# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_p21c

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H26 Cl F3 N3 O4 Rh S'
_chemical_formula_weight         671.92

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'
Cl Cl 0.1484 0.1585 '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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)/c  '

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

_cell_length_a                   8.583(4)
_cell_length_b                   16.929(7)
_cell_length_c                   19.659(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.892(5)
_cell_angle_gamma                90.00
_cell_volume                     2814(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    1674
_cell_measurement_theta_min      2.41
_cell_measurement_theta_max      18.57

_exptl_crystal_description       block
_exptl_crystal_colour            'black red'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1360
_exptl_absorpt_coefficient_mu    0.833
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.8188
_exptl_absorpt_correction_T_max  0.9214
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      273(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16910
_diffrn_reflns_av_R_equivalents  0.1042
_diffrn_reflns_av_sigmaI/netI    0.1503
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.41
_diffrn_reflns_theta_max         27.71
_reflns_number_total             6409
_reflns_number_gt                2852
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0780P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6409
_refine_ls_number_parameters     358
_refine_ls_number_restraints     370
_refine_ls_R_factor_all          0.1869
_refine_ls_R_factor_gt           0.0813
_refine_ls_wR_factor_ref         0.1905
_refine_ls_wR_factor_gt          0.1528
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_restrained_S_all      0.946
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.11065(7) 0.77730(3) 0.47907(3) 0.0519(2) Uani 1 1 d U . .
S2 S 0.2494(2) 0.48497(13) 0.36775(11) 0.0630(6) Uani 1 1 d U . .
Cl1 Cl -0.1165(2) 0.86286(12) 0.45541(12) 0.0795(7) Uani 1 1 d U . .
N2 N 0.1222(7) 0.7817(3) 0.3737(3) 0.0538(13) Uani 1 1 d U . .
N1 N 0.0360(7) 0.7345(4) 0.3323(3) 0.0589(15) Uani 1 1 d U . .
C33 C 0.2188(10) 0.8439(4) 0.5699(4) 0.0638(17) Uani 1 1 d U . .
C32 C 0.1492(9) 0.7718(5) 0.5895(4) 0.0623(17) Uani 1 1 d U . .
C35 C 0.3445(9) 0.7410(5) 0.5264(4) 0.0611(17) Uani 1 1 d U . .
N4 N -0.0454(6) 0.6899(3) 0.4341(3) 0.0500(13) Uani 1 1 d U . .
C31 C 0.2316(8) 0.8283(5) 0.3419(4) 0.0584(17) Uani 1 1 d U . .
C12 C -0.0613(8) 0.6863(4) 0.3653(4) 0.0509(16) Uani 1 1 d U . .
C16 C 0.3285(9) 0.7898(5) 0.2994(4) 0.0644(18) Uani 1 1 d U . .
C34 C 0.3400(9) 0.8243(5) 0.5315(4) 0.0643(17) Uani 1 1 d U . .
C18 C 0.5231(11) 0.7276(6) 0.2103(5) 0.087(2) Uani 1 1 d U . .
H18 H 0.5838 0.7060 0.1801 0.105 Uiso 1 1 calc R . .
C8 C -0.1403(9) 0.6442(4) 0.4652(4) 0.0596(19) Uani 1 1 d U . .
H8 H -0.1341 0.6480 0.5127 0.072 Uiso 1 1 calc R . .
C9 C -0.2463(9) 0.5921(4) 0.4290(5) 0.063(2) Uani 1 1 d U . .
H9 H -0.3064 0.5594 0.4524 0.076 Uiso 1 1 calc R . .
C17 C 0.4340(9) 0.8411(5) 0.2665(4) 0.069(2) Uani 1 1 d U . .
C10 C -0.2628(9) 0.5885(5) 0.3594(5) 0.071(2) Uani 1 1 d U . .
H10 H -0.3360 0.5544 0.3343 0.085 Uiso 1 1 calc R . .
C36 C 0.2325(9) 0.7078(4) 0.5643(4) 0.0598(17) Uani 1 1 d U . .
C20 C 0.5250(11) 0.8078(6) 0.2220(5) 0.085(2) Uani 1 1 d U . .
H20 H 0.5879 0.8402 0.1997 0.102 Uiso 1 1 calc R . .
C19 C 0.3352(9) 0.7077(5) 0.2889(4) 0.070(2) Uani 1 1 d U . .
H19 H 0.2768 0.6737 0.3120 0.084 Uiso 1 1 calc R . .
C40 C 0.4593(10) 0.6947(5) 0.4925(5) 0.088(3) Uani 1 1 d U . .
H40A H 0.5117 0.7295 0.4652 0.131 Uiso 1 1 calc R . .
H40B H 0.4034 0.6547 0.4634 0.131 Uiso 1 1 calc R . .
H40C H 0.5363 0.6702 0.5274 0.131 Uiso 1 1 calc R . .
C11 C -0.1687(8) 0.6366(5) 0.3257(4) 0.067(2) Uani 1 1 d U . .
H11 H -0.1778 0.6354 0.2779 0.080 Uiso 1 1 calc R . .
C28 C 0.2359(10) 0.9089(5) 0.3533(4) 0.067(2) Uani 1 1 d U . .
C41 C 0.2119(12) 0.6215(5) 0.5751(5) 0.095(3) Uani 1 1 d U . .
H41A H 0.2973 0.6024 0.6092 0.142 Uiso 1 1 calc R . .
H41B H 0.2119 0.5940 0.5324 0.142 Uiso 1 1 calc R . .
H41C H 0.1133 0.6125 0.5906 0.142 Uiso 1 1 calc R . .
C37 C 0.0243(12) 0.7636(6) 0.6338(5) 0.101(3) Uani 1 1 d U . .
H37A H 0.0726 0.7657 0.6816 0.152 Uiso 1 1 calc R . .
H37B H -0.0289 0.7139 0.6243 0.152 Uiso 1 1 calc R . .
H37C H -0.0506 0.8058 0.6238 0.152 Uiso 1 1 calc R . .
C25 C 0.4277(10) 0.6777(6) 0.2447(5) 0.085(2) Uani 1 1 d U . .
H25 H 0.4282 0.6235 0.2370 0.101 Uiso 1 1 calc R . .
C38 C 0.1742(12) 0.9259(5) 0.5891(5) 0.095(3) Uani 1 1 d U . .
H38A H 0.0669 0.9260 0.5969 0.143 Uiso 1 1 calc R . .
H38B H 0.1842 0.9616 0.5522 0.143 Uiso 1 1 calc R . .
H38C H 0.2432 0.9424 0.6303 0.143 Uiso 1 1 calc R . .
C39 C 0.4544(10) 0.8822(6) 0.5070(5) 0.096(3) Uani 1 1 d U . .
H39A H 0.5543 0.8801 0.5376 0.144 Uiso 1 1 calc R . .
H39B H 0.4120 0.9347 0.5068 0.144 Uiso 1 1 calc R . .
H39C H 0.4689 0.8683 0.4612 0.144 Uiso 1 1 calc R . .
C26 C 0.4375(10) 0.9217(6) 0.2807(5) 0.083(2) Uani 1 1 d U . .
H26 H 0.5062 0.9537 0.2611 0.099 Uiso 1 1 calc R . .
C27 C 0.3445(11) 0.9553(5) 0.3218(5) 0.083(2) Uani 1 1 d U . .
H27 H 0.3511 1.0094 0.3298 0.099 Uiso 1 1 calc R . .
O4 O 0.1453(8) 0.9491(3) 0.3901(3) 0.0845(17) Uani 1 1 d U . .
H4 H 0.0887 0.9183 0.4068 0.127 Uiso 1 1 calc R . .
O1 O 0.1822(8) 0.5451(4) 0.4032(3) 0.116(2) Uani 1 1 d U . .
O3 O 0.3927(7) 0.5050(4) 0.3441(3) 0.097(2) Uani 1 1 d U . .
O2 O 0.2483(7) 0.4071(4) 0.3945(3) 0.098(2) Uani 1 1 d U . .
C30 C 0.1092(11) 0.4763(5) 0.2868(5) 0.070(2) Uani 1 1 d U . .
F3 F -0.0337(6) 0.4564(4) 0.2973(3) 0.1156(19) Uani 1 1 d U . .
F2 F 0.0905(7) 0.5441(4) 0.2532(3) 0.1177(19) Uani 1 1 d U . .
F1 F 0.1548(7) 0.4256(4) 0.2449(3) 0.126(2) Uani 1 1 d U . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 N4 2.087(6) . ?
Rh1 N2 2.093(6) . ?
Rh1 C32 2.141(8) . ?
Rh1 C35 2.152(7) . ?
Rh1 C36 2.165(7) . ?
Rh1 C33 2.180(8) . ?
Rh1 C34 2.208(8) . ?
Rh1 Cl1 2.409(2) . ?
S2 O1 1.412(6) . ?
S2 O2 1.420(6) . ?
S2 O3 1.428(6) . ?
S2 C30 1.828(9) . ?
N2 N1 1.280(8) . ?
N2 C31 1.449(9) . ?
N1 C12 1.404(9) . ?
C33 C34 1.426(10) . ?
C33 C32 1.440(10) . ?
C33 C38 1.504(10) . ?
C32 C36 1.433(10) . ?
C32 C37 1.499(11) . ?
C35 C34 1.415(11) . ?
C35 C36 1.430(11) . ?
C35 C40 1.501(11) . ?
N4 C12 1.337(8) . ?
N4 C8 1.344(8) . ?
C31 C28 1.382(11) . ?
C31 C16 1.431(11) . ?
C12 C11 1.385(10) . ?
C16 C19 1.409(10) . ?
C16 C17 1.481(11) . ?
C34 C39 1.523(10) . ?
C18 C20 1.377(12) . ?
C18 C25 1.426(12) . ?
C8 C9 1.374(10) . ?
C9 C10 1.354(10) . ?
C17 C20 1.389(11) . ?
C17 C26 1.392(11) . ?
C10 C11 1.391(11) . ?
C36 C41 1.491(10) . ?
C19 C25 1.371(11) . ?
C28 O4 1.337(10) . ?
C28 C27 1.437(11) . ?
C26 C27 1.354(12) . ?
C30 F1 1.298(9) . ?
C30 F2 1.320(9) . ?
C30 F3 1.321(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
N4 Rh1 N2 75.1(2) . . ?
N4 Rh1 C32 112.0(3) . . ?
N2 Rh1 C32 168.6(3) . . ?
N4 Rh1 C35 117.6(3) . . ?
N2 Rh1 C35 103.8(3) . . ?
C32 Rh1 C35 65.1(3) . . ?
N4 Rh1 C36 97.6(3) . . ?
N2 Rh1 C36 133.4(3) . . ?
C32 Rh1 C36 38.9(3) . . ?
C35 Rh1 C36 38.7(3) . . ?
N4 Rh1 C33 149.9(3) . . ?
N2 Rh1 C33 135.0(3) . . ?
C32 Rh1 C33 38.9(3) . . ?
C35 Rh1 C33 63.9(3) . . ?
C36 Rh1 C33 64.3(3) . . ?
N4 Rh1 C34 155.4(3) . . ?
N2 Rh1 C34 105.0(3) . . ?
C32 Rh1 C34 64.7(3) . . ?
C35 Rh1 C34 37.9(3) . . ?
C36 Rh1 C34 64.0(3) . . ?
C33 Rh1 C34 37.9(3) . . ?
N4 Rh1 Cl1 84.55(16) . . ?
N2 Rh1 Cl1 87.81(16) . . ?
C32 Rh1 Cl1 101.6(2) . . ?
C35 Rh1 Cl1 156.8(2) . . ?
C36 Rh1 Cl1 138.1(2) . . ?
C33 Rh1 Cl1 93.6(2) . . ?
C34 Rh1 Cl1 120.0(2) . . ?
O1 S2 O2 117.2(5) . . ?
O1 S2 O3 115.9(5) . . ?
O2 S2 O3 113.7(4) . . ?
O1 S2 C30 102.9(4) . . ?
O2 S2 C30 101.7(4) . . ?
O3 S2 C30 102.2(4) . . ?
N1 N2 C31 114.4(6) . . ?
N1 N2 Rh1 119.1(4) . . ?
C31 N2 Rh1 126.3(5) . . ?
N2 N1 C12 113.2(6) . . ?
C34 C33 C32 108.5(7) . . ?
C34 C33 C38 125.9(8) . . ?
C32 C33 C38 125.5(8) . . ?
C34 C33 Rh1 72.1(4) . . ?
C32 C33 Rh1 69.1(4) . . ?
C38 C33 Rh1 126.3(6) . . ?
C36 C32 C33 107.1(7) . . ?
C36 C32 C37 125.4(8) . . ?
C33 C32 C37 127.2(8) . . ?
C36 C32 Rh1 71.5(4) . . ?
C33 C32 Rh1 72.0(4) . . ?
C37 C32 Rh1 126.2(6) . . ?
C34 C35 C36 109.0(7) . . ?
C34 C35 C40 125.5(8) . . ?
C36 C35 C40 125.3(8) . . ?
C34 C35 Rh1 73.2(4) . . ?
C36 C35 Rh1 71.2(4) . . ?
C40 C35 Rh1 126.3(5) . . ?
C12 N4 C8 117.9(6) . . ?
C12 N4 Rh1 114.0(5) . . ?
C8 N4 Rh1 127.7(5) . . ?
C28 C31 C16 122.8(7) . . ?
C28 C31 N2 118.0(7) . . ?
C16 C31 N2 119.2(7) . . ?
N4 C12 C11 122.6(7) . . ?
N4 C12 N1 118.4(6) . . ?
C11 C12 N1 119.0(7) . . ?
C19 C16 C31 125.3(7) . . ?
C19 C16 C17 118.1(8) . . ?
C31 C16 C17 116.6(8) . . ?
C35 C34 C33 107.5(7) . . ?
C35 C34 C39 126.3(8) . . ?
C33 C34 C39 125.9(8) . . ?
C35 C34 Rh1 68.9(4) . . ?
C33 C34 Rh1 70.0(4) . . ?
C39 C34 Rh1 131.0(5) . . ?
C20 C18 C25 119.8(9) . . ?
N4 C8 C9 122.3(8) . . ?
C10 C9 C8 119.8(8) . . ?
C20 C17 C26 121.9(9) . . ?
C20 C17 C16 119.4(9) . . ?
C26 C17 C16 118.8(8) . . ?
C9 C10 C11 119.1(8) . . ?
C35 C36 C32 107.6(6) . . ?
C35 C36 C41 124.5(8) . . ?
C32 C36 C41 127.9(8) . . ?
C35 C36 Rh1 70.2(4) . . ?
C32 C36 Rh1 69.7(4) . . ?
C41 C36 Rh1 126.1(5) . . ?
C18 C20 C17 120.8(9) . . ?
C25 C19 C16 120.1(8) . . ?
C12 C11 C10 118.2(8) . . ?
O4 C28 C31 126.1(7) . . ?
O4 C28 C27 115.9(8) . . ?
C31 C28 C27 118.1(8) . . ?
C19 C25 C18 121.5(10) . . ?
C27 C26 C17 122.4(9) . . ?
C26 C27 C28 121.3(9) . . ?
F1 C30 F2 106.3(8) . . ?
F1 C30 F3 108.6(8) . . ?
F2 C30 F3 105.3(8) . . ?
F1 C30 S2 112.4(6) . . ?
F2 C30 S2 111.8(6) . . ?
F3 C30 S2 112.0(6) . . ?

_diffrn_measured_fraction_theta_max 0.971
_diffrn_reflns_theta_full        27.71
_diffrn_measured_fraction_theta_full 0.971
_refine_diff_density_max         1.194
_refine_diff_density_min         -0.759
_refine_diff_density_rms         0.117
_database_code_depnum_ccdc_archive 'CCDC 979114'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_p-1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C27 H26 F6 Ir N3 O8 S2'
_chemical_formula_weight         890.83

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'

_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                   9.205(2)
_cell_length_b                   11.366(3)
_cell_length_c                   16.818(4)
_cell_angle_alpha                102.389(3)
_cell_angle_beta                 96.745(3)
_cell_angle_gamma                104.938(2)
_cell_volume                     1632.4(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4459
_cell_measurement_theta_min      2.52
_cell_measurement_theta_max      25.37

_exptl_crystal_description       block
_exptl_crystal_colour            'black red'
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.812
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             872
_exptl_absorpt_coefficient_mu    4.303
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4249
_exptl_absorpt_correction_T_max  0.5646
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10170
_diffrn_reflns_av_R_equivalents  0.0213
_diffrn_reflns_av_sigmaI/netI    0.0493
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.52
_diffrn_reflns_theta_max         27.48
_reflns_number_total             7188
_reflns_number_gt                6144
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0738P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7188
_refine_ls_number_parameters     430
_refine_ls_number_restraints     425
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0429
_refine_ls_wR_factor_ref         0.1155
_refine_ls_wR_factor_gt          0.1101
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.004
_refine_ls_shift/su_max          0.037
_refine_ls_shift/su_mean         0.002

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
Ir1 Ir 0.58587(2) 0.606734(19) 0.720118(13) 0.03192(9) Uani 1 1 d U . .
S2 S 0.1918(2) 0.80159(19) 0.57823(12) 0.0580(4) Uani 1 1 d U . .
O2 O 0.3740(5) 0.5558(4) 0.6320(3) 0.0454(10) Uani 1 1 d U . .
N1 N 0.5284(5) 0.7553(4) 0.7927(3) 0.0326(9) Uani 1 1 d U . .
O1 O 0.2685(5) 0.5824(4) 0.7958(3) 0.0490(11) Uani 1 1 d U . .
H1 H 0.1951 0.5306 0.8039 0.073 Uiso 1 1 calc R . .
N3 N 0.6423(6) 0.7546(4) 0.6626(3) 0.0372(10) Uani 1 1 d U . .
N2 N 0.5600(6) 0.8623(4) 0.7758(3) 0.0396(11) Uani 1 1 d U . .
C17 C 0.5912(8) 0.9204(6) 1.0934(4) 0.0492(15) Uani 1 1 d U . .
H17 H 0.5527 0.9166 1.1418 0.059 Uiso 1 1 calc R . .
C13 C 0.3445(7) 0.6631(5) 0.8683(4) 0.0391(12) Uani 1 1 d U . .
C21 C 0.5654(7) 0.8443(5) 0.9433(4) 0.0360(12) Uani 1 1 d U . .
C6 C 0.6198(7) 0.8629(5) 0.7040(4) 0.0374(12) Uani 1 1 d U . .
C12 C 0.4767(7) 0.7541(5) 0.8680(3) 0.0344(11) Uani 1 1 d U . .
C4 C 0.5766(7) 0.4417(6) 0.7677(5) 0.0462(13) Uani 1 1 d U . .
C5 C 0.6200(8) 0.4196(6) 0.6890(5) 0.0498(14) Uani 1 1 d U . .
C3 C 0.6924(9) 0.5469(6) 0.8207(4) 0.0517(14) Uani 1 1 d U . .
C2 C 0.8010(8) 0.5902(7) 0.7704(6) 0.0648(17) Uani 1 1 d U . .
C1 C 0.7578(9) 0.5099(7) 0.6904(5) 0.0577(16) Uani 1 1 d U . .
C10 C 0.6954(8) 0.7525(7) 0.5922(4) 0.0490(15) Uani 1 1 d U . .
H10 H 0.7095 0.6784 0.5626 0.059 Uiso 1 1 calc R . .
C9 C 0.7301(9) 0.8589(7) 0.5621(4) 0.0563(17) Uani 1 1 d U . .
H9 H 0.7682 0.8556 0.5131 0.068 Uiso 1 1 calc R . .
C7 C 0.6510(8) 0.9708(6) 0.6765(4) 0.0504(16) Uani 1 1 d U . .
H7 H 0.6337 1.0435 0.7059 0.060 Uiso 1 1 calc R . .
C8 C 0.7089(9) 0.9682(7) 0.6037(4) 0.0570(18) Uani 1 1 d U . .
H8 H 0.7328 1.0398 0.5838 0.068 Uiso 1 1 calc R . .
C20 C 0.7060(7) 0.9344(6) 0.9495(4) 0.0436(13) Uani 1 1 d U . .
H20 H 0.7459 0.9414 0.9019 0.052 Uiso 1 1 calc R . .
C16 C 0.5076(7) 0.8365(6) 1.0182(4) 0.0422(13) Uani 1 1 d U . .
C14 C 0.2914(7) 0.6572(6) 0.9430(4) 0.0465(14) Uani 1 1 d U . .
H14 H 0.2029 0.5952 0.9432 0.056 Uiso 1 1 calc R . .
C15 C 0.3699(8) 0.7425(6) 1.0148(4) 0.0476(14) Uani 1 1 d U . .
H15 H 0.3318 0.7391 1.0633 0.057 Uiso 1 1 calc R . .
C19 C 0.7847(9) 1.0115(7) 1.0240(5) 0.0538(17) Uani 1 1 d U . .
H19 H 0.8789 1.0688 1.0267 0.065 Uiso 1 1 calc R . .
C18 C 0.7250(9) 1.0058(7) 1.0972(4) 0.0578(17) Uani 1 1 d U . .
H18 H 0.7780 1.0607 1.1476 0.069 Uiso 1 1 calc R . .
O3 O 0.2493(8) 0.7484(6) 0.6390(5) 0.095(2) Uani 1 1 d U . .
O4 O 0.0379(8) 0.7383(7) 0.5387(4) 0.091(2) Uani 1 1 d U . .
O5 O 0.3009(10) 0.8432(9) 0.5277(5) 0.125(3) Uani 1 1 d U . .
C22 C 0.1787(12) 0.9471(9) 0.6399(6) 0.078(2) Uani 1 1 d U . .
F1 F 0.0826(8) 0.9301(6) 0.6897(4) 0.109(2) Uani 1 1 d U . .
F3 F 0.1243(10) 1.0130(6) 0.5916(5) 0.122(2) Uani 1 1 d U . .
F2 F 0.3083(9) 1.0190(7) 0.6841(6) 0.144(3) Uani 1 1 d U . .
C26 C 0.4463(10) 0.3603(9) 0.7926(7) 0.089(3) Uani 1 1 d U . .
H26A H 0.4309 0.2740 0.7641 0.134 Uiso 1 1 calc R . .
H26B H 0.3558 0.3841 0.7786 0.134 Uiso 1 1 calc R . .
H26C H 0.4677 0.3698 0.8513 0.134 Uiso 1 1 calc R . .
C23 C 0.8469(14) 0.5132(12) 0.6226(8) 0.110(4) Uani 1 1 d U . .
H23A H 0.8983 0.5991 0.6246 0.165 Uiso 1 1 calc R . .
H23B H 0.7790 0.4743 0.5703 0.165 Uiso 1 1 calc R . .
H23C H 0.9210 0.4684 0.6290 0.165 Uiso 1 1 calc R . .
C25 C 0.6998(15) 0.5893(10) 0.9112(5) 0.105(4) Uani 1 1 d U . .
H25A H 0.7455 0.5383 0.9387 0.158 Uiso 1 1 calc R . .
H25B H 0.5983 0.5812 0.9225 0.158 Uiso 1 1 calc R . .
H25C H 0.7603 0.6758 0.9310 0.158 Uiso 1 1 calc R . .
C27 C 0.5345(13) 0.3136(9) 0.6163(7) 0.102(4) Uani 1 1 d U . .
H27A H 0.5539 0.2372 0.6235 0.153 Uiso 1 1 calc R . .
H27B H 0.5675 0.3311 0.5669 0.153 Uiso 1 1 calc R . .
H27C H 0.4269 0.3043 0.6116 0.153 Uiso 1 1 calc R . .
C24 C 0.9467(10) 0.7015(9) 0.8028(9) 0.118(5) Uani 1 1 d U . .
H24A H 1.0127 0.6832 0.8440 0.177 Uiso 1 1 calc R . .
H24B H 0.9200 0.7758 0.8268 0.177 Uiso 1 1 calc R . .
H24C H 0.9986 0.7151 0.7578 0.177 Uiso 1 1 calc R . .
S1 S 0.9298(2) 0.3087(2) 0.80348(19) 0.0818(8) Uani 1 1 d U . .
O8 O 0.7746(6) 0.2617(5) 0.7956(4) 0.0739(16) Uani 1 1 d U . .
O7 O 0.9650(15) 0.2535(15) 0.7171(7) 0.186(5) Uani 1 1 d U . .
C28 C 1.0168(10) 0.2184(10) 0.8567(8) 0.084(3) Uani 1 1 d U . .
F4 F 1.1629(6) 0.2592(8) 0.8779(5) 0.131(3) Uani 1 1 d U . .
F5 F 0.9547(11) 0.1053(8) 0.8391(9) 0.208(5) Uani 1 1 d U . .
F6 F 0.9811(11) 0.2322(15) 0.9306(6) 0.202(5) Uani 1 1 d U . .
O9 O 1.0090(9) 0.4200(7) 0.8178(9) 0.187(5) Uani 1 1 d U . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ir1 N1 2.085(5) . ?
Ir1 N3 2.097(5) . ?
Ir1 C2 2.130(7) . ?
Ir1 O2 2.170(4) . ?
Ir1 C3 2.175(6) . ?
Ir1 C4 2.178(6) . ?
Ir1 C5 2.192(6) . ?
Ir1 C1 2.194(7) . ?
S2 O3 1.412(7) . ?
S2 O4 1.419(7) . ?
S2 O5 1.443(7) . ?
S2 C22 1.795(10) . ?
N1 N2 1.277(6) . ?
N1 C12 1.407(7) . ?
O1 C13 1.344(7) . ?
N3 C10 1.331(8) . ?
N3 C6 1.357(8) . ?
N2 C6 1.385(8) . ?
C17 C18 1.343(10) . ?
C17 C16 1.405(9) . ?
C13 C12 1.381(8) . ?
C13 C14 1.408(9) . ?
C21 C20 1.405(8) . ?
C21 C16 1.435(8) . ?
C21 C12 1.445(8) . ?
C6 C7 1.375(8) . ?
C4 C5 1.418(10) . ?
C4 C3 1.421(10) . ?
C4 C26 1.477(10) . ?
C5 C1 1.406(10) . ?
C5 C27 1.489(10) . ?
C3 C2 1.442(12) . ?
C3 C25 1.483(11) . ?
C2 C1 1.400(12) . ?
C2 C24 1.534(11) . ?
C1 C23 1.482(12) . ?
C10 C9 1.386(10) . ?
C9 C8 1.363(11) . ?
C7 C8 1.388(10) . ?
C20 C19 1.360(9) . ?
C16 C15 1.418(9) . ?
C14 C15 1.361(9) . ?
C19 C18 1.414(11) . ?
C22 F1 1.296(11) . ?
C22 F2 1.293(11) . ?
C22 F3 1.352(11) . ?
S1 O9 1.242(7) . ?
S1 O8 1.370(6) . ?
S1 O7 1.559(12) . ?
S1 C28 1.773(9) . ?
C28 F5 1.219(12) . ?
C28 F4 1.283(10) . ?
C28 F6 1.309(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
N1 Ir1 N3 74.62(18) . . ?
N1 Ir1 C2 112.6(3) . . ?
N3 Ir1 C2 104.4(3) . . ?
N1 Ir1 O2 91.36(17) . . ?
N3 Ir1 O2 81.72(18) . . ?
C2 Ir1 O2 156.0(3) . . ?
N1 Ir1 C3 97.5(2) . . ?
N3 Ir1 C3 137.2(3) . . ?
C2 Ir1 C3 39.1(3) . . ?
O2 Ir1 C3 141.0(2) . . ?
N1 Ir1 C4 117.5(2) . . ?
N3 Ir1 C4 165.4(2) . . ?
C2 Ir1 C4 64.3(3) . . ?
O2 Ir1 C4 105.0(2) . . ?
C3 Ir1 C4 38.1(3) . . ?
N1 Ir1 C5 155.4(2) . . ?
N3 Ir1 C5 129.8(2) . . ?
C2 Ir1 C5 62.8(3) . . ?
O2 Ir1 C5 95.3(2) . . ?
C3 Ir1 C5 63.1(3) . . ?
C4 Ir1 C5 37.9(3) . . ?
N1 Ir1 C1 149.3(3) . . ?
N3 Ir1 C1 101.5(2) . . ?
C2 Ir1 C1 37.7(3) . . ?
O2 Ir1 C1 118.6(3) . . ?
C3 Ir1 C1 64.1(3) . . ?
C4 Ir1 C1 63.9(3) . . ?
C5 Ir1 C1 37.4(3) . . ?
O3 S2 O4 114.6(5) . . ?
O3 S2 O5 113.5(5) . . ?
O4 S2 O5 118.1(5) . . ?
O3 S2 C22 102.0(5) . . ?
O4 S2 C22 102.8(5) . . ?
O5 S2 C22 102.8(5) . . ?
N2 N1 C12 114.9(5) . . ?
N2 N1 Ir1 119.6(4) . . ?
C12 N1 Ir1 124.8(4) . . ?
C10 N3 C6 118.6(5) . . ?
C10 N3 Ir1 127.6(4) . . ?
C6 N3 Ir1 113.9(4) . . ?
N1 N2 C6 113.8(5) . . ?
C18 C17 C16 121.8(6) . . ?
O1 C13 C12 118.2(5) . . ?
O1 C13 C14 121.6(6) . . ?
C12 C13 C14 120.2(6) . . ?
C20 C21 C16 117.7(6) . . ?
C20 C21 C12 125.5(5) . . ?
C16 C21 C12 116.8(5) . . ?
N3 C6 C7 122.6(6) . . ?
N3 C6 N2 117.8(5) . . ?
C7 C6 N2 119.6(6) . . ?
C13 C12 N1 118.6(5) . . ?
C13 C12 C21 121.7(5) . . ?
N1 C12 C21 119.6(5) . . ?
C5 C4 C3 107.3(6) . . ?
C5 C4 C26 125.9(7) . . ?
C3 C4 C26 126.4(8) . . ?
C5 C4 Ir1 71.6(4) . . ?
C3 C4 Ir1 70.8(4) . . ?
C26 C4 Ir1 128.8(5) . . ?
C1 C5 C4 110.0(6) . . ?
C1 C5 C27 125.1(8) . . ?
C4 C5 C27 124.9(8) . . ?
C1 C5 Ir1 71.4(4) . . ?
C4 C5 Ir1 70.5(4) . . ?
C27 C5 Ir1 126.1(5) . . ?
C4 C3 C2 106.5(6) . . ?
C4 C3 C25 123.7(8) . . ?
C2 C3 C25 129.5(8) . . ?
C4 C3 Ir1 71.0(4) . . ?
C2 C3 Ir1 68.8(4) . . ?
C25 C3 Ir1 129.8(5) . . ?
C1 C2 C3 109.4(6) . . ?
C1 C2 C24 126.1(10) . . ?
C3 C2 C24 124.3(10) . . ?
C1 C2 Ir1 73.6(4) . . ?
C3 C2 Ir1 72.1(4) . . ?
C24 C2 Ir1 124.0(5) . . ?
C5 C1 C2 106.8(7) . . ?
C5 C1 C23 126.6(9) . . ?
C2 C1 C23 126.5(9) . . ?
C5 C1 Ir1 71.2(4) . . ?
C2 C1 Ir1 68.7(4) . . ?
C23 C1 Ir1 128.8(6) . . ?
N3 C10 C9 121.1(6) . . ?
C8 C9 C10 120.5(6) . . ?
C6 C7 C8 118.3(6) . . ?
C9 C8 C7 118.8(6) . . ?
C19 C20 C21 121.2(6) . . ?
C17 C16 C15 121.8(6) . . ?
C17 C16 C21 119.0(6) . . ?
C15 C16 C21 119.2(6) . . ?
C15 C14 C13 119.8(6) . . ?
C14 C15 C16 122.3(6) . . ?
C20 C19 C18 120.8(7) . . ?
C17 C18 C19 119.4(6) . . ?
F1 C22 F2 107.4(9) . . ?
F1 C22 F3 104.5(9) . . ?
F2 C22 F3 107.7(9) . . ?
F1 C22 S2 112.6(7) . . ?
F2 C22 S2 113.2(8) . . ?
F3 C22 S2 110.9(7) . . ?
O9 S1 O8 128.9(5) . . ?
O9 S1 O7 100.6(9) . . ?
O8 S1 O7 104.8(6) . . ?
O9 S1 C28 112.9(5) . . ?
O8 S1 C28 107.9(4) . . ?
O7 S1 C28 95.8(7) . . ?
F5 C28 F4 118.9(10) . . ?
F5 C28 F6 91.5(10) . . ?
F4 C28 F6 98.8(10) . . ?
F5 C28 S1 117.0(9) . . ?
F4 C28 S1 116.0(7) . . ?
F6 C28 S1 108.3(9) . . ?

_diffrn_measured_fraction_theta_max 0.962
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.962
_refine_diff_density_max         2.382
_refine_diff_density_min         -1.602
_refine_diff_density_rms         0.148
_database_code_depnum_ccdc_archive 'CCDC 979115'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_p-1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C27 H27 F6 N3 O8 Rh S2'
_chemical_formula_weight         802.55

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'

_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                   9.1279(17)
_cell_length_b                   11.394(2)
_cell_length_c                   16.825(3)
_cell_angle_alpha                102.330(3)
_cell_angle_beta                 96.882(2)
_cell_angle_gamma                104.537(2)
_cell_volume                     1626.8(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2444
_cell_measurement_theta_min      2.45
_cell_measurement_theta_max      27.52

_exptl_crystal_description       block
_exptl_crystal_colour            'black red'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             810
_exptl_absorpt_coefficient_mu    0.739
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.8368
_exptl_absorpt_correction_T_max  0.8973
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7914
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_sigmaI/netI    0.0801
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.45
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5503
_reflns_number_gt                4060
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0678P)²+29.7039P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5503
_refine_ls_number_parameters     431
_refine_ls_number_restraints     431
_refine_ls_R_factor_all          0.1343
_refine_ls_R_factor_gt           0.0962
_refine_ls_wR_factor_ref         0.2546
_refine_ls_wR_factor_gt          0.2134
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.000
_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
Rh1 Rh 0.58655(10) 0.60331(8) 0.71832(5) 0.0354(3) Uani 1 1 d U . .
S2 S 0.1969(4) 0.8044(3) 0.5783(2) 0.0630(9) Uani 1 1 d U . .
S3 S 0.9357(4) 0.3144(4) 0.8089(4) 0.0891(15) Uani 1 1 d U . .
N3 N 0.6467(11) 0.7518(9) 0.6618(6) 0.044(2) Uani 1 1 d U . .
N2 N 0.5719(11) 0.8616(8) 0.7774(5) 0.042(2) Uani 1 1 d U . .
N1 N 0.5322(10) 0.7555(8) 0.7915(5) 0.0368(17) Uani 1 1 d U . .
O2 O 0.2789(10) 0.5845(8) 0.7973(5) 0.056(2) Uani 1 1 d U . .
H2 H 0.2061 0.5316 0.8049 0.084 Uiso 1 1 calc R . .
O1 O 0.3740(10) 0.5531(8) 0.6286(5) 0.0519(19) Uani 1 1 d U . .
H1 H 0.3186 0.4853 0.6306 0.078 Uiso 1 1 calc R . .
C11 C 0.5801(16) 0.4397(12) 0.7649(9) 0.057(2) Uani 1 1 d U . .
F3 F 0.1283(15) 1.0147(10) 0.5942(8) 0.123(4) Uani 1 1 d U . .
C5 C 0.6294(13) 0.8601(10) 0.7041(6) 0.040(2) Uani 1 1 d U . .
C21 C 0.5669(13) 0.8447(10) 0.9452(7) 0.042(2) Uani 1 1 d U . .
C16 C 0.5075(14) 0.8356(11) 1.0181(7) 0.045(2) Uani 1 1 d U . .
C12 C 0.4844(13) 0.7559(10) 0.8703(7) 0.041(2) Uani 1 1 d U . .
C15 C 0.3699(15) 0.7444(12) 1.0142(8) 0.052(3) Uani 1 1 d U . .
H15 H 0.3301 0.7418 1.0623 0.063 Uiso 1 1 calc R . .
C13 C 0.3517(13) 0.6654(10) 0.8702(7) 0.041(2) Uani 1 1 d U . .
C1 C 0.6966(14) 0.7518(12) 0.5916(8) 0.052(3) Uani 1 1 d U . .
H1A H 0.7081 0.6776 0.5608 0.063 Uiso 1 1 calc R . .
C17 C 0.5905(15) 0.9221(11) 1.0942(7) 0.050(3) Uani 1 1 d U . .
H17 H 0.5515 0.9199 1.1427 0.060 Uiso 1 1 calc R . .
C2 C 0.7326(14) 0.8572(12) 0.5620(8) 0.055(3) Uani 1 1 d U . .
H2A H 0.7660 0.8533 0.5117 0.066 Uiso 1 1 calc R . .
C3 C 0.7189(15) 0.9662(12) 0.6066(8) 0.057(3) Uani 1 1 d U . .
H3 H 0.7453 1.0386 0.5880 0.068 Uiso 1 1 calc R . .
C4 C 0.6653(16) 0.9690(11) 0.6801(8) 0.056(3) Uani 1 1 d U . .
H4 H 0.6540 1.0425 0.7120 0.067 Uiso 1 1 calc R . .
C10 C 0.6249(16) 0.4202(11) 0.6852(8) 0.057(2) Uani 1 1 d U . .
C9 C 0.7620(16) 0.5114(13) 0.6902(10) 0.065(3) Uani 1 1 d U . .
C8 C 0.7974(16) 0.5909(11) 0.7715(10) 0.065(3) Uani 1 1 d U . .
C7 C 0.6946(19) 0.5432(13) 0.8187(9) 0.065(3) Uani 1 1 d U . .
C20 C 0.7093(14) 0.9334(10) 0.9509(7) 0.046(3) Uani 1 1 d U . .
H20 H 0.7517 0.9389 0.9038 0.055 Uiso 1 1 calc R . .
C19 C 0.7850(15) 1.0117(11) 1.0266(8) 0.055(3) Uani 1 1 d U . .
H19 H 0.8795 1.0693 1.0302 0.066 Uiso 1 1 calc R . .
C14 C 0.2934(14) 0.6603(11) 0.9433(8) 0.050(3) Uani 1 1 d U . .
H14 H 0.2033 0.5996 0.9427 0.060 Uiso 1 1 calc R . .
C18 C 0.7244(17) 1.0066(12) 1.0965(8) 0.059(3) Uani 1 1 d U . .
H18 H 0.7767 1.0626 1.1466 0.071 Uiso 1 1 calc R . .
O3 O 0.2564(15) 0.7507(11) 0.6380(8) 0.107(4) Uani 1 1 d U . .
O4 O 0.0456(13) 0.7418(12) 0.5383(8) 0.103(4) Uani 1 1 d U . .
O5 O 0.3007(18) 0.8445(16) 0.5269(10) 0.139(5) Uani 1 1 d U . .
F1 F 0.0863(15) 0.9293(11) 0.6900(6) 0.118(3) Uani 1 1 d U . .
F2 F 0.3143(15) 1.0179(11) 0.6862(8) 0.146(5) Uani 1 1 d U . .
C22 C 0.186(2) 0.9511(15) 0.6367(10) 0.081(4) Uani 1 1 d U . .
C26 C 0.537(2) 0.3156(15) 0.6141(11) 0.103(6) Uani 1 1 d U . .
H26A H 0.5497 0.3400 0.5636 0.154 Uiso 1 1 calc R . .
H26B H 0.4298 0.2949 0.6179 0.154 Uiso 1 1 calc R . .
H26C H 0.5739 0.2439 0.6145 0.154 Uiso 1 1 calc R . .
C27 C 0.848(2) 0.515(2) 0.6190(14) 0.120(7) Uani 1 1 d U . .
H27A H 0.8748 0.5987 0.6117 0.180 Uiso 1 1 calc R . .
H27B H 0.7835 0.4585 0.5694 0.180 Uiso 1 1 calc R . .
H27C H 0.9397 0.4907 0.6308 0.180 Uiso 1 1 calc R . .
C24 C 0.707(2) 0.5894(19) 0.9084(9) 0.108(6) Uani 1 1 d U . .
H24A H 0.7635 0.5448 0.9367 0.162 Uiso 1 1 calc R . .
H24B H 0.6064 0.5763 0.9219 0.162 Uiso 1 1 calc R . .
H24C H 0.7609 0.6773 0.9252 0.162 Uiso 1 1 calc R . .
C25 C 0.450(2) 0.3562(17) 0.7895(14) 0.110(6) Uani 1 1 d U . .
H25A H 0.4837 0.2916 0.8079 0.164 Uiso 1 1 calc R . .
H25B H 0.3672 0.3188 0.7429 0.164 Uiso 1 1 calc R . .
H25C H 0.4151 0.4043 0.8336 0.164 Uiso 1 1 calc R . .
C23 C 0.9467(16) 0.7011(16) 0.8038(16) 0.135(8) Uani 1 1 d U . .
H23A H 0.9209 0.7765 0.8264 0.202 Uiso 1 1 calc R . .
H23B H 1.0002 0.7122 0.7589 0.202 Uiso 1 1 calc R . .
H23C H 1.0116 0.6830 0.8460 0.202 Uiso 1 1 calc R . .
O7 O 0.7804(11) 0.2644(9) 0.7956(7) 0.081(3) Uani 1 1 d U . .
O6 O 1.0190(15) 0.4171(13) 0.8093(14) 0.172(7) Uani 1 1 d U . .
C28 C 1.024(2) 0.2267(18) 0.8569(15) 0.100(4) Uani 1 1 d U . .
F4 F 1.1704(12) 0.2670(13) 0.8839(9) 0.133(4) Uani 1 1 d U . .
F6 F 0.982(3) 0.1147(15) 0.8267(18) 0.296(12) Uani 1 1 d U . .
F5 F 0.9823(18) 0.221(3) 0.9264(12) 0.236(9) Uani 1 1 d U . .
O8 O 0.974(3) 0.245(2) 0.7192(13) 0.212(8) Uani 1 1 d U . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 C8 2.075(13) . ?
Rh1 N3 2.102(9) . ?
Rh1 N1 2.106(9) . ?
Rh1 C11 2.161(12) . ?
Rh1 C9 2.168(12) . ?
Rh1 C10 2.169(12) . ?
Rh1 C7 2.174(13) . ?
Rh1 O1 2.178(8) . ?
S2 O4 1.395(11) . ?
S2 O3 1.406(12) . ?
S2 O5 1.414(13) . ?
S2 C22 1.780(16) . ?
S3 O6 1.224(12) . ?
S3 O7 1.360(10) . ?
S3 O8 1.67(2) . ?
S3 C28 1.700(17) . ?
N3 C1 1.315(14) . ?
N3 C5 1.342(13) . ?
N2 N1 1.254(11) . ?
N2 C5 1.397(13) . ?
N1 C12 1.445(13) . ?
O2 C13 1.345(13) . ?
C11 C7 1.41(2) . ?
C11 C10 1.436(18) . ?
C11 C25 1.485(19) . ?
F3 C22 1.281(18) . ?
C5 C4 1.361(15) . ?
C21 C20 1.410(15) . ?
C21 C16 1.412(15) . ?
C21 C12 1.423(15) . ?
C16 C15 1.399(17) . ?
C16 C17 1.429(16) . ?
C12 C13 1.378(15) . ?
C15 C14 1.343(17) . ?
C13 C14 1.404(15) . ?
C1 C2 1.378(17) . ?
C17 C18 1.344(18) . ?
C2 C3 1.350(18) . ?
C3 C4 1.381(17) . ?
C10 C9 1.392(19) . ?
C10 C26 1.475(19) . ?
C9 C8 1.42(2) . ?
C9 C27 1.51(2) . ?
C8 C7 1.38(2) . ?
C8 C23 1.550(19) . ?
C7 C24 1.47(2) . ?
C20 C19 1.374(16) . ?
C19 C18 1.364(18) . ?
F1 C22 1.37(2) . ?
F2 C22 1.298(19) . ?
C28 F6 1.21(2) . ?
C28 F5 1.28(2) . ?
C28 F4 1.290(19) . ?

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
C8 Rh1 N3 103.6(5) . . ?
C8 Rh1 N1 109.8(5) . . ?
N3 Rh1 N1 73.8(3) . . ?
C8 Rh1 C11 64.1(5) . . ?
N3 Rh1 C11 164.2(4) . . ?
N1 Rh1 C11 118.8(4) . . ?
C8 Rh1 C9 39.0(6) . . ?
N3 Rh1 C9 100.2(4) . . ?
N1 Rh1 C9 147.2(5) . . ?
C11 Rh1 C9 64.0(5) . . ?
C8 Rh1 C10 64.1(5) . . ?
N3 Rh1 C10 128.2(4) . . ?
N1 Rh1 C10 157.5(4) . . ?
C11 Rh1 C10 38.7(5) . . ?
C9 Rh1 C10 37.4(5) . . ?
C8 Rh1 C7 37.9(6) . . ?
N3 Rh1 C7 136.2(5) . . ?
N1 Rh1 C7 97.6(4) . . ?
C11 Rh1 C7 38.1(5) . . ?
C9 Rh1 C7 63.9(6) . . ?
C10 Rh1 C7 63.9(5) . . ?
C8 Rh1 O1 157.6(5) . . ?
N3 Rh1 O1 82.3(4) . . ?
N1 Rh1 O1 92.6(3) . . ?
C11 Rh1 O1 105.4(5) . . ?
C9 Rh1 O1 119.0(5) . . ?
C10 Rh1 O1 95.1(4) . . ?
C7 Rh1 O1 141.5(5) . . ?
O4 S2 O3 115.0(8) . . ?
O4 S2 O5 115.8(10) . . ?
O3 S2 O5 114.3(10) . . ?
O4 S2 C22 104.3(8) . . ?
O3 S2 C22 104.2(8) . . ?
O5 S2 C22 100.8(9) . . ?
O6 S3 O7 133.3(8) . . ?
O6 S3 O8 92.9(13) . . ?
O7 S3 O8 100.3(10) . . ?
O6 S3 C28 114.9(9) . . ?
O7 S3 C28 109.8(7) . . ?
O8 S3 C28 89.6(12) . . ?
C1 N3 C5 117.1(10) . . ?
C1 N3 Rh1 128.9(8) . . ?
C5 N3 Rh1 114.1(7) . . ?
N1 N2 C5 113.2(9) . . ?
N2 N1 C12 114.3(8) . . ?
N2 N1 Rh1 120.0(7) . . ?
C12 N1 Rh1 124.0(6) . . ?
C7 C11 C10 107.4(12) . . ?
C7 C11 C25 125.8(15) . . ?
C10 C11 C25 126.2(15) . . ?
C7 C11 Rh1 71.5(7) . . ?
C10 C11 Rh1 70.9(7) . . ?
C25 C11 Rh1 129.4(10) . . ?
N3 C5 C4 124.0(10) . . ?
N3 C5 N2 118.2(9) . . ?
C4 C5 N2 117.8(10) . . ?
C20 C21 C16 119.1(10) . . ?
C20 C21 C12 123.4(10) . . ?
C16 C21 C12 117.3(10) . . ?
C15 C16 C21 119.9(11) . . ?
C15 C16 C17 121.9(11) . . ?
C21 C16 C17 118.2(11) . . ?
C13 C12 C21 120.5(10) . . ?
C13 C12 N1 116.7(10) . . ?
C21 C12 N1 122.9(10) . . ?
C14 C15 C16 122.3(11) . . ?
O2 C13 C12 117.6(10) . . ?
O2 C13 C14 121.5(10) . . ?
C12 C13 C14 120.9(11) . . ?
N3 C1 C2 122.6(12) . . ?
C18 C17 C16 120.6(11) . . ?
C3 C2 C1 119.5(11) . . ?
C2 C3 C4 119.3(11) . . ?
C5 C4 C3 117.5(12) . . ?
C9 C10 C11 108.3(12) . . ?
C9 C10 C26 128.8(15) . . ?
C11 C10 C26 122.9(14) . . ?
C9 C10 Rh1 71.2(7) . . ?
C11 C10 Rh1 70.3(7) . . ?
C26 C10 Rh1 125.9(10) . . ?
C10 C9 C8 106.6(12) . . ?
C10 C9 C27 123.0(16) . . ?
C8 C9 C27 130.5(16) . . ?
C10 C9 Rh1 71.3(7) . . ?
C8 C9 Rh1 66.9(7) . . ?
C27 C9 Rh1 127.1(11) . . ?
C7 C8 C9 110.2(12) . . ?
C7 C8 C23 126.3(17) . . ?
C9 C8 C23 122.8(16) . . ?
C7 C8 Rh1 75.0(8) . . ?
C9 C8 Rh1 74.0(8) . . ?
C23 C8 Rh1 125.7(9) . . ?
C8 C7 C11 107.1(13) . . ?
C8 C7 C24 125.7(17) . . ?
C11 C7 C24 127.2(16) . . ?
C8 C7 Rh1 67.1(7) . . ?
C11 C7 Rh1 70.4(7) . . ?
C24 C7 Rh1 129.3(10) . . ?
C19 C20 C21 119.6(11) . . ?
C18 C19 C20 121.4(12) . . ?
C15 C14 C13 119.0(11) . . ?
C17 C18 C19 121.0(12) . . ?
F3 C22 F2 112.4(16) . . ?
F3 C22 F1 103.1(15) . . ?
F2 C22 F1 102.9(14) . . ?
F3 C22 S2 114.8(12) . . ?
F2 C22 S2 113.6(13) . . ?
F1 C22 S2 108.7(12) . . ?
F6 C28 F5 95(2) . . ?
F6 C28 F4 111.8(18) . . ?
F5 C28 F4 97.5(19) . . ?
F6 C28 S3 116.4(18) . . ?
F5 C28 S3 111.9(16) . . ?
F4 C28 S3 119.2(12) . . ?

_diffrn_measured_fraction_theta_max 0.959
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.959
_refine_diff_density_max         2.062
_refine_diff_density_min         -1.927
_refine_diff_density_rms         0.192
_database_code_depnum_ccdc_archive 'CCDC 979116'
