# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2a
_database_code_depnum_ccdc_archive 'CCDC 1440254'
_audit_update_record             
;
2016-01-25 deposited with the CCDC.
2016-01-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C100 H100 F12 Ir4 N12 O12 S4'
_chemical_formula_weight         2786.95

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'
F F 0.0171 0.0103 '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'

_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_H-M_alt        'P 42/n'
_space_group_name_Hall           '-P 4bc'

_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'
'-y, x+1/2, z+1/2'
'y+1/2, -x, z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y, -x-1/2, -z-1/2'
'-y-1/2, x, -z-1/2'

_cell_length_a                   18.9052(16)
_cell_length_b                   18.9052(16)
_cell_length_c                   16.5315(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5908.5(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    4935
_cell_measurement_theta_min      2.15
_cell_measurement_theta_max      21.37

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_F_000             2720
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    4.637
_shelx_estimated_absorpt_T_min   0.708
_shelx_estimated_absorpt_T_max   0.836
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.611
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_process_details   sadabs

_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            41241
_diffrn_reflns_av_unetI/netI     0.0837
_diffrn_reflns_av_R_equivalents  0.0806
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.959
_diffrn_reflns_theta_max         26.998
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             6439
_reflns_number_gt                3192
_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-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 
 In asymmetric unit of this data, there were disordered
 solvents which could not be restrained properly. Therefore,
 SQUEEZE algorithm was used to omit it.
 The pentamethylcyclopentadienyl ligand was disordered and 
 it was divided into two parts (65:35). 32 ISOR, 26 DFIX and 
 1 SIMU instructions were used to restrain Cp* fragment so 
 that there were 254 restraints in the data. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
; 
 w=1/[σ²(Fo²)+(0.1951P)²] 
 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         6439
_refine_ls_number_parameters     398
_refine_ls_number_restraints     254
_refine_ls_R_factor_all          0.1550
_refine_ls_R_factor_gt           0.0973
_refine_ls_wR_factor_ref         0.3027
_refine_ls_wR_factor_gt          0.2622
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_restrained_S_all      0.989
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001

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
1 0.250 0.250 0.250 148.8 69.4
2 0.750 0.750 0.250 39.1 9.5
3 0.750 0.750 0.750 148.9 78.9
4 0.250 0.250 0.750 39.1 14.7
_platon_squeeze_details          
; 

 In asymmetric unit of this data, there were disordered 
 solvents which could not be restrained properly. Therefore, 
 SQUEEZE algorithm was used to omit it. 
;

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 0.01046(4) 0.83387(3) 0.04941(4) 0.0857(3) Uani 1 1 d . . . . .
N1 N 0.0180(5) 0.8952(5) 0.1526(6) 0.060(2) Uani 1 1 d . . . . .
N2 N -0.0981(8) 0.8570(6) 0.0491(8) 0.083(4) Uani 1 1 d . . . . .
N3 N -0.2548(5) 0.9821(8) 0.3676(9) 0.101(4) Uani 1 1 d . U . . .
C1 C 0.0774(6) 0.9130(7) 0.1901(9) 0.073(4) Uani 1 1 d . . . . .
H1 H 0.1229 0.9043 0.1679 0.088 Uiso 1 1 calc R U . . .
C2 C 0.0670(7) 0.9469(8) 0.2679(10) 0.090(4) Uani 1 1 d . . . . .
H2 H 0.1016 0.9641 0.3047 0.108 Uiso 1 1 calc R U . . .
C3 C -0.0058(7) 0.9480(7) 0.2752(9) 0.078(4) Uani 1 1 d . . . . .
H3 H -0.0316 0.9661 0.3200 0.093 Uiso 1 1 calc R U . . .
C4 C -0.0366(6) 0.9166(6) 0.2027(8) 0.062(3) Uani 1 1 d . . . . .
C5 C -0.1068(7) 0.9105(7) 0.1858(8) 0.066(3) Uani 1 1 d . . . . .
C6 C -0.1365(8) 0.8855(8) 0.1138(10) 0.081(4) Uani 1 1 d . . . . .
C7 C -0.2097(9) 0.8774(11) 0.0948(13) 0.120(7) Uani 1 1 d . . . . .
H7 H -0.2490 0.8889 0.1280 0.144 Uiso 1 1 calc R U . . .
C8 C -0.2110(17) 0.8499(14) 0.0188(15) 0.141(9) Uani 1 1 d . . . . .
H8 H -0.2522 0.8394 -0.0117 0.169 Uiso 1 1 calc R U . . .
C9 C -0.1445(16) 0.8401(9) -0.0056(13) 0.117(7) Uani 1 1 d . . . . .
H9 H -0.1323 0.8226 -0.0576 0.140 Uiso 1 1 calc R U . . .
C10 C -0.2419(8) 1.0218(10) 0.3023(10) 0.096(5) Uani 1 1 d . . . . .
H10 H -0.2653 1.0659 0.2961 0.115 Uiso 1 1 calc R U . . .
C11 C -0.1933(8) 0.9984(10) 0.2418(10) 0.101(5) Uani 1 1 d . . . . .
H11 H -0.1865 1.0264 0.1948 0.121 Uiso 1 1 calc R U . . .
C12 C -0.1556(6) 0.9357(9) 0.2503(9) 0.082(4) Uani 1 1 d . . . . .
C13 C -0.1670(9) 0.8992(11) 0.3196(10) 0.120(6) Uani 1 1 d . U . . .
H13 H -0.1412 0.8571 0.3302 0.144 Uiso 1 1 calc R U . . .
C14 C -0.2169(10) 0.9238(12) 0.3756(13) 0.138(7) Uani 1 1 d . U . . .
H14 H -0.2241 0.8964 0.4231 0.166 Uiso 1 1 calc R U . . .
C15 C 0.0248(8) 0.8580(6) -0.0767(5) 0.086(6) Uani 0.65(3) 1 d G U P A 1
C16 C 0.0836(7) 0.8841(4) -0.0322(6) 0.084(5) Uani 0.65(3) 1 d G U P A 1
C17 C 0.1196(5) 0.8252(4) 0.0020(7) 0.094(5) Uani 0.65(3) 1 d G U P A 1
C18 C 0.0831(5) 0.7627(4) -0.0213(6) 0.102(5) Uani 0.65(3) 1 d G U P A 1
C19 C 0.0244(6) 0.7830(6) -0.0699(5) 0.106(6) Uani 0.65(3) 1 d G U P A 1
C20 C -0.0281(13) 0.9021(9) -0.1230(7) 0.093(9) Uani 0.65(3) 1 d G U P A 1
H20A H -0.0030 0.9326 -0.1615 0.140 Uiso 0.65(3) 1 calc R U P A 1
H20B H -0.0551 0.9315 -0.0851 0.140 Uiso 0.65(3) 1 calc R U P A 1
H20C H -0.0605 0.8710 -0.1525 0.140 Uiso 0.65(3) 1 calc R U P A 1
C21 C 0.1042(10) 0.9609(5) -0.0229(9) 0.091(8) Uani 0.65(3) 1 d G U P A 1
H21A H 0.1356 0.9745 -0.0674 0.136 Uiso 0.65(3) 1 calc R U P A 1
H21B H 0.1288 0.9675 0.0287 0.136 Uiso 0.65(3) 1 calc R U P A 1
H21C H 0.0617 0.9904 -0.0241 0.136 Uiso 0.65(3) 1 calc R U P A 1
C22 C 0.1853(6) 0.8285(6) 0.0541(12) 0.099(8) Uani 0.65(3) 1 d G U P A 1
H22A H 0.1755 0.8068 0.1067 0.148 Uiso 0.65(3) 1 calc R U P A 1
H22B H 0.1991 0.8780 0.0619 0.148 Uiso 0.65(3) 1 calc R U P A 1
H22C H 0.2238 0.8029 0.0273 0.148 Uiso 0.65(3) 1 calc R U P A 1
C23 C 0.1030(8) 0.6880(6) 0.0016(8) 0.149(10) Uani 0.65(3) 1 d G U P A 1
H23A H 0.1359 0.6688 -0.0386 0.223 Uiso 0.65(3) 1 calc R U P A 1
H23B H 0.0603 0.6585 0.0035 0.223 Uiso 0.65(3) 1 calc R U P A 1
H23C H 0.1257 0.6880 0.0549 0.223 Uiso 0.65(3) 1 calc R U P A 1
C24 C -0.0289(8) 0.7335(9) -0.1078(9) 0.176(13) Uani 0.65(3) 1 d G U P A 1
H24A H -0.0582 0.7597 -0.1465 0.264 Uiso 0.65(3) 1 calc R U P A 1
H24B H -0.0591 0.7133 -0.0655 0.264 Uiso 0.65(3) 1 calc R U P A 1
H24C H -0.0040 0.6953 -0.1361 0.264 Uiso 0.65(3) 1 calc R U P A 1
C15' C 0.0478(8) 0.8726(5) -0.0753(5) 0.086(6) Uani 0.35(3) 1 d G . P A 2
C16' C 0.1002(7) 0.8893(4) -0.0160(7) 0.084(5) Uani 0.35(3) 1 d G . P A 2
C17' C 0.1203(5) 0.8251(4) 0.0234(7) 0.094(5) Uani 0.35(3) 1 d G U P A 2
C18' C 0.0803(5) 0.7687(4) -0.0117(6) 0.102(5) Uani 0.35(3) 1 d G . P A 2
C19' C 0.0355(6) 0.7981(6) -0.0726(5) 0.106(6) Uani 0.35(3) 1 d G . P A 2
C20' C 0.0116(14) 0.9249(8) -0.1314(6) 0.072(12) Uani 0.35(3) 1 d G U P A 2
H20D H 0.0051 0.9700 -0.1032 0.108 Uiso 0.35(3) 1 calc R U P A 2
H20E H -0.0346 0.9061 -0.1476 0.108 Uiso 0.35(3) 1 calc R U P A 2
H20F H 0.0409 0.9323 -0.1795 0.108 Uiso 0.35(3) 1 calc R U P A 2
C21' C 0.1294(9) 0.9625(5) 0.0021(10) 0.070(12) Uani 0.35(3) 1 d G U P A 2
H21D H 0.1198 0.9746 0.0587 0.105 Uiso 0.35(3) 1 calc R U P A 2
H21E H 0.1067 0.9972 -0.0334 0.105 Uiso 0.35(3) 1 calc R U P A 2
H21F H 0.1806 0.9628 -0.0074 0.105 Uiso 0.35(3) 1 calc R U P A 2
C22' C 0.1746(8) 0.8180(6) 0.0906(11) 0.140(14) Uani 0.35(3) 1 d G U P A 2
H22D H 0.2220 0.8142 0.0670 0.211 Uiso 0.35(3) 1 calc R U P A 2
H22E H 0.1644 0.7754 0.1225 0.211 Uiso 0.35(3) 1 calc R U P A 2
H22F H 0.1724 0.8597 0.1257 0.211 Uiso 0.35(3) 1 calc R U P A 2
C23' C 0.0847(8) 0.6911(6) 0.0118(8) 0.149(10) Uani 0.35(3) 1 d G . P A 2
H23D H 0.1204 0.6675 -0.0216 0.223 Uiso 0.35(3) 1 calc R U P A 2
H23E H 0.0386 0.6687 0.0032 0.223 Uiso 0.35(3) 1 calc R U P A 2
H23F H 0.0978 0.6872 0.0690 0.223 Uiso 0.35(3) 1 calc R U P A 2
C24' C -0.0161(8) 0.7572(9) -0.1254(8) 0.176(13) Uani 0.35(3) 1 d G . P A 2
H24D H 0.0065 0.7458 -0.1771 0.264 Uiso 0.35(3) 1 calc R U P A 2
H24E H -0.0582 0.7862 -0.1351 0.264 Uiso 0.35(3) 1 calc R U P A 2
H24F H -0.0298 0.7134 -0.0979 0.264 Uiso 0.35(3) 1 calc R U P A 2
S1 S 0.2228(9) 0.6865(9) 0.2839(11) 0.172(6) Uani 0.5 1 d D U P . .
O1 O 0.1952(12) 0.6845(14) 0.2014(12) 0.103(7) Uani 0.5 1 d D U P . .
O2 O 0.2728(13) 0.6288(15) 0.2858(17) 0.139(9) Uani 0.5 1 d D U P . .
O3 O 0.1686(13) 0.6769(16) 0.3373(14) 0.131(9) Uani 0.5 1 d D U P . .
C25 C 0.2689(10) 0.7601(10) 0.2977(11) 0.039(6) Uani 0.5 1 d D U P . .
F1 F 0.2895(16) 0.7666(19) 0.3695(16) 0.197(13) Uani 0.5 1 d D U P . .
F2 F 0.3186(13) 0.7691(14) 0.2384(15) 0.144(8) Uani 0.5 1 d D U P . .
F3 F 0.218(2) 0.804(3) 0.285(3) 0.25(2) Uani 0.5 1 d D U P . .
S2 S 0.4085(12) 0.0510(14) 0.0329(12) 0.210(8) Uani 0.5 1 d D U P . .
O4 O 0.401(3) -0.002(2) -0.025(2) 0.25(2) Uani 0.5 1 d D U P . .
O5 O 0.377(2) 0.119(2) 0.016(3) 0.25(2) Uani 0.5 1 d D U P . .
O6 O 0.4821(17) 0.055(2) 0.053(3) 0.25(2) Uani 0.5 1 d D U P . .
C26 C 0.346(2) 0.012(3) 0.106(3) 0.33(6) Uani 0.5 1 d D U P . .
F4 F 0.2748(19) 0.0158(19) 0.120(2) 0.231(15) Uani 0.5 1 d D U P . .
F5 F 0.364(2) -0.051(2) 0.143(2) 0.256(17) Uani 0.5 1 d D U P . .
F6 F 0.362(3) 0.057(2) 0.167(3) 0.31(2) Uani 0.5 1 d D U P . .


_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 N1 2.068(10) . ?
Ir1 C18' 2.069(9) . ?
Ir1 N2 2.098(15) . ?
Ir1 N3 2.098(12) 7_466 ?
Ir1 C17' 2.127(9) . ?
Ir1 C15 2.151(8) . ?
Ir1 C16 2.152(8) . ?
Ir1 C19' 2.180(8) . ?
Ir1 C19 2.211(9) . ?
Ir1 C17 2.214(8) . ?
Ir1 C18 2.249(9) . ?
Ir1 C16' 2.268(8) . ?
N1 C1 1.326(16) . ?
N1 C4 1.383(14) . ?
N2 C9 1.30(2) . ?
N2 C6 1.40(2) . ?
N3 C14 1.32(2) . ?
N3 C10 1.336(19) . ?
N3 Ir1 2.098(12) 8_666 ?
C1 C2 1.45(2) . ?
C2 C3 1.383(18) . ?
C3 C4 1.459(19) . ?
C4 C5 1.362(17) . ?
C5 C6 1.40(2) . ?
C5 C12 1.488(18) . ?
C6 C7 1.43(2) . ?
C7 C8 1.36(3) . ?
C8 C9 1.33(3) . ?
C10 C11 1.43(2) . ?
C11 C12 1.39(2) . ?
C12 C13 1.355(19) . ?
C13 C14 1.40(2) . ?
C15 C16 1.422(4) . ?
C15 C19 1.422(4) . ?
C15 C20 1.511(5) . ?
C16 C17 1.422(4) . ?
C16 C21 1.512(5) . ?
C17 C18 1.422(4) . ?
C17 C22 1.511(5) . ?
C18 C19 1.422(4) . ?
C18 C23 1.511(5) . ?
C19 C24 1.511(5) . ?
C15' C16' 1.428(4) . ?
C15' C19' 1.429(4) . ?
C15' C20' 1.519(5) . ?
C16' C17' 1.429(4) . ?
C16' C21' 1.519(5) . ?
C17' C18' 1.429(4) . ?
C17' C22' 1.519(5) . ?
C18' C19' 1.429(4) . ?
C18' C23' 1.519(5) . ?
C19' C24' 1.519(5) . ?
S1 C25 1.05(3) 2_565 ?
S1 F3 1.13(4) 2_565 ?
S1 O3 1.36(2) . ?
S1 F2 1.37(3) 2_565 ?
S1 O2 1.44(2) . ?
S1 O1 1.46(2) . ?
S1 C25 1.66(2) . ?
S1 F1 1.69(3) 2_565 ?
O1 F2 1.10(3) 2_565 ?
O2 F3 1.27(5) 2_565 ?
O3 F1 1.43(4) 2_565 ?
O3 C25 1.80(3) 2_565 ?
C25 C25 0.81(3) 2_565 ?
C25 S1 1.05(3) 2_565 ?
C25 F1 1.26(2) . ?
C25 F3 1.26(5) 2_565 ?
C25 F3 1.29(3) . ?
C25 F2 1.37(2) . ?
C25 F1 1.70(3) 2_565 ?
C25 O3 1.80(3) 2_565 ?
F1 O3 1.43(4) 2_565 ?
F1 F1 1.62(6) 2_565 ?
F1 S1 1.69(3) 2_565 ?
F1 C25 1.70(3) 2_565 ?
F2 O1 1.10(3) 2_565 ?
F2 S1 1.37(3) 2_565 ?
F2 F3 1.73(5) 2_565 ?
F3 S1 1.13(4) 2_565 ?
F3 C25 1.26(5) 2_565 ?
F3 O2 1.27(5) 2_565 ?
F3 F2 1.73(5) 2_565 ?
S2 O4 1.40(2) . ?
S2 O6 1.43(3) . ?
S2 O5 1.45(2) . ?
S2 C26 1.84(3) . ?
C26 F6 1.35(3) . ?
C26 F4 1.37(3) . ?
C26 F5 1.37(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
N1 Ir1 C18' 133.8(4) . . ?
N1 Ir1 N2 87.3(5) . . ?
C18' Ir1 N2 138.3(5) . . ?
N1 Ir1 N3 82.9(4) . 7_466 ?
C18' Ir1 N3 93.3(5) . 7_466 ?
N2 Ir1 N3 84.3(5) . 7_466 ?
N1 Ir1 C17' 98.2(4) . . ?
C18' Ir1 C17' 39.80(17) . . ?
N2 Ir1 C17' 166.1(4) . . ?
N3 Ir1 C17' 109.0(5) 7_466 . ?
N1 Ir1 C15 132.3(4) . . ?
N2 Ir1 C15 94.4(5) . . ?
N3 Ir1 C15 144.8(5) 7_466 . ?
N1 Ir1 C16 103.1(4) . . ?
N2 Ir1 C16 122.4(4) . . ?
N3 Ir1 C16 152.6(5) 7_466 . ?
C15 Ir1 C16 38.58(17) . . ?
N1 Ir1 C19' 157.3(5) . . ?
C18' Ir1 C19' 39.18(17) . . ?
N2 Ir1 C19' 106.0(5) . . ?
N3 Ir1 C19' 116.1(5) 7_466 . ?
C17' Ir1 C19' 64.9(2) . . ?
N1 Ir1 C19 166.4(5) . . ?
N2 Ir1 C19 101.9(5) . . ?
N3 Ir1 C19 107.7(5) 7_466 . ?
C15 Ir1 C19 38.02(17) . . ?
C16 Ir1 C19 63.6(2) . . ?
N1 Ir1 C17 105.6(4) . . ?
N2 Ir1 C17 157.9(4) . . ?
N3 Ir1 C17 114.6(5) 7_466 . ?
C15 Ir1 C17 63.6(2) . . ?
C16 Ir1 C17 37.97(15) . . ?
C19 Ir1 C17 62.7(2) . . ?
N1 Ir1 C18 136.2(4) . . ?
N2 Ir1 C18 136.1(4) . . ?
N3 Ir1 C18 94.0(5) 7_466 . ?
C15 Ir1 C18 63.0(2) . . ?
C16 Ir1 C18 63.0(2) . . ?
C19 Ir1 C18 37.17(16) . . ?
C17 Ir1 C18 37.16(15) . . ?
N1 Ir1 C16' 94.8(4) . . ?
C18' Ir1 C16' 64.2(2) . . ?
N2 Ir1 C16' 129.4(4) . . ?
N3 Ir1 C16' 146.3(5) 7_466 . ?
C17' Ir1 C16' 37.78(15) . . ?
C19' Ir1 C16' 62.6(2) . . ?
C1 N1 C4 106.1(11) . . ?
C1 N1 Ir1 125.9(8) . . ?
C4 N1 Ir1 127.3(9) . . ?
C9 N2 C6 106.0(18) . . ?
C9 N2 Ir1 127.7(17) . . ?
C6 N2 Ir1 125.8(10) . . ?
C14 N3 C10 116.7(14) . . ?
C14 N3 Ir1 122.3(12) . 8_666 ?
C10 N3 Ir1 121.0(11) . 8_666 ?
N1 C1 C2 114.3(11) . . ?
C3 C2 C1 102.6(13) . . ?
C2 C3 C4 108.6(13) . . ?
C5 C4 N1 125.5(13) . . ?
C5 C4 C3 126.2(12) . . ?
N1 C4 C3 108.3(11) . . ?
C4 C5 C6 126.4(13) . . ?
C4 C5 C12 115.5(12) . . ?
C6 C5 C12 118.0(13) . . ?
C5 C6 N2 124.9(13) . . ?
C5 C6 C7 127.8(18) . . ?
N2 C6 C7 107.1(16) . . ?
C8 C7 C6 105(2) . . ?
C9 C8 C7 108(2) . . ?
N2 C9 C8 113(2) . . ?
N3 C10 C11 120.6(16) . . ?
C12 C11 C10 121.6(14) . . ?
C13 C12 C11 115.9(13) . . ?
C13 C12 C5 122.8(14) . . ?
C11 C12 C5 121.2(12) . . ?
C12 C13 C14 119.8(16) . . ?
N3 C14 C13 125.2(17) . . ?
C16 C15 C19 108.0 . . ?
C16 C15 C20 126.0 . . ?
C19 C15 C20 126.0 . . ?
C16 C15 Ir1 70.8(3) . . ?
C19 C15 Ir1 73.3(3) . . ?
C20 C15 Ir1 121.7(3) . . ?
C15 C16 C17 108.0 . . ?
C15 C16 C21 126.0 . . ?
C17 C16 C21 126.0 . . ?
C15 C16 Ir1 70.6(3) . . ?
C17 C16 Ir1 73.3(3) . . ?
C21 C16 Ir1 121.7(3) . . ?
C16 C17 C18 108.0 . . ?
C16 C17 C22 126.0 . . ?
C18 C17 C22 126.0 . . ?
C16 C17 Ir1 68.7(3) . . ?
C18 C17 Ir1 72.8(3) . . ?
C22 C17 Ir1 124.1(3) . . ?
C19 C18 C17 108.0 . . ?
C19 C18 C23 126.0 . . ?
C17 C18 C23 126.0 . . ?
C19 C18 Ir1 70.0(3) . . ?
C17 C18 Ir1 70.1(3) . . ?
C23 C18 Ir1 125.5(3) . . ?
C18 C19 C15 108.0 . . ?
C18 C19 C24 126.0 . . ?
C15 C19 C24 126.0 . . ?
C18 C19 Ir1 72.9(3) . . ?
C15 C19 Ir1 68.7(3) . . ?
C24 C19 Ir1 124.0(3) . . ?
C16' C15' C19' 108.0 . . ?
C16' C15' C20' 126.0 . . ?
C19' C15' C20' 126.0 . . ?
C16' C15' Ir1 70.6(3) . . ?
C19' C15' Ir1 66.9(3) . . ?
C20' C15' Ir1 128.0(3) . . ?
C15' C16' C17' 108.0 . . ?
C15' C16' C21' 126.0 . . ?
C17' C16' C21' 126.0 . . ?
C15' C16' Ir1 73.0(3) . . ?
C17' C16' Ir1 65.7(3) . . ?
C21' C16' Ir1 126.8(3) . . ?
C16' C17' C18' 108.0 . . ?
C16' C17' C22' 126.0 . . ?
C18' C17' C22' 126.0 . . ?
C16' C17' Ir1 76.5(3) . . ?
C18' C17' Ir1 67.9(3) . . ?
C22' C17' Ir1 121.2(3) . . ?
C19' C18' C17' 108.0 . . ?
C19' C18' C23' 126.0 . . ?
C17' C18' C23' 126.0 . . ?
C19' C18' Ir1 74.6(3) . . ?
C17' C18' Ir1 72.3(3) . . ?
C23' C18' Ir1 119.0(3) . . ?
C18' C19' C15' 108.0 . . ?
C18' C19' C24' 126.0 . . ?
C15' C19' C24' 126.0 . . ?
C18' C19' Ir1 66.2(3) . . ?
C15' C19' Ir1 76.0(3) . . ?
C24' C19' Ir1 123.3(3) . . ?
C25 S1 F3 73(2) 2_565 2_565 ?
C25 S1 O3 96(2) 2_565 . ?
F3 S1 O3 139(3) 2_565 . ?
C25 S1 F2 67.4(15) 2_565 2_565 ?
F3 S1 F2 118(3) 2_565 2_565 ?
O3 S1 F2 90.4(19) . 2_565 ?
C25 S1 O2 129(2) 2_565 . ?
F3 S1 O2 58(2) 2_565 . ?
O3 S1 O2 112.2(19) . . ?
F2 S1 O2 148(2) 2_565 . ?
C25 S1 O1 106.4(19) 2_565 . ?
F3 S1 O1 111(3) 2_565 . ?
O3 S1 O1 109.4(18) . . ?
F2 S1 O1 45.6(14) 2_565 . ?
O2 S1 O1 103.7(19) . . ?
C25 S1 C25 23.3(19) 2_565 . ?
F3 S1 C25 50(2) 2_565 . ?
O3 S1 C25 114.6(19) . . ?
F2 S1 C25 82.0(16) 2_565 . ?
O2 S1 C25 106.7(18) . . ?
O1 S1 C25 109.7(16) . . ?
C25 S1 F1 48.0(15) 2_565 2_565 ?
F3 S1 F1 93(2) 2_565 2_565 ?
O3 S1 F1 54.8(15) . 2_565 ?
F2 S1 F1 93.4(18) 2_565 2_565 ?
O2 S1 F1 118(2) . 2_565 ?
O1 S1 F1 138.4(19) . 2_565 ?
C25 S1 F1 61.0(13) . 2_565 ?
F2 O1 S1 62.9(17) 2_565 . ?
F3 O2 S1 48.8(18) 2_565 . ?
S1 O3 F1 74.2(18) . 2_565 ?
S1 O3 C25 35.4(12) . 2_565 ?
F1 O3 C25 43.9(11) 2_565 2_565 ?
C25 C25 S1 126(4) 2_565 2_565 ?
C25 C25 F1 108.7(16) 2_565 . ?
S1 C25 F1 94(2) 2_565 . ?
C25 C25 F3 74(3) 2_565 2_565 ?
S1 C25 F3 150(3) 2_565 2_565 ?
F1 C25 F3 101(3) . 2_565 ?
C25 C25 F3 70(4) 2_565 . ?
S1 C25 F3 57(3) 2_565 . ?
F1 C25 F3 109(3) . . ?
F3 C25 F3 138(3) 2_565 . ?
C25 C25 F2 131.6(15) 2_565 . ?
S1 C25 F2 67.7(17) 2_565 . ?
F1 C25 F2 117(2) . . ?
F3 C25 F2 82(3) 2_565 . ?
F3 C25 F2 108(2) . . ?
C25 C25 S1 31(2) 2_565 . ?
S1 C25 S1 149(2) 2_565 . ?
F1 C25 S1 112(2) . . ?
F3 C25 S1 43.0(19) 2_565 . ?
F3 C25 S1 97(3) . . ?
F2 C25 S1 111.5(16) . . ?
C25 C25 F1 44.5(11) 2_565 2_565 ?
S1 C25 F1 122(2) 2_565 2_565 ?
F1 C25 F1 65(2) . 2_565 ?
F3 C25 F1 88(2) 2_565 2_565 ?
F3 C25 F1 80(2) . 2_565 ?
F2 C25 F1 170(2) . 2_565 ?
S1 C25 F1 60.3(13) . 2_565 ?
C25 C25 O3 153(2) 2_565 2_565 ?
S1 C25 O3 48.9(14) 2_565 2_565 ?
F1 C25 O3 52.3(16) . 2_565 ?
F3 C25 O3 125(3) 2_565 2_565 ?
F3 C25 O3 97(3) . 2_565 ?
F2 C25 O3 74.1(15) . 2_565 ?
S1 C25 O3 161.9(19) . 2_565 ?
F1 C25 O3 111.7(17) 2_565 2_565 ?
C25 F1 O3 84(2) . 2_565 ?
C25 F1 F1 71.1(16) . 2_565 ?
O3 F1 F1 143(3) 2_565 2_565 ?
C25 F1 S1 38.3(13) . 2_565 ?
O3 F1 S1 51.1(13) 2_565 2_565 ?
F1 F1 S1 94.4(18) 2_565 2_565 ?
C25 F1 C25 26.9(12) . 2_565 ?
O3 F1 C25 108.7(18) 2_565 2_565 ?
F1 F1 C25 44.4(11) 2_565 2_565 ?
S1 F1 C25 58.7(11) 2_565 2_565 ?
O1 F2 C25 110(3) 2_565 . ?
O1 F2 S1 71.5(19) 2_565 2_565 ?
C25 F2 S1 44.9(13) . 2_565 ?
O1 F2 F3 142(3) 2_565 2_565 ?
C25 F2 F3 46.4(17) . 2_565 ?
S1 F2 F3 91.3(18) 2_565 2_565 ?
S1 F3 C25 87(3) 2_565 2_565 ?
S1 F3 O2 73(3) 2_565 2_565 ?
C25 F3 O2 158(4) 2_565 2_565 ?
S1 F3 C25 50.6(17) 2_565 . ?
C25 F3 C25 36.9(19) 2_565 . ?
O2 F3 C25 123(4) 2_565 . ?
S1 F3 F2 121(3) 2_565 2_565 ?
C25 F3 F2 52(2) 2_565 2_565 ?
O2 F3 F2 149(3) 2_565 2_565 ?
C25 F3 F2 81(3) . 2_565 ?
O4 S2 O6 107(3) . . ?
O4 S2 O5 118(3) . . ?
O6 S2 O5 113(3) . . ?
O4 S2 C26 95(3) . . ?
O6 S2 C26 119(3) . . ?
O5 S2 C26 103(3) . . ?
F6 C26 F4 93(3) . . ?
F6 C26 F5 99(3) . . ?
F4 C26 F5 103(3) . . ?
F6 C26 S2 95(4) . . ?
F4 C26 S2 136(4) . . ?
F5 C26 S2 118(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
C4 N1 C1 C2 0.5(15) . . . . ?
Ir1 N1 C1 C2 -170.8(9) . . . . ?
N1 C1 C2 C3 0.3(16) . . . . ?
C1 C2 C3 C4 -1.0(15) . . . . ?
C1 N1 C4 C5 177.6(12) . . . . ?
Ir1 N1 C4 C5 -11.3(16) . . . . ?
C1 N1 C4 C3 -1.1(13) . . . . ?
Ir1 N1 C4 C3 170.1(8) . . . . ?
C2 C3 C4 C5 -177.3(12) . . . . ?
C2 C3 C4 N1 1.4(14) . . . . ?
N1 C4 C5 C6 -4(2) . . . . ?
C3 C4 C5 C6 174.7(13) . . . . ?
N1 C4 C5 C12 178.4(11) . . . . ?
C3 C4 C5 C12 -3.1(18) . . . . ?
C4 C5 C6 N2 5(2) . . . . ?
C12 C5 C6 N2 -176.8(12) . . . . ?
C4 C5 C6 C7 178.9(14) . . . . ?
C12 C5 C6 C7 -3(2) . . . . ?
C9 N2 C6 C5 180.0(13) . . . . ?
Ir1 N2 C6 C5 7.7(18) . . . . ?
C9 N2 C6 C7 5.4(16) . . . . ?
Ir1 N2 C6 C7 -166.9(10) . . . . ?
C5 C6 C7 C8 -178.7(16) . . . . ?
N2 C6 C7 C8 -4.2(19) . . . . ?
C6 C7 C8 C9 2(2) . . . . ?
C6 N2 C9 C8 -5(2) . . . . ?
Ir1 N2 C9 C8 167.5(14) . . . . ?
C7 C8 C9 N2 2(3) . . . . ?
C14 N3 C10 C11 5(3) . . . . ?
Ir1 N3 C10 C11 -173.5(12) 8_666 . . . ?
N3 C10 C11 C12 -3(3) . . . . ?
C10 C11 C12 C13 -1(3) . . . . ?
C10 C11 C12 C5 178.0(14) . . . . ?
C4 C5 C12 C13 -74(2) . . . . ?
C6 C5 C12 C13 108.0(19) . . . . ?
C4 C5 C12 C11 107.0(16) . . . . ?
C6 C5 C12 C11 -71.1(18) . . . . ?
C11 C12 C13 C14 3(3) . . . . ?
C5 C12 C13 C14 -176.1(18) . . . . ?
C10 N3 C14 C13 -3(3) . . . . ?
Ir1 N3 C14 C13 175.2(18) 8_666 . . . ?
C12 C13 C14 N3 -1(4) . . . . ?
C19 C15 C16 C17 0.0 . . . . ?
C20 C15 C16 C17 180.0 . . . . ?
Ir1 C15 C16 C17 64.3(3) . . . . ?
C19 C15 C16 C21 180.0 . . . . ?
C20 C15 C16 C21 0.0 . . . . ?
Ir1 C15 C16 C21 -115.7(3) . . . . ?
C19 C15 C16 Ir1 -64.3(3) . . . . ?
C20 C15 C16 Ir1 115.7(3) . . . . ?
C15 C16 C17 C18 0.0 . . . . ?
C21 C16 C17 C18 180.0 . . . . ?
Ir1 C16 C17 C18 62.5(3) . . . . ?
C15 C16 C17 C22 180.0 . . . . ?
C21 C16 C17 C22 0.0 . . . . ?
Ir1 C16 C17 C22 -117.5(3) . . . . ?
C15 C16 C17 Ir1 -62.5(3) . . . . ?
C21 C16 C17 Ir1 117.5(3) . . . . ?
C16 C17 C18 C19 0.0 . . . . ?
C22 C17 C18 C19 -180.0 . . . . ?
Ir1 C17 C18 C19 60.0(3) . . . . ?
C16 C17 C18 C23 180.0 . . . . ?
C22 C17 C18 C23 0.0 . . . . ?
Ir1 C17 C18 C23 -120.1(3) . . . . ?
C16 C17 C18 Ir1 -59.9(3) . . . . ?
C22 C17 C18 Ir1 120.1(3) . . . . ?
C17 C18 C19 C15 0.0 . . . . ?
C23 C18 C19 C15 180.0 . . . . ?
Ir1 C18 C19 C15 60.0(3) . . . . ?
C17 C18 C19 C24 -180.0 . . . . ?
C23 C18 C19 C24 0.0 . . . . ?
Ir1 C18 C19 C24 -120.0(3) . . . . ?
C17 C18 C19 Ir1 -60.0(3) . . . . ?
C23 C18 C19 Ir1 120.0(3) . . . . ?
C16 C15 C19 C18 0.0 . . . . ?
C20 C15 C19 C18 -180.0 . . . . ?
Ir1 C15 C19 C18 -62.7(3) . . . . ?
C16 C15 C19 C24 180.0 . . . . ?
C20 C15 C19 C24 0.0 . . . . ?
Ir1 C15 C19 C24 117.3(3) . . . . ?
C16 C15 C19 Ir1 62.7(3) . . . . ?
C20 C15 C19 Ir1 -117.3(3) . . . . ?
C19' C15' C16' C17' 0.0 . . . . ?
C20' C15' C16' C17' 180.0 . . . . ?
Ir1 C15' C16' C17' 56.5(3) . . . . ?
C19' C15' C16' C21' 180.0 . . . . ?
C20' C15' C16' C21' 0.0 . . . . ?
Ir1 C15' C16' C21' -123.5(3) . . . . ?
C19' C15' C16' Ir1 -56.5(3) . . . . ?
C20' C15' C16' Ir1 123.4(3) . . . . ?
C15' C16' C17' C18' 0.0 . . . . ?
C21' C16' C17' C18' -180.0 . . . . ?
Ir1 C16' C17' C18' 61.0(3) . . . . ?
C15' C16' C17' C22' 180.0 . . . . ?
C21' C16' C17' C22' 0.0 . . . . ?
Ir1 C16' C17' C22' -119.0(3) . . . . ?
C15' C16' C17' Ir1 -61.0(3) . . . . ?
C21' C16' C17' Ir1 119.0(3) . . . . ?
C16' C17' C18' C19' 0.0 . . . . ?
C22' C17' C18' C19' -180.0 . . . . ?
Ir1 C17' C18' C19' 66.6(3) . . . . ?
C16' C17' C18' C23' 180.0 . . . . ?
C22' C17' C18' C23' 0.0 . . . . ?
Ir1 C17' C18' C23' -113.4(3) . . . . ?
C16' C17' C18' Ir1 -66.6(3) . . . . ?
C22' C17' C18' Ir1 113.4(3) . . . . ?
C17' C18' C19' C15' 0.0 . . . . ?
C23' C18' C19' C15' -180.0 . . . . ?
Ir1 C18' C19' C15' 65.1(3) . . . . ?
C17' C18' C19' C24' -180.0 . . . . ?
C23' C18' C19' C24' 0.0 . . . . ?
Ir1 C18' C19' C24' -114.9(3) . . . . ?
C17' C18' C19' Ir1 -65.1(3) . . . . ?
C23' C18' C19' Ir1 114.9(3) . . . . ?
C16' C15' C19' C18' 0.0 . . . . ?
C20' C15' C19' C18' -180.0 . . . . ?
Ir1 C15' C19' C18' -58.8(3) . . . . ?
C16' C15' C19' C24' 180.0 . . . . ?
C20' C15' C19' C24' 0.0 . . . . ?
Ir1 C15' C19' C24' 121.2(3) . . . . ?
C16' C15' C19' Ir1 58.8(3) . . . . ?
C20' C15' C19' Ir1 -121.2(3) . . . . ?
C25 S1 O1 F2 -32(2) 2_565 . . 2_565 ?
F3 S1 O1 F2 -109(3) 2_565 . . 2_565 ?
O3 S1 O1 F2 70(3) . . . 2_565 ?
O2 S1 O1 F2 -170(2) . . . 2_565 ?
C25 S1 O1 F2 -56(2) . . . 2_565 ?
F1 S1 O1 F2 12(3) 2_565 . . 2_565 ?
C25 S1 O2 F3 -17(3) 2_565 . . 2_565 ?
O3 S1 O2 F3 -135(4) . . . 2_565 ?
F2 S1 O2 F3 93(5) 2_565 . . 2_565 ?
O1 S1 O2 F3 107(3) . . . 2_565 ?
C25 S1 O2 F3 -9(3) . . . 2_565 ?
F1 S1 O2 F3 -74(3) 2_565 . . 2_565 ?
C25 S1 O3 F1 -27(2) 2_565 . . 2_565 ?
F3 S1 O3 F1 44(5) 2_565 . . 2_565 ?
F2 S1 O3 F1 -94(2) 2_565 . . 2_565 ?
O2 S1 O3 F1 109(2) . . . 2_565 ?
O1 S1 O3 F1 -136(2) . . . 2_565 ?
C25 S1 O3 F1 -12(2) . . . 2_565 ?
F3 S1 O3 C25 70(4) 2_565 . . 2_565 ?
F2 S1 O3 C25 -67.3(16) 2_565 . . 2_565 ?
O2 S1 O3 C25 136(3) . . . 2_565 ?
O1 S1 O3 C25 -110(2) . . . 2_565 ?
C25 S1 O3 C25 14.1(15) . . . 2_565 ?
F1 S1 O3 C25 27(2) 2_565 . . 2_565 ?
F3 S1 C25 C25 -173(4) 2_565 . . 2_565 ?
O3 S1 C25 C25 -38(2) . . . 2_565 ?
F2 S1 C25 C25 49(2) 2_565 . . 2_565 ?
O2 S1 C25 C25 -163(3) . . . 2_565 ?
O1 S1 C25 C25 86(2) . . . 2_565 ?
F1 S1 C25 C25 -50(2) 2_565 . . 2_565 ?
C25 S1 C25 S1 -55(5) 2_565 . . 2_565 ?
F3 S1 C25 S1 132(4) 2_565 . . 2_565 ?
O3 S1 C25 S1 -93(4) . . . 2_565 ?
F2 S1 C25 S1 -6(4) 2_565 . . 2_565 ?
O2 S1 C25 S1 142(3) . . . 2_565 ?
O1 S1 C25 S1 31(4) . . . 2_565 ?
F1 S1 C25 S1 -105(4) 2_565 . . 2_565 ?
C25 S1 C25 F1 90(2) 2_565 . . . ?
F3 S1 C25 F1 -83(4) 2_565 . . . ?
O3 S1 C25 F1 52(3) . . . . ?
F2 S1 C25 F1 138(3) 2_565 . . . ?
O2 S1 C25 F1 -73(3) . . . . ?
O1 S1 C25 F1 175(2) . . . . ?
F1 S1 C25 F1 40(3) 2_565 . . . ?
C25 S1 C25 F3 173(4) 2_565 . . 2_565 ?
O3 S1 C25 F3 135(4) . . . 2_565 ?
F2 S1 C25 F3 -139(4) 2_565 . . 2_565 ?
O2 S1 C25 F3 10(3) . . . 2_565 ?
O1 S1 C25 F3 -102(3) . . . 2_565 ?
F1 S1 C25 F3 123(3) 2_565 . . 2_565 ?
C25 S1 C25 F3 -25(3) 2_565 . . . ?
F3 S1 C25 F3 163(5) 2_565 . . . ?
O3 S1 C25 F3 -62(3) . . . . ?
F2 S1 C25 F3 24(2) 2_565 . . . ?
O2 S1 C25 F3 173(2) . . . . ?
O1 S1 C25 F3 61(2) . . . . ?
F1 S1 C25 F3 -74(2) 2_565 . . . ?
C25 S1 C25 F2 -137(3) 2_565 . . . ?
F3 S1 C25 F2 50(4) 2_565 . . . ?
O3 S1 C25 F2 -175(2) . . . . ?
F2 S1 C25 F2 -88(3) 2_565 . . . ?
O2 S1 C25 F2 60(2) . . . . ?
O1 S1 C25 F2 -52(3) . . . . ?
F1 S1 C25 F2 173(3) 2_565 . . . ?
C25 S1 C25 F1 50(2) 2_565 . . 2_565 ?
F3 S1 C25 F1 -123(3) 2_565 . . 2_565 ?
O3 S1 C25 F1 12(2) . . . 2_565 ?
F2 S1 C25 F1 98(2) 2_565 . . 2_565 ?
O2 S1 C25 F1 -113(2) . . . 2_565 ?
O1 S1 C25 F1 135(2) . . . 2_565 ?
C25 S1 C25 O3 118(4) 2_565 . . 2_565 ?
F3 S1 C25 O3 -55(6) 2_565 . . 2_565 ?
O3 S1 C25 O3 80(6) . . . 2_565 ?
F2 S1 C25 O3 167(5) 2_565 . . 2_565 ?
O2 S1 C25 O3 -45(5) . . . 2_565 ?
O1 S1 C25 O3 -157(5) . . . 2_565 ?
F1 S1 C25 O3 68(5) 2_565 . . 2_565 ?
C25 C25 F1 O3 -158(4) 2_565 . . 2_565 ?
S1 C25 F1 O3 -28(2) 2_565 . . 2_565 ?
F3 C25 F1 O3 126(3) 2_565 . . 2_565 ?
F3 C25 F1 O3 -84(3) . . . 2_565 ?
F2 C25 F1 O3 39(3) . . . 2_565 ?
S1 C25 F1 O3 169.3(18) . . . 2_565 ?
F1 C25 F1 O3 -152(4) 2_565 . . 2_565 ?
C25 C25 F1 F1 -6(4) 2_565 . . 2_565 ?
S1 C25 F1 F1 124(3) 2_565 . . 2_565 ?
F3 C25 F1 F1 -82(3) 2_565 . . 2_565 ?
F3 C25 F1 F1 68(3) . . . 2_565 ?
F2 C25 F1 F1 -169(3) . . . 2_565 ?
S1 C25 F1 F1 -38(3) . . . 2_565 ?
O3 C25 F1 F1 152(4) 2_565 . . 2_565 ?
C25 C25 F1 S1 -130(5) 2_565 . . 2_565 ?
F3 C25 F1 S1 154(3) 2_565 . . 2_565 ?
F3 C25 F1 S1 -56(3) . . . 2_565 ?
F2 C25 F1 S1 67(2) . . . 2_565 ?
S1 C25 F1 S1 -163(2) . . . 2_565 ?
F1 C25 F1 S1 -124(3) 2_565 . . 2_565 ?
O3 C25 F1 S1 28(2) 2_565 . . 2_565 ?
S1 C25 F1 C25 130(5) 2_565 . . 2_565 ?
F3 C25 F1 C25 -76(4) 2_565 . . 2_565 ?
F3 C25 F1 C25 74(4) . . . 2_565 ?
F2 C25 F1 C25 -163(5) . . . 2_565 ?
S1 C25 F1 C25 -33(3) . . . 2_565 ?
F1 C25 F1 C25 6(4) 2_565 . . 2_565 ?
O3 C25 F1 C25 158(4) 2_565 . . 2_565 ?
C25 C25 F2 O1 85(5) 2_565 . . 2_565 ?
S1 C25 F2 O1 -34(2) 2_565 . . 2_565 ?
F1 C25 F2 O1 -116(3) . . . 2_565 ?
F3 C25 F2 O1 145(3) 2_565 . . 2_565 ?
F3 C25 F2 O1 7(4) . . . 2_565 ?
S1 C25 F2 O1 113(3) . . . 2_565 ?
F1 C25 F2 O1 149(10) 2_565 . . 2_565 ?
O3 C25 F2 O1 -85(2) 2_565 . . 2_565 ?
C25 C25 F2 S1 119(6) 2_565 . . 2_565 ?
F1 C25 F2 S1 -83(3) . . . 2_565 ?
F3 C25 F2 S1 179(3) 2_565 . . 2_565 ?
F3 C25 F2 S1 41(3) . . . 2_565 ?
S1 C25 F2 S1 147(3) . . . 2_565 ?
F1 C25 F2 S1 -178(12) 2_565 . . 2_565 ?
O3 C25 F2 S1 -51.6(15) 2_565 . . 2_565 ?
C25 C25 F2 F3 -60(5) 2_565 . . 2_565 ?
S1 C25 F2 F3 -179(3) 2_565 . . 2_565 ?
F1 C25 F2 F3 99(3) . . . 2_565 ?
F3 C25 F2 F3 -138(3) . . . 2_565 ?
S1 C25 F2 F3 -32(2) . . . 2_565 ?
F1 C25 F2 F3 4(11) 2_565 . . 2_565 ?
O3 C25 F2 F3 130(3) 2_565 . . 2_565 ?
C25 C25 F3 S1 -175(3) 2_565 . . 2_565 ?
F1 C25 F3 S1 82(3) . . . 2_565 ?
F3 C25 F3 S1 -144(4) 2_565 . . 2_565 ?
F2 C25 F3 S1 -46(3) . . . 2_565 ?
S1 C25 F3 S1 -162(3) . . . 2_565 ?
F1 C25 F3 S1 140(2) 2_565 . . 2_565 ?
O3 C25 F3 S1 29(2) 2_565 . . 2_565 ?
S1 C25 F3 C25 175(3) 2_565 . . 2_565 ?
F1 C25 F3 C25 -103(2) . . . 2_565 ?
F3 C25 F3 C25 30(5) 2_565 . . 2_565 ?
F2 C25 F3 C25 128.6(17) . . . 2_565 ?
S1 C25 F3 C25 13.1(16) . . . 2_565 ?
F1 C25 F3 C25 -45.0(14) 2_565 . . 2_565 ?
O3 C25 F3 C25 -155.8(12) 2_565 . . 2_565 ?
C25 C25 F3 O2 169(5) 2_565 . . 2_565 ?
S1 C25 F3 O2 -16(3) 2_565 . . 2_565 ?
F1 C25 F3 O2 65(5) . . . 2_565 ?
F3 C25 F3 O2 -161(2) 2_565 . . 2_565 ?
F2 C25 F3 O2 -62(5) . . . 2_565 ?
S1 C25 F3 O2 -178(4) . . . 2_565 ?
F1 C25 F3 O2 124(4) 2_565 . . 2_565 ?
O3 C25 F3 O2 13(4) 2_565 . . 2_565 ?
C25 C25 F3 F2 -32.2(13) 2_565 . . 2_565 ?
S1 C25 F3 F2 143(3) 2_565 . . 2_565 ?
F1 C25 F3 F2 -136(2) . . . 2_565 ?
F3 C25 F3 F2 -2(6) 2_565 . . 2_565 ?
F2 C25 F3 F2 96(3) . . . 2_565 ?
S1 C25 F3 F2 -19.1(18) . . . 2_565 ?
F1 C25 F3 F2 -77.1(18) 2_565 . . 2_565 ?
O3 C25 F3 F2 172.0(17) 2_565 . . 2_565 ?
O4 S2 C26 F6 171(4) . . . . ?
O6 S2 C26 F6 58(4) . . . . ?
O5 S2 C26 F6 -69(4) . . . . ?
O4 S2 C26 F4 -89(6) . . . . ?
O6 S2 C26 F4 157(5) . . . . ?
O5 S2 C26 F4 31(6) . . . . ?
O4 S2 C26 F5 68(5) . . . . ?
O6 S2 C26 F5 -45(5) . . . . ?
O5 S2 C26 F5 -172(4) . . . . ?

_refine_diff_density_max         4.566
_refine_diff_density_min         -3.124
_refine_diff_density_rms         0.208

_shelxl_version_number           2013-2

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3b
_database_code_depnum_ccdc_archive 'CCDC 1440255'
_audit_update_record             
;
2016-01-07 deposited with the CCDC.
2016-01-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C84 H88 F12 N8 O16 Rh4 S4'
_chemical_formula_weight         2233.50

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'
F F 0.0171 0.0103 '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'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_H-M_alt        'P 42/n'
_space_group_name_Hall           '-P 4bc'

_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'
'-y, x+1/2, z+1/2'
'y+1/2, -x, z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y, -x-1/2, -z-1/2'
'-y-1/2, x, -z-1/2'

_cell_length_a                   19.927(3)
_cell_length_b                   19.927(3)
_cell_length_c                   12.252(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4865.1(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    1925
_cell_measurement_theta_min      2.63
_cell_measurement_theta_max      22.44

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_F_000             2256
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    0.839
_shelx_estimated_absorpt_T_min   0.906
_shelx_estimated_absorpt_T_max   0.951
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.656
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_process_details   sadabs

_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            21157
_diffrn_reflns_av_unetI/netI     0.1168
_diffrn_reflns_av_R_equivalents  0.0941
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.951
_diffrn_reflns_theta_max         27.391
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measured_fraction_theta_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             5432
_reflns_number_gt                2401
_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-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0914P)²] 
 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         5432
_refine_ls_number_parameters     294
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1560
_refine_ls_R_factor_gt           0.0647
_refine_ls_wR_factor_ref         0.1845
_refine_ls_wR_factor_gt          0.1512
_refine_ls_goodness_of_fit_ref   0.903
_refine_ls_restrained_S_all      0.902
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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
1 0.250 0.250 -0.066 359.9 9.0
2 0.750 0.750 0.018 360.0 8.4
_platon_squeeze_details          
; 
;

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
Rh1 Rh 0.96346(3) 0.34892(3) 0.12293(4) 0.0428(2) Uani 1 1 d . . . . .
N1 N 1.0380(3) 0.3379(3) 0.0090(4) 0.0538(16) Uani 1 1 d . . . . .
N2 N 1.2635(3) 0.4923(3) 0.3008(4) 0.0443(14) Uani 1 1 d . . . . .
O1 O 1.0452(2) 0.4002(2) 0.1967(4) 0.0475(12) Uani 1 1 d . . . . .
O2 O 1.0079(4) 0.2557(4) 0.6173(6) 0.109(2) Uani 1 1 d . . . . .
O3 O 0.9103(4) 0.2846(3) 0.7136(5) 0.101(2) Uani 1 1 d . . . . .
O4 O 0.9098(3) 0.2795(3) 0.5143(5) 0.091(2) Uani 1 1 d . . . . .
S1 S 0.94363(12) 0.29113(11) 0.61384(17) 0.0657(6) Uani 1 1 d . . . . .
F1 F 1.0052(3) 0.3903(3) 0.5166(5) 0.111(2) Uani 1 1 d . . . . .
F2 F 0.9147(4) 0.4159(3) 0.6058(6) 0.136(3) Uani 1 1 d . U . . .
F3 F 1.0085(3) 0.3954(3) 0.6908(4) 0.118(2) Uani 1 1 d . . . . .
C1 C 1.0483(5) 0.3072(4) -0.0900(6) 0.068(2) Uani 1 1 d . . . . .
H1 H 1.0135 0.2889 -0.1338 0.081 Uiso 1 1 calc R U . . .
C2 C 1.1168(6) 0.3062(5) -0.1188(8) 0.096(3) Uani 1 1 d . . . . .
H2 H 1.1360 0.2876 -0.1830 0.116 Uiso 1 1 calc R U . . .
C3 C 1.1501(5) 0.3378(5) -0.0343(8) 0.084(3) Uani 1 1 d . . . . .
H3 H 1.1973 0.3440 -0.0294 0.101 Uiso 1 1 calc R U . . .
C4 C 1.1010(4) 0.3603(4) 0.0461(7) 0.058(2) Uani 1 1 d . . . . .
C5 C 1.1002(4) 0.3945(3) 0.1450(5) 0.0443(17) Uani 1 1 d . . . . .
C6 C 1.2119(4) 0.4713(4) 0.3555(6) 0.0522(19) Uani 1 1 d . . . . .
H6 H 1.2113 0.4772 0.4324 0.063 Uiso 1 1 calc R U . . .
C7 C 1.1563(4) 0.4399(4) 0.3043(6) 0.058(2) Uani 1 1 d . . . . .
H7 H 1.1174 0.4288 0.3455 0.069 Uiso 1 1 calc R U . . .
C8 C 1.1589(3) 0.4259(3) 0.1975(5) 0.0385(15) Uani 1 1 d . . . . .
C9 C 1.2151(4) 0.4466(4) 0.1405(6) 0.058(2) Uani 1 1 d . . . . .
H9 H 1.2187 0.4384 0.0644 0.069 Uiso 1 1 calc R U . . .
C10 C 1.2662(4) 0.4793(4) 0.1955(6) 0.0535(19) Uani 1 1 d . . . . .
H10 H 1.3047 0.4930 0.1557 0.064 Uiso 1 1 calc R U . . .
C11 C 0.8963(3) 0.4317(3) 0.1153(6) 0.0471(17) Uani 1 1 d . . . . .
C12 C 0.8863(3) 0.3903(4) 0.0240(6) 0.0480(19) Uani 1 1 d . . . . .
C13 C 0.8666(4) 0.3257(4) 0.0613(7) 0.054(2) Uani 1 1 d . . . . .
C14 C 0.8628(3) 0.3289(4) 0.1780(6) 0.0489(18) Uani 1 1 d . . . . .
C15 C 0.8813(3) 0.3943(4) 0.2105(5) 0.0468(18) Uani 1 1 d . . . . .
C16 C 0.9170(4) 0.5031(4) 0.1170(6) 0.066(2) Uani 1 1 d . . . . .
H16A H 0.9369 0.5150 0.0465 0.099 Uiso 1 1 calc R U . . .
H16B H 0.9502 0.5100 0.1751 0.099 Uiso 1 1 calc R U . . .
H16C H 0.8778 0.5315 0.1307 0.099 Uiso 1 1 calc R U . . .
C17 C 0.8936(4) 0.4120(4) -0.0956(5) 0.062(2) Uani 1 1 d . . . . .
H17A H 0.8497 0.4258 -0.1240 0.093 Uiso 1 1 calc R U . . .
H17B H 0.9107 0.3743 -0.1388 0.093 Uiso 1 1 calc R U . . .
H17C H 0.9250 0.4497 -0.1005 0.093 Uiso 1 1 calc R U . . .
C18 C 0.8476(4) 0.2681(4) -0.0119(8) 0.079(3) Uani 1 1 d . . . . .
H18A H 0.8534 0.2257 0.0276 0.119 Uiso 1 1 calc R U . . .
H18B H 0.8766 0.2682 -0.0766 0.119 Uiso 1 1 calc R U . . .
H18C H 0.8007 0.2728 -0.0344 0.119 Uiso 1 1 calc R U . . .
C19 C 0.8417(4) 0.2735(4) 0.2487(7) 0.073(2) Uani 1 1 d . . . . .
H19A H 0.8683 0.2741 0.3160 0.109 Uiso 1 1 calc R U . . .
H19B H 0.8486 0.2308 0.2108 0.109 Uiso 1 1 calc R U . . .
H19C H 0.7940 0.2787 0.2667 0.109 Uiso 1 1 calc R U . . .
C20 C 0.8817(4) 0.4201(4) 0.3233(6) 0.061(2) Uani 1 1 d . . . . .
H20A H 0.9225 0.4466 0.3353 0.092 Uiso 1 1 calc R U . . .
H20B H 0.8808 0.3824 0.3745 0.092 Uiso 1 1 calc R U . . .
H20C H 0.8422 0.4485 0.3350 0.092 Uiso 1 1 calc R U . . .
C21 C 0.9740(7) 0.3754(6) 0.6074(8) 0.102(4) Uani 1 1 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
Rh1 N1 2.051(6) . ?
Rh1 C12 2.124(6) . ?
Rh1 C13 2.124(7) . ?
Rh1 O1 2.125(4) . ?
Rh1 C11 2.127(6) . ?
Rh1 N2 2.133(5) 8_746 ?
Rh1 C14 2.153(7) . ?
Rh1 C15 2.157(7) . ?
N1 C1 1.374(9) . ?
N1 C4 1.408(9) . ?
N2 C6 1.297(8) . ?
N2 C10 1.317(8) . ?
N2 Rh1 2.133(5) 7_676 ?
O1 C5 1.270(8) . ?
O2 S1 1.463(7) . ?
O3 S1 1.397(6) . ?
O4 S1 1.413(6) . ?
S1 C21 1.786(11) . ?
F1 C21 1.309(11) . ?
F2 C21 1.431(13) . ?
F3 C21 1.295(11) . ?
C1 C2 1.408(12) . ?
C2 C3 1.383(12) . ?
C3 C4 1.459(11) . ?
C4 C5 1.390(10) . ?
C5 C8 1.474(9) . ?
C6 C7 1.420(9) . ?
C7 C8 1.338(9) . ?
C8 C9 1.383(9) . ?
C9 C10 1.384(9) . ?
C11 C12 1.404(9) . ?
C11 C15 1.416(9) . ?
C11 C16 1.481(9) . ?
C12 C13 1.422(10) . ?
C12 C17 1.535(9) . ?
C13 C14 1.433(10) . ?
C13 C18 1.506(10) . ?
C14 C15 1.413(9) . ?
C14 C19 1.465(10) . ?
C15 C20 1.473(9) . ?

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
N1 Rh1 C12 100.2(3) . . ?
N1 Rh1 C13 113.2(3) . . ?
C12 Rh1 C13 39.1(3) . . ?
N1 Rh1 O1 77.6(2) . . ?
C12 Rh1 O1 127.6(2) . . ?
C13 Rh1 O1 162.3(2) . . ?
N1 Rh1 C11 120.6(3) . . ?
C12 Rh1 C11 38.6(3) . . ?
C13 Rh1 C11 65.2(3) . . ?
O1 Rh1 C11 97.4(2) . . ?
N1 Rh1 N2 85.0(2) . 8_746 ?
C12 Rh1 N2 149.2(3) . 8_746 ?
C13 Rh1 N2 111.0(3) . 8_746 ?
O1 Rh1 N2 83.1(2) . 8_746 ?
C11 Rh1 N2 154.0(2) . 8_746 ?
N1 Rh1 C14 150.3(3) . . ?
C12 Rh1 C14 65.0(3) . . ?
C13 Rh1 C14 39.1(3) . . ?
O1 Rh1 C14 132.1(2) . . ?
C11 Rh1 C14 64.6(3) . . ?
N2 Rh1 C14 95.7(2) 8_746 . ?
N1 Rh1 C15 159.0(3) . . ?
C12 Rh1 C15 64.6(3) . . ?
C13 Rh1 C15 65.0(3) . . ?
O1 Rh1 C15 99.7(2) . . ?
C11 Rh1 C15 38.6(3) . . ?
N2 Rh1 C15 115.5(2) 8_746 . ?
C14 Rh1 C15 38.3(2) . . ?
C1 N1 C4 107.1(7) . . ?
C1 N1 Rh1 139.2(6) . . ?
C4 N1 Rh1 113.1(5) . . ?
C6 N2 C10 118.4(6) . . ?
C6 N2 Rh1 122.6(5) . 7_676 ?
C10 N2 Rh1 118.5(5) . 7_676 ?
C5 O1 Rh1 114.0(4) . . ?
O3 S1 O4 120.8(4) . . ?
O3 S1 O2 110.2(5) . . ?
O4 S1 O2 111.4(4) . . ?
O3 S1 C21 106.7(4) . . ?
O4 S1 C21 106.1(4) . . ?
O2 S1 C21 99.1(5) . . ?
N1 C1 C2 111.8(8) . . ?
C3 C2 C1 105.8(8) . . ?
C2 C3 C4 108.9(8) . . ?
C5 C4 N1 115.2(7) . . ?
C5 C4 C3 138.3(8) . . ?
N1 C4 C3 106.4(7) . . ?
O1 C5 C4 119.3(7) . . ?
O1 C5 C8 115.4(6) . . ?
C4 C5 C8 125.4(7) . . ?
N2 C6 C7 122.2(6) . . ?
C8 C7 C6 119.6(7) . . ?
C7 C8 C9 117.6(6) . . ?
C7 C8 C5 118.9(6) . . ?
C9 C8 C5 123.3(6) . . ?
C10 C9 C8 119.4(7) . . ?
N2 C10 C9 122.6(7) . . ?
C12 C11 C15 108.5(6) . . ?
C12 C11 C16 127.9(7) . . ?
C15 C11 C16 123.5(7) . . ?
C12 C11 Rh1 70.6(4) . . ?
C15 C11 Rh1 71.9(4) . . ?
C16 C11 Rh1 124.6(5) . . ?
C11 C12 C13 108.4(6) . . ?
C11 C12 C17 125.7(7) . . ?
C13 C12 C17 125.9(7) . . ?
C11 C12 Rh1 70.8(4) . . ?
C13 C12 Rh1 70.4(4) . . ?
C17 C12 Rh1 125.9(5) . . ?
C12 C13 C14 107.2(7) . . ?
C12 C13 C18 124.7(8) . . ?
C14 C13 C18 127.9(8) . . ?
C12 C13 Rh1 70.5(4) . . ?
C14 C13 Rh1 71.5(4) . . ?
C18 C13 Rh1 127.3(5) . . ?
C15 C14 C13 108.0(7) . . ?
C15 C14 C19 127.1(7) . . ?
C13 C14 C19 124.9(7) . . ?
C15 C14 Rh1 71.0(4) . . ?
C13 C14 Rh1 69.3(4) . . ?
C19 C14 Rh1 126.4(5) . . ?
C14 C15 C11 107.9(6) . . ?
C14 C15 C20 126.0(7) . . ?
C11 C15 C20 126.0(7) . . ?
C14 C15 Rh1 70.7(4) . . ?
C11 C15 Rh1 69.5(4) . . ?
C20 C15 Rh1 127.5(5) . . ?
F3 C21 F1 110.3(10) . . ?
F3 C21 F2 106.0(9) . . ?
F1 C21 F2 104.7(9) . . ?
F3 C21 S1 115.7(7) . . ?
F1 C21 S1 114.4(8) . . ?
F2 C21 S1 104.6(8) . . ?

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
C4 N1 C1 C2 2.1(10) . . . . ?
Rh1 N1 C1 C2 -167.3(6) . . . . ?
N1 C1 C2 C3 -0.3(12) . . . . ?
C1 C2 C3 C4 -1.6(11) . . . . ?
C1 N1 C4 C5 178.4(6) . . . . ?
Rh1 N1 C4 C5 -9.0(8) . . . . ?
C1 N1 C4 C3 -3.0(8) . . . . ?
Rh1 N1 C4 C3 169.5(5) . . . . ?
C2 C3 C4 C5 -179.0(9) . . . . ?
C2 C3 C4 N1 2.9(10) . . . . ?
Rh1 O1 C5 C4 3.7(8) . . . . ?
Rh1 O1 C5 C8 -176.4(4) . . . . ?
N1 C4 C5 O1 3.5(10) . . . . ?
C3 C4 C5 O1 -174.4(9) . . . . ?
N1 C4 C5 C8 -176.5(6) . . . . ?
C3 C4 C5 C8 5.6(14) . . . . ?
C10 N2 C6 C7 -5.2(11) . . . . ?
Rh1 N2 C6 C7 -177.8(5) 7_676 . . . ?
N2 C6 C7 C8 5.8(12) . . . . ?
C6 C7 C8 C9 -3.5(11) . . . . ?
C6 C7 C8 C5 -178.8(6) . . . . ?
O1 C5 C8 C7 19.2(10) . . . . ?
C4 C5 C8 C7 -160.8(7) . . . . ?
O1 C5 C8 C9 -155.8(7) . . . . ?
C4 C5 C8 C9 24.2(11) . . . . ?
C7 C8 C9 C10 1.0(11) . . . . ?
C5 C8 C9 C10 176.1(7) . . . . ?
C6 N2 C10 C9 2.6(11) . . . . ?
Rh1 N2 C10 C9 175.5(6) 7_676 . . . ?
C8 C9 C10 N2 -0.5(12) . . . . ?
C15 C11 C12 C13 -1.5(8) . . . . ?
C16 C11 C12 C13 -179.9(7) . . . . ?
Rh1 C11 C12 C13 60.7(5) . . . . ?
C15 C11 C12 C17 176.8(7) . . . . ?
C16 C11 C12 C17 -1.7(11) . . . . ?
Rh1 C11 C12 C17 -121.0(7) . . . . ?
C15 C11 C12 Rh1 -62.2(5) . . . . ?
C16 C11 C12 Rh1 119.3(7) . . . . ?
C11 C12 C13 C14 1.5(8) . . . . ?
C17 C12 C13 C14 -176.8(7) . . . . ?
Rh1 C12 C13 C14 62.5(5) . . . . ?
C11 C12 C13 C18 176.6(7) . . . . ?
C17 C12 C13 C18 -1.7(12) . . . . ?
Rh1 C12 C13 C18 -122.4(7) . . . . ?
C11 C12 C13 Rh1 -61.0(5) . . . . ?
C17 C12 C13 Rh1 120.7(7) . . . . ?
C12 C13 C14 C15 -1.0(8) . . . . ?
C18 C13 C14 C15 -175.9(7) . . . . ?
Rh1 C13 C14 C15 60.8(5) . . . . ?
C12 C13 C14 C19 177.6(7) . . . . ?
C18 C13 C14 C19 2.7(13) . . . . ?
Rh1 C13 C14 C19 -120.7(7) . . . . ?
C12 C13 C14 Rh1 -61.8(5) . . . . ?
C18 C13 C14 Rh1 123.3(8) . . . . ?
C13 C14 C15 C11 0.1(8) . . . . ?
C19 C14 C15 C11 -178.4(7) . . . . ?
Rh1 C14 C15 C11 59.8(5) . . . . ?
C13 C14 C15 C20 177.4(7) . . . . ?
C19 C14 C15 C20 -1.1(12) . . . . ?
Rh1 C14 C15 C20 -122.8(7) . . . . ?
C13 C14 C15 Rh1 -59.8(5) . . . . ?
C19 C14 C15 Rh1 121.8(8) . . . . ?
C12 C11 C15 C14 0.9(8) . . . . ?
C16 C11 C15 C14 179.4(6) . . . . ?
Rh1 C11 C15 C14 -60.6(5) . . . . ?
C12 C11 C15 C20 -176.5(7) . . . . ?
C16 C11 C15 C20 2.1(11) . . . . ?
Rh1 C11 C15 C20 122.1(7) . . . . ?
C12 C11 C15 Rh1 61.4(5) . . . . ?
C16 C11 C15 Rh1 -120.0(7) . . . . ?
O3 S1 C21 F3 51.8(11) . . . . ?
O4 S1 C21 F3 -178.1(9) . . . . ?
O2 S1 C21 F3 -62.6(10) . . . . ?
O3 S1 C21 F1 -178.3(9) . . . . ?
O4 S1 C21 F1 -48.2(11) . . . . ?
O2 S1 C21 F1 67.3(10) . . . . ?
O3 S1 C21 F2 -64.4(7) . . . . ?
O4 S1 C21 F2 65.7(7) . . . . ?
O2 S1 C21 F2 -178.8(6) . . . . ?

_refine_diff_density_max         0.852
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.116

_shelxl_version_number           2013-2

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_4a
_database_code_depnum_ccdc_archive 'CCDC 1440256'
_audit_update_record             
;
2016-01-25 deposited with the CCDC.
2016-01-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C76 H104 F12 Ir4 N12 O20 S4'
_chemical_formula_weight         2630.75

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'
F F 0.0171 0.0103 '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'

_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_H-M_alt        'P 42/n'
_space_group_name_Hall           '-P 4bc'

_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'
'-y, x+1/2, z+1/2'
'y+1/2, -x, z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y, -x-1/2, -z-1/2'
'-y-1/2, x, -z-1/2'

_cell_length_a                   20.111(2)
_cell_length_b                   20.111(2)
_cell_length_c                   12.1229(19)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4903.4(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    6480
_cell_measurement_theta_min      2.21
_cell_measurement_theta_max      26.73

_exptl_crystal_description       rod
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.782
_exptl_crystal_F_000             2568
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    5.587
_shelx_estimated_absorpt_T_min   0.213
_shelx_estimated_absorpt_T_max   0.768
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.460
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_process_details   sadabs

_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            33333
_diffrn_reflns_av_unetI/netI     0.0668
_diffrn_reflns_av_R_equivalents  0.0821
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.432
_diffrn_reflns_theta_max         27.437
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5548
_reflns_number_gt                2940
_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-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 
 In asymmetric unit of this data, there were disordered
 solvents (half of a diethyl ether and a quarter of a water
 molecule) which could not be restrained properly.
 Therefore, SQUEEZE algorithm was used to omit them.
 The nitrogen atom N2 was partly oxidized so that this site 
 was occupied by NH2 and NO group (75:25). 5 ISOR and 5 DFIX 
 instructions were used to restrain anions and ligands so 
 that there were 35 restraints in the data. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
; 
 w=1/[σ²(Fo²)+(0.0912P)²] 
 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         5548
_refine_ls_number_parameters     276
_refine_ls_number_restraints     35
_refine_ls_R_factor_all          0.0986
_refine_ls_R_factor_gt           0.0531
_refine_ls_wR_factor_ref         0.1589
_refine_ls_wR_factor_gt          0.1420
_refine_ls_goodness_of_fit_ref   0.941
_refine_ls_restrained_S_all      0.946
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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
1 0.250 0.250 0.098 543.8 92.4
2 0.750 0.750 -0.127 543.8 92.5
_platon_squeeze_details          
; 
 In asymmetric unit of this data, there were disordered 
 solvents (half of a diethyl ether and a quarter of a water 
 molecule) which could not be restrained properly. 
 Therefore, SQUEEZE algorithm was used to omit them. 
;

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 0.84842(2) 0.46545(2) 0.12691(3) 0.03916(14) Uani 1 1 d . . . . .
N1 N 0.8689(4) 0.6053(3) 0.0530(6) 0.0481(18) Uani 1 1 d D . . . .
N2 N 0.8412(4) 0.5440(3) 0.0129(6) 0.053(2) Uani 0.75 1 d D . P A 1
H2A H 0.8646 0.5312 -0.0557 0.064 Uiso 0.75 1 calc R U P A 1
H2B H 0.7938 0.5512 -0.0055 0.064 Uiso 0.75 1 calc R U P A 1
N2' N 0.8412(4) 0.5440(3) 0.0129(6) 0.053(2) Uani 0.25 1 d . . P A 2
O5 O 0.8085(11) 0.5475(15) -0.075(2) 0.066(8) Uani 0.25 1 d . U P A 2
N3 N 0.9898(3) 0.7645(3) 0.3000(6) 0.0388(17) Uani 1 1 d . . . . .
O1 O 0.8987(3) 0.5429(3) 0.2055(5) 0.0422(14) Uani 1 1 d . . . . .
O2 O 0.5829(5) 0.2764(4) 0.0154(8) 0.116(3) Uani 1 1 d . U . . .
O3 O 0.5890(6) 0.2819(5) 0.2128(8) 0.136(4) Uani 1 1 d . U . . .
O4 O 0.4839(6) 0.2601(8) 0.1258(11) 0.199(7) Uani 1 1 d D U . . .
S1 S 0.5534(2) 0.28938(18) 0.1164(3) 0.0921(11) Uani 1 1 d D . . . .
F1 F 0.4870(5) 0.3862(5) 0.0222(9) 0.161(4) Uani 1 1 d . . . . .
F2 F 0.4884(5) 0.3883(5) 0.2019(9) 0.151(4) Uani 1 1 d . . . . .
F3 F 0.5836(6) 0.4097(5) 0.1048(10) 0.165(5) Uani 1 1 d D . . . .
C1 C 0.9827(5) 0.7066(4) 0.3541(7) 0.048(2) Uani 1 1 d . . . . .
H1A H 0.9997 0.7026 0.4269 0.058 Uiso 1 1 calc R U . . .
C2 C 0.9514(4) 0.6530(4) 0.3067(8) 0.048(2) Uani 1 1 d . . . . .
H2 H 0.9450 0.6135 0.3482 0.058 Uiso 1 1 calc R U . . .
C3 C 0.9293(4) 0.6565(4) 0.1999(7) 0.0370(18) Uani 1 1 d . . . . .
C4 C 0.9390(4) 0.7141(4) 0.1402(8) 0.047(2) Uani 1 1 d . . . . .
H4 H 0.9262 0.7172 0.0650 0.056 Uiso 1 1 calc R U . . .
C5 C 0.9683(4) 0.7670(4) 0.1945(8) 0.047(2) Uani 1 1 d . . . . .
H5 H 0.9736 0.8076 0.1553 0.057 Uiso 1 1 calc R U . . .
C6 C 0.8958(4) 0.5981(4) 0.1481(7) 0.038(2) Uani 1 1 d . . . . .
C7 C 0.9289(4) 0.3967(4) 0.1209(9) 0.047(2) Uani 1 1 d . . . . .
C8 C 0.8900(4) 0.3869(4) 0.0260(8) 0.046(2) Uani 1 1 d . . . . .
C9 C 0.8236(4) 0.3688(4) 0.0623(9) 0.050(2) Uani 1 1 d . . . . .
C10 C 0.8253(4) 0.3656(4) 0.1808(9) 0.047(2) Uani 1 1 d . . . . .
C11 C 0.8909(5) 0.3837(4) 0.2155(8) 0.047(2) Uani 1 1 d . . . . .
C12 C 1.0019(4) 0.4160(6) 0.1176(9) 0.067(3) Uani 1 1 d . . . . .
H12A H 1.0128 0.4426 0.1830 0.101 Uiso 1 1 calc R U . . .
H12B H 1.0108 0.4422 0.0511 0.101 Uiso 1 1 calc R U . . .
H12C H 1.0294 0.3758 0.1168 0.101 Uiso 1 1 calc R U . . .
C13 C 0.9095(5) 0.3926(6) -0.0937(8) 0.070(3) Uani 1 1 d . . . . .
H13A H 0.9551 0.4095 -0.0990 0.105 Uiso 1 1 calc R U . . .
H13B H 0.8792 0.4233 -0.1313 0.105 Uiso 1 1 calc R U . . .
H13C H 0.9070 0.3487 -0.1286 0.105 Uiso 1 1 calc R U . . .
C14 C 0.7675(5) 0.3491(5) -0.0114(10) 0.070(3) Uani 1 1 d . . . . .
H14A H 0.7728 0.3026 -0.0335 0.105 Uiso 1 1 calc R U . . .
H14B H 0.7675 0.3774 -0.0772 0.105 Uiso 1 1 calc R U . . .
H14C H 0.7253 0.3545 0.0280 0.105 Uiso 1 1 calc R U . . .
C15 C 0.7709(5) 0.3467(5) 0.2567(10) 0.069(3) Uani 1 1 d . . . . .
H15A H 0.7280 0.3581 0.2233 0.103 Uiso 1 1 calc R U . . .
H15B H 0.7759 0.3707 0.3265 0.103 Uiso 1 1 calc R U . . .
H15C H 0.7726 0.2987 0.2706 0.103 Uiso 1 1 calc R U . . .
C16 C 0.9151(6) 0.3854(6) 0.3322(10) 0.079(3) Uani 1 1 d . . . . .
H16A H 0.9380 0.3436 0.3493 0.119 Uiso 1 1 calc R U . . .
H16B H 0.8772 0.3910 0.3821 0.119 Uiso 1 1 calc R U . . .
H16C H 0.9460 0.4226 0.3416 0.119 Uiso 1 1 calc R U . . .
C17 C 0.5265(9) 0.3727(7) 0.1050(15) 0.128(6) Uani 1 1 d 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
Ir1 O1 2.086(5) . ?
Ir1 N2 2.104(8) . ?
Ir1 N3 2.108(7) 7_576 ?
Ir1 C7 2.130(8) . ?
Ir1 C11 2.142(9) . ?
Ir1 C9 2.155(8) . ?
Ir1 C10 2.163(9) . ?
Ir1 C8 2.166(8) . ?
N1 C6 1.282(11) . ?
N1 N2 1.438(7) . ?
N3 C1 1.344(10) . ?
N3 C5 1.351(11) . ?
N3 Ir1 2.108(7) 8_756 ?
O1 C6 1.312(9) . ?
O2 S1 1.385(9) . ?
O3 S1 1.379(9) . ?
O4 S1 1.521(10) . ?
S1 C17 1.766(15) . ?
F1 C17 1.308(18) . ?
F2 C17 1.437(18) . ?
F3 C17 1.370(13) . ?
C1 C2 1.373(11) . ?
C2 C3 1.371(12) . ?
C3 C4 1.379(11) . ?
C3 C6 1.494(11) . ?
C4 C5 1.384(12) . ?
C7 C11 1.403(13) . ?
C7 C8 1.405(12) . ?
C7 C12 1.521(11) . ?
C8 C9 1.452(11) . ?
C8 C13 1.508(13) . ?
C9 C10 1.438(14) . ?
C9 C14 1.493(13) . ?
C10 C11 1.433(12) . ?
C10 C15 1.480(13) . ?
C11 C16 1.497(14) . ?

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 Ir1 N2 76.9(2) . . ?
O1 Ir1 N3 82.9(2) . 7_576 ?
N2 Ir1 N3 84.3(3) . 7_576 ?
O1 Ir1 C7 97.6(3) . . ?
N2 Ir1 C7 121.1(3) . . ?
N3 Ir1 C7 154.2(3) 7_576 . ?
O1 Ir1 C11 98.7(3) . . ?
N2 Ir1 C11 158.9(3) . . ?
N3 Ir1 C11 115.9(3) 7_576 . ?
C7 Ir1 C11 38.3(3) . . ?
O1 Ir1 C9 162.1(3) . . ?
N2 Ir1 C9 115.0(4) . . ?
N3 Ir1 C9 110.7(3) 7_576 . ?
C7 Ir1 C9 65.0(3) . . ?
C11 Ir1 C9 65.3(4) . . ?
O1 Ir1 C10 131.3(3) . . ?
N2 Ir1 C10 151.7(3) . . ?
N3 Ir1 C10 95.6(3) 7_576 . ?
C7 Ir1 C10 64.6(3) . . ?
C11 Ir1 C10 38.9(3) . . ?
C9 Ir1 C10 38.9(4) . . ?
O1 Ir1 C8 128.0(3) . . ?
N2 Ir1 C8 101.7(3) . . ?
N3 Ir1 C8 149.1(3) 7_576 . ?
C7 Ir1 C8 38.2(3) . . ?
C11 Ir1 C8 64.5(3) . . ?
C9 Ir1 C8 39.3(3) . . ?
C10 Ir1 C8 64.9(4) . . ?
C6 N1 N2 111.7(7) . . ?
N1 N2 Ir1 113.3(6) . . ?
C1 N3 C5 117.4(7) . . ?
C1 N3 Ir1 122.3(6) . 8_756 ?
C5 N3 Ir1 120.3(6) . 8_756 ?
C6 O1 Ir1 111.6(5) . . ?
O3 S1 O2 120.4(8) . . ?
O3 S1 O4 111.8(8) . . ?
O2 S1 O4 112.8(8) . . ?
O3 S1 C17 109.2(7) . . ?
O2 S1 C17 103.9(7) . . ?
O4 S1 C17 95.2(8) . . ?
N3 C1 C2 121.6(8) . . ?
C3 C2 C1 120.2(8) . . ?
C2 C3 C4 119.5(8) . . ?
C2 C3 C6 120.2(8) . . ?
C4 C3 C6 120.2(8) . . ?
C3 C4 C5 117.1(9) . . ?
N3 C5 C4 123.9(9) . . ?
N1 C6 O1 126.3(8) . . ?
N1 C6 C3 118.6(8) . . ?
O1 C6 C3 115.0(7) . . ?
C11 C7 C8 109.9(7) . . ?
C11 C7 C12 126.5(9) . . ?
C8 C7 C12 123.6(9) . . ?
C11 C7 Ir1 71.3(5) . . ?
C8 C7 Ir1 72.3(5) . . ?
C12 C7 Ir1 124.7(6) . . ?
C7 C8 C9 107.4(8) . . ?
C7 C8 C13 129.2(8) . . ?
C9 C8 C13 123.5(9) . . ?
C7 C8 Ir1 69.5(5) . . ?
C9 C8 Ir1 69.9(5) . . ?
C13 C8 Ir1 126.1(7) . . ?
C10 C9 C8 107.1(8) . . ?
C10 C9 C14 127.1(9) . . ?
C8 C9 C14 125.4(10) . . ?
C10 C9 Ir1 70.9(5) . . ?
C8 C9 Ir1 70.8(4) . . ?
C14 C9 Ir1 129.1(6) . . ?
C11 C10 C9 107.6(8) . . ?
C11 C10 C15 124.3(10) . . ?
C9 C10 C15 128.0(9) . . ?
C11 C10 Ir1 69.8(5) . . ?
C9 C10 Ir1 70.2(5) . . ?
C15 C10 Ir1 125.9(6) . . ?
C7 C11 C10 108.0(9) . . ?
C7 C11 C16 126.3(9) . . ?
C10 C11 C16 125.7(10) . . ?
C7 C11 Ir1 70.3(5) . . ?
C10 C11 Ir1 71.3(5) . . ?
C16 C11 Ir1 125.9(7) . . ?
F1 C17 F3 113.3(15) . . ?
F1 C17 F2 105.0(14) . . ?
F3 C17 F2 109.3(12) . . ?
F1 C17 S1 116.3(10) . . ?
F3 C17 S1 104.9(12) . . ?
F2 C17 S1 107.9(11) . . ?

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
C6 N1 N2 Ir1 3.8(9) . . . . ?
C5 N3 C1 C2 -3.7(13) . . . . ?
Ir1 N3 C1 C2 177.7(7) 8_756 . . . ?
N3 C1 C2 C3 3.3(14) . . . . ?
C1 C2 C3 C4 0.3(14) . . . . ?
C1 C2 C3 C6 179.5(7) . . . . ?
C2 C3 C4 C5 -3.0(12) . . . . ?
C6 C3 C4 C5 177.8(7) . . . . ?
C1 N3 C5 C4 0.8(13) . . . . ?
Ir1 N3 C5 C4 179.4(7) 8_756 . . . ?
C3 C4 C5 N3 2.6(13) . . . . ?
N2 N1 C6 O1 -0.4(12) . . . . ?
N2 N1 C6 C3 177.7(7) . . . . ?
Ir1 O1 C6 N1 -3.1(10) . . . . ?
Ir1 O1 C6 C3 178.7(5) . . . . ?
C2 C3 C6 N1 172.0(8) . . . . ?
C4 C3 C6 N1 -8.8(11) . . . . ?
C2 C3 C6 O1 -9.7(11) . . . . ?
C4 C3 C6 O1 169.5(7) . . . . ?
C11 C7 C8 C9 1.8(10) . . . . ?
C12 C7 C8 C9 179.7(8) . . . . ?
Ir1 C7 C8 C9 -60.0(6) . . . . ?
C11 C7 C8 C13 -177.8(9) . . . . ?
C12 C7 C8 C13 0.1(15) . . . . ?
Ir1 C7 C8 C13 120.4(10) . . . . ?
C11 C7 C8 Ir1 61.8(6) . . . . ?
C12 C7 C8 Ir1 -120.3(9) . . . . ?
C7 C8 C9 C10 -2.3(9) . . . . ?
C13 C8 C9 C10 177.4(9) . . . . ?
Ir1 C8 C9 C10 -62.0(6) . . . . ?
C7 C8 C9 C14 -175.4(8) . . . . ?
C13 C8 C9 C14 4.2(14) . . . . ?
Ir1 C8 C9 C14 124.9(9) . . . . ?
C7 C8 C9 Ir1 59.7(6) . . . . ?
C13 C8 C9 Ir1 -120.7(9) . . . . ?
C8 C9 C10 C11 1.9(10) . . . . ?
C14 C9 C10 C11 174.9(8) . . . . ?
Ir1 C9 C10 C11 -60.0(6) . . . . ?
C8 C9 C10 C15 -177.5(8) . . . . ?
C14 C9 C10 C15 -4.5(15) . . . . ?
Ir1 C9 C10 C15 120.6(9) . . . . ?
C8 C9 C10 Ir1 61.9(6) . . . . ?
C14 C9 C10 Ir1 -125.1(9) . . . . ?
C8 C7 C11 C10 -0.6(10) . . . . ?
C12 C7 C11 C10 -178.4(8) . . . . ?
Ir1 C7 C11 C10 61.8(6) . . . . ?
C8 C7 C11 C16 177.0(9) . . . . ?
C12 C7 C11 C16 -0.8(15) . . . . ?
Ir1 C7 C11 C16 -120.6(9) . . . . ?
C8 C7 C11 Ir1 -62.4(6) . . . . ?
C12 C7 C11 Ir1 119.8(9) . . . . ?
C9 C10 C11 C7 -0.8(10) . . . . ?
C15 C10 C11 C7 178.6(8) . . . . ?
Ir1 C10 C11 C7 -61.1(6) . . . . ?
C9 C10 C11 C16 -178.4(9) . . . . ?
C15 C10 C11 C16 1.0(14) . . . . ?
Ir1 C10 C11 C16 121.3(9) . . . . ?
C9 C10 C11 Ir1 60.3(6) . . . . ?
C15 C10 C11 Ir1 -120.3(8) . . . . ?
O3 S1 C17 F1 -174.3(13) . . . . ?
O2 S1 C17 F1 56.0(15) . . . . ?
O4 S1 C17 F1 -59.0(14) . . . . ?
O3 S1 C17 F3 59.7(14) . . . . ?
O2 S1 C17 F3 -70.0(13) . . . . ?
O4 S1 C17 F3 175.0(12) . . . . ?
O3 S1 C17 F2 -56.7(13) . . . . ?
O2 S1 C17 F2 173.6(10) . . . . ?
O4 S1 C17 F2 58.5(11) . . . . ?

_refine_diff_density_max         2.639
_refine_diff_density_min         -1.727
_refine_diff_density_rms         0.172

_shelxl_version_number           2013-2

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_4b
_database_code_depnum_ccdc_archive 'CCDC 1440257'
_audit_update_record             
;
2016-01-07 deposited with the CCDC.
2016-01-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C76 H92 F12 N12 O16 Rh4 S4'
_chemical_formula_weight         2197.49

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'
F F 0.0171 0.0103 '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'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_H-M_alt        'P 42/n'
_space_group_name_Hall           '-P 4bc'

_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'
'-y, x+1/2, z+1/2'
'y+1/2, -x, z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y, -x-1/2, -z-1/2'
'-y-1/2, x, -z-1/2'

_cell_length_a                   20.036(3)
_cell_length_b                   20.036(3)
_cell_length_c                   12.234(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4911.4(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    7876
_cell_measurement_theta_min      2.20
_cell_measurement_theta_max      27.46

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_F_000             2224
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    0.830
_shelx_estimated_absorpt_T_min   0.801
_shelx_estimated_absorpt_T_max   0.937
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.559
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_process_details   sadabs

_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            34774
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.950
_diffrn_reflns_theta_max         27.542
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             5642
_reflns_number_gt                3821
_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-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0993P)²+7.3196P] 
 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         5642
_refine_ls_number_parameters     286
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_gt           0.0576
_refine_ls_wR_factor_ref         0.1768
_refine_ls_wR_factor_gt          0.1611
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
1 0.250 0.250 -0.009 414.4 30.7
2 0.750 0.750 -0.055 414.4 29.9
_platon_squeeze_details          
; 
;

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
Rh1 Rh 0.65091(2) 0.46399(2) 0.12789(3) 0.03140(15) Uani 1 1 d . . . . .
N1 N 0.50747(19) 0.76298(19) 0.2997(3) 0.0350(9) Uani 1 1 d . . . . .
N2 N 0.6304(2) 0.6033(2) 0.0566(3) 0.0418(10) Uani 1 1 d . . . . .
N3 N 0.6585(2) 0.5434(2) 0.0171(3) 0.0404(9) Uani 1 1 d . . . . .
O1 O 0.59915(16) 0.54078(15) 0.2070(3) 0.0359(7) Uani 1 1 d . . . . .
O2 O 0.9105(4) 0.2758(3) 0.0173(4) 0.108(2) Uani 1 1 d . . . . .
O3 O 1.0070(4) 0.2536(4) 0.1179(7) 0.133(3) Uani 1 1 d . . . . .
O4 O 0.9112(5) 0.2829(3) 0.2142(5) 0.139(3) Uani 1 1 d . U . . .
S1 S 0.94288(10) 0.28988(9) 0.11533(14) 0.0647(5) Uani 1 1 d . . . . .
F1 F 1.0051(3) 0.3883(2) 0.0159(4) 0.0969(15) Uani 1 1 d . . . . .
F2 F 0.9141(3) 0.4114(3) 0.1022(5) 0.128(2) Uani 1 1 d . . . . .
F3 F 1.0067(3) 0.3940(2) 0.1916(4) 0.0959(15) Uani 1 1 d . . . . .
C1 C 0.5292(3) 0.7653(2) 0.1967(4) 0.0417(11) Uani 1 1 d . . . . .
H1 H 0.5231 0.8057 0.1571 0.050 Uiso 1 1 calc R U . . .
C2 C 0.5601(3) 0.7126(3) 0.1439(4) 0.0424(12) Uani 1 1 d . . . . .
H2 H 0.5747 0.7163 0.0703 0.051 Uiso 1 1 calc R U . . .
C3 C 0.5689(2) 0.6544(2) 0.2024(4) 0.0347(10) Uani 1 1 d . . . . .
C4 C 0.5461(3) 0.6511(2) 0.3073(4) 0.0445(12) Uani 1 1 d . . . . .
H4 H 0.5512 0.6111 0.3481 0.053 Uiso 1 1 calc R U . . .
C5 C 0.5157(3) 0.7059(3) 0.3542(5) 0.0475(13) Uani 1 1 d . . . . .
H5 H 0.5001 0.7028 0.4273 0.057 Uiso 1 1 calc R U . . .
C6 C 0.6027(2) 0.5937(2) 0.1514(4) 0.0355(10) Uani 1 1 d . . . . .
C7 C 0.6863(3) 0.5455(3) -0.0740(6) 0.0632(16) Uani 1 1 d . . . . .
H7 H 0.7032 0.5047 -0.1023 0.076 Uiso 1 1 calc R U . . .
C8 C 0.6955(5) 0.6072(5) -0.1435(7) 0.103(3) Uani 1 1 d . . . . .
H8A H 0.6523 0.6293 -0.1538 0.155 Uiso 1 1 calc R U . . .
H8B H 0.7138 0.5945 -0.2148 0.155 Uiso 1 1 calc R U . . .
H8C H 0.7263 0.6379 -0.1069 0.155 Uiso 1 1 calc R U . . .
C9 C 0.5695(2) 0.3958(2) 0.1159(4) 0.0402(11) Uani 1 1 d . . . . .
C10 C 0.6075(3) 0.3811(2) 0.2136(4) 0.0405(11) Uani 1 1 d . . . . .
C11 C 0.6720(3) 0.3631(2) 0.1801(5) 0.0415(12) Uani 1 1 d . . . . .
C12 C 0.6759(2) 0.3681(2) 0.0636(5) 0.0416(12) Uani 1 1 d . . . . .
C13 C 0.6117(2) 0.3865(2) 0.0237(4) 0.0390(11) Uani 1 1 d . . . . .
C14 C 0.4965(3) 0.4150(3) 0.1140(5) 0.0547(15) Uani 1 1 d . . . . .
H14A H 0.4863 0.4379 0.0452 0.082 Uiso 1 1 calc R U . . .
H14B H 0.4869 0.4449 0.1755 0.082 Uiso 1 1 calc R U . . .
H14C H 0.4689 0.3748 0.1201 0.082 Uiso 1 1 calc R U . . .
C15 C 0.5806(3) 0.3821(3) 0.3275(5) 0.0548(14) Uani 1 1 d . . . . .
H15A H 0.5536 0.3421 0.3400 0.082 Uiso 1 1 calc R U . . .
H15B H 0.5529 0.4219 0.3376 0.082 Uiso 1 1 calc R U . . .
H15C H 0.6178 0.3830 0.3796 0.082 Uiso 1 1 calc R U . . .
C16 C 0.7272(3) 0.3435(3) 0.2540(6) 0.0632(17) Uani 1 1 d . . . . .
H16A H 0.7259 0.3712 0.3200 0.095 Uiso 1 1 calc R U . . .
H16B H 0.7699 0.3499 0.2166 0.095 Uiso 1 1 calc R U . . .
H16C H 0.7222 0.2965 0.2742 0.095 Uiso 1 1 calc R U . . .
C17 C 0.7335(3) 0.3497(3) -0.0088(6) 0.0593(16) Uani 1 1 d . . . . .
H17A H 0.7283 0.3034 -0.0336 0.089 Uiso 1 1 calc R U . . .
H17B H 0.7753 0.3540 0.0322 0.089 Uiso 1 1 calc R U . . .
H17C H 0.7346 0.3795 -0.0723 0.089 Uiso 1 1 calc R U . . .
C18 C 0.5910(3) 0.3925(3) -0.0941(5) 0.0559(15) Uani 1 1 d . . . . .
H18A H 0.5751 0.3492 -0.1204 0.084 Uiso 1 1 calc R U . . .
H18B H 0.6293 0.4068 -0.1381 0.084 Uiso 1 1 calc R U . . .
H18C H 0.5552 0.4256 -0.1005 0.084 Uiso 1 1 calc R U . . .
C19 C 0.9718(5) 0.3718(5) 0.1044(7) 0.090(3) Uani 1 1 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
Rh1 O1 2.092(3) . ?
Rh1 N3 2.096(4) . ?
Rh1 N1 2.126(4) 8_756 ?
Rh1 C9 2.132(5) . ?
Rh1 C12 2.135(5) . ?
Rh1 C10 2.149(5) . ?
Rh1 C13 2.157(5) . ?
Rh1 C11 2.162(5) . ?
N1 C5 1.334(6) . ?
N1 C1 1.335(6) . ?
N1 Rh1 2.126(4) 7_576 ?
N2 C6 1.300(6) . ?
N2 N3 1.410(6) . ?
N3 C7 1.247(7) . ?
O1 C6 1.261(6) . ?
O2 S1 1.393(5) . ?
O3 S1 1.476(7) . ?
O4 S1 1.373(6) . ?
S1 C19 1.745(10) . ?
F1 C19 1.313(10) . ?
F2 C19 1.402(10) . ?
F3 C19 1.351(9) . ?
C1 C2 1.385(7) . ?
C2 C3 1.379(7) . ?
C3 C4 1.364(7) . ?
C3 C6 1.526(7) . ?
C4 C5 1.380(7) . ?
C7 C8 1.512(10) . ?
C9 C13 1.422(7) . ?
C9 C10 1.447(7) . ?
C9 C14 1.514(7) . ?
C10 C11 1.403(7) . ?
C10 C15 1.494(8) . ?
C11 C12 1.431(8) . ?
C11 C16 1.481(8) . ?
C12 C13 1.423(7) . ?
C12 C17 1.502(7) . ?
C13 C18 1.504(8) . ?

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 Rh1 N3 77.09(14) . . ?
O1 Rh1 N1 84.74(13) . 8_756 ?
N3 Rh1 N1 84.23(16) . 8_756 ?
O1 Rh1 C9 97.13(16) . . ?
N3 Rh1 C9 119.83(18) . . ?
N1 Rh1 C9 155.75(18) 8_756 . ?
O1 Rh1 C12 161.42(16) . . ?
N3 Rh1 C12 115.34(19) . . ?
N1 Rh1 C12 109.40(17) 8_756 . ?
C9 Rh1 C12 64.98(18) . . ?
O1 Rh1 C10 98.18(16) . . ?
N3 Rh1 C10 158.75(18) . . ?
N1 Rh1 C10 116.25(17) 8_756 . ?
C9 Rh1 C10 39.50(19) . . ?
C12 Rh1 C10 65.09(19) . . ?
O1 Rh1 C13 128.46(16) . . ?
N3 Rh1 C13 100.99(18) . . ?
N1 Rh1 C13 146.79(17) 8_756 . ?
C9 Rh1 C13 38.71(19) . . ?
C12 Rh1 C13 38.73(19) . . ?
C10 Rh1 C13 65.44(19) . . ?
O1 Rh1 C11 130.38(18) . . ?
N3 Rh1 C11 152.50(19) . . ?
N1 Rh1 C11 95.84(17) 8_756 . ?
C9 Rh1 C11 64.55(19) . . ?
C12 Rh1 C11 38.9(2) . . ?
C10 Rh1 C11 37.97(19) . . ?
C13 Rh1 C11 64.7(2) . . ?
C5 N1 C1 117.5(4) . . ?
C5 N1 Rh1 122.6(3) . 7_576 ?
C1 N1 Rh1 119.9(3) . 7_576 ?
C6 N2 N3 110.5(4) . . ?
C7 N3 N2 117.2(5) . . ?
C7 N3 Rh1 129.5(4) . . ?
N2 N3 Rh1 113.3(3) . . ?
C6 O1 Rh1 109.9(3) . . ?
O4 S1 O2 121.5(5) . . ?
O4 S1 O3 109.4(5) . . ?
O2 S1 O3 108.9(4) . . ?
O4 S1 C19 108.5(4) . . ?
O2 S1 C19 106.2(4) . . ?
O3 S1 C19 100.1(5) . . ?
N1 C1 C2 124.0(5) . . ?
C3 C2 C1 117.4(5) . . ?
C4 C3 C2 119.1(5) . . ?
C4 C3 C6 119.7(4) . . ?
C2 C3 C6 121.2(4) . . ?
C3 C4 C5 120.0(5) . . ?
N1 C5 C4 122.0(5) . . ?
O1 C6 N2 129.1(5) . . ?
O1 C6 C3 115.1(4) . . ?
N2 C6 C3 115.8(4) . . ?
N3 C7 C8 125.7(7) . . ?
C13 C9 C10 108.5(4) . . ?
C13 C9 C14 126.6(5) . . ?
C10 C9 C14 124.9(5) . . ?
C13 C9 Rh1 71.6(3) . . ?
C10 C9 Rh1 70.9(3) . . ?
C14 C9 Rh1 125.3(4) . . ?
C11 C10 C9 107.2(5) . . ?
C11 C10 C15 127.4(5) . . ?
C9 C10 C15 125.4(5) . . ?
C11 C10 Rh1 71.5(3) . . ?
C9 C10 Rh1 69.6(3) . . ?
C15 C10 Rh1 126.1(4) . . ?
C10 C11 C12 108.9(4) . . ?
C10 C11 C16 125.3(5) . . ?
C12 C11 C16 125.9(5) . . ?
C10 C11 Rh1 70.5(3) . . ?
C12 C11 Rh1 69.5(3) . . ?
C16 C11 Rh1 125.0(4) . . ?
C13 C12 C11 108.1(4) . . ?
C13 C12 C17 123.8(5) . . ?
C11 C12 C17 127.7(5) . . ?
C13 C12 Rh1 71.4(3) . . ?
C11 C12 Rh1 71.6(3) . . ?
C17 C12 Rh1 128.2(4) . . ?
C9 C13 C12 107.4(5) . . ?
C9 C13 C18 125.9(5) . . ?
C12 C13 C18 126.7(5) . . ?
C9 C13 Rh1 69.7(3) . . ?
C12 C13 Rh1 69.8(3) . . ?
C18 C13 Rh1 127.5(4) . . ?
F1 C19 F3 107.8(8) . . ?
F1 C19 F2 105.1(7) . . ?
F3 C19 F2 104.7(7) . . ?
F1 C19 S1 117.9(6) . . ?
F3 C19 S1 115.0(6) . . ?
F2 C19 S1 105.0(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
C6 N2 N3 C7 179.4(5) . . . . ?
C6 N2 N3 Rh1 -3.7(5) . . . . ?
C5 N1 C1 C2 -0.7(8) . . . . ?
Rh1 N1 C1 C2 177.8(4) 7_576 . . . ?
N1 C1 C2 C3 -0.2(8) . . . . ?
C1 C2 C3 C4 1.1(7) . . . . ?
C1 C2 C3 C6 -179.8(4) . . . . ?
C2 C3 C4 C5 -1.1(8) . . . . ?
C6 C3 C4 C5 179.8(5) . . . . ?
C1 N1 C5 C4 0.8(8) . . . . ?
Rh1 N1 C5 C4 -177.7(4) 7_576 . . . ?
C3 C4 C5 N1 0.1(9) . . . . ?
Rh1 O1 C6 N2 3.0(6) . . . . ?
Rh1 O1 C6 C3 -177.9(3) . . . . ?
N3 N2 C6 O1 0.4(7) . . . . ?
N3 N2 C6 C3 -178.7(4) . . . . ?
C4 C3 C6 O1 9.0(6) . . . . ?
C2 C3 C6 O1 -170.1(4) . . . . ?
C4 C3 C6 N2 -171.7(5) . . . . ?
C2 C3 C6 N2 9.2(6) . . . . ?
N2 N3 C7 C8 3.1(10) . . . . ?
Rh1 N3 C7 C8 -173.2(6) . . . . ?
C13 C9 C10 C11 0.0(5) . . . . ?
C14 C9 C10 C11 177.8(5) . . . . ?
Rh1 C9 C10 C11 -62.1(3) . . . . ?
C13 C9 C10 C15 -177.4(5) . . . . ?
C14 C9 C10 C15 0.3(8) . . . . ?
Rh1 C9 C10 C15 120.5(5) . . . . ?
C13 C9 C10 Rh1 62.1(3) . . . . ?
C14 C9 C10 Rh1 -120.2(5) . . . . ?
C9 C10 C11 C12 1.7(5) . . . . ?
C15 C10 C11 C12 179.0(5) . . . . ?
Rh1 C10 C11 C12 -59.2(3) . . . . ?
C9 C10 C11 C16 -179.5(5) . . . . ?
C15 C10 C11 C16 -2.1(8) . . . . ?
Rh1 C10 C11 C16 119.7(5) . . . . ?
C9 C10 C11 Rh1 60.8(3) . . . . ?
C15 C10 C11 Rh1 -121.8(5) . . . . ?
C10 C11 C12 C13 -2.7(5) . . . . ?
C16 C11 C12 C13 178.4(5) . . . . ?
Rh1 C11 C12 C13 -62.5(3) . . . . ?
C10 C11 C12 C17 -175.7(5) . . . . ?
C16 C11 C12 C17 5.5(8) . . . . ?
Rh1 C11 C12 C17 124.5(5) . . . . ?
C10 C11 C12 Rh1 59.8(3) . . . . ?
C16 C11 C12 Rh1 -119.1(5) . . . . ?
C10 C9 C13 C12 -1.7(5) . . . . ?
C14 C9 C13 C12 -179.4(5) . . . . ?
Rh1 C9 C13 C12 59.9(3) . . . . ?
C10 C9 C13 C18 176.1(5) . . . . ?
C14 C9 C13 C18 -1.6(8) . . . . ?
Rh1 C9 C13 C18 -122.3(5) . . . . ?
C10 C9 C13 Rh1 -61.6(3) . . . . ?
C14 C9 C13 Rh1 120.7(5) . . . . ?
C11 C12 C13 C9 2.7(5) . . . . ?
C17 C12 C13 C9 176.0(5) . . . . ?
Rh1 C12 C13 C9 -59.9(3) . . . . ?
C11 C12 C13 C18 -175.1(5) . . . . ?
C17 C12 C13 C18 -1.7(8) . . . . ?
Rh1 C12 C13 C18 122.4(5) . . . . ?
C11 C12 C13 Rh1 62.6(3) . . . . ?
C17 C12 C13 Rh1 -124.1(5) . . . . ?
O4 S1 C19 F1 178.5(7) . . . . ?
O2 S1 C19 F1 -49.3(9) . . . . ?
O3 S1 C19 F1 63.9(8) . . . . ?
O4 S1 C19 F3 49.6(9) . . . . ?
O2 S1 C19 F3 -178.2(7) . . . . ?
O3 S1 C19 F3 -64.9(8) . . . . ?
O4 S1 C19 F2 -64.9(7) . . . . ?
O2 S1 C19 F2 67.3(7) . . . . ?
O3 S1 C19 F2 -179.5(6) . . . . ?

_refine_diff_density_max         1.293
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.126

_shelxl_version_number           2013-2

