# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Robert H. Crabtree' _publ_contact_author_address ; Chemistry Yale University 225, Prospect St. New Haven Connecticut 06520-8107 UNITED STATES OF AMERICA ; _publ_contact_author_email ROBERT.CRABTREE@YALE.EDU _publ_section_title ; A Planar Chelating Bitriazole N-heterocyclic Carbene Ligand and its Rhodium(III) and Dirhodium(II) Complexes ; loop_ _publ_author_name 'R. Crabtree' 'Christopher Incarvito' 'William McNamara' 'Eduardo Peris' 'Macarena Poyatos-Lorenzo' # Attachment 'new_complex4.cif' data_crabtree_ep01 _database_code_depnum_ccdc_archive 'CCDC 643541' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H11 I3 N7 Rh' _chemical_formula_weight 688.85 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' 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 Orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 27.320(6) _cell_length_b 8.2040(16) _cell_length_c 15.373(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3445.7(12) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.656 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2496 _exptl_absorpt_coefficient_mu 6.365 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.5686 _exptl_absorpt_correction_T_max 0.6299 _exptl_absorpt_process_details ? _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 'Nonius KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7923 _diffrn_reflns_av_R_equivalents 0.0363 _diffrn_reflns_av_sigmaI/netI 0.0501 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 28.27 _reflns_number_total 4241 _reflns_number_gt 3004 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement Denzo _computing_data_reduction Denzo _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^)+(0.0400P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4241 _refine_ls_number_parameters 175 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0632 _refine_ls_R_factor_gt 0.0345 _refine_ls_wR_factor_ref 0.0805 _refine_ls_wR_factor_gt 0.0738 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _refine_ls_shift/su_max 0.414 _refine_ls_shift/su_mean 0.015 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 0.374974(14) 0.18355(4) 0.17207(3) 0.02711(11) Uani 1 1 d . . . I1 I 0.290608(13) 0.08481(4) 0.24274(2) 0.03901(11) Uani 1 1 d . . . I2 I 0.386601(15) -0.08857(4) 0.07179(3) 0.04273(12) Uani 1 1 d . . . I3 I 0.454878(13) 0.31941(4) 0.10438(3) 0.04090(12) Uani 1 1 d . . . N1 N 0.34623(15) 0.5118(5) 0.1973(3) 0.0313(9) Uani 1 1 d . . . N2 N 0.36774(17) 0.6174(5) 0.3194(3) 0.0382(11) Uani 1 1 d . . . N3 N 0.38186(15) 0.4572(5) 0.3137(3) 0.0313(10) Uani 1 1 d . . . N4 N 0.32838(16) 0.4750(5) 0.1164(3) 0.0322(10) Uani 1 1 d . . . N5 N 0.29214(16) 0.4605(5) -0.0079(3) 0.0423(11) Uani 1 1 d . . . N6 N 0.31354(15) 0.3127(5) 0.0140(3) 0.0326(10) Uani 1 1 d . . . N7 N 0.41536(16) 0.0576(4) 0.2642(3) 0.0337(10) Uani 1 1 d . . . C1 C 0.36910(17) 0.3886(5) 0.2393(3) 0.0269(11) Uani 1 1 d . . . C2 C 0.3456(2) 0.6493(6) 0.2467(3) 0.0348(12) Uani 1 1 d . . . H2A H 0.3315 0.7508 0.2308 0.042 Uiso 1 1 calc R . . C3 C 0.4062(2) 0.3826(7) 0.3864(4) 0.0485(15) Uani 1 1 d . . . H3A H 0.3853 0.2969 0.4108 0.073 Uiso 1 1 calc R . . H3B H 0.4127 0.4652 0.4310 0.073 Uiso 1 1 calc R . . H3C H 0.4372 0.3347 0.3670 0.073 Uiso 1 1 calc R . . C4 C 0.33668(18) 0.3171(5) 0.0901(3) 0.0300(11) Uani 1 1 d . . . C5 C 0.3018(2) 0.5565(6) 0.0571(4) 0.0388(13) Uani 1 1 d . . . H5A H 0.2916 0.6668 0.0619 0.047 Uiso 1 1 calc R . . C6 C 0.3080(2) 0.1766(6) -0.0464(3) 0.0409(13) Uani 1 1 d . . . H6A H 0.3382 0.1632 -0.0800 0.061 Uiso 1 1 calc R . . H6B H 0.2806 0.1986 -0.0860 0.061 Uiso 1 1 calc R . . H6C H 0.3013 0.0766 -0.0136 0.061 Uiso 1 1 calc R . . C7 C 0.4383(2) -0.0169(6) 0.3109(3) 0.0352(12) Uani 1 1 d . . . C8 C 0.4683(2) -0.1125(7) 0.3719(4) 0.0506(16) Uani 1 1 d . . . H8A H 0.4519 -0.1174 0.4286 0.076 Uiso 1 1 calc R . . H8B H 0.5004 -0.0605 0.3786 0.076 Uiso 1 1 calc R . . H8C H 0.4727 -0.2232 0.3492 0.076 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 0.0315(2) 0.02283(19) 0.0270(2) -0.00061(16) -0.00069(16) 0.00182(16) I1 0.0360(2) 0.03238(18) 0.0487(2) 0.00904(15) 0.00698(17) 0.00186(15) I2 0.0543(2) 0.03314(19) 0.0407(2) -0.00853(15) 0.00250(18) 0.00041(16) I3 0.0352(2) 0.0429(2) 0.0446(2) 0.00053(16) 0.00473(16) -0.00308(16) N1 0.039(2) 0.027(2) 0.028(2) 0.0002(18) -0.0018(19) 0.0027(19) N2 0.048(3) 0.030(2) 0.038(3) -0.005(2) 0.001(2) 0.000(2) N3 0.036(2) 0.026(2) 0.032(3) -0.0038(18) -0.0005(19) 0.0054(18) N4 0.037(2) 0.023(2) 0.037(3) 0.0002(18) -0.006(2) 0.0006(18) N5 0.047(3) 0.042(2) 0.038(3) 0.008(2) -0.007(2) 0.009(2) N6 0.035(2) 0.033(2) 0.030(3) 0.0024(18) -0.002(2) -0.0019(19) N7 0.039(3) 0.026(2) 0.037(3) -0.0017(19) 0.000(2) 0.004(2) C1 0.027(3) 0.026(2) 0.027(3) 0.003(2) 0.005(2) 0.004(2) C2 0.048(3) 0.021(2) 0.035(3) -0.003(2) -0.003(3) 0.003(2) C3 0.062(4) 0.046(3) 0.038(4) -0.002(3) -0.014(3) 0.009(3) C4 0.035(3) 0.024(2) 0.032(3) -0.002(2) 0.002(2) -0.001(2) C5 0.043(3) 0.038(3) 0.036(3) 0.005(2) -0.004(3) 0.006(2) C6 0.048(3) 0.043(3) 0.031(3) -0.003(2) -0.002(3) -0.016(3) C7 0.044(3) 0.034(3) 0.028(3) -0.001(2) 0.006(3) 0.002(3) C8 0.048(4) 0.053(3) 0.051(4) 0.020(3) -0.009(3) 0.002(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 1.981(5) . ? Rh1 C4 1.971(5) . ? Rh1 N7 2.071(4) . ? Rh1 I3 2.6629(6) . ? Rh1 I1 2.6737(7) . ? Rh1 I2 2.7316(6) . ? N1 C1 1.352(6) . ? N1 C2 1.360(6) . ? N1 N4 1.370(6) . ? N2 C2 1.297(7) . ? N2 N3 1.373(6) . ? N3 C1 1.321(6) . ? N3 C3 1.438(7) . ? N4 C5 1.344(6) . ? N4 C4 1.376(6) . ? N5 C5 1.299(6) . ? N5 N6 1.387(5) . ? N6 C4 1.331(6) . ? N6 C6 1.459(6) . ? N7 C7 1.133(6) . ? C7 C8 1.473(8) . ? 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 C4 79.54(19) . . ? C1 Rh1 N7 96.32(18) . . ? C4 Rh1 N7 175.86(17) . . ? C1 Rh1 I3 85.11(14) . . ? C4 Rh1 I3 87.28(14) . . ? N7 Rh1 I3 92.25(12) . . ? C1 Rh1 I1 88.60(14) . . ? C4 Rh1 I1 88.32(14) . . ? N7 Rh1 I1 91.74(12) . . ? I3 Rh1 I1 172.889(18) . . ? C1 Rh1 I2 176.33(14) . . ? C4 Rh1 I2 98.93(13) . . ? N7 Rh1 I2 85.19(11) . . ? I3 Rh1 I2 91.499(19) . . ? I1 Rh1 I2 94.700(18) . . ? C1 N1 C2 111.1(4) . . ? C1 N1 N4 115.7(4) . . ? C2 N1 N4 133.2(4) . . ? C2 N2 N3 105.6(4) . . ? C1 N3 N2 112.9(4) . . ? C1 N3 C3 127.9(4) . . ? N2 N3 C3 119.2(4) . . ? C5 N4 N1 134.4(4) . . ? C5 N4 C4 110.9(4) . . ? N1 N4 C4 114.6(4) . . ? C5 N5 N6 104.9(4) . . ? C4 N6 N5 112.9(4) . . ? C4 N6 C6 129.0(4) . . ? N5 N6 C6 118.1(4) . . ? C7 N7 Rh1 176.1(4) . . ? N3 C1 N1 102.5(4) . . ? N3 C1 Rh1 142.4(4) . . ? N1 C1 Rh1 115.0(3) . . ? N2 C2 N1 107.9(4) . . ? N6 C4 N4 101.9(4) . . ? N6 C4 Rh1 143.1(3) . . ? N4 C4 Rh1 115.0(3) . . ? N5 C5 N4 109.3(4) . . ? N7 C7 C8 179.5(6) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.865 _refine_diff_density_min -1.217 _refine_diff_density_rms 0.145 # Attachment 'new_complex5.cif' data_crabtree_bm01 _database_code_depnum_ccdc_archive 'CCDC 643542' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H29 I3 N13 O Rh' _chemical_formula_weight 927.15 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 11.691(2) _cell_length_b 9.883(2) _cell_length_c 26.375(5) _cell_angle_alpha 90.00 _cell_angle_beta 97.77(3) _cell_angle_gamma 90.00 _cell_volume 3019.4(10) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description blade _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.040 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1760 _exptl_absorpt_coefficient_mu 3.669 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.5274 _exptl_absorpt_correction_T_max 0.7579 _exptl_absorpt_process_details ? _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 'Nonius KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12618 _diffrn_reflns_av_R_equivalents 0.0379 _diffrn_reflns_av_sigmaI/netI 0.0665 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 29.06 _reflns_number_total 7790 _reflns_number_gt 5345 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement Denzo _computing_data_reduction Denzo _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^)+(0.0800P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0039(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7790 _refine_ls_number_parameters 331 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0861 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.1427 _refine_ls_wR_factor_gt 0.1279 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.685 _refine_ls_shift/su_mean 0.020 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 0.43860(4) 0.44072(5) 0.145990(17) 0.02958(14) Uani 1 1 d . . . I1 I 0.33307(4) 0.48315(5) 0.049270(16) 0.04672(15) Uani 1 1 d . . . I2 I 0.29055(4) 0.23978(4) 0.163474(17) 0.04198(15) Uani 1 1 d . . . I3 I 0.89302(4) 0.40476(5) 0.236792(17) 0.04368(15) Uani 1 1 d . . . N1 N 0.6117(4) 0.2429(5) 0.17664(19) 0.0327(11) Uani 1 1 d . . . N2 N 0.6754(5) 0.1242(6) 0.1177(2) 0.0451(14) Uani 1 1 d . . . N3 N 0.5906(5) 0.2126(5) 0.0980(2) 0.0376(12) Uani 1 1 d . . . N4 N 0.5917(4) 0.2993(5) 0.22195(19) 0.0329(11) Uani 1 1 d . . . N5 N 0.5879(5) 0.3678(6) 0.2999(2) 0.0409(13) Uani 1 1 d . . . N6 N 0.5147(4) 0.4430(5) 0.26495(19) 0.0341(11) Uani 1 1 d . . . N7 N 0.5088(4) 0.7169(5) 0.1404(2) 0.0357(12) Uani 1 1 d . . . N8 N 0.6722(5) 0.7504(6) 0.1130(2) 0.0441(14) Uani 1 1 d . . . N9 N 0.6460(4) 0.6107(5) 0.1165(2) 0.0385(12) Uani 1 1 d . . . N10 N 0.4018(4) 0.7258(5) 0.15810(19) 0.0360(12) Uani 1 1 d . . . N11 N 0.2445(5) 0.7891(6) 0.1849(2) 0.0404(13) Uani 1 1 d . . . N12 N 0.2502(4) 0.6508(5) 0.18022(19) 0.0353(11) Uani 1 1 d . . . C1 C 0.5488(5) 0.2875(6) 0.1341(2) 0.0348(14) Uani 1 1 d . . . C2 C 0.6893(5) 0.1450(6) 0.1674(3) 0.0388(14) Uani 1 1 d . . . H2A H 0.7429 0.1006 0.1922 0.047 Uiso 1 1 calc R . . C3 C 0.5574(7) 0.2164(8) 0.0427(3) 0.0521(18) Uani 1 1 d . . . H3A H 0.4902 0.2755 0.0345 0.078 Uiso 1 1 calc R . . H3B H 0.5380 0.1248 0.0301 0.078 Uiso 1 1 calc R . . H3C H 0.6218 0.2514 0.0264 0.078 Uiso 1 1 calc R . . C4 C 0.5143(5) 0.4043(6) 0.2173(2) 0.0301(12) Uani 1 1 d . . . C5 C 0.6357(5) 0.2830(7) 0.2727(2) 0.0393(15) Uani 1 1 d . . . H5A H 0.6927 0.2186 0.2855 0.047 Uiso 1 1 calc R . . C6 C 0.4437(6) 0.5472(7) 0.2843(3) 0.0446(16) Uani 1 1 d . . . H6A H 0.4485 0.6307 0.2647 0.067 Uiso 1 1 calc R . . H6B H 0.4716 0.5644 0.3205 0.067 Uiso 1 1 calc R . . H6C H 0.3633 0.5165 0.2808 0.067 Uiso 1 1 calc R . . C7 C 0.5458(5) 0.5891(6) 0.1328(2) 0.0328(13) Uani 1 1 d . . . C8 C 0.5851(5) 0.8120(7) 0.1286(2) 0.0393(14) Uani 1 1 d . . . H8A H 0.5763 0.9072 0.1313 0.047 Uiso 1 1 calc R . . C9 C 0.7283(6) 0.5167(7) 0.1007(3) 0.0443(16) Uani 1 1 d . . . H9A H 0.7516 0.4523 0.1284 0.066 Uiso 1 1 calc R . . H9B H 0.7963 0.5662 0.0927 0.066 Uiso 1 1 calc R . . H9C H 0.6932 0.4677 0.0702 0.066 Uiso 1 1 calc R . . C10 C 0.3464(5) 0.6065(7) 0.1636(2) 0.0342(14) Uani 1 1 d . . . C11 C 0.3393(6) 0.8333(7) 0.1715(3) 0.0411(15) Uani 1 1 d . . . H11A H 0.3621 0.9255 0.1711 0.049 Uiso 1 1 calc R . . C12 C 0.1534(5) 0.5706(8) 0.1917(3) 0.0492(18) Uani 1 1 d . . . H12A H 0.1489 0.4871 0.1715 0.074 Uiso 1 1 calc R . . H12B H 0.0819 0.6223 0.1832 0.074 Uiso 1 1 calc R . . H12C H 0.1638 0.5481 0.2282 0.074 Uiso 1 1 calc R . . N13 N 0.3787(7) -0.0552(9) 0.0667(3) 0.074(2) Uani 1 1 d . . . C13 C 0.3098(8) -0.0021(9) 0.0407(3) 0.059(2) Uani 1 1 d . . . C14 C 0.2235(8) 0.0750(11) 0.0061(4) 0.086(3) Uani 1 1 d . . . H14A H 0.2007 0.1558 0.0239 0.130 Uiso 1 1 calc R . . H14B H 0.1555 0.0182 -0.0040 0.130 Uiso 1 1 calc R . . H14C H 0.2570 0.1022 -0.0244 0.130 Uiso 1 1 calc R . . O1 O 0.0398(5) 0.7829(7) -0.0024(2) 0.0683(16) Uani 1 1 d . . . C15 C 0.0288(11) 0.8412(16) 0.0846(4) 0.127(6) Uani 1 1 d . . . H15A H 0.0169 0.8040 0.1179 0.191 Uiso 1 1 calc R . . H15B H -0.0319 0.9073 0.0735 0.191 Uiso 1 1 calc R . . H15C H 0.1044 0.8856 0.0875 0.191 Uiso 1 1 calc R . . C16 C 0.0241(12) 0.7237(14) 0.0443(4) 0.124(5) Uani 1 1 d . . . H16A H 0.0859 0.6568 0.0547 0.149 Uiso 1 1 calc R . . H16B H -0.0514 0.6769 0.0413 0.149 Uiso 1 1 calc R . . C17 C 0.0342(10) 0.6813(12) -0.0413(4) 0.092(3) Uani 1 1 d . . . H17A H -0.0403 0.6326 -0.0436 0.110 Uiso 1 1 calc R . . H17B H 0.0971 0.6148 -0.0325 0.110 Uiso 1 1 calc R . . C18 C 0.0453(8) 0.7436(12) -0.0904(3) 0.083(3) Uani 1 1 d . . . H18A H 0.0401 0.6737 -0.1170 0.125 Uiso 1 1 calc R . . H18B H 0.1202 0.7894 -0.0884 0.125 Uiso 1 1 calc R . . H18C H -0.0168 0.8097 -0.0989 0.125 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 0.0320(3) 0.0270(2) 0.0308(3) 0.00041(18) 0.00809(19) -0.00188(19) I1 0.0529(3) 0.0506(3) 0.0352(3) 0.00318(19) 0.0010(2) -0.0008(2) I2 0.0416(3) 0.0339(2) 0.0523(3) 0.00122(19) 0.01325(19) -0.00826(18) I3 0.0410(2) 0.0465(3) 0.0447(3) -0.0023(2) 0.01014(19) -0.00287(19) N1 0.033(3) 0.030(3) 0.038(3) -0.005(2) 0.016(2) -0.003(2) N2 0.040(3) 0.035(3) 0.062(4) -0.003(3) 0.018(3) 0.001(2) N3 0.049(3) 0.030(3) 0.036(3) -0.003(2) 0.015(2) -0.002(2) N4 0.032(3) 0.028(3) 0.039(3) 0.005(2) 0.009(2) 0.000(2) N5 0.040(3) 0.043(3) 0.039(3) 0.002(3) 0.004(2) -0.007(3) N6 0.037(3) 0.034(3) 0.031(3) 0.000(2) 0.006(2) 0.002(2) N7 0.039(3) 0.028(3) 0.042(3) -0.001(2) 0.010(2) -0.003(2) N8 0.044(3) 0.035(3) 0.053(4) 0.007(3) 0.006(3) -0.012(3) N9 0.038(3) 0.035(3) 0.044(3) 0.003(2) 0.007(2) -0.005(2) N10 0.038(3) 0.031(3) 0.039(3) -0.001(2) 0.006(2) -0.003(2) N11 0.050(3) 0.032(3) 0.042(3) -0.002(2) 0.013(3) -0.002(2) N12 0.041(3) 0.030(3) 0.036(3) -0.001(2) 0.009(2) 0.007(2) C1 0.040(3) 0.021(3) 0.046(4) 0.001(3) 0.015(3) -0.002(2) C2 0.042(3) 0.033(3) 0.045(4) 0.003(3) 0.018(3) 0.005(3) C3 0.074(5) 0.041(4) 0.044(4) -0.001(3) 0.019(4) 0.000(4) C4 0.026(3) 0.028(3) 0.037(3) 0.002(2) 0.009(2) -0.001(2) C5 0.034(3) 0.044(4) 0.038(4) 0.007(3) 0.001(3) 0.000(3) C6 0.058(4) 0.037(4) 0.043(4) -0.008(3) 0.022(3) 0.007(3) C7 0.033(3) 0.033(3) 0.033(3) 0.002(3) 0.004(2) -0.004(3) C8 0.045(4) 0.031(3) 0.044(4) 0.004(3) 0.014(3) 0.001(3) C9 0.047(4) 0.045(4) 0.044(4) 0.002(3) 0.017(3) 0.005(3) C10 0.033(3) 0.040(4) 0.029(3) 0.001(3) 0.002(2) -0.007(3) C11 0.046(4) 0.029(3) 0.049(4) -0.007(3) 0.007(3) 0.008(3) C12 0.036(3) 0.046(4) 0.069(5) -0.005(4) 0.017(3) -0.007(3) N13 0.078(5) 0.085(6) 0.062(5) 0.006(4) 0.017(4) 0.027(5) C13 0.075(6) 0.058(5) 0.048(5) -0.003(4) 0.020(4) -0.005(4) C14 0.073(6) 0.080(7) 0.105(8) 0.024(6) 0.005(6) 0.010(5) O1 0.069(4) 0.081(4) 0.056(3) 0.002(3) 0.014(3) 0.008(3) C15 0.114(9) 0.213(17) 0.055(6) -0.025(9) 0.012(6) 0.050(11) C16 0.141(11) 0.148(12) 0.097(8) 0.079(9) 0.067(8) 0.080(9) C17 0.097(8) 0.096(8) 0.089(8) -0.004(7) 0.035(6) 0.030(6) C18 0.073(6) 0.116(9) 0.061(6) -0.011(6) 0.014(5) 0.003(6) _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 C7 1.990(6) . ? Rh1 C4 2.000(6) . ? Rh1 C1 2.040(6) . ? Rh1 C10 2.048(7) . ? Rh1 I1 2.7120(10) . ? Rh1 I2 2.7143(7) . ? N1 C1 1.331(8) . ? N1 N4 1.367(7) . ? N1 C2 1.370(8) . ? N2 C2 1.316(8) . ? N2 N3 1.370(8) . ? N3 C1 1.348(8) . ? N3 C3 1.457(8) . ? N4 C4 1.371(7) . ? N4 C5 1.377(8) . ? N5 C5 1.280(8) . ? N5 N6 1.386(7) . ? N6 C4 1.313(8) . ? N6 C6 1.457(8) . ? N7 C8 1.361(8) . ? N7 C7 1.359(8) . ? N7 N10 1.395(7) . ? N8 C8 1.300(9) . ? N8 N9 1.419(7) . ? N9 C7 1.319(8) . ? N9 C9 1.439(8) . ? N10 C10 1.362(8) . ? N10 C11 1.363(8) . ? N11 C11 1.284(8) . ? N11 N12 1.374(7) . ? N12 C10 1.336(8) . ? N12 C12 1.447(8) . ? N13 C13 1.117(10) . ? C13 C14 1.477(13) . ? O1 C16 1.396(10) . ? O1 C17 1.432(12) . ? C15 C16 1.571(18) . ? C17 C18 1.455(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 C7 Rh1 C4 95.1(2) . . ? C7 Rh1 C1 95.4(2) . . ? C4 Rh1 C1 78.6(2) . . ? C7 Rh1 C10 79.2(2) . . ? C4 Rh1 C10 96.3(2) . . ? C1 Rh1 C10 172.4(2) . . ? C7 Rh1 I1 86.47(17) . . ? C4 Rh1 I1 178.40(17) . . ? C1 Rh1 I1 100.74(19) . . ? C10 Rh1 I1 84.42(16) . . ? C7 Rh1 I2 179.40(18) . . ? C4 Rh1 I2 85.42(16) . . ? C1 Rh1 I2 85.03(17) . . ? C10 Rh1 I2 100.35(17) . . ? I1 Rh1 I2 93.06(3) . . ? C1 N1 N4 117.5(5) . . ? C1 N1 C2 112.8(5) . . ? N4 N1 C2 129.7(5) . . ? C2 N2 N3 105.3(5) . . ? C1 N3 N2 113.3(5) . . ? C1 N3 C3 128.2(6) . . ? N2 N3 C3 118.5(5) . . ? N1 N4 C4 114.8(5) . . ? N1 N4 C5 135.8(5) . . ? C4 N4 C5 109.3(5) . . ? C5 N5 N6 104.8(5) . . ? C4 N6 N5 113.7(5) . . ? C4 N6 C6 127.8(5) . . ? N5 N6 C6 118.4(5) . . ? C8 N7 C7 112.1(5) . . ? C8 N7 N10 132.7(5) . . ? C7 N7 N10 115.2(5) . . ? C8 N8 N9 104.5(5) . . ? C7 N9 N8 112.8(5) . . ? C7 N9 C9 130.4(6) . . ? N8 N9 C9 116.8(5) . . ? C10 N10 C11 111.6(5) . . ? C10 N10 N7 116.2(5) . . ? C11 N10 N7 132.2(5) . . ? C11 N11 N12 105.0(5) . . ? C10 N12 N11 114.1(5) . . ? C10 N12 C12 127.4(5) . . ? N11 N12 C12 118.5(5) . . ? N1 C1 N3 101.6(5) . . ? N1 C1 Rh1 113.8(4) . . ? N3 C1 Rh1 144.4(5) . . ? N2 C2 N1 107.0(6) . . ? N6 C4 N4 102.6(5) . . ? N6 C4 Rh1 142.3(4) . . ? N4 C4 Rh1 115.0(4) . . ? N5 C5 N4 109.5(6) . . ? N9 C7 N7 102.3(5) . . ? N9 C7 Rh1 141.7(5) . . ? N7 C7 Rh1 116.0(4) . . ? N8 C8 N7 108.4(6) . . ? N12 C10 N10 100.6(5) . . ? N12 C10 Rh1 146.0(5) . . ? N10 C10 Rh1 113.4(4) . . ? N11 C11 N10 108.6(6) . . ? N13 C13 C14 176.5(10) . . ? C16 O1 C17 109.9(9) . . ? O1 C16 C15 106.8(11) . . ? O1 C17 C18 109.9(10) . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 29.06 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 1.239 _refine_diff_density_min -0.942 _refine_diff_density_rms 0.162 # Attachment 'new_complex6.cif' data_crabtree_mpl02 _database_code_depnum_ccdc_archive 'CCDC 643543' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H37 B4 F16 N19 Rh2' _chemical_formula_weight 1168.81 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' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 20.137(4) _cell_length_b 11.200(2) _cell_length_c 19.736(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.01(3) _cell_angle_gamma 90.00 _cell_volume 4396.3(15) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.766 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2320 _exptl_absorpt_coefficient_mu 0.867 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8810 _exptl_absorpt_correction_T_max 0.9339 _exptl_absorpt_process_details ? _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 'Nonius KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20259 _diffrn_reflns_av_R_equivalents 0.0453 _diffrn_reflns_av_sigmaI/netI 0.0764 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 29.01 _reflns_number_total 11606 _reflns_number_gt 8005 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement Denzo _computing_data_reduction Denzo _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^)+(0.0534P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11606 _refine_ls_number_parameters 615 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0814 _refine_ls_R_factor_gt 0.0445 _refine_ls_wR_factor_ref 0.1084 _refine_ls_wR_factor_gt 0.0968 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.996 _refine_ls_shift/su_max 0.484 _refine_ls_shift/su_mean 0.015 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 0.781039(12) 0.18180(2) 0.282183(13) 0.02017(7) Uani 1 1 d . . . Rh2 Rh 0.679963(12) 0.16307(2) 0.352553(13) 0.01931(7) Uani 1 1 d . . . N1 N 0.84706(14) 0.2096(3) 0.37246(16) 0.0314(7) Uani 1 1 d . . . N2 N 0.80256(13) 0.0017(2) 0.29875(14) 0.0254(6) Uani 1 1 d . . . N3 N 0.86698(13) 0.1793(2) 0.22868(15) 0.0283(6) Uani 1 1 d . . . N4 N 0.66826(12) 0.0743(2) 0.18468(13) 0.0204(6) Uani 1 1 d . . . N5 N 0.66514(14) 0.1596(3) 0.08519(15) 0.0305(7) Uani 1 1 d . . . N6 N 0.71612(13) 0.2052(2) 0.13413(14) 0.0240(6) Uani 1 1 d . . . N7 N 0.65620(12) -0.0091(2) 0.23231(13) 0.0205(6) Uani 1 1 d . . . N8 N 0.64034(14) -0.1851(2) 0.27394(15) 0.0290(6) Uani 1 1 d . . . N9 N 0.64511(13) -0.0971(2) 0.32373(14) 0.0233(6) Uani 1 1 d . . . N10 N 0.70074(12) 0.4110(2) 0.26335(14) 0.0225(6) Uani 1 1 d . . . N11 N 0.77199(13) 0.5567(2) 0.28549(16) 0.0324(7) Uani 1 1 d . . . N12 N 0.80388(13) 0.4471(2) 0.28658(14) 0.0267(6) Uani 1 1 d . . . N13 N 0.63914(12) 0.3546(2) 0.24889(13) 0.0202(6) Uani 1 1 d . . . N14 N 0.53396(13) 0.3312(2) 0.20688(14) 0.0272(6) Uani 1 1 d . . . N15 N 0.55664(12) 0.2445(2) 0.25481(14) 0.0228(6) Uani 1 1 d . . . N16 N 0.74404(13) 0.0695(2) 0.42636(14) 0.0257(6) Uani 1 1 d . . . N17 N 0.70805(13) 0.3195(2) 0.40596(14) 0.0238(6) Uani 1 1 d . . . N18 N 0.60229(14) 0.1551(2) 0.41736(14) 0.0269(6) Uani 1 1 d . . . C1 C 0.89065(19) 0.2197(4) 0.4154(2) 0.0397(9) Uani 1 1 d . . . C2 C 0.9481(2) 0.2330(5) 0.4719(2) 0.0686(14) Uani 1 1 d . . . H2A H 0.9442 0.3092 0.4954 0.103 Uiso 1 1 calc R . . H2B H 0.9903 0.2316 0.4530 0.103 Uiso 1 1 calc R . . H2C H 0.9477 0.1672 0.5045 0.103 Uiso 1 1 calc R . . C3 C 0.82502(17) -0.0868(3) 0.3157(2) 0.0334(8) Uani 1 1 d . . . C4 C 0.8533(2) -0.2019(3) 0.3390(3) 0.0580(13) Uani 1 1 d . . . H4A H 0.8315 -0.2308 0.3769 0.087 Uiso 1 1 calc R . . H4B H 0.9017 -0.1933 0.3546 0.087 Uiso 1 1 calc R . . H4C H 0.8458 -0.2592 0.3010 0.087 Uiso 1 1 calc R . . C5 C 0.91031(17) 0.1560(3) 0.20212(19) 0.0300(8) Uani 1 1 d . . . C6 C 0.96670(19) 0.1246(4) 0.1673(2) 0.0493(11) Uani 1 1 d . . . H6A H 1.0017 0.0852 0.1997 0.074 Uiso 1 1 calc R . . H6B H 0.9851 0.1971 0.1496 0.074 Uiso 1 1 calc R . . H6C H 0.9512 0.0703 0.1291 0.074 Uiso 1 1 calc R . . C7 C 0.71996(14) 0.1540(3) 0.19547(16) 0.0203(6) Uani 1 1 d . . . C8 C 0.63710(16) 0.0791(3) 0.11816(18) 0.0279(7) Uani 1 1 d . . . H8A H 0.6003 0.0305 0.0989 0.034 Uiso 1 1 calc R . . C9 C 0.75888(18) 0.2964(3) 0.10995(19) 0.0357(9) Uani 1 1 d . . . H9A H 0.7919 0.3244 0.1485 0.053 Uiso 1 1 calc R . . H9B H 0.7310 0.3637 0.0907 0.053 Uiso 1 1 calc R . . H9C H 0.7823 0.2622 0.0745 0.053 Uiso 1 1 calc R . . C10 C 0.65623(15) 0.0124(3) 0.30079(16) 0.0218(7) Uani 1 1 d . . . C11 C 0.64818(16) -0.1277(3) 0.21840(18) 0.0277(7) Uani 1 1 d . . . H11A H 0.6483 -0.1633 0.1747 0.033 Uiso 1 1 calc R . . C12 C 0.63651(18) -0.1358(3) 0.39237(18) 0.0325(8) Uani 1 1 d . . . H12A H 0.6768 -0.1789 0.4136 0.049 Uiso 1 1 calc R . . H12B H 0.5973 -0.1886 0.3893 0.049 Uiso 1 1 calc R . . H12C H 0.6296 -0.0659 0.4203 0.049 Uiso 1 1 calc R . . C13 C 0.76207(16) 0.3552(3) 0.27438(17) 0.0238(7) Uani 1 1 d . . . C14 C 0.70888(17) 0.5318(3) 0.27192(18) 0.0276(7) Uani 1 1 d . . . H14A H 0.6734 0.5884 0.2684 0.033 Uiso 1 1 calc R . . C15 C 0.87752(16) 0.4479(3) 0.2971(2) 0.0414(10) Uani 1 1 d . . . H15A H 0.8945 0.4874 0.3407 0.062 Uiso 1 1 calc R . . H15B H 0.8931 0.4913 0.2594 0.062 Uiso 1 1 calc R . . H15C H 0.8942 0.3656 0.2982 0.062 Uiso 1 1 calc R . . C16 C 0.62111(14) 0.2560(3) 0.28245(16) 0.0200(7) Uani 1 1 d . . . C17 C 0.58630(15) 0.3972(3) 0.20436(17) 0.0272(7) Uani 1 1 d . . . H17A H 0.5875 0.4651 0.1757 0.033 Uiso 1 1 calc R . . C18 C 0.50755(16) 0.1578(3) 0.27186(19) 0.0301(8) Uani 1 1 d . . . H18A H 0.5305 0.0832 0.2871 0.045 Uiso 1 1 calc R . . H18B H 0.4740 0.1424 0.2312 0.045 Uiso 1 1 calc R . . H18C H 0.4852 0.1898 0.3087 0.045 Uiso 1 1 calc R . . C19 C 0.77916(19) 0.0166(3) 0.4656(2) 0.0377(9) Uani 1 1 d . . . C20 C 0.8268(2) -0.0521(4) 0.5142(2) 0.0661(14) Uani 1 1 d . . . H20A H 0.8053 -0.1259 0.5263 0.099 Uiso 1 1 calc R . . H20B H 0.8406 -0.0046 0.5557 0.099 Uiso 1 1 calc R . . H20C H 0.8664 -0.0718 0.4931 0.099 Uiso 1 1 calc R . . C21 C 0.71252(15) 0.4077(3) 0.43363(17) 0.0271(7) Uani 1 1 d . . . C22 C 0.71766(19) 0.5229(3) 0.4684(2) 0.0395(9) Uani 1 1 d . . . H22A H 0.7401 0.5801 0.4419 0.059 Uiso 1 1 calc R . . H22B H 0.7438 0.5140 0.5143 0.059 Uiso 1 1 calc R . . H22C H 0.6725 0.5521 0.4722 0.059 Uiso 1 1 calc R . . C23 C 0.56617(17) 0.1740(3) 0.45415(18) 0.0283(8) Uani 1 1 d . . . C24 C 0.51825(19) 0.1986(4) 0.5013(2) 0.0443(10) Uani 1 1 d . . . H24A H 0.5037 0.2820 0.4964 0.066 Uiso 1 1 calc R . . H24B H 0.5400 0.1841 0.5486 0.066 Uiso 1 1 calc R . . H24C H 0.4791 0.1460 0.4904 0.066 Uiso 1 1 calc R . . B1 B 0.8958(3) -0.0836(5) -0.0186(3) 0.0563(14) Uani 1 1 d . . . F1 F 0.93396(19) -0.0694(4) 0.04602(19) 0.1191(13) Uani 1 1 d . . . F2 F 0.86291(17) 0.0227(3) -0.0372(2) 0.1161(14) Uani 1 1 d . . . F3 F 0.93747(13) -0.1113(3) -0.06419(14) 0.0748(8) Uani 1 1 d . . . F4 F 0.84970(15) -0.1726(2) -0.01452(16) 0.0700(8) Uani 1 1 d . . . B2 B 1.0176(3) -0.0323(5) 0.3479(3) 0.0517(13) Uani 1 1 d . . . F5 F 1.02858(18) 0.0828(3) 0.33447(18) 0.1052(12) Uani 1 1 d . . . F6 F 1.07758(15) -0.0923(3) 0.36892(17) 0.0965(11) Uani 1 1 d . . . F7 F 0.97955(16) -0.0405(3) 0.39988(15) 0.0855(9) Uani 1 1 d . . . F8 F 0.98489(13) -0.0881(2) 0.28986(13) 0.0680(8) Uani 1 1 d . . . B3 B 0.5388(2) 0.4963(4) 0.3887(2) 0.0378(10) Uani 1 1 d . . . F9 F 0.58972(10) 0.4988(2) 0.34800(11) 0.0459(6) Uani 1 1 d . . . F10 F 0.51354(11) 0.6101(2) 0.39167(13) 0.0538(6) Uani 1 1 d . . . F11 F 0.56449(12) 0.4570(3) 0.45356(13) 0.0626(7) Uani 1 1 d . . . F12 F 0.48835(12) 0.4213(2) 0.35989(16) 0.0735(8) Uani 1 1 d . . . B4 B 0.6577(3) -0.1131(4) 0.5890(3) 0.0449(12) Uani 1 1 d . . . F13 F 0.61870(14) -0.1417(2) 0.63835(13) 0.0619(7) Uani 1 1 d . . . F14 F 0.62823(18) -0.0186(3) 0.55171(16) 0.0936(10) Uani 1 1 d . . . F15 F 0.66187(18) -0.2073(3) 0.54897(16) 0.1015(12) Uani 1 1 d . . . F16 F 0.71977(16) -0.0787(4) 0.62320(18) 0.1076(12) Uani 1 1 d . . . C25 C 0.8706(2) -0.2242(5) 0.1556(3) 0.0730(15) Uani 1 1 d . . . H25A H 0.8544 -0.2978 0.1744 0.109 Uiso 1 1 calc R . . H25B H 0.9080 -0.1915 0.1881 0.109 Uiso 1 1 calc R . . H25C H 0.8861 -0.2417 0.1120 0.109 Uiso 1 1 calc R . . C26 C 0.8157(2) -0.1366(4) 0.1442(2) 0.0553(12) Uani 1 1 d . . . N19 N 0.7736(2) -0.0730(4) 0.1370(2) 0.0704(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.01638(12) 0.02153(13) 0.02262(14) -0.00188(10) 0.00309(10) 0.00001(9) Rh2 0.01875(13) 0.02001(13) 0.01938(14) -0.00042(10) 0.00363(10) 0.00008(9) N1 0.0242(15) 0.0372(17) 0.0301(17) -0.0067(13) -0.0041(13) 0.0029(13) N2 0.0214(13) 0.0283(16) 0.0263(15) -0.0002(12) 0.0027(12) 0.0027(12) N3 0.0204(14) 0.0351(16) 0.0298(17) -0.0013(13) 0.0052(13) -0.0033(12) N4 0.0192(13) 0.0225(13) 0.0201(14) 0.0018(11) 0.0047(11) -0.0015(10) N5 0.0313(16) 0.0355(17) 0.0234(16) 0.0020(13) 0.0001(13) -0.0020(13) N6 0.0227(14) 0.0262(14) 0.0226(15) 0.0037(12) 0.0018(12) -0.0010(11) N7 0.0206(13) 0.0181(13) 0.0224(14) -0.0003(11) 0.0027(11) -0.0005(10) N8 0.0325(15) 0.0237(15) 0.0304(17) -0.0034(12) 0.0037(13) -0.0011(12) N9 0.0259(14) 0.0211(14) 0.0238(15) -0.0005(11) 0.0062(12) -0.0023(11) N10 0.0206(13) 0.0196(13) 0.0285(16) 0.0002(11) 0.0072(12) -0.0021(11) N11 0.0286(15) 0.0230(15) 0.046(2) -0.0049(13) 0.0057(14) -0.0034(12) N12 0.0234(14) 0.0228(14) 0.0343(17) -0.0045(12) 0.0052(12) -0.0035(11) N13 0.0145(12) 0.0216(13) 0.0245(15) 0.0027(11) 0.0025(11) 0.0003(10) N14 0.0258(14) 0.0285(15) 0.0261(16) 0.0045(12) 0.0004(12) 0.0028(12) N15 0.0222(13) 0.0211(14) 0.0254(15) 0.0002(11) 0.0049(12) 0.0015(11) N16 0.0258(14) 0.0293(15) 0.0213(15) 0.0015(12) 0.0018(12) 0.0037(12) N17 0.0211(13) 0.0246(15) 0.0249(15) -0.0036(12) 0.0012(12) -0.0027(11) N18 0.0296(15) 0.0284(15) 0.0241(16) 0.0024(12) 0.0080(13) 0.0005(12) C1 0.037(2) 0.042(2) 0.040(2) -0.0072(18) 0.0076(19) -0.0018(18) C2 0.057(3) 0.078(4) 0.060(3) -0.010(3) -0.027(3) -0.004(3) C3 0.0254(18) 0.033(2) 0.040(2) -0.0050(17) -0.0004(16) -0.0038(16) C4 0.059(3) 0.027(2) 0.084(4) 0.011(2) -0.003(3) 0.001(2) C5 0.0258(18) 0.0325(19) 0.031(2) 0.0000(15) 0.0030(16) -0.0006(14) C6 0.040(2) 0.059(3) 0.055(3) 0.006(2) 0.026(2) 0.016(2) C7 0.0169(15) 0.0193(15) 0.0247(17) -0.0020(13) 0.0036(13) 0.0033(12) C8 0.0219(16) 0.0341(19) 0.0262(19) -0.0008(15) -0.0008(14) -0.0032(14) C9 0.0346(19) 0.040(2) 0.033(2) 0.0105(17) 0.0074(17) -0.0091(17) C10 0.0206(15) 0.0211(16) 0.0240(18) 0.0006(13) 0.0049(13) -0.0004(12) C11 0.0283(17) 0.0249(17) 0.030(2) -0.0025(14) 0.0047(15) -0.0018(14) C12 0.043(2) 0.0273(18) 0.029(2) 0.0060(15) 0.0117(17) -0.0033(16) C13 0.0226(16) 0.0221(16) 0.0273(18) -0.0041(13) 0.0056(14) -0.0022(13) C14 0.0312(18) 0.0186(16) 0.034(2) 0.0014(14) 0.0082(16) -0.0009(14) C15 0.0227(17) 0.038(2) 0.063(3) -0.007(2) 0.0061(18) -0.0080(16) C16 0.0209(15) 0.0188(15) 0.0215(17) -0.0043(12) 0.0072(13) -0.0013(12) C17 0.0260(17) 0.0279(18) 0.0271(19) 0.0040(14) 0.0021(15) 0.0017(14) C18 0.0207(16) 0.0295(18) 0.040(2) 0.0023(16) 0.0034(15) -0.0056(14) C19 0.043(2) 0.035(2) 0.034(2) -0.0077(17) 0.0043(19) -0.0022(18) C20 0.079(3) 0.055(3) 0.053(3) -0.002(2) -0.025(3) 0.026(3) C21 0.0234(16) 0.0325(19) 0.0257(19) 0.0008(15) 0.0050(14) -0.0009(14) C22 0.047(2) 0.033(2) 0.038(2) -0.0148(17) 0.0068(18) -0.0066(17) C23 0.0286(18) 0.0285(18) 0.0269(19) 0.0020(15) 0.0015(16) -0.0019(14) C24 0.041(2) 0.058(3) 0.040(2) -0.006(2) 0.0257(19) -0.0023(19) B1 0.059(3) 0.058(3) 0.056(4) 0.000(3) 0.023(3) 0.011(3) F1 0.135(3) 0.148(4) 0.078(3) -0.040(2) 0.027(2) -0.038(3) F2 0.092(2) 0.0546(19) 0.221(4) 0.040(2) 0.085(3) 0.0172(17) F3 0.0623(17) 0.101(2) 0.065(2) 0.0116(17) 0.0216(15) 0.0172(16) F4 0.084(2) 0.0453(16) 0.086(2) 0.0000(14) 0.0302(17) -0.0008(13) B2 0.049(3) 0.053(3) 0.050(3) -0.001(3) -0.001(3) -0.014(2) F5 0.138(3) 0.060(2) 0.113(3) 0.0081(19) 0.005(2) -0.042(2) F6 0.0683(19) 0.122(3) 0.088(2) -0.035(2) -0.0225(18) 0.0219(19) F7 0.099(2) 0.098(2) 0.063(2) -0.0105(17) 0.0234(17) -0.0128(19) F8 0.0732(18) 0.0767(19) 0.0481(17) -0.0059(14) -0.0091(14) -0.0183(15) B3 0.029(2) 0.044(3) 0.042(3) -0.005(2) 0.010(2) 0.0073(19) F9 0.0391(12) 0.0599(15) 0.0404(13) 0.0004(11) 0.0114(10) 0.0175(11) F10 0.0583(15) 0.0427(13) 0.0664(17) -0.0041(12) 0.0288(13) 0.0122(11) F11 0.0543(15) 0.0858(19) 0.0502(16) 0.0233(14) 0.0161(13) 0.0042(14) F12 0.0448(14) 0.0681(18) 0.105(2) -0.0332(16) 0.0046(15) -0.0088(13) B4 0.053(3) 0.046(3) 0.036(3) 0.005(2) 0.008(2) -0.004(2) F13 0.097(2) 0.0448(14) 0.0528(16) 0.0049(12) 0.0377(15) -0.0031(13) F14 0.136(3) 0.071(2) 0.072(2) 0.0393(17) 0.0122(19) 0.0178(19) F15 0.133(3) 0.100(2) 0.071(2) -0.0414(19) 0.014(2) 0.041(2) F16 0.086(2) 0.136(3) 0.095(3) -0.001(2) -0.004(2) -0.030(2) C25 0.076(4) 0.079(4) 0.060(3) 0.005(3) 0.001(3) 0.029(3) C26 0.068(3) 0.063(3) 0.034(3) -0.005(2) 0.005(2) 0.013(3) N19 0.078(3) 0.084(3) 0.047(3) -0.006(2) 0.003(2) 0.043(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 C7 1.970(3) . ? Rh1 C13 1.980(3) . ? Rh1 N1 2.073(3) . ? Rh1 N2 2.078(3) . ? Rh1 N3 2.164(3) . ? Rh1 Rh2 2.6460(7) . ? Rh2 C16 1.972(3) . ? Rh2 C10 1.992(3) . ? Rh2 N16 2.073(3) . ? Rh2 N17 2.077(3) . ? Rh2 N18 2.172(3) . ? N1 C1 1.126(4) . ? N2 C3 1.119(4) . ? N3 C5 1.117(4) . ? N4 C7 1.362(4) . ? N4 C8 1.365(4) . ? N4 N7 1.374(3) . ? N5 C8 1.292(4) . ? N5 N6 1.392(4) . ? N6 C7 1.331(4) . ? N6 C9 1.463(4) . ? N7 C11 1.361(4) . ? N7 C10 1.373(4) . ? N8 C11 1.301(4) . ? N8 N9 1.384(4) . ? N9 C10 1.338(4) . ? N9 C12 1.458(4) . ? N10 C13 1.371(4) . ? N10 C14 1.370(4) . ? N10 N13 1.381(3) . ? N11 C14 1.288(4) . ? N11 N12 1.383(4) . ? N12 C13 1.328(4) . ? N12 C15 1.465(4) . ? N13 C17 1.357(4) . ? N13 C16 1.365(4) . ? N14 C17 1.295(4) . ? N14 N15 1.383(4) . ? N15 C16 1.334(4) . ? N15 C18 1.462(4) . ? N16 C19 1.131(4) . ? N17 C21 1.126(4) . ? N18 C23 1.125(4) . ? C1 C2 1.483(5) . ? C3 C4 1.455(5) . ? C5 C6 1.460(5) . ? C19 C20 1.464(5) . ? C21 C22 1.457(5) . ? C23 C24 1.468(5) . ? B1 F3 1.358(6) . ? B1 F4 1.373(6) . ? B1 F2 1.384(6) . ? B1 F1 1.391(6) . ? B2 F5 1.341(6) . ? B2 F7 1.377(6) . ? B2 F8 1.378(6) . ? B2 F6 1.387(6) . ? B3 F12 1.371(5) . ? B3 F10 1.378(5) . ? B3 F11 1.375(5) . ? B3 F9 1.399(5) . ? B4 F15 1.329(6) . ? B4 F14 1.370(5) . ? B4 F16 1.379(6) . ? B4 F13 1.381(5) . ? C25 C26 1.469(6) . ? C26 N19 1.099(5) . ? 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 C7 Rh1 C13 90.06(13) . . ? C7 Rh1 N1 178.74(12) . . ? C13 Rh1 N1 90.54(13) . . ? C7 Rh1 N2 93.99(11) . . ? C13 Rh1 N2 175.46(12) . . ? N1 Rh1 N2 85.46(11) . . ? C7 Rh1 N3 90.70(12) . . ? C13 Rh1 N3 97.70(12) . . ? N1 Rh1 N3 88.12(11) . . ? N2 Rh1 N3 84.34(10) . . ? C7 Rh1 Rh2 90.95(9) . . ? C13 Rh1 Rh2 87.92(9) . . ? N1 Rh1 Rh2 90.19(8) . . ? N2 Rh1 Rh2 89.95(7) . . ? N3 Rh1 Rh2 174.15(7) . . ? C16 Rh2 C10 91.03(12) . . ? C16 Rh2 N16 178.22(11) . . ? C10 Rh2 N16 90.29(12) . . ? C16 Rh2 N17 89.80(11) . . ? C10 Rh2 N17 178.06(11) . . ? N16 Rh2 N17 88.84(10) . . ? C16 Rh2 N18 91.49(11) . . ? C10 Rh2 N18 97.47(11) . . ? N16 Rh2 N18 89.52(11) . . ? N17 Rh2 N18 84.26(10) . . ? C16 Rh2 Rh1 90.98(9) . . ? C10 Rh2 Rh1 86.59(9) . . ? N16 Rh2 Rh1 87.91(8) . . ? N17 Rh2 Rh1 91.65(7) . . ? N18 Rh2 Rh1 175.21(7) . . ? C1 N1 Rh1 168.9(3) . . ? C3 N2 Rh1 166.3(3) . . ? C5 N3 Rh1 167.2(3) . . ? C7 N4 C8 110.4(3) . . ? C7 N4 N7 123.5(3) . . ? C8 N4 N7 125.5(3) . . ? C8 N5 N6 103.9(3) . . ? C7 N6 N5 113.8(3) . . ? C7 N6 C9 130.1(3) . . ? N5 N6 C9 116.0(3) . . ? C11 N7 C10 110.6(3) . . ? C11 N7 N4 123.7(3) . . ? C10 N7 N4 125.5(2) . . ? C11 N8 N9 104.0(3) . . ? C10 N9 N8 114.1(3) . . ? C10 N9 C12 129.6(3) . . ? N8 N9 C12 116.3(3) . . ? C13 N10 C14 110.1(3) . . ? C13 N10 N13 125.6(2) . . ? C14 N10 N13 124.3(3) . . ? C14 N11 N12 104.6(3) . . ? C13 N12 N11 113.9(3) . . ? C13 N12 C15 129.0(3) . . ? N11 N12 C15 117.0(3) . . ? C17 N13 C16 111.0(2) . . ? C17 N13 N10 124.1(3) . . ? C16 N13 N10 124.6(2) . . ? C17 N14 N15 104.1(3) . . ? C16 N15 N14 114.1(3) . . ? C16 N15 C18 128.4(3) . . ? N14 N15 C18 117.5(2) . . ? C19 N16 Rh2 178.5(3) . . ? C21 N17 Rh2 168.9(3) . . ? C23 N18 Rh2 165.9(3) . . ? N1 C1 C2 179.9(6) . . ? N2 C3 C4 178.7(4) . . ? N3 C5 C6 179.6(4) . . ? N6 C7 N4 101.9(3) . . ? N6 C7 Rh1 131.4(2) . . ? N4 C7 Rh1 126.7(2) . . ? N5 C8 N4 109.9(3) . . ? N9 C10 N7 101.4(3) . . ? N9 C10 Rh2 130.0(2) . . ? N7 C10 Rh2 128.1(2) . . ? N8 C11 N7 109.8(3) . . ? N12 C13 N10 101.8(3) . . ? N12 C13 Rh1 129.6(2) . . ? N10 C13 Rh1 128.1(2) . . ? N11 C14 N10 109.5(3) . . ? N15 C16 N13 101.3(3) . . ? N15 C16 Rh2 132.5(2) . . ? N13 C16 Rh2 126.2(2) . . ? N14 C17 N13 109.6(3) . . ? N16 C19 C20 177.4(4) . . ? N17 C21 C22 179.0(4) . . ? N18 C23 C24 179.2(4) . . ? F3 B1 F4 111.5(4) . . ? F3 B1 F2 110.0(4) . . ? F4 B1 F2 109.9(4) . . ? F3 B1 F1 108.9(4) . . ? F4 B1 F1 108.1(5) . . ? F2 B1 F1 108.5(5) . . ? F5 B2 F7 109.8(5) . . ? F5 B2 F8 110.1(4) . . ? F7 B2 F8 109.8(4) . . ? F5 B2 F6 111.2(4) . . ? F7 B2 F6 107.8(4) . . ? F8 B2 F6 108.1(4) . . ? F12 B3 F10 109.3(3) . . ? F12 B3 F11 109.7(4) . . ? F10 B3 F11 110.1(4) . . ? F12 B3 F9 109.6(3) . . ? F10 B3 F9 108.3(3) . . ? F11 B3 F9 109.8(3) . . ? F15 B4 F14 110.9(4) . . ? F15 B4 F16 112.1(4) . . ? F14 B4 F16 109.2(4) . . ? F15 B4 F13 109.3(4) . . ? F14 B4 F13 108.2(4) . . ? F16 B4 F13 107.0(4) . . ? N19 C26 C25 177.8(6) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 29.01 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.721 _refine_diff_density_min -0.841 _refine_diff_density_rms 0.111