Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Anthony Haynes' 'P. Maitlis' 'Ruhksana Quyoum' 'Claire Pulling' 'Harry Adams' 'Richard Strange' _publ_contact_author_name 'Dr Anthony Haynes' _publ_contact_author_address ; Dr Anthony Haynes Department of Chemistry University of Sheffield Brook Hill Sheffield South Yorkshire S3 7HF UK ; _publ_contact_author_email 'a.haynes@sheffield.ac.uk' _publ_section_title ; Structure and reactivity of polymer supported carbonylation catalysts ; data_imt2m _database_code_CSD 178080 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H8 I2 N O2 Rh' _chemical_formula_weight 506.86 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' 'O' 'O' 0.0106 0.0060 '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' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.137(2) _cell_length_b 7.503(3) _cell_length_c 12.697(3) _cell_angle_alpha 78.932(18) _cell_angle_beta 87.860(17) _cell_angle_gamma 75.72(3) _cell_volume 646.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 43 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.604 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 460 _exptl_absorpt_coefficient_mu 6.073 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.2250 _exptl_absorpt_correction_T_max 0.3764 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4331 _diffrn_reflns_av_R_equivalents 0.0616 _diffrn_reflns_av_sigmaI/netI 0.0460 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 28.35 _reflns_number_total 2977 _reflns_number_gt 2879 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0347P)^2^+1.7756P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0062(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2977 _refine_ls_number_parameters 129 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0342 _refine_ls_R_factor_gt 0.0309 _refine_ls_wR_factor_ref 0.0857 _refine_ls_wR_factor_gt 0.0846 _refine_ls_goodness_of_fit_ref 1.183 _refine_ls_restrained_S_all 1.183 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.77652(4) 0.80571(5) 0.21030(3) 0.02536(12) Uani 1 1 d . . . I2 I 0.71549(4) 0.91264(4) 0.39927(2) 0.02841(11) Uani 1 1 d . . . I1 I 0.68549(5) 1.15622(4) 0.10292(2) 0.03672(12) Uani 1 1 d . . . O1 O 0.8379(7) 0.6805(7) -0.0009(4) 0.0532(11) Uani 1 1 d . . . O2 O 0.8791(7) 0.4164(6) 0.3366(4) 0.0512(10) Uani 1 1 d . . . N1 N 1.2457(5) 0.8558(5) 0.2893(3) 0.0243(7) Uani 1 1 d . . . C1 C 0.8149(7) 0.7288(8) 0.0783(4) 0.0368(10) Uani 1 1 d . . . C2 C 0.8411(7) 0.5638(7) 0.2877(4) 0.0360(10) Uani 1 1 d . . . C3 C 1.2908(7) 0.7828(7) 0.2008(4) 0.0332(9) Uani 1 1 d . . . H4A H 1.2800 0.8615 0.1340 0.040 Uiso 1 1 calc R . . C4 C 1.3528(8) 0.5929(8) 0.2079(5) 0.0399(11) Uani 1 1 d . . . H5A H 1.3836 0.5423 0.1463 0.048 Uiso 1 1 calc R . . C5 C 1.3691(7) 0.4778(7) 0.3072(5) 0.0407(11) Uani 1 1 d . . . H6A H 1.4153 0.3489 0.3136 0.049 Uiso 1 1 calc R . . C6 C 1.3166(7) 0.5550(7) 0.3970(4) 0.0367(10) Uani 1 1 d . . . H7A H 1.3224 0.4778 0.4641 0.044 Uiso 1 1 calc R . . C7 C 1.2551(7) 0.7468(7) 0.3876(4) 0.0307(9) Uani 1 1 d . . . H8A H 1.2207 0.8000 0.4481 0.037 Uiso 1 1 calc R . . C8 C 1.1836(7) 1.0619(7) 0.2792(5) 0.0359(10) Uani 1 1 d . . . H9A H 1.1882 1.0943 0.3484 0.054 Uiso 1 1 calc R . . H9B H 1.0538 1.1059 0.2512 0.054 Uiso 1 1 calc R . . H9C H 1.2684 1.1191 0.2313 0.054 Uiso 1 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 Rh1 0.02093(18) 0.02724(18) 0.02829(19) -0.00829(13) 0.00019(12) -0.00426(12) I2 0.03010(17) 0.03085(17) 0.02467(16) -0.00550(11) 0.00184(10) -0.00819(11) I1 0.0462(2) 0.03298(18) 0.02682(17) -0.00240(12) 0.00002(12) -0.00424(13) O1 0.054(2) 0.063(3) 0.043(2) -0.026(2) 0.0006(18) -0.002(2) O2 0.057(2) 0.0298(19) 0.063(3) -0.0054(18) -0.004(2) -0.0042(17) N1 0.0188(15) 0.0268(17) 0.0275(17) -0.0037(14) -0.0020(12) -0.0068(13) C1 0.030(2) 0.041(3) 0.041(3) -0.015(2) -0.0004(18) -0.0041(19) C2 0.032(2) 0.031(2) 0.044(3) -0.012(2) 0.0028(19) -0.0041(18) C3 0.032(2) 0.035(2) 0.031(2) -0.0049(18) 0.0014(17) -0.0071(18) C4 0.037(2) 0.040(3) 0.048(3) -0.019(2) 0.001(2) -0.009(2) C5 0.031(2) 0.029(2) 0.064(3) -0.008(2) -0.005(2) -0.0087(18) C6 0.033(2) 0.032(2) 0.043(3) 0.010(2) -0.0068(19) -0.0156(19) C7 0.029(2) 0.036(2) 0.029(2) -0.0044(18) 0.0000(16) -0.0123(18) C8 0.033(2) 0.028(2) 0.045(3) -0.006(2) -0.0020(19) -0.0040(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C2 1.846(5) . ? Rh1 C1 1.864(5) . ? Rh1 I1 2.6539(12) . ? Rh1 I2 2.6606(8) . ? Rh1 N1 3.657(3) . ? O1 C1 1.126(7) . ? O2 C2 1.132(7) . ? N1 C3 1.338(6) . ? N1 C7 1.348(6) . ? N1 C8 1.481(6) . ? C3 C4 1.370(7) . ? C4 C5 1.376(9) . ? C5 C6 1.374(8) . ? C6 C7 1.380(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 Rh1 C1 93.4(2) . . ? C2 Rh1 I1 178.71(17) . . ? C1 Rh1 I1 87.78(17) . . ? C2 Rh1 I2 86.18(16) . . ? C1 Rh1 I2 178.86(16) . . ? I1 Rh1 I2 92.63(3) . . ? C2 Rh1 N1 87.86(17) . . ? C1 Rh1 N1 105.85(16) . . ? I1 Rh1 N1 91.36(7) . . ? I2 Rh1 N1 75.21(6) . . ? C3 N1 C7 121.8(4) . . ? C3 N1 C8 119.1(4) . . ? C7 N1 C8 119.1(4) . . ? C3 N1 Rh1 78.3(2) . . ? C7 N1 Rh1 96.9(2) . . ? C8 N1 Rh1 94.9(2) . . ? O1 C1 Rh1 179.2(5) . . ? O2 C2 Rh1 178.8(5) . . ? N1 C3 C4 120.5(5) . . ? C3 C4 C5 119.3(5) . . ? C4 C5 C6 119.4(5) . . ? C5 C6 C7 120.1(5) . . ? N1 C7 C6 118.9(5) . . ? 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 C2 Rh1 N1 C3 86.9(3) . . . . ? C1 Rh1 N1 C3 -6.1(3) . . . . ? I1 Rh1 N1 C3 -94.1(3) . . . . ? I2 Rh1 N1 C3 173.5(3) . . . . ? C2 Rh1 N1 C7 -34.2(3) . . . . ? C1 Rh1 N1 C7 -127.2(3) . . . . ? I1 Rh1 N1 C7 144.7(3) . . . . ? I2 Rh1 N1 C7 52.4(3) . . . . ? C2 Rh1 N1 C8 -154.3(3) . . . . ? C1 Rh1 N1 C8 112.7(3) . . . . ? I1 Rh1 N1 C8 24.7(3) . . . . ? I2 Rh1 N1 C8 -67.7(3) . . . . ? C2 Rh1 C1 O1 21(36) . . . . ? I1 Rh1 C1 O1 -160(36) . . . . ? I2 Rh1 C1 O1 -49(41) . . . . ? N1 Rh1 C1 O1 109(36) . . . . ? C1 Rh1 C2 O2 -159(25) . . . . ? I1 Rh1 C2 O2 43(30) . . . . ? I2 Rh1 C2 O2 20(25) . . . . ? N1 Rh1 C2 O2 95(25) . . . . ? C7 N1 C3 C4 -1.5(7) . . . . ? C8 N1 C3 C4 178.6(4) . . . . ? Rh1 N1 C3 C4 -92.4(4) . . . . ? N1 C3 C4 C5 -0.3(8) . . . . ? C3 C4 C5 C6 2.3(8) . . . . ? C4 C5 C6 C7 -2.5(7) . . . . ? C3 N1 C7 C6 1.3(6) . . . . ? C8 N1 C7 C6 -178.8(4) . . . . ? Rh1 N1 C7 C6 81.7(4) . . . . ? C5 C6 C7 N1 0.7(7) . . . . ? _diffrn_measured_fraction_theta_max 0.925 _diffrn_reflns_theta_full 28.35 _diffrn_measured_fraction_theta_full 0.925 _refine_diff_density_max 0.827 _refine_diff_density_min -1.309 _refine_diff_density_rms 0.193 #===END data_compound_2 _database_code_CSD 178081 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H12 I2 N O2 Rh' _chemical_formula_weight 534.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rh' 'Rh' -1.1178 0.9187 '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' _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 9.127(2) _cell_length_b 13.553(3) _cell_length_c 12.251(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.465(5) _cell_angle_gamma 90.00 _cell_volume 1514.1(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 100 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.347 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 5.193 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.1986 _exptl_absorpt_correction_T_max 0.5301 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8771 _diffrn_reflns_av_R_equivalents 0.0751 _diffrn_reflns_av_sigmaI/netI 0.0614 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 28.33 _reflns_number_total 3598 _reflns_number_gt 3034 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of 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^)+(0.0656P)^2^+2.3183P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3598 _refine_ls_number_parameters 147 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0595 _refine_ls_R_factor_gt 0.0467 _refine_ls_wR_factor_ref 0.1178 _refine_ls_wR_factor_gt 0.1122 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.24131(5) 0.16310(3) 0.11867(4) 0.02511(13) Uani 1 1 d . . . I1 I 0.49822(5) 0.21501(3) 0.21359(3) 0.03416(13) Uani 1 1 d . . . I2 I 0.11349(5) 0.33676(3) 0.15019(3) 0.03325(13) Uani 1 1 d . . . O1 O -0.0440(6) 0.1047(3) 0.0114(5) 0.0513(14) Uani 1 1 d . . . O2 O 0.3767(5) -0.0327(3) 0.0749(4) 0.0384(10) Uani 1 1 d . . . N1 N 0.1188(6) 0.1685(3) 0.4157(4) 0.0285(10) Uani 1 1 d . . . C1 C 0.0645(7) 0.1266(4) 0.0520(6) 0.0327(13) Uani 1 1 d . . . C2 C 0.3264(7) 0.0420(4) 0.0925(5) 0.0304(12) Uani 1 1 d . . . C3 C 0.1480(7) 0.0747(4) 0.3829(5) 0.0306(12) Uani 1 1 d . . . H3A H 0.2465 0.0520 0.3820 0.037 Uiso 1 1 calc R . . C4 C 0.0349(7) 0.0133(4) 0.3512(5) 0.0296(12) Uani 1 1 d . . . H4A H 0.0558 -0.0518 0.3276 0.035 Uiso 1 1 calc R . . C5 C -0.1104(7) 0.0444(4) 0.3530(5) 0.0305(13) Uani 1 1 d . . . C6 C -0.1348(8) 0.1413(5) 0.3834(5) 0.0311(12) Uani 1 1 d . . . H6A H -0.2323 0.1658 0.3837 0.037 Uiso 1 1 calc R . . C7 C -0.0199(7) 0.2022(4) 0.4132(5) 0.0300(12) Uani 1 1 d . . . H7A H -0.0385 0.2688 0.4323 0.036 Uiso 1 1 calc R . . C8 C 0.2398(7) 0.2342(5) 0.4507(5) 0.0334(13) Uani 1 1 d . . . H8A H 0.2139 0.2697 0.5169 0.050 Uiso 1 1 calc R . . H8B H 0.2577 0.2818 0.3925 0.050 Uiso 1 1 calc R . . H8C H 0.3286 0.1951 0.4661 0.050 Uiso 1 1 calc R . . C9 C -0.2347(8) -0.0239(5) 0.3208(6) 0.0386(15) Uani 1 1 d . . . H9A H -0.3275 0.0042 0.3460 0.046 Uiso 1 1 calc R . . H9B H -0.2188 -0.0882 0.3578 0.046 Uiso 1 1 calc R . . C10 C -0.2489(9) -0.0403(5) 0.1993(6) 0.0433(16) Uani 1 1 d . . . H10A H -0.3275 -0.0880 0.1827 0.065 Uiso 1 1 calc R . . H10B H -0.1562 -0.0660 0.1735 0.065 Uiso 1 1 calc R . . H10C H -0.2722 0.0223 0.1626 0.065 Uiso 1 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 Rh1 0.0254(3) 0.0228(2) 0.0274(2) 0.00045(14) 0.00419(17) 0.00059(17) I1 0.0275(2) 0.0345(2) 0.0402(2) -0.00355(15) -0.00100(16) 0.00195(16) I2 0.0296(3) 0.0272(2) 0.0431(2) -0.00512(14) 0.00304(17) 0.00435(15) O1 0.039(3) 0.032(2) 0.082(4) -0.006(2) -0.013(3) 0.005(2) O2 0.039(3) 0.026(2) 0.050(3) 0.0000(18) 0.005(2) 0.0061(19) N1 0.031(3) 0.027(2) 0.027(2) 0.0024(17) 0.005(2) 0.001(2) C1 0.023(3) 0.024(3) 0.051(4) 0.001(2) -0.005(3) 0.003(2) C2 0.031(3) 0.029(3) 0.031(3) 0.002(2) 0.003(2) -0.007(2) C3 0.026(3) 0.030(3) 0.037(3) 0.002(2) 0.008(2) 0.004(2) C4 0.028(3) 0.028(3) 0.033(3) -0.003(2) 0.003(2) -0.001(2) C5 0.037(4) 0.028(3) 0.027(3) 0.002(2) 0.003(2) -0.004(2) C6 0.032(3) 0.040(3) 0.022(3) -0.002(2) 0.006(2) 0.004(3) C7 0.033(4) 0.028(3) 0.029(3) -0.003(2) 0.001(2) 0.008(2) C8 0.031(4) 0.038(3) 0.032(3) 0.002(2) 0.001(2) -0.005(3) C9 0.031(4) 0.042(3) 0.043(4) 0.004(3) 0.002(3) -0.015(3) C10 0.050(5) 0.042(3) 0.038(4) -0.005(3) 0.001(3) -0.010(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C1 1.845(7) . ? Rh1 C2 1.850(6) . ? Rh1 I2 2.6623(8) . ? Rh1 I1 2.6667(8) . ? Rh1 N1 3.853(5) . ? O1 C1 1.129(8) . ? O2 C2 1.136(7) . ? N1 C7 1.345(8) . ? N1 C3 1.364(7) . ? N1 C8 1.469(8) . ? C3 C4 1.369(9) . ? C4 C5 1.392(9) . ? C5 C6 1.385(8) . ? C5 C9 1.504(9) . ? C6 C7 1.372(10) . ? C9 C10 1.505(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Rh1 C2 92.9(3) . . ? C1 Rh1 I2 85.46(18) . . ? C2 Rh1 I2 178.10(19) . . ? C1 Rh1 I1 179.5(2) . . ? C2 Rh1 I1 86.67(19) . . ? I2 Rh1 I1 94.94(2) . . ? C1 Rh1 N1 98.0(2) . . ? C2 Rh1 N1 108.76(19) . . ? I2 Rh1 N1 72.51(7) . . ? I1 Rh1 N1 82.45(8) . . ? C7 N1 C3 120.4(5) . . ? C7 N1 C8 119.7(5) . . ? C3 N1 C8 119.8(5) . . ? C7 N1 Rh1 107.3(3) . . ? C3 N1 Rh1 68.6(3) . . ? C8 N1 Rh1 92.4(3) . . ? O1 C1 Rh1 179.6(6) . . ? O2 C2 Rh1 178.7(6) . . ? N1 C3 C4 119.7(6) . . ? C3 C4 C5 121.2(5) . . ? C6 C5 C4 117.1(6) . . ? C6 C5 C9 121.7(6) . . ? C4 C5 C9 121.2(6) . . ? C7 C6 C5 120.8(6) . . ? N1 C7 C6 120.6(5) . . ? C5 C9 C10 112.5(6) . . ? 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 C1 Rh1 N1 C7 -36.0(4) . . . . ? C2 Rh1 N1 C7 -131.9(4) . . . . ? I2 Rh1 N1 C7 46.6(4) . . . . ? I1 Rh1 N1 C7 144.2(4) . . . . ? C1 Rh1 N1 C3 80.6(4) . . . . ? C2 Rh1 N1 C3 -15.3(4) . . . . ? I2 Rh1 N1 C3 163.2(4) . . . . ? I1 Rh1 N1 C3 -99.2(4) . . . . ? C1 Rh1 N1 C8 -158.2(4) . . . . ? C2 Rh1 N1 C8 105.9(4) . . . . ? I2 Rh1 N1 C8 -75.6(3) . . . . ? I1 Rh1 N1 C8 22.0(3) . . . . ? C2 Rh1 C1 O1 176(100) . . . . ? I2 Rh1 C1 O1 -5(100) . . . . ? I1 Rh1 C1 O1 -144(100) . . . . ? N1 Rh1 C1 O1 67(100) . . . . ? C1 Rh1 C2 O2 21(26) . . . . ? I2 Rh1 C2 O2 -11(31) . . . . ? I1 Rh1 C2 O2 -158(26) . . . . ? N1 Rh1 C2 O2 121(26) . . . . ? C7 N1 C3 C4 -2.5(8) . . . . ? C8 N1 C3 C4 179.4(5) . . . . ? Rh1 N1 C3 C4 -100.5(6) . . . . ? N1 C3 C4 C5 -0.7(9) . . . . ? C3 C4 C5 C6 2.8(8) . . . . ? C3 C4 C5 C9 -178.5(6) . . . . ? C4 C5 C6 C7 -1.7(8) . . . . ? C9 C5 C6 C7 179.5(6) . . . . ? C3 N1 C7 C6 3.5(8) . . . . ? C8 N1 C7 C6 -178.3(5) . . . . ? Rh1 N1 C7 C6 78.5(6) . . . . ? C5 C6 C7 N1 -1.4(9) . . . . ? C6 C5 C9 C10 104.6(7) . . . . ? C4 C5 C9 C10 -74.1(8) . . . . ? _diffrn_measured_fraction_theta_max 0.953 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.953 _refine_diff_density_max 1.631 _refine_diff_density_min -1.484 _refine_diff_density_rms 0.248 #===END