# Copyright The Royal Society of Chemistry, 1998
 
data_1 
  
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C20 H32 Cl2 N3 O4 Rh' 
_chemical_formula_weight          552.30 
_chemical_melting_point           ? 
_chemical_compound_source         ? 
  
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0181   0.0091 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'N'  'N'   0.0311   0.0180 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'   0.0492   0.0322 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Cl'  'Cl'   0.3639   0.7018 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Rh'  'Rh'   0.0927   3.6045 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
  
_symmetry_cell_setting            Monoclinic 
_symmetry_space_group_name_H-M    C2/c 
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y, -z+1/2' 
 'x+1/2, y+1/2, z' 
 '-x+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y, z-1/2' 
 '-x+1/2, -y+1/2, -z' 
 'x+1/2, -y+1/2, z-1/2' 
  
_cell_length_a                    16.0046(14) 
_cell_length_b                    9.9312(5) 
_cell_length_c                    29.8421(15) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  96.905(5) 
_cell_angle_gamma                 90.00 
_cell_volume                      4708.8(5) 
_cell_formula_units_Z             8 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     28 
_cell_measurement_theta_min       10.78 
_cell_measurement_theta_max       22.42 
  
_exptl_crystal_description        Plates 
_exptl_crystal_colour             Yellow 
_exptl_crystal_size_max           0.37 
_exptl_crystal_size_mid           0.23 
_exptl_crystal_size_min           0.04 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.558 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              2272 
_exptl_absorpt_coefficient_mu     8.212 
_exptl_absorpt_correction_type    Semi-empirical 
_exptl_absorpt_correction_T_min   0.3009 
_exptl_absorpt_correction_T_max   0.7659 
  
_exptl_special_details 
; 
 ? 
; 
  
_diffrn_ambient_temperature       293(2) 
_diffrn_radiation_wavelength      1.54178 
_diffrn_radiation_type            CuK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device        'Siemens P4' 
_diffrn_measurement_method        '\w scans' 
_diffrn_standards_number          3 
_diffrn_standards_interval_count  97 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         14.87 
_diffrn_reflns_number             3854 
_diffrn_reflns_av_R_equivalents   0.0839 
_diffrn_reflns_av_sigmaI/netI     0.0710 
_diffrn_reflns_limit_h_min        0 
_diffrn_reflns_limit_h_max        18 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        11 
_diffrn_reflns_limit_l_min        -34 
_diffrn_reflns_limit_l_max        34 
_diffrn_reflns_theta_min          2.98 
_diffrn_reflns_theta_max          63.97 
_reflns_number_total              3709 
_reflns_number_observed           2702 
_reflns_observed_criterion        >2sigma(I) 
  
_computing_data_collection        'Siemens XSCANS' 
_computing_cell_refinement        'Siemens XSCANS' 
_computing_data_reduction         'Siemens SHELXTL' 
_computing_structure_solution     'SHELXS-86 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)' 
_computing_molecular_graphics     'Siemens SHELXTL' 
_computing_publication_material   'Siemens SHELXTL' 
  
_refine_special_details 
; 
 Refinement on F^2^ for ALL reflections except for 14 with very negative F^2^ 
 or flagged by the user for potential systematic errors.  Weighted R-factors 
 wR and all goodnesses 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 observed criterion 
 of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0840P)^2^+0.0000P] 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     ? 
_refine_ls_extinction_method      SHELXL 
_refine_ls_extinction_coef        0.00031(4) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' 
_refine_ls_number_reflns          3695 
_refine_ls_number_parameters      280 
_refine_ls_number_restraints      2 
_refine_ls_R_factor_all           0.0854 
_refine_ls_R_factor_obs           0.0570 
_refine_ls_wR_factor_all          0.1500 
_refine_ls_wR_factor_obs          0.1314 
_refine_ls_goodness_of_fit_all    1.030 
_refine_ls_goodness_of_fit_obs    1.085 
_refine_ls_restrained_S_all       1.051 
_refine_ls_restrained_S_obs       1.085 
_refine_ls_shift/esd_max          -0.005 
_refine_ls_shift/esd_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_thermal_displace_type 
 _atom_site_occupancy 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_group 
Rh Rh 0.71065(3) 0.51175(5) 0.16177(2) 0.0318(2) Uani 1 d . . 
N1 N 0.8425(3) 0.5080(6) 0.1619(2) 0.0316(11) Uani 1 d . . 
C2 C 0.8648(4) 0.5330(6) 0.1196(2) 0.0341(13) Uani 1 d . . 
C3 C 0.9456(5) 0.5419(7) 0.1093(3) 0.041(2) Uani 1 d . . 
H3A H 0.9568(5) 0.5585(7) 0.0799(3) 0.049 Uiso 1 calc R . 
C4 C 1.0120(4) 0.5249(7) 0.1452(3) 0.0383(14) Uani 1 d . . 
O4 O 1.0884(3) 0.5292(7) 0.1414(2) 0.059(2) Uani 1 d . . 
N5 N 0.9872(3) 0.5037(6) 0.1865(2) 0.0367(12) Uani 1 d D . 
H5A H 1.0253(47) 0.5033(99) 0.2113(20) 0.059(28) Uiso 1 d D . 
C6 C 0.9049(4) 0.4937(6) 0.1968(2) 0.0289(12) Uani 1 d . . 
O6 O 0.8913(3) 0.4730(6) 0.2356(2) 0.0413(11) Uani 1 d . . 
C7 C 0.7923(5) 0.5519(9) 0.0820(3) 0.043(2) Uani 1 d . . 
O7 O 0.8066(4) 0.5703(9) 0.0432(2) 0.071(2) Uani 1 d . . 
O8 O 0.7179(3) 0.5433(7) 0.0944(2) 0.056(2) Uani 1 d . . 
C11 C 0.5912(5) 0.6048(8) 0.1554(3) 0.043(2) Uani 1 d . . 
H11A H 0.6064(5) 0.6543(8) 0.1312(3) 0.052 Uiso 1 calc R . 
C12 C 0.5800(5) 0.4661(9) 0.1493(3) 0.048(2) Uani 1 d . . 
H12A H 0.5907(5) 0.4282(9) 0.1221(3) 0.058 Uiso 1 calc R . 
C13 C 0.5508(5) 0.3732(9) 0.1856(4) 0.055(2) Uani 1 d . . 
H13A H 0.5159(5) 0.4243(9) 0.2039(4) 0.066 Uiso 1 calc R . 
H13B H 0.5166(5) 0.3014(9) 0.1710(4) 0.066 Uiso 1 calc R . 
C14 C 0.6232(5) 0.3123(8) 0.2158(3) 0.047(2) Uani 1 d . . 
H14A H 0.6379(5) 0.2268(8) 0.2032(3) 0.056 Uiso 1 calc R . 
H14B H 0.6053(5) 0.2947(8) 0.2452(3) 0.056 Uiso 1 calc R . 
C15 C 0.7003(5) 0.4017(7) 0.2217(3) 0.039(2) Uani 1 d . . 
H15A H 0.7516(5) 0.3613(7) 0.2183(3) 0.047 Uiso 1 calc R . 
C16 C 0.7017(4) 0.5380(7) 0.2317(2) 0.0357(14) Uani 1 d . . 
H16A H 0.7525(4) 0.5842(7) 0.2332(2) 0.043 Uiso 1 calc R . 
C17 C 0.6220(5) 0.6155(7) 0.2404(3) 0.041(2) Uani 1 d . . 
H17A H 0.5827(5) 0.5537(7) 0.2519(3) 0.049 Uiso 1 calc R . 
H17B H 0.6369(5) 0.6837(7) 0.2632(3) 0.049 Uiso 1 calc R . 
C18 C 0.5803(5) 0.6811(8) 0.1987(3) 0.048(2) Uani 1 d . . 
H18A H 0.6032(5) 0.7711(8) 0.1966(3) 0.058 Uiso 1 calc R . 
H18B H 0.5207(5) 0.6898(8) 0.2011(3) 0.058 Uiso 1 calc R . 
N20 N 0.2298(4) 0.5481(7) 0.1016(2) 0.0426(14) Uani 1 d D . 
H20A H 0.1765(26) 0.5513(110) 0.1083(40) 0.075(34) Uiso 1 d D . 
C21 C 0.2647(6) 0.4099(8) 0.1114(3) 0.051(2) Uani 1 d . . 
H21A H 0.3165(6) 0.4011(8) 0.0977(3) 0.061 Uiso 1 calc R . 
H21B H 0.2251(6) 0.3445(8) 0.0971(3) 0.061 Uiso 1 calc R . 
C22 C 0.2826(7) 0.3760(10) 0.1606(4) 0.069(3) Uani 1 d . . 
H22A H 0.3047(7) 0.2862(10) 0.1639(4) 0.104 Uiso 1 calc R . 
H22B H 0.2315(7) 0.3817(10) 0.1744(4) 0.104 Uiso 1 calc R . 
H22C H 0.3231(7) 0.4384(10) 0.1751(4) 0.104 Uiso 1 calc R . 
C23 C 0.2789(5) 0.6559(8) 0.1271(3) 0.050(2) Uani 1 d . . 
H23A H 0.2815(5) 0.6366(8) 0.1591(3) 0.060 Uiso 1 calc R . 
H23B H 0.2494(5) 0.7407(8) 0.1215(3) 0.060 Uiso 1 calc R . 
C24 C 0.3683(6) 0.6713(10) 0.1150(5) 0.077(3) Uani 1 d . . 
H24A H 0.3963(6) 0.7424(10) 0.1326(5) 0.116 Uiso 1 calc R . 
H24B H 0.3663(6) 0.6927(10) 0.0835(5) 0.116 Uiso 1 calc R . 
H24C H 0.3985(6) 0.5886(10) 0.1211(5) 0.116 Uiso 1 calc R . 
C25 C 0.2153(7) 0.5730(13) 0.0518(3) 0.070(3) Uani 1 d . . 
H25A H 0.1854(7) 0.4968(13) 0.0373(3) 0.084 Uiso 1 calc R . 
H25B H 0.2693(7) 0.5795(13) 0.0403(3) 0.084 Uiso 1 calc R . 
C26 C 0.1652(9) 0.7008(17) 0.0396(5) 0.100(5) Uani 1 d . . 
H26A H 0.1577(9) 0.7118(17) 0.0074(5) 0.150 Uiso 1 calc R . 
H26B H 0.1951(9) 0.7769(17) 0.0534(5) 0.150 Uiso 1 calc R . 
H26C H 0.1112(9) 0.6942(17) 0.0504(5) 0.150 Uiso 1 calc R . 
C30 C 0.8939(7) 0.8097(13) -0.0083(4) 0.070(3) Uani 1 d . . 
H30A H 0.8488(7) 0.7559(13) 0.0015(4) 0.084 Uiso 1 calc R . 
H30B H 0.8687(7) 0.8791(13) -0.0284(4) 0.084 Uiso 1 calc R . 
Cl31 Cl 0.9514(2) 0.8860(4) 0.03926(11) 0.0927(10) Uani 1 d . . 
Cl32 Cl 0.9577(2) 0.7069(4) -0.03767(12) 0.0890(9) Uani 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 
Rh 0.0228(3) 0.0427(3) 0.0303(3) -0.0001(2) 0.0047(2) 0.0029(2) 
N1 0.025(2) 0.039(3) 0.031(2) 0.004(2) 0.007(2) 0.003(2) 
C2 0.038(3) 0.035(3) 0.030(3) 0.000(3) 0.007(3) 0.005(3) 
C3 0.037(4) 0.047(4) 0.043(4) 0.001(3) 0.019(3) -0.001(3) 
C4 0.021(3) 0.044(3) 0.051(4) -0.004(3) 0.010(3) -0.003(3) 
O4 0.029(3) 0.094(5) 0.057(3) -0.001(3) 0.017(2) -0.006(3) 
N5 0.025(3) 0.041(3) 0.045(3) 0.004(3) 0.009(2) 0.001(2) 
C6 0.020(3) 0.032(3) 0.035(3) -0.003(3) 0.005(2) -0.001(2) 
O6 0.029(2) 0.064(3) 0.032(2) 0.008(2) 0.007(2) -0.004(2) 
C7 0.037(4) 0.060(4) 0.034(3) -0.002(3) 0.006(3) 0.000(3) 
O7 0.053(4) 0.135(6) 0.028(3) 0.011(3) 0.012(3) -0.002(4) 
O8 0.031(3) 0.101(5) 0.036(2) -0.001(3) 0.005(2) 0.010(3) 
C11 0.031(4) 0.061(4) 0.037(3) 0.013(3) 0.005(3) 0.009(3) 
C12 0.031(4) 0.070(5) 0.043(4) -0.008(4) 0.001(3) 0.000(3) 
C13 0.038(4) 0.057(5) 0.074(6) -0.019(5) 0.020(4) -0.010(3) 
C14 0.038(4) 0.039(3) 0.065(5) -0.002(4) 0.013(4) -0.011(3) 
C15 0.032(4) 0.040(3) 0.048(4) 0.005(3) 0.015(3) -0.001(3) 
C16 0.029(3) 0.041(3) 0.038(3) 0.003(3) 0.009(3) -0.006(3) 
C17 0.040(4) 0.041(3) 0.043(4) -0.009(3) 0.017(3) 0.004(3) 
C18 0.036(4) 0.044(4) 0.068(5) 0.010(4) 0.019(4) 0.012(3) 
N20 0.034(3) 0.058(4) 0.039(3) 0.000(3) 0.016(3) -0.005(3) 
C21 0.058(5) 0.040(4) 0.057(5) -0.009(4) 0.014(4) -0.001(3) 
C22 0.075(7) 0.058(5) 0.072(7) 0.014(5) 0.000(6) -0.003(5) 
C23 0.045(4) 0.045(4) 0.059(5) -0.010(4) 0.007(4) 0.004(3) 
C24 0.051(5) 0.055(5) 0.123(10) -0.014(6) -0.003(6) -0.020(4) 
C25 0.068(6) 0.102(8) 0.041(5) 0.006(5) 0.014(4) -0.017(6) 
C26 0.084(9) 0.143(13) 0.073(8) 0.038(9) 0.011(7) 0.016(9) 
C30 0.056(5) 0.101(8) 0.051(5) 0.010(5) 0.003(4) 0.006(5) 
Cl31 0.080(2) 0.126(3) 0.073(2) -0.029(2) 0.0112(15) -0.004(2) 
Cl32 0.082(2) 0.110(2) 0.077(2) -0.018(2) 0.017(2) 0.003(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 
Rh O8 2.053(6) . ? 
Rh C11 2.111(7) . ? 
Rh N1 2.111(5) . ? 
Rh C15 2.120(7) . ? 
Rh C16 2.125(7) . ? 
Rh C12 2.128(8) . ? 
N1 C6 1.360(8) . ? 
N1 C2 1.377(8) . ? 
C2 C3 1.367(10) . ? 
C2 C7 1.525(10) . ? 
C3 C4 1.425(11) . ? 
C4 O4 1.242(9) . ? 
C4 N5 1.357(10) . ? 
N5 C6 1.391(8) . ? 
C6 O6 1.222(8) . ? 
C7 O7 1.222(10) . ? 
C7 O8 1.291(9) . ? 
C11 C12 1.398(12) . ? 
C11 C18 1.527(12) . ? 
C12 C13 1.538(13) . ? 
C13 C14 1.506(13) . ? 
C14 C15 1.514(9) . ? 
C15 C16 1.386(10) . ? 
C16 C17 1.538(9) . ? 
C17 C18 1.489(12) . ? 
N20 C23 1.482(10) . ? 
N20 C25 1.495(11) . ? 
N20 C21 1.497(10) . ? 
C21 C22 1.502(14) . ? 
C23 C24 1.526(13) . ? 
C25 C26 1.52(2) . ? 
C30 Cl32 1.752(12) . ? 
C30 Cl31 1.766(11) . ? 
  
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 
O8 Rh C11 90.1(3) . . ? 
O8 Rh N1 80.3(2) . . ? 
C11 Rh N1 154.5(3) . . ? 
O8 Rh C15 157.7(3) . . ? 
C11 Rh C15 98.1(3) . . ? 
N1 Rh C15 99.7(2) . . ? 
O8 Rh C16 164.2(3) . . ? 
C11 Rh C16 82.4(3) . . ? 
N1 Rh C16 100.7(2) . . ? 
C15 Rh C16 38.1(3) . . ? 
O8 Rh C12 91.8(3) . . ? 
C11 Rh C12 38.5(3) . . ? 
N1 Rh C12 163.4(3) . . ? 
C15 Rh C12 82.1(3) . . ? 
C16 Rh C12 90.9(3) . . ? 
C6 N1 C2 118.3(5) . . ? 
C6 N1 Rh 130.2(4) . . ? 
C2 N1 Rh 111.4(4) . . ? 
C3 C2 N1 125.1(7) . . ? 
C3 C2 C7 118.9(7) . . ? 
N1 C2 C7 116.0(6) . . ? 
C2 C3 C4 117.6(7) . . ? 
O4 C4 N5 119.0(7) . . ? 
O4 C4 C3 125.6(7) . . ? 
N5 C4 C3 115.4(6) . . ? 
C4 N5 C6 126.8(6) . . ? 
O6 C6 N1 123.0(5) . . ? 
O6 C6 N5 120.2(6) . . ? 
N1 C6 N5 116.8(6) . . ? 
O7 C7 O8 124.3(8) . . ? 
O7 C7 C2 120.2(7) . . ? 
O8 C7 C2 115.4(7) . . ? 
C7 O8 Rh 116.9(5) . . ? 
C12 C11 C18 124.9(7) . . ? 
C12 C11 Rh 71.4(5) . . ? 
C18 C11 Rh 109.6(5) . . ? 
C11 C12 C13 123.1(8) . . ? 
C11 C12 Rh 70.1(5) . . ? 
C13 C12 Rh 112.4(5) . . ? 
C14 C13 C12 112.6(7) . . ? 
C13 C14 C15 113.1(7) . . ? 
C16 C15 C14 126.1(7) . . ? 
C16 C15 Rh 71.1(4) . . ? 
C14 C15 Rh 110.5(6) . . ? 
C15 C16 C17 122.2(6) . . ? 
C15 C16 Rh 70.8(4) . . ? 
C17 C16 Rh 112.5(5) . . ? 
C18 C17 C16 112.0(6) . . ? 
C17 C18 C11 113.9(6) . . ? 
C23 N20 C25 113.6(7) . . ? 
C23 N20 C21 113.5(6) . . ? 
C25 N20 C21 110.8(8) . . ? 
N20 C21 C22 114.8(8) . . ? 
N20 C23 C24 113.8(7) . . ? 
N20 C25 C26 112.9(10) . . ? 
Cl32 C30 Cl31 111.9(6) . . ? 
  
_refine_diff_density_max    0.629 
_refine_diff_density_min   -1.701 
_refine_diff_density_rms    0.117 

#=END


data_2 
  
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C20 H32 N3 O4 Cl2 Ir' 
_chemical_formula_weight          641.59 
_chemical_melting_point           ? 
_chemical_compound_source         ? 
  
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0181   0.0091 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'N'  'N'   0.0311   0.0180 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'   0.0492   0.0322 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Cl'  'Cl'   0.3639   0.7018 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Ir'  'Ir'  -4.7710   6.5667 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
  
_symmetry_cell_setting            Monoclinic 
_symmetry_space_group_name_H-M    C2/c 
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y, -z+1/2' 
 'x+1/2, y+1/2, z' 
 '-x+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y, z-1/2' 
 '-x+1/2, -y+1/2, -z' 
 'x+1/2, -y+1/2, z-1/2' 
  
_cell_length_a                    15.9618(10) 
_cell_length_b                    9.8810(2) 
_cell_length_c                    29.6845(11) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  96.832(4) 
_cell_angle_gamma                 90.00 
_cell_volume                      4648.6(4) 
_cell_formula_units_Z             8 
_cell_measurement_temperature     203(2) 
_cell_measurement_reflns_used     30 
_cell_measurement_theta_min       11.20 
_cell_measurement_theta_max       27.98 
  
_exptl_crystal_description        Prisms 
_exptl_crystal_colour             Yellow 
_exptl_crystal_size_max           0.23 
_exptl_crystal_size_mid           0.10 
_exptl_crystal_size_min           0.08 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.833 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              2528 
_exptl_absorpt_coefficient_mu     13.498 
_exptl_absorpt_correction_type    Semi-empirical 
_exptl_absorpt_correction_T_min   0.0868 
_exptl_absorpt_correction_T_max   0.2200 
  
_exptl_special_details 
; 
 ? 
; 
  
_diffrn_ambient_temperature       203(2) 
_diffrn_radiation_wavelength      1.54178 
_diffrn_radiation_type            CuK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device        'Siemens P4' 
_diffrn_measurement_method        '\w scans' 
_diffrn_standards_number          3 
_diffrn_standards_interval_count  97 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         10.45 
_diffrn_reflns_number             3795 
_diffrn_reflns_av_R_equivalents   0.0388 
_diffrn_reflns_av_sigmaI/netI     0.0384 
_diffrn_reflns_limit_h_min        0 
_diffrn_reflns_limit_h_max        18 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        11 
_diffrn_reflns_limit_l_min        -33 
_diffrn_reflns_limit_l_max        33 
_diffrn_reflns_theta_min          3.00 
_diffrn_reflns_theta_max          61.99 
_reflns_number_total              3649 
_reflns_number_observed           3063 
_reflns_observed_criterion        >2sigma(I) 
  
_computing_data_collection        'Siemens XSCANS' 
_computing_cell_refinement        'Siemens XSCANS' 
_computing_data_reduction         'Siemens SHELXTL' 
_computing_structure_solution     'SHELXS-86 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)' 
_computing_molecular_graphics     'Siemens SHELXTL' 
_computing_publication_material   'Siemens SHELXTL' 
  
_refine_special_details 
; 
 Refinement on F^2^ for ALL reflections except for 15 with very negative F^2^ 
 or flagged by the user for potential systematic errors.  Weighted R-factors 
 wR and all goodnesses 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 observed criterion 
 of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0679P)^2^+10.0693P] 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     ? 
_refine_ls_extinction_method      SHELXL 
_refine_ls_extinction_coef        0.00009(2) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' 
_refine_ls_number_reflns          3634 
_refine_ls_number_parameters      280 
_refine_ls_number_restraints      8 
_refine_ls_R_factor_all           0.0526 
_refine_ls_R_factor_obs           0.0419 
_refine_ls_wR_factor_all          0.1136 
_refine_ls_wR_factor_obs          0.1040 
_refine_ls_goodness_of_fit_all    1.046 
_refine_ls_goodness_of_fit_obs    1.071 
_refine_ls_restrained_S_all       1.067 
_refine_ls_restrained_S_obs       1.069 
_refine_ls_shift/esd_max          -0.001 
_refine_ls_shift/esd_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_thermal_displace_type 
 _atom_site_occupancy 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_group 
Ir Ir 0.71124(2) 0.01114(3) 0.661457(9) 0.0304(2) Uani 1 d . . 
N1 N 0.8427(4) 0.0077(5) 0.6608(2) 0.0292(12) Uani 1 d . . 
C2 C 0.8654(5) 0.0337(7) 0.6188(2) 0.0301(14) Uani 1 d . . 
C3 C 0.9466(5) 0.0433(8) 0.6094(2) 0.036(2) Uani 1 d . . 
H3A H 0.9585(5) 0.0619(8) 0.5797(2) 0.044 Uiso 1 calc R . 
C4 C 1.0132(5) 0.0246(7) 0.6455(2) 0.034(2) Uani 1 d D . 
O4 O 1.0897(3) 0.0283(7) 0.6417(2) 0.0483(14) Uani 1 d . . 
N5 N 0.9874(4) 0.0022(5) 0.6866(2) 0.0332(13) Uani 1 d D . 
H5A H 1.0267(9) -0.0086(17) 0.7107(4) 0.119(45) Uiso 1 d DU . 
C6 C 0.9044(4) -0.0063(6) 0.6962(2) 0.0273(14) Uani 1 d D . 
O6 O 0.8914(3) -0.0297(5) 0.7359(2) 0.0354(11) Uani 1 d . . 
C7 C 0.7924(5) 0.0547(9) 0.5816(2) 0.039(2) Uani 1 d . . 
O7 O 0.8069(4) 0.0770(8) 0.5426(2) 0.060(2) Uani 1 d . . 
O8 O 0.7185(3) 0.0481(7) 0.5939(2) 0.0490(14) Uani 1 d . . 
C11 C 0.5915(5) 0.1052(8) 0.6557(3) 0.042(2) Uani 1 d . . 
H11A H 0.6074(5) 0.1563(8) 0.6314(3) 0.051 Uiso 1 calc R . 
C12 C 0.5811(5) -0.0364(9) 0.6489(3) 0.046(2) Uani 1 d . . 
H12A H 0.5934(5) -0.0743(9) 0.6214(3) 0.055 Uiso 1 calc R . 
C13 C 0.5507(5) -0.1282(8) 0.6846(3) 0.045(2) Uani 1 d . . 
H13A H 0.5162(5) -0.2008(8) 0.6695(3) 0.054 Uiso 1 calc R . 
H13B H 0.5150(5) -0.0760(8) 0.7029(3) 0.054 Uiso 1 calc R . 
C14 C 0.6234(5) -0.1905(8) 0.7157(3) 0.044(2) Uani 1 d . . 
H14A H 0.6055(5) -0.2051(8) 0.7458(3) 0.052 Uiso 1 calc R . 
H14B H 0.6373(5) -0.2790(8) 0.7036(3) 0.052 Uiso 1 calc R . 
C15 C 0.7014(5) -0.1026(8) 0.7204(2) 0.037(2) Uani 1 d . . 
H15A H 0.7530(5) -0.1428(8) 0.7156(2) 0.044 Uiso 1 calc R . 
C16 C 0.7015(5) 0.0387(8) 0.7316(3) 0.035(2) Uani 1 d . . 
H16A H 0.7528(5) 0.0864(8) 0.7336(3) 0.042 Uiso 1 calc R . 
C17 C 0.6224(5) 0.1143(8) 0.7405(3) 0.039(2) Uani 1 d . . 
H17A H 0.5832(5) 0.0509(8) 0.7523(3) 0.047 Uiso 1 calc R . 
H17B H 0.6373(5) 0.1836(8) 0.7637(3) 0.047 Uiso 1 calc R . 
C18 C 0.5792(5) 0.1804(8) 0.6986(3) 0.040(2) Uani 1 d . . 
H18A H 0.6011(5) 0.2727(8) 0.6966(3) 0.048 Uiso 1 calc R . 
H18B H 0.5187(5) 0.1869(8) 0.7011(3) 0.048 Uiso 1 calc R . 
N20 N 1.2324(4) 0.0467(7) 0.6017(2) 0.0383(14) Uani 1 d D . 
H20A H 1.1812(6) 0.0483(19) 0.6116(6) 0.103(39) Uiso 1 d DU . 
C21 C 1.2167(6) 0.0717(10) 0.5515(3) 0.054(2) Uani 1 d D . 
H21A H 1.2710(6) 0.0770(10) 0.5393(3) 0.064 Uiso 1 calc R . 
H21B H 1.1855(6) -0.0052(10) 0.5370(3) 0.064 Uiso 1 calc R . 
C22 C 1.1681(8) 0.1987(14) 0.5396(4) 0.084(4) Uani 1 d . . 
H22A H 1.1599(8) 0.2095(14) 0.5069(4) 0.126 Uiso 1 calc R . 
H22B H 1.1993(8) 0.2756(14) 0.5533(4) 0.126 Uiso 1 calc R . 
H22C H 1.1137(8) 0.1934(14) 0.5509(4) 0.126 Uiso 1 calc R . 
C23 C 1.2820(5) 0.1575(8) 0.6277(3) 0.044(2) Uani 1 d D . 
H23A H 1.2530(5) 0.2440(8) 0.6213(3) 0.052 Uiso 1 calc R . 
H23B H 1.2840(5) 0.1397(8) 0.6603(3) 0.052 Uiso 1 calc R . 
C24 C 1.3701(6) 0.1687(10) 0.6158(4) 0.059(2) Uani 1 d . . 
H24A H 1.3993(6) 0.2411(10) 0.6333(4) 0.089 Uiso 1 calc R . 
H24B H 1.3686(6) 0.1884(10) 0.5837(4) 0.089 Uiso 1 calc R . 
H24C H 1.3997(6) 0.0840(10) 0.6226(4) 0.089 Uiso 1 calc R . 
C25 C 1.2670(6) -0.0922(8) 0.6109(3) 0.046(2) Uani 1 d D . 
H25A H 1.3192(6) -0.1020(8) 0.5969(3) 0.055 Uiso 1 calc R . 
H25B H 1.2264(6) -0.1587(8) 0.5969(3) 0.055 Uiso 1 calc R . 
C26 C 1.2851(7) -0.1221(9) 0.6613(3) 0.055(2) Uani 1 d . . 
H26A H 1.3074(7) -0.2132(9) 0.6655(3) 0.083 Uiso 1 calc R . 
H26B H 1.2334(7) -0.1145(9) 0.6752(3) 0.083 Uiso 1 calc R . 
H26C H 1.3262(7) -0.0578(9) 0.6752(3) 0.083 Uiso 1 calc R . 
C30 C 0.8964(6) 0.3139(11) 0.4911(3) 0.057(2) Uani 1 d . . 
H30A H 0.8753(6) 0.3863(11) 0.4702(3) 0.068 Uiso 1 calc R . 
H30B H 0.8476(6) 0.2649(11) 0.5000(3) 0.068 Uiso 1 calc R . 
Cl1 Cl 0.9592(2) 0.2018(3) 0.46305(9) 0.0702(7) Uani 1 d . . 
Cl2 Cl 0.9538(2) 0.3856(3) 0.53958(8) 0.0695(7) Uani 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 
Ir 0.0288(2) 0.0361(2) 0.0260(2) -0.00062(11) 0.00235(12) 0.00213(12) 
N1 0.035(3) 0.027(3) 0.026(3) 0.001(2) 0.004(2) 0.002(2) 
C2 0.036(4) 0.030(3) 0.025(3) 0.000(3) 0.007(3) 0.003(3) 
C3 0.039(4) 0.042(4) 0.029(4) 0.004(3) 0.009(3) 0.001(3) 
C4 0.033(4) 0.037(4) 0.033(4) -0.005(3) 0.011(3) -0.005(3) 
O4 0.028(3) 0.073(4) 0.046(3) -0.004(3) 0.013(2) -0.003(3) 
N5 0.031(3) 0.037(3) 0.032(3) 0.003(2) 0.005(3) 0.001(2) 
C6 0.029(4) 0.026(3) 0.027(4) -0.008(2) 0.006(3) -0.003(3) 
O6 0.028(3) 0.049(3) 0.029(3) 0.006(2) 0.001(2) -0.001(2) 
C7 0.038(4) 0.052(4) 0.025(4) -0.002(3) 0.002(3) 0.004(3) 
O7 0.049(4) 0.113(6) 0.018(3) 0.010(3) 0.006(2) 0.006(4) 
O8 0.031(3) 0.076(4) 0.040(3) 0.002(3) 0.005(2) 0.011(3) 
C11 0.033(4) 0.054(5) 0.040(4) 0.013(3) 0.007(3) 0.009(4) 
C12 0.033(4) 0.055(5) 0.049(5) -0.015(4) -0.004(4) 0.012(4) 
C13 0.042(5) 0.040(4) 0.052(5) -0.011(4) 0.004(4) -0.004(4) 
C14 0.040(5) 0.036(4) 0.056(5) -0.006(3) 0.012(4) -0.005(3) 
C15 0.037(4) 0.039(4) 0.036(4) -0.003(3) 0.009(3) 0.000(3) 
C16 0.027(4) 0.037(4) 0.041(4) 0.001(3) 0.006(3) -0.001(3) 
C17 0.038(4) 0.041(4) 0.039(4) -0.001(3) 0.009(3) 0.001(3) 
C18 0.035(4) 0.035(4) 0.052(5) 0.001(3) 0.015(4) 0.004(3) 
N20 0.040(4) 0.048(4) 0.028(3) -0.004(3) 0.008(3) -0.008(3) 
C21 0.053(5) 0.077(6) 0.030(4) -0.004(4) 0.001(4) -0.014(5) 
C22 0.067(7) 0.122(11) 0.059(7) 0.025(7) -0.011(6) 0.007(7) 
C23 0.043(5) 0.042(4) 0.044(4) -0.006(3) 0.000(4) 0.002(4) 
C24 0.046(5) 0.047(5) 0.081(7) -0.004(5) -0.003(5) -0.011(4) 
C25 0.052(5) 0.039(4) 0.048(5) -0.012(3) 0.014(4) -0.005(4) 
C26 0.070(6) 0.043(5) 0.053(5) 0.005(4) 0.008(5) 0.004(4) 
C30 0.056(6) 0.075(6) 0.038(4) 0.001(4) -0.002(4) 0.005(5) 
Cl1 0.070(2) 0.083(2) 0.0584(14) -0.0135(12) 0.0105(12) 0.0001(14) 
Cl2 0.066(2) 0.092(2) 0.0504(13) -0.0157(12) 0.0045(11) -0.0020(14) 
  
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
  
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
Ir O8 2.055(6) . ? 
Ir C15 2.100(7) . ? 
Ir N1 2.102(6) . ? 
Ir C11 2.114(8) . ? 
Ir C12 2.119(9) . ? 
Ir C16 2.125(7) . ? 
N1 C6 1.360(9) . ? 
N1 C2 1.362(9) . ? 
C2 C3 1.361(11) . ? 
C2 C7 1.521(10) . ? 
C3 C4 1.431(10) . ? 
C4 O4 1.240(10) . ? 
C4 N5 1.352(10) . ? 
N5 C6 1.389(9) . ? 
C6 O6 1.243(9) . ? 
C7 O7 1.226(9) . ? 
C7 O8 1.277(9) . ? 
C11 C12 1.420(12) . ? 
C11 C18 1.506(11) . ? 
C12 C13 1.518(12) . ? 
C13 C14 1.525(11) . ? 
C14 C15 1.511(10) . ? 
C15 C16 1.435(10) . ? 
C16 C17 1.517(10) . ? 
C17 C18 1.498(11) . ? 
N20 C25 1.493(11) . ? 
N20 C21 1.503(10) . ? 
N20 C23 1.509(10) . ? 
C21 C22 1.50(2) . ? 
C23 C24 1.494(12) . ? 
C25 C26 1.517(12) . ? 
C30 Cl2 1.760(9) . ? 
C30 Cl1 1.767(10) . ? 
  
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 
O8 Ir C15 157.8(3) . . ? 
O8 Ir N1 79.7(2) . . ? 
C15 Ir N1 100.0(3) . . ? 
O8 Ir C11 90.0(3) . . ? 
C15 Ir C11 98.4(3) . . ? 
N1 Ir C11 154.3(3) . . ? 
O8 Ir C12 92.0(3) . . ? 
C15 Ir C12 81.9(3) . . ? 
N1 Ir C12 162.5(3) . . ? 
C11 Ir C12 39.2(3) . . ? 
O8 Ir C16 162.4(3) . . ? 
C15 Ir C16 39.7(3) . . ? 
N1 Ir C16 101.6(3) . . ? 
C11 Ir C16 81.5(3) . . ? 
C12 Ir C16 91.0(3) . . ? 
C6 N1 C2 118.7(6) . . ? 
C6 N1 Ir 128.8(5) . . ? 
C2 N1 Ir 112.3(5) . . ? 
C3 C2 N1 124.3(7) . . ? 
C3 C2 C7 120.4(6) . . ? 
N1 C2 C7 115.2(6) . . ? 
C2 C3 C4 118.6(6) . . ? 
O4 C4 N5 119.8(7) . . ? 
O4 C4 C3 125.5(7) . . ? 
N5 C4 C3 114.7(7) . . ? 
C4 N5 C6 126.6(6) . . ? 
O6 C6 N1 124.4(6) . . ? 
O6 C6 N5 118.5(6) . . ? 
N1 C6 N5 117.1(6) . . ? 
O7 C7 O8 124.3(7) . . ? 
O7 C7 C2 119.7(7) . . ? 
O8 C7 C2 116.0(6) . . ? 
C7 O8 Ir 116.8(5) . . ? 
C12 C11 C18 125.7(7) . . ? 
C12 C11 Ir 70.6(5) . . ? 
C18 C11 Ir 110.9(5) . . ? 
C11 C12 C13 122.0(7) . . ? 
C11 C12 Ir 70.2(5) . . ? 
C13 C12 Ir 113.4(6) . . ? 
C12 C13 C14 112.4(7) . . ? 
C15 C14 C13 112.5(7) . . ? 
C16 C15 C14 124.0(7) . . ? 
C16 C15 Ir 71.1(4) . . ? 
C14 C15 Ir 111.9(5) . . ? 
C15 C16 C17 122.8(7) . . ? 
C15 C16 Ir 69.2(4) . . ? 
C17 C16 Ir 113.1(5) . . ? 
C18 C17 C16 112.4(6) . . ? 
C17 C18 C11 113.1(6) . . ? 
C25 N20 C21 110.3(7) . . ? 
C25 N20 C23 114.4(6) . . ? 
C21 N20 C23 113.8(6) . . ? 
C22 C21 N20 113.1(8) . . ? 
C24 C23 N20 112.6(7) . . ? 
N20 C25 C26 112.5(6) . . ? 
Cl2 C30 Cl1 111.6(5) . . ? 
  
_refine_diff_density_max    1.065 
_refine_diff_density_min   -0.897 
_refine_diff_density_rms    0.146 
  
#=END


data_1' 
  
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C29 H50 N3 O4 Rh' 
_chemical_formula_weight          607.63 
_chemical_melting_point           ? 
_chemical_compound_source         ? 
  
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0181   0.0091 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'N'  'N'   0.0311   0.0180 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'   0.0492   0.0322 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Rh'  'Rh'   0.0927   3.6045 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
  
_symmetry_cell_setting            Tetragonal 
_symmetry_space_group_name_H-M    I4(1)/a 
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x+1/2, -y, z+1/2' 
 '-y+3/4, x+1/4, z+1/4' 
 'y+3/4, -x+3/4, z+3/4' 
 'x+1/2, y+1/2, z+1/2' 
 '-x+1, -y+1/2, z+1' 
 '-y+5/4, x+3/4, z+3/4' 
 'y+5/4, -x+5/4, z+5/4' 
 '-x, -y, -z' 
 'x-1/2, y, -z-1/2' 
 'y-3/4, -x-1/4, -z-1/4' 
 '-y-3/4, x-3/4, -z-3/4' 
 '-x+1/2, -y+1/2, -z+1/2' 
 'x, y+1/2, -z' 
 'y-1/4, -x+1/4, -z+1/4' 
 '-y-1/4, x-1/4, -z-1/4' 
  
_cell_length_a                    20.2726(5) 
_cell_length_b                    20.2726(5) 
_cell_length_c                    30.435(3) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      12508.3(13) 
_cell_formula_units_Z             16 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     39 
_cell_measurement_theta_min       11.06 
_cell_measurement_theta_max       24.92 
  
_exptl_crystal_description        Needles 
_exptl_crystal_colour             Yellow 
_exptl_crystal_size_max           0.30 
_exptl_crystal_size_mid           0.17 
_exptl_crystal_size_min           0.13 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.291 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              5152 
_exptl_absorpt_coefficient_mu     4.691 
_exptl_absorpt_correction_type    Semi-empirical 
_exptl_absorpt_correction_T_min   0.3529 
_exptl_absorpt_correction_T_max   0.4791 
  
_exptl_special_details 
; 
 ? 
; 
  
_diffrn_ambient_temperature       293(2) 
_diffrn_radiation_wavelength      1.54178 
_diffrn_radiation_type            CuK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device        'Siemens P4' 
_diffrn_measurement_method        '\w scans' 
_diffrn_standards_number          3 
_diffrn_standards_interval_count  97 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             5388 
_diffrn_reflns_av_R_equivalents   0.0340 
_diffrn_reflns_av_sigmaI/netI     0.0734 
_diffrn_reflns_limit_h_min        -21 
_diffrn_reflns_limit_h_max        23 
_diffrn_reflns_limit_k_min        -18 
_diffrn_reflns_limit_k_max        23 
_diffrn_reflns_limit_l_min        -35 
_diffrn_reflns_limit_l_max        20 
_diffrn_reflns_theta_min          2.62 
_diffrn_reflns_theta_max          63.00 
_reflns_number_total              5065 
_reflns_number_observed           3250 
_reflns_observed_criterion        >2sigma(I) 
  
_computing_data_collection        'Siemens XSCANS' 
_computing_cell_refinement        'Siemens XSCANS' 
_computing_data_reduction         'Siemens SHELXTL' 
_computing_structure_solution     'SHELXS-86 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)' 
_computing_molecular_graphics     'Siemens SHELXTL' 
_computing_publication_material   'Siemens SHELXTL' 
  
_refine_special_details 
; 
 Refinement on F^2^ for ALL reflections except for 11 with very negative F^2^ 
 or flagged by the user for potential systematic errors.  Weighted R-factors 
 wR and all goodnesses 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 observed criterion 
 of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0499P)^2^+28.6032P] 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     ? 
_refine_ls_extinction_method      SHELXL 
_refine_ls_extinction_coef        0.000045(8) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' 
_refine_ls_number_reflns          5054 
_refine_ls_number_parameters      347 
_refine_ls_number_restraints      144 
_refine_ls_R_factor_all           0.1086 
_refine_ls_R_factor_obs           0.0615 
_refine_ls_wR_factor_all          0.1609 
_refine_ls_wR_factor_obs          0.1296 
_refine_ls_goodness_of_fit_all    1.080 
_refine_ls_goodness_of_fit_obs    1.116 
_refine_ls_restrained_S_all       1.085 
_refine_ls_restrained_S_obs       1.100 
_refine_ls_shift/esd_max          -0.004 
_refine_ls_shift/esd_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_thermal_displace_type 
 _atom_site_occupancy 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_group 
Rh Rh 0.27874(3) 0.64669(3) 0.03418(2) 0.0629(2) Uani 1 d . . 
N1 N 0.1840(3) 0.6643(3) 0.0584(2) 0.0590(15) Uani 1 d . . 
C2 C 0.1525(3) 0.6080(3) 0.0698(3) 0.057(2) Uani 1 d . . 
C3 C 0.0887(4) 0.6039(4) 0.0838(3) 0.065(2) Uani 1 d . . 
H3A H 0.0700(4) 0.5632(4) 0.0903(3) 0.078 Uiso 1 calc R . 
C4 C 0.0511(4) 0.6633(4) 0.0884(3) 0.069(2) Uani 1 d D . 
O4 O -0.0076(3) 0.6664(3) 0.0994(2) 0.089(2) Uani 1 d . . 
N5 N 0.0860(3) 0.7191(3) 0.0785(3) 0.066(2) Uani 1 d D . 
H5A H 0.0656(18) 0.7580(4) 0.0829(32) 0.112(37) Uiso 1 d D . 
C6 C 0.1504(3) 0.7232(4) 0.0635(3) 0.064(2) Uani 1 d D . 
O6 O 0.1742(3) 0.7775(2) 0.0560(2) 0.081(2) Uani 1 d . . 
C7 C 0.1926(4) 0.5458(4) 0.0659(3) 0.067(2) Uani 1 d . . 
O7 O 0.1708(3) 0.4938(3) 0.0807(2) 0.085(2) Uani 1 d . . 
O8 O 0.2494(3) 0.5517(2) 0.0473(2) 0.078(2) Uani 1 d . . 
C11 C 0.3792(4) 0.6194(5) 0.0328(4) 0.091(3) Uani 1 d . . 
H11A H 0.3683(4) 0.5883(5) 0.0541(4) 0.109 Uiso 1 calc R . 
C12 C 0.3528(5) 0.6101(5) -0.0080(4) 0.094(3) Uani 1 d . . 
H12A H 0.3259(5) 0.5736(5) -0.0125(4) 0.113 Uiso 1 calc R . 
C13 C 0.3643(7) 0.6545(7) -0.0449(5) 0.135(5) Uani 1 d . . 
H13A H 0.3475(7) 0.6333(7) -0.0712(5) 0.162 Uiso 1 calc R . 
H13B H 0.4117(7) 0.6590(7) -0.0486(5) 0.162 Uiso 1 calc R . 
C14 C 0.3358(8) 0.7215(7) -0.0428(5) 0.149(6) Uani 1 d . . 
H14A H 0.3077(8) 0.7281(7) -0.0683(5) 0.179 Uiso 1 calc R . 
H14B H 0.3713(8) 0.7535(7) -0.0444(5) 0.179 Uiso 1 calc R . 
C15 C 0.2959(5) 0.7345(4) -0.0018(4) 0.091(3) Uani 1 d . . 
H15A H 0.2503(5) 0.7374(4) -0.0049(4) 0.109 Uiso 1 calc R . 
C16 C 0.3213(4) 0.7423(4) 0.0401(4) 0.089(3) Uani 1 d . . 
H16A H 0.2918(4) 0.7497(4) 0.0629(4) 0.107 Uiso 1 calc R . 
C17 C 0.3943(5) 0.7396(6) 0.0513(6) 0.154(7) Uani 1 d . . 
H17A H 0.4177(5) 0.7700(6) 0.0323(6) 0.184 Uiso 1 calc R . 
H17B H 0.4002(5) 0.7547(6) 0.0813(6) 0.184 Uiso 1 calc R . 
C18 C 0.4241(5) 0.6745(6) 0.0470(5) 0.120(4) Uani 1 d . . 
H18A H 0.4433(5) 0.6627(6) 0.0751(5) 0.143 Uiso 1 calc R . 
H18B H 0.4599(5) 0.6776(6) 0.0260(5) 0.143 Uiso 1 calc R . 
N20 N 0.8295(3) 0.5337(3) 0.0828(2) 0.065(2) Uani 1 d D . 
C21 C 0.8276(4) 0.4584(4) 0.0763(4) 0.085(3) Uani 1 d D . 
H21A H 0.7895(4) 0.4413(4) 0.0919(4) 0.102 Uiso 1 calc R . 
H21B H 0.8208(4) 0.4496(4) 0.0453(4) 0.102 Uiso 1 calc R . 
C22 C 0.8870(5) 0.4206(4) 0.0910(5) 0.115(4) Uani 1 d D . 
H22A H 0.8871(5) 0.4175(4) 0.1228(5) 0.138 Uiso 0.60 calc PR 1 
H22B H 0.9266(5) 0.4438(4) 0.0820(5) 0.138 Uiso 0.60 calc PR 1 
H22C H 0.8977(5) 0.4361(4) 0.1199(5) 0.138 Uiso 0.40 d PR 2 
H22D H 0.9233(5) 0.4313(4) 0.0720(5) 0.138 Uiso 0.40 d PR 2 
C23 C 0.8868(11) 0.3511(7) 0.0710(10) 0.130(9) Uani 0.60 d PD 1 
H23A H 0.8792(11) 0.3544(7) 0.0396(10) 0.156 Uiso 0.60 calc PR 1 
H23B H 0.9297(11) 0.3310(7) 0.0754(10) 0.156 Uiso 0.60 calc PR 1 
C24 C 0.8358(17) 0.3087(10) 0.0907(10) 0.203(16) Uani 0.60 d PD 1 
H24A H 0.8373(17) 0.2659(10) 0.0773(10) 0.304 Uiso 0.60 calc PR 1 
H24B H 0.7931(17) 0.3280(10) 0.0859(10) 0.304 Uiso 0.60 calc PR 1 
H24C H 0.8436(17) 0.3047(10) 0.1217(10) 0.304 Uiso 0.60 calc PR 1 
C23' C 0.8776(18) 0.3480(9) 0.0938(9) 0.113(13) Uiso 0.40 d PD 2 
H23C H 0.8372(18) 0.3387(9) 0.1098(9) 0.135 Uiso 0.40 calc PR 2 
H23D H 0.9140(18) 0.3288(9) 0.1101(9) 0.135 Uiso 0.40 calc PR 2 
C24' C 0.8739(29) 0.3170(17) 0.0496(13) 0.200(24) Uiso 0.40 d PD 2 
H24D H 0.8678(29) 0.2703(17) 0.0527(13) 0.300 Uiso 0.40 calc PR 2 
H24E H 0.9140(29) 0.3254(17) 0.0338(13) 0.300 Uiso 0.40 calc PR 2 
H24F H 0.8373(29) 0.3354(17) 0.0336(13) 0.300 Uiso 0.40 calc PR 2 
C25 C 0.7660(4) 0.5611(4) 0.0645(3) 0.074(2) Uani 1 d D . 
H25A H 0.7619(4) 0.5469(4) 0.0342(3) 0.088 Uiso 1 calc R . 
H25B H 0.7689(4) 0.6088(4) 0.0645(3) 0.088 Uiso 1 calc R . 
C26 C 0.7043(4) 0.5412(5) 0.0888(3) 0.084(3) Uani 1 d D . 
H26A H 0.6995(4) 0.4936(5) 0.0876(3) 0.101 Uiso 1 calc R . 
H26B H 0.7084(4) 0.5539(5) 0.1194(3) 0.101 Uiso 1 calc R . 
C27 C 0.6443(4) 0.5729(6) 0.0696(4) 0.103(3) Uani 1 d D . 
H27A H 0.6475(4) 0.6202(6) 0.0739(4) 0.124 Uiso 1 calc R . 
H27B H 0.6439(4) 0.5647(6) 0.0382(4) 0.124 Uiso 1 calc R . 
C28 C 0.5808(5) 0.5496(7) 0.0884(5) 0.134(5) Uani 1 d D . 
H28A H 0.5449(5) 0.5723(7) 0.0744(5) 0.201 Uiso 1 calc R . 
H28B H 0.5800(5) 0.5586(7) 0.1194(5) 0.201 Uiso 1 calc R . 
H28C H 0.5764(5) 0.5030(7) 0.0836(5) 0.201 Uiso 1 calc R . 
C29 C 0.8376(4) 0.5481(4) 0.1310(3) 0.071(2) Uani 1 d D . 
H29A H 0.8038(4) 0.5243(4) 0.1470(3) 0.086 Uiso 1 calc R . 
H29B H 0.8801(4) 0.5310(4) 0.1404(3) 0.086 Uiso 1 calc R . 
C30 C 0.8338(5) 0.6197(4) 0.1433(3) 0.091(3) Uani 1 d D . 
H30A H 0.7922(5) 0.6378(4) 0.1331(3) 0.109 Uiso 1 calc R . 
H30B H 0.8692(5) 0.6436(4) 0.1290(3) 0.109 Uiso 1 calc R . 
C31 C 0.8391(6) 0.6284(5) 0.1925(3) 0.092(3) Uani 1 d D . 
H31A H 0.8026(6) 0.6059(5) 0.2066(3) 0.110 Uiso 1 calc R . 
H31B H 0.8797(6) 0.6084(5) 0.2027(3) 0.110 Uiso 1 calc R . 
C32 C 0.8382(9) 0.6999(6) 0.2051(4) 0.160(7) Uani 1 d D . 
H32A H 0.8416(9) 0.7039(6) 0.2364(4) 0.241 Uiso 1 calc R . 
H32B H 0.7976(9) 0.7196(6) 0.1953(4) 0.241 Uiso 1 calc R . 
H32C H 0.8747(9) 0.7221(6) 0.1915(4) 0.241 Uiso 1 calc R . 
C33 C 0.8865(4) 0.5637(4) 0.0578(3) 0.078(2) Uani 1 d D . 
H33A H 0.8825(4) 0.6114(4) 0.0592(3) 0.093 Uiso 1 calc R . 
H33B H 0.9271(4) 0.5519(4) 0.0728(3) 0.093 Uiso 1 calc R . 
C34 C 0.8927(5) 0.5441(5) 0.0108(3) 0.104(3) Uani 1 d D . 
H34A H 0.8511(5) 0.5525(5) -0.0040(3) 0.124 Uiso 1 calc R . 
H34B H 0.9014(5) 0.4971(5) 0.0092(3) 0.124 Uiso 1 calc R . 
C35 C 0.9472(6) 0.5810(6) -0.0127(4) 0.113(4) Uani 1 d D . 
H35A H 0.9870(6) 0.5790(6) 0.0049(4) 0.136 Uiso 1 calc R . 
H35B H 0.9562(6) 0.5593(6) -0.0404(4) 0.136 Uiso 1 calc R . 
C36 C 0.9306(9) 0.6511(6) -0.0212(5) 0.166(7) Uani 1 d D . 
H36A H 0.9667(9) 0.6720(6) -0.0361(5) 0.250 Uiso 1 calc R . 
H36B H 0.9226(9) 0.6732(6) 0.0061(5) 0.250 Uiso 1 calc R . 
H36C H 0.8918(9) 0.6535(6) -0.0392(5) 0.250 Uiso 1 calc R . 
  
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 
Rh 0.0546(3) 0.0499(3) 0.0843(4) -0.0024(3) 0.0025(3) 0.0066(2) 
N1 0.049(3) 0.050(3) 0.079(4) 0.000(3) -0.010(3) -0.001(2) 
C2 0.057(4) 0.050(4) 0.064(5) 0.007(3) -0.016(3) 0.001(3) 
C3 0.056(4) 0.056(4) 0.084(6) 0.009(4) -0.013(4) -0.001(3) 
C4 0.051(4) 0.073(5) 0.082(6) 0.011(4) -0.009(4) 0.003(3) 
O4 0.050(3) 0.080(4) 0.136(6) 0.023(4) 0.004(3) -0.003(3) 
N5 0.049(3) 0.054(3) 0.095(5) -0.001(3) -0.004(3) 0.001(3) 
C6 0.045(4) 0.056(4) 0.090(6) -0.003(4) -0.003(4) 0.003(3) 
O6 0.057(3) 0.047(3) 0.139(6) 0.000(3) 0.012(3) 0.002(2) 
C7 0.067(5) 0.052(4) 0.081(6) 0.005(4) -0.018(4) 0.004(3) 
O7 0.072(3) 0.054(3) 0.131(6) 0.022(3) -0.018(4) -0.001(3) 
O8 0.073(3) 0.050(3) 0.110(5) -0.001(3) 0.002(3) 0.012(2) 
C11 0.068(5) 0.082(6) 0.123(9) -0.001(6) 0.013(6) 0.017(4) 
C12 0.091(7) 0.077(6) 0.114(9) 0.000(6) 0.016(6) 0.020(5) 
C13 0.147(11) 0.126(10) 0.132(11) 0.012(9) 0.060(9) 0.053(9) 
C14 0.181(14) 0.109(9) 0.156(14) 0.027(9) 0.079(11) 0.026(9) 
C15 0.087(6) 0.064(5) 0.122(9) 0.011(6) 0.024(6) 0.003(4) 
C16 0.061(5) 0.054(4) 0.153(11) -0.014(6) 0.020(6) -0.011(4) 
C17 0.059(6) 0.089(7) 0.312(22) -0.029(10) -0.019(9) 0.000(5) 
C18 0.067(6) 0.099(7) 0.193(14) -0.014(8) -0.021(7) 0.008(5) 
N20 0.062(3) 0.058(3) 0.074(5) -0.004(3) 0.002(3) -0.008(3) 
C21 0.079(5) 0.062(5) 0.113(8) 0.007(5) 0.005(5) -0.004(4) 
C22 0.098(8) 0.075(6) 0.170(13) 0.009(7) 0.020(8) 0.017(5) 
C23 0.148(21) 0.073(12) 0.169(26) 0.001(14) 0.036(21) 0.038(12) 
C24 0.291(42) 0.101(17) 0.216(34) -0.062(20) 0.041(30) -0.072(22) 
C25 0.077(5) 0.064(5) 0.080(6) -0.004(4) -0.005(4) 0.002(4) 
C26 0.081(6) 0.075(5) 0.097(7) 0.004(5) -0.004(5) 0.005(4) 
C27 0.076(6) 0.112(8) 0.121(9) 0.030(7) -0.012(6) 0.019(5) 
C28 0.074(7) 0.161(13) 0.167(13) 0.048(10) -0.016(8) 0.011(7) 
C29 0.070(5) 0.068(5) 0.076(6) 0.013(4) -0.001(4) -0.008(4) 
C30 0.093(6) 0.080(6) 0.099(7) 0.002(5) 0.001(6) -0.013(5) 
C31 0.100(7) 0.100(7) 0.076(7) -0.006(5) -0.008(5) -0.004(6) 
C32 0.260(20) 0.099(9) 0.122(12) -0.036(8) -0.020(12) -0.033(11) 
C33 0.080(5) 0.070(5) 0.084(6) -0.003(4) 0.020(5) -0.010(4) 
C34 0.100(7) 0.110(8) 0.101(8) 0.002(7) 0.023(6) -0.008(6) 
C35 0.118(9) 0.124(9) 0.098(8) -0.015(7) 0.038(7) 0.007(7) 
C36 0.221(18) 0.131(12) 0.148(14) 0.043(10) 0.083(13) 0.043(12) 
  
_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 
Rh O8 2.054(5) . ? 
Rh N1 2.089(6) . ? 
Rh C12 2.110(10) . ? 
Rh C11 2.111(9) . ? 
Rh C15 2.118(9) . ? 
Rh C16 2.130(8) . ? 
N1 C2 1.352(9) . ? 
N1 C6 1.384(9) . ? 
C2 C3 1.364(10) . ? 
C2 C7 1.505(10) . ? 
C3 C4 1.433(11) . ? 
C4 O4 1.237(9) . ? 
C4 N5 1.368(10) . ? 
N5 C6 1.386(9) . ? 
C6 O6 1.222(9) . ? 
C7 O7 1.228(9) . ? 
C7 O8 1.289(10) . ? 
C11 C12 1.368(15) . ? 
C11 C18 1.505(14) . ? 
C12 C13 1.46(2) . ? 
C13 C14 1.48(2) . ? 
C14 C15 1.51(2) . ? 
C15 C16 1.383(15) . ? 
C16 C17 1.519(13) . ? 
C17 C18 1.457(15) . ? 
N20 C29 1.503(10) . ? 
N20 C25 1.507(10) . ? 
N20 C33 1.512(9) . ? 
N20 C21 1.540(10) . ? 
C21 C22 1.496(11) . ? 
C22 C23' 1.49(2) . ? 
C22 C23 1.53(2) . ? 
C23 C24 1.47(2) . ? 
C23' C24' 1.49(2) . ? 
C25 C26 1.508(10) . ? 
C26 C27 1.496(10) . ? 
C27 C28 1.487(12) . ? 
C29 C30 1.501(10) . ? 
C30 C31 1.510(11) . ? 
C31 C32 1.500(12) . ? 
C33 C34 1.490(11) . ? 
C34 C35 1.514(12) . ? 
C35 C36 1.484(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 
O8 Rh N1 79.9(2) . . ? 
O8 Rh C12 89.7(3) . . ? 
N1 Rh C12 158.3(4) . . ? 
O8 Rh C11 92.1(3) . . ? 
N1 Rh C11 159.9(4) . . ? 
C12 Rh C11 37.8(4) . . ? 
O8 Rh C15 159.3(4) . . ? 
N1 Rh C15 100.9(3) . . ? 
C12 Rh C15 82.2(4) . . ? 
C11 Rh C15 93.0(4) . . ? 
O8 Rh C16 162.6(4) . . ? 
N1 Rh C16 100.8(3) . . ? 
C12 Rh C16 94.7(4) . . ? 
C11 Rh C16 81.3(4) . . ? 
C15 Rh C16 38.0(4) . . ? 
C2 N1 C6 118.0(6) . . ? 
C2 N1 Rh 112.4(5) . . ? 
C6 N1 Rh 129.7(5) . . ? 
N1 C2 C3 125.4(7) . . ? 
N1 C2 C7 115.6(6) . . ? 
C3 C2 C7 119.1(7) . . ? 
C2 C3 C4 118.9(7) . . ? 
O4 C4 N5 121.1(7) . . ? 
O4 C4 C3 125.5(8) . . ? 
N5 C4 C3 113.4(7) . . ? 
C4 N5 C6 127.6(6) . . ? 
O6 C6 N1 124.3(7) . . ? 
O6 C6 N5 119.2(6) . . ? 
N1 C6 N5 116.5(6) . . ? 
O7 C7 O8 124.3(7) . . ? 
O7 C7 C2 119.6(8) . . ? 
O8 C7 C2 116.0(7) . . ? 
C7 O8 Rh 115.5(5) . . ? 
C12 C11 C18 126.8(12) . . ? 
C12 C11 Rh 71.0(6) . . ? 
C18 C11 Rh 112.5(6) . . ? 
C11 C12 C13 123.6(12) . . ? 
C11 C12 Rh 71.1(6) . . ? 
C13 C12 Rh 111.5(7) . . ? 
C12 C13 C14 118.1(10) . . ? 
C13 C14 C15 113.9(11) . . ? 
C16 C15 C14 125.5(11) . . ? 
C16 C15 Rh 71.5(6) . . ? 
C14 C15 Rh 111.6(7) . . ? 
C15 C16 C17 124.5(11) . . ? 
C15 C16 Rh 70.5(5) . . ? 
C17 C16 Rh 112.4(6) . . ? 
C18 C17 C16 114.6(9) . . ? 
C17 C18 C11 116.6(8) . . ? 
C29 N20 C25 112.6(6) . . ? 
C29 N20 C33 109.1(6) . . ? 
C25 N20 C33 108.6(6) . . ? 
C29 N20 C21 108.7(6) . . ? 
C25 N20 C21 107.2(6) . . ? 
C33 N20 C21 110.7(6) . . ? 
C22 C21 N20 116.7(7) . . ? 
C23' C22 C21 114.9(15) . . ? 
C21 C22 C23 110.5(12) . . ? 
C24 C23 C22 112.1(16) . . ? 
C22 C23' C24' 111.8(19) . . ? 
N20 C25 C26 115.3(7) . . ? 
C27 C26 C25 111.6(8) . . ? 
C28 C27 C26 114.7(9) . . ? 
C30 C29 N20 115.2(7) . . ? 
C29 C30 C31 111.0(8) . . ? 
C32 C31 C30 111.4(9) . . ? 
C34 C33 N20 116.0(7) . . ? 
C33 C34 C35 112.5(9) . . ? 
C36 C35 C34 113.0(10) . . ? 
  
_refine_diff_density_max    0.476 
_refine_diff_density_min   -0.387 
_refine_diff_density_rms    0.067 
  
#=END


data_3 
  
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C35 H59 Cl2 N6 O4 Rh' 
_chemical_formula_weight          801.69 
_chemical_melting_point           ? 
_chemical_compound_source         ? 
  
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0181   0.0091 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'N'  'N'   0.0311   0.0180 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'   0.0492   0.0322 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Cl'  'Cl'   0.3639   0.7018 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Rh'  'Rh'   0.0927   3.6045 
 '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)/n 
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x-1/2, -y-1/2, z-1/2' 
  
_cell_length_a                    8.5900(10) 
_cell_length_b                    23.1529(11) 
_cell_length_c                    20.7496(14) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  97.941(6) 
_cell_angle_gamma                 90.00 
_cell_volume                      4087.2(6) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     26 
_cell_measurement_theta_min       10.56 
_cell_measurement_theta_max       28.01 
  
_exptl_crystal_description        'Platy needles' 
_exptl_crystal_colour             Yellow 
_exptl_crystal_size_max           0.53 
_exptl_crystal_size_mid           0.50 
_exptl_crystal_size_min           0.17 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.303 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              1688 
_exptl_absorpt_coefficient_mu     4.915 
_exptl_absorpt_correction_type    Semi-empirical 
_exptl_absorpt_correction_T_min   0.1465 
_exptl_absorpt_correction_T_max   0.4409 
  
_exptl_special_details 
; 
 ? 
; 
  
_diffrn_ambient_temperature       293(2) 
_diffrn_radiation_wavelength      1.54178 
_diffrn_radiation_type            CuK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device        'Siemens P4' 
_diffrn_measurement_method        '\w scans' 
_diffrn_standards_number          3 
_diffrn_standards_interval_count  97 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         15.45 
_diffrn_reflns_number             6498 
_diffrn_reflns_av_R_equivalents   0.0451 
_diffrn_reflns_av_sigmaI/netI     0.0838 
_diffrn_reflns_limit_h_min        0 
_diffrn_reflns_limit_h_max        9 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        26 
_diffrn_reflns_limit_l_min        -23 
_diffrn_reflns_limit_l_max        23 
_diffrn_reflns_theta_min          2.87 
_diffrn_reflns_theta_max          59.99 
_reflns_number_total              6046 
_reflns_number_observed           4038 
_reflns_observed_criterion        >2sigma(I) 
  
_computing_data_collection        'Siemens XSCANS' 
_computing_cell_refinement        'Siemens XSCANS' 
_computing_data_reduction         'Siemens SHELXTL' 
_computing_structure_solution     'SHELXS-86 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)' 
_computing_molecular_graphics     'Siemens SHELXTL' 
_computing_publication_material   'Siemens SHELXTL' 
  
_refine_special_details 
; 
 Refinement on F^2^ for ALL reflections except for 3 with very negative F^2^ 
 or flagged by the user for potential systematic errors.  Weighted R-factors 
 wR and all goodnesses 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 observed criterion 
 of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0818P)^2^+0.3155P] 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     ? 
_refine_ls_extinction_method      SHELXL 
_refine_ls_extinction_coef        0.00096(11) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' 
_refine_ls_number_reflns          6043 
_refine_ls_number_parameters      454 
_refine_ls_number_restraints      5 
_refine_ls_R_factor_all           0.1047 
_refine_ls_R_factor_obs           0.0614 
_refine_ls_wR_factor_all          0.1685 
_refine_ls_wR_factor_obs          0.1380 
_refine_ls_goodness_of_fit_all    1.040 
_refine_ls_goodness_of_fit_obs    1.084 
_refine_ls_restrained_S_all       1.065 
_refine_ls_restrained_S_obs       1.083 
_refine_ls_shift/esd_max          0.013 
_refine_ls_shift/esd_mean         0.001 
  
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_thermal_displace_type 
 _atom_site_occupancy 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_group 
Rh Rh 0.19058(7) 0.16030(2) 0.49646(2) 0.0574(2) Uani 1 d . . 
N1 N 0.2764(7) 0.2451(2) 0.4975(2) 0.0526(13) Uani 1 d . . 
C2 C 0.2429(10) 0.2709(3) 0.4388(3) 0.061(2) Uani 1 d . . 
C3 C 0.2881(11) 0.3247(3) 0.4249(3) 0.070(2) Uani 1 d . . 
H3A H 0.2617(11) 0.3397(3) 0.3833(3) 0.083 Uiso 1 calc R . 
C4 C 0.3765(12) 0.3585(3) 0.4745(3) 0.070(2) Uani 1 d . . 
O4 O 0.4285(12) 0.4070(3) 0.4695(3) 0.112(3) Uani 1 d . . 
N5 N 0.4007(7) 0.3308(2) 0.5345(2) 0.0523(12) Uani 1 d D . 
H5A H 0.4544(93) 0.3499(35) 0.5683(29) 0.082(27) Uiso 1 d D . 
C6 C 0.3571(8) 0.2757(3) 0.5474(3) 0.0495(14) Uani 1 d . . 
O6 O 0.3914(7) 0.2570(2) 0.6032(2) 0.0627(13) Uani 1 d . . 
C7 C 0.1468(13) 0.2345(3) 0.3861(3) 0.078(3) Uani 1 d . . 
O7 O 0.1175(12) 0.2544(3) 0.3316(3) 0.118(3) Uani 1 d . . 
O8 O 0.1073(9) 0.1852(2) 0.4029(3) 0.085(2) Uani 1 d . . 
C11 C 0.0268(12) 0.0923(4) 0.4926(5) 0.082(3) Uani 1 d . . 
H11A H -0.0396(12) 0.1150(4) 0.4638(5) 0.099 Uiso 1 calc R . 
C12 C 0.1597(14) 0.0720(3) 0.4714(4) 0.086(3) Uani 1 d . . 
H12A H 0.1767(14) 0.0817(3) 0.4294(4) 0.104 Uiso 1 calc R . 
C13 C 0.2837(14) 0.0340(4) 0.5123(5) 0.094(3) Uani 1 d . . 
H13A H 0.2305(14) 0.0072(4) 0.5379(5) 0.113 Uiso 1 calc R . 
H13B H 0.3388(14) 0.0114(4) 0.4832(5) 0.113 Uiso 1 calc R . 
C14 C 0.4017(17) 0.0680(4) 0.5572(6) 0.112(4) Uani 1 d . . 
H14A H 0.4258(17) 0.0468(4) 0.5977(6) 0.135 Uiso 1 calc R . 
H14B H 0.4978(17) 0.0708(4) 0.5378(6) 0.135 Uiso 1 calc R . 
C15 C 0.3508(12) 0.1272(3) 0.5723(4) 0.075(2) Uani 1 d . . 
H15A H 0.4172(12) 0.1573(3) 0.5643(4) 0.090 Uiso 1 calc R . 
C16 C 0.2157(12) 0.1419(3) 0.5969(4) 0.073(2) Uani 1 d . . 
H16A H 0.1947(12) 0.1807(3) 0.6034(4) 0.087 Uiso 1 calc R . 
C17 C 0.0998(17) 0.0969(5) 0.6137(5) 0.112(4) Uani 1 d . . 
H17A H 0.1572(17) 0.0623(5) 0.6287(5) 0.134 Uiso 1 calc R . 
H17B H 0.0486(17) 0.1113(5) 0.6493(5) 0.134 Uiso 1 calc R . 
C18 C -0.0228(15) 0.0814(6) 0.5584(6) 0.109(4) Uani 1 d . . 
H18A H -0.1171(15) 0.1036(6) 0.5620(6) 0.131 Uiso 1 calc R . 
H18B H -0.0489(15) 0.0409(6) 0.5618(6) 0.131 Uiso 1 calc R . 
N20 N 0.5617(7) 0.3989(2) 0.6502(2) 0.0543(13) Uani 1 d . . 
C21 C 0.5827(10) 0.4558(3) 0.6439(4) 0.066(2) Uani 1 d . . 
N21 N 0.5911(13) 0.4745(3) 0.5829(4) 0.095(3) Uani 1 d D . 
H21A H 0.6066(88) 0.4515(26) 0.5494(23) 0.054(19) Uiso 1 d D . 
H21B H 0.6046(118) 0.5128(8) 0.5791(43) 0.087(28) Uiso 1 d D . 
C22 C 0.6073(14) 0.4931(3) 0.6970(5) 0.093(3) Uani 1 d . . 
H22A H 0.6277(14) 0.5322(3) 0.6919(5) 0.112 Uiso 1 calc R . 
C23 C 0.5999(14) 0.4694(4) 0.7577(4) 0.093(3) Uani 1 d . . 
H23A H 0.6082(14) 0.4938(4) 0.7936(4) 0.112 Uiso 1 calc R . 
C24 C 0.5814(11) 0.4127(4) 0.7671(4) 0.077(2) Uani 1 d . . 
H24A H 0.5800(11) 0.3973(4) 0.8084(4) 0.092 Uiso 1 calc R . 
C25 C 0.5639(8) 0.3772(3) 0.7107(3) 0.0534(15) Uani 1 d . . 
N25 N 0.5550(9) 0.3195(3) 0.7162(3) 0.071(2) Uani 1 d D . 
H25A H 0.5227(113) 0.3034(39) 0.6772(22) 0.086(28) Uiso 1 d D . 
H25B H 0.5622(85) 0.3009(26) 0.7546(16) 0.050(18) Uiso 1 d D . 
N30 N 0.0489(9) 0.3597(5) 0.6865(4) 0.102(3) Uani 1 d . . 
C31 C -0.0870(10) 0.3387(6) 0.6372(5) 0.103(3) Uani 1 d . . 
H31A H -0.1473(10) 0.3109(6) 0.6585(5) 0.124 Uiso 1 calc R . 
H31B H -0.1554(10) 0.3713(6) 0.6245(5) 0.124 Uiso 1 calc R . 
C32 C -0.0433(15) 0.3112(8) 0.5764(6) 0.126(5) Uani 1 d . . 
H32A H 0.0226(15) 0.2776(8) 0.5875(6) 0.151 Uiso 1 calc R . 
H32B H 0.0146(15) 0.3384(8) 0.5532(6) 0.151 Uiso 1 calc R . 
C33 C -0.1962(21) 0.2931(9) 0.5334(8) 0.170(8) Uani 1 d . . 
H33A H -0.2598(21) 0.2729(9) 0.5613(8) 0.203 Uiso 1 calc R . 
H33B H -0.2521(21) 0.3283(9) 0.5195(8) 0.203 Uiso 1 calc R . 
C34 C -0.1940(29) 0.2630(14) 0.4843(15) 0.317(23) Uani 1 d . . 
H34A H -0.2997(29) 0.2562(14) 0.4640(15) 0.475 Uiso 1 calc R . 
H34B H -0.1441(29) 0.2268(14) 0.4965(15) 0.475 Uiso 1 calc R . 
H34C H -0.1365(29) 0.2826(14) 0.4544(15) 0.475 Uiso 1 calc R . 
C35 C 0.1578(12) 0.3086(7) 0.7103(5) 0.109(4) Uani 1 d . . 
H35A H 0.2046(12) 0.2940(7) 0.6736(5) 0.130 Uiso 1 calc R . 
H35B H 0.2425(12) 0.3232(7) 0.7419(5) 0.130 Uiso 1 calc R . 
C36 C 0.0799(16) 0.2578(7) 0.7413(7) 0.126(5) Uani 1 d . . 
H36A H 0.0179(16) 0.2726(7) 0.7734(7) 0.151 Uiso 1 calc R . 
H36B H 0.0091(16) 0.2381(7) 0.7080(7) 0.151 Uiso 1 calc R . 
C37 C 0.1952(22) 0.2163(10) 0.7727(7) 0.151(7) Uani 1 d . . 
H37A H 0.2535(22) 0.2006(10) 0.7399(7) 0.181 Uiso 1 calc R . 
H37B H 0.2692(22) 0.2369(10) 0.8041(7) 0.181 Uiso 1 calc R . 
C38 C 0.1304(26) 0.1687(10) 0.8058(9) 0.181(9) Uani 1 d . . 
H38A H 0.2141(26) 0.1440(10) 0.8247(9) 0.272 Uiso 1 calc R . 
H38B H 0.0592(26) 0.1471(10) 0.7751(9) 0.272 Uiso 1 calc R . 
H38C H 0.0750(26) 0.1835(10) 0.8394(9) 0.272 Uiso 1 calc R . 
C39 C -0.0236(13) 0.3857(6) 0.7423(6) 0.104(3) Uani 1 d . . 
H39A H -0.0814(13) 0.3558(6) 0.7616(6) 0.125 Uiso 1 calc R . 
H39B H -0.0983(13) 0.4152(6) 0.7251(6) 0.125 Uiso 1 calc R . 
C40 C 0.0954(16) 0.4127(7) 0.7957(6) 0.121(5) Uani 1 d . . 
H40A H 0.1927(16) 0.3909(7) 0.7998(6) 0.145 Uiso 1 calc R . 
H40B H 0.1180(16) 0.4520(7) 0.7836(6) 0.145 Uiso 1 calc R . 
C41 C 0.0323(24) 0.4129(8) 0.8603(8) 0.150(6) Uani 1 d . . 
H41A H 0.0989(24) 0.4384(8) 0.8893(8) 0.180 Uiso 1 calc R . 
H41B H -0.0713(24) 0.4304(8) 0.8532(8) 0.180 Uiso 1 calc R . 
C42 C 0.0198(34) 0.3622(10) 0.8923(9) 0.205(11) Uani 1 d . . 
H42A H -0.0217(34) 0.3694(10) 0.9322(9) 0.308 Uiso 1 calc R . 
H42B H 0.1217(34) 0.3447(10) 0.9018(9) 0.308 Uiso 1 calc R . 
H42C H -0.0494(34) 0.3366(10) 0.8654(9) 0.308 Uiso 1 calc R . 
C43 C 0.1470(13) 0.4026(7) 0.6573(6) 0.115(5) Uani 1 d . . 
H43A H 0.1927(13) 0.3837(7) 0.6227(6) 0.138 Uiso 1 calc R . 
H43B H 0.2329(13) 0.4139(7) 0.6903(6) 0.138 Uiso 1 calc R . 
C44 C 0.0645(17) 0.4572(9) 0.6298(7) 0.136(6) Uani 1 d . . 
H44A H -0.0209(17) 0.4467(9) 0.5963(7) 0.163 Uiso 1 calc R . 
H44B H 0.0198(17) 0.4770(9) 0.6641(7) 0.163 Uiso 1 calc R . 
C45 C 0.1715(23) 0.4963(12) 0.6022(10) 0.176(9) Uani 1 d . . 
H45A H 0.2170(23) 0.4762(12) 0.5683(10) 0.211 Uiso 1 calc R . 
H45B H 0.2566(23) 0.5068(12) 0.6359(10) 0.211 Uiso 1 calc R . 
C46 C 0.0896(31) 0.5523(11) 0.5733(9) 0.197(11) Uani 1 d . . 
H46A H 0.1651(31) 0.5762(11) 0.5560(9) 0.295 Uiso 1 calc R . 
H46B H 0.0464(31) 0.5729(11) 0.6068(9) 0.295 Uiso 1 calc R . 
H46C H 0.0068(31) 0.5423(11) 0.5392(9) 0.295 Uiso 1 calc R . 
C50 C 0.5813(17) 0.1531(6) 0.7211(5) 0.118(4) Uani 1 d . . 
H50A H 0.5000(17) 0.1732(6) 0.6925(5) 0.142 Uiso 1 calc R . 
H50B H 0.6148(17) 0.1780(6) 0.7580(5) 0.142 Uiso 1 calc R . 
Cl51 Cl 0.5051(9) 0.0908(3) 0.7479(3) 0.198(3) Uani 1 d . . 
Cl52 Cl 0.7365(6) 0.1402(4) 0.6804(3) 0.215(3) Uani 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 
Rh 0.0766(3) 0.0415(3) 0.0498(3) -0.0061(2) -0.0063(2) -0.0034(3) 
N1 0.068(4) 0.048(3) 0.040(2) -0.005(2) -0.001(2) 0.003(2) 
C2 0.093(5) 0.046(3) 0.038(3) -0.007(2) -0.011(3) 0.009(3) 
C3 0.103(6) 0.058(4) 0.043(3) 0.009(3) -0.007(3) 0.001(4) 
C4 0.101(6) 0.055(4) 0.052(4) 0.009(3) -0.002(4) -0.002(4) 
O4 0.197(9) 0.054(3) 0.074(3) 0.021(3) -0.026(4) -0.037(4) 
N5 0.068(3) 0.042(3) 0.045(2) 0.000(2) 0.001(2) -0.008(2) 
C6 0.064(4) 0.042(3) 0.042(3) 0.001(2) 0.005(3) -0.005(3) 
O6 0.092(4) 0.054(2) 0.038(2) 0.004(2) -0.006(2) -0.017(2) 
C7 0.123(7) 0.061(4) 0.042(3) -0.009(3) -0.016(4) -0.003(4) 
O7 0.213(9) 0.076(4) 0.048(3) 0.001(3) -0.039(4) -0.023(5) 
O8 0.120(5) 0.061(3) 0.063(3) -0.013(2) -0.028(3) -0.005(3) 
C11 0.092(7) 0.054(4) 0.095(6) -0.019(4) -0.008(5) -0.017(4) 
C12 0.135(9) 0.054(4) 0.063(4) -0.015(3) -0.010(5) -0.010(5) 
C13 0.118(9) 0.057(4) 0.101(6) -0.008(4) -0.014(6) 0.005(5) 
C14 0.136(10) 0.064(5) 0.121(8) -0.010(5) -0.037(7) 0.024(6) 
C15 0.106(7) 0.046(4) 0.069(4) 0.002(3) -0.007(4) -0.010(4) 
C16 0.103(7) 0.054(4) 0.059(4) 0.000(3) 0.005(4) -0.019(4) 
C17 0.145(11) 0.095(7) 0.097(7) -0.012(6) 0.020(7) -0.049(8) 
C18 0.101(8) 0.101(8) 0.127(9) -0.025(6) 0.015(7) -0.039(7) 
N20 0.063(3) 0.047(3) 0.050(3) 0.005(2) -0.005(2) -0.006(2) 
C21 0.075(5) 0.050(3) 0.069(4) 0.007(3) -0.006(4) -0.007(3) 
N21 0.152(8) 0.053(4) 0.072(4) 0.014(3) -0.008(5) -0.021(4) 
C22 0.131(9) 0.048(4) 0.091(6) -0.010(4) -0.022(6) -0.004(5) 
C23 0.119(8) 0.087(6) 0.066(5) -0.024(4) -0.015(5) 0.010(6) 
C24 0.086(6) 0.090(6) 0.050(4) -0.009(4) -0.002(4) 0.000(5) 
C25 0.044(3) 0.065(4) 0.050(3) 0.005(3) 0.001(3) -0.006(3) 
N25 0.092(5) 0.065(3) 0.048(3) 0.011(2) -0.012(3) -0.019(3) 
N30 0.056(4) 0.149(9) 0.101(5) -0.050(5) 0.004(4) 0.017(5) 
C31 0.054(5) 0.135(9) 0.117(7) -0.046(7) -0.002(4) 0.005(6) 
C32 0.090(8) 0.180(14) 0.101(7) -0.053(8) -0.010(6) 0.030(8) 
C33 0.139(13) 0.187(17) 0.158(13) -0.079(13) -0.066(11) 0.026(12) 
C34 0.192(24) 0.287(36) 0.409(42) -0.172(34) -0.175(28) 0.095(25) 
C35 0.056(5) 0.169(12) 0.098(7) -0.042(7) 0.002(5) 0.020(7) 
C36 0.087(8) 0.145(12) 0.144(11) -0.054(10) 0.012(8) 0.006(8) 
C37 0.145(14) 0.203(20) 0.099(9) -0.008(10) -0.001(8) 0.054(14) 
C38 0.183(19) 0.199(22) 0.147(14) -0.001(14) -0.030(13) 0.045(19) 
C39 0.079(7) 0.123(9) 0.113(8) -0.036(7) 0.020(6) 0.005(6) 
C40 0.108(9) 0.151(12) 0.103(8) -0.055(8) 0.012(6) -0.013(9) 
C41 0.171(16) 0.131(12) 0.142(12) -0.054(10) 0.004(11) 0.007(12) 
C42 0.311(34) 0.166(20) 0.159(16) -0.018(14) 0.104(19) -0.015(21) 
C43 0.063(6) 0.185(14) 0.098(7) -0.030(8) 0.013(5) -0.004(8) 
C44 0.087(8) 0.197(18) 0.121(9) -0.034(10) 0.010(7) 0.004(11) 
C45 0.123(14) 0.236(28) 0.169(16) -0.030(17) 0.024(12) -0.031(17) 
C46 0.245(28) 0.198(24) 0.140(14) 0.001(14) 0.003(15) -0.067(22) 
C50 0.139(10) 0.120(9) 0.083(6) -0.022(6) -0.028(6) 0.027(9) 
Cl51 0.285(8) 0.155(4) 0.157(4) 0.043(3) 0.042(4) 0.030(5) 
Cl52 0.107(3) 0.272(9) 0.264(7) -0.049(6) 0.018(3) 0.016(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 
Rh O8 2.056(5) . ? 
Rh C15 2.088(8) . ? 
Rh N1 2.097(5) . ? 
Rh C11 2.106(8) . ? 
Rh C16 2.108(7) . ? 
Rh C12 2.117(8) . ? 
N1 C2 1.351(8) . ? 
N1 C6 1.362(8) . ? 
C2 C3 1.348(11) . ? 
C2 C7 1.529(9) . ? 
C3 C4 1.424(11) . ? 
C4 O4 1.219(10) . ? 
C4 N5 1.391(8) . ? 
N5 C6 1.364(8) . ? 
C6 O6 1.233(7) . ? 
C7 O7 1.215(9) . ? 
C7 O8 1.255(11) . ? 
C11 C12 1.363(15) . ? 
C11 C18 1.51(2) . ? 
C12 C13 1.543(13) . ? 
C13 C14 1.501(14) . ? 
C14 C15 1.485(12) . ? 
C15 C16 1.374(14) . ? 
C16 C17 1.515(13) . ? 
C17 C18 1.490(15) . ? 
N20 C21 1.339(9) . ? 
N20 C25 1.348(8) . ? 
C21 N21 1.348(11) . ? 
C21 C22 1.395(11) . ? 
C22 C23 1.384(14) . ? 
C23 C24 1.340(14) . ? 
C24 C25 1.420(10) . ? 
C25 N25 1.344(10) . ? 
N30 C43 1.48(2) . ? 
N30 C39 1.512(13) . ? 
N30 C31 1.523(11) . ? 
N30 C35 1.55(2) . ? 
C31 C32 1.506(14) . ? 
C32 C33 1.54(2) . ? 
C33 C34 1.24(3) . ? 
C35 C36 1.54(2) . ? 
C36 C37 1.47(2) . ? 
C37 C38 1.45(3) . ? 
C39 C40 1.533(14) . ? 
C40 C41 1.51(2) . ? 
C41 C42 1.36(2) . ? 
C43 C44 1.52(2) . ? 
C44 C45 1.46(3) . ? 
C45 C46 1.56(3) . ? 
C50 Cl52 1.70(2) . ? 
C50 Cl51 1.71(2) . ? 
  
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
O8 Rh C15 157.1(4) . . ? 
O8 Rh N1 79.8(2) . . ? 
C15 Rh N1 98.2(3) . . ? 
O8 Rh C11 91.7(3) . . ? 
C15 Rh C11 97.0(4) . . ? 
N1 Rh C11 158.9(3) . . ? 
O8 Rh C16 164.6(4) . . ? 
C15 Rh C16 38.2(4) . . ? 
N1 Rh C16 101.0(2) . . ? 
C11 Rh C16 82.1(3) . . ? 
O8 Rh C12 91.3(3) . . ? 
C15 Rh C12 83.0(3) . . ? 
N1 Rh C12 159.9(4) . . ? 
C11 Rh C12 37.6(4) . . ? 
C16 Rh C12 92.3(3) . . ? 
C2 N1 C6 118.6(6) . . ? 
C2 N1 Rh 111.9(4) . . ? 
C6 N1 Rh 129.5(4) . . ? 
C3 C2 N1 124.6(6) . . ? 
C3 C2 C7 120.0(6) . . ? 
N1 C2 C7 115.4(6) . . ? 
C2 C3 C4 119.6(6) . . ? 
O4 C4 N5 119.3(7) . . ? 
O4 C4 C3 127.6(7) . . ? 
N5 C4 C3 113.1(6) . . ? 
C6 N5 C4 126.5(5) . . ? 
O6 C6 N1 124.2(6) . . ? 
O6 C6 N5 118.3(5) . . ? 
N1 C6 N5 117.5(5) . . ? 
O7 C7 O8 125.1(7) . . ? 
O7 C7 C2 118.6(7) . . ? 
O8 C7 C2 116.3(6) . . ? 
C7 O8 Rh 116.5(4) . . ? 
C12 C11 C18 126.1(10) . . ? 
C12 C11 Rh 71.6(5) . . ? 
C18 C11 Rh 111.2(6) . . ? 
C11 C12 C13 124.4(9) . . ? 
C11 C12 Rh 70.7(5) . . ? 
C13 C12 Rh 111.2(5) . . ? 
C14 C13 C12 113.5(7) . . ? 
C15 C14 C13 115.0(9) . . ? 
C16 C15 C14 126.5(10) . . ? 
C16 C15 Rh 71.7(5) . . ? 
C14 C15 Rh 111.3(6) . . ? 
C15 C16 C17 122.0(9) . . ? 
C15 C16 Rh 70.1(5) . . ? 
C17 C16 Rh 112.7(6) . . ? 
C18 C17 C16 113.9(9) . . ? 
C17 C18 C11 113.5(10) . . ? 
C21 N20 C25 118.2(6) . . ? 
N20 C21 N21 115.7(7) . . ? 
N20 C21 C22 122.7(7) . . ? 
N21 C21 C22 121.4(7) . . ? 
C23 C22 C21 116.9(8) . . ? 
C24 C23 C22 122.9(8) . . ? 
C23 C24 C25 116.6(8) . . ? 
N25 C25 N20 117.1(6) . . ? 
N25 C25 C24 120.3(7) . . ? 
N20 C25 C24 122.5(7) . . ? 
C43 N30 C39 111.3(10) . . ? 
C43 N30 C31 111.4(10) . . ? 
C39 N30 C31 106.4(8) . . ? 
C43 N30 C35 106.9(9) . . ? 
C39 N30 C35 110.8(9) . . ? 
C31 N30 C35 110.1(9) . . ? 
C32 C31 N30 116.2(8) . . ? 
C31 C32 C33 107.9(11) . . ? 
C34 C33 C32 121.4(19) . . ? 
C36 C35 N30 116.1(9) . . ? 
C37 C36 C35 112.4(13) . . ? 
C38 C37 C36 115.4(17) . . ? 
N30 C39 C40 114.3(9) . . ? 
C41 C40 C39 110.9(12) . . ? 
C42 C41 C40 119.3(15) . . ? 
N30 C43 C44 116.6(10) . . ? 
C45 C44 C43 112.1(15) . . ? 
C44 C45 C46 113.1(18) . . ? 
Cl52 C50 Cl51 112.1(8) . . ? 
  
_refine_diff_density_max    0.616 
_refine_diff_density_min   -0.468 
_refine_diff_density_rms    0.078