# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name B.Messerle L.Field P.Turner K.Q.Vuong _publ_contact_author_name 'Barbara Messerle' _publ_contact_author_email B.MESSERLE@UNSW.EDU.AU data_bam10 _database_code_depnum_ccdc_archive 'CCDC 711455' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H49 B Ir N2 P' _chemical_formula_weight 899.88 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' P P 0.1023 0.0942 '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/c ' _symmetry_Int_Tables_number 14 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 13.971(3) _cell_length_b 9.6981(18) _cell_length_c 29.840(6) _cell_angle_alpha 90.00 _cell_angle_beta 96.844(3) _cell_angle_gamma 90.00 _cell_volume 4014.3(13) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1000 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 28.2 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.326 _exptl_crystal_size_mid 0.145 _exptl_crystal_size_min 0.139 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.489 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1816 _exptl_absorpt_coefficient_mu 3.403 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.414 _exptl_absorpt_correction_T_max 0.651 _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 383 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.04 _diffrn_reflns_number 39147 _diffrn_reflns_av_R_equivalents 0.0389 _diffrn_reflns_av_sigmaI/netI 0.0241 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 28.29 _reflns_number_total 9556 _reflns_number_gt 8112 _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^)+(0.02P)^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 9556 _refine_ls_number_parameters 504 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0315 _refine_ls_R_factor_gt 0.0243 _refine_ls_wR_factor_ref 0.0528 _refine_ls_wR_factor_gt 0.0515 _refine_ls_goodness_of_fit_ref 1.316 _refine_ls_restrained_S_all 1.316 _refine_ls_shift/su_max 0.004 _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 0.356213(7) 0.274957(10) 0.351683(3) 0.02767(4) Uani 1 1 d . . . P1 P 0.29016(4) 0.41631(6) 0.40051(2) 0.02432(13) Uani 1 1 d . . . N1 N 0.30353(14) 0.4241(2) 0.30608(6) 0.0292(5) Uani 1 1 d . . . N2 N 0.22315(14) 0.6128(2) 0.28429(6) 0.0270(4) Uani 1 1 d . . . C1 C 0.46710(19) 0.1994(3) 0.31159(9) 0.0351(6) Uani 1 1 d . . . H1 H 0.485(2) 0.275(3) 0.2931(10) 0.040(8) Uiso 1 1 d . . . C2 C 0.3848(2) 0.1239(3) 0.29965(10) 0.0426(7) Uani 1 1 d . . . H2 H 0.3461(19) 0.150(3) 0.2738(9) 0.040(8) Uiso 1 1 d . . . C3 C 0.3690(3) -0.0209(3) 0.31568(12) 0.0661(10) Uani 1 1 d . . . H3A H 0.3181 -0.0642 0.2943 0.079 Uiso 1 1 calc R . . H3B H 0.4290 -0.0740 0.3142 0.079 Uiso 1 1 calc R . . C4 C 0.3414(4) -0.0346(4) 0.36151(14) 0.0956(15) Uani 1 1 d . . . H4A H 0.3807 -0.1092 0.3771 0.115 Uiso 1 1 calc R . . H4B H 0.2732 -0.0641 0.3590 0.115 Uiso 1 1 calc R . . C5 C 0.3525(3) 0.0910(3) 0.39030(11) 0.0504(8) Uani 1 1 d . . . H5 H 0.306(2) 0.099(3) 0.4116(10) 0.047(9) Uiso 1 1 d . . . C6 C 0.4396(2) 0.1590(4) 0.40280(10) 0.0509(9) Uani 1 1 d . . . H6 H 0.448(2) 0.211(3) 0.4290(11) 0.053(9) Uiso 1 1 d . . . C7 C 0.5352(2) 0.1099(5) 0.38881(12) 0.0876(15) Uani 1 1 d . . . H7A H 0.5880 0.1464 0.4107 0.105 Uiso 1 1 calc R . . H7B H 0.5374 0.0080 0.3908 0.105 Uiso 1 1 calc R . . C8 C 0.5534(2) 0.1507(3) 0.34303(11) 0.0488(8) Uani 1 1 d . . . H8A H 0.5821 0.0710 0.3288 0.059 Uiso 1 1 calc R . . H8B H 0.6020 0.2254 0.3458 0.059 Uiso 1 1 calc R . . C9 C 0.31641(18) 0.4524(3) 0.26174(8) 0.0372(6) Uani 1 1 d . . . H9 H 0.3540 0.3991 0.2436 0.045 Uiso 1 1 calc R . . C10 C 0.26725(18) 0.5676(3) 0.24831(9) 0.0362(6) Uani 1 1 d . . . H10 H 0.2638 0.6096 0.2194 0.043 Uiso 1 1 calc R . . C11 C 0.24515(16) 0.5248(2) 0.31839(8) 0.0243(5) Uani 1 1 d . . . C12 C 0.21022(16) 0.5311(2) 0.36349(7) 0.0239(5) Uani 1 1 d . . . H12A H 0.1425 0.4992 0.3616 0.029 Uiso 1 1 calc R . . H12B H 0.2138 0.6267 0.3752 0.029 Uiso 1 1 calc R . . C13 C 0.15539(19) 0.7283(2) 0.28425(9) 0.0314(6) Uani 1 1 d . . . H13A H 0.1637 0.7735 0.3138 0.047 Uiso 1 1 calc R . . H13B H 0.0892 0.6938 0.2779 0.047 Uiso 1 1 calc R . . H13C H 0.1680 0.7949 0.2609 0.047 Uiso 1 1 calc R . . C14 C 0.21741(17) 0.3390(2) 0.43998(8) 0.0273(5) Uani 1 1 d . . . C15 C 0.13700(19) 0.2621(3) 0.42262(10) 0.0362(6) Uani 1 1 d . . . H15 H 0.1186 0.2588 0.3909 0.043 Uiso 1 1 calc R . . C16 C 0.0840(2) 0.1906(3) 0.45139(11) 0.0447(7) Uani 1 1 d . . . H16 H 0.0287 0.1395 0.4395 0.054 Uiso 1 1 calc R . . C17 C 0.1116(2) 0.1939(3) 0.49715(11) 0.0469(8) Uani 1 1 d . . . H17 H 0.0759 0.1436 0.5168 0.056 Uiso 1 1 calc R . . C18 C 0.1905(2) 0.2693(3) 0.51459(10) 0.0499(8) Uani 1 1 d . . . H18 H 0.2086 0.2718 0.5463 0.060 Uiso 1 1 calc R . . C19 C 0.2439(2) 0.3420(3) 0.48613(9) 0.0379(6) Uani 1 1 d . . . H19 H 0.2986 0.3938 0.4983 0.045 Uiso 1 1 calc R . . C20 C 0.37454(17) 0.5367(3) 0.43028(8) 0.0299(5) Uani 1 1 d . . . C21 C 0.3438(2) 0.6386(3) 0.45822(9) 0.0399(7) Uani 1 1 d . . . H21 H 0.2790 0.6399 0.4648 0.048 Uiso 1 1 calc R . . C22 C 0.4085(2) 0.7385(3) 0.47647(11) 0.0527(8) Uani 1 1 d . . . H22 H 0.3882 0.8073 0.4959 0.063 Uiso 1 1 calc R . . C23 C 0.5031(2) 0.7374(4) 0.46616(11) 0.0578(9) Uani 1 1 d . . . H23 H 0.5472 0.8060 0.4784 0.069 Uiso 1 1 calc R . . C24 C 0.5328(2) 0.6379(4) 0.43849(10) 0.0557(9) Uani 1 1 d . . . H24 H 0.5973 0.6383 0.4315 0.067 Uiso 1 1 calc R . . C25 C 0.46949(18) 0.5362(3) 0.42049(9) 0.0410(7) Uani 1 1 d . . . H25 H 0.4909 0.4666 0.4016 0.049 Uiso 1 1 calc R . . C26 C 0.95259(16) 0.5997(2) 0.38414(8) 0.0221(5) Uani 1 1 d . . . C27 C 0.98198(18) 0.7285(2) 0.36902(8) 0.0275(5) Uani 1 1 d . . . H27 H 0.9554 0.7596 0.3400 0.033 Uiso 1 1 calc R . . C28 C 1.04835(18) 0.8127(3) 0.39470(8) 0.0311(6) Uani 1 1 d . . . H28 H 1.0654 0.8997 0.3833 0.037 Uiso 1 1 calc R . . C29 C 1.08940(18) 0.7692(2) 0.43688(9) 0.0316(6) Uani 1 1 d . . . H29 H 1.1344 0.8261 0.4547 0.038 Uiso 1 1 calc R . . C30 C 1.06410(17) 0.6420(3) 0.45263(8) 0.0293(5) Uani 1 1 d . . . H30 H 1.0923 0.6105 0.4814 0.035 Uiso 1 1 calc R . . C31 C 0.99751(16) 0.5599(2) 0.42661(8) 0.0249(5) Uani 1 1 d . . . H31 H 0.9817 0.4726 0.4382 0.030 Uiso 1 1 calc R . . C32 C 0.85496(16) 0.3556(2) 0.37399(8) 0.0225(5) Uani 1 1 d . . . C33 C 0.81644(17) 0.3484(2) 0.41558(8) 0.0290(5) Uani 1 1 d . . . H33 H 0.8048 0.4319 0.4307 0.035 Uiso 1 1 calc R . . C34 C 0.79497(19) 0.2246(3) 0.43520(9) 0.0330(6) Uani 1 1 d . . . H34 H 0.7698 0.2247 0.4634 0.040 Uiso 1 1 calc R . . C35 C 0.80982(18) 0.1009(3) 0.41422(9) 0.0319(6) Uani 1 1 d . . . H35 H 0.7949 0.0159 0.4276 0.038 Uiso 1 1 calc R . . C36 C 0.84686(17) 0.1034(2) 0.37331(9) 0.0312(6) Uani 1 1 d . . . H36 H 0.8571 0.0193 0.3583 0.037 Uiso 1 1 calc R . . C37 C 0.86923(17) 0.2279(2) 0.35401(8) 0.0259(5) Uani 1 1 d . . . H37 H 0.8953 0.2262 0.3260 0.031 Uiso 1 1 calc R . . C38 C 0.91175(16) 0.5003(2) 0.30215(8) 0.0223(5) Uani 1 1 d . . . C39 C 0.99453(16) 0.4256(2) 0.29480(8) 0.0258(5) Uani 1 1 d . . . H39 H 1.0261 0.3725 0.3189 0.031 Uiso 1 1 calc R . . C40 C 1.03237(18) 0.4257(2) 0.25380(8) 0.0311(6) Uani 1 1 d . . . H40 H 1.0884 0.3732 0.2504 0.037 Uiso 1 1 calc R . . C41 C 0.9887(2) 0.5022(2) 0.21803(9) 0.0356(6) Uani 1 1 d . . . H41 H 1.0144 0.5031 0.1900 0.043 Uiso 1 1 calc R . . C42 C 0.90700(19) 0.5776(3) 0.22370(8) 0.0333(6) Uani 1 1 d . . . H42 H 0.8761 0.6305 0.1994 0.040 Uiso 1 1 calc R . . C43 C 0.86997(18) 0.5762(2) 0.26475(8) 0.0270(5) Uani 1 1 d . . . H43 H 0.8138 0.6290 0.2677 0.032 Uiso 1 1 calc R . . C44 C 0.76569(17) 0.5822(2) 0.34564(8) 0.0248(5) Uani 1 1 d . . . C45 C 0.68605(18) 0.5094(3) 0.32450(9) 0.0357(6) Uani 1 1 d . . . H45 H 0.6950 0.4165 0.3158 0.043 Uiso 1 1 calc R . . C46 C 0.59531(19) 0.5667(3) 0.31574(10) 0.0458(7) Uani 1 1 d . . . H46 H 0.5434 0.5134 0.3014 0.055 Uiso 1 1 calc R . . C47 C 0.5803(2) 0.7015(3) 0.32788(11) 0.0511(8) Uani 1 1 d . . . H47 H 0.5182 0.7419 0.3219 0.061 Uiso 1 1 calc R . . C48 C 0.6561(2) 0.7766(3) 0.34878(11) 0.0471(8) Uani 1 1 d . . . H48 H 0.6463 0.8694 0.3574 0.057 Uiso 1 1 calc R . . C49 C 0.74715(19) 0.7175(2) 0.35735(9) 0.0328(6) Uani 1 1 d . . . H49 H 0.7986 0.7717 0.3717 0.039 Uiso 1 1 calc R . . B1 B 0.87243(18) 0.5076(3) 0.35183(9) 0.0221(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 Ir1 0.02557(5) 0.03492(6) 0.02234(5) 0.00053(4) 0.00210(4) 0.01164(4) P1 0.0222(3) 0.0319(3) 0.0187(3) 0.0021(2) 0.0020(2) 0.0058(2) N1 0.0255(11) 0.0429(13) 0.0192(11) 0.0012(9) 0.0029(8) 0.0095(9) N2 0.0252(11) 0.0315(11) 0.0241(11) 0.0063(9) 0.0025(8) 0.0017(8) C1 0.0333(15) 0.0384(17) 0.0352(15) -0.0004(12) 0.0113(12) 0.0122(12) C2 0.0443(18) 0.0486(18) 0.0347(17) -0.0130(14) 0.0039(14) 0.0080(14) C3 0.078(3) 0.053(2) 0.068(3) -0.0208(18) 0.012(2) -0.0130(18) C4 0.172(5) 0.035(2) 0.080(3) 0.004(2) 0.018(3) 0.013(2) C5 0.063(2) 0.0424(18) 0.046(2) 0.0114(15) 0.0074(17) 0.0219(16) C6 0.056(2) 0.068(2) 0.0283(16) 0.0055(15) 0.0054(14) 0.0387(18) C7 0.055(2) 0.159(4) 0.049(2) 0.009(2) 0.0048(18) 0.062(3) C8 0.0320(15) 0.0521(19) 0.064(2) 0.0149(16) 0.0116(14) 0.0131(13) C9 0.0356(15) 0.0567(18) 0.0207(13) 0.0032(12) 0.0088(11) 0.0128(13) C10 0.0342(15) 0.0536(17) 0.0220(13) 0.0090(12) 0.0080(11) 0.0041(12) C11 0.0207(12) 0.0300(13) 0.0218(12) 0.0017(10) 0.0015(9) 0.0000(9) C12 0.0241(12) 0.0274(12) 0.0197(12) 0.0002(9) 0.0006(9) 0.0049(9) C13 0.0355(14) 0.0249(12) 0.0328(14) 0.0059(11) 0.0004(11) 0.0030(11) C14 0.0275(13) 0.0295(13) 0.0257(13) 0.0052(10) 0.0071(10) 0.0105(10) C15 0.0347(15) 0.0392(15) 0.0348(15) 0.0059(12) 0.0039(12) 0.0014(11) C16 0.0352(16) 0.0376(16) 0.063(2) 0.0117(14) 0.0131(14) 0.0034(12) C17 0.0494(18) 0.0420(17) 0.055(2) 0.0167(14) 0.0287(16) 0.0117(14) C18 0.064(2) 0.059(2) 0.0295(16) 0.0129(14) 0.0184(15) 0.0089(16) C19 0.0418(16) 0.0445(16) 0.0279(14) 0.0045(12) 0.0060(12) 0.0036(13) C20 0.0258(13) 0.0417(15) 0.0211(13) 0.0047(11) -0.0017(10) 0.0005(11) C21 0.0339(15) 0.0486(17) 0.0365(16) -0.0056(13) 0.0015(12) -0.0026(12) C22 0.051(2) 0.061(2) 0.0445(19) -0.0145(15) -0.0018(15) -0.0098(15) C23 0.049(2) 0.082(2) 0.0404(19) -0.0025(17) -0.0066(15) -0.0287(17) C24 0.0336(16) 0.102(3) 0.0314(17) -0.0001(17) 0.0030(13) -0.0217(17) C25 0.0302(15) 0.066(2) 0.0270(15) 0.0008(13) 0.0032(11) -0.0052(13) C26 0.0246(12) 0.0212(12) 0.0211(12) -0.0015(9) 0.0060(9) 0.0045(9) C27 0.0356(14) 0.0240(11) 0.0224(12) 0.0008(10) 0.0017(10) 0.0015(10) C28 0.0372(14) 0.0242(13) 0.0322(14) -0.0023(10) 0.0059(11) -0.0025(10) C29 0.0290(13) 0.0318(13) 0.0332(14) -0.0093(11) 0.0010(11) -0.0016(10) C30 0.0282(13) 0.0370(15) 0.0222(13) -0.0007(10) 0.0010(10) 0.0053(10) C31 0.0276(13) 0.0242(12) 0.0241(13) 0.0018(10) 0.0076(10) 0.0050(9) C32 0.0238(12) 0.0208(12) 0.0225(12) 0.0000(9) 0.0004(9) 0.0002(9) C33 0.0354(14) 0.0267(14) 0.0257(13) -0.0030(10) 0.0070(11) -0.0022(10) C34 0.0368(14) 0.0382(14) 0.0255(13) 0.0021(11) 0.0094(11) -0.0072(11) C35 0.0347(14) 0.0250(13) 0.0357(15) 0.0081(11) 0.0029(12) -0.0052(10) C36 0.0356(14) 0.0193(13) 0.0397(15) -0.0007(11) 0.0081(12) -0.0003(10) C37 0.0290(13) 0.0233(11) 0.0262(13) 0.0013(10) 0.0065(10) 0.0000(9) C38 0.0279(12) 0.0173(11) 0.0217(12) -0.0034(9) 0.0036(9) -0.0056(9) C39 0.0282(13) 0.0212(12) 0.0281(13) -0.0032(10) 0.0042(10) -0.0060(9) C40 0.0333(14) 0.0258(13) 0.0366(15) -0.0102(11) 0.0144(12) -0.0077(10) C41 0.0556(18) 0.0287(14) 0.0260(14) -0.0091(11) 0.0197(12) -0.0180(12) C42 0.0513(17) 0.0271(13) 0.0212(13) 0.0018(10) 0.0030(12) -0.0093(12) C43 0.0353(14) 0.0222(12) 0.0237(13) -0.0006(10) 0.0036(10) -0.0034(10) C44 0.0299(13) 0.0254(12) 0.0204(12) 0.0062(9) 0.0082(10) 0.0041(10) C45 0.0323(14) 0.0353(15) 0.0399(16) 0.0014(12) 0.0057(12) 0.0029(11) C46 0.0293(15) 0.063(2) 0.0460(18) 0.0126(15) 0.0065(13) 0.0011(13) C47 0.0361(17) 0.062(2) 0.058(2) 0.0281(17) 0.0151(15) 0.0227(15) C48 0.0505(19) 0.0380(15) 0.057(2) 0.0156(15) 0.0222(16) 0.0199(14) C49 0.0393(15) 0.0280(13) 0.0328(14) 0.0078(11) 0.0114(12) 0.0073(11) B1 0.0262(14) 0.0200(13) 0.0210(13) -0.0002(10) 0.0057(11) 0.0025(10) _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 N1 2.061(2) . ? Ir1 C6 2.127(3) . ? Ir1 C5 2.128(3) . ? Ir1 C1 2.193(3) . ? Ir1 C2 2.206(3) . ? Ir1 P1 2.2747(7) . ? P1 C14 1.808(2) . ? P1 C20 1.815(3) . ? P1 C12 1.848(2) . ? N1 C11 1.351(3) . ? N1 C9 1.384(3) . ? N2 C11 1.335(3) . ? N2 C10 1.372(3) . ? N2 C13 1.467(3) . ? C1 C2 1.374(4) . ? C1 C8 1.512(4) . ? C1 H1 0.97(3) . ? C2 C3 1.508(4) . ? C2 H2 0.92(3) . ? C3 C4 1.470(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.487(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.396(5) . ? C5 H5 0.96(3) . ? C6 C7 1.523(4) . ? C6 H6 0.93(3) . ? C7 C8 1.473(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.347(4) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.486(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C19 1.383(3) . ? C14 C15 1.396(4) . ? C15 C16 1.385(4) . ? C15 H15 0.9500 . ? C16 C17 1.374(4) . ? C16 H16 0.9500 . ? C17 C18 1.372(5) . ? C17 H17 0.9500 . ? C18 C19 1.388(4) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C25 1.392(3) . ? C20 C21 1.393(4) . ? C21 C22 1.391(4) . ? C21 H21 0.9500 . ? C22 C23 1.393(5) . ? C22 H22 0.9500 . ? C23 C24 1.366(5) . ? C23 H23 0.9500 . ? C24 C25 1.389(4) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C31 1.400(3) . ? C26 C27 1.406(3) . ? C26 B1 1.650(3) . ? C27 C28 1.394(3) . ? C27 H27 0.9500 . ? C28 C29 1.385(4) . ? C28 H28 0.9500 . ? C29 C30 1.381(3) . ? C29 H29 0.9500 . ? C30 C31 1.389(3) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 C37 1.400(3) . ? C32 C33 1.412(3) . ? C32 B1 1.646(3) . ? C33 C34 1.385(3) . ? C33 H33 0.9500 . ? C34 C35 1.380(3) . ? C34 H34 0.9500 . ? C35 C36 1.382(3) . ? C35 H35 0.9500 . ? C36 C37 1.389(3) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C38 C39 1.404(3) . ? C38 C43 1.405(3) . ? C38 B1 1.643(3) . ? C39 C40 1.389(3) . ? C39 H39 0.9500 . ? C40 C41 1.381(4) . ? C40 H40 0.9500 . ? C41 C42 1.382(4) . ? C41 H41 0.9500 . ? C42 C43 1.385(3) . ? C42 H42 0.9500 . ? C43 H43 0.9500 . ? C44 C49 1.391(3) . ? C44 C45 1.402(3) . ? C44 B1 1.648(3) . ? C45 C46 1.380(3) . ? C45 H45 0.9500 . ? C46 C47 1.380(4) . ? C46 H46 0.9500 . ? C47 C48 1.372(5) . ? C47 H47 0.9500 . ? C48 C49 1.391(4) . ? C48 H48 0.9500 . ? C49 H49 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 N1 Ir1 C6 165.14(13) . . ? N1 Ir1 C5 156.36(12) . . ? C6 Ir1 C5 38.30(13) . . ? N1 Ir1 C1 95.40(9) . . ? C6 Ir1 C1 81.52(11) . . ? C5 Ir1 C1 94.59(12) . . ? N1 Ir1 C2 94.69(10) . . ? C6 Ir1 C2 91.37(12) . . ? C5 Ir1 C2 80.93(13) . . ? C1 Ir1 C2 36.40(10) . . ? N1 Ir1 P1 81.94(6) . . ? C6 Ir1 P1 95.08(8) . . ? C5 Ir1 P1 96.92(9) . . ? C1 Ir1 P1 156.57(8) . . ? C2 Ir1 P1 166.56(8) . . ? C14 P1 C20 109.32(12) . . ? C14 P1 C12 107.02(11) . . ? C20 P1 C12 102.48(11) . . ? C14 P1 Ir1 118.02(8) . . ? C20 P1 Ir1 114.32(8) . . ? C12 P1 Ir1 104.05(7) . . ? C11 N1 C9 105.5(2) . . ? C11 N1 Ir1 120.50(15) . . ? C9 N1 Ir1 133.92(17) . . ? C11 N2 C10 107.9(2) . . ? C11 N2 C13 125.4(2) . . ? C10 N2 C13 126.4(2) . . ? C2 C1 C8 125.1(3) . . ? C2 C1 Ir1 72.30(16) . . ? C8 C1 Ir1 109.19(19) . . ? C2 C1 H1 121.2(17) . . ? C8 C1 H1 110.7(17) . . ? Ir1 C1 H1 107.5(16) . . ? C1 C2 C3 124.3(3) . . ? C1 C2 Ir1 71.30(16) . . ? C3 C2 Ir1 110.4(2) . . ? C1 C2 H2 117.2(18) . . ? C3 C2 H2 115.5(18) . . ? Ir1 C2 H2 105.4(17) . . ? C4 C3 C2 116.3(3) . . ? C4 C3 H3A 108.2 . . ? C2 C3 H3A 108.2 . . ? C4 C3 H3B 108.2 . . ? C2 C3 H3B 108.2 . . ? H3A C3 H3B 107.4 . . ? C3 C4 C5 116.3(3) . . ? C3 C4 H4A 108.2 . . ? C5 C4 H4A 108.2 . . ? C3 C4 H4B 108.2 . . ? C5 C4 H4B 108.2 . . ? H4A C4 H4B 107.4 . . ? C6 C5 C4 124.6(3) . . ? C6 C5 Ir1 70.80(18) . . ? C4 C5 Ir1 112.4(2) . . ? C6 C5 H5 114.6(17) . . ? C4 C5 H5 114.7(18) . . ? Ir1 C5 H5 110.5(17) . . ? C5 C6 C7 123.0(3) . . ? C5 C6 Ir1 70.90(17) . . ? C7 C6 Ir1 113.1(2) . . ? C5 C6 H6 120(2) . . ? C7 C6 H6 112(2) . . ? Ir1 C6 H6 108.6(19) . . ? C8 C7 C6 115.1(3) . . ? C8 C7 H7A 108.5 . . ? C6 C7 H7A 108.5 . . ? C8 C7 H7B 108.5 . . ? C6 C7 H7B 108.5 . . ? H7A C7 H7B 107.5 . . ? C7 C8 C1 116.5(2) . . ? C7 C8 H8A 108.2 . . ? C1 C8 H8A 108.2 . . ? C7 C8 H8B 108.2 . . ? C1 C8 H8B 108.2 . . ? H8A C8 H8B 107.3 . . ? C10 C9 N1 109.2(2) . . ? C10 C9 H9 125.4 . . ? N1 C9 H9 125.4 . . ? C9 C10 N2 107.0(2) . . ? C9 C10 H10 126.5 . . ? N2 C10 H10 126.5 . . ? N2 C11 N1 110.3(2) . . ? N2 C11 C12 126.4(2) . . ? N1 C11 C12 123.3(2) . . ? C11 C12 P1 106.04(15) . . ? C11 C12 H12A 110.5 . . ? P1 C12 H12A 110.5 . . ? C11 C12 H12B 110.5 . . ? P1 C12 H12B 110.5 . . ? H12A C12 H12B 108.7 . . ? N2 C13 H13A 109.5 . . ? N2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C19 C14 C15 119.3(2) . . ? C19 C14 P1 122.4(2) . . ? C15 C14 P1 118.04(19) . . ? C16 C15 C14 120.3(3) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C17 C16 C15 119.7(3) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C18 C17 C16 120.5(3) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C17 C18 C19 120.3(3) . . ? C17 C18 H18 119.8 . . ? C19 C18 H18 119.8 . . ? C14 C19 C18 119.9(3) . . ? C14 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C25 C20 C21 119.8(2) . . ? C25 C20 P1 118.3(2) . . ? C21 C20 P1 121.40(19) . . ? C22 C21 C20 119.8(3) . . ? C22 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? C21 C22 C23 119.8(3) . . ? C21 C22 H22 120.1 . . ? C23 C22 H22 120.1 . . ? C24 C23 C22 120.2(3) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C23 C24 C25 120.7(3) . . ? C23 C24 H24 119.6 . . ? C25 C24 H24 119.6 . . ? C24 C25 C20 119.6(3) . . ? C24 C25 H25 120.2 . . ? C20 C25 H25 120.2 . . ? C31 C26 C27 114.8(2) . . ? C31 C26 B1 125.4(2) . . ? C27 C26 B1 119.8(2) . . ? C28 C27 C26 123.0(2) . . ? C28 C27 H27 118.5 . . ? C26 C27 H27 118.5 . . ? C29 C28 C27 119.8(2) . . ? C29 C28 H28 120.1 . . ? C27 C28 H28 120.1 . . ? C30 C29 C28 119.1(2) . . ? C30 C29 H29 120.4 . . ? C28 C29 H29 120.4 . . ? C29 C30 C31 120.2(2) . . ? C29 C30 H30 119.9 . . ? C31 C30 H30 119.9 . . ? C30 C31 C26 123.1(2) . . ? C30 C31 H31 118.5 . . ? C26 C31 H31 118.5 . . ? C37 C32 C33 114.8(2) . . ? C37 C32 B1 125.9(2) . . ? C33 C32 B1 119.2(2) . . ? C34 C33 C32 122.6(2) . . ? C34 C33 H33 118.7 . . ? C32 C33 H33 118.7 . . ? C35 C34 C33 120.7(2) . . ? C35 C34 H34 119.7 . . ? C33 C34 H34 119.7 . . ? C34 C35 C36 118.6(2) . . ? C34 C35 H35 120.7 . . ? C36 C35 H35 120.7 . . ? C35 C36 C37 120.5(2) . . ? C35 C36 H36 119.8 . . ? C37 C36 H36 119.8 . . ? C36 C37 C32 122.8(2) . . ? C36 C37 H37 118.6 . . ? C32 C37 H37 118.6 . . ? C39 C38 C43 114.7(2) . . ? C39 C38 B1 122.3(2) . . ? C43 C38 B1 122.8(2) . . ? C40 C39 C38 122.9(2) . . ? C40 C39 H39 118.5 . . ? C38 C39 H39 118.5 . . ? C41 C40 C39 120.1(2) . . ? C41 C40 H40 119.9 . . ? C39 C40 H40 119.9 . . ? C40 C41 C42 119.0(2) . . ? C40 C41 H41 120.5 . . ? C42 C41 H41 120.5 . . ? C41 C42 C43 120.3(2) . . ? C41 C42 H42 119.9 . . ? C43 C42 H42 119.9 . . ? C42 C43 C38 122.9(2) . . ? C42 C43 H43 118.5 . . ? C38 C43 H43 118.5 . . ? C49 C44 C45 115.2(2) . . ? C49 C44 B1 125.4(2) . . ? C45 C44 B1 119.3(2) . . ? C46 C45 C44 123.0(3) . . ? C46 C45 H45 118.5 . . ? C44 C45 H45 118.5 . . ? C47 C46 C45 119.8(3) . . ? C47 C46 H46 120.1 . . ? C45 C46 H46 120.1 . . ? C48 C47 C46 119.3(3) . . ? C48 C47 H47 120.4 . . ? C46 C47 H47 120.4 . . ? C47 C48 C49 120.3(3) . . ? C47 C48 H48 119.9 . . ? C49 C48 H48 119.9 . . ? C48 C49 C44 122.4(3) . . ? C48 C49 H49 118.8 . . ? C44 C49 H49 118.8 . . ? C38 B1 C32 113.90(18) . . ? C38 B1 C44 108.26(18) . . ? C32 B1 C44 105.21(18) . . ? C38 B1 C26 105.91(18) . . ? C32 B1 C26 111.89(18) . . ? C44 B1 C26 111.74(18) . . ? 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 N1 Ir1 P1 C14 133.62(11) . . . . ? C6 Ir1 P1 C14 -61.04(14) . . . . ? C5 Ir1 P1 C14 -22.57(13) . . . . ? C1 Ir1 P1 C14 -141.4(2) . . . . ? C2 Ir1 P1 C14 57.3(4) . . . . ? N1 Ir1 P1 C20 -95.70(10) . . . . ? C6 Ir1 P1 C20 69.65(14) . . . . ? C5 Ir1 P1 C20 108.12(13) . . . . ? C1 Ir1 P1 C20 -10.7(2) . . . . ? C2 Ir1 P1 C20 -172.0(4) . . . . ? N1 Ir1 P1 C12 15.26(10) . . . . ? C6 Ir1 P1 C12 -179.40(13) . . . . ? C5 Ir1 P1 C12 -140.93(13) . . . . ? C1 Ir1 P1 C12 100.2(2) . . . . ? C2 Ir1 P1 C12 -61.0(4) . . . . ? C6 Ir1 N1 C11 -88.3(4) . . . . ? C5 Ir1 N1 C11 79.9(3) . . . . ? C1 Ir1 N1 C11 -165.50(19) . . . . ? C2 Ir1 N1 C11 157.96(19) . . . . ? P1 Ir1 N1 C11 -8.95(17) . . . . ? C6 Ir1 N1 C9 89.2(4) . . . . ? C5 Ir1 N1 C9 -102.6(3) . . . . ? C1 Ir1 N1 C9 12.0(3) . . . . ? C2 Ir1 N1 C9 -24.5(3) . . . . ? P1 Ir1 N1 C9 168.6(2) . . . . ? N1 Ir1 C1 C2 -90.59(18) . . . . ? C6 Ir1 C1 C2 104.1(2) . . . . ? C5 Ir1 C1 C2 68.0(2) . . . . ? P1 Ir1 C1 C2 -172.76(16) . . . . ? N1 Ir1 C1 C8 147.56(19) . . . . ? C6 Ir1 C1 C8 -17.8(2) . . . . ? C5 Ir1 C1 C8 -53.9(2) . . . . ? C2 Ir1 C1 C8 -121.9(3) . . . . ? P1 Ir1 C1 C8 65.4(3) . . . . ? C8 C1 C2 C3 -1.0(5) . . . . ? Ir1 C1 C2 C3 -102.4(3) . . . . ? C8 C1 C2 Ir1 101.4(3) . . . . ? N1 Ir1 C2 C1 92.74(18) . . . . ? C6 Ir1 C2 C1 -73.7(2) . . . . ? C5 Ir1 C2 C1 -110.7(2) . . . . ? P1 Ir1 C2 C1 167.6(3) . . . . ? N1 Ir1 C2 C3 -146.6(2) . . . . ? C6 Ir1 C2 C3 47.0(2) . . . . ? C5 Ir1 C2 C3 10.0(2) . . . . ? C1 Ir1 C2 C3 120.6(3) . . . . ? P1 Ir1 C2 C3 -71.8(5) . . . . ? C1 C2 C3 C4 79.1(5) . . . . ? Ir1 C2 C3 C4 -1.7(4) . . . . ? C2 C3 C4 C5 -12.5(6) . . . . ? C3 C4 C5 C6 -60.6(5) . . . . ? C3 C4 C5 Ir1 20.9(5) . . . . ? N1 Ir1 C5 C6 -175.1(2) . . . . ? C1 Ir1 C5 C6 70.1(2) . . . . ? C2 Ir1 C5 C6 104.0(2) . . . . ? P1 Ir1 C5 C6 -89.45(18) . . . . ? N1 Ir1 C5 C4 64.4(4) . . . . ? C6 Ir1 C5 C4 -120.5(4) . . . . ? C1 Ir1 C5 C4 -50.4(3) . . . . ? C2 Ir1 C5 C4 -16.5(3) . . . . ? P1 Ir1 C5 C4 150.1(3) . . . . ? C4 C5 C6 C7 -1.2(5) . . . . ? Ir1 C5 C6 C7 -105.7(3) . . . . ? C4 C5 C6 Ir1 104.5(3) . . . . ? N1 Ir1 C6 C5 172.4(3) . . . . ? C1 Ir1 C6 C5 -108.6(2) . . . . ? C2 Ir1 C6 C5 -73.5(2) . . . . ? P1 Ir1 C6 C5 94.73(19) . . . . ? N1 Ir1 C6 C7 -69.0(5) . . . . ? C5 Ir1 C6 C7 118.6(4) . . . . ? C1 Ir1 C6 C7 10.0(3) . . . . ? C2 Ir1 C6 C7 45.2(3) . . . . ? P1 Ir1 C6 C7 -146.7(3) . . . . ? C5 C6 C7 C8 81.6(5) . . . . ? Ir1 C6 C7 C8 0.1(5) . . . . ? C6 C7 C8 C1 -16.4(5) . . . . ? C2 C1 C8 C7 -57.8(4) . . . . ? Ir1 C1 C8 C7 23.7(4) . . . . ? C11 N1 C9 C10 0.4(3) . . . . ? Ir1 N1 C9 C10 -177.42(19) . . . . ? N1 C9 C10 N2 0.1(3) . . . . ? C11 N2 C10 C9 -0.6(3) . . . . ? C13 N2 C10 C9 -174.6(2) . . . . ? C10 N2 C11 N1 0.8(3) . . . . ? C13 N2 C11 N1 174.9(2) . . . . ? C10 N2 C11 C12 -177.8(2) . . . . ? C13 N2 C11 C12 -3.8(4) . . . . ? C9 N1 C11 N2 -0.7(3) . . . . ? Ir1 N1 C11 N2 177.40(15) . . . . ? C9 N1 C11 C12 178.0(2) . . . . ? Ir1 N1 C11 C12 -3.9(3) . . . . ? N2 C11 C12 P1 -164.21(19) . . . . ? N1 C11 C12 P1 17.3(3) . . . . ? C14 P1 C12 C11 -146.09(16) . . . . ? C20 P1 C12 C11 98.93(17) . . . . ? Ir1 P1 C12 C11 -20.43(16) . . . . ? C20 P1 C14 C19 -17.7(2) . . . . ? C12 P1 C14 C19 -128.0(2) . . . . ? Ir1 P1 C14 C19 115.3(2) . . . . ? C20 P1 C14 C15 168.86(19) . . . . ? C12 P1 C14 C15 58.6(2) . . . . ? Ir1 P1 C14 C15 -58.2(2) . . . . ? C19 C14 C15 C16 0.5(4) . . . . ? P1 C14 C15 C16 174.2(2) . . . . ? C14 C15 C16 C17 -1.0(4) . . . . ? C15 C16 C17 C18 1.1(4) . . . . ? C16 C17 C18 C19 -0.7(5) . . . . ? C15 C14 C19 C18 -0.2(4) . . . . ? P1 C14 C19 C18 -173.5(2) . . . . ? C17 C18 C19 C14 0.3(4) . . . . ? C14 P1 C20 C25 136.4(2) . . . . ? C12 P1 C20 C25 -110.3(2) . . . . ? Ir1 P1 C20 C25 1.6(2) . . . . ? C14 P1 C20 C21 -51.2(2) . . . . ? C12 P1 C20 C21 62.1(2) . . . . ? Ir1 P1 C20 C21 174.01(18) . . . . ? C25 C20 C21 C22 -0.6(4) . . . . ? P1 C20 C21 C22 -172.8(2) . . . . ? C20 C21 C22 C23 1.0(5) . . . . ? C21 C22 C23 C24 -0.5(5) . . . . ? C22 C23 C24 C25 -0.4(5) . . . . ? C23 C24 C25 C20 0.9(5) . . . . ? C21 C20 C25 C24 -0.4(4) . . . . ? P1 C20 C25 C24 172.1(2) . . . . ? C31 C26 C27 C28 -2.0(3) . . . . ? B1 C26 C27 C28 179.1(2) . . . . ? C26 C27 C28 C29 1.0(4) . . . . ? C27 C28 C29 C30 0.4(4) . . . . ? C28 C29 C30 C31 -0.7(4) . . . . ? C29 C30 C31 C26 -0.4(4) . . . . ? C27 C26 C31 C30 1.7(3) . . . . ? B1 C26 C31 C30 -179.5(2) . . . . ? C37 C32 C33 C34 0.4(3) . . . . ? B1 C32 C33 C34 176.5(2) . . . . ? C32 C33 C34 C35 -0.7(4) . . . . ? C33 C34 C35 C36 0.2(4) . . . . ? C34 C35 C36 C37 0.5(4) . . . . ? C35 C36 C37 C32 -0.8(4) . . . . ? C33 C32 C37 C36 0.3(3) . . . . ? B1 C32 C37 C36 -175.5(2) . . . . ? C43 C38 C39 C40 -0.2(3) . . . . ? B1 C38 C39 C40 -175.6(2) . . . . ? C38 C39 C40 C41 0.3(3) . . . . ? C39 C40 C41 C42 -0.3(3) . . . . ? C40 C41 C42 C43 0.1(4) . . . . ? C41 C42 C43 C38 -0.1(4) . . . . ? C39 C38 C43 C42 0.1(3) . . . . ? B1 C38 C43 C42 175.4(2) . . . . ? C49 C44 C45 C46 0.0(4) . . . . ? B1 C44 C45 C46 -176.3(2) . . . . ? C44 C45 C46 C47 0.2(4) . . . . ? C45 C46 C47 C48 -0.3(4) . . . . ? C46 C47 C48 C49 0.4(4) . . . . ? C47 C48 C49 C44 -0.3(4) . . . . ? C45 C44 C49 C48 0.1(4) . . . . ? B1 C44 C49 C48 176.1(2) . . . . ? C39 C38 B1 C32 -54.3(3) . . . . ? C43 C38 B1 C32 130.8(2) . . . . ? C39 C38 B1 C44 -170.9(2) . . . . ? C43 C38 B1 C44 14.1(3) . . . . ? C39 C38 B1 C26 69.1(3) . . . . ? C43 C38 B1 C26 -105.9(2) . . . . ? C37 C32 B1 C38 -1.0(3) . . . . ? C33 C32 B1 C38 -176.7(2) . . . . ? C37 C32 B1 C44 117.4(2) . . . . ? C33 C32 B1 C44 -58.3(3) . . . . ? C37 C32 B1 C26 -121.1(2) . . . . ? C33 C32 B1 C26 63.2(3) . . . . ? C49 C44 B1 C38 -103.3(3) . . . . ? C45 C44 B1 C38 72.5(3) . . . . ? C49 C44 B1 C32 134.5(2) . . . . ? C45 C44 B1 C32 -49.6(3) . . . . ? C49 C44 B1 C26 12.9(3) . . . . ? C45 C44 B1 C26 -171.2(2) . . . . ? C31 C26 B1 C38 -128.1(2) . . . . ? C27 C26 B1 C38 50.7(3) . . . . ? C31 C26 B1 C32 -3.5(3) . . . . ? C27 C26 B1 C32 175.3(2) . . . . ? C31 C26 B1 C44 114.2(2) . . . . ? C27 C26 B1 C44 -67.0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.959 _refine_diff_density_max 1.564 _refine_diff_density_min -1.180 _refine_diff_density_rms 0.075 # Attachment 'bam13.cif' data_bam13 _database_code_depnum_ccdc_archive 'CCDC 711456' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H53 B Cl2 N2 P Rh' _chemical_formula_weight 909.54 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' Cl Cl 0.1484 0.1585 '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' P P 0.1023 0.0942 '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/c ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? 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 14.459(4) _cell_length_b 27.437(8) _cell_length_c 11.669(3) _cell_angle_alpha 90.00 _cell_angle_beta 108.354(5) _cell_angle_gamma 90.00 _cell_volume 4394(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 996 _cell_measurement_theta_min 2.303 _cell_measurement_theta_max 27.458 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.468 _exptl_crystal_size_mid 0.247 _exptl_crystal_size_min 0.030 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.375 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1888 _exptl_absorpt_coefficient_mu 0.585 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.800 _exptl_absorpt_correction_T_max 0.982 _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 159 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.01 _diffrn_reflns_number 42551 _diffrn_reflns_av_R_equivalents 0.0616 _diffrn_reflns_av_sigmaI/netI 0.0605 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 28.33 _reflns_number_total 10445 _reflns_number_gt 7358 _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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10445 _refine_ls_number_parameters 524 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0610 _refine_ls_R_factor_gt 0.0328 _refine_ls_wR_factor_ref 0.0774 _refine_ls_wR_factor_gt 0.0690 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.793710(13) 0.090849(6) -0.000886(15) 0.01851(5) Uani 1 1 d . . . P1 P 0.79402(4) 0.13053(2) 0.17112(5) 0.01982(13) Uani 1 1 d . . . N1 N 0.94291(13) 0.11045(6) 0.03429(16) 0.0212(4) Uani 1 1 d . . . N2 N 1.09352(13) 0.13784(6) 0.11117(17) 0.0230(4) Uani 1 1 d . . . C1 C 0.80743(18) 0.03065(8) -0.12378(19) 0.0252(5) Uani 1 1 d . . . H1 H 0.8761 0.0229 -0.1191 0.030 Uiso 1 1 calc R . . C2 C 0.76866(18) 0.06988(8) -0.1956(2) 0.0259(5) Uani 1 1 d . . . H2 H 0.8143 0.0858 -0.2331 0.031 Uiso 1 1 calc R . . C3 C 0.66203(19) 0.07440(9) -0.2690(2) 0.0323(6) Uani 1 1 d . . . H3A H 0.6333 0.0414 -0.2871 0.039 Uiso 1 1 calc R . . H3B H 0.6565 0.0906 -0.3468 0.039 Uiso 1 1 calc R . . C4 C 0.60446(19) 0.10381(9) -0.2022(2) 0.0357(6) Uani 1 1 d . . . H4A H 0.6105 0.1389 -0.2178 0.043 Uiso 1 1 calc R . . H4B H 0.5347 0.0950 -0.2351 0.043 Uiso 1 1 calc R . . C5 C 0.63856(17) 0.09524(9) -0.0678(2) 0.0280(5) Uani 1 1 d . . . H5 H 0.6101 0.1184 -0.0219 0.034 Uiso 1 1 calc R . . C6 C 0.66470(17) 0.05026(8) -0.0109(2) 0.0271(5) Uani 1 1 d . . . H6 H 0.6517 0.0477 0.0681 0.032 Uiso 1 1 calc R . . C7 C 0.65627(18) 0.00177(8) -0.0776(2) 0.0308(6) Uani 1 1 d . . . H7A H 0.6030 0.0040 -0.1553 0.037 Uiso 1 1 calc R . . H7B H 0.6390 -0.0241 -0.0288 0.037 Uiso 1 1 calc R . . C8 C 0.75056(18) -0.01229(8) -0.1021(2) 0.0294(6) Uani 1 1 d . . . H8A H 0.7921 -0.0310 -0.0323 0.035 Uiso 1 1 calc R . . H8B H 0.7345 -0.0339 -0.1737 0.035 Uiso 1 1 calc R . . C9 C 0.99333(18) 0.10405(8) -0.0482(2) 0.0260(5) Uani 1 1 d . . . H9 H 0.9670 0.0898 -0.1259 0.031 Uiso 1 1 calc R . . C10 C 1.08490(18) 0.12105(8) -0.0021(2) 0.0266(5) Uani 1 1 d . . . H10 H 1.1338 0.1213 -0.0406 0.032 Uiso 1 1 calc R . . C11 C 1.00726(16) 0.13145(8) 0.1308(2) 0.0198(5) Uani 1 1 d . . . C12 C 0.99441(17) 0.14962(8) 0.2454(2) 0.0247(5) Uani 1 1 d . . . H12A H 0.9824 0.1852 0.2371 0.030 Uiso 1 1 calc R . . H12B H 1.0566 0.1448 0.3110 0.030 Uiso 1 1 calc R . . C13 C 0.91315(16) 0.12661(8) 0.28474(19) 0.0231(5) Uani 1 1 d . . . H13A H 0.9104 0.1430 0.3592 0.028 Uiso 1 1 calc R . . H13B H 0.9290 0.0919 0.3044 0.028 Uiso 1 1 calc R . . C14 C 1.18005(17) 0.16205(9) 0.1924(2) 0.0332(6) Uani 1 1 d . . . H14A H 1.1649 0.1963 0.2024 0.050 Uiso 1 1 calc R . . H14B H 1.2336 0.1602 0.1579 0.050 Uiso 1 1 calc R . . H14C H 1.1994 0.1458 0.2712 0.050 Uiso 1 1 calc R . . C15 C 0.76738(16) 0.19555(8) 0.15363(19) 0.0201(5) Uani 1 1 d . . . C16 C 0.72346(17) 0.21474(8) 0.0386(2) 0.0262(5) Uani 1 1 d . . . H16 H 0.7073 0.1938 -0.0297 0.031 Uiso 1 1 calc R . . C17 C 0.70322(18) 0.26410(9) 0.0235(2) 0.0307(6) Uani 1 1 d . . . H17 H 0.6726 0.2767 -0.0552 0.037 Uiso 1 1 calc R . . C18 C 0.72691(18) 0.29500(9) 0.1210(2) 0.0321(6) Uani 1 1 d . . . H18 H 0.7131 0.3288 0.1098 0.039 Uiso 1 1 calc R . . C19 C 0.77106(18) 0.27662(9) 0.2359(2) 0.0315(6) Uani 1 1 d . . . H19 H 0.7878 0.2979 0.3035 0.038 Uiso 1 1 calc R . . C20 C 0.79097(17) 0.22716(8) 0.2523(2) 0.0263(5) Uani 1 1 d . . . H20 H 0.8209 0.2147 0.3314 0.032 Uiso 1 1 calc R . . C21 C 0.71494(16) 0.10677(8) 0.25228(19) 0.0221(5) Uani 1 1 d . . . C22 C 0.63242(17) 0.13125(9) 0.2588(2) 0.0285(6) Uani 1 1 d . . . H22 H 0.6167 0.1624 0.2224 0.034 Uiso 1 1 calc R . . C23 C 0.57303(19) 0.11031(10) 0.3182(2) 0.0375(6) Uani 1 1 d . . . H23 H 0.5171 0.1273 0.3229 0.045 Uiso 1 1 calc R . . C24 C 0.59465(19) 0.06499(10) 0.3706(2) 0.0372(6) Uani 1 1 d . . . H24 H 0.5537 0.0508 0.4111 0.045 Uiso 1 1 calc R . . C25 C 0.67568(19) 0.04021(10) 0.3642(2) 0.0375(6) Uani 1 1 d . . . H25 H 0.6904 0.0089 0.3999 0.045 Uiso 1 1 calc R . . C26 C 0.73534(18) 0.06085(9) 0.3060(2) 0.0330(6) Uani 1 1 d . . . H26 H 0.7913 0.0436 0.3023 0.040 Uiso 1 1 calc R . . C27 C 0.26040(15) 0.13995(7) -0.20189(19) 0.0185(5) Uani 1 1 d . . . C28 C 0.34100(16) 0.11039(8) -0.1433(2) 0.0237(5) Uani 1 1 d . . . H28 H 0.3533 0.0824 -0.1842 0.028 Uiso 1 1 calc R . . C29 C 0.40332(17) 0.12045(8) -0.0281(2) 0.0262(5) Uani 1 1 d . . . H29 H 0.4562 0.0992 0.0085 0.031 Uiso 1 1 calc R . . C30 C 0.38860(18) 0.16131(9) 0.0336(2) 0.0288(6) Uani 1 1 d . . . H30 H 0.4306 0.1682 0.1126 0.035 Uiso 1 1 calc R . . C31 C 0.31161(18) 0.19190(9) -0.0220(2) 0.0279(6) Uani 1 1 d . . . H31 H 0.3009 0.2203 0.0187 0.034 Uiso 1 1 calc R . . C32 C 0.24977(16) 0.18141(8) -0.13720(19) 0.0217(5) Uani 1 1 d . . . H32 H 0.1980 0.2033 -0.1736 0.026 Uiso 1 1 calc R . . C33 C 0.11530(16) 0.17282(7) -0.39313(19) 0.0187(5) Uani 1 1 d . . . C34 C 0.13318(17) 0.20244(8) -0.48151(19) 0.0226(5) Uani 1 1 d . . . H34 H 0.1867 0.1948 -0.5091 0.027 Uiso 1 1 calc R . . C35 C 0.07524(18) 0.24279(8) -0.5307(2) 0.0281(6) Uani 1 1 d . . . H35 H 0.0895 0.2617 -0.5913 0.034 Uiso 1 1 calc R . . C36 C -0.00235(17) 0.25533(8) -0.4920(2) 0.0286(6) Uani 1 1 d . . . H36 H -0.0420 0.2826 -0.5257 0.034 Uiso 1 1 calc R . . C37 C -0.02166(17) 0.22738(8) -0.4030(2) 0.0277(5) Uani 1 1 d . . . H37 H -0.0744 0.2357 -0.3746 0.033 Uiso 1 1 calc R . . C38 C 0.03594(17) 0.18757(8) -0.3558(2) 0.0240(5) Uani 1 1 d . . . H38 H 0.0213 0.1691 -0.2948 0.029 Uiso 1 1 calc R . . C39 C 0.11084(16) 0.08082(7) -0.31335(18) 0.0180(5) Uani 1 1 d . . . C40 C 0.01515(17) 0.07437(8) -0.3892(2) 0.0259(5) Uani 1 1 d . . . H40 H -0.0101 0.0969 -0.4532 0.031 Uiso 1 1 calc R . . C41 C -0.04492(17) 0.03672(8) -0.3760(2) 0.0284(6) Uani 1 1 d . . . H41 H -0.1092 0.0338 -0.4304 0.034 Uiso 1 1 calc R . . C42 C -0.01064(17) 0.00350(8) -0.2832(2) 0.0233(5) Uani 1 1 d . . . H42 H -0.0512 -0.0222 -0.2726 0.028 Uiso 1 1 calc R . . C43 C 0.08315(17) 0.00818(8) -0.2066(2) 0.0232(5) Uani 1 1 d . . . H43 H 0.1078 -0.0146 -0.1429 0.028 Uiso 1 1 calc R . . C44 C 0.14213(16) 0.04611(7) -0.22196(19) 0.0205(5) Uani 1 1 d . . . H44 H 0.2066 0.0485 -0.1677 0.025 Uiso 1 1 calc R . . C45 C 0.24122(16) 0.10568(7) -0.42492(19) 0.0182(5) Uani 1 1 d . . . C46 C 0.20119(17) 0.07129(8) -0.51534(19) 0.0222(5) Uani 1 1 d . . . H46 H 0.1381 0.0587 -0.5241 0.027 Uiso 1 1 calc R . . C47 C 0.25014(17) 0.05482(8) -0.5928(2) 0.0269(5) Uani 1 1 d . . . H47 H 0.2202 0.0314 -0.6530 0.032 Uiso 1 1 calc R . . C48 C 0.34210(17) 0.07224(9) -0.5833(2) 0.0271(5) Uani 1 1 d . . . H48 H 0.3759 0.0608 -0.6358 0.033 Uiso 1 1 calc R . . C49 C 0.38345(17) 0.10648(9) -0.4960(2) 0.0270(5) Uani 1 1 d . . . H49 H 0.4463 0.1191 -0.4882 0.032 Uiso 1 1 calc R . . C50 C 0.33337(17) 0.12266(8) -0.4193(2) 0.0247(5) Uani 1 1 d . . . H50 H 0.3634 0.1464 -0.3601 0.030 Uiso 1 1 calc R . . B1 B 0.18208(18) 0.12523(9) -0.3338(2) 0.0188(5) Uani 1 1 d . . . C51 C 0.4346(3) 0.23187(10) -0.2040(4) 0.0736(12) Uani 1 1 d . . . H51A H 0.4573 0.2078 -0.1378 0.088 Uiso 1 1 calc R . . H51B H 0.3721 0.2199 -0.2599 0.088 Uiso 1 1 calc R . . Cl1 Cl 0.51927(5) 0.23462(2) -0.28121(6) 0.03991(17) Uani 1 1 d . . . Cl2 Cl 0.41395(6) 0.28730(2) -0.14292(7) 0.04732(19) 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 0.02078(10) 0.01872(9) 0.01741(9) -0.00099(7) 0.00800(7) -0.00043(8) P1 0.0229(3) 0.0206(3) 0.0178(3) 0.0013(2) 0.0091(3) 0.0031(2) N1 0.0245(11) 0.0212(10) 0.0203(10) -0.0014(8) 0.0106(9) -0.0003(8) N2 0.0198(10) 0.0227(10) 0.0272(11) 0.0020(8) 0.0084(9) -0.0001(8) C1 0.0338(14) 0.0241(12) 0.0198(12) -0.0079(10) 0.0115(11) -0.0006(10) C2 0.0346(14) 0.0273(12) 0.0185(12) -0.0046(10) 0.0124(11) -0.0056(11) C3 0.0398(16) 0.0299(13) 0.0225(13) 0.0049(10) 0.0032(12) -0.0073(11) C4 0.0289(14) 0.0338(15) 0.0377(15) 0.0033(11) 0.0008(12) 0.0014(11) C5 0.0207(12) 0.0300(13) 0.0335(14) -0.0049(11) 0.0086(11) -0.0012(10) C6 0.0254(13) 0.0310(13) 0.0279(13) -0.0028(10) 0.0126(11) -0.0078(11) C7 0.0394(15) 0.0241(13) 0.0280(13) 0.0018(10) 0.0092(12) -0.0102(11) C8 0.0435(16) 0.0210(12) 0.0215(12) -0.0030(10) 0.0071(12) -0.0011(11) C9 0.0302(14) 0.0259(13) 0.0263(13) -0.0046(10) 0.0150(11) -0.0013(10) C10 0.0297(14) 0.0247(13) 0.0315(14) -0.0008(10) 0.0185(12) 0.0028(10) C11 0.0207(12) 0.0170(11) 0.0219(12) 0.0022(9) 0.0072(10) 0.0026(9) C12 0.0236(13) 0.0283(13) 0.0214(12) -0.0017(10) 0.0059(10) 0.0005(10) C13 0.0258(13) 0.0259(12) 0.0183(11) -0.0007(9) 0.0080(10) 0.0039(10) C14 0.0230(14) 0.0399(15) 0.0343(15) 0.0002(12) 0.0058(12) -0.0076(11) C15 0.0181(12) 0.0225(12) 0.0211(12) 0.0007(9) 0.0081(10) 0.0023(9) C16 0.0296(14) 0.0270(13) 0.0220(12) 0.0000(10) 0.0081(11) -0.0010(10) C17 0.0329(15) 0.0282(13) 0.0293(14) 0.0071(10) 0.0072(12) 0.0041(11) C18 0.0354(15) 0.0214(13) 0.0431(16) 0.0014(11) 0.0174(13) 0.0050(11) C19 0.0367(15) 0.0294(14) 0.0310(14) -0.0088(11) 0.0145(12) 0.0021(11) C20 0.0311(14) 0.0274(13) 0.0215(12) -0.0011(10) 0.0100(11) 0.0033(10) C21 0.0242(13) 0.0254(12) 0.0179(11) 0.0004(9) 0.0085(10) 0.0041(10) C22 0.0293(14) 0.0277(13) 0.0317(14) 0.0051(11) 0.0142(12) 0.0067(11) C23 0.0317(15) 0.0447(16) 0.0441(16) 0.0078(13) 0.0234(13) 0.0115(12) C24 0.0327(15) 0.0500(17) 0.0364(15) 0.0143(13) 0.0217(13) 0.0050(13) C25 0.0365(16) 0.0401(16) 0.0418(16) 0.0191(13) 0.0206(13) 0.0097(12) C26 0.0311(15) 0.0340(14) 0.0401(15) 0.0118(12) 0.0200(13) 0.0136(11) C27 0.0176(12) 0.0202(11) 0.0201(11) 0.0010(9) 0.0093(10) -0.0044(9) C28 0.0241(13) 0.0214(11) 0.0270(13) 0.0002(10) 0.0100(11) -0.0041(10) C29 0.0204(13) 0.0280(13) 0.0287(13) 0.0072(10) 0.0056(11) -0.0042(10) C30 0.0267(14) 0.0379(14) 0.0193(12) -0.0021(10) 0.0036(11) -0.0093(11) C31 0.0329(15) 0.0292(13) 0.0244(13) -0.0077(10) 0.0128(11) -0.0058(11) C32 0.0228(12) 0.0230(12) 0.0215(12) -0.0003(9) 0.0101(10) -0.0018(9) C33 0.0200(12) 0.0190(11) 0.0155(11) -0.0040(9) 0.0034(9) -0.0026(9) C34 0.0249(13) 0.0218(12) 0.0225(12) -0.0029(9) 0.0094(10) -0.0023(10) C35 0.0365(15) 0.0223(12) 0.0245(13) 0.0023(10) 0.0079(11) -0.0052(11) C36 0.0265(13) 0.0192(12) 0.0327(14) 0.0004(10) -0.0014(11) 0.0011(10) C37 0.0233(13) 0.0250(13) 0.0358(14) -0.0051(11) 0.0106(11) -0.0003(10) C38 0.0270(13) 0.0231(12) 0.0247(12) 0.0005(10) 0.0120(11) -0.0024(10) C39 0.0210(12) 0.0196(11) 0.0152(11) -0.0036(8) 0.0085(9) 0.0006(9) C40 0.0272(14) 0.0267(12) 0.0220(12) 0.0039(10) 0.0053(11) -0.0031(10) C41 0.0194(13) 0.0308(13) 0.0300(13) -0.0015(11) 0.0009(11) -0.0070(10) C42 0.0250(13) 0.0196(12) 0.0276(13) -0.0040(10) 0.0115(11) -0.0055(10) C43 0.0287(13) 0.0185(11) 0.0232(12) 0.0029(9) 0.0094(11) 0.0011(10) C44 0.0188(12) 0.0207(11) 0.0214(12) -0.0020(9) 0.0053(10) -0.0012(9) C45 0.0207(12) 0.0162(11) 0.0175(11) 0.0026(8) 0.0059(9) 0.0020(9) C46 0.0219(12) 0.0250(11) 0.0208(12) -0.0019(9) 0.0083(10) -0.0028(10) C47 0.0288(14) 0.0316(13) 0.0214(12) -0.0082(10) 0.0092(11) -0.0035(11) C48 0.0263(14) 0.0350(13) 0.0232(13) -0.0029(10) 0.0125(11) 0.0027(11) C49 0.0200(12) 0.0376(14) 0.0258(13) 0.0006(11) 0.0108(11) -0.0029(10) C50 0.0233(13) 0.0285(13) 0.0222(12) -0.0063(10) 0.0072(10) -0.0041(10) B1 0.0199(13) 0.0187(13) 0.0183(13) -0.0001(10) 0.0067(11) -0.0020(10) C51 0.098(3) 0.0311(17) 0.128(3) -0.0146(19) 0.087(3) -0.0131(17) Cl1 0.0414(4) 0.0337(4) 0.0492(4) 0.0076(3) 0.0208(3) 0.0023(3) Cl2 0.0633(5) 0.0297(4) 0.0569(5) -0.0028(3) 0.0303(4) -0.0036(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C5 2.134(2) . ? Rh1 N1 2.1340(19) . ? Rh1 C6 2.144(2) . ? Rh1 C1 2.237(2) . ? Rh1 C2 2.259(2) . ? Rh1 P1 2.2821(8) . ? P1 C13 1.816(2) . ? P1 C21 1.820(2) . ? P1 C15 1.823(2) . ? N1 C11 1.344(3) . ? N1 C9 1.390(3) . ? N2 C11 1.349(3) . ? N2 C10 1.368(3) . ? N2 C14 1.469(3) . ? C1 C2 1.371(3) . ? C1 C8 1.503(3) . ? C1 H1 1.0000 . ? C2 C3 1.515(3) . ? C2 H2 1.0000 . ? C3 C4 1.536(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.507(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.396(3) . ? C5 H5 1.0000 . ? C6 C7 1.527(3) . ? C6 H6 1.0000 . ? C7 C8 1.528(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.346(3) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.492(3) . ? C12 C13 1.526(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.394(3) . ? C15 C20 1.396(3) . ? C16 C17 1.385(3) . ? C16 H16 0.9500 . ? C17 C18 1.373(3) . ? C17 H17 0.9500 . ? C18 C19 1.385(3) . ? C18 H18 0.9500 . ? C19 C20 1.388(3) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.392(3) . ? C21 C26 1.397(3) . ? C22 C23 1.387(3) . ? C22 H22 0.9500 . ? C23 C24 1.377(3) . ? C23 H23 0.9500 . ? C24 C25 1.377(3) . ? C24 H24 0.9500 . ? C25 C26 1.376(3) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C32 1.400(3) . ? C27 C28 1.408(3) . ? C27 B1 1.649(3) . ? C28 C29 1.391(3) . ? C28 H28 0.9500 . ? C29 C30 1.384(3) . ? C29 H29 0.9500 . ? C30 C31 1.382(3) . ? C30 H30 0.9500 . ? C31 C32 1.390(3) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C34 1.399(3) . ? C33 C38 1.409(3) . ? C33 B1 1.642(3) . ? C34 C35 1.398(3) . ? C34 H34 0.9500 . ? C35 C36 1.378(3) . ? C35 H35 0.9500 . ? C36 C37 1.389(3) . ? C36 H36 0.9500 . ? C37 C38 1.379(3) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C44 1.395(3) . ? C39 C40 1.399(3) . ? C39 B1 1.661(3) . ? C40 C41 1.389(3) . ? C40 H40 0.9500 . ? C41 C42 1.382(3) . ? C41 H41 0.9500 . ? C42 C43 1.375(3) . ? C42 H42 0.9500 . ? C43 C44 1.392(3) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C50 1.393(3) . ? C45 C46 1.398(3) . ? C45 B1 1.650(3) . ? C46 C47 1.388(3) . ? C46 H46 0.9500 . ? C47 C48 1.384(3) . ? C47 H47 0.9500 . ? C48 C49 1.376(3) . ? C48 H48 0.9500 . ? C49 C50 1.390(3) . ? C49 H49 0.9500 . ? C50 H50 0.9500 . ? C51 Cl1 1.735(3) . ? C51 Cl2 1.745(3) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 Rh1 N1 159.85(8) . . ? C5 Rh1 C6 38.09(9) . . ? N1 Rh1 C6 161.98(8) . . ? C5 Rh1 C1 95.87(9) . . ? N1 Rh1 C1 91.20(8) . . ? C6 Rh1 C1 80.37(9) . . ? C5 Rh1 C2 80.17(9) . . ? N1 Rh1 C2 95.16(8) . . ? C6 Rh1 C2 87.22(9) . . ? C1 Rh1 C2 35.50(8) . . ? C5 Rh1 P1 90.32(7) . . ? N1 Rh1 P1 89.35(5) . . ? C6 Rh1 P1 93.24(7) . . ? C1 Rh1 P1 160.07(6) . . ? C2 Rh1 P1 163.96(6) . . ? C13 P1 C21 101.88(10) . . ? C13 P1 C15 104.95(10) . . ? C21 P1 C15 105.28(10) . . ? C13 P1 Rh1 110.65(8) . . ? C21 P1 Rh1 117.34(8) . . ? C15 P1 Rh1 115.25(7) . . ? C11 N1 C9 105.00(18) . . ? C11 N1 Rh1 131.34(15) . . ? C9 N1 Rh1 123.64(15) . . ? C11 N2 C10 108.21(19) . . ? C11 N2 C14 126.5(2) . . ? C10 N2 C14 125.2(2) . . ? C2 C1 C8 125.3(2) . . ? C2 C1 Rh1 73.14(13) . . ? C8 C1 Rh1 107.89(15) . . ? C2 C1 H1 114.2 . . ? C8 C1 H1 114.2 . . ? Rh1 C1 H1 114.2 . . ? C1 C2 C3 123.9(2) . . ? C1 C2 Rh1 71.36(13) . . ? C3 C2 Rh1 111.14(16) . . ? C1 C2 H2 114.2 . . ? C3 C2 H2 114.2 . . ? Rh1 C2 H2 114.2 . . ? C2 C3 C4 111.9(2) . . ? C2 C3 H3A 109.2 . . ? C4 C3 H3A 109.2 . . ? C2 C3 H3B 109.2 . . ? C4 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? C5 C4 C3 113.2(2) . . ? C5 C4 H4A 108.9 . . ? C3 C4 H4A 108.9 . . ? C5 C4 H4B 108.9 . . ? C3 C4 H4B 108.9 . . ? H4A C4 H4B 107.7 . . ? C6 C5 C4 125.7(2) . . ? C6 C5 Rh1 71.34(13) . . ? C4 C5 Rh1 110.57(16) . . ? C6 C5 H5 113.8 . . ? C4 C5 H5 113.8 . . ? Rh1 C5 H5 113.8 . . ? C5 C6 C7 124.2(2) . . ? C5 C6 Rh1 70.57(13) . . ? C7 C6 Rh1 114.14(16) . . ? C5 C6 H6 113.6 . . ? C7 C6 H6 113.6 . . ? Rh1 C6 H6 113.6 . . ? C6 C7 C8 112.49(19) . . ? C6 C7 H7A 109.1 . . ? C8 C7 H7A 109.1 . . ? C6 C7 H7B 109.1 . . ? C8 C7 H7B 109.1 . . ? H7A C7 H7B 107.8 . . ? C1 C8 C7 113.67(19) . . ? C1 C8 H8A 108.8 . . ? C7 C8 H8A 108.8 . . ? C1 C8 H8B 108.8 . . ? C7 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? C10 C9 N1 110.1(2) . . ? C10 C9 H9 124.9 . . ? N1 C9 H9 124.9 . . ? C9 C10 N2 106.4(2) . . ? C9 C10 H10 126.8 . . ? N2 C10 H10 126.8 . . ? N1 C11 N2 110.29(19) . . ? N1 C11 C12 130.2(2) . . ? N2 C11 C12 119.4(2) . . ? C11 C12 C13 117.15(19) . . ? C11 C12 H12A 108.0 . . ? C13 C12 H12A 108.0 . . ? C11 C12 H12B 108.0 . . ? C13 C12 H12B 108.0 . . ? H12A C12 H12B 107.3 . . ? C12 C13 P1 113.51(15) . . ? C12 C13 H13A 108.9 . . ? P1 C13 H13A 108.9 . . ? C12 C13 H13B 108.9 . . ? P1 C13 H13B 108.9 . . ? H13A C13 H13B 107.7 . . ? N2 C14 H14A 109.5 . . ? N2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C20 118.6(2) . . ? C16 C15 P1 119.57(17) . . ? C20 C15 P1 121.85(17) . . ? C17 C16 C15 120.4(2) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C18 C17 C16 120.7(2) . . ? C18 C17 H17 119.6 . . ? C16 C17 H17 119.6 . . ? C17 C18 C19 119.7(2) . . ? C17 C18 H18 120.1 . . ? C19 C18 H18 120.1 . . ? C18 C19 C20 120.2(2) . . ? C18 C19 H19 119.9 . . ? C20 C19 H19 119.9 . . ? C19 C20 C15 120.5(2) . . ? C19 C20 H20 119.8 . . ? C15 C20 H20 119.8 . . ? C22 C21 C26 118.3(2) . . ? C22 C21 P1 123.05(18) . . ? C26 C21 P1 118.56(17) . . ? C23 C22 C21 120.2(2) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C24 C23 C22 120.4(2) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C25 C24 C23 120.0(2) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C26 C25 C24 120.0(2) . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C25 C26 C21 121.1(2) . . ? C25 C26 H26 119.5 . . ? C21 C26 H26 119.5 . . ? C32 C27 C28 114.9(2) . . ? C32 C27 B1 122.87(19) . . ? C28 C27 B1 122.17(19) . . ? C29 C28 C27 122.7(2) . . ? C29 C28 H28 118.6 . . ? C27 C28 H28 118.6 . . ? C30 C29 C28 120.3(2) . . ? C30 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? C31 C30 C29 118.7(2) . . ? C31 C30 H30 120.6 . . ? C29 C30 H30 120.6 . . ? C30 C31 C32 120.4(2) . . ? C30 C31 H31 119.8 . . ? C32 C31 H31 119.8 . . ? C31 C32 C27 122.9(2) . . ? C31 C32 H32 118.6 . . ? C27 C32 H32 118.6 . . ? C34 C33 C38 114.7(2) . . ? C34 C33 B1 123.49(19) . . ? C38 C33 B1 121.75(19) . . ? C35 C34 C33 122.5(2) . . ? C35 C34 H34 118.8 . . ? C33 C34 H34 118.8 . . ? C36 C35 C34 120.5(2) . . ? C36 C35 H35 119.7 . . ? C34 C35 H35 119.7 . . ? C35 C36 C37 118.9(2) . . ? C35 C36 H36 120.6 . . ? C37 C36 H36 120.6 . . ? C38 C37 C36 119.9(2) . . ? C38 C37 H37 120.1 . . ? C36 C37 H37 120.1 . . ? C37 C38 C33 123.5(2) . . ? C37 C38 H38 118.2 . . ? C33 C38 H38 118.2 . . ? C44 C39 C40 114.6(2) . . ? C44 C39 B1 122.98(19) . . ? C40 C39 B1 122.43(19) . . ? C41 C40 C39 123.5(2) . . ? C41 C40 H40 118.3 . . ? C39 C40 H40 118.3 . . ? C42 C41 C40 119.7(2) . . ? C42 C41 H41 120.2 . . ? C40 C41 H41 120.2 . . ? C43 C42 C41 119.0(2) . . ? C43 C42 H42 120.5 . . ? C41 C42 H42 120.5 . . ? C42 C43 C44 120.3(2) . . ? C42 C43 H43 119.8 . . ? C44 C43 H43 119.8 . . ? C43 C44 C39 123.0(2) . . ? C43 C44 H44 118.5 . . ? C39 C44 H44 118.5 . . ? C50 C45 C46 115.1(2) . . ? C50 C45 B1 122.87(19) . . ? C46 C45 B1 122.03(19) . . ? C47 C46 C45 122.5(2) . . ? C47 C46 H46 118.8 . . ? C45 C46 H46 118.8 . . ? C48 C47 C46 120.6(2) . . ? C48 C47 H47 119.7 . . ? C46 C47 H47 119.7 . . ? C49 C48 C47 118.5(2) . . ? C49 C48 H48 120.7 . . ? C47 C48 H48 120.7 . . ? C48 C49 C50 120.1(2) . . ? C48 C49 H49 119.9 . . ? C50 C49 H49 119.9 . . ? C49 C50 C45 123.2(2) . . ? C49 C50 H50 118.4 . . ? C45 C50 H50 118.4 . . ? C33 B1 C27 109.79(17) . . ? C33 B1 C45 110.03(17) . . ? C27 B1 C45 109.78(18) . . ? C33 B1 C39 109.58(18) . . ? C27 B1 C39 108.68(17) . . ? C45 B1 C39 108.96(17) . . ? Cl1 C51 Cl2 114.44(17) . . ? Cl1 C51 H51A 108.7 . . ? Cl2 C51 H51A 108.7 . . ? Cl1 C51 H51B 108.7 . . ? Cl2 C51 H51B 108.7 . . ? H51A C51 H51B 107.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 Rh1 P1 C13 167.81(10) . . . . ? N1 Rh1 P1 C13 -32.34(9) . . . . ? C6 Rh1 P1 C13 129.81(10) . . . . ? C1 Rh1 P1 C13 59.4(2) . . . . ? C2 Rh1 P1 C13 -139.0(2) . . . . ? C5 Rh1 P1 C21 51.54(11) . . . . ? N1 Rh1 P1 C21 -148.61(10) . . . . ? C6 Rh1 P1 C21 13.55(11) . . . . ? C1 Rh1 P1 C21 -56.9(2) . . . . ? C2 Rh1 P1 C21 104.8(2) . . . . ? C5 Rh1 P1 C15 -73.34(10) . . . . ? N1 Rh1 P1 C15 86.51(9) . . . . ? C6 Rh1 P1 C15 -111.34(10) . . . . ? C1 Rh1 P1 C15 178.3(2) . . . . ? C2 Rh1 P1 C15 -20.1(2) . . . . ? C5 Rh1 N1 C11 97.3(3) . . . . ? C6 Rh1 N1 C11 -90.3(3) . . . . ? C1 Rh1 N1 C11 -151.91(19) . . . . ? C2 Rh1 N1 C11 172.76(19) . . . . ? P1 Rh1 N1 C11 8.17(19) . . . . ? C5 Rh1 N1 C9 -80.8(3) . . . . ? C6 Rh1 N1 C9 91.6(3) . . . . ? C1 Rh1 N1 C9 30.00(18) . . . . ? C2 Rh1 N1 C9 -5.33(18) . . . . ? P1 Rh1 N1 C9 -169.92(16) . . . . ? C5 Rh1 C1 C2 63.90(15) . . . . ? N1 Rh1 C1 C2 -97.20(15) . . . . ? C6 Rh1 C1 C2 98.82(15) . . . . ? P1 Rh1 C1 C2 171.37(15) . . . . ? C5 Rh1 C1 C8 -58.58(17) . . . . ? N1 Rh1 C1 C8 140.32(16) . . . . ? C6 Rh1 C1 C8 -23.66(16) . . . . ? C2 Rh1 C1 C8 -122.5(2) . . . . ? P1 Rh1 C1 C8 48.9(3) . . . . ? C8 C1 C2 C3 -3.1(4) . . . . ? Rh1 C1 C2 C3 -103.4(2) . . . . ? C8 C1 C2 Rh1 100.3(2) . . . . ? C5 Rh1 C2 C1 -114.96(16) . . . . ? N1 Rh1 C2 C1 84.82(15) . . . . ? C6 Rh1 C2 C1 -77.27(15) . . . . ? P1 Rh1 C2 C1 -169.33(18) . . . . ? C5 Rh1 C2 C3 5.09(16) . . . . ? N1 Rh1 C2 C3 -155.13(16) . . . . ? C6 Rh1 C2 C3 42.78(17) . . . . ? C1 Rh1 C2 C3 120.0(2) . . . . ? P1 Rh1 C2 C3 -49.3(3) . . . . ? C1 C2 C3 C4 95.7(3) . . . . ? Rh1 C2 C3 C4 14.5(2) . . . . ? C2 C3 C4 C5 -36.0(3) . . . . ? C3 C4 C5 C6 -41.2(3) . . . . ? C3 C4 C5 Rh1 40.2(2) . . . . ? N1 Rh1 C5 C6 176.16(19) . . . . ? C1 Rh1 C5 C6 66.18(15) . . . . ? C2 Rh1 C5 C6 98.13(15) . . . . ? P1 Rh1 C5 C6 -94.84(13) . . . . ? N1 Rh1 C5 C4 54.1(3) . . . . ? C6 Rh1 C5 C4 -122.1(2) . . . . ? C1 Rh1 C5 C4 -55.91(17) . . . . ? C2 Rh1 C5 C4 -23.96(16) . . . . ? P1 Rh1 C5 C4 143.06(16) . . . . ? C4 C5 C6 C7 -4.2(4) . . . . ? Rh1 C5 C6 C7 -106.5(2) . . . . ? C4 C5 C6 Rh1 102.4(2) . . . . ? N1 Rh1 C6 C5 -175.7(2) . . . . ? C1 Rh1 C6 C5 -112.63(15) . . . . ? C2 Rh1 C6 C5 -77.57(15) . . . . ? P1 Rh1 C6 C5 86.38(14) . . . . ? C5 Rh1 C6 C7 119.7(2) . . . . ? N1 Rh1 C6 C7 -56.1(3) . . . . ? C1 Rh1 C6 C7 7.04(17) . . . . ? C2 Rh1 C6 C7 42.10(17) . . . . ? P1 Rh1 C6 C7 -153.95(16) . . . . ? C5 C6 C7 C8 93.2(3) . . . . ? Rh1 C6 C7 C8 11.0(3) . . . . ? C2 C1 C8 C7 -44.5(3) . . . . ? Rh1 C1 C8 C7 37.2(2) . . . . ? C6 C7 C8 C1 -32.8(3) . . . . ? C11 N1 C9 C10 -0.3(2) . . . . ? Rh1 N1 C9 C10 178.20(15) . . . . ? N1 C9 C10 N2 0.8(3) . . . . ? C11 N2 C10 C9 -0.9(2) . . . . ? C14 N2 C10 C9 -176.6(2) . . . . ? C9 N1 C11 N2 -0.3(2) . . . . ? Rh1 N1 C11 N2 -178.63(14) . . . . ? C9 N1 C11 C12 176.2(2) . . . . ? Rh1 N1 C11 C12 -2.1(3) . . . . ? C10 N2 C11 N1 0.8(2) . . . . ? C14 N2 C11 N1 176.3(2) . . . . ? C10 N2 C11 C12 -176.19(19) . . . . ? C14 N2 C11 C12 -0.6(3) . . . . ? N1 C11 C12 C13 25.2(3) . . . . ? N2 C11 C12 C13 -158.55(19) . . . . ? C11 C12 C13 P1 -55.8(2) . . . . ? C21 P1 C13 C12 -173.75(16) . . . . ? C15 P1 C13 C12 -64.18(18) . . . . ? Rh1 P1 C13 C12 60.74(17) . . . . ? C13 P1 C15 C16 139.33(18) . . . . ? C21 P1 C15 C16 -113.58(19) . . . . ? Rh1 P1 C15 C16 17.4(2) . . . . ? C13 P1 C15 C20 -39.7(2) . . . . ? C21 P1 C15 C20 67.3(2) . . . . ? Rh1 P1 C15 C20 -161.71(16) . . . . ? C20 C15 C16 C17 -0.5(3) . . . . ? P1 C15 C16 C17 -179.60(18) . . . . ? C15 C16 C17 C18 0.7(4) . . . . ? C16 C17 C18 C19 -0.3(4) . . . . ? C17 C18 C19 C20 -0.2(4) . . . . ? C18 C19 C20 C15 0.4(4) . . . . ? C16 C15 C20 C19 -0.1(3) . . . . ? P1 C15 C20 C19 179.03(18) . . . . ? C13 P1 C21 C22 128.3(2) . . . . ? C15 P1 C21 C22 19.0(2) . . . . ? Rh1 P1 C21 C22 -110.72(19) . . . . ? C13 P1 C21 C26 -54.7(2) . . . . ? C15 P1 C21 C26 -163.98(19) . . . . ? Rh1 P1 C21 C26 66.3(2) . . . . ? C26 C21 C22 C23 0.5(4) . . . . ? P1 C21 C22 C23 177.5(2) . . . . ? C21 C22 C23 C24 -0.5(4) . . . . ? C22 C23 C24 C25 0.0(4) . . . . ? C23 C24 C25 C26 0.4(4) . . . . ? C24 C25 C26 C21 -0.3(4) . . . . ? C22 C21 C26 C25 -0.1(4) . . . . ? P1 C21 C26 C25 -177.3(2) . . . . ? C32 C27 C28 C29 2.4(3) . . . . ? B1 C27 C28 C29 -175.0(2) . . . . ? C27 C28 C29 C30 -1.0(3) . . . . ? C28 C29 C30 C31 -0.6(3) . . . . ? C29 C30 C31 C32 0.6(3) . . . . ? C30 C31 C32 C27 0.9(3) . . . . ? C28 C27 C32 C31 -2.3(3) . . . . ? B1 C27 C32 C31 175.0(2) . . . . ? C38 C33 C34 C35 -1.4(3) . . . . ? B1 C33 C34 C35 180.0(2) . . . . ? C33 C34 C35 C36 0.8(3) . . . . ? C34 C35 C36 C37 0.3(3) . . . . ? C35 C36 C37 C38 -0.6(3) . . . . ? C36 C37 C38 C33 -0.2(4) . . . . ? C34 C33 C38 C37 1.2(3) . . . . ? B1 C33 C38 C37 179.8(2) . . . . ? C44 C39 C40 C41 0.0(3) . . . . ? B1 C39 C40 C41 178.1(2) . . . . ? C39 C40 C41 C42 0.5(4) . . . . ? C40 C41 C42 C43 -0.8(3) . . . . ? C41 C42 C43 C44 0.5(3) . . . . ? C42 C43 C44 C39 0.0(3) . . . . ? C40 C39 C44 C43 -0.3(3) . . . . ? B1 C39 C44 C43 -178.4(2) . . . . ? C50 C45 C46 C47 0.8(3) . . . . ? B1 C45 C46 C47 179.6(2) . . . . ? C45 C46 C47 C48 -0.1(4) . . . . ? C46 C47 C48 C49 -0.5(4) . . . . ? C47 C48 C49 C50 0.4(4) . . . . ? C48 C49 C50 C45 0.3(4) . . . . ? C46 C45 C50 C49 -0.9(3) . . . . ? B1 C45 C50 C49 -179.8(2) . . . . ? C34 C33 B1 C27 99.3(2) . . . . ? C38 C33 B1 C27 -79.2(2) . . . . ? C34 C33 B1 C45 -21.6(3) . . . . ? C38 C33 B1 C45 159.92(19) . . . . ? C34 C33 B1 C39 -141.4(2) . . . . ? C38 C33 B1 C39 40.1(3) . . . . ? C32 C27 B1 C33 17.8(3) . . . . ? C28 C27 B1 C33 -165.12(19) . . . . ? C32 C27 B1 C45 138.8(2) . . . . ? C28 C27 B1 C45 -44.0(3) . . . . ? C32 C27 B1 C39 -102.1(2) . . . . ? C28 C27 B1 C39 75.0(2) . . . . ? C50 C45 B1 C33 89.6(2) . . . . ? C46 C45 B1 C33 -89.2(2) . . . . ? C50 C45 B1 C27 -31.3(3) . . . . ? C46 C45 B1 C27 149.9(2) . . . . ? C50 C45 B1 C39 -150.2(2) . . . . ? C46 C45 B1 C39 31.0(3) . . . . ? C44 C39 B1 C33 -150.68(19) . . . . ? C40 C39 B1 C33 31.4(3) . . . . ? C44 C39 B1 C27 -30.7(3) . . . . ? C40 C39 B1 C27 151.3(2) . . . . ? C44 C39 B1 C45 88.9(2) . . . . ? C40 C39 B1 C45 -89.1(2) . . . . ? _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 0.565 _refine_diff_density_min -0.369 _refine_diff_density_rms 0.073 # Attachment 'bam14.cif' data_bam14 _database_code_depnum_ccdc_archive 'CCDC 711457' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H21 Cl N2 O P Rh' _chemical_formula_weight 378.64 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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/c ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? 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 16.711(7) _cell_length_b 7.318(3) _cell_length_c 12.865(5) _cell_angle_alpha 90.00 _cell_angle_beta 98.043(6) _cell_angle_gamma 90.00 _cell_volume 1557.7(11) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1012 _cell_measurement_theta_min 2.462 _cell_measurement_theta_max 27.906 _exptl_crystal_description blade _exptl_crystal_colour yellow _exptl_crystal_size_max 0.445 _exptl_crystal_size_mid 0.146 _exptl_crystal_size_min 0.038 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.614 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 1.361 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.629 _exptl_absorpt_correction_T_max 0.948 _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 178 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.02 _diffrn_reflns_number 14330 _diffrn_reflns_av_R_equivalents 0.0462 _diffrn_reflns_av_sigmaI/netI 0.0339 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 28.29 _reflns_number_total 3710 _reflns_number_gt 3181 _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^)+(0.02P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3710 _refine_ls_number_parameters 168 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0283 _refine_ls_R_factor_gt 0.0215 _refine_ls_wR_factor_ref 0.0531 _refine_ls_wR_factor_gt 0.0512 _refine_ls_goodness_of_fit_ref 1.168 _refine_ls_restrained_S_all 1.168 _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 0.241749(9) 0.948915(18) 0.122846(11) 0.01930(6) Uani 1 1 d . . . Cl1 Cl 0.16749(3) 1.12678(6) -0.01476(4) 0.02721(11) Uani 1 1 d . . . P1 P 0.29079(3) 0.76969(6) 0.25606(4) 0.01916(11) Uani 1 1 d . . . O1 O 0.39086(10) 1.1715(2) 0.14224(13) 0.0437(4) Uani 1 1 d . . . N1 N 0.14332(10) 0.7726(2) 0.12118(11) 0.0215(3) Uani 1 1 d . . . N2 N 0.08167(10) 0.5230(2) 0.16161(12) 0.0236(3) Uani 1 1 d . . . C1 C 0.33224(13) 1.0862(3) 0.13361(16) 0.0270(4) Uani 1 1 d . . . C2 C 0.06359(12) 0.7828(3) 0.07672(15) 0.0260(4) Uani 1 1 d . . . H2 H 0.0396 0.8812 0.0354 0.031 Uiso 1 1 calc R . . C3 C 0.02489(12) 0.6299(3) 0.10146(15) 0.0266(4) Uani 1 1 d . . . H3 H -0.0306 0.6016 0.0814 0.032 Uiso 1 1 calc R . . C4 C 0.15211(12) 0.6136(2) 0.17251(14) 0.0212(4) Uani 1 1 d . . . C5 C 0.23035(12) 0.5576(2) 0.23415(15) 0.0228(4) Uani 1 1 d . . . H5A H 0.2583 0.4672 0.1946 0.027 Uiso 1 1 calc R . . H5B H 0.2215 0.5027 0.3019 0.027 Uiso 1 1 calc R . . C6 C 0.06808(14) 0.3401(3) 0.20279(16) 0.0326(5) Uani 1 1 d . . . H6A H 0.0933 0.2484 0.1624 0.049 Uiso 1 1 calc R . . H6B H 0.0099 0.3166 0.1967 0.049 Uiso 1 1 calc R . . H6C H 0.0920 0.3334 0.2767 0.049 Uiso 1 1 calc R . . C7 C 0.39701(12) 0.6944(3) 0.27892(15) 0.0247(4) Uani 1 1 d . . . H7 H 0.4301 0.8018 0.3071 0.030 Uiso 1 1 calc R . . C8 C 0.42662(13) 0.6381(3) 0.17603(17) 0.0323(5) Uani 1 1 d . . . H8A H 0.4851 0.6174 0.1887 0.048 Uiso 1 1 calc R . . H8B H 0.4144 0.7356 0.1240 0.048 Uiso 1 1 calc R . . H8C H 0.3993 0.5255 0.1497 0.048 Uiso 1 1 calc R . . C9 C 0.41140(14) 0.5428(3) 0.36100(19) 0.0373(5) Uani 1 1 d . . . H9A H 0.3837 0.4313 0.3334 0.056 Uiso 1 1 calc R . . H9B H 0.3903 0.5809 0.4249 0.056 Uiso 1 1 calc R . . H9C H 0.4695 0.5189 0.3773 0.056 Uiso 1 1 calc R . . C10 C 0.26954(12) 0.8553(3) 0.38393(14) 0.0235(4) Uani 1 1 d . . . H10 H 0.2857 0.7594 0.4382 0.028 Uiso 1 1 calc R . . C11 C 0.17906(13) 0.8937(3) 0.38049(16) 0.0293(5) Uani 1 1 d . . . H11A H 0.1692 0.9469 0.4475 0.044 Uiso 1 1 calc R . . H11B H 0.1488 0.7792 0.3684 0.044 Uiso 1 1 calc R . . H11C H 0.1613 0.9796 0.3234 0.044 Uiso 1 1 calc R . . C12 C 0.31894(15) 1.0275(3) 0.41418(17) 0.0362(5) Uani 1 1 d . . . H12A H 0.3053 1.1213 0.3602 0.054 Uiso 1 1 calc R . . H12B H 0.3767 0.9987 0.4200 0.054 Uiso 1 1 calc R . . H12C H 0.3066 1.0731 0.4818 0.054 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.02070(9) 0.01751(8) 0.01933(8) 0.00212(5) 0.00154(6) 0.00063(6) Cl1 0.0313(3) 0.0261(2) 0.0231(2) 0.00925(18) -0.0001(2) 0.0046(2) P1 0.0185(2) 0.0178(2) 0.0207(2) 0.00142(18) 0.00084(19) 0.00056(19) O1 0.0319(9) 0.0343(8) 0.0631(11) 0.0085(8) 0.0003(8) -0.0098(7) N1 0.0219(8) 0.0214(8) 0.0208(8) 0.0000(6) 0.0014(6) 0.0005(7) N2 0.0233(9) 0.0260(8) 0.0213(8) -0.0029(6) 0.0032(7) -0.0049(7) C1 0.0315(12) 0.0197(9) 0.0292(10) 0.0047(8) 0.0020(9) 0.0041(8) C2 0.0230(10) 0.0316(10) 0.0224(10) -0.0036(8) 0.0001(8) 0.0044(8) C3 0.0204(10) 0.0350(11) 0.0233(9) -0.0077(8) -0.0004(8) -0.0004(9) C4 0.0210(10) 0.0234(9) 0.0194(9) -0.0033(7) 0.0038(8) -0.0011(8) C5 0.0235(10) 0.0185(9) 0.0256(10) 0.0022(7) 0.0005(8) -0.0016(8) C6 0.0350(12) 0.0314(11) 0.0313(11) 0.0022(9) 0.0041(9) -0.0130(9) C7 0.0198(10) 0.0234(9) 0.0302(10) 0.0012(8) 0.0004(8) 0.0003(8) C8 0.0260(11) 0.0328(11) 0.0388(12) 0.0001(9) 0.0075(9) 0.0046(9) C9 0.0291(12) 0.0406(13) 0.0410(13) 0.0126(10) 0.0005(10) 0.0131(10) C10 0.0282(11) 0.0234(9) 0.0186(9) 0.0022(7) 0.0031(8) 0.0025(8) C11 0.0316(12) 0.0312(11) 0.0262(10) 0.0013(8) 0.0083(9) 0.0049(9) C12 0.0400(14) 0.0369(12) 0.0309(12) -0.0109(9) 0.0024(10) -0.0037(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C1 1.804(2) . ? Rh1 N1 2.0882(17) . ? Rh1 P1 2.2217(7) . ? Rh1 Cl1 2.3986(7) . ? P1 C10 1.841(2) . ? P1 C7 1.842(2) . ? P1 C5 1.8518(19) . ? O1 C1 1.154(3) . ? N1 C4 1.336(2) . ? N1 C2 1.376(3) . ? N2 C4 1.341(3) . ? N2 C3 1.380(3) . ? N2 C6 1.469(2) . ? C2 C3 1.352(3) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 C5 1.489(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C9 1.527(3) . ? C7 C8 1.533(3) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C12 1.527(3) . ? C10 C11 1.532(3) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 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 C1 Rh1 N1 174.33(7) . . ? C1 Rh1 P1 93.13(6) . . ? N1 Rh1 P1 81.27(5) . . ? C1 Rh1 Cl1 95.51(7) . . ? N1 Rh1 Cl1 90.13(5) . . ? P1 Rh1 Cl1 170.608(19) . . ? C10 P1 C7 105.14(9) . . ? C10 P1 C5 104.60(9) . . ? C7 P1 C5 105.45(9) . . ? C10 P1 Rh1 113.08(7) . . ? C7 P1 Rh1 122.88(6) . . ? C5 P1 Rh1 104.06(6) . . ? C4 N1 C2 106.59(16) . . ? C4 N1 Rh1 120.08(13) . . ? C2 N1 Rh1 133.32(13) . . ? C4 N2 C3 107.63(16) . . ? C4 N2 C6 126.18(17) . . ? C3 N2 C6 126.15(17) . . ? O1 C1 Rh1 178.52(18) . . ? C3 C2 N1 108.93(18) . . ? C3 C2 H2 125.5 . . ? N1 C2 H2 125.5 . . ? C2 C3 N2 106.68(17) . . ? C2 C3 H3 126.7 . . ? N2 C3 H3 126.7 . . ? N1 C4 N2 110.15(17) . . ? N1 C4 C5 122.05(17) . . ? N2 C4 C5 127.76(17) . . ? C4 C5 P1 105.67(12) . . ? C4 C5 H5A 110.6 . . ? P1 C5 H5A 110.6 . . ? C4 C5 H5B 110.6 . . ? P1 C5 H5B 110.6 . . ? H5A C5 H5B 108.7 . . ? N2 C6 H6A 109.5 . . ? N2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C9 C7 C8 111.31(17) . . ? C9 C7 P1 112.49(14) . . ? C8 C7 P1 111.25(14) . . ? C9 C7 H7 107.2 . . ? C8 C7 H7 107.2 . . ? P1 C7 H7 107.2 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C12 C10 C11 110.62(17) . . ? C12 C10 P1 110.10(14) . . ? C11 C10 P1 110.46(13) . . ? C12 C10 H10 108.5 . . ? C11 C10 H10 108.5 . . ? P1 C10 H10 108.5 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 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 C1 Rh1 P1 C10 89.06(10) . . . . ? N1 Rh1 P1 C10 -91.82(8) . . . . ? Cl1 Rh1 P1 C10 -67.94(14) . . . . ? C1 Rh1 P1 C7 -38.77(10) . . . . ? N1 Rh1 P1 C7 140.35(9) . . . . ? Cl1 Rh1 P1 C7 164.23(12) . . . . ? C1 Rh1 P1 C5 -158.04(9) . . . . ? N1 Rh1 P1 C5 21.08(8) . . . . ? Cl1 Rh1 P1 C5 44.97(14) . . . . ? C1 Rh1 N1 C4 -7.0(8) . . . . ? P1 Rh1 N1 C4 -15.90(13) . . . . ? Cl1 Rh1 N1 C4 167.89(13) . . . . ? C1 Rh1 N1 C2 171.9(7) . . . . ? P1 Rh1 N1 C2 163.04(17) . . . . ? Cl1 Rh1 N1 C2 -13.18(17) . . . . ? N1 Rh1 C1 O1 -7(9) . . . . ? P1 Rh1 C1 O1 2(8) . . . . ? Cl1 Rh1 C1 O1 178(100) . . . . ? C4 N1 C2 C3 0.0(2) . . . . ? Rh1 N1 C2 C3 -179.06(13) . . . . ? N1 C2 C3 N2 -0.4(2) . . . . ? C4 N2 C3 C2 0.6(2) . . . . ? C6 N2 C3 C2 -177.22(18) . . . . ? C2 N1 C4 N2 0.4(2) . . . . ? Rh1 N1 C4 N2 179.63(11) . . . . ? C2 N1 C4 C5 -177.73(17) . . . . ? Rh1 N1 C4 C5 1.5(2) . . . . ? C3 N2 C4 N1 -0.7(2) . . . . ? C6 N2 C4 N1 177.18(17) . . . . ? C3 N2 C4 C5 177.36(18) . . . . ? C6 N2 C4 C5 -4.8(3) . . . . ? N1 C4 C5 P1 17.5(2) . . . . ? N2 C4 C5 P1 -160.34(16) . . . . ? C10 P1 C5 C4 93.04(14) . . . . ? C7 P1 C5 C4 -156.35(13) . . . . ? Rh1 P1 C5 C4 -25.82(14) . . . . ? C10 P1 C7 C9 60.51(16) . . . . ? C5 P1 C7 C9 -49.71(17) . . . . ? Rh1 P1 C7 C9 -168.32(12) . . . . ? C10 P1 C7 C8 -173.83(14) . . . . ? C5 P1 C7 C8 75.95(15) . . . . ? Rh1 P1 C7 C8 -42.65(16) . . . . ? C7 P1 C10 C12 66.73(16) . . . . ? C5 P1 C10 C12 177.56(14) . . . . ? Rh1 P1 C10 C12 -69.86(15) . . . . ? C7 P1 C10 C11 -170.80(13) . . . . ? C5 P1 C10 C11 -59.97(15) . . . . ? Rh1 P1 C10 C11 52.60(15) . . . . ? _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 0.593 _refine_diff_density_min -0.261 _refine_diff_density_rms 0.074 # Attachment 'bam15.cif' data_bam15 _database_code_depnum_ccdc_archive 'CCDC 711458' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H19 Cl N2 O P Rh' _chemical_formula_weight 460.69 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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/c ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? 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 13.989(3) _cell_length_b 8.913(2) _cell_length_c 16.393(4) _cell_angle_alpha 90.00 _cell_angle_beta 111.975(4) _cell_angle_gamma 90.00 _cell_volume 1895.5(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 937 _cell_measurement_theta_min 3.424 _cell_measurement_theta_max 28.240 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.372 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.097 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.614 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 928 _exptl_absorpt_coefficient_mu 1.135 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.923 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ; SADABS (Sheldrick, 1996) ; _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 238 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.02 _diffrn_reflns_number 17968 _diffrn_reflns_av_R_equivalents 0.0375 _diffrn_reflns_av_sigmaI/netI 0.0278 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 28.33 _reflns_number_total 4508 _reflns_number_gt 3902 _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^+0.5P] 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 4508 _refine_ls_number_parameters 227 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0271 _refine_ls_R_factor_gt 0.0218 _refine_ls_wR_factor_ref 0.0595 _refine_ls_wR_factor_gt 0.0564 _refine_ls_goodness_of_fit_ref 1.162 _refine_ls_restrained_S_all 1.162 _refine_ls_shift/su_max 0.004 _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 0.338657(10) 0.810299(14) 0.273320(8) 0.02070(5) Uani 1 1 d . . . Cl1 Cl 0.39375(4) 1.04853(5) 0.34444(3) 0.03158(11) Uani 1 1 d . . . P1 P 0.28378(3) 0.59318(5) 0.20655(3) 0.01855(9) Uani 1 1 d . . . O1 O 0.16521(14) 0.97803(19) 0.14462(12) 0.0563(5) Uani 1 1 d . . . N1 N 0.46725(12) 0.69822(15) 0.36770(10) 0.0228(3) Uani 1 1 d . . . N2 N 0.58673(12) 0.53834(18) 0.44552(10) 0.0275(3) Uani 1 1 d . . . C1 C 0.23158(16) 0.9102(2) 0.19412(14) 0.0335(4) Uani 1 1 d . . . C2 C 0.53314(15) 0.7689(2) 0.44341(12) 0.0294(4) Uani 1 1 d . . . H2 H 0.5272 0.8701 0.4590 0.035 Uiso 1 1 calc R . . C3 C 0.60676(16) 0.6723(2) 0.49138(13) 0.0317(4) Uani 1 1 d . . . H3 H 0.6615 0.6921 0.5458 0.038 Uiso 1 1 calc R . . C4 C 0.50226(13) 0.55757(19) 0.37177(11) 0.0226(3) Uani 1 1 d . . . C5 C 0.45860(14) 0.42943(19) 0.31069(11) 0.0249(4) Uani 1 1 d . . . H5A H 0.4172 0.3670 0.3352 0.030 Uiso 1 1 calc R . . H5B H 0.5165 0.3668 0.3094 0.030 Uiso 1 1 calc R . . C6 C 0.39131(13) 0.47033(19) 0.21634(11) 0.0223(3) Uani 1 1 d . . . H6A H 0.3639 0.3769 0.1832 0.027 Uiso 1 1 calc R . . H6B H 0.4348 0.5200 0.1886 0.027 Uiso 1 1 calc R . . C7 C 0.64632(16) 0.4005(2) 0.47359(13) 0.0359(4) Uani 1 1 d . . . H7A H 0.6001 0.3180 0.4738 0.054 Uiso 1 1 calc R . . H7B H 0.6983 0.4140 0.5329 0.054 Uiso 1 1 calc R . . H7C H 0.6806 0.3768 0.4328 0.054 Uiso 1 1 calc R . . C8 C 0.20404(13) 0.48658(18) 0.25224(10) 0.0203(3) Uani 1 1 d . . . C9 C 0.15679(14) 0.5615(2) 0.30182(12) 0.0273(4) Uani 1 1 d . . . H9 H 0.1642 0.6671 0.3093 0.033 Uiso 1 1 calc R . . C10 C 0.09893(16) 0.4826(2) 0.34041(13) 0.0347(4) Uani 1 1 d . . . H10 H 0.0663 0.5343 0.3736 0.042 Uiso 1 1 calc R . . C11 C 0.08895(16) 0.3287(2) 0.33034(14) 0.0359(5) Uani 1 1 d . . . H11 H 0.0505 0.2745 0.3576 0.043 Uiso 1 1 calc R . . C12 C 0.13481(15) 0.2535(2) 0.28069(14) 0.0324(4) Uani 1 1 d . . . H12 H 0.1273 0.1478 0.2735 0.039 Uiso 1 1 calc R . . C13 C 0.19163(15) 0.3322(2) 0.24147(12) 0.0264(4) Uani 1 1 d . . . H13 H 0.2224 0.2802 0.2069 0.032 Uiso 1 1 calc R . . C14 C 0.20868(13) 0.59557(18) 0.08859(11) 0.0214(3) Uani 1 1 d . . . C15 C 0.10724(15) 0.6461(2) 0.05834(13) 0.0326(4) Uani 1 1 d . . . H15 H 0.0775 0.6744 0.0995 0.039 Uiso 1 1 calc R . . C16 C 0.04905(17) 0.6558(3) -0.03080(14) 0.0392(5) Uani 1 1 d . . . H16 H -0.0199 0.6915 -0.0506 0.047 Uiso 1 1 calc R . . C17 C 0.09183(17) 0.6133(2) -0.09104(13) 0.0356(5) Uani 1 1 d . . . H17 H 0.0518 0.6186 -0.1523 0.043 Uiso 1 1 calc R . . C18 C 0.19173(17) 0.5638(2) -0.06247(12) 0.0350(4) Uani 1 1 d . . . H18 H 0.2209 0.5356 -0.1040 0.042 Uiso 1 1 calc R . . C19 C 0.25078(15) 0.5543(2) 0.02728(12) 0.0274(4) Uani 1 1 d . . . H19 H 0.3199 0.5196 0.0466 0.033 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.02407(8) 0.01720(8) 0.02388(8) -0.00371(5) 0.01247(6) -0.00200(5) Cl1 0.0300(2) 0.0194(2) 0.0472(3) -0.01165(18) 0.0167(2) -0.00431(16) P1 0.0206(2) 0.01768(19) 0.0191(2) -0.00226(15) 0.00935(17) -0.00071(15) O1 0.0600(11) 0.0375(9) 0.0532(10) -0.0038(8) 0.0004(9) 0.0193(8) N1 0.0241(8) 0.0239(7) 0.0220(7) -0.0037(6) 0.0103(6) -0.0039(6) N2 0.0259(8) 0.0343(8) 0.0213(7) -0.0004(6) 0.0078(6) -0.0006(6) C1 0.0402(11) 0.0247(9) 0.0354(11) -0.0073(8) 0.0140(9) 0.0017(8) C2 0.0326(10) 0.0305(9) 0.0260(9) -0.0079(7) 0.0120(8) -0.0099(8) C3 0.0302(10) 0.0392(11) 0.0237(9) -0.0065(8) 0.0079(8) -0.0081(8) C4 0.0223(8) 0.0264(9) 0.0212(8) 0.0002(7) 0.0106(7) -0.0023(7) C5 0.0247(9) 0.0213(8) 0.0272(9) -0.0022(7) 0.0079(7) 0.0021(7) C6 0.0222(8) 0.0225(8) 0.0235(8) -0.0052(7) 0.0102(7) 0.0006(6) C7 0.0328(10) 0.0427(11) 0.0287(10) 0.0052(9) 0.0075(8) 0.0071(9) C8 0.0184(8) 0.0236(8) 0.0177(8) 0.0010(6) 0.0056(6) -0.0006(6) C9 0.0285(9) 0.0287(9) 0.0285(9) -0.0028(7) 0.0149(8) -0.0018(7) C10 0.0331(10) 0.0460(12) 0.0325(10) -0.0031(9) 0.0210(9) -0.0039(9) C11 0.0313(11) 0.0448(12) 0.0338(11) 0.0095(9) 0.0148(9) -0.0079(9) C12 0.0313(10) 0.0266(9) 0.0387(11) 0.0061(8) 0.0122(9) -0.0029(8) C13 0.0270(9) 0.0243(9) 0.0291(9) -0.0002(7) 0.0120(8) -0.0006(7) C14 0.0255(8) 0.0184(7) 0.0206(8) -0.0012(6) 0.0092(7) -0.0032(6) C15 0.0279(10) 0.0444(11) 0.0272(10) -0.0001(8) 0.0124(8) 0.0022(8) C16 0.0289(10) 0.0498(12) 0.0331(11) 0.0050(9) 0.0050(9) 0.0011(9) C17 0.0438(12) 0.0368(11) 0.0205(9) 0.0031(8) 0.0054(8) -0.0089(9) C18 0.0484(12) 0.0366(10) 0.0228(9) -0.0037(8) 0.0167(9) -0.0045(9) C19 0.0306(9) 0.0284(9) 0.0248(9) -0.0013(7) 0.0124(8) 0.0011(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 Rh1 C1 1.807(2) . ? Rh1 N1 2.1319(16) . ? Rh1 P1 2.2144(6) . ? Rh1 Cl1 2.4062(6) . ? P1 C6 1.8185(17) . ? P1 C14 1.8230(18) . ? P1 C8 1.8257(17) . ? O1 C1 1.150(3) . ? N1 C4 1.339(2) . ? N1 C2 1.390(2) . ? N2 C4 1.348(2) . ? N2 C3 1.382(2) . ? N2 C7 1.459(3) . ? C2 C3 1.347(3) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 C5 1.491(2) . ? C5 C6 1.524(2) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C13 1.390(2) . ? C8 C9 1.395(2) . ? C9 C10 1.391(3) . ? C9 H9 0.9500 . ? C10 C11 1.382(3) . ? C10 H10 0.9500 . ? C11 C12 1.384(3) . ? C11 H11 0.9500 . ? C12 C13 1.386(3) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C19 1.391(2) . ? C14 C15 1.391(3) . ? C15 C16 1.384(3) . ? C15 H15 0.9500 . ? C16 C17 1.385(3) . ? C16 H16 0.9500 . ? C17 C18 1.370(3) . ? C17 H17 0.9500 . ? C18 C19 1.394(3) . ? C18 H18 0.9500 . ? C19 H19 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 C1 Rh1 N1 178.41(7) . . ? C1 Rh1 P1 91.98(6) . . ? N1 Rh1 P1 89.51(4) . . ? C1 Rh1 Cl1 86.70(6) . . ? N1 Rh1 Cl1 91.81(4) . . ? P1 Rh1 Cl1 178.515(16) . . ? C6 P1 C14 103.29(8) . . ? C6 P1 C8 105.23(8) . . ? C14 P1 C8 104.07(8) . . ? C6 P1 Rh1 111.12(6) . . ? C14 P1 Rh1 118.01(5) . . ? C8 P1 Rh1 113.84(6) . . ? C4 N1 C2 105.79(15) . . ? C4 N1 Rh1 131.97(12) . . ? C2 N1 Rh1 122.23(12) . . ? C4 N2 C3 108.01(16) . . ? C4 N2 C7 126.53(16) . . ? C3 N2 C7 125.45(16) . . ? O1 C1 Rh1 177.76(19) . . ? C3 C2 N1 109.76(17) . . ? C3 C2 H2 125.1 . . ? N1 C2 H2 125.1 . . ? C2 C3 N2 106.23(16) . . ? C2 C3 H3 126.9 . . ? N2 C3 H3 126.9 . . ? N1 C4 N2 110.20(15) . . ? N1 C4 C5 129.33(16) . . ? N2 C4 C5 120.41(16) . . ? C4 C5 C6 116.15(14) . . ? C4 C5 H5A 108.2 . . ? C6 C5 H5A 108.2 . . ? C4 C5 H5B 108.2 . . ? C6 C5 H5B 108.2 . . ? H5A C5 H5B 107.4 . . ? C5 C6 P1 114.20(12) . . ? C5 C6 H6A 108.7 . . ? P1 C6 H6A 108.7 . . ? C5 C6 H6B 108.7 . . ? P1 C6 H6B 108.7 . . ? H6A C6 H6B 107.6 . . ? N2 C7 H7A 109.5 . . ? N2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C13 C8 C9 118.97(16) . . ? C13 C8 P1 121.97(13) . . ? C9 C8 P1 119.03(13) . . ? C10 C9 C8 120.40(17) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C11 C10 C9 119.85(18) . . ? C11 C10 H10 120.1 . . ? C9 C10 H10 120.1 . . ? C10 C11 C12 120.19(18) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C11 C12 C13 120.02(18) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C12 C13 C8 120.55(18) . . ? C12 C13 H13 119.7 . . ? C8 C13 H13 119.7 . . ? C19 C14 C15 118.62(17) . . ? C19 C14 P1 122.11(14) . . ? C15 C14 P1 119.21(13) . . ? C16 C15 C14 121.00(18) . . ? C16 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? C15 C16 C17 119.7(2) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? C18 C17 C16 120.12(18) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C17 C18 C19 120.39(18) . . ? C17 C18 H18 119.8 . . ? C19 C18 H18 119.8 . . ? C14 C19 C18 120.17(18) . . ? C14 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Rh1 P1 C6 147.17(9) . . . . ? N1 Rh1 P1 C6 -32.28(7) . . . . ? Cl1 Rh1 P1 C6 175(12) . . . . ? C1 Rh1 P1 C14 28.17(9) . . . . ? N1 Rh1 P1 C14 -151.28(8) . . . . ? Cl1 Rh1 P1 C14 55.6(7) . . . . ? C1 Rh1 P1 C8 -94.25(9) . . . . ? N1 Rh1 P1 C8 86.30(7) . . . . ? Cl1 Rh1 P1 C8 -66.8(7) . . . . ? C1 Rh1 N1 C4 -151(3) . . . . ? P1 Rh1 N1 C4 8.39(15) . . . . ? Cl1 Rh1 N1 C4 -172.28(15) . . . . ? C1 Rh1 N1 C2 30(3) . . . . ? P1 Rh1 N1 C2 -170.26(13) . . . . ? Cl1 Rh1 N1 C2 9.07(13) . . . . ? N1 Rh1 C1 O1 -3(7) . . . . ? P1 Rh1 C1 O1 -163(5) . . . . ? Cl1 Rh1 C1 O1 18(5) . . . . ? C4 N1 C2 C3 0.6(2) . . . . ? Rh1 N1 C2 C3 179.51(13) . . . . ? N1 C2 C3 N2 -0.3(2) . . . . ? C4 N2 C3 C2 0.0(2) . . . . ? C7 N2 C3 C2 -179.13(18) . . . . ? C2 N1 C4 N2 -0.58(19) . . . . ? Rh1 N1 C4 N2 -179.39(11) . . . . ? C2 N1 C4 C5 176.55(17) . . . . ? Rh1 N1 C4 C5 -2.3(3) . . . . ? C3 N2 C4 N1 0.4(2) . . . . ? C7 N2 C4 N1 179.47(17) . . . . ? C3 N2 C4 C5 -177.03(16) . . . . ? C7 N2 C4 C5 2.0(3) . . . . ? N1 C4 C5 C6 24.9(3) . . . . ? N2 C4 C5 C6 -158.19(15) . . . . ? C4 C5 C6 P1 -55.36(19) . . . . ? C14 P1 C6 C5 -171.21(12) . . . . ? C8 P1 C6 C5 -62.35(14) . . . . ? Rh1 P1 C6 C5 61.30(13) . . . . ? C6 P1 C8 C13 -35.76(17) . . . . ? C14 P1 C8 C13 72.53(16) . . . . ? Rh1 P1 C8 C13 -157.67(13) . . . . ? C6 P1 C8 C9 142.15(14) . . . . ? C14 P1 C8 C9 -109.56(14) . . . . ? Rh1 P1 C8 C9 20.24(15) . . . . ? C13 C8 C9 C10 0.5(3) . . . . ? P1 C8 C9 C10 -177.44(15) . . . . ? C8 C9 C10 C11 0.6(3) . . . . ? C9 C10 C11 C12 -1.2(3) . . . . ? C10 C11 C12 C13 0.5(3) . . . . ? C11 C12 C13 C8 0.7(3) . . . . ? C9 C8 C13 C12 -1.2(3) . . . . ? P1 C8 C13 C12 176.73(14) . . . . ? C6 P1 C14 C19 -19.40(16) . . . . ? C8 P1 C14 C19 -129.12(15) . . . . ? Rh1 P1 C14 C19 103.63(14) . . . . ? C6 P1 C14 C15 163.36(15) . . . . ? C8 P1 C14 C15 53.63(16) . . . . ? Rh1 P1 C14 C15 -73.61(16) . . . . ? C19 C14 C15 C16 -0.2(3) . . . . ? P1 C14 C15 C16 177.18(17) . . . . ? C14 C15 C16 C17 0.6(3) . . . . ? C15 C16 C17 C18 -0.8(3) . . . . ? C16 C17 C18 C19 0.6(3) . . . . ? C15 C14 C19 C18 -0.1(3) . . . . ? P1 C14 C19 C18 -177.34(14) . . . . ? C17 C18 C19 C14 -0.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.955 _refine_diff_density_max 0.577 _refine_diff_density_min -0.402 _refine_diff_density_rms 0.069