  
data_mj09 
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C54 H64 Cl2 N4 O Rh2' 
_chemical_formula_weight          1061.81 
  
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0033   0.0016 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'N'  'N'   0.0061   0.0033 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'   0.0106   0.0060 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Cl'  'Cl'   0.1484   0.1585 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Rh'  'Rh'  -1.1178   0.9187 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
  
_symmetry_cell_setting            Trigonal 
_symmetry_space_group_name_H-M    P 32 2 1 
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-y, x-y, z+2/3' 
 '-x+y, -x, z+1/3' 
 'y, x, -z' 
 'x-y, -y, -z+1/3' 
 '-x, -x+y, -z+2/3' 
  
_cell_length_a                    11.9962(3) 
_cell_length_b                    11.9962(3) 
_cell_length_c                    28.3024(16) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 120.00 
_cell_volume                      3527.3(2) 
_cell_formula_units_Z             3 
_cell_measurement_temperature     173(2) 
_cell_measurement_reflns_used     70 
_cell_measurement_theta_min       2.0 
_cell_measurement_theta_max       28.0 
  
_exptl_crystal_description        hx. 
_exptl_crystal_colour             yellow 
_exptl_crystal_size_max           0.12 
_exptl_crystal_size_mid           0.11 
_exptl_crystal_size_min           0.02 
_exptl_crystal_density_meas       'not measured' 
_exptl_crystal_density_diffrn     1.500 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1644 
_exptl_absorpt_coefficient_mu     0.860 
_exptl_absorpt_correction_type    integration 
_exptl_absorpt_correction_T_min   0.9136 
_exptl_absorpt_correction_T_max   0.9787 
_exptl_absorpt_process_details 
'based on measured indexed crystal faces, Bruker SHELXTL  v6.12 (Bruker 1998)' 
  
_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   'SMART CCD area detector' 
_diffrn_measurement_method        'ω scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          0 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         1 
_diffrn_reflns_number             22318 
_diffrn_reflns_av_R_equivalents   0.0956 
_diffrn_reflns_av_sigmaI/netI     0.1028 
_diffrn_reflns_limit_h_min        -6 
_diffrn_reflns_limit_h_max        15 
_diffrn_reflns_limit_k_min        -15 
_diffrn_reflns_limit_k_max        14 
_diffrn_reflns_limit_l_min        -36 
_diffrn_reflns_limit_l_max        36 
_diffrn_reflns_theta_min          1.96 
_diffrn_reflns_theta_max          27.50 
_reflns_number_total              5373 
_reflns_number_gt                 3677 
_reflns_threshold_expression      'I>2σ(I)' 
  
_computing_data_collection        'Bruker SMART v5.624 (Bruker 1998)' 
_computing_cell_refinement  'Bruker SMART v5.624 & SAINT 6.36a (Bruker 1998)' 
_computing_data_reduction         'Bruker SHELXTL v6.14 (Bruker 2000)' 
_computing_structure_solution     'Bruker SHELXTL v6.14' 
_computing_structure_refinement   'Bruker SHELXTL v6.14' 
_computing_molecular_graphics     'Bruker SHELXTL v6.14' 
_computing_publication_material   'Bruker SHELXTL v6.14' 
  
_refine_special_details 
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
; 
  
_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
 'calc w=1/[σ²(Fo²)+(0.0495P)²] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_abs_structure_details 
 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    0.52(5) 
_refine_ls_number_reflns          5373 
_refine_ls_number_parameters      263 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0985 
_refine_ls_R_factor_gt            0.0530 
_refine_ls_wR_factor_ref          0.1127 
_refine_ls_wR_factor_gt           0.1014 
_refine_ls_goodness_of_fit_ref    1.007 
_refine_ls_restrained_S_all       1.007 
_refine_ls_shift/su_max           0.001 
_refine_ls_shift/su_mean          0.000 
  
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_adp_type 
 _atom_site_occupancy 
 _atom_site_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Rh Rh 0.63542(5) 0.56556(5) 0.267361(16) 0.03046(13) Uani 1 1 d . . . 
Cl Cl 0.61450(15) 0.57999(17) 0.35049(5) 0.0431(4) Uani 1 1 d . . . 
C16 C 1.0028(6) 0.5976(6) 0.2751(2) 0.0328(15) Uani 1 1 d . . . 
C11 C 0.9238(6) 0.4636(6) 0.2773(2) 0.0335(15) Uani 1 1 d . . . 
C13 C 1.1056(6) 0.4391(6) 0.2729(2) 0.0437(16) Uani 1 1 d . . . 
H13A H 1.1440 0.3865 0.2720 0.052 Uiso 1 1 calc R . . 
N2 N 0.9218(5) 0.6494(5) 0.27447(17) 0.0282(12) Uani 1 1 d . . . 
C21 C 1.0554(6) 1.0641(6) 0.3788(2) 0.0304(14) Uani 1 1 d . . . 
N1 N 0.7982(4) 0.4403(4) 0.27786(16) 0.0312(12) Uani 1 1 d . . . 
C20 C 1.1350(5) 1.0996(5) 0.3385(2) 0.0299(13) Uani 1 1 d . . . 
C12 C 0.9740(6) 0.3815(7) 0.27640(19) 0.0412(16) Uani 1 1 d . . . 
H12A H 0.9205 0.2907 0.2781 0.049 Uiso 1 1 calc R . . 
C9 C 0.7942(6) 0.5529(5) 0.27528(19) 0.0302(14) Uani 1 1 d . . . 
C17 C 0.9628(6) 0.7864(6) 0.2682(2) 0.0351(15) Uani 1 1 d . . . 
H17A H 0.8855 0.7939 0.2624 0.042 Uiso 1 1 calc R . . 
H17B H 1.0176 0.8183 0.2397 0.042 Uiso 1 1 calc R . . 
C18 C 1.0370(5) 0.8733(6) 0.30978(19) 0.0304(12) Uani 1 1 d . . . 
H18A H 1.1185 0.8709 0.3141 0.036 Uiso 1 1 calc R . . 
C4 C 0.4345(6) 0.5118(7) 0.2595(2) 0.0408(17) Uani 1 1 d . . . 
H4A H 0.3850 0.4864 0.2898 0.049 Uiso 1 1 calc R . . 
C10 C 0.6851(6) 0.3110(6) 0.2812(2) 0.0451(18) Uani 1 1 d . . . 
H10A H 0.6068 0.3173 0.2811 0.068 Uiso 1 1 calc R . . 
H10B H 0.6893 0.2701 0.3106 0.068 Uiso 1 1 calc R . . 
H10C H 0.6837 0.2592 0.2542 0.068 Uiso 1 1 calc R . . 
C15 C 1.1362(6) 0.6552(6) 0.2721(2) 0.0335(15) Uani 1 1 d . . . 
H15A H 1.1907 0.7459 0.2710 0.040 Uiso 1 1 calc R . . 
C22 C 1.0941(7) 1.1348(6) 0.4187(2) 0.0380(15) Uani 1 1 d . . . 
H22A H 1.0386 1.1105 0.4453 0.046 Uiso 1 1 calc R . . 
C24 C 1.2985(6) 1.2806(6) 0.3815(3) 0.0400(16) Uani 1 1 d . . . 
H24A H 1.3822 1.3542 0.3829 0.048 Uiso 1 1 calc R . . 
C14 C 1.1843(7) 0.5720(6) 0.2707(2) 0.0428(16) Uani 1 1 d . . . 
H14A H 1.2747 0.6070 0.2682 0.051 Uiso 1 1 calc R . . 
C25 C 1.2573(6) 1.2087(5) 0.3405(2) 0.0373(15) Uani 1 1 d . . . 
H25A H 1.3122 1.2334 0.3136 0.045 Uiso 1 1 calc R . . 
C1 C 0.6059(7) 0.4913(6) 0.19780(19) 0.0388(15) Uani 1 1 d . . . 
H1A H 0.6478 0.4388 0.1914 0.047 Uiso 1 1 calc R . . 
C2 C 0.4684(7) 0.4293(6) 0.1809(2) 0.0429(16) Uani 1 1 d . . . 
H2A H 0.4440 0.3450 0.1665 0.051 Uiso 1 1 calc R . . 
H2B H 0.4619 0.4842 0.1562 0.051 Uiso 1 1 calc R . . 
C7 C 0.6565(7) 0.7222(7) 0.1829(2) 0.0476(17) Uani 1 1 d . . . 
H7A H 0.6498 0.7217 0.1480 0.057 Uiso 1 1 calc R . . 
H7B H 0.7269 0.8083 0.1924 0.057 Uiso 1 1 calc R . . 
C8 C 0.6913(7) 0.6239(6) 0.19720(18) 0.0378(16) Uani 1 1 d . . . 
H8A H 0.7824 0.6485 0.1900 0.045 Uiso 1 1 calc R . . 
C5 C 0.5046(6) 0.6392(7) 0.2530(2) 0.0426(17) Uani 1 1 d . . . 
H5A H 0.4980 0.6918 0.2791 0.051 Uiso 1 1 calc R . . 
C6 C 0.5301(8) 0.7018(7) 0.2042(2) 0.053(2) Uani 1 1 d . . . 
H6A H 0.5338 0.7859 0.2068 0.063 Uiso 1 1 calc R . . 
H6B H 0.4580 0.6465 0.1828 0.063 Uiso 1 1 calc R . . 
C23 C 1.2184(6) 1.2459(6) 0.4205(2) 0.0434(17) Uani 1 1 d . . . 
H23A H 1.2466 1.2963 0.4485 0.052 Uiso 1 1 calc R . . 
C19 C 1.0725(6) 1.0135(6) 0.2965(2) 0.0316(14) Uani 1 1 d . . . 
H19A H 1.1292 1.0449 0.2680 0.038 Uiso 1 1 calc R . . 
C3 C 0.3747(6) 0.4095(7) 0.2204(2) 0.0451(17) Uani 1 1 d . . . 
H3A H 0.3435 0.3234 0.2346 0.054 Uiso 1 1 calc R . . 
H3B H 0.2995 0.4114 0.2070 0.054 Uiso 1 1 calc R . . 
  
  
_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 C9 1.998(6) . ? 
Rh C8 2.101(5) . ? 
Rh C1 2.116(6) . ? 
Rh C4 2.172(6) . ? 
Rh C5 2.190(6) . ? 
Rh Cl 2.3816(15) . ? 
C16 N2 1.391(7) . ? 
C16 C15 1.393(8) . ? 
C16 C11 1.401(9) . ? 
C11 C12 1.387(9) . ? 
C11 N1 1.389(7) . ? 
C13 C12 1.374(8) . ? 
C13 C14 1.390(9) . ? 
C13 H13A 0.9500 . ? 
N2 C9 1.383(7) . ? 
N2 C17 1.472(7) . ? 
C21 C22 1.346(8) . ? 
C21 C20 1.410(8) . ? 
C21 C19 1.525(8) 6_765 ? 
N1 C9 1.377(7) . ? 
N1 C10 1.467(7) . ? 
C20 C25 1.396(8) . ? 
C20 C19 1.506(8) . ? 
C12 H12A 0.9500 . ? 
C17 C18 1.528(8) . ? 
C17 H17A 0.9900 . ? 
C17 H17B 0.9900 . ? 
C18 C18 1.539(11) 6_765 ? 
C18 C19 1.560(8) . ? 
C18 H18A 1.0000 . ? 
C4 C5 1.338(9) . ? 
C4 C3 1.537(9) . ? 
C4 H4A 1.0000 . ? 
C10 H10A 0.9800 . ? 
C10 H10B 0.9800 . ? 
C10 H10C 0.9800 . ? 
C15 C14 1.380(8) . ? 
C15 H15A 0.9500 . ? 
C22 C23 1.420(10) . ? 
C22 H22A 0.9500 . ? 
C24 C25 1.382(9) . ? 
C24 C23 1.385(9) . ? 
C24 H24A 0.9500 . ? 
C14 H14A 0.9500 . ? 
C25 H25A 0.9500 . ? 
C1 C8 1.396(8) . ? 
C1 C2 1.509(9) . ? 
C1 H1A 1.0000 . ? 
C2 C3 1.518(9) . ? 
C2 H2A 0.9900 . ? 
C2 H2B 0.9900 . ? 
C7 C8 1.491(9) . ? 
C7 C6 1.533(9) . ? 
C7 H7A 0.9900 . ? 
C7 H7B 0.9900 . ? 
C8 H8A 1.0000 . ? 
C5 C6 1.529(9) . ? 
C5 H5A 1.0000 . ? 
C6 H6A 0.9900 . ? 
C6 H6B 0.9900 . ? 
C23 H23A 0.9500 . ? 
C19 C21 1.525(8) 6_765 ? 
C19 H19A 1.0000 . ? 
C3 H3A 0.9900 . ? 
C3 H3B 0.9900 . ? 
  
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 
C9 Rh C8 88.5(2) . . ? 
C9 Rh C1 92.2(3) . . ? 
C8 Rh C1 38.7(2) . . ? 
C9 Rh C4 161.3(2) . . ? 
C8 Rh C4 97.1(3) . . ? 
C1 Rh C4 81.5(3) . . ? 
C9 Rh C5 162.6(3) . . ? 
C8 Rh C5 82.2(3) . . ? 
C1 Rh C5 89.7(3) . . ? 
C4 Rh C5 35.7(2) . . ? 
C9 Rh Cl 91.94(16) . . ? 
C8 Rh Cl 159.59(17) . . ? 
C1 Rh Cl 161.45(18) . . ? 
C4 Rh Cl 88.92(19) . . ? 
C5 Rh Cl 91.78(18) . . ? 
N2 C16 C15 131.6(6) . . ? 
N2 C16 C11 106.9(5) . . ? 
C15 C16 C11 121.5(5) . . ? 
C12 C11 N1 132.1(6) . . ? 
C12 C11 C16 121.9(6) . . ? 
N1 C11 C16 105.9(5) . . ? 
C12 C13 C14 122.0(6) . . ? 
C12 C13 H13A 119.0 . . ? 
C14 C13 H13A 119.0 . . ? 
C9 N2 C16 110.7(5) . . ? 
C9 N2 C17 123.3(5) . . ? 
C16 N2 C17 125.6(5) . . ? 
C22 C21 C20 121.3(6) . . ? 
C22 C21 C19 127.4(6) . 6_765 ? 
C20 C21 C19 111.3(5) . 6_765 ? 
C9 N1 C11 111.6(5) . . ? 
C9 N1 C10 125.0(5) . . ? 
C11 N1 C10 123.4(5) . . ? 
C25 C20 C21 119.1(6) . . ? 
C25 C20 C19 127.1(6) . . ? 
C21 C20 C19 113.7(5) . . ? 
C13 C12 C11 116.2(6) . . ? 
C13 C12 H12A 121.9 . . ? 
C11 C12 H12A 121.9 . . ? 
N1 C9 N2 104.8(5) . . ? 
N1 C9 Rh 125.6(4) . . ? 
N2 C9 Rh 129.3(4) . . ? 
N2 C17 C18 115.2(5) . . ? 
N2 C17 H17A 108.5 . . ? 
C18 C17 H17A 108.5 . . ? 
N2 C17 H17B 108.5 . . ? 
C18 C17 H17B 108.5 . . ? 
H17A C17 H17B 107.5 . . ? 
C17 C18 C18 114.5(6) . 6_765 ? 
C17 C18 C19 107.6(5) . . ? 
C18 C18 C19 109.1(3) 6_765 . ? 
C17 C18 H18A 108.5 . . ? 
C18 C18 H18A 108.5 6_765 . ? 
C19 C18 H18A 108.5 . . ? 
C5 C4 C3 126.1(7) . . ? 
C5 C4 Rh 72.8(4) . . ? 
C3 C4 Rh 108.5(4) . . ? 
C5 C4 H4A 113.8 . . ? 
C3 C4 H4A 113.8 . . ? 
Rh C4 H4A 113.8 . . ? 
N1 C10 H10A 109.5 . . ? 
N1 C10 H10B 109.5 . . ? 
H10A C10 H10B 109.5 . . ? 
N1 C10 H10C 109.5 . . ? 
H10A C10 H10C 109.5 . . ? 
H10B C10 H10C 109.5 . . ? 
C14 C15 C16 115.8(6) . . ? 
C14 C15 H15A 122.1 . . ? 
C16 C15 H15A 122.1 . . ? 
C21 C22 C23 119.4(6) . . ? 
C21 C22 H22A 120.3 . . ? 
C23 C22 H22A 120.3 . . ? 
C25 C24 C23 120.3(6) . . ? 
C25 C24 H24A 119.8 . . ? 
C23 C24 H24A 119.8 . . ? 
C15 C14 C13 122.6(6) . . ? 
C15 C14 H14A 118.7 . . ? 
C13 C14 H14A 118.7 . . ? 
C24 C25 C20 119.9(6) . . ? 
C24 C25 H25A 120.1 . . ? 
C20 C25 H25A 120.1 . . ? 
C8 C1 C2 123.8(6) . . ? 
C8 C1 Rh 70.1(3) . . ? 
C2 C1 Rh 114.4(4) . . ? 
C8 C1 H1A 113.7 . . ? 
C2 C1 H1A 113.7 . . ? 
Rh C1 H1A 113.7 . . ? 
C1 C2 C3 112.7(5) . . ? 
C1 C2 H2A 109.1 . . ? 
C3 C2 H2A 109.1 . . ? 
C1 C2 H2B 109.1 . . ? 
C3 C2 H2B 109.1 . . ? 
H2A C2 H2B 107.8 . . ? 
C8 C7 C6 114.4(6) . . ? 
C8 C7 H7A 108.7 . . ? 
C6 C7 H7A 108.7 . . ? 
C8 C7 H7B 108.7 . . ? 
C6 C7 H7B 108.7 . . ? 
H7A C7 H7B 107.6 . . ? 
C1 C8 C7 124.6(6) . . ? 
C1 C8 Rh 71.3(3) . . ? 
C7 C8 Rh 110.6(4) . . ? 
C1 C8 H8A 114.2 . . ? 
C7 C8 H8A 114.2 . . ? 
Rh C8 H8A 114.2 . . ? 
C4 C5 C6 122.8(7) . . ? 
C4 C5 Rh 71.4(4) . . ? 
C6 C5 Rh 111.0(4) . . ? 
C4 C5 H5A 114.6 . . ? 
C6 C5 H5A 114.6 . . ? 
Rh C5 H5A 114.6 . . ? 
C5 C6 C7 111.8(5) . . ? 
C5 C6 H6A 109.3 . . ? 
C7 C6 H6A 109.3 . . ? 
C5 C6 H6B 109.3 . . ? 
C7 C6 H6B 109.3 . . ? 
H6A C6 H6B 107.9 . . ? 
C24 C23 C22 119.9(6) . . ? 
C24 C23 H23A 120.1 . . ? 
C22 C23 H23A 120.1 . . ? 
C20 C19 C21 107.4(5) . 6_765 ? 
C20 C19 C18 108.8(5) . . ? 
C21 C19 C18 105.7(5) 6_765 . ? 
C20 C19 H19A 111.5 . . ? 
C21 C19 H19A 111.5 6_765 . ? 
C18 C19 H19A 111.5 . . ? 
C2 C3 C4 113.0(6) . . ? 
C2 C3 H3A 109.0 . . ? 
C4 C3 H3A 109.0 . . ? 
C2 C3 H3B 109.0 . . ? 
C4 C3 H3B 109.0 . . ? 
H3A C3 H3B 107.8 . . ? 
  
_diffrn_measured_fraction_theta_max    0.998 
_diffrn_reflns_theta_full              27.50 
_diffrn_measured_fraction_theta_full   0.998 
_refine_diff_density_max    0.529 
_refine_diff_density_min   -0.751 
_refine_diff_density_rms    0.094 
