data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'Martin Albrecht'
_publ_contact_author_email       MARTIN.ALBRECHT@UCD.IE

_publ_section_title              
;
Rhodium-mediated functionalization of an unactivated C(alkyl)-H Bond
;
loop_
_publ_author_name
'Martin Albrecht'
'Anneke Kruger'
'Antonia Neels'

# Attachment 'new3a.cif'

data_3a
_database_code_depnum_ccdc_archive 'CCDC 743284'
#TrackingRef 'new3a.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H68 I4 N8 Rh2'
_chemical_formula_weight         1374.44

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
I I -0.4742 1.8119 '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'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pmnb

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

_cell_length_a                   15.2889(13)
_cell_length_b                   15.9079(13)
_cell_length_c                   20.8008(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5059.1(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    8000
_cell_measurement_theta_min      2.15
_cell_measurement_theta_max      25.75

_exptl_crystal_description       rod
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    1.805
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2664
_exptl_absorpt_coefficient_mu    3.128
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.358
_exptl_absorpt_correction_T_max  0.514
_exptl_absorpt_process_details   'MULscanABS, (PLATON03, Speck, 2003)'

_exptl_special_details           
;
The Rint is higher than 0.1 related to the relatively low
number of observed data (<50%). Nevertheless, the structure
was refined with acceptable standard uncertenties in atomic
positions, bond distances and angles.
;

_diffrn_ambient_temperature      173(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  'STOE IPDS'
_diffrn_measurement_method       'phi oscillation'
_diffrn_detector_area_resol_mean 0.81\%A
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            36742
_diffrn_reflns_av_R_equivalents  0.1149
_diffrn_reflns_av_sigmaI/netI    0.0882
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.34
_diffrn_reflns_theta_max         26.22
_reflns_number_total             5201
_reflns_number_gt                2511
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'EXPOSE (Stoe IPDS Software, 2000)'
_computing_cell_refinement       'CELL (Stoe IPDS Software, 2000)'
_computing_data_reduction        'INTEGRATE (Stoe IPDS Software, 2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'PLATON99 (Spek, 1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.1355P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0025(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         5201
_refine_ls_number_parameters     140
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1170
_refine_ls_R_factor_gt           0.0751
_refine_ls_wR_factor_ref         0.2086
_refine_ls_wR_factor_gt          0.1913
_refine_ls_goodness_of_fit_ref   0.844
_refine_ls_restrained_S_all      0.844
_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
C1 C 0.4386(11) 0.3148(12) 0.0554(9) 0.1055(19) Uani 1 1 d . . .
C2 C 0.4606(10) 0.3065(11) -0.0062(9) 0.1055(19) Uani 1 1 d . . .
H8 H 0.4328 0.2700 -0.0361 0.127 Uiso 1 1 calc R . .
C3 C 0.5545(11) 0.3992(12) 0.0321(10) 0.1055(19) Uani 1 1 d . . .
C4 C 0.4958(11) 0.4024(12) 0.1459(9) 0.1055(19) Uani 1 1 d . . .
H6A H 0.4673 0.4582 0.1481 0.127 Uiso 1 1 calc R . .
H6B H 0.5553 0.4070 0.1644 0.127 Uiso 1 1 calc R . .
C5 C 0.4413(8) 0.3361(8) 0.1828(6) 0.069(3) Uani 1 1 d . . .
H5A H 0.4050 0.3661 0.2156 0.083 Uiso 1 1 calc R . .
C6 C 0.4980(12) 0.2689(11) 0.2183(9) 0.1047(19) Uani 1 1 d . . .
H4A H 0.5576 0.2913 0.2253 0.126 Uiso 1 1 calc R . .
H4B H 0.4718 0.2565 0.2608 0.126 Uiso 1 1 calc R . .
C7 C 0.4377(11) 0.1777(12) 0.1331(9) 0.1047(19) Uani 1 1 d . . .
C8 C 0.4560(11) 0.1016(11) 0.1099(9) 0.1047(19) Uani 1 1 d . . .
H2 H 0.4254 0.0730 0.0767 0.126 Uiso 1 1 calc R . .
C9 C 0.5564(11) 0.1267(12) 0.1866(10) 0.1047(19) Uani 1 1 d . . .
C10 C 0.5688(11) 0.3677(12) -0.0870(9) 0.1055(19) Uani 1 1 d . . .
H14A H 0.6072 0.4185 -0.0893 0.127 Uiso 1 1 calc R . .
C11 C 0.5067(10) 0.3689(12) -0.1382(9) 0.1055(19) Uani 1 1 d . . .
H15A H 0.4524 0.3953 -0.1233 0.158 Uiso 1 1 calc R . .
H15B H 0.4945 0.3112 -0.1521 0.158 Uiso 1 1 calc R . .
H15C H 0.5305 0.4011 -0.1744 0.158 Uiso 1 1 calc R . .
C12 C 0.6245(11) 0.2867(11) -0.0957(9) 0.1055(19) Uani 1 1 d . . .
H16A H 0.6250 0.2706 -0.1412 0.158 Uiso 1 1 calc R . .
H16B H 0.5992 0.2411 -0.0702 0.158 Uiso 1 1 calc R . .
H16C H 0.6845 0.2974 -0.0814 0.158 Uiso 1 1 calc R . .
C13 C 0.6270(10) 0.4599(12) 0.0376(8) 0.1055(19) Uani 1 1 d . . .
H17A H 0.6322 0.4918 -0.0026 0.158 Uiso 1 1 calc R . .
H17B H 0.6817 0.4297 0.0458 0.158 Uiso 1 1 calc R . .
H17C H 0.6153 0.4987 0.0731 0.158 Uiso 1 1 calc R . .
C14 C 0.5707(11) -0.0117(11) 0.1359(9) 0.1047(19) Uani 1 1 d . . .
H10A H 0.6305 -0.0137 0.1552 0.126 Uiso 1 1 calc R . .
C15 C 0.5717(10) -0.0404(11) 0.0679(9) 0.1047(19) Uani 1 1 d . . .
H11A H 0.5116 -0.0434 0.0516 0.157 Uiso 1 1 calc R . .
H11B H 0.5988 -0.0962 0.0654 0.157 Uiso 1 1 calc R . .
H11C H 0.6054 -0.0007 0.0418 0.157 Uiso 1 1 calc R . .
C16 C 0.5158(11) -0.0743(11) 0.1623(9) 0.1047(19) Uani 1 1 d . . .
H12A H 0.4709 -0.0899 0.1308 0.157 Uiso 1 1 calc R . .
H12B H 0.4876 -0.0526 0.2012 0.157 Uiso 1 1 calc R . .
H12C H 0.5508 -0.1240 0.1731 0.157 Uiso 1 1 calc R . .
C17 C 0.6288(11) 0.1225(11) 0.2328(9) 0.1047(19) Uani 1 1 d . . .
H13A H 0.6843 0.1176 0.2096 0.157 Uiso 1 1 calc R . .
H13B H 0.6210 0.0735 0.2607 0.157 Uiso 1 1 calc R . .
H13C H 0.6293 0.1737 0.2590 0.157 Uiso 1 1 calc R . .
I1 I 0.2500 0.18724(8) 0.03375(6) 0.0662(4) Uani 1 2 d S . .
I2 I 0.2500 0.21953(8) 0.22123(6) 0.0703(4) Uani 1 2 d S . .
I3 I 0.2500 0.41587(8) 0.10865(6) 0.0655(4) Uani 1 2 d S . .
I4 I 0.7500 0.38361(14) 0.23565(12) 0.1297(8) Uani 1 2 d S . .
N1 N 0.5305(8) 0.3594(9) -0.0202(6) 0.093(4) Uani 1 1 d . . .
N2 N 0.4999(6) 0.3723(7) 0.0785(6) 0.072(3) Uani 1 1 d . . .
N3 N 0.5025(6) 0.1932(7) 0.1809(6) 0.074(3) Uani 1 1 d . . .
N4 N 0.5305(8) 0.0711(8) 0.1444(7) 0.091(4) Uani 1 1 d . . .
Rh1 Rh 0.35775(5) 0.27336(6) 0.12118(5) 0.0584(3) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.077(3) 0.111(5) 0.128(5) 0.004(4) 0.030(3) -0.007(3)
C2 0.077(3) 0.111(5) 0.128(5) 0.004(4) 0.030(3) -0.007(3)
C3 0.077(3) 0.111(5) 0.128(5) 0.004(4) 0.030(3) -0.007(3)
C4 0.077(3) 0.111(5) 0.128(5) 0.004(4) 0.030(3) -0.007(3)
C5 0.055(7) 0.076(9) 0.077(8) 0.001(7) -0.002(6) 0.002(6)
C6 0.086(4) 0.096(4) 0.132(5) 0.009(4) 0.002(4) 0.023(3)
C7 0.086(4) 0.096(4) 0.132(5) 0.009(4) 0.002(4) 0.023(3)
C8 0.086(4) 0.096(4) 0.132(5) 0.009(4) 0.002(4) 0.023(3)
C9 0.086(4) 0.096(4) 0.132(5) 0.009(4) 0.002(4) 0.023(3)
C10 0.077(3) 0.111(5) 0.128(5) 0.004(4) 0.030(3) -0.007(3)
C11 0.077(3) 0.111(5) 0.128(5) 0.004(4) 0.030(3) -0.007(3)
C12 0.077(3) 0.111(5) 0.128(5) 0.004(4) 0.030(3) -0.007(3)
C13 0.077(3) 0.111(5) 0.128(5) 0.004(4) 0.030(3) -0.007(3)
C14 0.086(4) 0.096(4) 0.132(5) 0.009(4) 0.002(4) 0.023(3)
C15 0.086(4) 0.096(4) 0.132(5) 0.009(4) 0.002(4) 0.023(3)
C16 0.086(4) 0.096(4) 0.132(5) 0.009(4) 0.002(4) 0.023(3)
C17 0.086(4) 0.096(4) 0.132(5) 0.009(4) 0.002(4) 0.023(3)
I1 0.0536(6) 0.0723(8) 0.0725(7) 0.0002(6) 0.000 0.000
I2 0.0558(6) 0.0810(8) 0.0741(8) 0.0120(6) 0.000 0.000
I3 0.0460(5) 0.0654(7) 0.0851(8) 0.0127(6) 0.000 0.000
I4 0.0616(8) 0.1357(16) 0.192(2) -0.0693(15) 0.000 0.000
N1 0.070(7) 0.119(11) 0.092(9) 0.015(8) 0.026(6) -0.011(7)
N2 0.039(5) 0.078(7) 0.100(8) 0.015(6) 0.015(5) 0.008(5)
N3 0.047(5) 0.079(8) 0.097(8) 0.005(6) 0.005(5) 0.011(5)
N4 0.081(8) 0.073(8) 0.119(10) 0.011(7) 0.021(7) 0.031(6)
Rh1 0.0399(4) 0.0629(6) 0.0724(6) 0.0070(5) 0.0007(4) 0.0014(4)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.33(2) . ?
C1 N2 1.39(2) . ?
C1 Rh1 1.958(16) . ?
C2 N1 1.391(19) . ?
C2 H8 0.9500 . ?
C3 N1 1.31(2) . ?
C3 N2 1.347(19) . ?
C3 C13 1.47(2) . ?
C4 N2 1.48(2) . ?
C4 C5 1.55(2) . ?
C4 H6A 0.9900 . ?
C4 H6B 0.9900 . ?
C5 C6 1.561(19) . ?
C5 Rh1 2.066(12) . ?
C5 H5A 1.0000 . ?
C6 N3 1.44(2) . ?
C6 H4A 0.9900 . ?
C6 H4B 0.9900 . ?
C7 C8 1.33(2) . ?
C7 N3 1.42(2) . ?
C7 Rh1 1.968(17) . ?
C8 N4 1.43(2) . ?
C8 H2 0.9500 . ?
C9 N4 1.31(2) . ?
C9 N3 1.346(19) . ?
C9 C17 1.47(2) . ?
C10 C11 1.43(2) . ?
C10 N1 1.51(2) . ?
C10 C12 1.55(2) . ?
C10 H14A 1.0000 . ?
C11 H15A 0.9800 . ?
C11 H15B 0.9800 . ?
C11 H15C 0.9800 . ?
C12 H16A 0.9800 . ?
C12 H16B 0.9800 . ?
C12 H16C 0.9800 . ?
C13 H17A 0.9800 . ?
C13 H17B 0.9800 . ?
C13 H17C 0.9800 . ?
C14 C16 1.41(2) . ?
C14 N4 1.464(19) . ?
C14 C15 1.49(2) . ?
C14 H10A 1.0000 . ?
C15 H11A 0.9800 . ?
C15 H11B 0.9800 . ?
C15 H11C 0.9800 . ?
C16 H12A 0.9800 . ?
C16 H12B 0.9800 . ?
C16 H12C 0.9800 . ?
C17 H13A 0.9800 . ?
C17 H13B 0.9800 . ?
C17 H13C 0.9800 . ?
I1 Rh1 2.8104(13) . ?
I1 Rh1 2.8104(13) 7_655 ?
I2 Rh1 2.7890(13) 7_655 ?
I2 Rh1 2.7890(13) . ?
I3 Rh1 2.8145(13) 7_655 ?
I3 Rh1 2.8145(13) . ?

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
C2 C1 N2 103.1(14) . . ?
C2 C1 Rh1 143.0(16) . . ?
N2 C1 Rh1 113.8(13) . . ?
C1 C2 N1 109.6(17) . . ?
C1 C2 H8 125.2 . . ?
N1 C2 H8 125.2 . . ?
N1 C3 N2 105.5(14) . . ?
N1 C3 C13 126.2(16) . . ?
N2 C3 C13 128.2(18) . . ?
N2 C4 C5 105.7(13) . . ?
N2 C4 H6A 110.6 . . ?
C5 C4 H6A 110.6 . . ?
N2 C4 H6B 110.6 . . ?
C5 C4 H6B 110.6 . . ?
H6A C4 H6B 108.7 . . ?
C4 C5 C6 113.7(12) . . ?
C4 C5 Rh1 110.8(10) . . ?
C6 C5 Rh1 107.8(10) . . ?
C4 C5 H5A 108.1 . . ?
C6 C5 H5A 108.1 . . ?
Rh1 C5 H5A 108.1 . . ?
N3 C6 C5 110.1(13) . . ?
N3 C6 H4A 109.6 . . ?
C5 C6 H4A 109.6 . . ?
N3 C6 H4B 109.6 . . ?
C5 C6 H4B 109.6 . . ?
H4A C6 H4B 108.2 . . ?
C8 C7 N3 105.3(15) . . ?
C8 C7 Rh1 141.9(16) . . ?
N3 C7 Rh1 112.7(12) . . ?
C7 C8 N4 107.0(17) . . ?
C7 C8 H2 126.5 . . ?
N4 C8 H2 126.5 . . ?
N4 C9 N3 106.7(15) . . ?
N4 C9 C17 129.6(16) . . ?
N3 C9 C17 123.7(18) . . ?
C11 C10 N1 115.4(13) . . ?
C11 C10 C12 106.8(16) . . ?
N1 C10 C12 104.3(14) . . ?
C11 C10 H14A 110.0 . . ?
N1 C10 H14A 110.0 . . ?
C12 C10 H14A 110.0 . . ?
C10 C11 H15A 109.5 . . ?
C10 C11 H15B 109.5 . . ?
H15A C11 H15B 109.5 . . ?
C10 C11 H15C 109.5 . . ?
H15A C11 H15C 109.5 . . ?
H15B C11 H15C 109.5 . . ?
C10 C12 H16A 109.5 . . ?
C10 C12 H16B 109.5 . . ?
H16A C12 H16B 109.5 . . ?
C10 C12 H16C 109.5 . . ?
H16A C12 H16C 109.5 . . ?
H16B C12 H16C 109.5 . . ?
C3 C13 H17A 109.5 . . ?
C3 C13 H17B 109.5 . . ?
H17A C13 H17B 109.5 . . ?
C3 C13 H17C 109.5 . . ?
H17A C13 H17C 109.5 . . ?
H17B C13 H17C 109.5 . . ?
C16 C14 N4 109.7(14) . . ?
C16 C14 C15 99.1(16) . . ?
N4 C14 C15 113.4(14) . . ?
C16 C14 H10A 111.3 . . ?
N4 C14 H10A 111.3 . . ?
C15 C14 H10A 111.3 . . ?
C14 C15 H11A 109.5 . . ?
C14 C15 H11B 109.5 . . ?
H11A C15 H11B 109.5 . . ?
C14 C15 H11C 109.5 . . ?
H11A C15 H11C 109.5 . . ?
H11B C15 H11C 109.5 . . ?
C14 C16 H12A 109.5 . . ?
C14 C16 H12B 109.5 . . ?
H12A C16 H12B 109.5 . . ?
C14 C16 H12C 109.5 . . ?
H12A C16 H12C 109.5 . . ?
H12B C16 H12C 109.5 . . ?
C9 C17 H13A 109.5 . . ?
C9 C17 H13B 109.5 . . ?
H13A C17 H13B 109.5 . . ?
C9 C17 H13C 109.5 . . ?
H13A C17 H13C 109.5 . . ?
H13B C17 H13C 109.5 . . ?
Rh1 I1 Rh1 71.77(5) . 7_655 ?
Rh1 I2 Rh1 72.41(5) 7_655 . ?
Rh1 I3 Rh1 71.65(5) 7_655 . ?
C3 N1 C2 109.5(13) . . ?
C3 N1 C10 127.6(14) . . ?
C2 N1 C10 122.9(15) . . ?
C3 N2 C1 112.2(14) . . ?
C3 N2 C4 127.0(14) . . ?
C1 N2 C4 120.6(12) . . ?
C9 N3 C7 110.5(14) . . ?
C9 N3 C6 129.9(14) . . ?
C7 N3 C6 119.3(12) . . ?
C9 N4 C8 110.4(14) . . ?
C9 N4 C14 124.3(15) . . ?
C8 N4 C14 125.3(16) . . ?
C1 Rh1 C7 87.5(8) . . ?
C1 Rh1 C5 83.1(7) . . ?
C7 Rh1 C5 84.9(7) . . ?
C1 Rh1 I2 176.0(6) . . ?
C7 Rh1 I2 92.0(5) . . ?
C5 Rh1 I2 92.9(4) . . ?
C1 Rh1 I1 94.7(6) . . ?
C7 Rh1 I1 94.0(6) . . ?
C5 Rh1 I1 177.6(4) . . ?
I2 Rh1 I1 89.25(4) . . ?
C1 Rh1 I3 91.9(5) . . ?
C7 Rh1 I3 176.6(6) . . ?
C5 Rh1 I3 91.7(4) . . ?
I2 Rh1 I3 88.32(4) . . ?
I1 Rh1 I3 89.41(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
N2 C1 C2 N1 -2(2) . . . . ?
Rh1 C1 C2 N1 -178.9(18) . . . . ?
N2 C4 C5 C6 96.1(15) . . . . ?
N2 C4 C5 Rh1 -25.5(14) . . . . ?
C4 C5 C6 N3 -99.3(16) . . . . ?
Rh1 C5 C6 N3 24.0(15) . . . . ?
N3 C7 C8 N4 1.0(19) . . . . ?
Rh1 C7 C8 N4 177.4(17) . . . . ?
N2 C3 N1 C2 -0.6(19) . . . . ?
C13 C3 N1 C2 179.1(17) . . . . ?
N2 C3 N1 C10 178.5(14) . . . . ?
C13 C3 N1 C10 -2(3) . . . . ?
C1 C2 N1 C3 2(2) . . . . ?
C1 C2 N1 C10 -177.3(16) . . . . ?
C11 C10 N1 C3 -138.7(19) . . . . ?
C12 C10 N1 C3 105(2) . . . . ?
C11 C10 N1 C2 40(2) . . . . ?
C12 C10 N1 C2 -76.5(19) . . . . ?
N1 C3 N2 C1 -1(2) . . . . ?
C13 C3 N2 C1 179.6(18) . . . . ?
N1 C3 N2 C4 -175.7(14) . . . . ?
C13 C3 N2 C4 5(3) . . . . ?
C2 C1 N2 C3 2(2) . . . . ?
Rh1 C1 N2 C3 179.7(11) . . . . ?
C2 C1 N2 C4 177.1(14) . . . . ?
Rh1 C1 N2 C4 -5.1(19) . . . . ?
C5 C4 N2 C3 -165.0(14) . . . . ?
C5 C4 N2 C1 20.6(19) . . . . ?
N4 C9 N3 C7 1.2(19) . . . . ?
C17 C9 N3 C7 -178.6(16) . . . . ?
N4 C9 N3 C6 175.3(15) . . . . ?
C17 C9 N3 C6 -5(3) . . . . ?
C8 C7 N3 C9 -1(2) . . . . ?
Rh1 C7 N3 C9 -179.0(12) . . . . ?
C8 C7 N3 C6 -176.2(15) . . . . ?
Rh1 C7 N3 C6 6.2(19) . . . . ?
C5 C6 N3 C9 165.7(15) . . . . ?
C5 C6 N3 C7 -21(2) . . . . ?
N3 C9 N4 C8 -1(2) . . . . ?
C17 C9 N4 C8 179.2(18) . . . . ?
N3 C9 N4 C14 -178.6(14) . . . . ?
C17 C9 N4 C14 1(3) . . . . ?
C7 C8 N4 C9 0(2) . . . . ?
C7 C8 N4 C14 177.7(16) . . . . ?
C16 C14 N4 C9 105(2) . . . . ?
C15 C14 N4 C9 -144.8(17) . . . . ?
C16 C14 N4 C8 -72(2) . . . . ?
C15 C14 N4 C8 37(2) . . . . ?
C2 C1 Rh1 C7 83(3) . . . . ?
N2 C1 Rh1 C7 -94.0(13) . . . . ?
C2 C1 Rh1 C5 168(3) . . . . ?
N2 C1 Rh1 C5 -8.8(12) . . . . ?
C2 C1 Rh1 I2 166(6) . . . . ?
N2 C1 Rh1 I2 -10(9) . . . . ?
C2 C1 Rh1 I1 -11(3) . . . . ?
N2 C1 Rh1 I1 172.3(11) . . . . ?
C2 C1 Rh1 I3 -101(2) . . . . ?
N2 C1 Rh1 I3 82.7(12) . . . . ?
C8 C7 Rh1 C1 -86(2) . . . . ?
N3 C7 Rh1 C1 90.4(13) . . . . ?
C8 C7 Rh1 C5 -169(2) . . . . ?
N3 C7 Rh1 C5 7.1(11) . . . . ?
C8 C7 Rh1 I2 98(2) . . . . ?
N3 C7 Rh1 I2 -85.6(11) . . . . ?
C8 C7 Rh1 I1 9(2) . . . . ?
N3 C7 Rh1 I1 -175.0(11) . . . . ?
C8 C7 Rh1 I3 -166(7) . . . . ?
N3 C7 Rh1 I3 10(10) . . . . ?
C4 C5 Rh1 C1 19.9(11) . . . . ?
C6 C5 Rh1 C1 -105.2(11) . . . . ?
C4 C5 Rh1 C7 107.9(11) . . . . ?
C6 C5 Rh1 C7 -17.1(11) . . . . ?
C4 C5 Rh1 I2 -160.3(9) . . . . ?
C6 C5 Rh1 I2 74.7(9) . . . . ?
C4 C5 Rh1 I1 46(9) . . . . ?
C6 C5 Rh1 I1 -79(9) . . . . ?
C4 C5 Rh1 I3 -71.9(10) . . . . ?
C6 C5 Rh1 I3 163.1(9) . . . . ?
Rh1 I2 Rh1 C1 139(8) 7_655 . . . ?
Rh1 I2 Rh1 C7 -138.1(6) 7_655 . . . ?
Rh1 I2 Rh1 C5 136.9(4) 7_655 . . . ?
Rh1 I2 Rh1 I1 -44.20(4) 7_655 . . . ?
Rh1 I2 Rh1 I3 45.23(4) 7_655 . . . ?
Rh1 I1 Rh1 C1 -136.2(5) 7_655 . . . ?
Rh1 I1 Rh1 C7 136.0(5) 7_655 . . . ?
Rh1 I1 Rh1 C5 -163(9) 7_655 . . . ?
Rh1 I1 Rh1 I2 43.97(4) 7_655 . . . ?
Rh1 I1 Rh1 I3 -44.36(4) 7_655 . . . ?
Rh1 I3 Rh1 C1 139.0(6) 7_655 . . . ?
Rh1 I3 Rh1 C7 -141(9) 7_655 . . . ?
Rh1 I3 Rh1 C5 -137.8(4) 7_655 . . . ?
Rh1 I3 Rh1 I2 -44.96(4) 7_655 . . . ?
Rh1 I3 Rh1 I1 44.31(4) 7_655 . . . ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        26.22
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         1.850
_refine_diff_density_min         -1.722
_refine_diff_density_rms         0.260

# start Validation Reply Form
_vrf_PLAT601_2a                  
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of .
232.00 A**3 RESPONSE:Pronounced disorder was found in
co-crystallised hexane molecules. Therefore, the SQUEEZE
option in PLATON was used to calculate the potential solvent
accessible volume; 1320 \%A3 were calculated containing about
247 electrons. Four hexane molecules (4 x 50 electrons) per
unit cell were included in all calculations.
;
# end Validation Reply Form

# end Validation Reply Form

#################################################END

data_complex3a
_database_code_depnum_ccdc_archive 'CCDC 743285'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H33 I2 N6 Rh'
_chemical_formula_weight         726.24

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'
I I -0.4742 1.8119 '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'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pca21

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

_cell_length_a                   13.2142(12)
_cell_length_b                   13.7680(13)
_cell_length_c                   15.0238(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2733.3(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    8000
_cell_measurement_theta_min      2.15
_cell_measurement_theta_max      25.75

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    1.765
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1408
_exptl_absorpt_coefficient_mu    2.902
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.492
_exptl_absorpt_correction_T_max  0.554
_exptl_absorpt_process_details   'MULscanABS, (PLATON03, Speck, 2003)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(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  'STOE IPDS'
_diffrn_measurement_method       'phi oscillation'
_diffrn_detector_area_resol_mean 0.81\%A
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            18938
_diffrn_reflns_av_R_equivalents  0.0593
_diffrn_reflns_av_sigmaI/netI    0.0543
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.14
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4629
_reflns_number_gt                3878
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'EXPOSE (Stoe IPDS Software, 2000)'
_computing_cell_refinement       'CELL (Stoe IPDS Software, 2000)'
_computing_data_reduction        'INTEGRATE (Stoe IPDS Software, 2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'PLATON99 (Spek, 1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0532P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.08(3)
_refine_ls_number_reflns         4629
_refine_ls_number_parameters     255
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0374
_refine_ls_wR_factor_ref         0.0875
_refine_ls_wR_factor_gt          0.0846
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_restrained_S_all      0.985
_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
C1 C 0.6128(5) 0.3554(6) 0.2833(6) 0.0247(18) Uani 1 1 d . . .
C2 C 0.6043(6) 0.3180(6) 0.3652(6) 0.0270(19) Uani 1 1 d . . .
H2 H 0.6562 0.3173 0.4089 0.032 Uiso 1 1 calc R . .
C3 C 0.4540(5) 0.2944(5) 0.3031(5) 0.0245(19) Uani 1 1 d . . .
C4 C 0.4954(6) 0.3728(7) 0.1557(6) 0.035(2) Uani 1 1 d . . .
H4A H 0.4618 0.4369 0.1593 0.041 Uiso 1 1 calc R . .
H4B H 0.4496 0.3274 0.1243 0.041 Uiso 1 1 calc R . .
C5 C 0.5967(6) 0.3820(6) 0.1043(6) 0.0279(19) Uani 1 1 d . . .
H5 H 0.5918 0.4375 0.0616 0.034 Uiso 1 1 calc R . .
C6 C 0.6241(6) 0.2911(6) 0.0537(6) 0.032(2) Uani 1 1 d . . .
H6A H 0.5619 0.2546 0.0382 0.038 Uiso 1 1 calc R . .
H6B H 0.6593 0.3085 -0.0022 0.038 Uiso 1 1 calc R . .
C7 C 0.7454(5) 0.2761(5) 0.1771(5) 0.0225(18) Uani 1 1 d . . .
C8 C 0.7956(5) 0.2016(5) 0.2157(6) 0.029(2) Uani 1 1 d . . .
H8 H 0.8410 0.2076 0.2644 0.034 Uiso 1 1 calc R . .
C9 C 0.7056(6) 0.1353(6) 0.1064(6) 0.0301(19) Uani 1 1 d . . .
C10 C 0.4643(9) 0.2437(8) 0.4612(8) 0.0583(16) Uani 1 1 d . . .
H10 H 0.4028 0.2052 0.4452 0.070 Uiso 1 1 calc R . .
C11 C 0.5359(8) 0.1743(8) 0.5051(9) 0.0583(16) Uani 1 1 d . . .
H11A H 0.5495 0.1197 0.4650 0.087 Uiso 1 1 calc R . .
H11B H 0.5056 0.1500 0.5603 0.087 Uiso 1 1 calc R . .
H11C H 0.5995 0.2078 0.5188 0.087 Uiso 1 1 calc R . .
C12 C 0.4282(8) 0.3271(8) 0.5159(8) 0.0583(16) Uani 1 1 d . . .
H12A H 0.4856 0.3563 0.5472 0.087 Uiso 1 1 calc R . .
H12B H 0.3784 0.3040 0.5593 0.087 Uiso 1 1 calc R . .
H12C H 0.3968 0.3757 0.4771 0.087 Uiso 1 1 calc R . .
C13 C 0.3453(6) 0.2751(7) 0.2852(7) 0.037(2) Uani 1 1 d . . .
H13A H 0.3160 0.2392 0.3353 0.056 Uiso 1 1 calc R . .
H13B H 0.3387 0.2365 0.2307 0.056 Uiso 1 1 calc R . .
H13C H 0.3094 0.3369 0.2778 0.056 Uiso 1 1 calc R . .
C14 C 0.7986(7) 0.0184(6) 0.2030(9) 0.045(2) Uani 1 1 d . . .
H14 H 0.7878 -0.0280 0.1527 0.054 Uiso 1 1 calc R . .
C15 C 0.9082(8) 0.0134(8) 0.2319(9) 0.0592(18) Uani 1 1 d . . .
H15A H 0.9521 0.0258 0.1806 0.089 Uiso 1 1 calc R . .
H15B H 0.9226 -0.0513 0.2559 0.089 Uiso 1 1 calc R . .
H15C H 0.9208 0.0624 0.2779 0.089 Uiso 1 1 calc R . .
C16 C 0.7263(8) -0.0085(8) 0.2799(9) 0.0592(18) Uani 1 1 d . . .
H16A H 0.7413 0.0321 0.3318 0.089 Uiso 1 1 calc R . .
H16B H 0.7355 -0.0770 0.2955 0.089 Uiso 1 1 calc R . .
H16C H 0.6562 0.0024 0.2612 0.089 Uiso 1 1 calc R . .
C17 C 0.6578(8) 0.0649(7) 0.0437(9) 0.0592(18) Uani 1 1 d . . .
H17A H 0.5945 0.0407 0.0694 0.089 Uiso 1 1 calc R . .
H17B H 0.7040 0.0104 0.0334 0.089 Uiso 1 1 calc R . .
H17C H 0.6436 0.0975 -0.0130 0.089 Uiso 1 1 calc R . .
C18 C 0.8314(5) 0.5040(6) 0.0312(5) 0.0251(17) Uani 1 1 d . . .
C19 C 0.8735(6) 0.5513(6) -0.0452(7) 0.032(2) Uani 1 1 d . . .
H19A H 0.8338 0.5343 -0.0981 0.048 Uiso 1 1 calc R . .
H19B H 0.9437 0.5300 -0.0535 0.048 Uiso 1 1 calc R . .
H19C H 0.8719 0.6218 -0.0365 0.048 Uiso 1 1 calc R . .
C20 C 0.6191(6) 0.6274(6) 0.2365(6) 0.0297(19) Uani 1 1 d . . .
C21 C 0.5796(7) 0.7221(6) 0.2547(8) 0.047(3) Uani 1 1 d . . .
H21A H 0.5877 0.7368 0.3182 0.070 Uiso 1 1 calc R . .
H21B H 0.5076 0.7241 0.2391 0.070 Uiso 1 1 calc R . .
H21C H 0.6164 0.7704 0.2194 0.070 Uiso 1 1 calc R . .
I1 I 0.85913(3) 0.43950(4) 0.32662(4) 0.02880(13) Uani 1 1 d . . .
I2 I 0.33807(5) 0.16692(5) 0.00615(5) 0.0543(2) Uani 1 1 d . . .
N1 N 0.5066(5) 0.2799(5) 0.3765(5) 0.0291(15) Uani 1 1 d . . .
N2 N 0.5166(4) 0.3368(5) 0.2446(5) 0.0252(15) Uani 1 1 d . . .
N3 N 0.6900(5) 0.2306(5) 0.1089(5) 0.0263(15) Uani 1 1 d . . .
N4 N 0.7710(5) 0.1157(5) 0.1738(5) 0.0341(19) Uani 1 1 d . . .
N5 N 0.7979(5) 0.4681(5) 0.0925(5) 0.0281(16) Uani 1 1 d . . .
N6 N 0.6529(4) 0.5524(5) 0.2208(5) 0.0259(17) Uani 1 1 d . . .
Rh1 Rh 0.70929(4) 0.41199(4) 0.19796(5) 0.02102(13) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.017(3) 0.032(5) 0.025(5) -0.007(4) -0.006(3) 0.003(3)
C2 0.022(4) 0.040(5) 0.019(5) 0.008(4) 0.000(3) -0.005(3)
C3 0.015(3) 0.027(4) 0.031(6) 0.001(3) 0.001(3) -0.003(3)
C4 0.032(4) 0.052(5) 0.019(5) 0.005(4) -0.008(4) 0.003(4)
C5 0.022(4) 0.039(5) 0.023(5) 0.006(4) 0.001(3) 0.002(3)
C6 0.022(4) 0.046(5) 0.027(6) 0.006(4) -0.005(3) 0.003(3)
C7 0.017(3) 0.035(4) 0.016(5) -0.006(3) 0.002(3) -0.006(3)
C8 0.021(4) 0.028(4) 0.037(6) -0.004(3) -0.001(3) 0.000(3)
C9 0.023(4) 0.039(5) 0.028(5) -0.005(4) 0.000(4) 0.002(3)
C10 0.060(4) 0.068(4) 0.047(4) 0.019(3) 0.015(3) -0.007(3)
C11 0.060(4) 0.068(4) 0.047(4) 0.019(3) 0.015(3) -0.007(3)
C12 0.060(4) 0.068(4) 0.047(4) 0.019(3) 0.015(3) -0.007(3)
C13 0.017(4) 0.045(5) 0.049(6) 0.001(4) 0.004(4) -0.005(3)
C14 0.045(5) 0.033(4) 0.057(7) 0.005(5) 0.003(5) 0.003(4)
C15 0.053(4) 0.045(3) 0.080(5) 0.005(3) -0.008(3) 0.005(3)
C16 0.053(4) 0.045(3) 0.080(5) 0.005(3) -0.008(3) 0.005(3)
C17 0.053(4) 0.045(3) 0.080(5) 0.005(3) -0.008(3) 0.005(3)
C18 0.026(4) 0.038(5) 0.011(5) 0.005(3) -0.001(3) -0.003(3)
C19 0.029(4) 0.037(5) 0.029(6) 0.004(4) 0.003(4) -0.007(4)
C20 0.034(4) 0.028(5) 0.027(5) 0.005(4) -0.003(4) 0.003(4)
C21 0.044(5) 0.032(5) 0.065(8) -0.008(5) -0.008(5) 0.006(4)
I1 0.0209(2) 0.0397(3) 0.0258(3) 0.0020(3) -0.0044(2) -0.0022(2)
I2 0.0598(4) 0.0497(4) 0.0533(5) 0.0144(3) -0.0224(3) -0.0216(3)
N1 0.021(3) 0.041(4) 0.026(4) 0.002(3) 0.002(3) -0.002(3)
N2 0.020(3) 0.039(4) 0.017(4) 0.002(3) -0.003(3) 0.001(3)
N3 0.020(3) 0.033(4) 0.026(4) -0.006(3) 0.003(3) 0.003(3)
N4 0.030(4) 0.030(4) 0.041(6) -0.002(3) 0.003(3) 0.006(3)
N5 0.020(3) 0.035(4) 0.029(5) -0.007(3) -0.004(3) -0.001(3)
N6 0.017(3) 0.033(4) 0.027(5) 0.007(3) -0.004(2) -0.005(3)
Rh1 0.0174(2) 0.0276(3) 0.0180(3) 0.0017(3) -0.0008(3) -0.0015(2)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.339(12) . ?
C1 N2 1.421(10) . ?
C1 Rh1 1.969(9) . ?
C2 N1 1.404(10) . ?
C2 H2 0.9500 . ?
C3 N1 1.319(10) . ?
C3 N2 1.340(10) . ?
C3 C13 1.485(10) . ?
C4 N2 1.452(11) . ?
C4 C5 1.551(12) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.509(12) . ?
C5 Rh1 2.089(8) . ?
C5 H5 1.0000 . ?
C6 N3 1.463(10) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.352(11) . ?
C7 N3 1.406(10) . ?
C7 Rh1 1.957(8) . ?
C8 N4 1.379(10) . ?
C8 H8 0.9500 . ?
C9 N3 1.329(11) . ?
C9 N4 1.358(11) . ?
C9 C17 1.492(14) . ?
C10 N1 1.476(12) . ?
C10 C12 1.490(16) . ?
C10 C11 1.498(16) . ?
C10 H10 1.0000 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 N4 1.456(11) . ?
C14 C15 1.514(14) . ?
C14 C16 1.544(16) . ?
C14 H14 1.0000 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 N5 1.135(10) . ?
C18 C19 1.432(12) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 N6 1.150(10) . ?
C20 C21 1.431(12) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
I1 Rh1 2.7929(8) . ?
N5 Rh1 2.116(7) . ?
N6 Rh1 2.100(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 N2 103.4(7) . . ?
C2 C1 Rh1 143.7(6) . . ?
N2 C1 Rh1 112.6(6) . . ?
C1 C2 N1 109.4(7) . . ?
C1 C2 H2 125.3 . . ?
N1 C2 H2 125.3 . . ?
N1 C3 N2 106.8(6) . . ?
N1 C3 C13 129.3(7) . . ?
N2 C3 C13 123.8(7) . . ?
N2 C4 C5 108.7(7) . . ?
N2 C4 H4A 110.0 . . ?
C5 C4 H4A 110.0 . . ?
N2 C4 H4B 110.0 . . ?
C5 C4 H4B 110.0 . . ?
H4A C4 H4B 108.3 . . ?
C6 C5 C4 113.0(7) . . ?
C6 C5 Rh1 109.4(5) . . ?
C4 C5 Rh1 107.1(6) . . ?
C6 C5 H5 109.1 . . ?
C4 C5 H5 109.1 . . ?
Rh1 C5 H5 109.1 . . ?
N3 C6 C5 109.2(7) . . ?
N3 C6 H6A 109.8 . . ?
C5 C6 H6A 109.8 . . ?
N3 C6 H6B 109.8 . . ?
C5 C6 H6B 109.8 . . ?
H6A C6 H6B 108.3 . . ?
C8 C7 N3 103.3(7) . . ?
C8 C7 Rh1 140.9(6) . . ?
N3 C7 Rh1 114.5(5) . . ?
C7 C8 N4 109.8(7) . . ?
C7 C8 H8 125.1 . . ?
N4 C8 H8 125.1 . . ?
N3 C9 N4 105.9(7) . . ?
N3 C9 C17 126.4(8) . . ?
N4 C9 C17 127.7(8) . . ?
N1 C10 C12 109.7(9) . . ?
N1 C10 C11 110.9(9) . . ?
C12 C10 C11 116.8(11) . . ?
N1 C10 H10 106.3 . . ?
C12 C10 H10 106.3 . . ?
C11 C10 H10 106.3 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C3 C13 H13A 109.5 . . ?
C3 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C3 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N4 C14 C15 111.6(7) . . ?
N4 C14 C16 107.0(8) . . ?
C15 C14 C16 111.5(10) . . ?
N4 C14 H14 108.9 . . ?
C15 C14 H14 108.9 . . ?
C16 C14 H14 108.9 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C9 C17 H17A 109.5 . . ?
C9 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C9 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N5 C18 C19 178.8(9) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N6 C20 C21 178.3(9) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C3 N1 C2 109.1(7) . . ?
C3 N1 C10 124.9(7) . . ?
C2 N1 C10 125.3(8) . . ?
C3 N2 C1 111.3(7) . . ?
C3 N2 C4 129.2(7) . . ?
C1 N2 C4 119.2(7) . . ?
C9 N3 C7 112.3(7) . . ?
C9 N3 C6 129.6(7) . . ?
C7 N3 C6 118.1(7) . . ?
C9 N4 C8 108.6(7) . . ?
C9 N4 C14 124.6(8) . . ?
C8 N4 C14 126.3(8) . . ?
C18 N5 Rh1 169.2(6) . . ?
C20 N6 Rh1 176.7(7) . . ?
C7 Rh1 C1 83.3(3) . . ?
C7 Rh1 C5 82.9(3) . . ?
C1 Rh1 C5 84.2(3) . . ?
C7 Rh1 N6 173.3(3) . . ?
C1 Rh1 N6 91.6(3) . . ?
C5 Rh1 N6 92.3(3) . . ?
C7 Rh1 N5 95.4(3) . . ?
C1 Rh1 N5 172.0(3) . . ?
C5 Rh1 N5 87.8(3) . . ?
N6 Rh1 N5 89.0(3) . . ?
C7 Rh1 I1 93.9(2) . . ?
C1 Rh1 I1 93.6(2) . . ?
C5 Rh1 I1 176.3(2) . . ?
N6 Rh1 I1 90.78(18) . . ?
N5 Rh1 I1 94.38(18) . . ?

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
N2 C1 C2 N1 -1.0(8) . . . . ?
Rh1 C1 C2 N1 -172.6(8) . . . . ?
N2 C4 C5 C6 90.6(9) . . . . ?
N2 C4 C5 Rh1 -30.0(8) . . . . ?
C4 C5 C6 N3 -93.7(8) . . . . ?
Rh1 C5 C6 N3 25.6(8) . . . . ?
N3 C7 C8 N4 -0.6(9) . . . . ?
Rh1 C7 C8 N4 165.1(7) . . . . ?
N2 C3 N1 C2 2.5(9) . . . . ?
C13 C3 N1 C2 -174.1(8) . . . . ?
N2 C3 N1 C10 173.6(8) . . . . ?
C13 C3 N1 C10 -3.0(14) . . . . ?
C1 C2 N1 C3 -0.9(9) . . . . ?
C1 C2 N1 C10 -171.9(8) . . . . ?
C12 C10 N1 C3 -88.8(12) . . . . ?
C11 C10 N1 C3 140.8(10) . . . . ?
C12 C10 N1 C2 80.9(11) . . . . ?
C11 C10 N1 C2 -49.5(13) . . . . ?
N1 C3 N2 C1 -3.2(9) . . . . ?
C13 C3 N2 C1 173.6(7) . . . . ?
N1 C3 N2 C4 -176.3(8) . . . . ?
C13 C3 N2 C4 0.5(13) . . . . ?
C2 C1 N2 C3 2.6(9) . . . . ?
Rh1 C1 N2 C3 177.3(5) . . . . ?
C2 C1 N2 C4 176.5(7) . . . . ?
Rh1 C1 N2 C4 -8.9(9) . . . . ?
C5 C4 N2 C3 -160.7(8) . . . . ?
C5 C4 N2 C1 26.7(10) . . . . ?
N4 C9 N3 C7 0.6(9) . . . . ?
C17 C9 N3 C7 179.0(9) . . . . ?
N4 C9 N3 C6 -178.0(8) . . . . ?
C17 C9 N3 C6 0.3(14) . . . . ?
C8 C7 N3 C9 0.0(9) . . . . ?
Rh1 C7 N3 C9 -170.2(5) . . . . ?
C8 C7 N3 C6 178.8(7) . . . . ?
Rh1 C7 N3 C6 8.6(9) . . . . ?
C5 C6 N3 C9 155.4(8) . . . . ?
C5 C6 N3 C7 -23.2(10) . . . . ?
N3 C9 N4 C8 -1.0(9) . . . . ?
C17 C9 N4 C8 -179.3(9) . . . . ?
N3 C9 N4 C14 171.4(8) . . . . ?
C17 C9 N4 C14 -6.9(14) . . . . ?
C7 C8 N4 C9 1.0(9) . . . . ?
C7 C8 N4 C14 -171.2(8) . . . . ?
C15 C14 N4 C9 144.5(9) . . . . ?
C16 C14 N4 C9 -93.3(11) . . . . ?
C15 C14 N4 C8 -44.4(14) . . . . ?
C16 C14 N4 C8 77.8(10) . . . . ?
C19 C18 N5 Rh1 75(41) . . . . ?
C21 C20 N6 Rh1 162(27) . . . . ?
C8 C7 Rh1 C1 -74.1(9) . . . . ?
N3 C7 Rh1 C1 90.6(6) . . . . ?
C8 C7 Rh1 C5 -159.0(9) . . . . ?
N3 C7 Rh1 C5 5.6(5) . . . . ?
C8 C7 Rh1 N6 -115(2) . . . . ?
N3 C7 Rh1 N6 50(3) . . . . ?
C8 C7 Rh1 N5 113.8(9) . . . . ?
N3 C7 Rh1 N5 -81.5(5) . . . . ?
C8 C7 Rh1 I1 19.1(9) . . . . ?
N3 C7 Rh1 I1 -176.3(5) . . . . ?
C2 C1 Rh1 C7 79.6(11) . . . . ?
N2 C1 Rh1 C7 -91.6(6) . . . . ?
C2 C1 Rh1 C5 163.1(11) . . . . ?
N2 C1 Rh1 C5 -8.0(5) . . . . ?
C2 C1 Rh1 N6 -104.8(11) . . . . ?
N2 C1 Rh1 N6 84.1(5) . . . . ?
C2 C1 Rh1 N5 160.9(17) . . . . ?
N2 C1 Rh1 N5 -10(2) . . . . ?
C2 C1 Rh1 I1 -13.9(11) . . . . ?
N2 C1 Rh1 I1 174.9(5) . . . . ?
C6 C5 Rh1 C7 -17.6(6) . . . . ?
C4 C5 Rh1 C7 105.2(6) . . . . ?
C6 C5 Rh1 C1 -101.6(6) . . . . ?
C4 C5 Rh1 C1 21.2(6) . . . . ?
C6 C5 Rh1 N6 167.0(6) . . . . ?
C4 C5 Rh1 N6 -70.2(6) . . . . ?
C6 C5 Rh1 N5 78.1(6) . . . . ?
C4 C5 Rh1 N5 -159.1(6) . . . . ?
C6 C5 Rh1 I1 -48(4) . . . . ?
C4 C5 Rh1 I1 75(4) . . . . ?
C20 N6 Rh1 C7 47(13) . . . . ?
C20 N6 Rh1 C1 6(12) . . . . ?
C20 N6 Rh1 C5 90(12) . . . . ?
C20 N6 Rh1 N5 178(100) . . . . ?
C20 N6 Rh1 I1 -88(12) . . . . ?
C18 N5 Rh1 C7 122(4) . . . . ?
C18 N5 Rh1 C1 41(5) . . . . ?
C18 N5 Rh1 C5 39(4) . . . . ?
C18 N5 Rh1 N6 -53(4) . . . . ?
C18 N5 Rh1 I1 -144(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         1.099
_refine_diff_density_min         -1.467
_refine_diff_density_rms         0.151

#################################################END