Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_coden_Cambridge 222 _publ_contact_author_name 'Barbara A. Messerle' _publ_contact_author_address ; School of Chemical Sciences, University of New South Wales, NSW 2052, Australia ; _publ_contact_author_email b.messerle@unsw.edu.au _publ_contact_author_fax +61-2-9385-6141 _publ_contact_author_phone +61-2-9385-4653 _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Rhodium(I) and Iridium(I) Complexes of Pyrazolyl-N-Heterocyclic Carbene Ligands ; loop_ _publ_author_name _publ_author_address 'Barbara A. Messerle' ; School of Chemical Sciences, University of New South Wales, NSW 2052, Australia ; 'Michael J. Page' ; School of Chemical Sciences, University of New South Wales, NSW 2052, Australia ; 'Peter Turner' ; School of Chemistry, University of Sydney, NSW 2006, Australia ; #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_bam21 _database_code_depnum_ccdc_archive 'CCDC 600823' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48.50 H53.25 B Ir N8 O0.38' _chemical_formula_weight 957.25 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c ' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 31.705(6) _cell_length_b 13.512(3) _cell_length_c 24.585(5) _cell_angle_alpha 90.00 _cell_angle_beta 117.508(3) _cell_angle_gamma 90.00 _cell_volume 9341(3) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 959 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 25.03 _exptl_crystal_description blade _exptl_crystal_colour orange _exptl_crystal_size_max 0.347 _exptl_crystal_size_mid 0.204 _exptl_crystal_size_min 0.049 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.361 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3882 _exptl_absorpt_coefficient_mu 2.900 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.552 _exptl_absorpt_correction_T_max 0.931 _exptl_absorpt_process_details ; Gaussian (Coppens et al., 1965) XPREP (Bruker, 1995) ; _diffrn_crystal_treatment ; attached with Exxon Paratone N, to a short length of fibre supported on a thin piece of copper wire inserted in a copper mounting pin. The crystal was quenched in a cold nitrogen gas stream from an Oxford Cryosystems Cryostream. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 308 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.11 _diffrn_reflns_number 44772 _diffrn_reflns_av_R_equivalents 0.0666 _diffrn_reflns_av_sigmaI/netI 0.0631 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 28.34 _reflns_number_total 11157 _reflns_number_gt 7636 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker,1995)' _computing_cell_refinement 'SAINT (Bruker,1995)' _computing_data_reduction 'SAINT and XPREP (Bruker 1995)' _computing_structure_solution 'SIR97 (Altomare, et. al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; teXsan for Windows (MSC, 1997) xtal 3.6 (Hall,du Boulay, D.J. & Olthof-Hazekamp, R. 1999) ORTEPII (Johnson,C.K., 1976). WinGX (Farrugia, 1999) ; _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.03P)^2^] 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_number_reflns 11157 _refine_ls_number_parameters 539 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0735 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.0916 _refine_ls_wR_factor_gt 0.0823 _refine_ls_goodness_of_fit_ref 1.213 _refine_ls_restrained_S_all 1.213 _refine_ls_shift/su_max 0.005 _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 0.152962(6) 0.842901(12) 0.005978(8) 0.03256(6) Uani 1 1 d . . . N1 N 0.07030(12) 0.7626(2) 0.02518(16) 0.0336(8) Uani 1 1 d . . . N2 N 0.10559(11) 0.8769(2) 0.08999(16) 0.0313(8) Uani 1 1 d . . . N3 N 0.16205(12) 0.9356(2) 0.18877(16) 0.0349(8) Uani 1 1 d . . . N4 N 0.19721(12) 0.8682(3) 0.21044(18) 0.0395(9) Uani 1 1 d . . . N5 N 0.20901(13) 0.6593(3) 0.07748(16) 0.0383(9) Uani 1 1 d . . . N6 N 0.24538(12) 0.7917(3) 0.12238(16) 0.0353(8) Uani 1 1 d . . . N7 N 0.30467(13) 0.9192(3) 0.14815(17) 0.0425(9) Uani 1 1 d . . . N8 N 0.31461(14) 0.9350(3) 0.10092(18) 0.0524(11) Uani 1 1 d . . . C1 C 0.11886(16) 0.9810(3) -0.0381(2) 0.0489(13) Uani 1 1 d . . . H1 H 0.1154 0.9950 -0.0025 0.059 Uiso 1 1 calc R . . C2 C 0.09259(16) 0.9043(4) -0.0752(2) 0.0438(12) Uani 1 1 d . . . H2 H 0.0718 0.8695 -0.0639 0.053 Uiso 1 1 calc R . . C3 C 0.09463(19) 0.8718(5) -0.1326(2) 0.0737(19) Uani 1 1 d . . . H3A H 0.0678 0.8260 -0.1551 0.088 Uiso 1 1 calc R . . H3B H 0.0894 0.9309 -0.1588 0.088 Uiso 1 1 calc R . . C4 C 0.13737(18) 0.8242(5) -0.1254(2) 0.0697(18) Uani 1 1 d . . . H4A H 0.1491 0.8607 -0.1506 0.084 Uiso 1 1 calc R . . H4B H 0.1288 0.7567 -0.1428 0.084 Uiso 1 1 calc R . . C5 C 0.17777(15) 0.8150(4) -0.0618(2) 0.0417(11) Uani 1 1 d . . . H5 H 0.1861 0.7502 -0.0452 0.050 Uiso 1 1 calc R . . C6 C 0.20406(15) 0.8932(3) -0.0252(2) 0.0367(10) Uani 1 1 d . . . H6 H 0.2291 0.8780 0.0142 0.044 Uiso 1 1 calc R . . C7 C 0.19569(19) 1.0001(3) -0.0437(3) 0.0596(15) Uani 1 1 d . . . H7A H 0.2226 1.0390 -0.0129 0.072 Uiso 1 1 calc R . . H7B H 0.1965 1.0072 -0.0833 0.072 Uiso 1 1 calc R . . C8 C 0.1525(2) 1.0438(4) -0.0502(4) 0.095(2) Uani 1 1 d . . . H8A H 0.1350 1.0694 -0.0926 0.114 Uiso 1 1 calc R . . H8B H 0.1611 1.1016 -0.0224 0.114 Uiso 1 1 calc R . . C9 C 0.10768(14) 0.8250(3) 0.04379(19) 0.0317(10) Uani 1 1 d . . . C10 C 0.04579(15) 0.7743(3) 0.0583(2) 0.0370(10) Uani 1 1 d . . . H10 H 0.0183 0.7386 0.0530 0.044 Uiso 1 1 calc R . . C11 C 0.06801(14) 0.8459(3) 0.0998(2) 0.0367(10) Uani 1 1 d . . . H11 H 0.0596 0.8703 0.1297 0.044 Uiso 1 1 calc R . . C12 C 0.05550(17) 0.6939(3) -0.0259(2) 0.0477(12) Uani 1 1 d . . . H12A H 0.0745 0.7051 -0.0474 0.072 Uiso 1 1 calc R . . H12B H 0.0218 0.7043 -0.0542 0.072 Uiso 1 1 calc R . . H12C H 0.0602 0.6258 -0.0104 0.072 Uiso 1 1 calc R . . C13 C 0.13787(14) 0.9559(3) 0.12374(19) 0.0349(10) Uani 1 1 d . . . H13A H 0.1617 0.9645 0.1086 0.042 Uiso 1 1 calc R . . H13B H 0.1198 1.0185 0.1164 0.042 Uiso 1 1 calc R . . C14 C 0.15045(16) 0.9665(4) 0.2325(2) 0.0498(13) Uani 1 1 d . . . H14 H 0.1264 1.0128 0.2275 0.060 Uiso 1 1 calc R . . C15 C 0.17971(18) 0.9186(4) 0.2844(2) 0.0556(14) Uani 1 1 d . . . H15 H 0.1808 0.9248 0.3235 0.067 Uiso 1 1 calc R . . C16 C 0.20788(16) 0.8586(3) 0.2689(2) 0.0461(12) Uani 1 1 d . . . H16 H 0.2319 0.8158 0.2968 0.055 Uiso 1 1 calc R . . C17 C 0.20557(15) 0.7594(3) 0.07178(19) 0.0351(10) Uani 1 1 d . . . C18 C 0.24846(15) 0.6304(3) 0.1296(2) 0.0424(12) Uani 1 1 d . . . H18 H 0.2581 0.5644 0.1428 0.051 Uiso 1 1 calc R . . C19 C 0.27083(16) 0.7138(4) 0.1584(2) 0.0442(12) Uani 1 1 d . . . H19 H 0.2990 0.7180 0.1964 0.053 Uiso 1 1 calc R . . C20 C 0.17484(17) 0.5913(3) 0.0323(2) 0.0470(12) Uani 1 1 d . . . H20A H 0.1543 0.5633 0.0483 0.070 Uiso 1 1 calc R . . H20B H 0.1920 0.5378 0.0241 0.070 Uiso 1 1 calc R . . H20C H 0.1554 0.6272 -0.0059 0.070 Uiso 1 1 calc R . . C21 C 0.25712(15) 0.8949(3) 0.1377(2) 0.0414(11) Uani 1 1 d . . . H21A H 0.2340 0.9364 0.1039 0.050 Uiso 1 1 calc R . . H21B H 0.2541 0.9107 0.1751 0.050 Uiso 1 1 calc R . . C22 C 0.34301(17) 0.9375(4) 0.2029(2) 0.0537(14) Uani 1 1 d . . . H22 H 0.3445 0.9322 0.2423 0.064 Uiso 1 1 calc R . . C23 C 0.37881(19) 0.9650(5) 0.1904(3) 0.0728(18) Uani 1 1 d . . . H23 H 0.4104 0.9822 0.2190 0.087 Uiso 1 1 calc R . . C24 C 0.35934(18) 0.9625(5) 0.1269(3) 0.0678(17) Uani 1 1 d . . . H24 H 0.3764 0.9788 0.1049 0.081 Uiso 1 1 calc R . . C25 C 0.16655(15) 0.2532(3) 0.1035(2) 0.0422(12) Uani 1 1 d . . . C26 C 0.19163(17) 0.2783(4) 0.0711(2) 0.0519(13) Uani 1 1 d . . . H26 H 0.1788 0.3275 0.0400 0.062 Uiso 1 1 calc R . . C27 C 0.23457(18) 0.2338(4) 0.0828(2) 0.0578(14) Uani 1 1 d . . . H27 H 0.2504 0.2531 0.0598 0.069 Uiso 1 1 calc R . . C28 C 0.25431(18) 0.1628(4) 0.1270(3) 0.0625(16) Uani 1 1 d . . . H28 H 0.2835 0.1321 0.1345 0.075 Uiso 1 1 calc R . . C29 C 0.23114(18) 0.1364(3) 0.1606(3) 0.0586(16) Uani 1 1 d . . . H29 H 0.2445 0.0871 0.1915 0.070 Uiso 1 1 calc R . . C30 C 0.18832(16) 0.1815(3) 0.1495(2) 0.0450(12) Uani 1 1 d . . . H30 H 0.1734 0.1632 0.1738 0.054 Uiso 1 1 calc R . . C31 C 0.08450(15) 0.2317(3) 0.1104(2) 0.0407(11) Uani 1 1 d . . . C32 C 0.05378(15) 0.1571(3) 0.0734(2) 0.0447(12) Uani 1 1 d . . . H32 H 0.0497 0.1497 0.0328 0.054 Uiso 1 1 calc R . . C33 C 0.02916(16) 0.0937(3) 0.0929(3) 0.0538(15) Uani 1 1 d . . . H33 H 0.0090 0.0442 0.0659 0.065 Uiso 1 1 calc R . . C34 C 0.03371(17) 0.1021(4) 0.1513(3) 0.0599(16) Uani 1 1 d . . . H34 H 0.0168 0.0590 0.1648 0.072 Uiso 1 1 calc R . . C35 C 0.06331(19) 0.1744(4) 0.1897(3) 0.0635(16) Uani 1 1 d . . . H35 H 0.0668 0.1818 0.2300 0.076 Uiso 1 1 calc R . . C36 C 0.08820(17) 0.2368(4) 0.1688(2) 0.0525(13) Uani 1 1 d . . . H36 H 0.1087 0.2852 0.1963 0.063 Uiso 1 1 calc R . . C37 C 0.12344(15) 0.4124(3) 0.1241(2) 0.0371(10) Uani 1 1 d . . . C38 C 0.08575(16) 0.4635(3) 0.1255(2) 0.0489(13) Uani 1 1 d . . . H38 H 0.0553 0.4329 0.1079 0.059 Uiso 1 1 calc R . . C39 C 0.09042(18) 0.5571(3) 0.1514(2) 0.0526(13) Uani 1 1 d . . . H39 H 0.0637 0.5890 0.1513 0.063 Uiso 1 1 calc R . . C40 C 0.1340(2) 0.6028(4) 0.1771(2) 0.0536(14) Uani 1 1 d . . . H40 H 0.1374 0.6673 0.1941 0.064 Uiso 1 1 calc R . . C41 C 0.17266(18) 0.5551(4) 0.1781(2) 0.0498(13) Uani 1 1 d . . . H41 H 0.2029 0.5864 0.1962 0.060 Uiso 1 1 calc R . . C42 C 0.16744(16) 0.4609(3) 0.1526(2) 0.0416(11) Uani 1 1 d . . . H42 H 0.1947 0.4284 0.1546 0.050 Uiso 1 1 calc R . . C43 C 0.08618(16) 0.3239(3) 0.0140(2) 0.0411(11) Uani 1 1 d . . . C44 C 0.06169(15) 0.4106(3) -0.0142(2) 0.0438(12) Uani 1 1 d . . . H44 H 0.0610 0.4633 0.0109 0.053 Uiso 1 1 calc R . . C45 C 0.03828(17) 0.4226(4) -0.0778(2) 0.0551(14) Uani 1 1 d . . . H45 H 0.0225 0.4832 -0.0946 0.066 Uiso 1 1 calc R . . C46 C 0.03755(18) 0.3488(4) -0.1164(3) 0.0587(14) Uani 1 1 d . . . H46 H 0.0218 0.3580 -0.1596 0.070 Uiso 1 1 calc R . . C47 C 0.06024(18) 0.2605(4) -0.0911(2) 0.0588(15) Uani 1 1 d . . . H47 H 0.0597 0.2077 -0.1169 0.071 Uiso 1 1 calc R . . C48 C 0.08388(17) 0.2495(3) -0.0277(2) 0.0512(13) Uani 1 1 d . . . H48 H 0.0994 0.1883 -0.0114 0.061 Uiso 1 1 calc R . . B1 B 0.11497(18) 0.3051(4) 0.0888(3) 0.0388(13) Uani 1 1 d . . . O1 O 0.0000 0.2174(11) -0.2500 0.035(4) Uiso 0.25 2 d SP . . C49 C 0.0503(6) 0.1778(12) -0.2419(8) 0.038(4) Uiso 0.25 1 d P . . H49A H 0.0638 0.1319 -0.2065 0.045 Uiso 0.25 1 calc PR . . H49B H 0.0450 0.1398 -0.2789 0.045 Uiso 0.25 1 calc PR . . C50 C 0.0817(7) 0.2485(15) -0.2331(10) 0.061(6) Uiso 0.25 1 d P . . H50A H 0.1115 0.2187 -0.2283 0.091 Uiso 0.25 1 calc PR . . H50B H 0.0879 0.2858 -0.1960 0.091 Uiso 0.25 1 calc PR . . H50C H 0.0692 0.2932 -0.2685 0.091 Uiso 0.25 1 calc PR . . O2 O 0.0127(5) 0.6109(12) -0.1867(7) 0.072(4) Uiso 0.25 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 Ir1 0.03074(10) 0.03186(9) 0.03520(10) 0.00423(8) 0.01531(7) 0.01019(8) N1 0.032(2) 0.0251(17) 0.039(2) 0.0010(15) 0.0124(17) 0.0045(15) N2 0.0260(18) 0.0331(18) 0.032(2) 0.0019(15) 0.0113(15) 0.0051(15) N3 0.0296(19) 0.0337(19) 0.039(2) -0.0053(16) 0.0142(17) 0.0024(15) N4 0.032(2) 0.040(2) 0.043(2) 0.0057(17) 0.0146(17) 0.0090(16) N5 0.041(2) 0.037(2) 0.040(2) 0.0091(18) 0.0213(17) 0.0107(18) N6 0.0294(19) 0.041(2) 0.035(2) 0.0037(17) 0.0149(16) 0.0099(16) N7 0.032(2) 0.051(2) 0.042(2) -0.0054(19) 0.0158(18) 0.0041(17) N8 0.048(3) 0.068(3) 0.045(3) -0.009(2) 0.026(2) -0.006(2) C1 0.050(3) 0.041(3) 0.059(3) 0.021(2) 0.028(3) 0.021(2) C2 0.040(3) 0.058(3) 0.037(3) 0.019(2) 0.021(2) 0.020(2) C3 0.053(3) 0.126(5) 0.038(3) 0.009(3) 0.018(3) 0.038(3) C4 0.044(3) 0.109(5) 0.043(3) -0.021(3) 0.009(2) 0.023(3) C5 0.037(3) 0.052(3) 0.038(3) 0.003(2) 0.019(2) 0.012(2) C6 0.036(2) 0.044(3) 0.034(2) 0.008(2) 0.019(2) 0.011(2) C7 0.065(4) 0.048(3) 0.082(4) 0.018(3) 0.047(3) 0.015(3) C8 0.077(4) 0.042(3) 0.195(8) 0.034(4) 0.087(5) 0.020(3) C9 0.030(2) 0.029(2) 0.032(2) 0.0085(17) 0.0110(18) 0.0121(17) C10 0.029(2) 0.035(2) 0.046(3) 0.009(2) 0.016(2) 0.0033(19) C11 0.030(2) 0.041(2) 0.042(3) 0.006(2) 0.019(2) 0.005(2) C12 0.044(3) 0.039(2) 0.056(3) -0.009(2) 0.019(2) -0.001(2) C13 0.029(2) 0.029(2) 0.042(3) 0.0042(19) 0.013(2) 0.0058(18) C14 0.038(3) 0.061(3) 0.053(3) -0.019(3) 0.023(2) 0.001(2) C15 0.050(3) 0.078(4) 0.038(3) -0.020(3) 0.019(3) -0.017(3) C16 0.038(3) 0.051(3) 0.038(3) 0.005(2) 0.008(2) -0.005(2) C17 0.035(2) 0.040(2) 0.036(3) 0.004(2) 0.021(2) 0.0087(19) C18 0.035(3) 0.040(3) 0.054(3) 0.016(2) 0.022(2) 0.015(2) C19 0.035(3) 0.057(3) 0.040(3) 0.013(2) 0.017(2) 0.017(2) C20 0.052(3) 0.035(2) 0.053(3) 0.002(2) 0.023(2) 0.008(2) C21 0.040(3) 0.046(3) 0.041(3) -0.003(2) 0.021(2) 0.006(2) C22 0.039(3) 0.071(4) 0.043(3) -0.014(3) 0.012(2) 0.003(2) C23 0.038(3) 0.113(5) 0.063(4) -0.037(4) 0.020(3) -0.021(3) C24 0.042(3) 0.100(5) 0.067(4) -0.027(4) 0.031(3) -0.017(3) C25 0.033(3) 0.031(2) 0.050(3) -0.002(2) 0.009(2) 0.0025(19) C26 0.044(3) 0.054(3) 0.055(3) 0.001(3) 0.020(3) 0.008(2) C27 0.042(3) 0.071(4) 0.057(3) -0.012(3) 0.020(3) 0.005(3) C28 0.037(3) 0.053(3) 0.079(4) -0.016(3) 0.011(3) 0.011(3) C29 0.043(3) 0.038(3) 0.068(4) -0.004(2) 0.002(3) 0.009(2) C30 0.042(3) 0.030(2) 0.049(3) 0.003(2) 0.009(2) 0.0013(19) C31 0.031(2) 0.031(2) 0.051(3) 0.006(2) 0.011(2) 0.0078(19) C32 0.032(2) 0.034(2) 0.059(3) 0.009(2) 0.014(2) 0.013(2) C33 0.027(3) 0.036(3) 0.081(4) 0.013(3) 0.011(3) 0.006(2) C34 0.034(3) 0.053(3) 0.084(4) 0.029(3) 0.021(3) 0.008(2) C35 0.054(3) 0.070(4) 0.060(4) 0.019(3) 0.020(3) 0.005(3) C36 0.045(3) 0.049(3) 0.057(3) 0.008(3) 0.018(3) -0.002(2) C37 0.038(3) 0.033(2) 0.036(3) 0.0038(19) 0.013(2) 0.0025(19) C38 0.037(3) 0.038(3) 0.058(3) -0.004(2) 0.010(2) 0.003(2) C39 0.052(3) 0.040(3) 0.052(3) -0.005(2) 0.012(3) 0.010(2) C40 0.070(4) 0.039(3) 0.048(3) -0.006(2) 0.024(3) -0.005(3) C41 0.053(3) 0.050(3) 0.046(3) -0.008(2) 0.022(3) -0.022(2) C42 0.041(3) 0.047(3) 0.037(3) 0.002(2) 0.018(2) -0.002(2) C43 0.041(3) 0.031(2) 0.050(3) -0.003(2) 0.020(2) 0.0024(19) C44 0.044(3) 0.031(2) 0.045(3) 0.001(2) 0.011(2) 0.007(2) C45 0.051(3) 0.044(3) 0.059(3) 0.010(3) 0.015(3) 0.011(2) C46 0.050(3) 0.071(4) 0.046(3) 0.001(3) 0.015(3) 0.011(3) C47 0.053(3) 0.059(3) 0.054(3) -0.014(3) 0.016(3) 0.013(3) C48 0.049(3) 0.039(3) 0.059(3) -0.002(2) 0.020(3) 0.015(2) B1 0.033(3) 0.032(2) 0.045(3) 0.003(2) 0.012(2) 0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 C17 2.045(4) . ? Ir1 C9 2.053(4) . ? Ir1 C1 2.178(4) . ? Ir1 C5 2.179(5) . ? Ir1 C2 2.193(4) . ? Ir1 C6 2.197(4) . ? N1 C9 1.351(5) . ? N1 C10 1.370(5) . ? N1 C12 1.454(5) . ? N2 C9 1.362(5) . ? N2 C11 1.384(5) . ? N2 C13 1.447(5) . ? N3 N4 1.345(4) . ? N3 C14 1.352(6) . ? N3 C13 1.445(5) . ? N4 C16 1.322(6) . ? N5 C17 1.358(5) . ? N5 C18 1.371(5) . ? N5 C20 1.463(5) . ? N6 C19 1.371(5) . ? N6 C17 1.371(5) . ? N6 C21 1.448(6) . ? N7 N8 1.353(5) . ? N7 C22 1.356(6) . ? N7 C21 1.445(5) . ? N8 C24 1.312(6) . ? C1 C2 1.379(6) . ? C1 C8 1.497(7) . ? C1 H1 0.9500 . ? C2 C3 1.507(7) . ? C2 H2 0.9500 . ? C3 C4 1.435(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.500(6) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.389(6) . ? C5 H5 0.9500 . ? C6 C7 1.501(6) . ? C6 H6 0.9500 . ? C7 C8 1.430(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C10 C11 1.344(6) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.347(7) . ? C14 H14 0.9500 . ? C15 C16 1.384(7) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C18 C19 1.346(6) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.357(7) . ? C22 H22 0.9500 . ? C23 C24 1.389(7) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.404(7) . ? C25 C30 1.404(6) . ? C25 B1 1.659(7) . ? C26 C27 1.391(7) . ? C26 H26 0.9500 . ? C27 C28 1.364(7) . ? C27 H27 0.9500 . ? C28 C29 1.382(8) . ? C28 H28 0.9500 . ? C29 C30 1.396(7) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C36 1.388(7) . ? C31 C32 1.406(6) . ? C31 B1 1.635(7) . ? C32 C33 1.385(7) . ? C32 H32 0.9500 . ? C33 C34 1.380(8) . ? C33 H33 0.9500 . ? C34 C35 1.381(7) . ? C34 H34 0.9500 . ? C35 C36 1.404(7) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C38 1.395(6) . ? C37 C42 1.401(6) . ? C37 B1 1.646(7) . ? C38 C39 1.393(6) . ? C38 H38 0.9500 . ? C39 C40 1.372(7) . ? C39 H39 0.9500 . ? C40 C41 1.375(7) . ? C40 H40 0.9500 . ? C41 C42 1.396(6) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C44 1.399(6) . ? C43 C48 1.412(6) . ? C43 B1 1.652(7) . ? C44 C45 1.396(6) . ? C44 H44 0.9500 . ? C45 C46 1.369(7) . ? C45 H45 0.9500 . ? C46 C47 1.384(7) . ? C46 H46 0.9500 . ? C47 C48 1.391(7) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? O1 C49 1.605(18) 2_554 ? O1 C49 1.605(18) . ? C49 C50 1.32(2) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? 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 C17 Ir1 C9 93.57(16) . . ? C17 Ir1 C1 154.51(19) . . ? C9 Ir1 C1 92.04(17) . . ? C17 Ir1 C5 93.37(16) . . ? C9 Ir1 C5 154.24(17) . . ? C1 Ir1 C5 92.28(18) . . ? C17 Ir1 C2 168.33(18) . . ? C9 Ir1 C2 87.58(16) . . ? C1 Ir1 C2 36.77(17) . . ? C5 Ir1 C2 80.85(17) . . ? C17 Ir1 C6 89.06(16) . . ? C9 Ir1 C6 167.78(16) . . ? C1 Ir1 C6 80.66(17) . . ? C5 Ir1 C6 37.01(16) . . ? C2 Ir1 C6 92.25(17) . . ? C9 N1 C10 112.1(4) . . ? C9 N1 C12 125.0(4) . . ? C10 N1 C12 122.8(4) . . ? C9 N2 C11 111.5(4) . . ? C9 N2 C13 124.3(4) . . ? C11 N2 C13 124.1(4) . . ? N4 N3 C14 112.0(4) . . ? N4 N3 C13 119.1(3) . . ? C14 N3 C13 128.4(4) . . ? C16 N4 N3 104.3(4) . . ? C17 N5 C18 112.1(4) . . ? C17 N5 C20 123.4(4) . . ? C18 N5 C20 124.5(4) . . ? C19 N6 C17 111.2(4) . . ? C19 N6 C21 124.5(4) . . ? C17 N6 C21 124.1(3) . . ? N8 N7 C22 111.4(4) . . ? N8 N7 C21 121.4(4) . . ? C22 N7 C21 127.0(4) . . ? C24 N8 N7 104.8(4) . . ? C2 C1 C8 124.2(5) . . ? C2 C1 Ir1 72.2(2) . . ? C8 C1 Ir1 110.4(3) . . ? C2 C1 H1 117.9 . . ? C8 C1 H1 117.9 . . ? Ir1 C1 H1 87.4 . . ? C1 C2 C3 124.4(5) . . ? C1 C2 Ir1 71.0(2) . . ? C3 C2 Ir1 110.2(3) . . ? C1 C2 H2 117.8 . . ? C3 C2 H2 117.8 . . ? Ir1 C2 H2 88.8 . . ? C4 C3 C2 117.5(4) . . ? C4 C3 H3A 107.9 . . ? C2 C3 H3A 107.9 . . ? C4 C3 H3B 107.9 . . ? C2 C3 H3B 107.9 . . ? H3A C3 H3B 107.2 . . ? C3 C4 C5 118.0(5) . . ? C3 C4 H4A 107.8 . . ? C5 C4 H4A 107.8 . . ? C3 C4 H4B 107.8 . . ? C5 C4 H4B 107.8 . . ? H4A C4 H4B 107.1 . . ? C6 C5 C4 125.4(5) . . ? C6 C5 Ir1 72.2(3) . . ? C4 C5 Ir1 110.2(3) . . ? C6 C5 H5 117.3 . . ? C4 C5 H5 117.3 . . ? Ir1 C5 H5 87.5 . . ? C5 C6 C7 124.6(4) . . ? C5 C6 Ir1 70.8(3) . . ? C7 C6 Ir1 110.4(3) . . ? C5 C6 H6 117.7 . . ? C7 C6 H6 117.7 . . ? Ir1 C6 H6 88.8 . . ? C8 C7 C6 117.2(4) . . ? C8 C7 H7A 108.0 . . ? C6 C7 H7A 108.0 . . ? C8 C7 H7B 108.0 . . ? C6 C7 H7B 108.0 . . ? H7A C7 H7B 107.2 . . ? C7 C8 C1 118.5(4) . . ? C7 C8 H8A 107.7 . . ? C1 C8 H8A 107.7 . . ? C7 C8 H8B 107.7 . . ? C1 C8 H8B 107.7 . . ? H8A C8 H8B 107.1 . . ? N1 C9 N2 103.3(4) . . ? N1 C9 Ir1 127.4(3) . . ? N2 C9 Ir1 129.1(3) . . ? C11 C10 N1 106.9(4) . . ? C11 C10 H10 126.5 . . ? N1 C10 H10 126.5 . . ? C10 C11 N2 106.1(4) . . ? C10 C11 H11 126.9 . . ? N2 C11 H11 126.9 . . ? N1 C12 H12A 109.5 . . ? N1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N3 C13 N2 111.6(3) . . ? N3 C13 H13A 109.3 . . ? N2 C13 H13A 109.3 . . ? N3 C13 H13B 109.3 . . ? N2 C13 H13B 109.3 . . ? H13A C13 H13B 108.0 . . ? C15 C14 N3 106.5(4) . . ? C15 C14 H14 126.7 . . ? N3 C14 H14 126.7 . . ? C14 C15 C16 105.6(5) . . ? C14 C15 H15 127.2 . . ? C16 C15 H15 127.2 . . ? N4 C16 C15 111.6(4) . . ? N4 C16 H16 124.2 . . ? C15 C16 H16 124.2 . . ? N5 C17 N6 103.1(4) . . ? N5 C17 Ir1 128.9(3) . . ? N6 C17 Ir1 127.9(3) . . ? C19 C18 N5 106.5(4) . . ? C19 C18 H18 126.8 . . ? N5 C18 H18 126.8 . . ? C18 C19 N6 107.1(4) . . ? C18 C19 H19 126.5 . . ? N6 C19 H19 126.5 . . ? N5 C20 H20A 109.5 . . ? N5 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N5 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N7 C21 N6 112.8(3) . . ? N7 C21 H21A 109.0 . . ? N6 C21 H21A 109.0 . . ? N7 C21 H21B 109.0 . . ? N6 C21 H21B 109.0 . . ? H21A C21 H21B 107.8 . . ? N7 C22 C23 106.6(5) . . ? N7 C22 H22 126.7 . . ? C23 C22 H22 126.7 . . ? C22 C23 C24 105.3(5) . . ? C22 C23 H23 127.4 . . ? C24 C23 H23 127.4 . . ? N8 C24 C23 111.9(5) . . ? N8 C24 H24 124.1 . . ? C23 C24 H24 124.1 . . ? C26 C25 C30 115.3(4) . . ? C26 C25 B1 122.2(4) . . ? C30 C25 B1 122.4(5) . . ? C27 C26 C25 122.3(5) . . ? C27 C26 H26 118.9 . . ? C25 C26 H26 118.9 . . ? C28 C27 C26 121.0(6) . . ? C28 C27 H27 119.5 . . ? C26 C27 H27 119.5 . . ? C27 C28 C29 118.8(5) . . ? C27 C28 H28 120.6 . . ? C29 C28 H28 120.6 . . ? C28 C29 C30 120.6(5) . . ? C28 C29 H29 119.7 . . ? C30 C29 H29 119.7 . . ? C29 C30 C25 122.0(5) . . ? C29 C30 H30 119.0 . . ? C25 C30 H30 119.0 . . ? C36 C31 C32 114.0(4) . . ? C36 C31 B1 121.8(4) . . ? C32 C31 B1 124.2(5) . . ? C33 C32 C31 123.5(5) . . ? C33 C32 H32 118.2 . . ? C31 C32 H32 118.2 . . ? C34 C33 C32 120.3(5) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? C33 C34 C35 118.8(5) . . ? C33 C34 H34 120.6 . . ? C35 C34 H34 120.6 . . ? C34 C35 C36 119.6(6) . . ? C34 C35 H35 120.2 . . ? C36 C35 H35 120.2 . . ? C31 C36 C35 123.8(5) . . ? C31 C36 H36 118.1 . . ? C35 C36 H36 118.1 . . ? C38 C37 C42 115.0(4) . . ? C38 C37 B1 121.1(4) . . ? C42 C37 B1 123.9(4) . . ? C39 C38 C37 123.4(4) . . ? C39 C38 H38 118.3 . . ? C37 C38 H38 118.3 . . ? C40 C39 C38 119.4(5) . . ? C40 C39 H39 120.3 . . ? C38 C39 H39 120.3 . . ? C39 C40 C41 119.8(5) . . ? C39 C40 H40 120.1 . . ? C41 C40 H40 120.1 . . ? C40 C41 C42 120.0(4) . . ? C40 C41 H41 120.0 . . ? C42 C41 H41 120.0 . . ? C41 C42 C37 122.4(4) . . ? C41 C42 H42 118.8 . . ? C37 C42 H42 118.8 . . ? C44 C43 C48 114.0(4) . . ? C44 C43 B1 125.0(4) . . ? C48 C43 B1 121.0(4) . . ? C45 C44 C43 122.5(4) . . ? C45 C44 H44 118.7 . . ? C43 C44 H44 118.7 . . ? C46 C45 C44 121.5(5) . . ? C46 C45 H45 119.3 . . ? C44 C45 H45 119.3 . . ? C45 C46 C47 118.5(5) . . ? C45 C46 H46 120.8 . . ? C47 C46 H46 120.8 . . ? C46 C47 C48 119.7(5) . . ? C46 C47 H47 120.1 . . ? C48 C47 H47 120.1 . . ? C47 C48 C43 123.8(4) . . ? C47 C48 H48 118.1 . . ? C43 C48 H48 118.1 . . ? C31 B1 C37 109.8(4) . . ? C31 B1 C43 110.4(4) . . ? C37 B1 C43 108.9(4) . . ? C31 B1 C25 110.1(4) . . ? C37 B1 C25 110.7(4) . . ? C43 B1 C25 106.9(4) . . ? C49 O1 C49 141.1(15) 2_554 . ? C50 C49 O1 114.2(15) . . ? C50 C49 H49A 108.7 . . ? O1 C49 H49A 108.7 . . ? C50 C49 H49B 108.7 . . ? O1 C49 H49B 108.7 . . ? H49A C49 H49B 107.6 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C14 N3 N4 C16 -0.9(5) . . . . ? C13 N3 N4 C16 -173.0(4) . . . . ? C22 N7 N8 C24 0.4(6) . . . . ? C21 N7 N8 C24 175.2(4) . . . . ? C17 Ir1 C1 C2 174.1(4) . . . . ? C9 Ir1 C1 C2 -83.2(3) . . . . ? C5 Ir1 C1 C2 71.4(3) . . . . ? C6 Ir1 C1 C2 106.6(3) . . . . ? C17 Ir1 C1 C8 53.4(7) . . . . ? C9 Ir1 C1 C8 156.1(5) . . . . ? C5 Ir1 C1 C8 -49.3(5) . . . . ? C2 Ir1 C1 C8 -120.7(6) . . . . ? C6 Ir1 C1 C8 -14.0(4) . . . . ? C8 C1 C2 C3 1.0(7) . . . . ? Ir1 C1 C2 C3 -102.0(4) . . . . ? C8 C1 C2 Ir1 103.0(4) . . . . ? C17 Ir1 C2 C1 -167.4(8) . . . . ? C9 Ir1 C2 C1 96.7(3) . . . . ? C5 Ir1 C2 C1 -106.4(3) . . . . ? C6 Ir1 C2 C1 -71.1(3) . . . . ? C17 Ir1 C2 C3 -46.7(11) . . . . ? C9 Ir1 C2 C3 -142.7(4) . . . . ? C1 Ir1 C2 C3 120.7(5) . . . . ? C5 Ir1 C2 C3 14.2(4) . . . . ? C6 Ir1 C2 C3 49.6(4) . . . . ? C1 C2 C3 C4 69.9(8) . . . . ? Ir1 C2 C3 C4 -10.5(8) . . . . ? C2 C3 C4 C5 -3.2(10) . . . . ? C3 C4 C5 C6 -66.8(8) . . . . ? C3 C4 C5 Ir1 15.3(7) . . . . ? C17 Ir1 C5 C6 -84.0(3) . . . . ? C9 Ir1 C5 C6 170.6(3) . . . . ? C1 Ir1 C5 C6 71.2(3) . . . . ? C2 Ir1 C5 C6 106.3(3) . . . . ? C17 Ir1 C5 C4 154.0(4) . . . . ? C9 Ir1 C5 C4 48.6(6) . . . . ? C1 Ir1 C5 C4 -50.9(4) . . . . ? C2 Ir1 C5 C4 -15.8(4) . . . . ? C6 Ir1 C5 C4 -122.0(5) . . . . ? C4 C5 C6 C7 0.6(7) . . . . ? Ir1 C5 C6 C7 -102.0(4) . . . . ? C4 C5 C6 Ir1 102.6(5) . . . . ? C17 Ir1 C6 C5 96.9(3) . . . . ? C9 Ir1 C6 C5 -160.5(6) . . . . ? C1 Ir1 C6 C5 -106.6(3) . . . . ? C2 Ir1 C6 C5 -71.5(3) . . . . ? C17 Ir1 C6 C7 -142.4(4) . . . . ? C9 Ir1 C6 C7 -39.7(9) . . . . ? C1 Ir1 C6 C7 14.2(4) . . . . ? C5 Ir1 C6 C7 120.8(5) . . . . ? C2 Ir1 C6 C7 49.2(4) . . . . ? C5 C6 C7 C8 68.0(7) . . . . ? Ir1 C6 C7 C8 -12.3(7) . . . . ? C6 C7 C8 C1 0.2(9) . . . . ? C2 C1 C8 C7 -69.8(8) . . . . ? Ir1 C1 C8 C7 12.0(8) . . . . ? C10 N1 C9 N2 -0.2(4) . . . . ? C12 N1 C9 N2 176.8(3) . . . . ? C10 N1 C9 Ir1 -176.0(3) . . . . ? C12 N1 C9 Ir1 1.0(5) . . . . ? C11 N2 C9 N1 0.6(4) . . . . ? C13 N2 C9 N1 -178.0(3) . . . . ? C11 N2 C9 Ir1 176.4(3) . . . . ? C13 N2 C9 Ir1 -2.3(5) . . . . ? C17 Ir1 C9 N1 -101.1(3) . . . . ? C1 Ir1 C9 N1 103.8(3) . . . . ? C5 Ir1 C9 N1 4.2(6) . . . . ? C2 Ir1 C9 N1 67.2(3) . . . . ? C6 Ir1 C9 N1 156.7(6) . . . . ? C17 Ir1 C9 N2 84.1(4) . . . . ? C1 Ir1 C9 N2 -71.0(4) . . . . ? C5 Ir1 C9 N2 -170.5(3) . . . . ? C2 Ir1 C9 N2 -107.5(4) . . . . ? C6 Ir1 C9 N2 -18.0(9) . . . . ? C9 N1 C10 C11 -0.3(5) . . . . ? C12 N1 C10 C11 -177.4(4) . . . . ? N1 C10 C11 N2 0.7(4) . . . . ? C9 N2 C11 C10 -0.9(5) . . . . ? C13 N2 C11 C10 177.8(3) . . . . ? N4 N3 C13 N2 74.7(5) . . . . ? C14 N3 C13 N2 -95.9(5) . . . . ? C9 N2 C13 N3 -122.5(4) . . . . ? C11 N2 C13 N3 59.0(5) . . . . ? N4 N3 C14 C15 1.1(5) . . . . ? C13 N3 C14 C15 172.3(4) . . . . ? N3 C14 C15 C16 -0.8(5) . . . . ? N3 N4 C16 C15 0.4(5) . . . . ? C14 C15 C16 N4 0.3(6) . . . . ? C18 N5 C17 N6 1.1(5) . . . . ? C20 N5 C17 N6 -177.7(4) . . . . ? C18 N5 C17 Ir1 -176.8(3) . . . . ? C20 N5 C17 Ir1 4.3(6) . . . . ? C19 N6 C17 N5 -2.2(5) . . . . ? C21 N6 C17 N5 -178.4(4) . . . . ? C19 N6 C17 Ir1 175.8(3) . . . . ? C21 N6 C17 Ir1 -0.4(6) . . . . ? C9 Ir1 C17 N5 77.9(4) . . . . ? C1 Ir1 C17 N5 -179.8(4) . . . . ? C5 Ir1 C17 N5 -77.3(4) . . . . ? C2 Ir1 C17 N5 -17.5(11) . . . . ? C6 Ir1 C17 N5 -114.1(4) . . . . ? C9 Ir1 C17 N6 -99.6(4) . . . . ? C1 Ir1 C17 N6 2.7(7) . . . . ? C5 Ir1 C17 N6 105.2(4) . . . . ? C2 Ir1 C17 N6 165.0(7) . . . . ? C6 Ir1 C17 N6 68.4(4) . . . . ? C17 N5 C18 C19 0.4(5) . . . . ? C20 N5 C18 C19 179.2(4) . . . . ? N5 C18 C19 N6 -1.7(5) . . . . ? C17 N6 C19 C18 2.5(5) . . . . ? C21 N6 C19 C18 178.7(4) . . . . ? N8 N7 C21 N6 79.8(5) . . . . ? C22 N7 C21 N6 -106.3(5) . . . . ? C19 N6 C21 N7 57.0(6) . . . . ? C17 N6 C21 N7 -127.4(4) . . . . ? N8 N7 C22 C23 -0.6(6) . . . . ? C21 N7 C22 C23 -175.0(5) . . . . ? N7 C22 C23 C24 0.6(6) . . . . ? N7 N8 C24 C23 0.0(7) . . . . ? C22 C23 C24 N8 -0.4(7) . . . . ? C30 C25 C26 C27 1.3(7) . . . . ? B1 C25 C26 C27 -179.1(4) . . . . ? C25 C26 C27 C28 0.1(8) . . . . ? C26 C27 C28 C29 -0.7(8) . . . . ? C27 C28 C29 C30 0.0(8) . . . . ? C28 C29 C30 C25 1.4(7) . . . . ? C26 C25 C30 C29 -2.0(6) . . . . ? B1 C25 C30 C29 178.4(4) . . . . ? C36 C31 C32 C33 0.0(6) . . . . ? B1 C31 C32 C33 178.2(4) . . . . ? C31 C32 C33 C34 0.5(7) . . . . ? C32 C33 C34 C35 -0.2(7) . . . . ? C33 C34 C35 C36 -0.5(7) . . . . ? C32 C31 C36 C35 -0.8(7) . . . . ? B1 C31 C36 C35 -179.0(4) . . . . ? C34 C35 C36 C31 1.0(8) . . . . ? C42 C37 C38 C39 1.9(7) . . . . ? B1 C37 C38 C39 -175.9(5) . . . . ? C37 C38 C39 C40 0.0(8) . . . . ? C38 C39 C40 C41 -1.3(8) . . . . ? C39 C40 C41 C42 0.6(8) . . . . ? C40 C41 C42 C37 1.5(7) . . . . ? C38 C37 C42 C41 -2.7(7) . . . . ? B1 C37 C42 C41 175.0(4) . . . . ? C48 C43 C44 C45 -1.6(7) . . . . ? B1 C43 C44 C45 179.4(5) . . . . ? C43 C44 C45 C46 0.8(8) . . . . ? C44 C45 C46 C47 0.7(8) . . . . ? C45 C46 C47 C48 -1.3(8) . . . . ? C46 C47 C48 C43 0.4(9) . . . . ? C44 C43 C48 C47 1.0(7) . . . . ? B1 C43 C48 C47 180.0(5) . . . . ? C36 C31 B1 C37 -31.3(5) . . . . ? C32 C31 B1 C37 150.6(4) . . . . ? C36 C31 B1 C43 -151.5(4) . . . . ? C32 C31 B1 C43 30.4(6) . . . . ? C36 C31 B1 C25 90.8(5) . . . . ? C32 C31 B1 C25 -87.3(5) . . . . ? C38 C37 B1 C31 -49.4(6) . . . . ? C42 C37 B1 C31 133.0(4) . . . . ? C38 C37 B1 C43 71.7(6) . . . . ? C42 C37 B1 C43 -105.9(5) . . . . ? C38 C37 B1 C25 -171.1(4) . . . . ? C42 C37 B1 C25 11.3(6) . . . . ? C44 C43 B1 C31 104.5(5) . . . . ? C48 C43 B1 C31 -74.4(6) . . . . ? C44 C43 B1 C37 -16.2(6) . . . . ? C48 C43 B1 C37 164.9(4) . . . . ? C44 C43 B1 C25 -135.8(5) . . . . ? C48 C43 B1 C25 45.3(6) . . . . ? C26 C25 B1 C31 155.6(4) . . . . ? C30 C25 B1 C31 -24.8(6) . . . . ? C26 C25 B1 C37 -82.8(5) . . . . ? C30 C25 B1 C37 96.8(5) . . . . ? C26 C25 B1 C43 35.6(6) . . . . ? C30 C25 B1 C43 -144.8(4) . . . . ? C49 O1 C49 C50 -175.9(18) 2_554 . . . ? _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.957 _refine_diff_density_max 2.683 _refine_diff_density_min -1.102 _refine_diff_density_rms 0.119 #===END data_bam25 _database_code_depnum_ccdc_archive 'CCDC 600824' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H42 B N4 Rh' _chemical_formula_weight 692.50 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 'P 21/n ' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.396(5) _cell_length_b 19.599(11) _cell_length_c 18.476(11) _cell_angle_alpha 90.00 _cell_angle_beta 93.911(10) _cell_angle_gamma 90.00 _cell_volume 3394(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 945 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 26.37 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.366 _exptl_crystal_size_mid 0.119 _exptl_crystal_size_min 0.078 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.355 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1440 _exptl_absorpt_coefficient_mu 0.537 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _diffrn_crystal_treatment ; attached with Exxon Paratone N, to a short length of fibre supported on a thin piece of copper wire inserted in a copper mounting pin. The crystal was quenched in a cold nitrogen gas stream from an Oxford Cryosystems Cryostream. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 225 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.25 _diffrn_reflns_number 33922 _diffrn_reflns_av_R_equivalents 0.0612 _diffrn_reflns_av_sigmaI/netI 0.0522 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 28.31 _reflns_number_total 8150 _reflns_number_gt 6019 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker,1995)' _computing_cell_refinement 'SAINT (Bruker,1995)' _computing_data_reduction 'SAINT and XPREP (Bruker 1995)' _computing_structure_solution 'SIR97 (Altomare, et. al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; teXsan for Windows (MSC, 1997) xtal 3.6 (Hall,du Boulay, D.J. & Olthof-Hazekamp, R. 1999) ORTEPII (Johnson,C.K., 1976). WinGX (Farrugia, 1999) ; _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.03P)^2^] 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_number_reflns 8150 _refine_ls_number_parameters 432 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0522 _refine_ls_R_factor_gt 0.0324 _refine_ls_wR_factor_ref 0.0749 _refine_ls_wR_factor_gt 0.0696 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _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 -0.015841(18) 0.213007(8) 0.013428(9) 0.02477(6) Uani 1 1 d . . . N1 N -0.15635(18) 0.16349(9) 0.15669(9) 0.0283(4) Uani 1 1 d . . . N2 N -0.10590(17) 0.26856(8) 0.15191(9) 0.0241(4) Uani 1 1 d . . . N3 N -0.14350(18) 0.34715(8) 0.05585(9) 0.0261(4) Uani 1 1 d . . . N4 N -0.13531(19) 0.30295(8) -0.00049(9) 0.0268(4) Uani 1 1 d . . . C1 C 0.1710(3) 0.15792(12) 0.04911(14) 0.0395(6) Uani 1 1 d . . . H1 H 0.173(2) 0.1552(10) 0.0994(12) 0.026(6) Uiso 1 1 d . . . C2 C 0.0796(3) 0.11357(13) 0.01145(15) 0.0450(6) Uani 1 1 d . . . H2 H 0.024(3) 0.0856(13) 0.0414(14) 0.057(8) Uiso 1 1 d . . . C3 C 0.0970(3) 0.08806(15) -0.06466(16) 0.0642(9) Uani 1 1 d . . . H3A H 0.1998 0.0870 -0.0733 0.077 Uiso 1 1 calc R . . H3B H 0.0603 0.0408 -0.0690 0.077 Uiso 1 1 calc R . . C4 C 0.0201(3) 0.13161(17) -0.12204(16) 0.0772(11) Uani 1 1 d . . . H4A H -0.0783 0.1141 -0.1312 0.093 Uiso 1 1 calc R . . H4B H 0.0687 0.1271 -0.1677 0.093 Uiso 1 1 calc R . . C5 C 0.0132(3) 0.20694(16) -0.10219(13) 0.0553(8) Uani 1 1 d . . . H5 H -0.070(3) 0.2324(13) -0.1241(14) 0.056(8) Uiso 1 1 d . . . C6 C 0.1227(3) 0.24449(16) -0.07140(14) 0.0491(7) Uani 1 1 d . . . H6 H 0.107(3) 0.2938(13) -0.0724(14) 0.056(8) Uiso 1 1 d . . . C7 C 0.2733(3) 0.21903(14) -0.05586(16) 0.0551(7) Uani 1 1 d . . . H7A H 0.2926 0.1823 -0.0906 0.066 Uiso 1 1 calc R . . H7B H 0.3409 0.2568 -0.0632 0.066 Uiso 1 1 calc R . . C8 C 0.2985(3) 0.19221(15) 0.02031(15) 0.0521(7) Uani 1 1 d . . . H8A H 0.3784 0.1592 0.0216 0.063 Uiso 1 1 calc R . . H8B H 0.3278 0.2306 0.0528 0.063 Uiso 1 1 calc R . . C9 C -0.0945(2) 0.20964(10) 0.11433(10) 0.0219(4) Uani 1 1 d . . . C10 C -0.2047(2) 0.19333(12) 0.21808(12) 0.0332(5) Uani 1 1 d . . . H10 H -0.2510 0.1708 0.2555 0.040 Uiso 1 1 calc R . . C11 C -0.1741(2) 0.25976(12) 0.21499(11) 0.0297(5) Uani 1 1 d . . . H11 H -0.1951 0.2939 0.2492 0.036 Uiso 1 1 calc R . . C12 C -0.1685(3) 0.09042(11) 0.14232(13) 0.0428(6) Uani 1 1 d . . . H12A H -0.1831 0.0828 0.0899 0.064 Uiso 1 1 calc R . . H12B H -0.2498 0.0719 0.1665 0.064 Uiso 1 1 calc R . . H12C H -0.0808 0.0675 0.1609 0.064 Uiso 1 1 calc R . . C13 C -0.0604(2) 0.33312(10) 0.12283(11) 0.0257(5) Uani 1 1 d . . . H13A H -0.0741 0.3701 0.1582 0.031 Uiso 1 1 calc R . . H13B H 0.0421 0.3310 0.1138 0.031 Uiso 1 1 calc R . . C14 C -0.2339(2) 0.39848(11) 0.03902(13) 0.0366(6) Uani 1 1 d . . . H14 H -0.2572 0.4350 0.0699 0.044 Uiso 1 1 calc R . . C15 C -0.2862(3) 0.38831(12) -0.03073(13) 0.0451(6) Uani 1 1 d . . . H15 H -0.3523 0.4162 -0.0583 0.054 Uiso 1 1 calc R . . C16 C -0.2229(2) 0.32886(11) -0.05310(12) 0.0358(6) Uani 1 1 d . . . H16 H -0.2398 0.3091 -0.0999 0.043 Uiso 1 1 calc R . . C17 C 0.16565(19) 0.46347(9) 0.17788(10) 0.0207(4) Uani 1 1 d . . . C18 C 0.1246(2) 0.47086(11) 0.10421(11) 0.0275(5) Uani 1 1 d . . . H18 H 0.0464 0.5000 0.0909 0.033 Uiso 1 1 calc R . . C19 C 0.1915(2) 0.43802(11) 0.04956(12) 0.0321(5) Uani 1 1 d . . . H19 H 0.1589 0.4450 0.0003 0.039 Uiso 1 1 calc R . . C20 C 0.3054(2) 0.39511(11) 0.06645(12) 0.0303(5) Uani 1 1 d . . . H20 H 0.3510 0.3719 0.0293 0.036 Uiso 1 1 calc R . . C21 C 0.3518(2) 0.38654(11) 0.13828(12) 0.0300(5) Uani 1 1 d . . . H21 H 0.4308 0.3576 0.1509 0.036 Uiso 1 1 calc R . . C22 C 0.2834(2) 0.42009(10) 0.19209(11) 0.0261(5) Uani 1 1 d . . . H22 H 0.3179 0.4134 0.2411 0.031 Uiso 1 1 calc R . . C23 C 0.1514(2) 0.58120(10) 0.25170(10) 0.0225(4) Uani 1 1 d . . . C24 C 0.2866(2) 0.59899(11) 0.23193(11) 0.0300(5) Uani 1 1 d . . . H24 H 0.3462 0.5645 0.2142 0.036 Uiso 1 1 calc R . . C25 C 0.3379(3) 0.66596(13) 0.23726(12) 0.0400(6) Uani 1 1 d . . . H25 H 0.4309 0.6761 0.2231 0.048 Uiso 1 1 calc R . . C26 C 0.2545(3) 0.71727(12) 0.26286(13) 0.0462(7) Uani 1 1 d . . . H26 H 0.2885 0.7629 0.2655 0.055 Uiso 1 1 calc R . . C27 C 0.1222(3) 0.70147(11) 0.28435(14) 0.0435(7) Uani 1 1 d . . . H27 H 0.0638 0.7362 0.3027 0.052 Uiso 1 1 calc R . . C28 C 0.0731(2) 0.63479(11) 0.27944(12) 0.0332(5) Uani 1 1 d . . . H28 H -0.0184 0.6250 0.2958 0.040 Uiso 1 1 calc R . . C29 C 0.1067(2) 0.46130(10) 0.31932(11) 0.0224(4) Uani 1 1 d . . . C30 C 0.1351(2) 0.49295(11) 0.38640(12) 0.0325(5) Uani 1 1 d . . . H30 H 0.1451 0.5412 0.3880 0.039 Uiso 1 1 calc R . . C31 C 0.1493(3) 0.45640(13) 0.45106(12) 0.0429(6) Uani 1 1 d . . . H31 H 0.1686 0.4800 0.4956 0.052 Uiso 1 1 calc R . . C32 C 0.1359(2) 0.38662(12) 0.45135(12) 0.0388(6) Uani 1 1 d . . . H32 H 0.1461 0.3618 0.4956 0.047 Uiso 1 1 calc R . . C33 C 0.1072(2) 0.35304(11) 0.38610(12) 0.0309(5) Uani 1 1 d . . . H33 H 0.0974 0.3048 0.3851 0.037 Uiso 1 1 calc R . . C34 C 0.0928(2) 0.39002(10) 0.32230(11) 0.0254(5) Uani 1 1 d . . . H34 H 0.0724 0.3660 0.2782 0.030 Uiso 1 1 calc R . . C35 C -0.0862(2) 0.50968(9) 0.21701(10) 0.0202(4) Uani 1 1 d . . . C36 C -0.1907(2) 0.46565(10) 0.24050(10) 0.0230(4) Uani 1 1 d . . . H36 H -0.1632 0.4322 0.2759 0.028 Uiso 1 1 calc R . . C37 C -0.3327(2) 0.46854(11) 0.21451(11) 0.0292(5) Uani 1 1 d . . . H37 H -0.3992 0.4368 0.2315 0.035 Uiso 1 1 calc R . . C38 C -0.3779(2) 0.51724(11) 0.16414(11) 0.0292(5) Uani 1 1 d . . . H38 H -0.4749 0.5193 0.1460 0.035 Uiso 1 1 calc R . . C39 C -0.2792(2) 0.56292(10) 0.14069(11) 0.0270(5) Uani 1 1 d . . . H39 H -0.3087 0.5973 0.1067 0.032 Uiso 1 1 calc R . . C40 C -0.1375(2) 0.55897(10) 0.16641(10) 0.0243(4) Uani 1 1 d . . . H40 H -0.0720 0.5910 0.1491 0.029 Uiso 1 1 calc R . . B1 B 0.0858(2) 0.50377(11) 0.24254(13) 0.0211(5) 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 0.03212(10) 0.02240(9) 0.01935(9) -0.00171(7) -0.00140(6) 0.00442(7) N1 0.0311(10) 0.0242(10) 0.0288(10) 0.0042(8) -0.0051(8) -0.0045(8) N2 0.0282(9) 0.0240(9) 0.0198(9) -0.0002(7) -0.0003(7) -0.0030(7) N3 0.0350(10) 0.0208(9) 0.0221(9) -0.0018(7) -0.0001(8) 0.0022(7) N4 0.0353(10) 0.0239(10) 0.0208(9) -0.0004(7) -0.0010(8) 0.0027(7) C1 0.0457(15) 0.0380(14) 0.0342(14) 0.0042(11) -0.0016(12) 0.0195(11) C2 0.0613(18) 0.0250(13) 0.0503(16) -0.0026(12) 0.0153(14) 0.0114(12) C3 0.078(2) 0.0469(17) 0.069(2) -0.0308(15) 0.0092(17) 0.0069(15) C4 0.074(2) 0.110(3) 0.0460(18) -0.0508(19) -0.0142(16) 0.037(2) C5 0.064(2) 0.082(2) 0.0190(12) -0.0032(13) 0.0010(12) 0.0356(18) C6 0.0561(18) 0.0569(19) 0.0365(15) 0.0167(13) 0.0193(13) 0.0266(15) C7 0.0464(16) 0.0586(19) 0.0629(19) 0.0069(15) 0.0221(14) 0.0104(13) C8 0.0366(15) 0.0667(19) 0.0525(18) -0.0056(14) 0.0003(13) 0.0124(13) C9 0.0244(10) 0.0201(10) 0.0209(10) 0.0020(8) -0.0017(8) -0.0006(8) C10 0.0312(12) 0.0442(14) 0.0244(12) 0.0058(10) 0.0036(9) -0.0057(10) C11 0.0316(12) 0.0368(13) 0.0208(11) -0.0007(9) 0.0027(9) -0.0004(10) C12 0.0599(16) 0.0229(12) 0.0455(15) 0.0080(10) 0.0032(13) -0.0078(11) C13 0.0338(12) 0.0197(10) 0.0234(11) -0.0012(8) 0.0001(9) -0.0035(9) C14 0.0485(14) 0.0215(12) 0.0394(14) -0.0001(10) 0.0009(11) 0.0102(10) C15 0.0597(17) 0.0323(14) 0.0411(15) 0.0044(11) -0.0118(13) 0.0159(12) C16 0.0475(14) 0.0303(13) 0.0282(12) 0.0037(10) -0.0091(11) 0.0055(11) C17 0.0196(10) 0.0172(10) 0.0254(10) 0.0009(8) 0.0023(8) -0.0050(8) C18 0.0285(11) 0.0249(11) 0.0292(11) 0.0060(9) 0.0036(9) 0.0060(9) C19 0.0387(13) 0.0340(13) 0.0241(11) 0.0033(9) 0.0052(10) 0.0051(10) C20 0.0354(12) 0.0262(12) 0.0306(12) -0.0031(9) 0.0114(10) 0.0023(9) C21 0.0251(11) 0.0264(12) 0.0388(13) -0.0003(10) 0.0049(10) 0.0050(9) C22 0.0242(11) 0.0277(11) 0.0259(11) -0.0015(9) -0.0016(9) -0.0003(9) C23 0.0259(11) 0.0221(11) 0.0186(10) 0.0034(8) -0.0062(8) -0.0013(8) C24 0.0322(12) 0.0341(13) 0.0230(11) -0.0004(9) -0.0023(9) -0.0072(10) C25 0.0426(14) 0.0479(16) 0.0277(12) 0.0113(11) -0.0099(11) -0.0259(12) C26 0.0719(19) 0.0240(13) 0.0384(14) 0.0078(11) -0.0263(13) -0.0179(13) C27 0.0559(17) 0.0221(13) 0.0495(16) -0.0051(10) -0.0194(13) 0.0011(11) C28 0.0316(12) 0.0260(12) 0.0410(13) -0.0046(10) -0.0061(10) 0.0000(9) C29 0.0186(10) 0.0226(11) 0.0258(11) 0.0001(8) -0.0001(8) -0.0004(8) C30 0.0417(14) 0.0264(12) 0.0286(13) -0.0011(9) -0.0030(10) -0.0019(10) C31 0.0615(17) 0.0437(15) 0.0225(12) 0.0007(10) -0.0055(11) -0.0063(12) C32 0.0431(14) 0.0436(15) 0.0291(13) 0.0140(11) -0.0028(11) -0.0053(11) C33 0.0275(11) 0.0274(12) 0.0373(13) 0.0097(10) -0.0011(10) -0.0012(9) C34 0.0231(11) 0.0251(11) 0.0276(11) 0.0000(9) -0.0012(9) -0.0003(8) C35 0.0230(10) 0.0189(10) 0.0187(10) -0.0058(8) 0.0003(8) 0.0022(8) C36 0.0245(10) 0.0257(11) 0.0187(10) -0.0011(8) 0.0008(8) 0.0010(8) C37 0.0236(11) 0.0397(13) 0.0246(11) -0.0007(10) 0.0040(9) -0.0036(9) C38 0.0201(11) 0.0433(14) 0.0240(11) -0.0070(10) -0.0014(9) 0.0056(9) C39 0.0318(12) 0.0286(12) 0.0201(10) -0.0024(9) -0.0015(9) 0.0113(9) C40 0.0278(11) 0.0222(11) 0.0232(10) -0.0024(8) 0.0033(9) 0.0025(8) B1 0.0212(12) 0.0181(11) 0.0238(13) -0.0005(9) -0.0005(10) -0.0016(9) _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 C9 2.053(2) . ? Rh1 N4 2.0962(19) . ? Rh1 C1 2.127(2) . ? Rh1 C2 2.147(3) . ? Rh1 C5 2.175(3) . ? Rh1 C6 2.193(3) . ? N1 C9 1.353(3) . ? N1 C10 1.380(3) . ? N1 C12 1.460(3) . ? N2 C9 1.355(2) . ? N2 C11 1.379(3) . ? N2 C13 1.450(3) . ? N3 C14 1.340(3) . ? N3 N4 1.360(2) . ? N3 C13 1.444(3) . ? N4 C16 1.331(3) . ? C1 C2 1.377(4) . ? C1 C8 1.503(4) . ? C1 H1 0.93(2) . ? C2 C3 1.512(4) . ? C2 H2 0.96(3) . ? C3 C4 1.507(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.524(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.358(4) . ? C5 H5 0.99(3) . ? C6 C7 1.510(4) . ? C6 H6 0.98(2) . ? C7 C8 1.506(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C10 C11 1.335(3) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.362(3) . ? C14 H14 0.9500 . ? C15 C16 1.384(3) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C18 1.397(3) . ? C17 C22 1.406(3) . ? C17 B1 1.654(3) . ? C18 C19 1.384(3) . ? C18 H18 0.9500 . ? C19 C20 1.380(3) . ? C19 H19 0.9500 . ? C20 C21 1.379(3) . ? C20 H20 0.9500 . ? C21 C22 1.386(3) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.390(3) . ? C23 C28 1.399(3) . ? C23 B1 1.642(3) . ? C24 C25 1.400(3) . ? C24 H24 0.9500 . ? C25 C26 1.378(4) . ? C25 H25 0.9500 . ? C26 C27 1.366(4) . ? C26 H26 0.9500 . ? C27 C28 1.387(3) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C30 1.395(3) . ? C29 C34 1.404(3) . ? C29 B1 1.645(3) . ? C30 C31 1.392(3) . ? C30 H30 0.9500 . ? C31 C32 1.374(3) . ? C31 H31 0.9500 . ? C32 C33 1.384(3) . ? C32 H32 0.9500 . ? C33 C34 1.383(3) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 C36 1.398(3) . ? C35 C40 1.406(3) . ? C35 B1 1.656(3) . ? C36 C37 1.388(3) . ? C36 H36 0.9500 . ? C37 C38 1.380(3) . ? C37 H37 0.9500 . ? C38 C39 1.380(3) . ? C38 H38 0.9500 . ? C39 C40 1.385(3) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C9 Rh1 N4 85.14(7) . . ? C9 Rh1 C1 92.46(9) . . ? N4 Rh1 C1 152.70(9) . . ? C9 Rh1 C2 99.38(9) . . ? N4 Rh1 C2 169.16(9) . . ? C1 Rh1 C2 37.59(10) . . ? C9 Rh1 C5 165.27(10) . . ? N4 Rh1 C5 91.58(9) . . ? C1 Rh1 C5 96.92(10) . . ? C2 Rh1 C5 81.56(11) . . ? C9 Rh1 C6 157.83(10) . . ? N4 Rh1 C6 90.85(9) . . ? C1 Rh1 C6 81.19(10) . . ? C2 Rh1 C6 88.53(11) . . ? C5 Rh1 C6 36.22(11) . . ? C9 N1 C10 111.75(18) . . ? C9 N1 C12 125.60(19) . . ? C10 N1 C12 122.62(19) . . ? C9 N2 C11 112.57(17) . . ? C9 N2 C13 121.20(17) . . ? C11 N2 C13 126.01(17) . . ? C14 N3 N4 111.64(17) . . ? C14 N3 C13 129.72(18) . . ? N4 N3 C13 118.63(16) . . ? C16 N4 N3 104.56(17) . . ? C16 N4 Rh1 135.22(15) . . ? N3 N4 Rh1 119.96(12) . . ? C2 C1 C8 126.0(3) . . ? C2 C1 Rh1 71.98(15) . . ? C8 C1 Rh1 108.93(17) . . ? C2 C1 H1 115.9(13) . . ? C8 C1 H1 114.8(13) . . ? Rh1 C1 H1 107.3(13) . . ? C1 C2 C3 125.1(3) . . ? C1 C2 Rh1 70.43(14) . . ? C3 C2 Rh1 112.83(19) . . ? C1 C2 H2 114.6(16) . . ? C3 C2 H2 116.5(16) . . ? Rh1 C2 H2 105.2(16) . . ? C4 C3 C2 112.9(2) . . ? C4 C3 H3A 109.0 . . ? C2 C3 H3A 109.0 . . ? C4 C3 H3B 109.0 . . ? C2 C3 H3B 109.0 . . ? H3A C3 H3B 107.8 . . ? C3 C4 C5 113.9(2) . . ? C3 C4 H4A 108.8 . . ? C5 C4 H4A 108.8 . . ? C3 C4 H4B 108.8 . . ? C5 C4 H4B 108.8 . . ? H4A C4 H4B 107.7 . . ? C6 C5 C4 125.6(3) . . ? C6 C5 Rh1 72.62(15) . . ? C4 C5 Rh1 107.44(19) . . ? C6 C5 H5 116.9(15) . . ? C4 C5 H5 115.8(15) . . ? Rh1 C5 H5 103.1(15) . . ? C5 C6 C7 125.0(3) . . ? C5 C6 Rh1 71.16(16) . . ? C7 C6 Rh1 111.44(17) . . ? C5 C6 H6 114.7(15) . . ? C7 C6 H6 118.0(16) . . ? Rh1 C6 H6 101.2(16) . . ? C8 C7 C6 112.2(2) . . ? C8 C7 H7A 109.2 . . ? C6 C7 H7A 109.2 . . ? C8 C7 H7B 109.2 . . ? C6 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? C1 C8 C7 114.1(2) . . ? C1 C8 H8A 108.7 . . ? C7 C8 H8A 108.7 . . ? C1 C8 H8B 108.7 . . ? C7 C8 H8B 108.7 . . ? H8A C8 H8B 107.6 . . ? N1 C9 N2 102.79(18) . . ? N1 C9 Rh1 137.93(15) . . ? N2 C9 Rh1 118.92(14) . . ? C11 C10 N1 107.11(19) . . ? C11 C10 H10 126.4 . . ? N1 C10 H10 126.4 . . ? C10 C11 N2 105.77(19) . . ? C10 C11 H11 127.1 . . ? N2 C11 H11 127.1 . . ? N1 C12 H12A 109.5 . . ? N1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N3 C13 N2 109.15(15) . . ? N3 C13 H13A 109.8 . . ? N2 C13 H13A 109.8 . . ? N3 C13 H13B 109.8 . . ? N2 C13 H13B 109.8 . . ? H13A C13 H13B 108.3 . . ? N3 C14 C15 107.0(2) . . ? N3 C14 H14 126.5 . . ? C15 C14 H14 126.5 . . ? C14 C15 C16 105.7(2) . . ? C14 C15 H15 127.1 . . ? C16 C15 H15 127.1 . . ? N4 C16 C15 111.1(2) . . ? N4 C16 H16 124.4 . . ? C15 C16 H16 124.4 . . ? C18 C17 C22 113.97(18) . . ? C18 C17 B1 123.05(17) . . ? C22 C17 B1 122.96(17) . . ? C19 C18 C17 123.6(2) . . ? C19 C18 H18 118.2 . . ? C17 C18 H18 118.2 . . ? C20 C19 C18 120.1(2) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C21 C20 C19 118.8(2) . . ? C21 C20 H20 120.6 . . ? C19 C20 H20 120.6 . . ? C20 C21 C22 120.1(2) . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C21 C22 C17 123.41(19) . . ? C21 C22 H22 118.3 . . ? C17 C22 H22 118.3 . . ? C24 C23 C28 114.86(19) . . ? C24 C23 B1 123.23(19) . . ? C28 C23 B1 121.91(19) . . ? C23 C24 C25 122.2(2) . . ? C23 C24 H24 118.9 . . ? C25 C24 H24 118.9 . . ? C26 C25 C24 120.5(2) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C27 C26 C25 119.0(2) . . ? C27 C26 H26 120.5 . . ? C25 C26 H26 120.5 . . ? C26 C27 C28 120.0(2) . . ? C26 C27 H27 120.0 . . ? C28 C27 H27 120.0 . . ? C27 C28 C23 123.4(2) . . ? C27 C28 H28 118.3 . . ? C23 C28 H28 118.3 . . ? C30 C29 C34 114.84(19) . . ? C30 C29 B1 123.04(18) . . ? C34 C29 B1 122.09(17) . . ? C31 C30 C29 122.4(2) . . ? C31 C30 H30 118.8 . . ? C29 C30 H30 118.8 . . ? C32 C31 C30 120.8(2) . . ? C32 C31 H31 119.6 . . ? C30 C31 H31 119.6 . . ? C31 C32 C33 118.9(2) . . ? C31 C32 H32 120.6 . . ? C33 C32 H32 120.6 . . ? C34 C33 C32 119.7(2) . . ? C34 C33 H33 120.2 . . ? C32 C33 H33 120.2 . . ? C33 C34 C29 123.4(2) . . ? C33 C34 H34 118.3 . . ? C29 C34 H34 118.3 . . ? C36 C35 C40 114.48(18) . . ? C36 C35 B1 124.08(17) . . ? C40 C35 B1 121.39(18) . . ? C37 C36 C35 123.09(19) . . ? C37 C36 H36 118.5 . . ? C35 C36 H36 118.5 . . ? C38 C37 C36 120.4(2) . . ? C38 C37 H37 119.8 . . ? C36 C37 H37 119.8 . . ? C39 C38 C37 118.58(19) . . ? C39 C38 H38 120.7 . . ? C37 C38 H38 120.7 . . ? C38 C39 C40 120.45(19) . . ? C38 C39 H39 119.8 . . ? C40 C39 H39 119.8 . . ? C39 C40 C35 122.98(19) . . ? C39 C40 H40 118.5 . . ? C35 C40 H40 118.5 . . ? C23 B1 C29 110.91(16) . . ? C23 B1 C17 109.27(17) . . ? C29 B1 C17 110.35(16) . . ? C23 B1 C35 108.47(15) . . ? C29 B1 C35 109.74(17) . . ? C17 B1 C35 108.03(15) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C14 N3 N4 C16 0.5(2) . . . . ? C13 N3 N4 C16 179.48(18) . . . . ? C14 N3 N4 Rh1 -174.56(14) . . . . ? C13 N3 N4 Rh1 4.4(2) . . . . ? C9 Rh1 N4 C16 -134.6(2) . . . . ? C1 Rh1 N4 C16 139.5(2) . . . . ? C2 Rh1 N4 C16 -19.3(6) . . . . ? C5 Rh1 N4 C16 31.0(2) . . . . ? C6 Rh1 N4 C16 67.3(2) . . . . ? C9 Rh1 N4 N3 38.59(15) . . . . ? C1 Rh1 N4 N3 -47.4(3) . . . . ? C2 Rh1 N4 N3 153.8(5) . . . . ? C5 Rh1 N4 N3 -155.79(17) . . . . ? C6 Rh1 N4 N3 -119.57(17) . . . . ? C9 Rh1 C1 C2 102.21(17) . . . . ? N4 Rh1 C1 C2 -173.60(17) . . . . ? C5 Rh1 C1 C2 -66.41(18) . . . . ? C6 Rh1 C1 C2 -99.14(18) . . . . ? C9 Rh1 C1 C8 -134.92(18) . . . . ? N4 Rh1 C1 C8 -50.7(3) . . . . ? C2 Rh1 C1 C8 122.9(3) . . . . ? C5 Rh1 C1 C8 56.5(2) . . . . ? C6 Rh1 C1 C8 23.72(19) . . . . ? C8 C1 C2 C3 4.0(4) . . . . ? Rh1 C1 C2 C3 104.7(3) . . . . ? C8 C1 C2 Rh1 -100.7(2) . . . . ? C9 Rh1 C2 C1 -81.77(17) . . . . ? N4 Rh1 C2 C1 164.2(4) . . . . ? C5 Rh1 C2 C1 113.12(18) . . . . ? C6 Rh1 C2 C1 77.41(18) . . . . ? C9 Rh1 C2 C3 157.4(2) . . . . ? N4 Rh1 C2 C3 43.4(6) . . . . ? C1 Rh1 C2 C3 -120.9(3) . . . . ? C5 Rh1 C2 C3 -7.7(2) . . . . ? C6 Rh1 C2 C3 -43.4(2) . . . . ? C1 C2 C3 C4 -92.0(3) . . . . ? Rh1 C2 C3 C4 -10.5(3) . . . . ? C2 C3 C4 C5 32.3(4) . . . . ? C3 C4 C5 C6 43.7(4) . . . . ? C3 C4 C5 Rh1 -37.1(3) . . . . ? C9 Rh1 C5 C6 166.1(3) . . . . ? N4 Rh1 C5 C6 89.28(17) . . . . ? C1 Rh1 C5 C6 -64.73(18) . . . . ? C2 Rh1 C5 C6 -99.14(18) . . . . ? C9 Rh1 C5 C4 -71.1(4) . . . . ? N4 Rh1 C5 C4 -147.9(2) . . . . ? C1 Rh1 C5 C4 58.0(2) . . . . ? C2 Rh1 C5 C4 23.6(2) . . . . ? C6 Rh1 C5 C4 122.8(3) . . . . ? C4 C5 C6 C7 4.1(4) . . . . ? Rh1 C5 C6 C7 103.4(2) . . . . ? C4 C5 C6 Rh1 -99.3(3) . . . . ? C9 Rh1 C6 C5 -170.7(2) . . . . ? N4 Rh1 C6 C5 -91.51(17) . . . . ? C1 Rh1 C6 C5 114.71(18) . . . . ? C2 Rh1 C6 C5 77.67(18) . . . . ? C9 Rh1 C6 C7 68.1(3) . . . . ? N4 Rh1 C6 C7 147.3(2) . . . . ? C1 Rh1 C6 C7 -6.5(2) . . . . ? C2 Rh1 C6 C7 -43.5(2) . . . . ? C5 Rh1 C6 C7 -121.2(3) . . . . ? C5 C6 C7 C8 -93.9(3) . . . . ? Rh1 C6 C7 C8 -12.4(3) . . . . ? C2 C1 C8 C7 42.3(4) . . . . ? Rh1 C1 C8 C7 -38.8(3) . . . . ? C6 C7 C8 C1 34.1(3) . . . . ? C10 N1 C9 N2 0.3(2) . . . . ? C12 N1 C9 N2 -177.87(18) . . . . ? C10 N1 C9 Rh1 -172.26(16) . . . . ? C12 N1 C9 Rh1 9.6(3) . . . . ? C11 N2 C9 N1 -0.8(2) . . . . ? C13 N2 C9 N1 -175.81(16) . . . . ? C11 N2 C9 Rh1 173.50(13) . . . . ? C13 N2 C9 Rh1 -1.5(2) . . . . ? N4 Rh1 C9 N1 132.2(2) . . . . ? C1 Rh1 C9 N1 -75.0(2) . . . . ? C2 Rh1 C9 N1 -37.9(2) . . . . ? C5 Rh1 C9 N1 54.6(5) . . . . ? C6 Rh1 C9 N1 -147.5(2) . . . . ? N4 Rh1 C9 N2 -39.51(15) . . . . ? C1 Rh1 C9 N2 113.24(16) . . . . ? C2 Rh1 C9 N2 150.42(16) . . . . ? C5 Rh1 C9 N2 -117.1(4) . . . . ? C6 Rh1 C9 N2 40.7(3) . . . . ? C9 N1 C10 C11 0.3(2) . . . . ? C12 N1 C10 C11 178.54(19) . . . . ? N1 C10 C11 N2 -0.8(2) . . . . ? C9 N2 C11 C10 1.0(2) . . . . ? C13 N2 C11 C10 175.72(18) . . . . ? C14 N3 C13 N2 117.3(2) . . . . ? N4 N3 C13 N2 -61.5(2) . . . . ? C9 N2 C13 N3 61.1(2) . . . . ? C11 N2 C13 N3 -113.1(2) . . . . ? N4 N3 C14 C15 -0.6(3) . . . . ? C13 N3 C14 C15 -179.4(2) . . . . ? N3 C14 C15 C16 0.4(3) . . . . ? N3 N4 C16 C15 -0.2(3) . . . . ? Rh1 N4 C16 C15 173.68(17) . . . . ? C14 C15 C16 N4 -0.1(3) . . . . ? C22 C17 C18 C19 0.9(3) . . . . ? B1 C17 C18 C19 179.28(19) . . . . ? C17 C18 C19 C20 0.0(3) . . . . ? C18 C19 C20 C21 -0.9(3) . . . . ? C19 C20 C21 C22 0.7(3) . . . . ? C20 C21 C22 C17 0.3(3) . . . . ? C18 C17 C22 C21 -1.0(3) . . . . ? B1 C17 C22 C21 -179.44(19) . . . . ? C28 C23 C24 C25 -2.0(3) . . . . ? B1 C23 C24 C25 177.14(18) . . . . ? C23 C24 C25 C26 0.1(3) . . . . ? C24 C25 C26 C27 1.3(3) . . . . ? C25 C26 C27 C28 -0.7(3) . . . . ? C26 C27 C28 C23 -1.4(4) . . . . ? C24 C23 C28 C27 2.7(3) . . . . ? B1 C23 C28 C27 -176.5(2) . . . . ? C34 C29 C30 C31 0.4(3) . . . . ? B1 C29 C30 C31 178.5(2) . . . . ? C29 C30 C31 C32 0.1(4) . . . . ? C30 C31 C32 C33 -0.3(4) . . . . ? C31 C32 C33 C34 0.0(3) . . . . ? C32 C33 C34 C29 0.4(3) . . . . ? C30 C29 C34 C33 -0.6(3) . . . . ? B1 C29 C34 C33 -178.79(19) . . . . ? C40 C35 C36 C37 2.0(3) . . . . ? B1 C35 C36 C37 -175.33(19) . . . . ? C35 C36 C37 C38 -1.3(3) . . . . ? C36 C37 C38 C39 -0.3(3) . . . . ? C37 C38 C39 C40 1.1(3) . . . . ? C38 C39 C40 C35 -0.3(3) . . . . ? C36 C35 C40 C39 -1.2(3) . . . . ? B1 C35 C40 C39 176.21(18) . . . . ? C24 C23 B1 C29 97.4(2) . . . . ? C28 C23 B1 C29 -83.5(2) . . . . ? C24 C23 B1 C17 -24.5(2) . . . . ? C28 C23 B1 C17 154.64(18) . . . . ? C24 C23 B1 C35 -142.03(19) . . . . ? C28 C23 B1 C35 37.1(2) . . . . ? C30 C29 B1 C23 18.0(3) . . . . ? C34 C29 B1 C23 -163.97(18) . . . . ? C30 C29 B1 C17 139.2(2) . . . . ? C34 C29 B1 C17 -42.7(2) . . . . ? C30 C29 B1 C35 -101.8(2) . . . . ? C34 C29 B1 C35 76.2(2) . . . . ? C18 C17 B1 C23 -82.8(2) . . . . ? C22 C17 B1 C23 95.4(2) . . . . ? C18 C17 B1 C29 154.96(18) . . . . ? C22 C17 B1 C29 -26.8(2) . . . . ? C18 C17 B1 C35 35.0(2) . . . . ? C22 C17 B1 C35 -146.74(18) . . . . ? C36 C35 B1 C23 -142.99(19) . . . . ? C40 C35 B1 C23 39.8(2) . . . . ? C36 C35 B1 C29 -21.7(3) . . . . ? C40 C35 B1 C29 161.12(17) . . . . ? C36 C35 B1 C17 98.7(2) . . . . ? C40 C35 B1 C17 -78.5(2) . . . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.802 _refine_diff_density_min -0.488 _refine_diff_density_rms 0.067