Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Andrew Hallett' _publ_contact_author_address ; Chemistry Cardiff University Main Building Park Place Cardiff CF10 3AT UNITED KINGDOM ; _publ_contact_author_email HALLETTAJ@CARDIFF.AC.UK _publ_section_title ; Solid state and solution structures of rhodium and iridium poly(pyrazolyl)borate diene complexes ; loop_ _publ_author_name 'Andrew Hallett' 'Chris Adams' 'Kirsty M. Anderson' 'Jonathan Charmant' 'N. Connelly' ; B.A.Field ; 'Mathew Horne' data_2 _database_code_depnum_ccdc_archive 'CCDC 670936' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H27 B N5 Rh' _chemical_formula_weight 439.18 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 10.6609(9) _cell_length_b 12.3423(10) _cell_length_c 14.9842(13) _cell_angle_alpha 90.00 _cell_angle_beta 91.574(2) _cell_angle_gamma 90.00 _cell_volume 1970.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 94 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.480 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 0.879 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.690329 _exptl_absorpt_correction_T_max 0.825076 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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_% none _diffrn_reflns_number 5288 _diffrn_reflns_av_R_equivalents 0.0244 _diffrn_reflns_av_sigmaI/netI 0.0231 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1829 _reflns_number_gt 1678 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0485P)^2^+0.7437P] 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 1829 _refine_ls_number_parameters 139 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0303 _refine_ls_R_factor_gt 0.0273 _refine_ls_wR_factor_ref 0.0705 _refine_ls_wR_factor_gt 0.0695 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _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 Rh1 Rh 0.72228(2) 0.0000 0.108824(16) 0.01971(12) Uani 1 2 d S . . B1 B 0.8928(4) 0.0000 0.2766(3) 0.0249(9) Uani 1 2 d S . . N1 N 0.72025(19) 0.11720(17) 0.21124(13) 0.0224(4) Uani 1 1 d . . . N2 N 0.80665(19) 0.10158(17) 0.28001(12) 0.0232(5) Uani 1 1 d . . . C1 C 0.7993(2) 0.0948(2) 0.00620(16) 0.0251(5) Uani 1 1 d . . . H1A H 0.8485 0.1606 0.0177 0.030 Uiso 1 1 calc R . . C5 C 0.8461(4) 0.0000 -0.0509(2) 0.0275(8) Uani 1 2 d S . . H2A H 0.9348 0.0000 -0.0663 0.033 Uiso 1 2 calc SR . . C3 C 0.7476(4) 0.0000 -0.1289(2) 0.0275(8) Uani 1 2 d S . . H3A H 0.7515 0.0645 -0.1657 0.033 Uiso 0.50 1 calc PR . . H3B H 0.7515 -0.0645 -0.1657 0.033 Uiso 0.50 1 calc PR . . C4 C 0.6353(3) 0.0000 -0.0667(2) 0.0251(8) Uani 1 2 d S . . H4A H 0.5511 0.0000 -0.0947 0.030 Uiso 1 2 calc SR . . C2 C 0.6692(2) -0.0947(2) -0.00366(16) 0.0238(5) Uani 1 1 d . . . H5A H 0.6182 -0.1605 0.0004 0.029 Uiso 1 1 calc R . . C6 C 0.5481(3) 0.2461(2) 0.17245(18) 0.0315(6) Uani 1 1 d . . . H6A H 0.4952 0.1858 0.1566 0.047 Uiso 1 1 calc R . . H6B H 0.5787 0.2790 0.1192 0.047 Uiso 1 1 calc R . . H6C H 0.5007 0.2984 0.2050 0.047 Uiso 1 1 calc R . . C7 C 0.6562(2) 0.2077(2) 0.22926(16) 0.0244(5) Uani 1 1 d . . . C8 C 0.7037(3) 0.2516(2) 0.30941(17) 0.0293(6) Uani 1 1 d . . . H8A H 0.6771 0.3148 0.3369 0.035 Uiso 1 1 calc R . . C9 C 0.7975(3) 0.1829(2) 0.33958(17) 0.0272(6) Uani 1 1 d . . . C10 C 0.8791(3) 0.1894(3) 0.42211(17) 0.0349(6) Uani 1 1 d . . . H10A H 0.9656 0.1899 0.4060 0.052 Uiso 1 1 calc R . . H10B H 0.8636 0.1278 0.4593 0.052 Uiso 1 1 calc R . . H10C H 0.8604 0.2546 0.4540 0.052 Uiso 1 1 calc R . . C98 C 0.3949(6) 0.0000 0.4062(4) 0.0613(15) Uani 1 2 d S . . N99 N 0.3167(6) 0.0000 0.4565(4) 0.092(2) Uani 1 2 d S . . C99 C 0.4932(7) 0.0000 0.3459(4) 0.0789(19) Uani 1 2 d S . . H99A H 0.5670 0.0305 0.3741 0.118 Uiso 0.50 1 calc PR . . H99B H 0.4696 0.0425 0.2944 0.118 Uiso 0.50 1 calc PR . . H99C H 0.5103 -0.0730 0.3278 0.118 Uiso 0.50 1 calc PR . . H98 H 0.953(5) 0.0000 0.336(3) 0.057(15) Uiso 1 2 d S . . H99 H 0.942(3) 0.0000 0.210(2) 0.016(9) Uiso 1 2 d S . . 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 0.02226(17) 0.01610(17) 0.02091(17) 0.000 0.00344(11) 0.000 B1 0.021(2) 0.025(2) 0.028(2) 0.000 0.0012(17) 0.000 N1 0.0242(11) 0.0206(10) 0.0224(10) -0.0006(9) 0.0029(9) 0.0001(9) N2 0.0230(11) 0.0247(11) 0.0219(10) -0.0016(9) 0.0027(8) -0.0026(9) C1 0.0307(14) 0.0217(13) 0.0231(12) 0.0036(10) 0.0024(10) -0.0069(11) C5 0.0223(19) 0.035(2) 0.0255(18) 0.000 0.0048(15) 0.000 C3 0.028(2) 0.030(2) 0.0247(18) 0.000 0.0019(15) 0.000 C4 0.0222(18) 0.0267(19) 0.0264(18) 0.000 -0.0002(15) 0.000 C2 0.0291(13) 0.0199(13) 0.0227(12) -0.0034(10) 0.0017(10) -0.0020(11) C6 0.0319(15) 0.0286(14) 0.0344(14) -0.0043(12) 0.0060(12) 0.0061(12) C7 0.0270(13) 0.0194(12) 0.0269(13) -0.0001(10) 0.0074(11) 0.0003(10) C8 0.0323(15) 0.0248(14) 0.0314(14) -0.0070(11) 0.0115(12) -0.0023(11) C9 0.0287(14) 0.0259(13) 0.0273(13) -0.0044(11) 0.0081(11) -0.0048(11) C10 0.0336(15) 0.0415(16) 0.0296(14) -0.0104(13) 0.0022(12) -0.0033(13) C98 0.071(4) 0.032(3) 0.082(4) 0.000 0.019(3) 0.000 N99 0.090(4) 0.071(4) 0.117(5) 0.000 0.064(4) 0.000 C99 0.088(5) 0.071(4) 0.080(4) 0.000 0.038(4) 0.000 _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 N1 2.1095(19) . ? Rh1 N1 2.1095(19) 6 ? Rh1 C2 2.115(2) . ? Rh1 C2 2.115(2) 6 ? Rh1 C1 2.116(2) . ? Rh1 C1 2.116(2) 6 ? B1 N2 1.556(3) 6 ? B1 N2 1.556(3) . ? N1 C7 1.340(3) . ? N1 N2 1.377(3) . ? N2 C9 1.348(3) . ? C1 C2 1.391(4) 6 ? C1 C5 1.541(3) . ? C5 C1 1.541(3) 6 ? C5 C3 1.549(5) . ? C3 C4 1.538(5) . ? C4 C2 1.539(3) 6 ? C4 C2 1.539(3) . ? C2 C1 1.391(4) 6 ? C6 C7 1.492(4) . ? C7 C8 1.400(3) . ? C8 C9 1.379(4) . ? C9 C10 1.494(4) . ? C98 N99 1.139(7) . ? C98 C99 1.403(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 N1 Rh1 N1 86.59(11) . 6 ? N1 Rh1 C2 161.92(9) . . ? N1 Rh1 C2 101.12(9) 6 . ? N1 Rh1 C2 101.12(9) . 6 ? N1 Rh1 C2 161.92(9) 6 6 ? C2 Rh1 C2 67.08(13) . 6 ? N1 Rh1 C1 99.30(9) . . ? N1 Rh1 C1 156.91(9) 6 . ? C2 Rh1 C1 80.05(10) . . ? C2 Rh1 C1 38.38(10) 6 . ? N1 Rh1 C1 156.91(9) . 6 ? N1 Rh1 C1 99.29(9) 6 6 ? C2 Rh1 C1 38.38(10) . 6 ? C2 Rh1 C1 80.04(10) 6 6 ? C1 Rh1 C1 67.14(14) . 6 ? N2 B1 N2 107.4(3) 6 . ? C7 N1 N2 107.45(19) . . ? C7 N1 Rh1 137.18(17) . . ? N2 N1 Rh1 115.37(15) . . ? C9 N2 N1 109.4(2) . . ? C9 N2 B1 132.5(2) . . ? N1 N2 B1 118.1(2) . . ? C2 C1 C5 106.1(2) 6 . ? C2 C1 Rh1 70.80(14) 6 . ? C5 C1 Rh1 97.01(16) . . ? C1 C5 C1 98.8(3) . 6 ? C1 C5 C3 101.3(2) . . ? C1 C5 C3 101.3(2) 6 . ? C4 C3 C5 93.8(3) . . ? C3 C4 C2 101.4(2) . 6 ? C3 C4 C2 101.4(2) . . ? C2 C4 C2 98.8(3) 6 . ? C1 C2 C4 106.4(2) 6 . ? C1 C2 Rh1 70.82(13) 6 . ? C4 C2 Rh1 97.03(16) . . ? N1 C7 C8 108.8(2) . . ? N1 C7 C6 122.7(2) . . ? C8 C7 C6 128.4(2) . . ? C9 C8 C7 106.5(2) . . ? N2 C9 C8 107.8(2) . . ? N2 C9 C10 122.5(2) . . ? C8 C9 C10 129.7(2) . . ? N99 C98 C99 178.7(8) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.056 _refine_diff_density_min -0.356 _refine_diff_density_rms 0.081 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 670937' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H37 B N7 Rh' _chemical_formula_weight 549.34 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.7043(14) _cell_length_b 14.368(2) _cell_length_c 11.1111(18) _cell_angle_alpha 90.00 _cell_angle_beta 111.748(2) _cell_angle_gamma 90.00 _cell_volume 1290.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 74 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.414 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 572 _exptl_absorpt_coefficient_mu 0.689 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.819686 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _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 'Siemens CCD area detector' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 8394 _diffrn_reflns_av_R_equivalents 0.0396 _diffrn_reflns_av_sigmaI/netI 0.0804 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5089 _reflns_number_gt 4000 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0244P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(3) _refine_ls_number_reflns 5089 _refine_ls_number_parameters 318 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0565 _refine_ls_R_factor_gt 0.0372 _refine_ls_wR_factor_ref 0.0676 _refine_ls_wR_factor_gt 0.0628 _refine_ls_goodness_of_fit_ref 0.911 _refine_ls_restrained_S_all 0.911 _refine_ls_shift/su_max 0.012 _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 0.41201(3) 0.26024(2) 0.02839(3) 0.02459(8) Uani 1 1 d . . . N1 N 0.2985(4) 0.3842(3) 0.0546(4) 0.0231(9) Uani 1 1 d . . . N2 N 0.3442(4) 0.4200(2) 0.1772(3) 0.0225(8) Uani 1 1 d . . . N3 N 0.6348(4) 0.3294(2) 0.1381(3) 0.0209(8) Uani 1 1 d . . . N4 N 0.6405(4) 0.3675(2) 0.2542(3) 0.0217(8) Uani 1 1 d . . . N5 N 0.2646(4) 0.2733(4) 0.3087(3) 0.0286(10) Uani 1 1 d . . . N6 N 0.4274(4) 0.2782(3) 0.3189(3) 0.0243(10) Uani 1 1 d . . . B B 0.4854(6) 0.3749(4) 0.2917(5) 0.0240(11) Uani 1 1 d . . . H1 H 0.520(4) 0.422(2) 0.383(3) 0.015(10) Uiso 1 1 d . . . C1 C 0.2231(5) 0.1648(3) 0.0210(5) 0.0315(12) Uani 1 1 d . . . H1A H 0.1576 0.1851 0.0737 0.038 Uiso 1 1 calc R . . C2 C 0.1755(5) 0.2092(3) -0.0980(5) 0.0322(12) Uani 1 1 d . . . H2A H 0.0828 0.2545 -0.1145 0.039 Uiso 1 1 calc R . . C6 C 0.1837(6) 0.1655(4) -0.2189(5) 0.0451(14) Uani 1 1 d . . . H3A H 0.1625 0.2138 -0.2867 0.054 Uiso 1 1 calc R . . H3B H 0.0961 0.1177 -0.2515 0.054 Uiso 1 1 calc R . . C5 C 0.3533(6) 0.1202(4) -0.1937(5) 0.0486(15) Uani 1 1 d . . . H4A H 0.3475 0.0534 -0.1738 0.058 Uiso 1 1 calc R . . H4B H 0.3783 0.1244 -0.2735 0.058 Uiso 1 1 calc R . . C4 C 0.4923(5) 0.1653(3) -0.0833(5) 0.0359(12) Uani 1 1 d . . . H5B H 0.5833 0.1901 -0.1088 0.043 Uiso 1 1 calc R . . C3 C 0.5456(5) 0.1341(3) 0.0438(5) 0.0333(12) Uani 1 1 d . . . H6A H 0.6674 0.1409 0.0918 0.040 Uiso 1 1 calc R . . C7 C 0.4705(5) 0.0543(3) 0.0907(5) 0.0418(13) Uani 1 1 d . . . H7A H 0.5187 0.0524 0.1866 0.050 Uiso 1 1 calc R . . H7B H 0.4985 -0.0048 0.0580 0.050 Uiso 1 1 calc R . . C8 C 0.2796(6) 0.0631(3) 0.0451(6) 0.0406(13) Uani 1 1 d . . . H8A H 0.2274 0.0270 -0.0358 0.049 Uiso 1 1 calc R . . H8B H 0.2425 0.0362 0.1118 0.049 Uiso 1 1 calc R . . C9 C 0.1891(5) 0.4437(3) -0.0268(4) 0.0267(11) Uani 1 1 d . . . C10 C 0.1259(6) 0.4324(4) -0.1698(5) 0.0440(13) Uani 1 1 d . . . H10A H 0.1968 0.3888 -0.1931 0.066 Uiso 1 1 calc R . . H10B H 0.1265 0.4929 -0.2105 0.066 Uiso 1 1 calc R . . H10C H 0.0126 0.4081 -0.2001 0.066 Uiso 1 1 calc R . . C11 C 0.1590(5) 0.5146(3) 0.0469(5) 0.0316(11) Uani 1 1 d . . . H11A H 0.0836 0.5646 0.0147 0.038 Uiso 1 1 calc R . . C12 C 0.2570(5) 0.4995(3) 0.1736(5) 0.0274(10) Uani 1 1 d . . . C13 C 0.2729(6) 0.5555(3) 0.2907(5) 0.0391(12) Uani 1 1 d . . . H13A H 0.3884 0.5745 0.3348 0.059 Uiso 1 1 calc R . . H13B H 0.2381 0.5179 0.3496 0.059 Uiso 1 1 calc R . . H13C H 0.2028 0.6109 0.2645 0.059 Uiso 1 1 calc R . . C14 C 0.7874(5) 0.3385(3) 0.1354(4) 0.0238(10) Uani 1 1 d . . . C15 C 0.8337(5) 0.3082(3) 0.0253(4) 0.0332(11) Uani 1 1 d . . . H15A H 0.7527 0.3323 -0.0560 0.050 Uiso 1 1 calc R . . H15B H 0.8352 0.2401 0.0220 0.050 Uiso 1 1 calc R . . H15C H 0.9437 0.3324 0.0373 0.050 Uiso 1 1 calc R . . C16 C 0.8903(5) 0.3819(3) 0.2485(4) 0.0268(10) Uani 1 1 d . . . H16A H 1.0039 0.3967 0.2709 0.032 Uiso 1 1 calc R . . C17 C 0.7959(5) 0.3993(3) 0.3214(4) 0.0249(10) Uani 1 1 d . . . C18 C 0.8455(6) 0.4452(3) 0.4520(4) 0.0382(12) Uani 1 1 d . . . H18A H 0.7779 0.5009 0.4450 0.057 Uiso 1 1 calc R . . H18B H 0.9625 0.4627 0.4822 0.057 Uiso 1 1 calc R . . H18C H 0.8283 0.4017 0.5138 0.057 Uiso 1 1 calc R . . C20 C 0.2476(5) 0.1887(3) 0.3523(5) 0.0315(11) Uani 1 1 d . . . C21 C 0.0837(5) 0.1594(4) 0.3549(5) 0.0467(14) Uani 1 1 d . . . H21A H -0.0035 0.1995 0.2969 0.070 Uiso 1 1 calc R . . H21B H 0.0858 0.1648 0.4434 0.070 Uiso 1 1 calc R . . H21C H 0.0617 0.0946 0.3260 0.070 Uiso 1 1 calc R . . C22 C 0.3976(5) 0.1392(3) 0.3921(4) 0.0333(11) Uani 1 1 d . . . H22A H 0.4174 0.0778 0.4260 0.040 Uiso 1 1 calc R . . C23 C 0.5088(5) 0.1980(3) 0.3717(5) 0.0300(11) Uani 1 1 d . . . C24 C 0.6892(5) 0.1832(3) 0.4007(5) 0.0374(12) Uani 1 1 d . . . H24A H 0.7537 0.2290 0.4650 0.056 Uiso 1 1 calc R . . H24B H 0.7116 0.1907 0.3210 0.056 Uiso 1 1 calc R . . H24C H 0.7206 0.1203 0.4351 0.056 Uiso 1 1 calc R . . C99 C 0.5939(13) 0.3342(6) 0.6588(7) 0.077(2) Uani 1 1 d . . . C100 C 0.4121(9) 0.3549(6) 0.6221(7) 0.097(3) Uani 1 1 d . . . H10D H 0.3960 0.4222 0.6247 0.145 Uiso 1 1 calc R . . H10E H 0.3717 0.3241 0.6834 0.145 Uiso 1 1 calc R . . H10F H 0.3506 0.3317 0.5344 0.145 Uiso 1 1 calc R . . N100 N 0.7211(9) 0.3185(5) 0.6841(6) 0.093(2) 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 0.01886(12) 0.02168(15) 0.03330(16) -0.0062(3) 0.00976(11) -0.0009(3) N1 0.0190(19) 0.023(2) 0.027(2) -0.0019(18) 0.0073(18) -0.0001(17) N2 0.0205(17) 0.0167(19) 0.031(2) 0.0011(16) 0.0105(17) -0.0004(15) N3 0.0190(17) 0.0188(19) 0.026(2) -0.0007(16) 0.0099(16) 0.0008(15) N4 0.0194(17) 0.019(2) 0.026(2) 0.0020(16) 0.0085(16) 0.0009(15) N5 0.0199(15) 0.027(3) 0.040(2) 0.001(2) 0.0117(14) -0.0044(19) N6 0.0195(15) 0.022(3) 0.0336(19) 0.0028(18) 0.0121(14) 0.0019(16) B 0.021(2) 0.024(3) 0.028(3) -0.008(2) 0.010(2) -0.003(2) C1 0.017(2) 0.031(3) 0.049(3) -0.008(3) 0.015(2) -0.003(2) C2 0.018(2) 0.034(3) 0.043(3) -0.006(2) 0.010(2) -0.002(2) C6 0.034(3) 0.053(4) 0.047(3) -0.023(3) 0.013(3) -0.012(3) C5 0.041(3) 0.056(4) 0.056(4) -0.033(3) 0.027(3) -0.014(3) C4 0.028(2) 0.036(3) 0.051(3) -0.020(3) 0.022(2) -0.003(2) C3 0.028(2) 0.020(3) 0.057(4) -0.013(2) 0.022(2) -0.002(2) C7 0.033(3) 0.026(3) 0.069(4) -0.001(3) 0.021(3) 0.006(2) C8 0.036(3) 0.028(3) 0.060(4) -0.011(3) 0.021(3) -0.006(2) C9 0.018(2) 0.029(3) 0.032(3) 0.008(2) 0.007(2) -0.001(2) C10 0.034(3) 0.045(3) 0.042(3) 0.012(3) 0.002(2) 0.003(2) C11 0.023(2) 0.017(2) 0.051(3) 0.006(2) 0.010(2) 0.0030(19) C12 0.020(2) 0.020(2) 0.046(3) 0.001(2) 0.016(2) -0.0009(19) C13 0.033(3) 0.032(3) 0.058(3) -0.017(3) 0.024(3) 0.000(2) C14 0.020(2) 0.020(2) 0.033(3) 0.001(2) 0.012(2) -0.0006(18) C15 0.030(2) 0.032(3) 0.044(3) -0.006(2) 0.021(2) -0.001(2) C16 0.026(2) 0.014(2) 0.038(3) 0.004(2) 0.009(2) -0.0002(18) C17 0.023(2) 0.016(2) 0.032(3) 0.0037(19) 0.006(2) -0.0004(18) C18 0.034(3) 0.042(3) 0.038(3) -0.006(2) 0.012(2) -0.013(2) C20 0.026(2) 0.035(3) 0.035(3) 0.007(2) 0.013(2) -0.003(2) C21 0.031(3) 0.045(3) 0.066(4) 0.022(3) 0.020(3) -0.004(2) C22 0.030(2) 0.025(3) 0.043(3) 0.007(2) 0.012(2) 0.001(2) C23 0.029(2) 0.024(3) 0.041(3) 0.008(2) 0.018(2) 0.006(2) C24 0.028(2) 0.028(3) 0.058(3) 0.014(2) 0.018(2) 0.005(2) C99 0.123(7) 0.080(5) 0.034(4) -0.008(4) 0.037(5) -0.041(6) C100 0.112(7) 0.128(7) 0.067(5) -0.028(5) 0.053(5) -0.061(6) N100 0.097(5) 0.135(6) 0.041(4) -0.010(3) 0.018(4) -0.057(5) _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 N1 2.109(4) . ? Rh1 N3 2.117(3) . ? Rh1 C1 2.119(4) . ? Rh1 C3 2.126(4) . ? Rh1 C4 2.129(4) . ? Rh1 C2 2.147(4) . ? N1 C9 1.348(5) . ? N1 N2 1.370(5) . ? N2 C12 1.363(5) . ? N2 B 1.547(6) . ? N3 C14 1.346(5) . ? N3 N4 1.386(5) . ? N4 C17 1.359(5) . ? N4 B 1.557(6) . ? N5 C20 1.336(6) . ? N5 N6 1.381(4) . ? N6 C23 1.365(5) . ? N6 B 1.546(6) . ? C1 C2 1.386(7) . ? C1 C8 1.534(7) . ? C2 C6 1.508(6) . ? C6 C5 1.541(6) . ? C5 C4 1.513(6) . ? C4 C3 1.388(7) . ? C3 C7 1.505(6) . ? C7 C8 1.552(6) . ? C9 C11 1.390(6) . ? C9 C10 1.485(6) . ? C11 C12 1.366(6) . ? C12 C13 1.492(6) . ? C14 C16 1.392(6) . ? C14 C15 1.488(6) . ? C16 C17 1.373(6) . ? C17 C18 1.504(6) . ? C20 C22 1.406(6) . ? C20 C21 1.498(6) . ? C22 C23 1.366(6) . ? C23 C24 1.497(6) . ? C99 N100 1.061(10) . ? C99 C100 1.510(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 N1 Rh1 N3 84.28(14) . . ? N1 Rh1 C1 98.94(18) . . ? N3 Rh1 C1 149.10(17) . . ? N1 Rh1 C3 168.35(17) . . ? N3 Rh1 C3 89.81(15) . . ? C1 Rh1 C3 81.07(18) . . ? N1 Rh1 C4 153.31(17) . . ? N3 Rh1 C4 101.98(15) . . ? C1 Rh1 C4 88.88(19) . . ? C3 Rh1 C4 38.07(18) . . ? N1 Rh1 C2 89.68(16) . . ? N3 Rh1 C2 171.54(17) . . ? C1 Rh1 C2 37.92(17) . . ? C3 Rh1 C2 97.15(18) . . ? C4 Rh1 C2 80.90(17) . . ? C9 N1 N2 107.6(4) . . ? C9 N1 Rh1 133.9(3) . . ? N2 N1 Rh1 118.4(3) . . ? C12 N2 N1 109.4(3) . . ? C12 N2 B 129.8(4) . . ? N1 N2 B 120.7(3) . . ? C14 N3 N4 106.7(3) . . ? C14 N3 Rh1 137.2(3) . . ? N4 N3 Rh1 115.5(2) . . ? C17 N4 N3 109.2(3) . . ? C17 N4 B 128.0(4) . . ? N3 N4 B 122.7(3) . . ? C20 N5 N6 105.3(4) . . ? C23 N6 N5 110.2(4) . . ? C23 N6 B 133.4(3) . . ? N5 N6 B 115.4(4) . . ? N6 B N2 108.6(3) . . ? N6 B N4 111.7(4) . . ? N2 B N4 108.2(4) . . ? C2 C1 C8 124.6(5) . . ? C2 C1 Rh1 72.1(3) . . ? C8 C1 Rh1 114.6(3) . . ? C1 C2 C6 124.2(5) . . ? C1 C2 Rh1 70.0(3) . . ? C6 C2 Rh1 112.0(3) . . ? C2 C6 C5 111.8(4) . . ? C4 C5 C6 113.0(4) . . ? C3 C4 C5 123.5(5) . . ? C3 C4 Rh1 70.8(3) . . ? C5 C4 Rh1 114.2(3) . . ? C4 C3 C7 125.1(4) . . ? C4 C3 Rh1 71.1(3) . . ? C7 C3 Rh1 112.5(3) . . ? C3 C7 C8 112.0(4) . . ? C1 C8 C7 111.7(4) . . ? N1 C9 C11 108.0(4) . . ? N1 C9 C10 122.5(4) . . ? C11 C9 C10 129.4(4) . . ? C12 C11 C9 108.0(4) . . ? N2 C12 C11 106.9(4) . . ? N2 C12 C13 123.7(4) . . ? C11 C12 C13 129.4(4) . . ? N3 C14 C16 109.5(4) . . ? N3 C14 C15 124.1(4) . . ? C16 C14 C15 126.4(4) . . ? C17 C16 C14 106.8(4) . . ? N4 C17 C16 107.8(4) . . ? N4 C17 C18 123.3(4) . . ? C16 C17 C18 128.9(4) . . ? N5 C20 C22 111.1(4) . . ? N5 C20 C21 119.8(4) . . ? C22 C20 C21 129.1(4) . . ? C23 C22 C20 105.5(4) . . ? N6 C23 C22 107.8(4) . . ? N6 C23 C24 123.3(4) . . ? C22 C23 C24 128.9(4) . . ? N100 C99 C100 179.1(10) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.360 _refine_diff_density_min -0.402 _refine_diff_density_rms 0.077 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 670938' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H31.50 B N6.50 Rh' _chemical_formula_weight 512.77 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6855(11) _cell_length_b 10.8695(11) _cell_length_c 12.6391(13) _cell_angle_alpha 94.624(2) _cell_angle_beta 111.348(2) _cell_angle_gamma 118.521(2) _cell_volume 1141.8(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.491 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 530 _exptl_absorpt_coefficient_mu 0.772 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.864 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details SADABS _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 '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_% 0 _diffrn_reflns_number 12019 _diffrn_reflns_av_R_equivalents 0.0430 _diffrn_reflns_av_sigmaI/netI 0.0697 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 27.52 _reflns_number_total 5191 _reflns_number_gt 4114 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0255P)^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 5191 _refine_ls_number_parameters 306 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0512 _refine_ls_R_factor_gt 0.0336 _refine_ls_wR_factor_ref 0.0652 _refine_ls_wR_factor_gt 0.0618 _refine_ls_goodness_of_fit_ref 0.943 _refine_ls_restrained_S_all 0.943 _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 Rh1 Rh -0.50524(3) -0.32482(2) -0.65744(2) 0.01679(7) Uani 1 1 d . . . B1 B -0.8089(4) -0.6457(3) -0.8414(3) 0.0196(7) Uani 1 1 d . . . H1 H -0.914(3) -0.759(2) -0.909(2) 0.008(6) Uiso 1 1 d . . . N5 N -0.6514(3) -0.3775(2) -0.84405(19) 0.0190(5) Uani 1 1 d . . . N6 N -0.7782(3) -0.5227(2) -0.90346(19) 0.0186(5) Uani 1 1 d . . . N3 N -0.7466(2) -0.4651(2) -0.66635(19) 0.0182(5) Uani 1 1 d . . . N4 N -0.8437(2) -0.6079(2) -0.74075(19) 0.0178(5) Uani 1 1 d . . . N1 N -0.5130(3) -0.5252(2) -0.72681(19) 0.0188(5) Uani 1 1 d . . . N2 N -0.6584(2) -0.6534(2) -0.79337(19) 0.0178(5) Uani 1 1 d . . . C14 C -0.5402(4) -0.1450(3) -0.8951(3) 0.0345(8) Uani 1 1 d . . . H14A H -0.5338 -0.0897 -0.8261 0.052 Uiso 1 1 calc R . . H14B H -0.5738 -0.1118 -0.9637 0.052 Uiso 1 1 calc R . . H14C H -0.4347 -0.1283 -0.8759 0.052 Uiso 1 1 calc R . . C15 C -0.6593(3) -0.3056(3) -0.9249(2) 0.0226(6) Uani 1 1 d . . . C16 C -0.7887(3) -0.4015(3) -1.0349(2) 0.0240(6) Uani 1 1 d . . . H16A H -0.8206 -0.3780 -1.1068 0.029 Uiso 1 1 calc R . . C17 C -0.8620(3) -0.5380(3) -1.0193(2) 0.0206(6) Uani 1 1 d . . . C18 C -1.0075(3) -0.6792(3) -1.1101(3) 0.0308(7) Uani 1 1 d . . . H18A H -1.0870 -0.7208 -1.0804 0.046 Uiso 1 1 calc R . . H18B H -0.9778 -0.7490 -1.1246 0.046 Uiso 1 1 calc R . . H18C H -1.0531 -0.6606 -1.1848 0.046 Uiso 1 1 calc R . . C9 C -0.7599(3) -0.3023(3) -0.5282(3) 0.0256(6) Uani 1 1 d . . . H9A H -0.6864 -0.2235 -0.5487 0.038 Uiso 1 1 calc R . . H9B H -0.7025 -0.2957 -0.4451 0.038 Uiso 1 1 calc R . . H9C H -0.8493 -0.2920 -0.5376 0.038 Uiso 1 1 calc R . . C10 C -0.8232(3) -0.4479(3) -0.6089(2) 0.0196(6) Uani 1 1 d . . . C11 C -0.9690(3) -0.5813(3) -0.6446(2) 0.0213(6) Uani 1 1 d . . . H11A H -1.0460 -0.6000 -0.6169 0.026 Uiso 1 1 calc R . . C12 C -0.9789(3) -0.6799(3) -0.7274(2) 0.0202(6) Uani 1 1 d . . . C13 C -1.1085(3) -0.8379(3) -0.7948(3) 0.0298(7) Uani 1 1 d . . . H13A H -1.0631 -0.8984 -0.7802 0.045 Uiso 1 1 calc R . . H13B H -1.1563 -0.8500 -0.8804 0.045 Uiso 1 1 calc R . . H13C H -1.1911 -0.8689 -0.7679 0.045 Uiso 1 1 calc R . . C19 C -0.2273(3) -0.4315(3) -0.6674(3) 0.0259(6) Uani 1 1 d . . . H19A H -0.2167 -0.3379 -0.6729 0.039 Uiso 1 1 calc R . . H19B H -0.1766 -0.4538 -0.7102 0.039 Uiso 1 1 calc R . . H19C H -0.1746 -0.4239 -0.5833 0.039 Uiso 1 1 calc R . . C20 C -0.4012(3) -0.5520(3) -0.7224(2) 0.0204(6) Uani 1 1 d . . . C21 C -0.4759(3) -0.7000(3) -0.7837(2) 0.0244(6) Uani 1 1 d . . . H21A H -0.4247 -0.7485 -0.7929 0.029 Uiso 1 1 calc R . . C22 C -0.6388(3) -0.7621(3) -0.8285(2) 0.0225(6) Uani 1 1 d . . . C23 C -0.7755(4) -0.9159(3) -0.9014(3) 0.0356(8) Uani 1 1 d . . . H23A H -0.8469 -0.9523 -0.8643 0.053 Uiso 1 1 calc R . . H23B H -0.7345 -0.9788 -0.9057 0.053 Uiso 1 1 calc R . . H23C H -0.8350 -0.9176 -0.9822 0.053 Uiso 1 1 calc R . . C1 C -0.4088(3) -0.2449(3) -0.4670(2) 0.0220(6) Uani 1 1 d . . . H1A H -0.4667 -0.2972 -0.4220 0.026 Uiso 1 1 calc R . . C2 C -0.3083(3) -0.2744(3) -0.4918(2) 0.0212(6) Uani 1 1 d . . . H2A H -0.2871 -0.3502 -0.4665 0.025 Uiso 1 1 calc R . . C5 C -0.1818(3) -0.1312(3) -0.4976(2) 0.0229(6) Uani 1 1 d . . . H5A H -0.0816 -0.1229 -0.4906 0.028 Uiso 1 1 calc R . . C4 C -0.2919(3) -0.1297(3) -0.6172(2) 0.0227(6) Uani 1 1 d . . . H4A H -0.2565 -0.0976 -0.6787 0.027 Uiso 1 1 calc R . . C3 C -0.3960(3) -0.0988(3) -0.5909(2) 0.0224(6) Uani 1 1 d . . . H3A H -0.4399 -0.0436 -0.6328 0.027 Uiso 1 1 calc R . . C6 C -0.3450(3) -0.0820(3) -0.4571(3) 0.0255(6) Uani 1 1 d . . . H6A H -0.3814 -0.0329 -0.4163 0.031 Uiso 1 1 calc R . . C7 C -0.1633(3) -0.0147(3) -0.4046(3) 0.0285(7) Uani 1 1 d . . . H7A H -0.1152 -0.0166 -0.3219 0.034 Uiso 1 1 calc R . . H7B H -0.1036 0.0862 -0.4089 0.034 Uiso 1 1 calc R . . C98 C -0.5000 -0.5000 -1.0000 0.0394(12) Uani 1 2 d S . . H98A H -0.5209 -0.4329 -1.0392 0.059 Uiso 0.50 1 calc PR . . H98B H -0.4014 -0.4880 -0.9963 0.059 Uiso 0.50 1 calc PR . . H98C H -0.4876 -0.4772 -0.9188 0.059 Uiso 0.50 1 calc PR . . N99 N -0.7531(7) -0.7818(7) -1.1274(5) 0.0467(15) Uani 0.50 1 d P . . C99 C -0.6476(8) -0.6669(8) -1.0749(6) 0.0345(15) Uani 0.50 1 d P . . 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 0.01573(11) 0.01652(11) 0.01694(11) 0.00594(8) 0.00766(8) 0.00778(9) B1 0.0163(16) 0.0177(15) 0.0196(17) 0.0038(13) 0.0065(13) 0.0072(13) N5 0.0182(12) 0.0227(12) 0.0193(12) 0.0091(10) 0.0098(10) 0.0122(10) N6 0.0179(12) 0.0201(12) 0.0188(12) 0.0059(9) 0.0088(10) 0.0108(10) N3 0.0176(11) 0.0183(11) 0.0167(12) 0.0057(9) 0.0087(10) 0.0079(10) N4 0.0153(11) 0.0169(11) 0.0179(12) 0.0050(9) 0.0073(10) 0.0068(10) N1 0.0184(12) 0.0206(12) 0.0182(12) 0.0064(9) 0.0084(10) 0.0111(10) N2 0.0185(12) 0.0162(11) 0.0157(12) 0.0033(9) 0.0070(10) 0.0083(10) C14 0.0320(17) 0.0298(17) 0.0354(19) 0.0191(14) 0.0128(15) 0.0131(14) C15 0.0234(15) 0.0295(16) 0.0238(16) 0.0142(12) 0.0129(13) 0.0182(13) C16 0.0245(15) 0.0325(16) 0.0206(15) 0.0128(13) 0.0093(13) 0.0195(14) C17 0.0190(14) 0.0289(15) 0.0179(15) 0.0066(12) 0.0076(12) 0.0165(13) C18 0.0258(16) 0.0317(17) 0.0220(16) 0.0017(13) 0.0039(13) 0.0130(14) C9 0.0286(16) 0.0268(15) 0.0282(17) 0.0059(12) 0.0152(14) 0.0185(13) C10 0.0189(14) 0.0251(14) 0.0174(14) 0.0089(11) 0.0081(12) 0.0136(12) C11 0.0177(14) 0.0287(15) 0.0219(15) 0.0123(12) 0.0109(12) 0.0137(12) C12 0.0157(14) 0.0204(14) 0.0217(15) 0.0104(12) 0.0067(12) 0.0089(12) C13 0.0217(15) 0.0223(15) 0.0363(18) 0.0090(13) 0.0137(14) 0.0055(13) C19 0.0257(16) 0.0316(16) 0.0260(16) 0.0109(13) 0.0142(13) 0.0175(14) C20 0.0205(14) 0.0258(15) 0.0173(14) 0.0089(12) 0.0089(12) 0.0139(12) C21 0.0310(17) 0.0282(15) 0.0210(15) 0.0061(12) 0.0118(13) 0.0213(14) C22 0.0277(16) 0.0216(14) 0.0186(15) 0.0043(11) 0.0089(13) 0.0152(13) C23 0.0348(18) 0.0241(16) 0.039(2) 0.0001(14) 0.0123(16) 0.0149(15) C1 0.0200(15) 0.0231(14) 0.0152(14) 0.0042(11) 0.0064(12) 0.0080(12) C2 0.0179(14) 0.0203(14) 0.0171(14) 0.0031(11) 0.0032(12) 0.0086(12) C5 0.0172(14) 0.0227(14) 0.0244(16) 0.0037(12) 0.0088(12) 0.0088(12) C4 0.0204(15) 0.0179(14) 0.0256(16) 0.0087(12) 0.0122(13) 0.0062(12) C3 0.0212(15) 0.0173(14) 0.0265(16) 0.0072(12) 0.0106(13) 0.0093(12) C6 0.0236(15) 0.0209(14) 0.0262(16) 0.0002(12) 0.0101(13) 0.0102(13) C7 0.0245(16) 0.0226(15) 0.0270(17) 0.0007(12) 0.0089(13) 0.0083(13) C98 0.046(3) 0.065(3) 0.034(3) 0.024(2) 0.026(2) 0.041(3) N99 0.052(4) 0.057(4) 0.038(4) 0.013(3) 0.025(3) 0.031(4) C99 0.045(4) 0.058(5) 0.028(4) 0.021(3) 0.023(3) 0.041(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 Rh1 C4 2.078(3) . ? Rh1 C3 2.078(3) . ? Rh1 N5 2.139(2) . ? Rh1 C1 2.148(3) . ? Rh1 C2 2.149(3) . ? Rh1 N1 2.234(2) . ? Rh1 N3 2.235(2) . ? B1 N4 1.527(4) . ? B1 N2 1.545(4) . ? B1 N6 1.564(4) . ? N5 C15 1.339(3) . ? N5 N6 1.385(3) . ? N6 C17 1.355(3) . ? N3 C10 1.337(3) . ? N3 N4 1.373(3) . ? N4 C12 1.359(3) . ? N1 C20 1.342(3) . ? N1 N2 1.362(3) . ? N2 C22 1.363(3) . ? C14 C15 1.493(4) . ? C15 C16 1.386(4) . ? C16 C17 1.379(4) . ? C17 C18 1.493(4) . ? C9 C10 1.489(4) . ? C10 C11 1.400(3) . ? C11 C12 1.373(4) . ? C12 C13 1.492(3) . ? C19 C20 1.496(4) . ? C20 C21 1.396(4) . ? C21 C22 1.380(4) . ? C22 C23 1.489(4) . ? C1 C2 1.383(4) . ? C1 C6 1.538(4) . ? C2 C5 1.528(4) . ? C5 C7 1.542(4) . ? C5 C4 1.548(4) . ? C4 C3 1.439(4) . ? C3 C6 1.540(4) . ? C6 C7 1.540(4) . ? C98 C99 1.606(8) . ? N99 C99 1.118(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 C4 Rh1 C3 40.50(11) . . ? C4 Rh1 N5 104.28(10) . . ? C3 Rh1 N5 104.01(10) . . ? C4 Rh1 C1 79.79(10) . . ? C3 Rh1 C1 66.27(10) . . ? N5 Rh1 C1 160.25(9) . . ? C4 Rh1 C2 66.37(10) . . ? C3 Rh1 C2 79.62(10) . . ? N5 Rh1 C2 161.38(9) . . ? C1 Rh1 C2 37.56(10) . . ? C4 Rh1 N1 113.05(10) . . ? C3 Rh1 N1 153.55(9) . . ? N5 Rh1 N1 80.70(8) . . ? C1 Rh1 N1 115.93(9) . . ? C2 Rh1 N1 88.24(9) . . ? C4 Rh1 N3 156.12(9) . . ? C3 Rh1 N3 115.68(9) . . ? N5 Rh1 N3 80.97(8) . . ? C1 Rh1 N3 87.93(9) . . ? C2 Rh1 N3 114.31(9) . . ? N1 Rh1 N3 90.72(8) . . ? N4 B1 N2 111.5(2) . . ? N4 B1 N6 108.7(2) . . ? N2 B1 N6 108.3(2) . . ? C15 N5 N6 106.3(2) . . ? C15 N5 Rh1 137.25(19) . . ? N6 N5 Rh1 116.42(15) . . ? C17 N6 N5 109.6(2) . . ? C17 N6 B1 127.7(2) . . ? N5 N6 B1 122.7(2) . . ? C10 N3 N4 107.1(2) . . ? C10 N3 Rh1 135.08(18) . . ? N4 N3 Rh1 117.70(16) . . ? C12 N4 N3 109.6(2) . . ? C12 N4 B1 130.3(2) . . ? N3 N4 B1 117.8(2) . . ? C20 N1 N2 107.0(2) . . ? C20 N1 Rh1 134.18(17) . . ? N2 N1 Rh1 118.72(16) . . ? N1 N2 C22 110.2(2) . . ? N1 N2 B1 118.0(2) . . ? C22 N2 B1 129.9(2) . . ? N5 C15 C16 110.2(2) . . ? N5 C15 C14 122.4(2) . . ? C16 C15 C14 127.4(2) . . ? C17 C16 C15 106.4(2) . . ? N6 C17 C16 107.5(2) . . ? N6 C17 C18 124.5(2) . . ? C16 C17 C18 127.9(3) . . ? N3 C10 C11 109.3(2) . . ? N3 C10 C9 122.2(2) . . ? C11 C10 C9 128.4(3) . . ? C12 C11 C10 106.5(2) . . ? N4 C12 C11 107.5(2) . . ? N4 C12 C13 123.0(3) . . ? C11 C12 C13 129.5(3) . . ? N1 C20 C21 109.3(2) . . ? N1 C20 C19 121.9(2) . . ? C21 C20 C19 128.6(3) . . ? C22 C21 C20 106.6(2) . . ? N2 C22 C21 106.9(2) . . ? N2 C22 C23 123.1(3) . . ? C21 C22 C23 130.0(3) . . ? C2 C1 C6 106.4(2) . . ? C2 C1 Rh1 71.25(16) . . ? C6 C1 Rh1 96.77(17) . . ? C1 C2 C5 106.7(2) . . ? C1 C2 Rh1 71.19(15) . . ? C5 C2 Rh1 96.89(16) . . ? C2 C5 C7 101.6(2) . . ? C2 C5 C4 97.6(2) . . ? C7 C5 C4 102.4(2) . . ? C3 C4 C5 105.1(2) . . ? C3 C4 Rh1 69.75(15) . . ? C5 C4 Rh1 99.16(16) . . ? C4 C3 C6 105.6(2) . . ? C4 C3 Rh1 69.74(15) . . ? C6 C3 Rh1 99.61(16) . . ? C1 C6 C3 97.3(2) . . ? C1 C6 C7 101.4(2) . . ? C3 C6 C7 102.6(2) . . ? C6 C7 C5 94.1(2) . . ? N99 C99 C98 178.0(6) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.456 _refine_diff_density_min -0.524 _refine_diff_density_rms 0.086 #===END data_6 _database_code_depnum_ccdc_archive 'CCDC 670939' _audit_creation_method shelxl-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H37 B Ir N7' _chemical_formula_weight 638.65 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' b b 0.0013 0.0007 'international tables vol c tables 4.2.6.8 and 6.1.1.4' ir ir -1.4442 7.9887 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_h-m P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.6937(10) _cell_length_b 14.3403(16) _cell_length_c 11.0382(13) _cell_angle_alpha 90.00 _cell_angle_beta 111.294(2) _cell_angle_gamma 90.00 _cell_volume 1282.2(3) _cell_formula_units_z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 72 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plate _exptl_crystal_colour Orange-yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.654 _exptl_crystal_density_method 'not measured' _exptl_crystal_f_000 636 _exptl_absorpt_coefficient_mu 5.234 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_t_min 0.88 _exptl_absorpt_correction_t_max 1.00 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'omega scans with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 8437 _diffrn_reflns_av_r_equivalents 0.0337 _diffrn_reflns_av_sigmai/neti 0.0819 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5286 _reflns_number_gt 4324 _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^)+(0.0241P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.042(10) _refine_ls_number_reflns 5286 _refine_ls_number_parameters 309 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0445 _refine_ls_R_factor_gt 0.0317 _refine_ls_wR_factor_ref 0.0631 _refine_ls_wR_factor_gt 0.0614 _refine_ls_goodness_of_fit_ref 0.893 _refine_ls_restrained_S_all 0.893 _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 Ir1 Ir -0.91237(3) 0.09602(2) -0.52849(2) 0.02044(7) Uani 1 1 d . . . N2 N -1.1404(7) -0.0096(4) -0.7554(6) 0.0192(13) Uani 1 1 d . . . N1 N -1.1351(7) 0.0279(4) -0.6383(5) 0.0172(13) Uani 1 1 d . . . N4 N -0.8466(6) -0.0632(4) -0.6809(6) 0.0186(13) Uani 1 1 d . . . N3 N -0.7984(7) -0.0280(4) -0.5552(6) 0.0193(14) Uani 1 1 d . . . N6 N -0.9276(6) 0.0781(4) -0.8234(6) 0.0185(17) Uani 1 1 d . . . N5 N -0.7641(6) 0.0826(6) -0.8137(6) 0.022(2) Uani 1 1 d . . . C23 C -1.3477(9) -0.0846(5) -0.9527(7) 0.0324(19) Uani 1 1 d . . . H23A H -1.2546 -0.0869 -0.9799 0.049 Uiso 1 1 calc R . . H23B H -1.4340 -0.0481 -1.0135 0.049 Uiso 1 1 calc R . . H23C H -1.3872 -0.1468 -0.9496 0.049 Uiso 1 1 calc R . . C22 C -1.2972(8) -0.0416(5) -0.8215(7) 0.0247(17) Uani 1 1 d . . . C21 C -1.3876(9) -0.0241(5) -0.7444(7) 0.0251(17) Uani 1 1 d . . . H21A H -1.4983 -0.0384 -0.7638 0.030 Uiso 1 1 calc R . . C20 C -1.2843(8) 0.0184(4) -0.6339(7) 0.0191(15) Uani 1 1 d . . . C19 C -1.3292(8) 0.0488(5) -0.5208(7) 0.0257(17) Uani 1 1 d . . . H19A H -1.2347 0.0766 -0.4556 0.039 Uiso 1 1 calc R . . H19B H -1.3646 -0.0042 -0.4847 0.039 Uiso 1 1 calc R . . H19C H -1.4171 0.0937 -0.5498 0.039 Uiso 1 1 calc R . . C18 C -0.7698(9) -0.1978(5) -0.7932(8) 0.037(2) Uani 1 1 d . . . H18A H -0.8487 -0.1696 -0.8693 0.056 Uiso 1 1 calc R . . H18B H -0.8049 -0.2599 -0.7835 0.056 Uiso 1 1 calc R . . H18C H -0.6639 -0.2002 -0.8020 0.056 Uiso 1 1 calc R . . C17 C -0.7570(8) -0.1413(5) -0.6761(8) 0.0233(17) Uani 1 1 d . . . C16 C -0.6585(8) -0.1571(5) -0.5487(8) 0.0276(18) Uani 1 1 d . . . H16A H -0.5839 -0.2058 -0.5173 0.033 Uiso 1 1 calc R . . C15 C -0.6916(9) -0.0864(5) -0.4758(8) 0.0272(19) Uani 1 1 d . . . C14 C -0.6273(9) -0.0755(5) -0.3316(8) 0.035(2) Uani 1 1 d . . . H14A H -0.6710 -0.0194 -0.3091 0.053 Uiso 1 1 calc R . . H14B H -0.5090 -0.0720 -0.2997 0.053 Uiso 1 1 calc R . . H14C H -0.6606 -0.1281 -0.2931 0.053 Uiso 1 1 calc R . . C13 C -1.1881(8) 0.1733(5) -0.9010(8) 0.032(2) Uani 1 1 d . . . H13A H -1.2324 0.1196 -0.8732 0.049 Uiso 1 1 calc R . . H13B H -1.2436 0.1819 -0.9929 0.049 Uiso 1 1 calc R . . H13C H -1.2040 0.2275 -0.8558 0.049 Uiso 1 1 calc R . . C12 C -1.0054(9) 0.1592(5) -0.8710(8) 0.0229(17) Uani 1 1 d . . . C11 C -0.8947(9) 0.2176(5) -0.8941(7) 0.0294(19) Uani 1 1 d . . . H11A H -0.9138 0.2776 -0.9282 0.035 Uiso 1 1 calc R . . C10 C -0.7461(9) 0.1674(5) -0.8552(8) 0.0265(18) Uani 1 1 d . . . C9 C -0.5826(9) 0.1965(6) -0.8552(9) 0.047(3) Uani 1 1 d . . . H9A H -0.5050 0.1465 -0.8226 0.071 Uiso 1 1 calc R . . H9B H -0.5452 0.2504 -0.8008 0.071 Uiso 1 1 calc R . . H9C H -0.5916 0.2114 -0.9424 0.071 Uiso 1 1 calc R . . C2 C -0.9928(9) 0.1905(5) -0.4151(8) 0.0315(19) Uani 1 1 d . . . H2A H -1.0822 0.1665 -0.3897 0.038 Uiso 1 1 calc R . . C1 C -1.0449(9) 0.2230(5) -0.5450(8) 0.0297(19) Uani 1 1 d . . . H1A H -1.1639 0.2164 -0.5924 0.036 Uiso 1 1 calc R . . C6 C -0.9700(9) 0.3039(5) -0.5915(9) 0.037(2) Uani 1 1 d . . . H6A H -0.9975 0.3617 -0.5584 0.044 Uiso 1 1 calc R . . H6B H -1.0159 0.3065 -0.6857 0.044 Uiso 1 1 calc R . . C5 C -0.7802(10) 0.2941(6) -0.5451(9) 0.034(2) Uani 1 1 d . . . H5B H -0.7298 0.3286 -0.4648 0.041 Uiso 1 1 calc R . . H5C H -0.7420 0.3210 -0.6098 0.041 Uiso 1 1 calc R . . C3 C -0.7238(9) 0.1890(6) -0.5220(8) 0.027(2) Uani 1 1 d . . . H3A H -0.6597 0.1688 -0.5742 0.032 Uiso 1 1 calc R . . C4 C -0.6767(8) 0.1465(5) -0.4030(7) 0.0235(17) Uani 1 1 d . . . H4A H -0.5864 0.1016 -0.3863 0.028 Uiso 1 1 calc R . . C7 C -0.6882(9) 0.1912(6) -0.2805(8) 0.038(2) Uani 1 1 d . . . H7A H -0.6695 0.1438 -0.2140 0.046 Uiso 1 1 calc R . . H7B H -0.6021 0.2378 -0.2478 0.046 Uiso 1 1 calc R . . C8 C -0.8542(10) 0.2366(6) -0.3058(8) 0.040(2) Uani 1 1 d . . . H8A H -0.8791 0.2340 -0.2270 0.048 Uiso 1 1 calc R . . H8B H -0.8480 0.3018 -0.3271 0.048 Uiso 1 1 calc R . . B1 B -0.9844(9) -0.0184(5) -0.7937(8) 0.0164(17) Uani 1 1 d . . . H1 H -1.0111 -0.0590 -0.8723 0.03(2) Uiso 1 1 d R . . N7 N -1.2318(13) 0.0410(7) -1.1839(9) 0.080(3) Uani 1 1 d . . . C24 C -1.0928(16) 0.0235(8) -1.1586(10) 0.061(3) Uani 1 1 d . . . C25 C -0.9185(13) 0.0053(7) -1.1302(11) 0.070(3) Uani 1 1 d . . . H25A H -0.8869 0.0312 -1.1980 0.106 Uiso 1 1 calc R . . H25B H -0.8996 -0.0608 -1.1254 0.106 Uiso 1 1 calc R . . H25C H -0.8541 0.0335 -1.0487 0.106 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 Ir1 0.01761(10) 0.01676(10) 0.02867(13) -0.0047(3) 0.01044(8) -0.0009(3) N2 0.020(3) 0.020(3) 0.019(4) -0.006(3) 0.010(3) -0.003(3) N1 0.024(3) 0.016(3) 0.014(3) 0.001(2) 0.009(2) 0.007(2) N4 0.020(3) 0.014(3) 0.024(4) -0.001(2) 0.011(3) 0.000(2) N3 0.016(3) 0.015(4) 0.029(4) -0.002(3) 0.011(3) 0.003(3) N6 0.017(2) 0.011(5) 0.030(3) 0.005(2) 0.012(2) 0.003(2) N5 0.019(2) 0.020(6) 0.033(3) 0.003(3) 0.015(2) -0.002(3) C23 0.027(4) 0.031(4) 0.038(5) -0.008(4) 0.010(4) -0.011(3) C22 0.022(4) 0.020(4) 0.033(5) 0.005(3) 0.010(3) 0.002(3) C21 0.020(4) 0.022(4) 0.035(5) 0.004(3) 0.012(3) -0.006(3) C20 0.021(3) 0.017(4) 0.019(4) 0.006(3) 0.006(3) -0.001(3) C19 0.018(3) 0.033(4) 0.028(5) -0.004(3) 0.012(3) 0.001(3) C18 0.028(4) 0.030(4) 0.055(6) -0.011(4) 0.019(4) 0.004(4) C17 0.020(4) 0.014(3) 0.042(5) -0.003(3) 0.018(3) -0.002(3) C16 0.018(4) 0.012(3) 0.054(6) 0.000(3) 0.015(4) 0.001(3) C15 0.018(4) 0.023(4) 0.042(6) 0.001(4) 0.013(4) -0.005(3) C14 0.031(4) 0.030(4) 0.037(5) 0.004(4) 0.005(4) 0.000(4) C13 0.024(4) 0.024(4) 0.052(6) 0.013(4) 0.018(4) 0.008(3) C12 0.022(4) 0.018(4) 0.035(5) 0.006(3) 0.017(4) 0.007(3) C11 0.036(4) 0.013(4) 0.038(5) 0.007(3) 0.012(4) -0.002(3) C10 0.029(4) 0.021(4) 0.038(5) 0.007(4) 0.023(4) 0.001(3) C9 0.027(4) 0.038(5) 0.076(7) 0.018(5) 0.017(4) -0.005(4) C2 0.033(4) 0.029(4) 0.043(6) -0.018(4) 0.026(4) -0.003(4) C1 0.022(4) 0.025(4) 0.046(6) -0.018(4) 0.018(4) 0.002(3) C6 0.033(4) 0.016(4) 0.065(6) -0.009(4) 0.022(4) -0.001(3) C5 0.034(5) 0.023(5) 0.051(7) -0.004(4) 0.020(4) 0.002(4) C3 0.012(4) 0.024(4) 0.045(6) -0.011(4) 0.010(4) 0.000(3) C4 0.019(3) 0.034(4) 0.015(4) -0.010(3) 0.004(3) -0.009(3) C7 0.023(4) 0.050(5) 0.041(6) -0.017(4) 0.011(4) -0.006(4) C8 0.045(5) 0.037(5) 0.048(6) -0.019(4) 0.027(4) -0.007(4) B1 0.016(4) 0.018(4) 0.017(5) -0.005(3) 0.009(3) -0.001(3) N7 0.090(7) 0.089(7) 0.053(7) -0.002(5) 0.018(6) -0.021(6) C24 0.079(8) 0.069(7) 0.037(7) -0.011(5) 0.023(6) -0.033(7) C25 0.089(9) 0.059(7) 0.079(9) -0.014(6) 0.049(7) -0.012(7) _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 Ir1 C3 2.094(7) . ? Ir1 N3 2.108(6) . ? Ir1 N1 2.114(6) . ? Ir1 C1 2.127(7) . ? Ir1 C2 2.128(7) . ? Ir1 C4 2.140(6) . ? N2 C22 1.370(8) . ? N2 N1 1.386(8) . ? N2 B1 1.565(9) . ? N1 C20 1.323(8) . ? N4 C17 1.355(8) . ? N4 N3 1.390(8) . ? N4 B1 1.521(9) . ? N3 C15 1.320(9) . ? N6 C12 1.352(8) . ? N6 N5 1.388(7) . ? N6 B1 1.543(9) . ? N5 C10 1.329(11) . ? C23 C22 1.487(10) . ? C22 C21 1.375(10) . ? C21 C20 1.367(9) . ? C20 C19 1.502(9) . ? C18 C17 1.495(10) . ? C17 C16 1.374(10) . ? C16 C15 1.387(10) . ? C15 C14 1.491(11) . ? C13 C12 1.514(9) . ? C12 C11 1.368(9) . ? C11 C10 1.403(10) . ? C10 C9 1.482(10) . ? C2 C1 1.417(11) . ? C2 C8 1.513(10) . ? C1 C6 1.509(10) . ? C6 C5 1.546(11) . ? C5 C3 1.577(11) . ? C3 C4 1.369(11) . ? C4 C7 1.532(10) . ? C7 C8 1.514(10) . ? N7 C24 1.164(13) . ? C24 C25 1.456(15) . ? 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 C3 Ir1 N3 98.0(3) . . ? C3 Ir1 N1 148.9(3) . . ? N3 Ir1 N1 84.8(2) . . ? C3 Ir1 C1 81.4(3) . . ? N3 Ir1 C1 167.9(3) . . ? N1 Ir1 C1 89.5(2) . . ? C3 Ir1 C2 89.7(3) . . ? N3 Ir1 C2 153.0(3) . . ? N1 Ir1 C2 101.7(2) . . ? C1 Ir1 C2 38.9(3) . . ? C3 Ir1 C4 37.7(3) . . ? N3 Ir1 C4 89.3(3) . . ? N1 Ir1 C4 171.8(3) . . ? C1 Ir1 C4 97.3(3) . . ? C2 Ir1 C4 81.1(3) . . ? C22 N2 N1 108.5(6) . . ? C22 N2 B1 128.4(6) . . ? N1 N2 B1 123.0(5) . . ? C20 N1 N2 107.0(5) . . ? C20 N1 Ir1 137.2(5) . . ? N2 N1 Ir1 115.3(4) . . ? C17 N4 N3 107.5(5) . . ? C17 N4 B1 130.7(6) . . ? N3 N4 B1 121.7(5) . . ? C15 N3 N4 108.5(6) . . ? C15 N3 Ir1 134.1(6) . . ? N4 N3 Ir1 117.3(4) . . ? C12 N6 N5 110.1(6) . . ? C12 N6 B1 134.4(5) . . ? N5 N6 B1 115.0(6) . . ? C10 N5 N6 105.1(7) . . ? N2 C22 C21 106.9(7) . . ? N2 C22 C23 122.9(6) . . ? C21 C22 C23 130.2(7) . . ? C20 C21 C22 107.2(6) . . ? N1 C20 C21 110.4(6) . . ? N1 C20 C19 123.7(6) . . ? C21 C20 C19 125.9(6) . . ? N4 C17 C16 108.2(6) . . ? N4 C17 C18 123.6(7) . . ? C16 C17 C18 128.2(6) . . ? C17 C16 C15 106.9(7) . . ? N3 C15 C16 108.8(8) . . ? N3 C15 C14 122.9(7) . . ? C16 C15 C14 128.3(7) . . ? N6 C12 C11 108.2(6) . . ? N6 C12 C13 122.5(6) . . ? C11 C12 C13 129.1(7) . . ? C12 C11 C10 105.1(6) . . ? N5 C10 C11 111.4(6) . . ? N5 C10 C9 119.4(7) . . ? C11 C10 C9 129.2(7) . . ? C1 C2 C8 122.2(7) . . ? C1 C2 Ir1 70.6(4) . . ? C8 C2 Ir1 114.3(5) . . ? C2 C1 C6 125.4(7) . . ? C2 C1 Ir1 70.6(4) . . ? C6 C1 Ir1 113.6(5) . . ? C1 C6 C5 111.0(6) . . ? C6 C5 C3 111.9(6) . . ? C4 C3 C5 123.2(7) . . ? C4 C3 Ir1 73.0(4) . . ? C5 C3 Ir1 114.2(5) . . ? C3 C4 C7 124.6(7) . . ? C3 C4 Ir1 69.3(4) . . ? C7 C4 Ir1 111.0(5) . . ? C8 C7 C4 112.4(7) . . ? C2 C8 C7 112.9(6) . . ? N4 B1 N6 109.5(5) . . ? N4 B1 N2 108.3(6) . . ? N6 B1 N2 111.2(6) . . ? N7 C24 C25 177.4(13) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.091 _refine_diff_density_min -1.076 _refine_diff_density_rms 0.125 #===END data_8 _database_code_depnum_ccdc_archive 'CCDC 670940' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H23.50 B N6.50 Rh' _chemical_formula_weight 444.65 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Cmc2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x, -y, z+1/2' '-x, y, z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z' _cell_length_a 10.8148(16) _cell_length_b 10.1274(14) _cell_length_c 33.316(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3649.0(9) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 77 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.619 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1816 _exptl_absorpt_coefficient_mu 0.953 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.778369 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'Siemens CCD area detector' _diffrn_measurement_method '\w scans with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 9597 _diffrn_reflns_av_R_equivalents 0.0530 _diffrn_reflns_av_sigmaI/netI 0.0507 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3272 _reflns_number_gt 2900 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0377P)^2^+3.9788P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(5) _refine_ls_number_reflns 3272 _refine_ls_number_parameters 272 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.0451 _refine_ls_R_factor_gt 0.0356 _refine_ls_wR_factor_ref 0.0774 _refine_ls_wR_factor_gt 0.0739 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.0000 0.60111(6) 0.418101(16) 0.01764(16) Uani 1 2 d S . . B1 B 0.0000 0.3531(9) 0.3544(3) 0.019(2) Uani 1 2 d S . . N5 N 0.0000 0.3961(7) 0.43007(18) 0.0210(16) Uani 1 2 d S . . N6 N 0.0000 0.3068(6) 0.3989(2) 0.0161(16) Uani 1 2 d S . . N1 N 0.1362(4) 0.5458(5) 0.36986(14) 0.0202(11) Uani 1 1 d . . . N2 N 0.1153(4) 0.4361(4) 0.34712(13) 0.0182(10) Uani 1 1 d . . . C10 C 0.0000 0.1842(10) 0.4143(4) 0.032(2) Uani 1 2 d S . . H1A H 0.0000 0.1052 0.3989 0.038 Uiso 1 2 calc SR . . C9 C 0.0000 0.1900(11) 0.4555(3) 0.040(3) Uani 1 2 d S . . H2A H 0.0000 0.1188 0.4740 0.048 Uiso 1 2 calc SR . . C8 C 0.0000 0.3273(9) 0.4637(3) 0.032(3) Uani 1 2 d S . . H3A H 0.0000 0.3647 0.4898 0.038 Uiso 1 2 calc SR . . C7 C 0.2084(6) 0.4190(6) 0.32050(18) 0.0234(14) Uani 1 1 d . . . H4A H 0.2148 0.3497 0.3014 0.028 Uiso 1 1 calc R . . C6 C 0.2924(6) 0.5200(6) 0.32601(19) 0.0288(15) Uani 1 1 d . . . H5A H 0.3669 0.5353 0.3116 0.035 Uiso 1 1 calc R . . C5 C 0.2432(6) 0.5948(6) 0.35747(19) 0.0236(16) Uani 1 1 d . . . H6A H 0.2816 0.6709 0.3685 0.028 Uiso 1 1 calc R . . C1 C 0.0634(5) 0.8004(5) 0.41030(18) 0.0254(15) Uani 1 1 d . . . H7 H 0.0997 0.8168 0.3831 0.031 Uiso 1 1 calc R . . C3 C 0.1453(6) 0.8459(6) 0.4438(2) 0.0357(16) Uani 1 1 d . . . H8A H 0.2311 0.8520 0.4336 0.043 Uiso 1 1 calc R . . H8B H 0.1194 0.9358 0.4518 0.043 Uiso 1 1 calc R . . C2 C 0.1452(11) 0.7614(10) 0.4796(3) 0.090(4) Uani 1 1 d . . . H9A H 0.1151 0.8134 0.5028 0.108 Uiso 1 1 calc R . . H9B H 0.2312 0.7338 0.4855 0.108 Uiso 1 1 calc R . . C4 C 0.0659(6) 0.6403(7) 0.47503(18) 0.0297(14) Uani 1 1 d . . . H10 H 0.1019 0.5607 0.4884 0.036 Uiso 1 1 calc R . . Rh11 Rh 0.0000 0.76338(5) 0.121394(17) 0.01749(16) Uani 1 2 d S . . B11 B 0.0000 0.5115(9) 0.1837(3) 0.019(2) Uani 1 2 d S . . N15 N 0.0000 0.5606(7) 0.10919(19) 0.0222(16) Uani 1 2 d SU . . N16 N 0.0000 0.4714(7) 0.1392(2) 0.0185(18) Uani 1 2 d SU . . N11 N 0.1352(4) 0.7071(5) 0.16957(14) 0.0205(10) Uani 1 1 d . . . N12 N 0.1148(4) 0.5955(5) 0.19163(13) 0.0213(10) Uani 1 1 d . . . C20 C 0.0000 0.3466(8) 0.1238(3) 0.0262(19) Uani 1 2 d S . . H11A H 0.0000 0.2660 0.1384 0.031 Uiso 1 2 calc SR . . C19 C 0.0000 0.3614(10) 0.0828(3) 0.041(3) Uani 1 2 d S . . H12A H 0.0000 0.2920 0.0636 0.049 Uiso 1 2 calc SR . . C18 C 0.0000 0.4904(11) 0.0747(3) 0.033(3) Uani 1 2 d SU . . H13A H 0.0000 0.5275 0.0485 0.040 Uiso 1 2 calc SR . . C17 C 0.2117(6) 0.5740(6) 0.21629(17) 0.0244(15) Uani 1 1 d . . . H14A H 0.2205 0.5015 0.2342 0.029 Uiso 1 1 calc R . . C16 C 0.2953(6) 0.6741(7) 0.2113(2) 0.0318(16) Uani 1 1 d . . . H15A H 0.3716 0.6860 0.2249 0.038 Uiso 1 1 calc R . . C15 C 0.2444(6) 0.7541(6) 0.1820(2) 0.0281(17) Uani 1 1 d . . . H16A H 0.2820 0.8322 0.1720 0.034 Uiso 1 1 calc R . . C11 C 0.0649(6) 0.9632(5) 0.13094(17) 0.0273(15) Uani 1 1 d . . . H17 H 0.1021 0.9780 0.1580 0.033 Uiso 1 1 calc R . . C13 C 0.1460(7) 1.0094(6) 0.0966(2) 0.0369(17) Uani 1 1 d . . . H18A H 0.1201 1.0997 0.0889 0.044 Uiso 1 1 calc R . . H18B H 0.2323 1.0147 0.1063 0.044 Uiso 1 1 calc R . . C12 C 0.1435(10) 0.9278(9) 0.0613(2) 0.079(4) Uani 1 1 d . . . H19A H 0.2295 0.9021 0.0547 0.094 Uiso 1 1 calc R . . H19B H 0.1119 0.9813 0.0387 0.094 Uiso 1 1 calc R . . C14 C 0.0657(6) 0.8029(6) 0.06440(18) 0.0290(15) Uani 1 1 d . . . H20 H 0.1031 0.7246 0.0507 0.035 Uiso 1 1 calc R . . N99 N 0.5000 0.4252(10) 0.2479(3) 0.049(2) Uani 1 2 d S . . C98 C 0.5000 0.2075(10) 0.2894(3) 0.033(2) Uani 1 2 d S . . H98A H 0.4726 0.2304 0.3165 0.050 Uiso 0.50 1 calc PR . . H98B H 0.5838 0.1708 0.2905 0.050 Uiso 0.50 1 calc PR . . H98C H 0.4436 0.1418 0.2779 0.050 Uiso 0.50 1 calc PR . . C99 C 0.5000 0.3259(12) 0.2643(3) 0.034(2) Uani 1 2 d S . . H1 H 0.0000 0.263(7) 0.334(2) 0.011(19) Uiso 1 2 d S . . H11 H 0.0000 0.421(13) 0.205(4) 0.10(5) Uiso 1 2 d S . . 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 0.0227(3) 0.0132(4) 0.0170(3) 0.0007(3) 0.000 0.000 B1 0.019(5) 0.020(5) 0.018(5) -0.001(4) 0.000 0.000 N5 0.029(4) 0.015(4) 0.019(4) -0.001(3) 0.000 0.000 N6 0.011(3) 0.016(4) 0.021(4) -0.002(3) 0.000 0.000 N1 0.019(3) 0.022(3) 0.020(3) 0.005(2) 0.003(2) -0.002(2) N2 0.020(3) 0.015(2) 0.020(3) -0.002(2) 0.000(2) 0.001(2) C10 0.030(5) 0.029(5) 0.036(6) 0.011(5) 0.000 0.000 C9 0.074(8) 0.022(6) 0.025(6) 0.001(4) 0.000 0.000 C8 0.078(8) 0.010(4) 0.008(4) 0.002(3) 0.000 0.000 C7 0.022(3) 0.023(3) 0.026(3) 0.000(3) 0.005(3) 0.001(3) C6 0.027(3) 0.028(4) 0.032(4) 0.005(3) 0.005(3) -0.001(3) C5 0.019(3) 0.024(4) 0.028(4) 0.001(2) 0.002(3) -0.005(2) C1 0.035(3) 0.008(3) 0.033(4) 0.004(2) 0.013(3) 0.001(2) C3 0.027(4) 0.028(4) 0.051(5) 0.006(3) -0.003(3) -0.002(3) C2 0.156(11) 0.079(7) 0.036(5) 0.010(5) -0.023(6) -0.090(8) C4 0.043(4) 0.027(4) 0.020(4) 0.001(3) -0.003(3) -0.004(3) Rh11 0.0225(3) 0.0125(4) 0.0174(3) 0.0005(3) 0.000 0.000 B11 0.021(5) 0.015(5) 0.020(5) 0.002(4) 0.000 0.000 N15 0.0225(18) 0.0221(18) 0.0219(18) -0.0003(10) 0.000 0.000 N16 0.0193(19) 0.018(2) 0.0181(19) -0.0013(10) 0.000 0.000 N11 0.025(3) 0.016(3) 0.020(3) 0.003(2) 0.004(2) -0.003(2) N12 0.023(3) 0.022(3) 0.019(2) -0.001(2) 0.001(2) 0.004(2) C20 0.038(5) 0.005(4) 0.036(5) 0.011(5) 0.000 0.000 C19 0.089(9) 0.018(5) 0.015(5) -0.012(4) 0.000 0.000 C18 0.034(3) 0.033(3) 0.033(3) -0.0007(10) 0.000 0.000 C17 0.032(3) 0.028(4) 0.013(3) 0.000(2) -0.005(3) 0.010(3) C16 0.030(4) 0.036(4) 0.030(4) -0.001(3) -0.015(3) -0.004(3) C15 0.029(4) 0.027(4) 0.028(4) -0.001(3) -0.001(3) -0.006(3) C11 0.041(3) 0.014(3) 0.026(4) 0.000(2) -0.004(3) -0.001(3) C13 0.031(4) 0.022(3) 0.058(5) -0.008(3) 0.000(3) -0.007(3) C12 0.130(9) 0.077(6) 0.028(5) -0.007(4) 0.017(5) -0.078(7) C14 0.045(4) 0.025(3) 0.018(3) -0.003(3) 0.005(3) -0.015(3) N99 0.053(6) 0.055(6) 0.038(6) 0.007(5) 0.000 0.000 C98 0.037(6) 0.030(5) 0.032(6) -0.002(5) 0.000 0.000 C99 0.025(5) 0.052(6) 0.025(5) -0.009(5) 0.000 0.000 _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 C4 2.064(6) . ? Rh1 C4 2.065(6) 4 ? Rh1 N5 2.114(7) . ? Rh1 C1 2.147(5) . ? Rh1 C1 2.147(5) 4 ? Rh1 N1 2.251(5) . ? Rh1 N1 2.251(5) 4 ? B1 N2 1.523(7) . ? B1 N2 1.523(7) 4 ? B1 N6 1.554(12) . ? N5 C8 1.319(11) . ? N5 N6 1.378(9) . ? N6 C10 1.342(12) . ? N1 C5 1.325(7) . ? N1 N2 1.364(6) . ? N2 C7 1.353(7) . ? C10 C9 1.373(15) . ? C9 C8 1.417(13) . ? C7 C6 1.381(9) . ? C6 C5 1.398(8) . ? C1 C1 1.372(12) 4 ? C1 C3 1.498(9) . ? C3 C2 1.467(10) . ? C2 C4 1.505(10) . ? C4 C4 1.425(14) 4 ? Rh11 C14 2.066(6) 4 ? Rh11 C14 2.066(6) . ? Rh11 N15 2.093(7) . ? Rh11 C11 2.165(6) 4 ? Rh11 C11 2.165(6) . ? Rh11 N11 2.245(5) . ? Rh11 N11 2.245(5) 4 ? B11 N12 1.528(7) . ? B11 N12 1.528(7) 4 ? B11 N16 1.534(12) . ? N15 N16 1.349(9) . ? N15 C18 1.350(12) . ? N16 C20 1.365(11) . ? N11 C15 1.339(8) . ? N11 N12 1.366(6) . ? N12 C17 1.350(7) . ? C20 C19 1.374(14) . ? C19 C18 1.334(14) . ? C17 C16 1.368(9) . ? C16 C15 1.382(9) . ? C11 C11 1.403(13) 4 ? C11 C13 1.517(9) . ? C13 C12 1.435(10) . ? C12 C14 1.523(9) . ? C14 C14 1.421(13) 4 ? N99 C99 1.144(13) . ? C98 C99 1.462(15) . ? 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 C4 Rh1 C4 40.4(4) . 4 ? C4 Rh1 N5 90.9(2) . . ? C4 Rh1 N5 90.9(2) 4 . ? C4 Rh1 C1 79.6(2) . . ? C4 Rh1 C1 92.3(2) 4 . ? N5 Rh1 C1 161.04(16) . . ? C4 Rh1 C1 92.3(2) . 4 ? C4 Rh1 C1 79.6(2) 4 4 ? N5 Rh1 C1 161.05(16) . 4 ? C1 Rh1 C1 37.3(3) . 4 ? C4 Rh1 N1 118.6(2) . . ? C4 Rh1 N1 158.4(2) 4 . ? N5 Rh1 N1 83.71(17) . . ? C1 Rh1 N1 86.46(19) . . ? C1 Rh1 N1 110.9(2) 4 . ? C4 Rh1 N1 158.4(2) . 4 ? C4 Rh1 N1 118.6(2) 4 4 ? N5 Rh1 N1 83.71(17) . 4 ? C1 Rh1 N1 110.9(2) . 4 ? C1 Rh1 N1 86.46(19) 4 4 ? N1 Rh1 N1 81.7(2) . 4 ? N2 B1 N2 109.9(7) . 4 ? N2 B1 N6 108.6(5) . . ? N2 B1 N6 108.6(5) 4 . ? C8 N5 N6 107.0(7) . . ? C8 N5 Rh1 132.8(6) . . ? N6 N5 Rh1 120.2(5) . . ? C10 N6 N5 108.7(7) . . ? C10 N6 B1 130.0(7) . . ? N5 N6 B1 121.3(6) . . ? C5 N1 N2 106.1(5) . . ? C5 N1 Rh1 134.5(4) . . ? N2 N1 Rh1 119.4(3) . . ? C7 N2 N1 110.2(5) . . ? C7 N2 B1 130.1(5) . . ? N1 N2 B1 119.7(5) . . ? N6 C10 C9 110.0(9) . . ? C10 C9 C8 103.6(9) . . ? N5 C8 C9 110.7(9) . . ? N2 C7 C6 107.9(5) . . ? C7 C6 C5 104.5(5) . . ? N1 C5 C6 111.3(5) . . ? C1 C1 C3 126.2(4) 4 . ? C1 C1 Rh1 71.37(15) 4 . ? C3 C1 Rh1 112.8(4) . . ? C2 C3 C1 115.2(6) . . ? C3 C2 C4 113.2(7) . . ? C4 C4 C2 124.8(6) 4 . ? C4 C4 Rh1 69.82(19) 4 . ? C2 C4 Rh1 116.5(5) . . ? C14 Rh11 C14 40.2(4) 4 . ? C14 Rh11 N15 90.7(2) 4 . ? C14 Rh11 N15 90.7(2) . . ? C14 Rh11 C11 80.9(2) 4 4 ? C14 Rh11 C11 93.7(2) . 4 ? N15 Rh11 C11 160.96(17) . 4 ? C14 Rh11 C11 93.7(2) 4 . ? C14 Rh11 C11 80.9(2) . . ? N15 Rh11 C11 160.97(17) . . ? C11 Rh11 C11 37.8(3) 4 . ? C14 Rh11 N11 158.5(2) 4 . ? C14 Rh11 N11 118.8(2) . . ? N15 Rh11 N11 83.66(18) . . ? C11 Rh11 N11 110.1(2) 4 . ? C11 Rh11 N11 85.5(2) . . ? C14 Rh11 N11 118.8(2) 4 4 ? C14 Rh11 N11 158.5(2) . 4 ? N15 Rh11 N11 83.66(18) . 4 ? C11 Rh11 N11 85.5(2) 4 4 ? C11 Rh11 N11 110.1(2) . 4 ? N11 Rh11 N11 81.3(2) . 4 ? N12 B11 N12 108.6(7) . 4 ? N12 B11 N16 108.4(5) . . ? N12 B11 N16 108.4(5) 4 . ? N16 N15 C18 106.2(8) . . ? N16 N15 Rh11 120.8(5) . . ? C18 N15 Rh11 133.0(7) . . ? N15 N16 C20 109.9(7) . . ? N15 N16 B11 122.6(6) . . ? C20 N16 B11 127.5(7) . . ? C15 N11 N12 105.7(5) . . ? C15 N11 Rh11 134.8(4) . . ? N12 N11 Rh11 119.3(3) . . ? C17 N12 N11 109.6(5) . . ? C17 N12 B11 130.3(6) . . ? N11 N12 B11 119.9(5) . . ? N16 C20 C19 105.9(8) . . ? C18 C19 C20 107.9(9) . . ? C19 C18 N15 110.1(10) . . ? N12 C17 C16 108.6(5) . . ? C17 C16 C15 104.9(6) . . ? N11 C15 C16 111.2(6) . . ? C11 C11 C13 125.3(4) 4 . ? C11 C11 Rh11 71.10(17) 4 . ? C13 C11 Rh11 111.4(4) . . ? C12 C13 C11 115.4(6) . . ? C13 C12 C14 115.6(6) . . ? C14 C14 C12 123.5(6) 4 . ? C14 C14 Rh11 69.89(19) 4 . ? C12 C14 Rh11 114.4(4) . . ? N99 C99 C98 173.5(13) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.488 _refine_diff_density_min -0.695 _refine_diff_density_rms 0.088 #===END data_13 _database_code_depnum_ccdc_archive 'CCDC 670941' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H24 B Ir N8' _chemical_formula_weight 579.48 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' B B 0.0013 0.0007 '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' Ir Ir -1.4442 7.9887 '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 8.419(4) _cell_length_b 25.113(14) _cell_length_c 9.675(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.27(3) _cell_angle_gamma 90.00 _cell_volume 2044.0(17) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7381 _cell_measurement_theta_min 2.421 _cell_measurement_theta_max 54.899 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.883 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 6.557 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.629 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method '0.3 \% frames in \w' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 17526 _diffrn_reflns_av_R_equivalents 0.0460 _diffrn_reflns_av_sigmaI/netI 0.0448 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 27.51 _reflns_number_total 4684 _reflns_number_gt 3832 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0001P)^2^+22.3631P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00077(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4684 _refine_ls_number_parameters 272 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0569 _refine_ls_R_factor_gt 0.0419 _refine_ls_wR_factor_ref 0.0859 _refine_ls_wR_factor_gt 0.0822 _refine_ls_goodness_of_fit_ref 1.134 _refine_ls_restrained_S_all 1.134 _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 Ir1 Ir 0.55876(3) 0.829521(10) 0.18555(3) 0.01667(9) Uani 1 1 d . . . C20 C 0.2642(8) 0.7574(3) 0.2291(7) 0.0211(14) Uani 1 1 d . . . H20A H 0.2938 0.7325 0.1609 0.025 Uiso 1 1 calc R . . C19 C 0.1281(9) 0.7543(3) 0.3035(8) 0.0250(16) Uani 1 1 d . . . H19A H 0.0477 0.7277 0.2971 0.030 Uiso 1 1 calc R . . C18 C 0.1347(8) 0.7981(3) 0.3890(7) 0.0221(15) Uani 1 1 d . . . H18A H 0.0568 0.8076 0.4530 0.027 Uiso 1 1 calc R . . C17 C 0.7360(9) 0.8917(3) 0.4240(8) 0.0253(16) Uani 1 1 d . . . H17A H 0.8385 0.8860 0.3888 0.030 Uiso 1 1 calc R . . C16 C 0.7060(9) 0.9177(3) 0.5475(8) 0.0272(17) Uani 1 1 d . . . H16A H 0.7818 0.9330 0.6111 0.033 Uiso 1 1 calc R . . C15 C 0.5452(9) 0.9167(3) 0.5578(7) 0.0252(16) Uani 1 1 d . . . H15A H 0.4880 0.9317 0.6310 0.030 Uiso 1 1 calc R . . C14 C 0.1456(10) 0.8987(3) 0.7421(8) 0.0314(18) Uani 1 1 d . . . H14A H 0.1289 0.8870 0.8338 0.038 Uiso 1 1 calc R . . C13 C 0.1068(9) 0.9495(3) 0.6928(9) 0.0335(19) Uani 1 1 d . . . H13A H 0.0626 0.9782 0.7423 0.040 Uiso 1 1 calc R . . C12 C 0.1467(9) 0.9486(3) 0.5576(8) 0.0263(16) Uani 1 1 d . . . H12A H 0.1341 0.9772 0.4939 0.032 Uiso 1 1 calc R . . C11 C 0.1096(10) 0.9445(3) 0.1094(8) 0.0289(17) Uani 1 1 d . . . H11A H 0.0224 0.9476 0.0446 0.035 Uiso 1 1 calc R . . C10 C 0.2497(10) 0.9730(3) 0.1019(8) 0.0330(18) Uani 1 1 d . . . H10A H 0.2761 0.9988 0.0349 0.040 Uiso 1 1 calc R . . C9 C 0.3418(9) 0.9556(3) 0.2127(8) 0.0260(16) Uani 1 1 d . . . H9A H 0.4469 0.9671 0.2367 0.031 Uiso 1 1 calc R . . C1 C 0.6841(9) 0.8849(3) 0.0677(8) 0.0230(15) Uani 1 1 d . . . H1A H 0.7022 0.9199 0.1151 0.028 Uiso 1 1 calc R . . C2 C 0.7898(9) 0.8446(3) 0.1141(8) 0.0258(16) Uani 1 1 d . . . H2A H 0.8679 0.8565 0.1883 0.031 Uiso 1 1 calc R . . C8 C 0.8539(9) 0.8026(3) 0.0188(8) 0.0316(18) Uani 1 1 d . . . H8A H 0.9648 0.7939 0.0483 0.038 Uiso 1 1 calc R . . H8B H 0.8544 0.8167 -0.0767 0.038 Uiso 1 1 calc R . . C7 C 0.7518(9) 0.7517(3) 0.0210(9) 0.0317(18) Uani 1 1 d . . . H7A H 0.7556 0.7338 -0.0700 0.038 Uiso 1 1 calc R . . H7B H 0.7977 0.7270 0.0917 0.038 Uiso 1 1 calc R . . C4 C 0.5807(9) 0.7626(3) 0.0521(7) 0.0240(15) Uani 1 1 d . . . H4A H 0.5199 0.7305 0.0806 0.029 Uiso 1 1 calc R . . C3 C 0.4868(9) 0.8023(3) -0.0143(7) 0.0214(15) Uani 1 1 d . . . H3A H 0.3714 0.7931 -0.0245 0.026 Uiso 1 1 calc R . . C6 C 0.5475(9) 0.8365(3) -0.1332(7) 0.0281(16) Uani 1 1 d . . . H6A H 0.4596 0.8433 -0.2020 0.034 Uiso 1 1 calc R . . H6B H 0.6327 0.8173 -0.1800 0.034 Uiso 1 1 calc R . . C5 C 0.6121(10) 0.8898(3) -0.0761(8) 0.0330(19) Uani 1 1 d . . . H5A H 0.6936 0.9034 -0.1382 0.040 Uiso 1 1 calc R . . H5B H 0.5244 0.9160 -0.0759 0.040 Uiso 1 1 calc R . . N4 N 0.2689(6) 0.8255(2) 0.3676(5) 0.0169(11) Uani 1 1 d . . . N3 N 0.3491(7) 0.8009(2) 0.2667(6) 0.0179(12) Uani 1 1 d . . . N2 N 0.4804(7) 0.8908(2) 0.4463(6) 0.0174(12) Uani 1 1 d . . . N1 N 0.5997(7) 0.8758(2) 0.3627(6) 0.0189(12) Uani 1 1 d . . . N8 N 0.2073(7) 0.9001(2) 0.5296(6) 0.0204(12) Uani 1 1 d . . . N7 N 0.2085(8) 0.8689(3) 0.6458(6) 0.0280(14) Uani 1 1 d . . . N6 N 0.2574(7) 0.9194(2) 0.2820(6) 0.0198(12) Uani 1 1 d . . . N5 N 0.1119(7) 0.9123(3) 0.2182(7) 0.0265(14) Uani 1 1 d . . . B1 B 0.3032(9) 0.8840(3) 0.4067(8) 0.0181(15) 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 Ir1 0.01789(13) 0.01590(13) 0.01618(13) -0.00172(12) 0.00016(8) -0.00126(12) C20 0.028(4) 0.017(3) 0.018(3) -0.001(3) 0.003(3) -0.003(3) C19 0.028(4) 0.021(4) 0.026(4) 0.002(3) 0.001(3) -0.009(3) C18 0.021(4) 0.023(4) 0.023(4) 0.004(3) 0.005(3) 0.000(3) C17 0.024(4) 0.023(4) 0.028(4) -0.001(3) 0.003(3) -0.006(3) C16 0.026(4) 0.034(4) 0.021(4) -0.004(3) -0.003(3) -0.012(3) C15 0.035(4) 0.024(4) 0.017(4) -0.001(3) 0.001(3) -0.006(3) C14 0.035(4) 0.037(5) 0.023(4) -0.002(3) 0.008(3) 0.001(4) C13 0.033(4) 0.034(4) 0.033(4) -0.012(4) 0.007(4) 0.007(3) C12 0.029(4) 0.020(4) 0.030(4) 0.000(3) 0.002(3) 0.009(3) C11 0.037(4) 0.024(4) 0.025(4) 0.006(3) -0.004(3) 0.006(3) C10 0.048(5) 0.023(4) 0.028(4) 0.010(3) 0.004(4) 0.004(4) C9 0.029(4) 0.015(3) 0.034(4) 0.004(3) 0.003(3) -0.002(3) C1 0.026(4) 0.020(3) 0.024(4) -0.009(3) 0.010(3) -0.012(3) C2 0.024(4) 0.031(4) 0.023(4) -0.004(3) 0.004(3) -0.002(3) C8 0.025(4) 0.042(5) 0.029(4) -0.002(4) 0.005(3) 0.006(3) C7 0.031(4) 0.033(4) 0.032(4) -0.007(3) 0.004(3) 0.010(3) C4 0.033(4) 0.018(3) 0.021(4) -0.006(3) 0.005(3) 0.000(3) C3 0.025(4) 0.023(4) 0.016(3) -0.003(3) 0.001(3) -0.006(3) C6 0.032(4) 0.036(5) 0.016(3) 0.001(3) -0.002(3) -0.001(3) C5 0.039(5) 0.031(4) 0.029(4) 0.007(3) 0.003(4) -0.005(4) N4 0.021(3) 0.021(3) 0.008(2) -0.002(2) -0.005(2) -0.003(2) N3 0.022(3) 0.016(3) 0.016(3) -0.001(2) -0.001(2) 0.000(2) N2 0.021(3) 0.018(3) 0.012(3) 0.001(2) 0.002(2) 0.001(2) N1 0.023(3) 0.019(3) 0.015(3) -0.002(2) -0.001(2) -0.004(2) N8 0.027(3) 0.016(3) 0.018(3) 0.003(2) 0.003(2) 0.000(2) N7 0.038(4) 0.025(3) 0.021(3) 0.005(3) 0.005(3) 0.002(3) N6 0.021(3) 0.017(3) 0.021(3) -0.001(2) -0.002(2) 0.000(2) N5 0.024(3) 0.027(3) 0.028(3) 0.006(3) -0.007(3) -0.002(3) B1 0.025(4) 0.014(3) 0.015(4) 0.003(3) 0.002(3) 0.001(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 Ir1 N3 2.088(6) . ? Ir1 N1 2.088(5) . ? Ir1 C1 2.108(7) . ? Ir1 C3 2.117(7) . ? Ir1 C2 2.124(7) . ? Ir1 C4 2.132(7) . ? C20 N3 1.346(9) . ? C20 C19 1.380(10) . ? C19 C18 1.377(10) . ? C18 N4 1.345(9) . ? C17 N1 1.332(9) . ? C17 C16 1.394(10) . ? C16 C15 1.361(11) . ? C15 N2 1.356(9) . ? C14 N7 1.323(10) . ? C14 C13 1.395(11) . ? C13 C12 1.364(11) . ? C12 N8 1.350(9) . ? C11 N5 1.326(9) . ? C11 C10 1.384(12) . ? C10 C9 1.369(11) . ? C9 N6 1.350(9) . ? C1 C2 1.408(11) . ? C1 C5 1.501(11) . ? C2 C8 1.516(10) . ? C8 C7 1.541(11) . ? C7 C4 1.508(10) . ? C4 C3 1.412(10) . ? C3 C6 1.539(10) . ? C6 C5 1.537(11) . ? N4 N3 1.358(7) . ? N4 B1 1.543(9) . ? N2 N1 1.368(8) . ? N2 B1 1.535(10) . ? N8 N7 1.372(8) . ? N8 B1 1.518(9) . ? N6 N5 1.361(8) . ? N6 B1 1.534(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 N3 Ir1 N1 89.9(2) . . ? N3 Ir1 C1 151.6(3) . . ? N1 Ir1 C1 90.4(2) . . ? N3 Ir1 C3 90.9(2) . . ? N1 Ir1 C3 164.0(3) . . ? C1 Ir1 C3 81.4(3) . . ? N3 Ir1 C2 169.3(3) . . ? N1 Ir1 C2 92.5(3) . . ? C1 Ir1 C2 38.9(3) . . ? C3 Ir1 C2 89.6(3) . . ? N3 Ir1 C4 92.9(3) . . ? N1 Ir1 C4 157.0(3) . . ? C1 Ir1 C4 97.8(3) . . ? C3 Ir1 C4 38.8(3) . . ? C2 Ir1 C4 80.9(3) . . ? N3 C20 C19 110.5(6) . . ? C18 C19 C20 104.6(6) . . ? N4 C18 C19 109.3(6) . . ? N1 C17 C16 109.9(7) . . ? C15 C16 C17 105.6(7) . . ? N2 C15 C16 108.7(6) . . ? N7 C14 C13 111.8(7) . . ? C12 C13 C14 104.5(7) . . ? N8 C12 C13 108.5(7) . . ? N5 C11 C10 111.8(7) . . ? C9 C10 C11 104.6(7) . . ? N6 C9 C10 108.1(7) . . ? C2 C1 C5 125.5(7) . . ? C2 C1 Ir1 71.2(4) . . ? C5 C1 Ir1 111.3(5) . . ? C1 C2 C8 122.8(7) . . ? C1 C2 Ir1 69.9(4) . . ? C8 C2 Ir1 115.2(5) . . ? C2 C8 C7 110.9(6) . . ? C4 C7 C8 112.9(6) . . ? C3 C4 C7 124.0(7) . . ? C3 C4 Ir1 70.0(4) . . ? C7 C4 Ir1 111.8(5) . . ? C4 C3 C6 122.6(7) . . ? C4 C3 Ir1 71.1(4) . . ? C6 C3 Ir1 114.3(5) . . ? C3 C6 C5 109.9(6) . . ? C1 C5 C6 112.7(6) . . ? C18 N4 N3 108.9(5) . . ? C18 N4 B1 126.8(6) . . ? N3 N4 B1 121.1(5) . . ? C20 N3 N4 106.8(5) . . ? C20 N3 Ir1 128.8(5) . . ? N4 N3 Ir1 124.4(4) . . ? C15 N2 N1 108.7(6) . . ? C15 N2 B1 127.5(6) . . ? N1 N2 B1 123.4(5) . . ? C17 N1 N2 107.1(6) . . ? C17 N1 Ir1 130.0(5) . . ? N2 N1 Ir1 122.5(4) . . ? C12 N8 N7 110.0(6) . . ? C12 N8 B1 127.9(6) . . ? N7 N8 B1 120.2(6) . . ? C14 N7 N8 105.2(6) . . ? C9 N6 N5 110.2(6) . . ? C9 N6 B1 131.3(6) . . ? N5 N6 B1 118.3(6) . . ? C11 N5 N6 105.4(6) . . ? N8 B1 N6 109.6(6) . . ? N8 B1 N2 108.4(6) . . ? N6 B1 N2 110.1(6) . . ? N8 B1 N4 110.3(5) . . ? N6 B1 N4 108.7(6) . . ? N2 B1 N4 109.8(5) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.730 _refine_diff_density_min -4.967 _refine_diff_density_rms 0.182