# Supplementary Material (ESI) for Journal of Materials Chemistry
# This journal is (C) The Royal Society of Chemistry 2005


data_global

_journal_coden_Cambridge         1145

loop_
_publ_author_name
'M. Bryce'
'Al Attar,Hameed A.'
'Andrei S. Batsanov'
'Sylvia Bettington'
'Fernando B. Dias'
'Andrew Monkman'
'Mustafa Tavasli'
'Amber L. Thompson'

_publ_contact_author_name        'M. Bryce'
_publ_contact_author_address     
;
Department of Chemistry
University of Durham
South Road
DURHAM
DH1 3LE
UNITED KINGDOM
;

_publ_contact_author_email       M.R.BRYCE@DURHAM.AC.UK

_publ_requested_journal          'Journal of Materials Chemistry'

_publ_section_title              
;
Bridged diiridium complexes for electrophosphorescent
OLEDs: synthesis, X-ray crystal structures, photophysics, and devices
;

data_(3)
_database_code_depnum_ccdc_archive 'CCDC 288216'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; tetrakis(9,9-dihexyl-2-(pyridin-2-yl)fluorene-C^2^,N')-bis-(\m-
chloro)diiridium, bis(dichloromethane) hydrate
;
_chemical_name_common            .
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C120 H144 Cl2 Ir2 N4,2(C H2 Cl2),H2 O'
_chemical_formula_sum            'C122 H150 Cl6 Ir2 N4 O'
_chemical_formula_weight         2285.56

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Fddd

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+3/4, -y+3/4, z'
'-x+3/4, y, -z+3/4'
'x, -y+3/4, -z+3/4'
'x, y+1/2, z+1/2'
'-x+3/4, -y+5/4, z+1/2'
'-x+3/4, y+1/2, -z+5/4'
'x, -y+5/4, -z+5/4'
'x+1/2, y, z+1/2'
'-x+5/4, -y+3/4, z+1/2'
'-x+5/4, y, -z+5/4'
'x+1/2, -y+3/4, -z+5/4'
'x+1/2, y+1/2, z'
'-x+5/4, -y+5/4, z'
'-x+5/4, y+1/2, -z+3/4'
'x+1/2, -y+5/4, -z+3/4'
'-x, -y, -z'
'x-3/4, y-3/4, -z'
'x-3/4, -y, z-3/4'
'-x, y-3/4, z-3/4'
'-x, -y+1/2, -z+1/2'
'x-3/4, y-1/4, -z+1/2'
'x-3/4, -y+1/2, z-1/4'
'-x, y-1/4, z-1/4'
'-x+1/2, -y, -z+1/2'
'x-1/4, y-3/4, -z+1/2'
'x-1/4, -y, z-1/4'
'-x+1/2, y-3/4, z-1/4'
'-x+1/2, -y+1/2, -z'
'x-1/4, y-1/4, -z'
'x-1/4, -y+1/2, z-3/4'
'-x+1/2, y-1/4, z-3/4'

_cell_length_a                   21.932(2)
_cell_length_b                   25.059(2)
_cell_length_c                   40.880(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     22467(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    6744
_cell_measurement_theta_min      3.173
_cell_measurement_theta_max      27.413

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             9392
_exptl_absorpt_coefficient_mu    2.559
_exptl_absorpt_correction_type   Integration
_exptl_absorpt_correction_T_min  0.4735
_exptl_absorpt_correction_T_max  0.6587
_exptl_absorpt_process_details   'XPREP (SHELXTL,1997)'

_exptl_special_details           
;
The data collection nominally covered full sphere
of reciprocal Space, by a combination of 4 sets of \w scans
each set at different \f and/or 2\q angles and each
scan (10s exposure) covering 0.3\% in \w. Crystal to
detector distance 4.51 cm.
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART 1K CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean 8
_diffrn_reflns_number            18780
_diffrn_reflns_av_R_equivalents  0.0962
_diffrn_reflns_av_sigmaI/netI    0.1074
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_theta_min         3.27
_diffrn_reflns_theta_max         27.41
_reflns_number_total             5808
_reflns_number_gt                3800
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       'SMART-NT V6.1 (Bruker, 2000)'
_computing_cell_refinement       'SMART-NT V6.1 (Bruker, 2000)'
_computing_data_reduction        'SMART-NT V6.1 (Bruker, 2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1P)^2^+3.0P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5808
_refine_ls_number_parameters     315
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1190
_refine_ls_R_factor_gt           0.0807
_refine_ls_wR_factor_ref         0.2335
_refine_ls_wR_factor_gt          0.2002
_refine_ls_goodness_of_fit_ref   1.272
_refine_ls_restrained_S_all      1.272
_refine_ls_shift/su_max          0.003
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ir Ir 0.1250 0.199033(18) 0.6250 0.0397(2) Uani 1 2 d S . .
Cl1 Cl 0.1250 0.1250 0.66611(7) 0.0422(7) Uani 1 2 d S . .
N1 N 0.0320(4) 0.2048(3) 0.62332(15) 0.0445(18) Uani 1 1 d . . .
C1 C -0.0073(4) 0.1818(4) 0.6434(2) 0.052(2) Uani 1 1 d . . .
H1 H 0.0082 0.1576 0.6593 0.062 Uiso 1 1 d R . .
C2 C -0.0682(5) 0.1900(4) 0.6428(2) 0.059(3) Uani 1 1 d . . .
H2 H -0.0943 0.1729 0.6581 0.071 Uiso 1 1 d R . .
C3 C -0.0921(5) 0.2248(5) 0.6189(3) 0.062(3) Uani 1 1 d . . .
H3 H -0.1347 0.2310 0.6176 0.074 Uiso 1 1 d R . .
C4 C -0.0527(4) 0.2492(4) 0.5978(2) 0.058(3) Uani 1 1 d . . .
H4 H -0.0679 0.2726 0.5814 0.070 Uiso 1 1 d R . .
C5 C 0.0100(4) 0.2397(4) 0.6004(2) 0.046(2) Uani 1 1 d . . .
C6 C 0.0579(4) 0.2651(4) 0.5803(2) 0.050(2) Uani 1 1 d . . .
C7 C 0.0435(5) 0.2987(4) 0.5540(2) 0.053(2) Uani 1 1 d . . .
H7 H 0.0026 0.3082 0.5491 0.064 Uiso 1 1 d R . .
C8 C 0.0917(5) 0.3176(4) 0.5354(3) 0.055(2) Uani 1 1 d . . .
C9 C 0.1520(5) 0.3046(4) 0.5432(2) 0.055(2) Uani 1 1 d . . .
C10 C 0.1640(5) 0.2726(4) 0.5693(2) 0.049(2) Uani 1 1 d . . .
H10 H 0.2052 0.2640 0.5741 0.059 Uiso 1 1 d R . .
C11 C 0.1190(4) 0.2533(4) 0.5885(2) 0.048(2) Uani 1 1 d . . .
C12 C 0.1929(5) 0.3304(4) 0.5187(2) 0.055(2) Uani 1 1 d . . .
C13 C 0.2544(5) 0.3280(4) 0.5147(2) 0.056(2) Uani 1 1 d . . .
H13 H 0.2784 0.3060 0.5286 0.067 Uiso 1 1 d R . .
C14 C 0.2815(6) 0.3576(4) 0.4904(3) 0.069(3) Uani 1 1 d . . .
H14 H 0.3244 0.3554 0.4873 0.083 Uiso 1 1 d R . .
C15 C 0.2472(6) 0.3903(4) 0.4703(3) 0.067(3) Uani 1 1 d . . .
H15 H 0.2667 0.4114 0.4541 0.081 Uiso 1 1 d R . .
C16 C 0.1851(6) 0.3923(4) 0.4736(3) 0.066(3) Uani 1 1 d . . .
H16 H 0.1616 0.4149 0.4599 0.079 Uiso 1 1 d R . .
C17 C 0.1563(5) 0.3603(4) 0.4978(2) 0.061(3) Uani 1 1 d . . .
C18 C 0.0899(5) 0.3553(4) 0.5048(2) 0.059(3) Uani 1 1 d . . .
C19 C 0.0535(5) 0.3302(5) 0.4772(2) 0.071(3) Uani 1 1 d . . .
H191 H 0.0558 0.3538 0.4578 0.086 Uiso 1 1 d R . .
H192 H 0.0101 0.3283 0.4839 0.086 Uiso 1 1 d R . .
C20 C 0.0745(6) 0.2734(6) 0.4674(3) 0.084(4) Uani 1 1 d . . .
H201 H 0.1175 0.2749 0.4601 0.100 Uiso 1 1 d R . .
H202 H 0.0722 0.2493 0.4865 0.100 Uiso 1 1 d R . .
C21 C 0.0353(6) 0.2512(6) 0.4398(3) 0.102(5) Uani 1 1 d . . .
H211 H -0.0076 0.2504 0.4473 0.122 Uiso 1 1 d R . .
H212 H 0.0375 0.2760 0.4210 0.122 Uiso 1 1 d R . .
C22 C 0.0535(8) 0.1956(6) 0.4286(3) 0.122(6) Uani 1 1 d . . .
H221 H 0.0530 0.1709 0.4475 0.146 Uiso 1 1 d R . .
H222 H 0.0956 0.1965 0.4198 0.146 Uiso 1 1 d R . .
C23 C 0.0090(9) 0.1754(9) 0.4021(4) 0.143(8) Uani 1 1 d . . .
H231 H -0.0327 0.1744 0.4113 0.172 Uiso 1 1 d R . .
H232 H 0.0087 0.2014 0.3838 0.172 Uiso 1 1 d R . .
C24 C 0.0211(12) 0.1249(9) 0.3898(7) 0.176(11) Uani 1 1 d . . .
H241 H -0.0169 0.1079 0.3823 0.264 Uiso 1 1 d R . .
H242 H 0.0400 0.1021 0.4066 0.264 Uiso 1 1 d R . .
H243 H 0.0492 0.1286 0.3712 0.264 Uiso 1 1 d R . .
C25 C 0.0589(6) 0.4091(5) 0.5140(3) 0.081(4) Uani 1 1 d . . .
H251 H 0.0571 0.4318 0.4942 0.098 Uiso 1 1 d R . .
H252 H 0.0165 0.4017 0.5209 0.098 Uiso 1 1 d R . .
C26 C 0.0906(7) 0.4406(5) 0.5412(4) 0.086(4) Uani 1 1 d . . .
H261 H 0.1318 0.4512 0.5337 0.103 Uiso 1 1 d R . .
H262 H 0.0953 0.4174 0.5606 0.103 Uiso 1 1 d R . .
C27 C 0.0542(7) 0.4905(6) 0.5505(4) 0.108(5) Uani 1 1 d . . .
H271 H 0.0467 0.5120 0.5306 0.130 Uiso 1 1 d R . .
H272 H 0.0140 0.4794 0.5592 0.130 Uiso 1 1 d R . .
C28 C 0.0866(9) 0.5258(8) 0.5751(5) 0.132(6) Uani 1 1 d . . .
H281 H 0.1282 0.5336 0.5669 0.172 Uiso 1 1 d R . .
H282 H 0.0907 0.5062 0.5960 0.172 Uiso 1 1 d R . .
C29 C 0.0510(12) 0.5821(14) 0.5819(10) 0.26(2) Uani 1 1 d . . .
H291 H 0.0733 0.6026 0.5988 0.335 Uiso 1 1 d R . .
H292 H 0.0505 0.6036 0.5616 0.335 Uiso 1 1 d R . .
C30 C -0.0059(14) 0.5736(10) 0.5918(5) 0.185(10) Uani 1 1 d . . .
H301 H -0.0266 0.6079 0.5948 0.278 Uiso 1 1 d R . .
H302 H -0.0053 0.5541 0.6126 0.278 Uiso 1 1 d R . .
H303 H -0.0276 0.5525 0.5753 0.278 Uiso 1 1 d R . .
Cl2 Cl 0.4096(6) 0.3621(6) 0.6800(4) 0.199(6) Uani 0.50 1 d PD A -1
Cl3 Cl 0.3712(4) 0.3175(7) 0.7351(3) 0.163(5) Uani 0.50 1 d PD A -1
C31 C 0.371(3) 0.387(2) 0.7179(11) 0.18(2) Uiso 0.50 1 d PD A -1
H311 H 0.3283 0.3974 0.7126 0.218 Uiso 0.50 1 d PR A -1
H312 H 0.3908 0.4154 0.7308 0.218 Uiso 0.50 1 d PR A -1
O1 O 0.1250 0.3457(8) 0.6250 0.061(5) Uiso 0.50 2 d SP . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ir 0.0442(3) 0.0492(3) 0.0258(3) 0.000 0.00135(19) 0.000
Cl1 0.0546(18) 0.0469(15) 0.0252(13) 0.000 0.000 -0.0017(14)
N1 0.044(4) 0.050(4) 0.040(4) -0.007(3) -0.003(3) 0.005(3)
C1 0.052(6) 0.068(6) 0.036(5) -0.002(4) 0.008(4) -0.012(5)
C2 0.062(7) 0.077(7) 0.038(6) -0.001(5) 0.020(5) -0.002(5)
C3 0.044(6) 0.082(7) 0.060(7) -0.011(6) 0.003(5) 0.005(5)
C4 0.052(6) 0.076(7) 0.047(5) 0.009(5) 0.004(4) 0.011(5)
C5 0.046(5) 0.066(6) 0.027(4) -0.010(4) 0.002(4) 0.006(4)
C6 0.058(6) 0.063(6) 0.030(4) -0.002(4) -0.001(4) 0.007(5)
C7 0.042(5) 0.071(7) 0.046(5) 0.002(5) 0.000(4) 0.009(4)
C8 0.053(6) 0.065(6) 0.047(6) 0.006(5) -0.002(5) 0.006(5)
C9 0.070(7) 0.054(6) 0.042(5) 0.000(4) 0.003(5) -0.002(5)
C10 0.061(6) 0.057(6) 0.031(4) 0.002(4) 0.002(4) -0.003(4)
C11 0.041(5) 0.074(6) 0.027(4) -0.019(4) 0.001(3) 0.010(4)
C12 0.070(7) 0.059(6) 0.035(5) 0.000(4) 0.010(4) -0.006(5)
C13 0.060(6) 0.065(6) 0.042(5) -0.002(4) 0.002(4) -0.007(5)
C14 0.085(8) 0.072(7) 0.051(6) 0.008(5) 0.014(6) -0.009(6)
C15 0.091(9) 0.071(7) 0.039(6) 0.005(5) 0.016(6) -0.015(6)
C16 0.081(8) 0.070(7) 0.045(6) -0.001(5) 0.016(5) -0.002(6)
C17 0.081(7) 0.070(7) 0.032(5) 0.004(4) 0.007(5) 0.006(5)
C18 0.075(7) 0.059(6) 0.044(6) 0.013(5) -0.002(5) 0.003(5)
C19 0.083(8) 0.098(9) 0.033(5) 0.019(5) 0.000(5) -0.011(7)
C20 0.094(9) 0.107(10) 0.050(6) 0.012(7) -0.004(6) -0.026(8)
C21 0.092(10) 0.153(15) 0.061(7) -0.017(9) 0.005(7) -0.032(9)
C22 0.177(16) 0.132(13) 0.057(8) -0.018(8) 0.006(9) -0.085(12)
C23 0.147(16) 0.178(19) 0.104(13) -0.068(13) 0.025(11) -0.055(14)
C24 0.21(3) 0.15(2) 0.16(2) -0.059(17) 0.04(2) -0.026(17)
C25 0.102(9) 0.082(8) 0.059(7) 0.014(6) -0.010(7) 0.024(7)
C26 0.082(9) 0.089(9) 0.086(10) 0.008(7) -0.003(8) 0.031(7)
C27 0.115(12) 0.091(10) 0.119(12) -0.007(9) -0.031(10) 0.014(9)
C28 0.124(14) 0.115(13) 0.157(17) -0.022(13) -0.022(13) -0.007(11)
C29 0.117(19) 0.28(4) 0.38(5) -0.19(4) 0.02(2) -0.02(2)
C30 0.27(4) 0.16(2) 0.128(19) 0.019(16) -0.01(2) 0.02(2)
Cl2 0.175(12) 0.229(15) 0.193(14) -0.051(11) -0.004(9) -0.065(11)
Cl3 0.081(6) 0.282(14) 0.127(9) 0.090(10) -0.040(5) -0.028(6)

_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
Ir C11 2.024(10) 11_455 ?
Ir C11 2.024(10) . ?
Ir N1 2.045(8) . ?
Ir N1 2.045(8) 11_455 ?
Ir Cl1 2.5034(19) . ?
Ir Cl1 2.5034(19) 11_455 ?
N1 C1 1.322(12) . ?
N1 C5 1.371(11) . ?
C1 C2 1.353(14) . ?
C2 C3 1.410(15) . ?
C3 C4 1.365(14) . ?
C4 C5 1.401(12) . ?
C5 C6 1.475(13) . ?
C6 C7 1.401(13) . ?
C6 C11 1.413(12) . ?
C7 C8 1.386(14) . ?
C8 C9 1.399(15) . ?
C8 C18 1.566(14) . ?
C9 C10 1.362(13) . ?
C9 C12 1.489(13) . ?
C10 C11 1.349(12) . ?
C12 C13 1.362(13) . ?
C12 C17 1.393(14) . ?
C13 C14 1.375(13) . ?
C14 C15 1.384(16) . ?
C15 C16 1.369(15) . ?
C16 C17 1.420(14) . ?
C17 C18 1.489(16) . ?
C18 C19 1.520(15) . ?
C18 C25 1.556(16) . ?
C19 C20 1.551(17) . ?
C20 C21 1.522(16) . ?
C21 C22 1.52(2) . ?
C22 C23 1.54(2) . ?
C23 C24 1.39(2) . ?
C25 C26 1.530(17) . ?
C26 C27 1.533(17) . ?
C27 C28 1.51(2) . ?
C28 C29 1.64(3) . ?
C29 C30 1.33(3) . ?
Cl2 C31 1.87(5) . ?
Cl3 C31 1.88(5) . ?

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
C11 Ir C11 95.5(5) 11_455 . ?
C11 Ir N1 92.4(3) 11_455 . ?
C11 Ir N1 82.1(3) . . ?
C11 Ir N1 82.1(3) 11_455 11_455 ?
C11 Ir N1 92.4(3) . 11_455 ?
N1 Ir N1 171.9(4) . 11_455 ?
C11 Ir Cl1 90.2(3) 11_455 . ?
C11 Ir Cl1 173.4(2) . . ?
N1 Ir Cl1 94.3(2) . . ?
N1 Ir Cl1 91.70(18) 11_455 . ?
C11 Ir Cl1 173.4(2) 11_455 11_455 ?
C11 Ir Cl1 90.2(3) . 11_455 ?
N1 Ir Cl1 91.70(18) . 11_455 ?
N1 Ir Cl1 94.3(2) 11_455 11_455 ?
Cl1 Ir Cl1 84.35(10) . 11_455 ?
Ir Cl1 Ir 95.65(10) . 14_445 ?
C1 N1 C5 118.3(9) . . ?
C1 N1 Ir 126.7(7) . . ?
C5 N1 Ir 114.8(6) . . ?
N1 C1 C2 124.5(10) . . ?
C1 C2 C3 118.3(9) . . ?
C4 C3 C2 118.7(9) . . ?
C3 C4 C5 119.9(9) . . ?
N1 C5 C4 120.3(8) . . ?
N1 C5 C6 113.9(8) . . ?
C4 C5 C6 125.7(9) . . ?
C7 C6 C11 121.3(9) . . ?
C7 C6 C5 121.8(9) . . ?
C11 C6 C5 117.0(8) . . ?
C8 C7 C6 117.2(9) . . ?
C7 C8 C9 121.1(9) . . ?
C7 C8 C18 128.8(9) . . ?
C9 C8 C18 110.2(9) . . ?
C10 C9 C8 119.9(10) . . ?
C10 C9 C12 131.7(10) . . ?
C8 C9 C12 108.4(9) . . ?
C11 C10 C9 121.7(10) . . ?
C10 C11 C6 118.8(9) . . ?
C10 C11 Ir 128.4(7) . . ?
C6 C11 Ir 112.1(7) . . ?
C13 C12 C17 121.3(9) . . ?
C13 C12 C9 131.2(10) . . ?
C17 C12 C9 107.4(9) . . ?
C12 C13 C14 119.5(11) . . ?
C13 C14 C15 120.9(11) . . ?
C16 C15 C14 120.2(10) . . ?
C15 C16 C17 119.4(11) . . ?
C12 C17 C16 118.4(11) . . ?
C12 C17 C18 113.4(9) . . ?
C16 C17 C18 128.1(10) . . ?
C17 C18 C19 113.9(9) . . ?
C17 C18 C25 113.6(10) . . ?
C19 C18 C25 107.8(9) . . ?
C17 C18 C8 100.5(8) . . ?
C19 C18 C8 110.9(9) . . ?
C25 C18 C8 109.9(9) . . ?
C18 C19 C20 114.5(10) . . ?
C21 C20 C19 111.0(11) . . ?
C22 C21 C20 114.1(13) . . ?
C21 C22 C23 110.2(16) . . ?
C24 C23 C22 116(2) . . ?
C26 C25 C18 115.1(9) . . ?
C25 C26 C27 111.5(11) . . ?
C28 C27 C26 113.4(13) . . ?
C27 C28 C29 113.1(16) . . ?
C30 C29 C28 111(3) . . ?
Cl2 C31 Cl3 90(3) . . ?

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
C11 Ir Cl1 Ir -176.3(2) 11_455 . . 14_445 ?
C11 Ir Cl1 Ir 34(2) . . . 14_445 ?
N1 Ir Cl1 Ir 91.28(18) . . . 14_445 ?
N1 Ir Cl1 Ir -94.14(19) 11_455 . . 14_445 ?
Cl1 Ir Cl1 Ir 0.0 11_455 . . 14_445 ?
C11 Ir N1 C1 -79.4(7) 11_455 . . . ?
C11 Ir N1 C1 -174.6(8) . . . . ?
N1 Ir N1 C1 -126.8(7) 11_455 . . . ?
Cl1 Ir N1 C1 11.0(7) . . . . ?
Cl1 Ir N1 C1 95.4(7) 11_455 . . . ?
C11 Ir N1 C5 95.1(6) 11_455 . . . ?
C11 Ir N1 C5 -0.2(6) . . . . ?
N1 Ir N1 C5 47.7(5) 11_455 . . . ?
Cl1 Ir N1 C5 -174.6(5) . . . . ?
Cl1 Ir N1 C5 -90.1(5) 11_455 . . . ?
C1 N1 C5 C6 177.2(8) . . . . ?
Ir N1 C5 C6 2.2(9) . . . . ?
C3 C4 C5 C6 -177.1(10) . . . . ?
N1 C5 C6 C7 175.1(8) . . . . ?
C4 C5 C6 C7 -5.8(14) . . . . ?
N1 C5 C6 C11 -4.1(11) . . . . ?
C4 C5 C6 C11 175.0(9) . . . . ?
C11 C6 C7 C8 3.4(14) . . . . ?
C5 C6 C7 C8 -175.7(9) . . . . ?
C9 C10 C11 Ir 172.3(7) . . . . ?
C7 C6 C11 C10 -3.8(14) . . . . ?
C5 C6 C11 C10 175.3(8) . . . . ?
C7 C6 C11 Ir -175.3(7) . . . . ?
C5 C6 C11 Ir 3.9(10) . . . . ?
C11 Ir C11 C10 95.8(9) 11_455 . . . ?
N1 Ir C11 C10 -172.5(9) . . . . ?
N1 Ir C11 C10 13.5(8) 11_455 . . . ?
Cl1 Ir C11 C10 -114.9(19) . . . . ?
Cl1 Ir C11 C10 -80.8(8) 11_455 . . . ?
C11 Ir C11 C6 -93.7(6) 11_455 . . . ?
N1 Ir C11 C6 -2.0(6) . . . . ?
N1 Ir C11 C6 -176.0(6) 11_455 . . . ?
Cl1 Ir C11 C6 56(2) . . . . ?
Cl1 Ir C11 C6 89.7(6) 11_455 . . . ?
C10 C9 C12 C13 2.6(18) . . . . ?
C8 C9 C12 C13 -176.6(10) . . . . ?
C10 C9 C12 C17 -178.1(10) . . . . ?
C8 C9 C12 C17 2.8(11) . . . . ?
C17 C12 C13 C14 2.9(15) . . . . ?
C9 C12 C13 C14 -177.8(10) . . . . ?
C12 C13 C14 C15 1.0(16) . . . . ?
C13 C14 C15 C16 -2.2(17) . . . . ?
C14 C15 C16 C17 -0.4(16) . . . . ?
C13 C12 C17 C16 -5.3(15) . . . . ?
C9 C12 C17 C16 175.2(9) . . . . ?
C13 C12 C17 C18 176.4(9) . . . . ?
C9 C12 C17 C18 -3.0(12) . . . . ?
C15 C16 C17 C12 4.1(15) . . . . ?
C15 C16 C17 C18 -178.0(10) . . . . ?
C12 C17 C18 C19 -116.6(10) . . . . ?
C16 C17 C18 C19 65.3(14) . . . . ?
C12 C17 C18 C25 119.3(10) . . . . ?
C16 C17 C18 C25 -58.7(14) . . . . ?
C12 C17 C18 C8 2.0(11) . . . . ?
C16 C17 C18 C8 -176.0(11) . . . . ?
C7 C8 C18 C17 178.5(11) . . . . ?
C9 C8 C18 C17 -0.1(10) . . . . ?
C7 C8 C18 C19 -60.7(15) . . . . ?
C9 C8 C18 C19 120.7(10) . . . . ?
C7 C8 C18 C25 58.5(15) . . . . ?
C9 C8 C18 C25 -120.1(10) . . . . ?
C17 C18 C19 C20 58.7(12) . . . . ?
C25 C18 C19 C20 -174.2(9) . . . . ?
C8 C18 C19 C20 -53.8(12) . . . . ?
C18 C19 C20 C21 179.5(9) . . . . ?
C19 C20 C21 C22 179.5(11) . . . . ?
C20 C21 C22 C23 176.8(12) . . . . ?
C21 C22 C23 C24 179.9(17) . . . . ?
C17 C18 C25 C26 -51.5(14) . . . . ?
C19 C18 C25 C26 -178.8(10) . . . . ?
C8 C18 C25 C26 60.2(14) . . . . ?
C18 C25 C26 C27 -175.3(12) . . . . ?
C25 C26 C27 C28 -174.5(14) . . . . ?
C26 C27 C28 C29 174(2) . . . . ?
C27 C28 C29 C30 56(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.907
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.977
_refine_diff_density_max         1.861
_refine_diff_density_min         -1.814
_refine_diff_density_rms         0.188

#============================================END

data_(5)
_database_code_depnum_ccdc_archive 'CCDC 288217'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
bis(9,9,-dihexyl-2-pyridin-2-yl)fluorene-C^2^,N')-
dimethylsulphoxide iridium(III) isocyanate,
bis-dimethylsulphoxide solvate
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C63 H78 Ir N3 O2 S,2(C2 H6 O S)'
_chemical_formula_sum            'C67 H90 Ir N3 O4 S3'
_chemical_formula_weight         1289.80

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   14.403(4)
_cell_length_b                   15.041(4)
_cell_length_c                   16.055(4)
_cell_angle_alpha                77.58(1)
_cell_angle_beta                 70.27(1)
_cell_angle_gamma                79.47(1)
_cell_volume                     3174.2(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    7868
_cell_measurement_theta_min      2.33
_cell_measurement_theta_max      30.50

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      'not measured '
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1340
_exptl_absorpt_coefficient_mu    2.250
_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.5183
_exptl_absorpt_correction_T_max  0.7734
_exptl_absorpt_process_details   
'XPREP v.6.12 (Bruker AXS,2001), R(int)=0.054 before correction'

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0.00 0.00 -1.00 0.0600
0.00 0.00 1.00 0.0700
1.00 0.00 0.00 0.0650
1.00 1.00 0.00 0.0700
-1.00 -1.00 0.00 0.1100
1.00 1.00 1.00 0.0660
-1.00 -1.00 -1.00 0.1100
0.00 1.00 0.00 0.1500
-1.00 0.00 0.00 0.1800

_exptl_special_details           
;The data collection nominally covered full sphere
of reciprocal space, by a combination of 5 sets of \w scans;
each set at different \f and/or 2\q angles and each
scan (20 sec exposure) covering 0.3\% in \w. Crystal to
detector distance 4.93 cm.
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         
'60W microfocus Bede Microsource with glass polycapillary optics'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'ProteumM APEX CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean 8
_diffrn_reflns_number            51421
_diffrn_reflns_av_R_equivalents  0.0229
_diffrn_reflns_av_sigmaI/netI    0.0269
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.70
_diffrn_reflns_theta_max         30.00
_reflns_number_total             18390
_reflns_number_gt                17101
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       'SMART version 5.625 (Bruker, 2001)'
_computing_cell_refinement       'SMART version 5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT version 6.28A (Bruker, 2002)'
_computing_structure_solution    'SHELXTL version 6.12 (Bruker, 2001)'
_computing_structure_refinement  'SHELXTL version 6.12 (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL version 5.10 (Bruker, 1997)'
_computing_publication_material  'SHELXTL version 5.10 (Bruker, 1997)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.
C(60)H~3~ is disordered between positions A (67%) and B (33%). In a
DMSO molecule of crystallisation, S(3), C(66)H~3~ and C(67)H~3~ are
disordered between positions A and B with 50% occupancies.
Methyl groups (except disordered) were refined as rotating bodies,
other H atoms - riding.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0313P)^2^+2.4326P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         18390
_refine_ls_number_parameters     725
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0270
_refine_ls_R_factor_gt           0.0239
_refine_ls_wR_factor_ref         0.0627
_refine_ls_wR_factor_gt          0.0609
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.005
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ir Ir 0.223892(5) 0.623785(4) 0.557445(4) 0.01463(2) Uani 1 1 d . . .
S1 S 0.12746(3) 0.58615(3) 0.70977(3) 0.02063(9) Uani 1 1 d . . .
O1 O 0.02293(12) 0.56795(13) 0.73246(11) 0.0337(4) Uani 1 1 d . . .
O2 O 0.25285(16) 0.32075(12) 0.57891(16) 0.0475(5) Uani 1 1 d . . .
N1 N 0.11762(12) 0.62799(11) 0.49614(11) 0.0185(3) Uani 1 1 d . . .
N2 N 0.34658(11) 0.62826(10) 0.59347(10) 0.0159(3) Uani 1 1 d . . .
N3 N 0.25411(13) 0.48051(12) 0.55128(11) 0.0223(3) Uani 1 1 d . . .
C1 C 0.30713(15) 0.65649(14) 0.27243(13) 0.0224(4) Uani 1 1 d . . .
H1 H 0.2742 0.6495 0.2324 0.027 Uiso 1 1 d R . .
C2 C 0.25878(14) 0.64481(12) 0.36541(13) 0.0186(3) Uani 1 1 d . . .
C3 C 0.30650(13) 0.65261(12) 0.42668(12) 0.0158(3) Uani 1 1 d . . .
C4 C 0.40409(14) 0.67534(12) 0.39219(12) 0.0172(3) Uani 1 1 d . . .
H4 H 0.4381 0.6816 0.4316 0.021 Uiso 1 1 d R . .
C5 C 0.62590(16) 0.73058(15) 0.27672(14) 0.0259(4) Uani 1 1 d . . .
H5 H 0.6178 0.7245 0.3388 0.031 Uiso 1 1 d R . .
C6 C 0.71421(17) 0.75516(17) 0.21203(16) 0.0328(5) Uani 1 1 d . . .
H6 H 0.7672 0.7654 0.2301 0.039 Uiso 1 1 d R . .
C7 C 0.72527(18) 0.76467(18) 0.12081(16) 0.0362(5) Uani 1 1 d . . .
H7 H 0.7854 0.7824 0.0775 0.043 Uiso 1 1 d R . .
C8 C 0.64968(18) 0.74861(17) 0.09247(15) 0.0328(5) Uani 1 1 d . . .
H8 H 0.6580 0.7546 0.0304 0.039 Uiso 1 1 d R . .
C9 C 0.47073(16) 0.69669(15) 0.14327(13) 0.0244(4) Uani 1 1 d . . .
C10 C 0.40355(15) 0.67858(13) 0.24001(12) 0.0210(4) Uani 1 1 d . . .
C11 C 0.45070(14) 0.68863(12) 0.30023(12) 0.0187(3) Uani 1 1 d . . .
C12 C 0.55027(15) 0.71513(13) 0.24831(13) 0.0215(4) Uani 1 1 d . . .
C13 C 0.56137(16) 0.72333(15) 0.15680(13) 0.0249(4) Uani 1 1 d . . .
C14 C 0.15402(14) 0.63024(13) 0.40548(13) 0.0194(3) Uani 1 1 d . . .
C15 C 0.09141(16) 0.62388(15) 0.35749(15) 0.0261(4) Uani 1 1 d . . .
H15 H 0.1178 0.6229 0.2949 0.031 Uiso 1 1 d R . .
C16 C -0.00879(17) 0.61885(17) 0.40043(16) 0.0317(5) Uani 1 1 d . . .
H16 H -0.0517 0.6145 0.3681 0.038 Uiso 1 1 d R . .
C17 C -0.04551(16) 0.61983(17) 0.49206(16) 0.0304(4) Uani 1 1 d . . .
H17 H -0.1144 0.6181 0.5231 0.036 Uiso 1 1 d R . .
C18 C 0.01941(15) 0.62322(14) 0.53774(14) 0.0241(4) Uani 1 1 d . . .
H18 H -0.0061 0.6225 0.6007 0.029 Uiso 1 1 d R . .
C19 C 0.42219(18) 0.77447(16) 0.08564(14) 0.0305(5) Uani 1 1 d . . .
H191 H 0.4693 0.7842 0.0241 0.040 Uiso 1 1 d R . .
H192 H 0.3621 0.7545 0.0819 0.040 Uiso 1 1 d R . .
C20 C 0.3932(2) 0.86616(16) 0.12007(16) 0.0352(5) Uani 1 1 d . . .
H201 H 0.3667 0.8540 0.1864 0.046 Uiso 1 1 d R . .
H202 H 0.4533 0.8974 0.1035 0.046 Uiso 1 1 d R . .
C21 C 0.3154(3) 0.9281(2) 0.0860(3) 0.0571(8) Uani 1 1 d . . .
H211 H 0.2559 0.8962 0.1019 0.074 Uiso 1 1 d R . .
H212 H 0.3425 0.9404 0.0198 0.074 Uiso 1 1 d R . .
C22 C 0.2847(2) 1.0207(2) 0.1193(2) 0.0485(7) Uani 1 1 d . . .
H221 H 0.2803 1.0104 0.1834 0.063 Uiso 1 1 d R . .
H222 H 0.3360 1.0622 0.0859 0.063 Uiso 1 1 d R . .
C23 C 0.1881(3) 1.0653(2) 0.1093(3) 0.0579(8) Uani 1 1 d . . .
H231 H 0.1930 1.0757 0.0450 0.075 Uiso 1 1 d R . .
H232 H 0.1373 1.0231 0.1420 0.075 Uiso 1 1 d R . .
C24 C 0.1537(3) 1.1557(2) 0.1421(2) 0.0545(8) Uani 1 1 d . . .
H241 H 0.1443 1.1457 0.2066 0.092(9) Uiso 1 1 d R . .
H242 H 0.0906 1.1820 0.1311 0.092(9) Uiso 1 1 d R . .
H243 H 0.2036 1.1980 0.1106 0.092(9) Uiso 1 1 d R . .
C25 C 0.49757(17) 0.60909(15) 0.10013(14) 0.0278(4) Uani 1 1 d . . .
H251 H 0.4354 0.5879 0.1025 0.036 Uiso 1 1 d R . .
H252 H 0.5365 0.6247 0.0362 0.036 Uiso 1 1 d R . .
C26 C 0.55700(19) 0.53090(16) 0.14442(15) 0.0311(5) Uani 1 1 d . . .
H261 H 0.5206 0.5188 0.2094 0.040 Uiso 1 1 d R . .
H262 H 0.6215 0.5505 0.1376 0.040 Uiso 1 1 d R . .
C27 C 0.57664(18) 0.44166(16) 0.10719(16) 0.0315(5) Uani 1 1 d . . .
H271 H 0.5140 0.4139 0.1258 0.041 Uiso 1 1 d R . .
H272 H 0.6004 0.4550 0.0408 0.041 Uiso 1 1 d R . .
C28 C 0.6540(2) 0.37294(17) 0.14083(17) 0.0355(5) Uani 1 1 d . . .
H281 H 0.7151 0.4027 0.1244 0.046 Uiso 1 1 d R . .
H282 H 0.6287 0.3592 0.2071 0.046 Uiso 1 1 d R . .
C29 C 0.6816(2) 0.28248(19) 0.1045(2) 0.0441(6) Uani 1 1 d . . .
H291 H 0.6980 0.2963 0.0384 0.057 Uiso 1 1 d R . .
H292 H 0.7420 0.2495 0.1186 0.057 Uiso 1 1 d R . .
C30 C 0.6015(3) 0.2205(2) 0.1411(2) 0.0505(7) Uani 1 1 d . . .
H301 H 0.5868 0.2040 0.2063 0.073(7) Uiso 1 1 d R . .
H302 H 0.6237 0.1648 0.1139 0.073(7) Uiso 1 1 d R . .
H303 H 0.5414 0.2522 0.1271 0.073(7) Uiso 1 1 d R . .
C31 C 0.27257(14) 0.87117(13) 0.61562(13) 0.0195(3) Uani 1 1 d . . .
H31 H 0.3265 0.8890 0.6271 0.023 Uiso 1 1 d R . .
C32 C 0.27916(13) 0.78468(12) 0.59305(12) 0.0167(3) Uani 1 1 d . . .
C33 C 0.20160(13) 0.75681(12) 0.57195(12) 0.0164(3) Uani 1 1 d . . .
C34 C 0.11535(14) 0.81925(12) 0.57557(12) 0.0181(3) Uani 1 1 d . . .
H34 H 0.0629 0.8042 0.5597 0.022 Uiso 1 1 d R . .
C35 C -0.07239(15) 0.98200(14) 0.61469(14) 0.0242(4) Uani 1 1 d . . .
H35 H -0.0911 0.9352 0.5943 0.029 Uiso 1 1 d R . .
C36 C -0.13974(16) 1.05854(15) 0.63845(15) 0.0290(4) Uani 1 1 d . . .
H36 H -0.2046 1.0642 0.6337 0.035 Uiso 1 1 d R . .
C37 C -0.11262(17) 1.12666(15) 0.66892(16) 0.0309(5) Uani 1 1 d . . .
H37 H -0.1594 1.1782 0.6854 0.037 Uiso 1 1 d R . .
C38 C -0.01769(17) 1.12020(14) 0.67572(16) 0.0298(4) Uani 1 1 d . . .
H38 H 0.0005 1.1672 0.6962 0.036 Uiso 1 1 d R . .
C39 C 0.15748(15) 1.02274(13) 0.65211(14) 0.0233(4) Uani 1 1 d . . .
C40 C 0.18587(14) 0.92994(13) 0.62069(13) 0.0197(3) Uani 1 1 d . . .
C41 C 0.10706(14) 0.90335(13) 0.60240(12) 0.0188(3) Uani 1 1 d . . .
C42 C 0.02234(15) 0.97523(13) 0.62156(13) 0.0210(4) Uani 1 1 d . . .
C43 C 0.04990(15) 1.04430(13) 0.65223(14) 0.0235(4) Uani 1 1 d . . .
C44 C 0.36245(13) 0.71380(12) 0.59765(12) 0.0164(3) Uani 1 1 d . . .
C45 C 0.45280(14) 0.72768(13) 0.60409(14) 0.0214(4) Uani 1 1 d . . .
H45 H 0.4633 0.7868 0.6085 0.026 Uiso 1 1 d R . .
C46 C 0.52711(15) 0.65467(14) 0.60417(15) 0.0246(4) Uani 1 1 d . . .
H46 H 0.5897 0.6642 0.6062 0.030 Uiso 1 1 d R . .
C47 C 0.50960(14) 0.56761(13) 0.60111(13) 0.0219(4) Uani 1 1 d . . .
H47 H 0.5593 0.5167 0.6024 0.026 Uiso 1 1 d R . .
C48 C 0.41847(14) 0.55691(13) 0.59607(12) 0.0186(3) Uani 1 1 d . . .
H48 H 0.4057 0.4975 0.5948 0.022 Uiso 1 1 d R . .
C49 C 0.16659(17) 1.01422(15) 0.74686(15) 0.0275(4) Uani 1 1 d . . .
H491 H 0.2374 0.9977 0.7434 0.036 Uiso 1 1 d R . .
H492 H 0.1446 1.0747 0.7666 0.036 Uiso 1 1 d R . .
C50 C 0.10633(18) 0.94331(16) 0.81733(15) 0.0307(4) Uani 1 1 d . . .
H501 H 0.1257 0.8837 0.7958 0.040 Uiso 1 1 d R . .
H502 H 0.0352 0.9619 0.8229 0.040 Uiso 1 1 d R . .
C51 C 0.11844(18) 0.92972(16) 0.90985(16) 0.0312(5) Uani 1 1 d . . .
H511 H 0.1893 0.9107 0.9053 0.041 Uiso 1 1 d R . .
H512 H 0.0980 0.9886 0.9328 0.041 Uiso 1 1 d R . .
C52 C 0.05590(18) 0.85731(17) 0.97562(15) 0.0322(5) Uani 1 1 d . . .
H521 H 0.0717 0.8009 0.9487 0.042 Uiso 1 1 d R . .
H522 H -0.0151 0.8796 0.9836 0.042 Uiso 1 1 d R . .
C53 C 0.07085(19) 0.83250(18) 1.06764(16) 0.0353(5) Uani 1 1 d . . .
H531 H 0.1403 0.8048 1.0612 0.046 Uiso 1 1 d R . .
H532 H 0.0594 0.8890 1.0937 0.046 Uiso 1 1 d R . .
C54 C 0.0004(2) 0.7653(2) 1.13077(18) 0.0464(6) Uani 1 1 d . . .
H541 H -0.0680 0.7958 1.1444 0.060(6) Uiso 1 1 d R . .
H542 H 0.0175 0.7444 1.1865 0.060(6) Uiso 1 1 d R . .
H543 H 0.0061 0.7125 1.1019 0.060(6) Uiso 1 1 d R . .
C55 C 0.22170(16) 1.09594(14) 0.58605(15) 0.0264(4) Uani 1 1 d . . .
H551 H 0.2925 1.0743 0.5800 0.034 Uiso 1 1 d R . .
H552 H 0.2043 1.1532 0.6117 0.034 Uiso 1 1 d R . .
C56 C 0.20930(16) 1.11760(15) 0.49273(16) 0.0278(4) Uani 1 1 d . . .
H561 H 0.2255 1.0602 0.4674 0.036 Uiso 1 1 d R . .
H562 H 0.1388 1.1405 0.4985 0.036 Uiso 1 1 d R . .
C57 C 0.27393(18) 1.18815(17) 0.42720(17) 0.0333(5) Uani 1 1 d . . .
H571 H 0.3447 1.1646 0.4192 0.043 Uiso 1 1 d R . .
H572 H 0.2594 1.2452 0.4528 0.043 Uiso 1 1 d R . .
C58 C 0.2565(2) 1.2096(2) 0.33580(18) 0.0415(6) Uani 1 1 d . C .
H581 H 0.2767 1.1534 0.3082 0.054 Uiso 1 1 d R . .
H582 H 0.1846 1.2272 0.3448 0.054 Uiso 1 1 d R . .
C59 C 0.3135(3) 1.2865(3) 0.2698(2) 0.0567(8) Uani 1 1 d . . .
H591 H 0.3805 1.2769 0.2720 0.074 Uiso 1 1 d R C .
H592 H 0.3152 1.2835 0.2102 0.074 Uiso 0.67 1 d PR A 1
H593 H 0.2826 1.3434 0.2901 0.074 Uiso 0.33 1 d PR B 2
C60A C 0.2666(3) 1.3845(3) 0.2910(3) 0.0544(12) Uani 0.67 1 d P C 1
H601 H 0.3027 1.4299 0.2459 0.082 Uiso 0.67 1 d PR C 1
H602 H 0.1987 1.3939 0.2914 0.082 Uiso 0.67 1 d PR C 1
H603 H 0.2690 1.3899 0.3487 0.082 Uiso 0.67 1 d PR C 1
C60B C 0.3151(8) 1.2967(7) 0.1809(7) 0.057(2) Uiso 0.33 1 d P C 2
H604 H 0.3457 1.2405 0.1590 0.085 Uiso 0.33 1 d PR C 2
H605 H 0.2486 1.3100 0.1775 0.085 Uiso 0.33 1 d PR C 2
H606 H 0.3528 1.3457 0.1450 0.085 Uiso 0.33 1 d PR C 2
C61 C 0.18948(18) 0.49010(15) 0.76485(14) 0.0298(4) Uani 1 1 d . . .
H611 H 0.1547 0.4817 0.8295 0.036(4) Uiso 1 1 d R . .
H612 H 0.2581 0.5007 0.7538 0.036(4) Uiso 1 1 d R . .
H613 H 0.1896 0.4350 0.7416 0.036(4) Uiso 1 1 d R . .
C62 C 0.12555(18) 0.67025(15) 0.77356(14) 0.0291(4) Uani 1 1 d . . .
H621 H 0.0858 0.7269 0.7562 0.034(4) Uiso 1 1 d R . .
H622 H 0.1936 0.6826 0.7621 0.034(4) Uiso 1 1 d R . .
H623 H 0.0964 0.6473 0.8375 0.034(4) Uiso 1 1 d R . .
C63 C 0.25325(15) 0.40269(14) 0.56497(14) 0.0241(4) Uani 1 1 d . . .
S2 S -0.07652(5) 0.48215(5) 0.93455(4) 0.03813(13) Uani 1 1 d . . .
O3 O -0.10637(18) 0.43646(17) 1.03048(13) 0.0563(6) Uani 1 1 d . . .
C64 C -0.1187(2) 0.6002(2) 0.9370(2) 0.0532(8) Uani 1 1 d . . .
H641 H -0.1883 0.6069 0.9747 0.047(5) Uiso 1 1 d R . .
H642 H -0.1133 0.6324 0.8759 0.047(5) Uiso 1 1 d R . .
H643 H -0.0783 0.6263 0.9618 0.047(5) Uiso 1 1 d R . .
C65 C -0.1668(3) 0.4590(3) 0.8885(2) 0.0552(8) Uani 1 1 d . . .
H651 H -0.1643 0.3926 0.8930 0.081(8) Uiso 1 1 d R . .
H652 H -0.1516 0.4879 0.8253 0.081(8) Uiso 1 1 d R . .
H653 H -0.2334 0.4839 0.9222 0.081(8) Uiso 1 1 d R . .
O4 O 0.52950(15) 1.06766(14) 0.35641(14) 0.0450(4) Uiso 1 1 d . . .
S3A S 0.54006(10) 0.96990(10) 0.33424(9) 0.0386(3) Uani 0.50 1 d P D 1
C66A C 0.4234(8) 0.9325(8) 0.3837(7) 0.096(3) Uiso 0.50 1 d P D 1
H661 H 0.4108 0.9167 0.4487 0.144 Uiso 0.50 1 d PR D 1
H662 H 0.4202 0.8785 0.3602 0.144 Uiso 0.50 1 d PR D 1
H663 H 0.3731 0.9820 0.3707 0.144 Uiso 0.50 1 d PR D 1
C67A C 0.5008(7) 0.9786(6) 0.2500(6) 0.068(2) Uiso 0.50 1 d P D 1
H671 H 0.5513 1.0018 0.1949 0.103 Uiso 0.50 1 d PR D 1
H672 H 0.4394 1.0211 0.2578 0.103 Uiso 0.50 1 d PR D 1
H673 H 0.4878 0.9183 0.2459 0.103 Uiso 0.50 1 d PR D 1
S3B S 0.46356(11) 1.00710(9) 0.35290(15) 0.0585(5) Uani 0.50 1 d P D 2
C66B C 0.4887(5) 0.9016(4) 0.4201(4) 0.0482(13) Uiso 0.50 1 d P D 2
H664 H 0.4519 0.9052 0.4832 0.072 Uiso 0.50 1 d PR D 2
H665 H 0.5601 0.8890 0.4125 0.072 Uiso 0.50 1 d PR D 2
H666 H 0.4677 0.8522 0.4022 0.072 Uiso 0.50 1 d PR D 2
C67B C 0.5525(5) 0.9722(4) 0.2262(4) 0.0451(13) Uiso 0.50 1 d P D 2
H674 H 0.5480 1.0246 0.1789 0.068 Uiso 0.50 1 d PR D 2
H675 H 0.5290 0.9197 0.2157 0.068 Uiso 0.50 1 d PR D 2
H676 H 0.6218 0.9561 0.2256 0.068 Uiso 0.50 1 d PR D 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ir 0.01455(3) 0.01408(3) 0.01593(3) -0.00310(2) -0.00529(2) -0.00154(2)
S1 0.0186(2) 0.0241(2) 0.0174(2) -0.00141(16) -0.00380(16) -0.00365(17)
O1 0.0212(7) 0.0522(10) 0.0251(7) 0.0020(7) -0.0041(6) -0.0139(7)
O2 0.0613(13) 0.0191(8) 0.0782(15) -0.0029(8) -0.0440(12) -0.0077(8)
N1 0.0182(7) 0.0169(7) 0.0221(7) -0.0043(6) -0.0084(6) -0.0012(6)
N2 0.0161(7) 0.0164(7) 0.0157(7) -0.0032(5) -0.0058(5) -0.0005(5)
N3 0.0202(8) 0.0228(8) 0.0230(8) -0.0025(6) -0.0064(6) -0.0025(6)
C1 0.0246(9) 0.0247(9) 0.0212(9) -0.0067(7) -0.0111(7) -0.0001(7)
C2 0.0192(8) 0.0166(8) 0.0215(8) -0.0049(6) -0.0081(7) -0.0004(6)
C3 0.0178(8) 0.0121(7) 0.0191(8) -0.0040(6) -0.0077(6) -0.0001(6)
C4 0.0187(8) 0.0167(8) 0.0175(8) -0.0037(6) -0.0070(6) -0.0019(6)
C5 0.0236(9) 0.0291(10) 0.0234(9) -0.0042(8) -0.0044(8) -0.0046(8)
C6 0.0237(10) 0.0397(12) 0.0321(11) -0.0044(9) -0.0034(9) -0.0085(9)
C7 0.0295(11) 0.0425(13) 0.0286(11) -0.0017(10) 0.0016(9) -0.0100(10)
C8 0.0321(11) 0.0389(12) 0.0199(9) -0.0012(8) -0.0001(8) -0.0055(9)
C9 0.0267(10) 0.0292(10) 0.0156(8) -0.0039(7) -0.0060(7) 0.0000(8)
C10 0.0240(9) 0.0226(9) 0.0163(8) -0.0049(7) -0.0065(7) -0.0001(7)
C11 0.0195(8) 0.0170(8) 0.0187(8) -0.0041(6) -0.0052(7) -0.0004(6)
C12 0.0222(9) 0.0204(9) 0.0192(8) -0.0029(7) -0.0032(7) -0.0024(7)
C13 0.0255(10) 0.0267(10) 0.0191(9) -0.0016(7) -0.0039(7) -0.0031(8)
C14 0.0199(8) 0.0173(8) 0.0234(9) -0.0049(7) -0.0098(7) -0.0006(6)
C15 0.0262(10) 0.0311(10) 0.0265(10) -0.0066(8) -0.0139(8) -0.0038(8)
C16 0.0268(10) 0.0402(12) 0.0358(12) -0.0051(9) -0.0186(9) -0.0072(9)
C17 0.0204(9) 0.0379(12) 0.0357(11) -0.0039(9) -0.0127(8) -0.0056(8)
C18 0.0192(9) 0.0263(10) 0.0285(10) -0.0051(8) -0.0087(8) -0.0039(7)
C19 0.0347(11) 0.0326(11) 0.0213(9) -0.0007(8) -0.0102(8) 0.0018(9)
C20 0.0421(13) 0.0294(11) 0.0306(11) -0.0016(9) -0.0118(10) 0.0013(10)
C21 0.066(2) 0.0431(16) 0.074(2) -0.0133(15) -0.0447(19) 0.0112(14)
C22 0.0488(16) 0.0441(15) 0.0529(17) -0.0048(13) -0.0221(14) 0.0016(12)
C23 0.0538(19) 0.0499(18) 0.072(2) -0.0126(16) -0.0226(17) -0.0029(14)
C24 0.0522(18) 0.0494(17) 0.0535(18) -0.0091(14) -0.0071(14) -0.0023(14)
C25 0.0325(11) 0.0333(11) 0.0182(9) -0.0080(8) -0.0089(8) 0.0010(9)
C26 0.0384(12) 0.0318(11) 0.0257(10) -0.0107(8) -0.0140(9) 0.0039(9)
C27 0.0336(11) 0.0330(11) 0.0300(11) -0.0133(9) -0.0098(9) 0.0005(9)
C28 0.0410(13) 0.0316(12) 0.0351(12) -0.0110(9) -0.0137(10) 0.0030(10)
C29 0.0454(15) 0.0379(13) 0.0477(15) -0.0181(12) -0.0115(12) 0.0056(11)
C30 0.066(2) 0.0374(14) 0.0466(16) -0.0112(12) -0.0145(14) -0.0043(13)
C31 0.0182(8) 0.0192(8) 0.0234(9) -0.0064(7) -0.0081(7) -0.0018(6)
C32 0.0156(8) 0.0172(8) 0.0175(8) -0.0037(6) -0.0056(6) -0.0011(6)
C33 0.0167(8) 0.0169(8) 0.0158(7) -0.0036(6) -0.0048(6) -0.0016(6)
C34 0.0172(8) 0.0179(8) 0.0201(8) -0.0034(6) -0.0074(6) -0.0009(6)
C35 0.0213(9) 0.0242(9) 0.0261(10) -0.0029(7) -0.0087(8) 0.0006(7)
C36 0.0210(9) 0.0290(10) 0.0320(11) -0.0015(8) -0.0081(8) 0.0046(8)
C37 0.0269(10) 0.0228(10) 0.0360(11) -0.0053(8) -0.0064(9) 0.0082(8)
C38 0.0323(11) 0.0198(9) 0.0366(11) -0.0101(8) -0.0103(9) 0.0044(8)
C39 0.0237(9) 0.0178(8) 0.0318(10) -0.0100(7) -0.0115(8) 0.0013(7)
C40 0.0206(8) 0.0162(8) 0.0238(9) -0.0064(7) -0.0077(7) -0.0005(6)
C41 0.0178(8) 0.0180(8) 0.0202(8) -0.0033(6) -0.0067(7) 0.0006(6)
C42 0.0215(9) 0.0182(8) 0.0223(9) -0.0038(7) -0.0070(7) 0.0007(7)
C43 0.0247(9) 0.0180(8) 0.0269(10) -0.0054(7) -0.0080(8) 0.0016(7)
C44 0.0168(8) 0.0166(8) 0.0148(7) -0.0031(6) -0.0043(6) -0.0003(6)
C45 0.0190(8) 0.0198(8) 0.0269(9) -0.0057(7) -0.0085(7) -0.0013(7)
C46 0.0180(9) 0.0256(10) 0.0328(10) -0.0067(8) -0.0110(8) -0.0007(7)
C47 0.0178(8) 0.0215(9) 0.0256(9) -0.0043(7) -0.0080(7) 0.0022(7)
C48 0.0194(8) 0.0167(8) 0.0183(8) -0.0024(6) -0.0057(7) 0.0007(6)
C49 0.0311(11) 0.0228(9) 0.0337(11) -0.0127(8) -0.0139(9) 0.0012(8)
C50 0.0357(12) 0.0310(11) 0.0289(11) -0.0116(9) -0.0110(9) -0.0030(9)
C51 0.0364(12) 0.0296(11) 0.0312(11) -0.0129(9) -0.0137(9) 0.0027(9)
C52 0.0317(11) 0.0374(12) 0.0293(11) -0.0137(9) -0.0103(9) 0.0026(9)
C53 0.0365(12) 0.0395(13) 0.0307(11) -0.0113(10) -0.0112(10) 0.0010(10)
C54 0.0532(17) 0.0511(16) 0.0324(13) -0.0117(12) -0.0076(12) -0.0054(13)
C55 0.0270(10) 0.0199(9) 0.0359(11) -0.0066(8) -0.0127(8) -0.0038(7)
C56 0.0260(10) 0.0239(10) 0.0361(11) -0.0065(8) -0.0120(9) -0.0037(8)
C57 0.0309(11) 0.0348(12) 0.0369(12) -0.0040(9) -0.0119(9) -0.0097(9)
C58 0.0417(14) 0.0482(15) 0.0358(13) -0.0009(11) -0.0127(11) -0.0144(12)
C59 0.0562(19) 0.074(2) 0.0386(15) 0.0014(15) -0.0074(13) -0.0304(17)
C60A 0.041(2) 0.056(3) 0.058(3) 0.018(2) -0.019(2) -0.010(2)
C61 0.0338(11) 0.0268(10) 0.0216(9) 0.0028(8) -0.0053(8) -0.0002(8)
C62 0.0350(11) 0.0298(10) 0.0202(9) -0.0058(8) -0.0061(8) -0.0013(9)
C63 0.0224(9) 0.0252(9) 0.0307(10) -0.0071(8) -0.0149(8) -0.0023(7)
S2 0.0398(3) 0.0422(3) 0.0265(3) -0.0010(2) -0.0065(2) -0.0031(3)
O3 0.0637(14) 0.0698(15) 0.0300(10) 0.0085(9) -0.0131(9) -0.0178(12)
C64 0.0508(17) 0.0461(16) 0.0541(18) -0.0145(14) -0.0083(14) 0.0077(13)
C65 0.063(2) 0.065(2) 0.0379(15) -0.0051(14) -0.0216(14) -0.0016(16)
S3A 0.0333(6) 0.0427(7) 0.0433(7) -0.0099(5) -0.0154(5) -0.0029(5)
S3B 0.0346(7) 0.0271(6) 0.1287(16) -0.0255(8) -0.0392(9) 0.0010(5)

_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
Ir C33 2.0188(19) . ?
Ir C3 2.0302(19) . ?
Ir N2 2.0523(16) . ?
Ir N1 2.0665(16) . ?
Ir N3 2.1361(18) . ?
Ir S1 2.3725(7) . ?
S1 O1 1.4872(16) . ?
S1 C62 1.782(2) . ?
S1 C61 1.783(2) . ?
O2 C63 1.205(3) . ?
N1 C18 1.353(3) . ?
N1 C14 1.366(2) . ?
N2 C48 1.352(2) . ?
N2 C44 1.366(2) . ?
N3 C63 1.145(3) . ?
C1 C10 1.384(3) . ?
C1 C2 1.405(3) . ?
C2 C3 1.410(2) . ?
C2 C14 1.464(3) . ?
C3 C4 1.403(3) . ?
C4 C11 1.387(3) . ?
C5 C12 1.387(3) . ?
C5 C6 1.396(3) . ?
C6 C7 1.397(3) . ?
C7 C8 1.389(4) . ?
C8 C13 1.396(3) . ?
C9 C10 1.524(3) . ?
C9 C13 1.527(3) . ?
C9 C19 1.545(3) . ?
C9 C25 1.546(3) . ?
C10 C11 1.401(3) . ?
C11 C12 1.473(3) . ?
C12 C13 1.404(3) . ?
C14 C15 1.396(3) . ?
C15 C16 1.382(3) . ?
C16 C17 1.388(3) . ?
C17 C18 1.383(3) . ?
C19 C20 1.531(3) . ?
C20 C21 1.495(4) . ?
C21 C22 1.535(4) . ?
C22 C23 1.475(4) . ?
C23 C24 1.503(5) . ?
C25 C26 1.518(3) . ?
C26 C27 1.527(3) . ?
C27 C28 1.532(3) . ?
C28 C29 1.528(3) . ?
C29 C30 1.499(4) . ?
C31 C40 1.381(3) . ?
C31 C32 1.403(3) . ?
C32 C33 1.423(2) . ?
C32 C44 1.463(2) . ?
C33 C34 1.406(2) . ?
C34 C41 1.394(3) . ?
C35 C42 1.389(3) . ?
C35 C36 1.394(3) . ?
C36 C37 1.390(3) . ?
C37 C38 1.392(3) . ?
C38 C43 1.387(3) . ?
C39 C43 1.523(3) . ?
C39 C40 1.525(3) . ?
C39 C49 1.547(3) . ?
C39 C55 1.549(3) . ?
C40 C41 1.406(3) . ?
C41 C42 1.470(3) . ?
C42 C43 1.408(3) . ?
C44 C45 1.395(3) . ?
C45 C46 1.386(3) . ?
C46 C47 1.392(3) . ?
C47 C48 1.382(3) . ?
C49 C50 1.525(3) . ?
C50 C51 1.520(3) . ?
C51 C52 1.528(4) . ?
C52 C53 1.522(3) . ?
C53 C54 1.522(4) . ?
C55 C56 1.527(3) . ?
C56 C57 1.523(3) . ?
C57 C58 1.528(4) . ?
C58 C59 1.539(4) . ?
C59 C60B 1.394(11) . ?
C59 C60A 1.563(6) . ?
S2 O3 1.495(2) . ?
S2 C64 1.772(3) . ?
S2 C65 1.813(3) . ?
O4 S3B 1.452(2) . ?
O4 S3A 1.555(2) . ?
S3A C67A 1.606(8) . ?
S3A C66A 1.739(11) . ?
S3B C66B 1.770(6) . ?
S3B C67B 2.124(7) . ?

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
C33 Ir C3 92.16(7) . . ?
C33 Ir N2 80.65(7) . . ?
C3 Ir N2 88.96(7) . . ?
C33 Ir N1 98.39(7) . . ?
C3 Ir N1 79.92(7) . . ?
N2 Ir N1 168.81(6) . . ?
C33 Ir N3 174.76(7) . . ?
C3 Ir N3 90.36(7) . . ?
N2 Ir N3 94.81(6) . . ?
N1 Ir N3 86.57(6) . . ?
C33 Ir S1 89.31(5) . . ?
C3 Ir S1 178.52(5) . . ?
N2 Ir S1 91.47(5) . . ?
N1 Ir S1 99.68(5) . . ?
N3 Ir S1 88.19(5) . . ?
O1 S1 C62 106.74(11) . . ?
O1 S1 C61 107.09(11) . . ?
C62 S1 C61 99.23(11) . . ?
O1 S1 Ir 119.92(7) . . ?
C62 S1 Ir 111.46(8) . . ?
C61 S1 Ir 110.33(8) . . ?
C18 N1 C14 118.84(17) . . ?
C18 N1 Ir 126.31(14) . . ?
C14 N1 Ir 114.72(12) . . ?
C48 N2 C44 119.85(16) . . ?
C48 N2 Ir 123.74(13) . . ?
C44 N2 Ir 115.18(12) . . ?
C63 N3 Ir 165.00(17) . . ?
C10 C1 C2 118.93(17) . . ?
C1 C2 C3 121.92(17) . . ?
C1 C2 C14 122.97(17) . . ?
C3 C2 C14 114.98(16) . . ?
C4 C3 C2 118.08(17) . . ?
C4 C3 Ir 127.77(13) . . ?
C2 C3 Ir 114.11(13) . . ?
C11 C4 C3 119.72(17) . . ?
C12 C5 C6 118.5(2) . . ?
C5 C6 C7 120.4(2) . . ?
C8 C7 C6 121.0(2) . . ?
C7 C8 C13 118.9(2) . . ?
C10 C9 C13 100.80(16) . . ?
C10 C9 C19 111.70(17) . . ?
C13 C9 C19 112.46(18) . . ?
C10 C9 C25 111.09(17) . . ?
C13 C9 C25 111.31(17) . . ?
C19 C9 C25 109.29(17) . . ?
C1 C10 C11 119.53(17) . . ?
C1 C10 C9 129.12(18) . . ?
C11 C10 C9 111.34(17) . . ?
C4 C11 C10 121.80(18) . . ?
C4 C11 C12 129.84(17) . . ?
C10 C11 C12 108.36(17) . . ?
C5 C12 C13 121.36(19) . . ?
C5 C12 C11 130.51(18) . . ?
C13 C12 C11 108.12(18) . . ?
C8 C13 C12 119.8(2) . . ?
C8 C13 C9 128.91(19) . . ?
C12 C13 C9 111.24(17) . . ?
N1 C14 C15 120.30(18) . . ?
N1 C14 C2 114.73(16) . . ?
C15 C14 C2 124.87(18) . . ?
C16 C15 C14 120.5(2) . . ?
C15 C16 C17 118.6(2) . . ?
C18 C17 C16 119.2(2) . . ?
N1 C18 C17 122.5(2) . . ?
C20 C19 C9 114.83(19) . . ?
C21 C20 C19 113.5(2) . . ?
C20 C21 C22 114.8(3) . . ?
C23 C22 C21 112.2(3) . . ?
C22 C23 C24 114.4(3) . . ?
C26 C25 C9 114.28(17) . . ?
C25 C26 C27 114.63(18) . . ?
C26 C27 C28 111.48(19) . . ?
C29 C28 C27 115.5(2) . . ?
C30 C29 C28 114.2(2) . . ?
C40 C31 C32 118.44(17) . . ?
C31 C32 C33 122.53(16) . . ?
C31 C32 C44 122.04(16) . . ?
C33 C32 C44 115.20(16) . . ?
C34 C33 C32 117.51(16) . . ?
C34 C33 Ir 128.07(14) . . ?
C32 C33 Ir 113.82(13) . . ?
C41 C34 C33 119.77(17) . . ?
C42 C35 C36 118.9(2) . . ?
C37 C36 C35 120.5(2) . . ?
C36 C37 C38 120.79(19) . . ?
C43 C38 C37 119.2(2) . . ?
C43 C39 C40 100.91(15) . . ?
C43 C39 C49 112.12(17) . . ?
C40 C39 C49 110.68(16) . . ?
C43 C39 C55 111.19(17) . . ?
C40 C39 C55 111.93(17) . . ?
C49 C39 C55 109.78(17) . . ?
C31 C40 C41 120.24(17) . . ?
C31 C40 C39 128.05(17) . . ?
C41 C40 C39 111.52(16) . . ?
C34 C41 C40 121.39(17) . . ?
C34 C41 C42 130.61(18) . . ?
C40 C41 C42 107.92(16) . . ?
C35 C42 C43 120.65(18) . . ?
C35 C42 C41 130.78(18) . . ?
C43 C42 C41 108.56(17) . . ?
C38 C43 C42 120.0(2) . . ?
C38 C43 C39 128.91(19) . . ?
C42 C43 C39 111.05(17) . . ?
N2 C44 C45 120.11(16) . . ?
N2 C44 C32 114.13(16) . . ?
C45 C44 C32 125.74(17) . . ?
C46 C45 C44 119.64(18) . . ?
C45 C46 C47 119.70(18) . . ?
C48 C47 C46 118.58(17) . . ?
N2 C48 C47 122.07(17) . . ?
C50 C49 C39 114.08(18) . . ?
C51 C50 C49 115.18(19) . . ?
C50 C51 C52 111.45(19) . . ?
C53 C52 C51 115.1(2) . . ?
C52 C53 C54 111.5(2) . . ?
C56 C55 C39 114.17(17) . . ?
C57 C56 C55 114.21(18) . . ?
C56 C57 C58 112.2(2) . . ?
C57 C58 C59 114.2(2) . . ?
C60B C59 C58 116.1(5) . . ?
C60B C59 C60A 100.6(5) . . ?
C58 C59 C60A 113.3(3) . . ?
N3 C63 O2 179.6(3) . . ?
O3 S2 C64 105.32(15) . . ?
O3 S2 C65 105.52(15) . . ?
C64 S2 C65 97.00(17) . . ?
S3B O4 S3A 43.31(9) . . ?
O4 S3A C67A 108.1(3) . . ?
O4 S3A C66A 106.3(4) . . ?
C67A S3A C66A 77.1(5) . . ?
O4 S3B C66B 106.0(2) . . ?
O4 S3B C67B 95.3(2) . . ?
C66B S3B C67B 97.9(3) . . ?

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
C24 C23 C22 C21 179.2(3) . . . . ?
C23 C22 C21 C20 -161.2(3) . . . . ?
C22 C21 C20 C19 -179.9(3) . . . . ?
C21 C20 C19 C9 -158.6(2) . . . . ?
C20 C19 C9 C25 -179.1(2) . . . . ?
C19 C9 C25 C26 173.0(2) . . . . ?
C9 C25 C26 C27 175.3(2) . . . . ?
C25 C26 C27 C28 168.3(2) . . . . ?
C26 C27 C28 C29 -177.9(2) . . . . ?
C27 C28 C29 C30 -71.1(3) . . . . ?
C54 C53 C52 C51 175.8(2) . . . . ?
C53 C52 C51 C50 174.4(2) . . . . ?
C52 C51 C50 C49 -179.71(19) . . . . ?
C51 C50 C49 C39 176.74(18) . . . . ?
C50 C49 C39 C55 -179.74(18) . . . . ?
C49 C39 C55 C56 -173.59(17) . . . . ?
C39 C55 C56 C57 -178.84(19) . . . . ?
C55 C56 C57 C58 -178.2(2) . . . . ?
C56 C57 C58 C59 175.1(3) . . . . ?
C57 C58 C59 C60A -76.0(4) . . . . ?
C57 C58 C59 C60B 168.3(6) . . . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        30.00
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         1.395
_refine_diff_density_min         -1.021
_refine_diff_density_rms         0.084

#===================================END