5 S4 C31B F4B 165.5(19) . . . . ?
O6A S4 C31B F4B 45(2) . . . . ?
C31A S4 C31B F4B -84(5) . . . . ?
O7 S4 C31B O6B -122.4(15) . . . . ?
O5 S4 C31B O6B 113.6(14) . . . . ?
O6A S4 C31B O6B -7(2) . . . . ?
C31A S4 C31B O6B -135(5) . . . . ?
O6B S4 C31B F6B 112(2) . . . . ?
O7 S4 C31B F6B -11(3) . . . . ?
O5 S4 C31B F6B -134.7(17) . . . . ?
O6A S4 C31B F6B 104.9(18) . . . . ?
C31A S4 C31B F6B -24(3) . . . . ?
F5B C31B F4B F6B -73(2) . . . . ?
S4 C31B F4B F6B 85.1(19) . . . . ?
O6B C31B F4B F6B 119.8(18) . . . . ?
F5B C31B F6B F4B 104(2) . . . . ?
S4 C31B F6B F4B -113(3) . . . . ?
O6B C31B F6B F4B -67(3) . . . . ?
O7 S4 O6B C31B 117.1(16) . . . . ?
O5 S4 O6B C31B -92.8(15) . . . . ?
O6A S4 O6B C31B 166(4) . . . . ?
C31A S4 O6B C31B 13.9(14) . . . . ?
F5B C31B O6B S4 142(15) . . . . ?
F4B C31B O6B S4 -133(2) . . . . ?
F6B C31B O6B S4 -80.3(18) . . . . ?
 
_refine_diff_density_max    0.982
_refine_diff_density_min   -0.870
_refine_diff_density_rms    0.106

_shelxl_version_number 2013-4




