Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Barbara A. Messerle' _publ_contact_author_address ; School of Chemical Sciences University of New South Wales NSW 2052, Australia ; _publ_contact_author_email b.messerle@unsw.edu.au _publ_contact_author_fax +61-2-9385-6141 _publ_contact_author_phone +61-2-9385-4653 _publ_section_title ; Rhodium(I) and Iridium(I) Complexes with Bidentate N,N and P,N Ligands as Catalysts for the Hydrothiolation of Alkynes. ; loop_ _publ_author_name _publ_author_address 'Suzanne Burling' ; School of Chemistry, University of Sydney, NSW 2006, Australia ; 'Leslie D. Field' ; School of Chemistry, University of Sydney, NSW 2006, Australia ; 'Barbara A. Messerle' ; School of Chemical Sciences, University of New South Wales, NSW 2052, Australia ; 'Khuong Q. Vuong' ; School of Chemical Sciences, University of New South Wales, NSW 2052, Australia ; 'Peter Turner' ; School of Chemistry, University of Sydney, NSW 2006, Australia ; data_bam5 _database_code_CSD 207600 _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 orthorhombic _symmetry_space_group_name_H-M 'F d d 2 ' _symmetry_Int_Tables_number 43 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 34.832(8) _cell_length_b 55.975(13) _cell_length_c 8.1474(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 15885(6) _cell_formula_units_Z 16 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1020 _cell_measurement_theta_min 2.593 _cell_measurement_theta_max 28.292 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.417 _exptl_crystal_size_mid 0.251 _exptl_crystal_size_min 0.178 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.505 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7264 _exptl_absorpt_coefficient_mu 3.440 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.316 _exptl_absorpt_correction_T_max 0.567 _exptl_absorpt_process_details ; Gaussian (Coppens et al., 1965) XPREP (Bruker, 1995) ; _exptl_special_details ; ? ; _diffrn_crystal_treatment ; attached with Exxon Paratone N, to a short length of fibre supported on a thin piece of copper wire inserted in a copper mounting pin. The crystal was quenched in a cold nitrogen gas stream from an Oxford Cryosystems Cryostream. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 663 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.2 _diffrn_reflns_number 39465 _diffrn_reflns_av_R_equivalents 0.0362 _diffrn_reflns_av_sigmaI/netI 0.0185 _diffrn_reflns_limit_h_min -46 _diffrn_reflns_limit_h_max 46 _diffrn_reflns_limit_k_min -74 _diffrn_reflns_limit_k_max 74 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 28.34 _reflns_number_total 9565 _reflns_number_gt 9216 _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), XSHELL (Bruker, 2000) 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^)+(0.0100P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.000(3) _refine_ls_number_reflns 9565 _refine_ls_number_parameters 503 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0190 _refine_ls_R_factor_gt 0.0179 _refine_ls_wR_factor_ref 0.0363 _refine_ls_wR_factor_gt 0.0362 _refine_ls_goodness_of_fit_ref 1.590 _refine_ls_restrained_S_all 1.590 _refine_ls_shift/su_max 0.003 _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 0.090916(2) 0.053174(2) 0.464048(13) 0.01715(2) Uani 1 1 d . . . P1 P 0.149270(18) 0.059337(12) 0.58761(8) 0.01892(13) Uani 1 1 d . . . N1 N 0.06502(6) 0.07442(4) 0.6430(2) 0.0202(4) Uani 1 1 d . . . N2 N 0.08046(5) 0.09515(3) 0.7020(3) 0.0207(4) Uani 1 1 d . . . C1 C 0.03540(8) 0.05412(5) 0.3295(3) 0.0224(6) Uani 1 1 d . . . H1 H 0.0222(7) 0.0654(5) 0.382(3) 0.018(7) Uiso 1 1 d . . . C2 C 0.03911(7) 0.03201(5) 0.4037(3) 0.0225(6) Uani 1 1 d . . . H2 H 0.0288(6) 0.0296(4) 0.507(3) 0.011(6) Uiso 1 1 d . . . C3 C 0.04894(7) 0.00915(5) 0.3104(3) 0.0247(6) Uani 1 1 d . . . H3A H 0.0408 0.0109 0.1946 0.030 Uiso 1 1 calc R . . H3B H 0.0344 -0.0043 0.3584 0.030 Uiso 1 1 calc R . . C4 C 0.09192(7) 0.00328(5) 0.3154(3) 0.0251(6) Uani 1 1 d . . . H4A H 0.0973 -0.0067 0.4131 0.030 Uiso 1 1 calc R . . H4B H 0.0987 -0.0061 0.2168 0.030 Uiso 1 1 calc R . . C5 C 0.11662(7) 0.02518(5) 0.3218(3) 0.0223(5) Uani 1 1 d . . . H5 H 0.1410(8) 0.0207(5) 0.356(3) 0.026(7) Uiso 1 1 d . . . C6 C 0.11171(7) 0.04557(4) 0.2243(4) 0.0225(5) Uani 1 1 d . . . H6 H 0.1343(7) 0.0551(4) 0.202(3) 0.015(6) Uiso 1 1 d . . . C7 C 0.08141(8) 0.04800(5) 0.0899(3) 0.0278(6) Uani 1 1 d . . . H7A H 0.0760 0.0320 0.0434 0.033 Uiso 1 1 calc R . . H7B H 0.0918 0.0581 0.0006 0.033 Uiso 1 1 calc R . . C8 C 0.04374(8) 0.05896(5) 0.1510(3) 0.0265(6) Uani 1 1 d . . . H8A H 0.0447 0.0765 0.1337 0.032 Uiso 1 1 calc R . . H8B H 0.0223 0.0526 0.0841 0.032 Uiso 1 1 calc R . . C9 C 0.03097(6) 0.07214(4) 0.7201(4) 0.0234(5) Uani 1 1 d . . . H9 H 0.0136 0.0593 0.7042 0.028 Uiso 1 1 calc R . . C10 C 0.02470(7) 0.09116(5) 0.8256(3) 0.0248(6) Uani 1 1 d . . . H10 H 0.0030 0.0938 0.8936 0.030 Uiso 1 1 calc R . . C11 C 0.05673(7) 0.10544(5) 0.8110(3) 0.0244(6) Uani 1 1 d . . . H11 H 0.0612 0.1200 0.8679 0.029 Uiso 1 1 calc R . . C12 C 0.11745(7) 0.10437(5) 0.6460(3) 0.0223(5) Uani 1 1 d . . . H12A H 0.1214 0.1206 0.6920 0.027 Uiso 1 1 calc R . . H12B H 0.1171 0.1058 0.5249 0.027 Uiso 1 1 calc R . . C13 C 0.15108(6) 0.08832(4) 0.6972(4) 0.0202(5) Uani 1 1 d . . . H13A H 0.1500 0.0855 0.8171 0.024 Uiso 1 1 calc R . . H13B H 0.1756 0.0965 0.6722 0.024 Uiso 1 1 calc R . . C14 C 0.19214(6) 0.05960(4) 0.4597(4) 0.0227(5) Uani 1 1 d . . . C15 C 0.19742(8) 0.07889(5) 0.3534(3) 0.0314(6) Uani 1 1 d . . . H15 H 0.1798 0.0919 0.3550 0.038 Uiso 1 1 calc R . . C16 C 0.22823(8) 0.07922(6) 0.2455(4) 0.0399(8) Uani 1 1 d . . . H16 H 0.2316 0.0924 0.1732 0.048 Uiso 1 1 calc R . . C17 C 0.25406(8) 0.06043(6) 0.2429(4) 0.0426(8) Uani 1 1 d . . . H17 H 0.2751 0.0607 0.1688 0.051 Uiso 1 1 calc R . . C18 C 0.24920(8) 0.04141(6) 0.3474(4) 0.0389(8) Uani 1 1 d . . . H18 H 0.2670 0.0286 0.3457 0.047 Uiso 1 1 calc R . . C19 C 0.21838(7) 0.04091(5) 0.4556(4) 0.0292(5) Uani 1 1 d . . . H19 H 0.2152 0.0277 0.5274 0.035 Uiso 1 1 calc R . . C20 C 0.15830(7) 0.03708(4) 0.7456(3) 0.0204(6) Uani 1 1 d . . . C21 C 0.13490(7) 0.01689(4) 0.7557(3) 0.0242(6) Uani 1 1 d . . . H21 H 0.1145 0.0148 0.6795 0.029 Uiso 1 1 calc R . . C22 C 0.14122(8) -0.00014(5) 0.8760(3) 0.0286(6) Uani 1 1 d . . . H22 H 0.1251 -0.0138 0.8825 0.034 Uiso 1 1 calc R . . C23 C 0.17099(8) 0.00271(5) 0.9869(4) 0.0319(6) Uani 1 1 d . . . H23 H 0.1755 -0.0090 1.0688 0.038 Uiso 1 1 calc R . . C24 C 0.19408(8) 0.02265(5) 0.9782(4) 0.0351(6) Uani 1 1 d . . . H24 H 0.2144 0.0247 1.0550 0.042 Uiso 1 1 calc R . . C25 C 0.18799(8) 0.03983(5) 0.8583(3) 0.0296(6) Uani 1 1 d . . . H25 H 0.2041 0.0535 0.8531 0.036 Uiso 1 1 calc R . . C26 C 0.17055(6) 0.15825(4) 0.7284(3) 0.0205(5) Uani 1 1 d . . . C27 C 0.16604(7) 0.15746(5) 0.5576(3) 0.0262(6) Uani 1 1 d . . . H27 H 0.1439 0.1646 0.5103 0.031 Uiso 1 1 calc R . . C28 C 0.19287(7) 0.14646(5) 0.4537(4) 0.0326(6) Uani 1 1 d . . . H28 H 0.1884 0.1461 0.3387 0.039 Uiso 1 1 calc R . . C29 C 0.22578(8) 0.13618(5) 0.5178(3) 0.0305(6) Uani 1 1 d . . . H29 H 0.2440 0.1287 0.4480 0.037 Uiso 1 1 calc R . . C30 C 0.23155(7) 0.13708(5) 0.6862(4) 0.0298(6) Uani 1 1 d . . . H30 H 0.2540 0.1303 0.7326 0.036 Uiso 1 1 calc R . . C31 C 0.20460(7) 0.14789(5) 0.7871(3) 0.0249(6) Uani 1 1 d . . . H31 H 0.2094 0.1483 0.9018 0.030 Uiso 1 1 calc R . . C32 C 0.13564(8) 0.12852(5) 1.0220(3) 0.0252(6) Uani 1 1 d . . . H32 H 0.1580 0.1232 0.9664 0.030 Uiso 1 1 calc R . . C33 C 0.11802(8) 0.11321(5) 1.1343(3) 0.0325(7) Uani 1 1 d . . . H33 H 0.1283 0.0977 1.1522 0.039 Uiso 1 1 calc R . . C34 C 0.08588(8) 0.12042(5) 1.2195(4) 0.0356(6) Uani 1 1 d . . . H34 H 0.0737 0.1100 1.2953 0.043 Uiso 1 1 calc R . . C35 C 0.07167(8) 0.14302(5) 1.1930(4) 0.0328(6) Uani 1 1 d . . . H35 H 0.0498 0.1483 1.2522 0.039 Uiso 1 1 calc R . . C36 C 0.08915(7) 0.15809(5) 1.0800(3) 0.0270(6) Uani 1 1 d . . . H36 H 0.0787 0.1736 1.0641 0.032 Uiso 1 1 calc R . . C37 C 0.12166(7) 0.15141(4) 0.9880(3) 0.0193(5) Uani 1 1 d . . . C38 C 0.10483(7) 0.18436(4) 0.7620(3) 0.0200(5) Uani 1 1 d . . . C39 C 0.07909(8) 0.17157(5) 0.6608(3) 0.0303(7) Uani 1 1 d . . . H39 H 0.0821 0.1548 0.6518 0.036 Uiso 1 1 calc R . . C40 C 0.04956(8) 0.18239(6) 0.5742(3) 0.0345(7) Uani 1 1 d . . . H40 H 0.0334 0.1731 0.5054 0.041 Uiso 1 1 calc R . . C41 C 0.04353(8) 0.20666(6) 0.5876(4) 0.0337(7) Uani 1 1 d . . . H41 H 0.0234 0.2142 0.5282 0.040 Uiso 1 1 calc R . . C42 C 0.06709(7) 0.21966(5) 0.6882(4) 0.0339(7) Uani 1 1 d . . . H42 H 0.0631 0.2364 0.6998 0.041 Uiso 1 1 calc R . . C43 C 0.09683(7) 0.20863(5) 0.7735(3) 0.0256(6) Uani 1 1 d . . . H43 H 0.1124 0.2182 0.8431 0.031 Uiso 1 1 calc R . . C44 C 0.16582(6) 0.19043(4) 0.9661(4) 0.0207(5) Uani 1 1 d . . . C45 C 0.18643(7) 0.20850(5) 0.8870(3) 0.0236(6) Uani 1 1 d . . . H45 H 0.1863 0.2090 0.7705 0.028 Uiso 1 1 calc R . . C46 C 0.20706(6) 0.22575(4) 0.9725(4) 0.0270(5) Uani 1 1 d . . . H46 H 0.2198 0.2382 0.9143 0.032 Uiso 1 1 calc R . . C47 C 0.20912(7) 0.22488(5) 1.1415(3) 0.0298(6) Uani 1 1 d . . . H47 H 0.2235 0.2365 1.2001 0.036 Uiso 1 1 calc R . . C48 C 0.19011(7) 0.20702(5) 1.2244(4) 0.0298(6) Uani 1 1 d . . . H48 H 0.1918 0.2061 1.3406 0.036 Uiso 1 1 calc R . . C49 C 0.16834(8) 0.19030(5) 1.1383(3) 0.0250(6) Uani 1 1 d . . . H49 H 0.1548 0.1784 1.1980 0.030 Uiso 1 1 calc R . . B1 B 0.14046(8) 0.17086(5) 0.8583(4) 0.0198(6) 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 0.01494(4) 0.01806(4) 0.01846(4) -0.00115(4) -0.00036(4) -0.00102(4) P1 0.0155(3) 0.0193(3) 0.0220(3) -0.0028(3) -0.0004(3) -0.0016(3) N1 0.0166(11) 0.0242(12) 0.0197(10) -0.0015(9) -0.0009(8) 0.0009(9) N2 0.0186(9) 0.0211(10) 0.0223(10) -0.0041(10) -0.0002(10) 0.0001(8) C1 0.0174(13) 0.0251(15) 0.0247(14) -0.0060(12) -0.0020(11) 0.0007(11) C2 0.0135(13) 0.0319(15) 0.0220(13) -0.0004(11) -0.0001(10) -0.0036(11) C3 0.0220(13) 0.0229(14) 0.0292(14) -0.0031(11) -0.0004(11) -0.0049(11) C4 0.0228(14) 0.0216(14) 0.0310(14) -0.0049(11) 0.0005(11) -0.0001(10) C5 0.0152(13) 0.0259(14) 0.0257(14) -0.0059(11) 0.0004(10) 0.0002(10) C6 0.0210(12) 0.0239(12) 0.0224(12) -0.0061(12) 0.0016(12) -0.0037(10) C7 0.0338(16) 0.0311(16) 0.0183(13) 0.0012(11) 0.0015(11) -0.0039(12) C8 0.0273(15) 0.0284(15) 0.0238(13) 0.0017(11) -0.0070(11) -0.0012(12) C9 0.0187(11) 0.0302(13) 0.0213(11) 0.0022(13) -0.0016(12) -0.0009(9) C10 0.0198(13) 0.0362(15) 0.0185(12) -0.0027(11) -0.0007(10) 0.0046(11) C11 0.0273(15) 0.0255(14) 0.0205(13) -0.0051(11) -0.0033(11) 0.0071(11) C12 0.0209(13) 0.0207(13) 0.0252(13) -0.0020(10) 0.0012(10) -0.0036(10) C13 0.0190(12) 0.0179(11) 0.0237(14) -0.0057(12) -0.0004(12) -0.0015(9) C14 0.0164(11) 0.0270(13) 0.0247(11) -0.0073(15) -0.0005(13) -0.0033(9) C15 0.0265(15) 0.0320(16) 0.0356(16) -0.0025(13) 0.0042(12) -0.0061(12) C16 0.0384(17) 0.0470(18) 0.0344(19) -0.0017(14) 0.0081(14) -0.0187(14) C17 0.0244(15) 0.067(2) 0.036(2) -0.0180(17) 0.0087(14) -0.0144(15) C18 0.0239(15) 0.055(2) 0.0378(17) -0.0175(16) 0.0026(13) 0.0050(14) C19 0.0215(12) 0.0369(14) 0.0292(13) -0.0069(15) -0.0025(14) 0.0039(10) C20 0.0184(11) 0.0232(12) 0.0196(16) -0.0019(9) 0.0005(10) 0.0015(10) C21 0.0218(13) 0.0242(14) 0.0266(15) -0.0037(10) -0.0021(10) -0.0008(10) C22 0.0302(15) 0.0253(15) 0.0304(15) 0.0017(11) 0.0023(12) -0.0032(12) C23 0.0355(15) 0.0359(16) 0.0242(15) 0.0053(13) 0.0014(13) 0.0081(12) C24 0.0327(15) 0.0446(17) 0.0279(15) 0.0013(15) -0.0115(14) 0.0013(12) C25 0.0241(14) 0.0316(16) 0.0331(16) -0.0038(12) -0.0046(12) -0.0051(12) C26 0.0196(11) 0.0154(11) 0.0265(13) 0.0001(11) 0.0005(12) -0.0020(8) C27 0.0277(14) 0.0241(14) 0.0269(14) 0.0037(11) 0.0003(11) 0.0061(11) C28 0.0396(15) 0.0336(15) 0.0246(13) 0.0025(14) 0.0071(15) 0.0049(12) C29 0.0265(14) 0.0250(14) 0.0401(17) -0.0036(11) 0.0098(12) 0.0013(11) C30 0.0202(13) 0.0260(14) 0.0431(19) -0.0047(12) -0.0012(12) 0.0008(10) C31 0.0204(13) 0.0267(14) 0.0277(13) -0.0042(11) -0.0028(11) -0.0016(11) C32 0.0274(14) 0.0217(14) 0.0265(13) -0.0017(10) -0.0073(11) -0.0029(11) C33 0.0405(17) 0.0233(15) 0.0335(15) 0.0076(12) -0.0155(14) -0.0063(13) C34 0.0449(16) 0.0391(16) 0.0230(13) 0.0072(14) -0.0045(16) -0.0204(12) C35 0.0301(14) 0.0427(17) 0.0255(15) -0.0019(14) 0.0014(13) -0.0099(12) C36 0.0248(14) 0.0276(15) 0.0284(14) -0.0004(12) -0.0006(12) -0.0028(11) C37 0.0201(12) 0.0191(12) 0.0188(14) -0.0010(10) -0.0034(10) -0.0025(9) C38 0.0175(12) 0.0227(13) 0.0198(13) 0.0010(10) 0.0033(9) 0.0006(10) C39 0.0279(15) 0.0282(15) 0.0349(16) -0.0087(12) -0.0046(12) 0.0077(12) C40 0.0274(15) 0.0457(19) 0.0304(15) -0.0083(13) -0.0085(12) 0.0054(13) C41 0.0209(14) 0.0489(19) 0.0313(15) 0.0151(14) 0.0002(12) 0.0081(13) C42 0.0235(13) 0.0219(14) 0.056(2) 0.0117(14) 0.0046(14) 0.0035(11) C43 0.0195(13) 0.0194(13) 0.0379(15) 0.0018(11) -0.0001(11) -0.0020(10) C44 0.0172(11) 0.0194(11) 0.0255(12) -0.0011(12) -0.0030(12) 0.0042(9) C45 0.0170(13) 0.0235(14) 0.0301(14) 0.0000(11) 0.0009(11) 0.0020(10) C46 0.0182(12) 0.0210(12) 0.0417(15) -0.0018(14) 0.0024(14) -0.0006(9) C47 0.0216(14) 0.0270(15) 0.0407(16) -0.0144(12) -0.0039(12) -0.0001(11) C48 0.0279(13) 0.0356(14) 0.0258(13) -0.0081(14) -0.0070(14) 0.0039(11) C49 0.0267(14) 0.0208(14) 0.0274(14) -0.0014(11) -0.0019(11) 0.0015(11) B1 0.0194(14) 0.0163(14) 0.0238(15) -0.0022(11) 0.0003(12) 0.0000(11) _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 2.086(2) . ? Ir1 C6 2.126(3) . ? Ir1 C5 2.145(3) . ? Ir1 C2 2.214(2) . ? Ir1 C1 2.224(3) . ? Ir1 P1 2.2943(8) . ? P1 C20 1.819(2) . ? P1 C14 1.821(3) . ? P1 C13 1.853(2) . ? N1 C9 1.348(3) . ? N1 N2 1.367(3) . ? N2 C11 1.342(3) . ? N2 C12 1.461(3) . ? C1 C2 1.384(4) . ? C1 C8 1.507(4) . ? C1 H1 0.89(3) . ? C2 C3 1.527(4) . ? C2 H2 0.92(2) . ? C3 C4 1.533(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.498(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.401(4) . ? C5 H5 0.93(3) . ? C6 C7 1.527(4) . ? C6 H6 0.97(2) . ? C7 C8 1.532(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.386(4) . ? C9 H9 0.9500 . ? C10 C11 1.377(4) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C13 1.534(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C19 1.389(3) . ? C14 C15 1.397(4) . ? C15 C16 1.387(4) . ? C15 H15 0.9500 . ? C16 C17 1.384(4) . ? C16 H16 0.9500 . ? C17 C18 1.374(4) . ? C17 H17 0.9500 . ? C18 C19 1.390(4) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C25 1.392(3) . ? C20 C21 1.396(3) . ? C21 C22 1.385(4) . ? C21 H21 0.9500 . ? C22 C23 1.385(4) . ? C22 H22 0.9500 . ? C23 C24 1.377(4) . ? C23 H23 0.9500 . ? C24 C25 1.387(4) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C27 1.401(4) . ? C26 C31 1.404(3) . ? C26 B1 1.649(4) . ? C27 C28 1.403(4) . ? C27 H27 0.9500 . ? C28 C29 1.385(4) . ? C28 H28 0.9500 . ? C29 C30 1.388(4) . ? C29 H29 0.9500 . ? C30 C31 1.386(3) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 C33 1.396(4) . ? C32 C37 1.398(3) . ? C32 H32 0.9500 . ? C33 C34 1.378(4) . ? C33 H33 0.9500 . ? C34 C35 1.376(4) . ? C34 H34 0.9500 . ? C35 C36 1.389(4) . ? C35 H35 0.9500 . ? C36 C37 1.409(3) . ? C36 H36 0.9500 . ? C37 B1 1.653(4) . ? C38 C43 1.390(3) . ? C38 C39 1.413(4) . ? C38 B1 1.652(4) . ? C39 C40 1.387(4) . ? C39 H39 0.9500 . ? C40 C41 1.379(4) . ? C40 H40 0.9500 . ? C41 C42 1.369(4) . ? C41 H41 0.9500 . ? C42 C43 1.392(4) . ? C42 H42 0.9500 . ? C43 H43 0.9500 . ? C44 C45 1.397(3) . ? C44 C49 1.406(4) . ? C44 B1 1.659(4) . ? C45 C46 1.390(3) . ? C45 H45 0.9500 . ? C46 C47 1.380(4) . ? C46 H46 0.9500 . ? C47 C48 1.376(4) . ? C47 H47 0.9500 . ? C48 C49 1.394(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 154.59(9) . . ? N1 Ir1 C5 167.02(9) . . ? C6 Ir1 C5 38.30(9) . . ? N1 Ir1 C2 96.19(9) . . ? C6 Ir1 C2 88.08(10) . . ? C5 Ir1 C2 80.17(10) . . ? N1 Ir1 C1 87.43(9) . . ? C6 Ir1 C1 81.25(10) . . ? C5 Ir1 C1 96.54(10) . . ? C2 Ir1 C1 36.33(10) . . ? N1 Ir1 P1 89.47(6) . . ? C6 Ir1 P1 97.55(7) . . ? C5 Ir1 P1 88.69(7) . . ? C2 Ir1 P1 154.15(7) . . ? C1 Ir1 P1 169.49(7) . . ? C20 P1 C14 105.58(12) . . ? C20 P1 C13 104.64(12) . . ? C14 P1 C13 103.95(11) . . ? C20 P1 Ir1 111.15(8) . . ? C14 P1 Ir1 118.47(9) . . ? C13 P1 Ir1 111.91(7) . . ? C9 N1 N2 105.21(19) . . ? C9 N1 Ir1 130.70(17) . . ? N2 N1 Ir1 124.05(15) . . ? C11 N2 N1 110.77(19) . . ? C11 N2 C12 126.7(2) . . ? N1 N2 C12 122.5(2) . . ? C2 C1 C8 124.4(3) . . ? C2 C1 Ir1 71.45(15) . . ? C8 C1 Ir1 108.21(18) . . ? C2 C1 H1 118.1(16) . . ? C8 C1 H1 115.9(16) . . ? Ir1 C1 H1 103.2(16) . . ? C1 C2 C3 123.5(2) . . ? C1 C2 Ir1 72.21(15) . . ? C3 C2 Ir1 112.10(16) . . ? C1 C2 H2 119.6(15) . . ? C3 C2 H2 114.6(15) . . ? Ir1 C2 H2 101.2(14) . . ? C2 C3 C4 112.6(2) . . ? C2 C3 H3A 109.1 . . ? C4 C3 H3A 109.1 . . ? C2 C3 H3B 109.1 . . ? C4 C3 H3B 109.1 . . ? H3A C3 H3B 107.8 . . ? C5 C4 C3 112.7(2) . . ? C5 C4 H4A 109.0 . . ? C3 C4 H4A 109.0 . . ? C5 C4 H4B 109.0 . . ? C3 C4 H4B 109.0 . . ? H4A C4 H4B 107.8 . . ? C6 C5 C4 125.2(2) . . ? C6 C5 Ir1 70.13(15) . . ? C4 C5 Ir1 112.12(16) . . ? C6 C5 H5 119.9(17) . . ? C4 C5 H5 108.5(17) . . ? Ir1 C5 H5 114.6(17) . . ? C5 C6 C7 124.3(2) . . ? C5 C6 Ir1 71.57(16) . . ? C7 C6 Ir1 113.95(16) . . ? C5 C6 H6 117.2(14) . . ? C7 C6 H6 112.1(16) . . ? Ir1 C6 H6 110.0(15) . . ? C6 C7 C8 113.2(2) . . ? C6 C7 H7A 108.9 . . ? C8 C7 H7A 108.9 . . ? C6 C7 H7B 108.9 . . ? C8 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? C1 C8 C7 114.0(2) . . ? C1 C8 H8A 108.8 . . ? C7 C8 H8A 108.8 . . ? C1 C8 H8B 108.8 . . ? C7 C8 H8B 108.8 . . ? H8A C8 H8B 107.6 . . ? N1 C9 C10 110.8(2) . . ? N1 C9 H9 124.6 . . ? C10 C9 H9 124.6 . . ? C11 C10 C9 105.3(2) . . ? C11 C10 H10 127.3 . . ? C9 C10 H10 127.3 . . ? N2 C11 C10 107.9(2) . . ? N2 C11 H11 126.1 . . ? C10 C11 H11 126.1 . . ? N2 C12 C13 112.5(2) . . ? N2 C12 H12A 109.1 . . ? C13 C12 H12A 109.1 . . ? N2 C12 H12B 109.1 . . ? C13 C12 H12B 109.1 . . ? H12A C12 H12B 107.8 . . ? C12 C13 P1 110.83(17) . . ? C12 C13 H13A 109.5 . . ? P1 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? P1 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? C19 C14 C15 118.7(3) . . ? C19 C14 P1 123.2(2) . . ? C15 C14 P1 117.98(19) . . ? C16 C15 C14 120.3(3) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C17 C16 C15 120.2(3) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C18 C17 C16 119.9(3) . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C17 C18 C19 120.3(3) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? C18 C19 C14 120.6(3) . . ? C18 C19 H19 119.7 . . ? C14 C19 H19 119.7 . . ? C25 C20 C21 119.0(2) . . ? C25 C20 P1 121.33(19) . . ? C21 C20 P1 119.69(18) . . ? C22 C21 C20 120.4(2) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C23 C22 C21 120.1(3) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C24 C23 C22 119.8(3) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C23 C24 C25 120.6(3) . . ? C23 C24 H24 119.7 . . ? C25 C24 H24 119.7 . . ? C24 C25 C20 120.1(3) . . ? C24 C25 H25 119.9 . . ? C20 C25 H25 119.9 . . ? C27 C26 C31 114.8(2) . . ? C27 C26 B1 125.5(2) . . ? C31 C26 B1 119.7(2) . . ? C26 C27 C28 122.6(2) . . ? C26 C27 H27 118.7 . . ? C28 C27 H27 118.7 . . ? C29 C28 C27 120.4(3) . . ? C29 C28 H28 119.8 . . ? C27 C28 H28 119.8 . . ? C28 C29 C30 118.5(3) . . ? C28 C29 H29 120.7 . . ? C30 C29 H29 120.7 . . ? C29 C30 C31 120.2(3) . . ? C29 C30 H30 119.9 . . ? C31 C30 H30 119.9 . . ? C30 C31 C26 123.4(3) . . ? C30 C31 H31 118.3 . . ? C26 C31 H31 118.3 . . ? C33 C32 C37 122.6(3) . . ? C33 C32 H32 118.7 . . ? C37 C32 H32 118.7 . . ? C34 C33 C32 120.5(3) . . ? C34 C33 H33 119.7 . . ? C32 C33 H33 119.7 . . ? C35 C34 C33 118.8(3) . . ? C35 C34 H34 120.6 . . ? C33 C34 H34 120.6 . . ? C34 C35 C36 120.3(3) . . ? C34 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C35 C36 C37 122.9(3) . . ? C35 C36 H36 118.5 . . ? C37 C36 H36 118.5 . . ? C32 C37 C36 114.7(2) . . ? C32 C37 B1 126.3(2) . . ? C36 C37 B1 118.9(2) . . ? C43 C38 C39 114.0(2) . . ? C43 C38 B1 124.4(2) . . ? C39 C38 B1 121.5(2) . . ? C40 C39 C38 123.1(3) . . ? C40 C39 H39 118.4 . . ? C38 C39 H39 118.4 . . ? C41 C40 C39 120.2(3) . . ? C41 C40 H40 119.9 . . ? C39 C40 H40 119.9 . . ? C42 C41 C40 118.7(3) . . ? C42 C41 H41 120.7 . . ? C40 C41 H41 120.7 . . ? C41 C42 C43 120.6(3) . . ? C41 C42 H42 119.7 . . ? C43 C42 H42 119.7 . . ? C38 C43 C42 123.3(2) . . ? C38 C43 H43 118.4 . . ? C42 C43 H43 118.4 . . ? C45 C44 C49 115.6(2) . . ? C45 C44 B1 120.5(2) . . ? C49 C44 B1 123.9(2) . . ? C46 C45 C44 122.5(3) . . ? C46 C45 H45 118.7 . . ? C44 C45 H45 118.7 . . ? C47 C46 C45 120.1(3) . . ? C47 C46 H46 119.9 . . ? C45 C46 H46 119.9 . . ? C48 C47 C46 119.4(3) . . ? C48 C47 H47 120.3 . . ? C46 C47 H47 120.3 . . ? C47 C48 C49 120.1(3) . . ? C47 C48 H48 119.9 . . ? C49 C48 H48 119.9 . . ? C48 C49 C44 122.2(3) . . ? C48 C49 H49 118.9 . . ? C44 C49 H49 118.9 . . ? C26 B1 C38 111.6(2) . . ? C26 B1 C37 112.4(2) . . ? C38 B1 C37 107.9(2) . . ? C26 B1 C44 106.52(19) . . ? C38 B1 C44 110.5(2) . . ? C37 B1 C44 107.9(2) . . ? 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 C20 88.40(10) . . . . ? C6 Ir1 P1 C20 -116.10(11) . . . . ? C5 Ir1 P1 C20 -78.74(11) . . . . ? C2 Ir1 P1 C20 -14.78(19) . . . . ? C1 Ir1 P1 C20 161.2(4) . . . . ? N1 Ir1 P1 C14 -149.10(10) . . . . ? C6 Ir1 P1 C14 6.40(11) . . . . ? C5 Ir1 P1 C14 43.75(11) . . . . ? C2 Ir1 P1 C14 107.71(18) . . . . ? C1 Ir1 P1 C14 -76.3(4) . . . . ? N1 Ir1 P1 C13 -28.19(12) . . . . ? C6 Ir1 P1 C13 127.30(12) . . . . ? C5 Ir1 P1 C13 164.66(13) . . . . ? C2 Ir1 P1 C13 -131.38(19) . . . . ? C1 Ir1 P1 C13 44.6(4) . . . . ? C6 Ir1 N1 C9 111.6(3) . . . . ? C5 Ir1 N1 C9 -59.9(5) . . . . ? C2 Ir1 N1 C9 13.0(2) . . . . ? C1 Ir1 N1 C9 48.3(2) . . . . ? P1 Ir1 N1 C9 -141.7(2) . . . . ? C6 Ir1 N1 N2 -65.7(3) . . . . ? C5 Ir1 N1 N2 122.8(4) . . . . ? C2 Ir1 N1 N2 -164.29(19) . . . . ? C1 Ir1 N1 N2 -128.98(19) . . . . ? P1 Ir1 N1 N2 40.98(18) . . . . ? C9 N1 N2 C11 -0.4(3) . . . . ? Ir1 N1 N2 C11 177.48(16) . . . . ? C9 N1 N2 C12 -178.8(2) . . . . ? Ir1 N1 N2 C12 -0.9(3) . . . . ? N1 Ir1 C1 C2 -104.08(16) . . . . ? C6 Ir1 C1 C2 98.75(17) . . . . ? C5 Ir1 C1 C2 63.52(17) . . . . ? P1 Ir1 C1 C2 -177.0(3) . . . . ? N1 Ir1 C1 C8 134.82(19) . . . . ? C6 Ir1 C1 C8 -22.36(19) . . . . ? C5 Ir1 C1 C8 -57.6(2) . . . . ? C2 Ir1 C1 C8 -121.1(3) . . . . ? P1 Ir1 C1 C8 61.9(5) . . . . ? C8 C1 C2 C3 -5.4(4) . . . . ? Ir1 C1 C2 C3 -105.1(2) . . . . ? C8 C1 C2 Ir1 99.8(3) . . . . ? N1 Ir1 C2 C1 77.08(16) . . . . ? C6 Ir1 C2 C1 -77.80(17) . . . . ? C5 Ir1 C2 C1 -115.51(17) . . . . ? P1 Ir1 C2 C1 178.75(14) . . . . ? N1 Ir1 C2 C3 -163.18(18) . . . . ? C6 Ir1 C2 C3 41.94(19) . . . . ? C5 Ir1 C2 C3 4.23(18) . . . . ? C1 Ir1 C2 C3 119.7(3) . . . . ? P1 Ir1 C2 C3 -61.5(3) . . . . ? C1 C2 C3 C4 96.1(3) . . . . ? Ir1 C2 C3 C4 13.4(3) . . . . ? C2 C3 C4 C5 -31.9(3) . . . . ? C3 C4 C5 C6 -45.1(3) . . . . ? C3 C4 C5 Ir1 35.6(3) . . . . ? N1 Ir1 C5 C6 174.1(3) . . . . ? C2 Ir1 C5 C6 99.48(16) . . . . ? C1 Ir1 C5 C6 66.91(15) . . . . ? P1 Ir1 C5 C6 -103.95(14) . . . . ? N1 Ir1 C5 C4 53.1(5) . . . . ? C6 Ir1 C5 C4 -121.0(2) . . . . ? C2 Ir1 C5 C4 -21.53(18) . . . . ? C1 Ir1 C5 C4 -54.1(2) . . . . ? P1 Ir1 C5 C4 135.05(18) . . . . ? C4 C5 C6 C7 -3.3(4) . . . . ? Ir1 C5 C6 C7 -106.9(2) . . . . ? C4 C5 C6 Ir1 103.6(2) . . . . ? N1 Ir1 C6 C5 -176.93(18) . . . . ? C2 Ir1 C6 C5 -76.51(16) . . . . ? C1 Ir1 C6 C5 -112.38(15) . . . . ? P1 Ir1 C6 C5 78.17(14) . . . . ? N1 Ir1 C6 C7 -56.8(3) . . . . ? C5 Ir1 C6 C7 120.1(2) . . . . ? C2 Ir1 C6 C7 43.61(18) . . . . ? C1 Ir1 C6 C7 7.74(18) . . . . ? P1 Ir1 C6 C7 -161.71(16) . . . . ? C5 C6 C7 C8 91.8(3) . . . . ? Ir1 C6 C7 C8 8.5(3) . . . . ? C2 C1 C8 C7 -45.8(4) . . . . ? Ir1 C1 C8 C7 33.8(3) . . . . ? C6 C7 C8 C1 -28.9(3) . . . . ? N2 N1 C9 C10 0.4(3) . . . . ? Ir1 N1 C9 C10 -177.31(17) . . . . ? N1 C9 C10 C11 -0.2(3) . . . . ? N1 N2 C11 C10 0.3(3) . . . . ? C12 N2 C11 C10 178.6(2) . . . . ? C9 C10 C11 N2 0.0(3) . . . . ? C11 N2 C12 C13 115.0(3) . . . . ? N1 N2 C12 C13 -66.9(3) . . . . ? N2 C12 C13 P1 68.0(3) . . . . ? C20 P1 C13 C12 -134.67(19) . . . . ? C14 P1 C13 C12 114.79(19) . . . . ? Ir1 P1 C13 C12 -14.2(2) . . . . ? C20 P1 C14 C19 19.6(3) . . . . ? C13 P1 C14 C19 129.5(2) . . . . ? Ir1 P1 C14 C19 -105.6(2) . . . . ? C20 P1 C14 C15 -164.5(2) . . . . ? C13 P1 C14 C15 -54.7(2) . . . . ? Ir1 P1 C14 C15 70.2(2) . . . . ? C19 C14 C15 C16 0.3(4) . . . . ? P1 C14 C15 C16 -175.7(2) . . . . ? C14 C15 C16 C17 -0.2(4) . . . . ? C15 C16 C17 C18 0.0(4) . . . . ? C16 C17 C18 C19 0.2(4) . . . . ? C17 C18 C19 C14 -0.1(4) . . . . ? C15 C14 C19 C18 -0.2(4) . . . . ? P1 C14 C19 C18 175.6(2) . . . . ? C14 P1 C20 C25 63.1(2) . . . . ? C13 P1 C20 C25 -46.2(2) . . . . ? Ir1 P1 C20 C25 -167.22(18) . . . . ? C14 P1 C20 C21 -117.5(2) . . . . ? C13 P1 C20 C21 133.18(19) . . . . ? Ir1 P1 C20 C21 12.2(2) . . . . ? C25 C20 C21 C22 -0.1(4) . . . . ? P1 C20 C21 C22 -179.52(19) . . . . ? C20 C21 C22 C23 -0.3(4) . . . . ? C21 C22 C23 C24 0.6(4) . . . . ? C22 C23 C24 C25 -0.6(4) . . . . ? C23 C24 C25 C20 0.2(4) . . . . ? C21 C20 C25 C24 0.1(4) . . . . ? P1 C20 C25 C24 179.6(2) . . . . ? C31 C26 C27 C28 2.0(4) . . . . ? B1 C26 C27 C28 179.8(2) . . . . ? C26 C27 C28 C29 -1.2(4) . . . . ? C27 C28 C29 C30 -0.2(4) . . . . ? C28 C29 C30 C31 0.6(4) . . . . ? C29 C30 C31 C26 0.4(4) . . . . ? C27 C26 C31 C30 -1.6(4) . . . . ? B1 C26 C31 C30 -179.5(2) . . . . ? C37 C32 C33 C34 -1.1(4) . . . . ? C32 C33 C34 C35 -0.6(4) . . . . ? C33 C34 C35 C36 1.1(4) . . . . ? C34 C35 C36 C37 0.0(4) . . . . ? C33 C32 C37 C36 2.0(4) . . . . ? C33 C32 C37 B1 179.7(2) . . . . ? C35 C36 C37 C32 -1.4(4) . . . . ? C35 C36 C37 B1 -179.3(2) . . . . ? C43 C38 C39 C40 3.0(4) . . . . ? B1 C38 C39 C40 -178.0(2) . . . . ? C38 C39 C40 C41 -1.7(4) . . . . ? C39 C40 C41 C42 -0.3(4) . . . . ? C40 C41 C42 C43 0.8(4) . . . . ? C39 C38 C43 C42 -2.5(4) . . . . ? B1 C38 C43 C42 178.6(3) . . . . ? C41 C42 C43 C38 0.7(4) . . . . ? C49 C44 C45 C46 -2.1(4) . . . . ? B1 C44 C45 C46 177.9(2) . . . . ? C44 C45 C46 C47 2.8(4) . . . . ? C45 C46 C47 C48 -1.0(4) . . . . ? C46 C47 C48 C49 -1.4(4) . . . . ? C47 C48 C49 C44 2.0(4) . . . . ? C45 C44 C49 C48 -0.3(4) . . . . ? B1 C44 C49 C48 179.7(2) . . . . ? C27 C26 B1 C38 -3.8(3) . . . . ? C31 C26 B1 C38 173.9(2) . . . . ? C27 C26 B1 C37 117.6(3) . . . . ? C31 C26 B1 C37 -64.7(3) . . . . ? C27 C26 B1 C44 -124.4(2) . . . . ? C31 C26 B1 C44 53.3(3) . . . . ? C43 C38 B1 C26 -119.8(2) . . . . ? C39 C38 B1 C26 61.3(3) . . . . ? C43 C38 B1 C37 116.3(3) . . . . ? C39 C38 B1 C37 -62.6(3) . . . . ? C43 C38 B1 C44 -1.5(3) . . . . ? C39 C38 B1 C44 179.6(2) . . . . ? C32 C37 B1 C26 17.2(3) . . . . ? C36 C37 B1 C26 -165.2(2) . . . . ? C32 C37 B1 C38 140.6(2) . . . . ? C36 C37 B1 C38 -41.7(3) . . . . ? C32 C37 B1 C44 -100.0(3) . . . . ? C36 C37 B1 C44 77.7(3) . . . . ? C45 C44 B1 C26 56.4(3) . . . . ? C49 C44 B1 C26 -123.6(2) . . . . ? C45 C44 B1 C38 -65.0(3) . . . . ? C49 C44 B1 C38 115.0(3) . . . . ? C45 C44 B1 C37 177.3(2) . . . . ? C49 C44 B1 C37 -2.7(3) . . . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.051 _refine_diff_density_min -0.403 _refine_diff_density_rms 0.061 #===EN data_bam6 _database_code_CSD 207601 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H49 B N2 P Rh' _chemical_formula_weight 810.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 orthorhombic _symmetry_space_group_name_H-M 'F d d 2 ' _symmetry_Int_Tables_number 43 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 34.868(8) _cell_length_b 56.131(12) _cell_length_c 8.1496(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 15950(6) _cell_formula_units_Z 16 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 991 _cell_measurement_theta_min 2.593 _cell_measurement_theta_max 28.100 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.290 _exptl_crystal_size_mid 0.240 _exptl_crystal_size_min 0.210 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.356 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6752 _exptl_absorpt_coefficient_mu 0.508 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.864 _exptl_absorpt_correction_T_max 0.929 _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 538 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.06 _diffrn_reflns_number 38657 _diffrn_reflns_av_R_equivalents 0.0359 _diffrn_reflns_av_sigmaI/netI 0.0268 _diffrn_reflns_limit_h_min -45 _diffrn_reflns_limit_h_max 45 _diffrn_reflns_limit_k_min -74 _diffrn_reflns_limit_k_max 74 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 28.34 _reflns_number_total 9654 _reflns_number_gt 9133 _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^+0.3P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.000(12) _refine_ls_number_reflns 9654 _refine_ls_number_parameters 503 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0264 _refine_ls_R_factor_gt 0.0240 _refine_ls_wR_factor_ref 0.0555 _refine_ls_wR_factor_gt 0.0547 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.097 _refine_ls_shift/su_max 0.003 _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 0.159190(4) 0.196757(2) 0.535945(16) 0.01701(4) Uani 1 1 d . . . P1 P 0.101020(14) 0.190443(9) 0.41337(6) 0.01896(10) Uani 1 1 d . . . N1 N 0.18478(4) 0.17537(3) 0.35417(19) 0.0208(3) Uani 1 1 d . . . N2 N 0.16966(4) 0.15445(3) 0.2985(2) 0.0209(3) Uani 1 1 d . . . C1 C 0.21566(5) 0.19638(3) 0.6689(3) 0.0221(4) Uani 1 1 d D . . H1 H 0.2303(5) 0.1851(3) 0.610(2) 0.034(6) Uiso 1 1 d D . . C2 C 0.21164(5) 0.21834(4) 0.5975(2) 0.0217(4) Uani 1 1 d . . . H2 H 0.2225(5) 0.2199(3) 0.491(3) 0.016(5) Uiso 1 1 d . . . C3 C 0.20095(5) 0.24084(3) 0.6900(2) 0.0250(4) Uani 1 1 d . . . H3A H 0.2156 0.2544 0.6439 0.030 Uiso 1 1 calc R . . H3B H 0.2085 0.2390 0.8064 0.030 Uiso 1 1 calc R . . C4 C 0.15799(5) 0.24652(3) 0.6815(3) 0.0254(4) Uani 1 1 d . . . H4A H 0.1509 0.2565 0.7771 0.031 Uiso 1 1 calc R . . H4B H 0.1529 0.2559 0.5810 0.031 Uiso 1 1 calc R . . C5 C 0.13307(5) 0.22449(3) 0.6801(2) 0.0218(4) Uani 1 1 d . . . H5 H 0.1093(6) 0.2286(3) 0.639(3) 0.021(5) Uiso 1 1 d . . . C6 C 0.13839(5) 0.20430(3) 0.7774(3) 0.0225(4) Uani 1 1 d . . . H6 H 0.1170(6) 0.1941(3) 0.789(3) 0.017(5) Uiso 1 1 d . . . C7 C 0.16911(6) 0.20174(4) 0.9096(3) 0.0284(4) Uani 1 1 d . . . H7A H 0.1590 0.1916 0.9989 0.034 Uiso 1 1 calc R . . H7B H 0.1746 0.2177 0.9565 0.034 Uiso 1 1 calc R . . C8 C 0.20696(6) 0.19083(4) 0.8466(2) 0.0271(4) Uani 1 1 d . . . H8A H 0.2283 0.1968 0.9153 0.032 Uiso 1 1 calc R . . H8B H 0.2058 0.1733 0.8604 0.032 Uiso 1 1 calc R . . C9 C 0.21845(5) 0.17768(3) 0.2757(3) 0.0236(4) Uani 1 1 d . . . H9 H 0.2355 0.1907 0.2895 0.028 Uiso 1 1 calc R . . C10 C 0.22499(5) 0.15852(3) 0.1719(2) 0.0244(4) Uani 1 1 d . . . H10 H 0.2467 0.1560 0.1035 0.029 Uiso 1 1 calc R . . C11 C 0.19353(5) 0.14407(4) 0.1891(2) 0.0243(4) Uani 1 1 d . . . H11 H 0.1893 0.1294 0.1339 0.029 Uiso 1 1 calc R . . C12 C 0.13264(5) 0.14532(3) 0.3549(2) 0.0225(4) Uani 1 1 d . . . H12A H 0.1331 0.1438 0.4760 0.027 Uiso 1 1 calc R . . H12B H 0.1285 0.1292 0.3085 0.027 Uiso 1 1 calc R . . C13 C 0.09935(5) 0.16149(3) 0.3046(3) 0.0216(4) Uani 1 1 d . . . H13A H 0.0748 0.1534 0.3296 0.026 Uiso 1 1 calc R . . H13B H 0.1004 0.1643 0.1848 0.026 Uiso 1 1 calc R . . C14 C 0.05794(5) 0.19017(3) 0.5409(3) 0.0234(4) Uani 1 1 d . . . C15 C 0.05253(6) 0.17085(4) 0.6469(3) 0.0314(5) Uani 1 1 d . . . H15 H 0.0699 0.1578 0.6445 0.038 Uiso 1 1 calc R . . C16 C 0.02178(7) 0.17063(4) 0.7558(3) 0.0406(6) Uani 1 1 d . . . H16 H 0.0184 0.1576 0.8285 0.049 Uiso 1 1 calc R . . C17 C -0.00391(6) 0.18949(5) 0.7581(3) 0.0434(6) Uani 1 1 d . . . H17 H -0.0250 0.1893 0.8318 0.052 Uiso 1 1 calc R . . C18 C 0.00116(6) 0.20847(5) 0.6536(3) 0.0388(6) Uani 1 1 d . . . H18 H -0.0164 0.2214 0.6561 0.047 Uiso 1 1 calc R . . C19 C 0.03181(5) 0.20896(4) 0.5445(3) 0.0291(4) Uani 1 1 d . . . H19 H 0.0349 0.2221 0.4723 0.035 Uiso 1 1 calc R . . C20 C 0.09202(5) 0.21267(3) 0.2551(2) 0.0206(4) Uani 1 1 d . . . C21 C 0.11584(5) 0.23253(3) 0.2429(2) 0.0239(4) Uani 1 1 d . . . H21 H 0.1366 0.2344 0.3175 0.029 Uiso 1 1 calc R . . C22 C 0.10959(6) 0.24965(4) 0.1232(3) 0.0289(4) Uani 1 1 d . . . H22 H 0.1260 0.2631 0.1160 0.035 Uiso 1 1 calc R . . C23 C 0.07942(6) 0.24707(4) 0.0139(3) 0.0313(5) Uani 1 1 d . . . H23 H 0.0750 0.2588 -0.0679 0.038 Uiso 1 1 calc R . . C24 C 0.05570(6) 0.22735(4) 0.0242(3) 0.0361(5) Uani 1 1 d . . . H24 H 0.0350 0.2256 -0.0508 0.043 Uiso 1 1 calc R . . C25 C 0.06196(6) 0.21018(4) 0.1434(3) 0.0297(4) Uani 1 1 d . . . H25 H 0.0457 0.1966 0.1491 0.036 Uiso 1 1 calc R . . C26 C 0.07936(5) 0.09142(3) 0.2719(3) 0.0206(4) Uani 1 1 d . . . C27 C 0.08377(6) 0.09226(3) 0.4428(2) 0.0268(4) Uani 1 1 d . . . H27 H 0.1058 0.0851 0.4905 0.032 Uiso 1 1 calc R . . C28 C 0.05699(6) 0.10329(3) 0.5461(3) 0.0317(4) Uani 1 1 d . . . H28 H 0.0614 0.1038 0.6610 0.038 Uiso 1 1 calc R . . C29 C 0.02418(6) 0.11350(4) 0.4816(3) 0.0301(5) Uani 1 1 d . . . H29 H 0.0060 0.1210 0.5513 0.036 Uiso 1 1 calc R . . C30 C 0.01834(5) 0.11258(3) 0.3132(3) 0.0291(4) Uani 1 1 d . . . H30 H -0.0042 0.1193 0.2670 0.035 Uiso 1 1 calc R . . C31 C 0.04536(5) 0.10186(3) 0.2121(3) 0.0253(4) Uani 1 1 d . . . H31 H 0.0407 0.1015 0.0972 0.030 Uiso 1 1 calc R . . C32 C 0.11436(6) 0.12111(3) -0.0210(2) 0.0247(4) Uani 1 1 d . . . H32 H 0.0920 0.1264 0.0350 0.030 Uiso 1 1 calc R . . C33 C 0.13205(7) 0.13645(4) -0.1344(3) 0.0326(5) Uani 1 1 d . . . H33 H 0.1218 0.1519 -0.1526 0.039 Uiso 1 1 calc R . . C34 C 0.16412(6) 0.12926(4) -0.2192(3) 0.0362(5) Uani 1 1 d . . . H34 H 0.1763 0.1397 -0.2949 0.043 Uiso 1 1 calc R . . C35 C 0.17841(6) 0.10667(4) -0.1928(3) 0.0330(5) Uani 1 1 d . . . H35 H 0.2003 0.1014 -0.2518 0.040 Uiso 1 1 calc R . . C36 C 0.16088(5) 0.09161(4) -0.0803(3) 0.0266(4) Uani 1 1 d . . . H36 H 0.1712 0.0761 -0.0650 0.032 Uiso 1 1 calc R . . C37 C 0.12851(5) 0.09829(3) 0.0122(2) 0.0197(4) Uani 1 1 d . . . C38 C 0.14508(5) 0.06526(3) 0.2383(2) 0.0199(4) Uani 1 1 d . . . C39 C 0.17054(6) 0.07793(4) 0.3403(3) 0.0305(5) Uani 1 1 d . . . H39 H 0.1674 0.0947 0.3506 0.037 Uiso 1 1 calc R . . C40 C 0.20011(6) 0.06704(4) 0.4267(3) 0.0360(5) Uani 1 1 d . . . H40 H 0.2162 0.0763 0.4959 0.043 Uiso 1 1 calc R . . C41 C 0.20630(6) 0.04269(4) 0.4123(3) 0.0342(5) Uani 1 1 d . . . H41 H 0.2263 0.0351 0.4714 0.041 Uiso 1 1 calc R . . C42 C 0.18264(5) 0.02986(4) 0.3100(3) 0.0342(5) Uani 1 1 d . . . H42 H 0.1866 0.0132 0.2972 0.041 Uiso 1 1 calc R . . C43 C 0.15300(5) 0.04101(4) 0.2251(3) 0.0268(4) Uani 1 1 d . . . H43 H 0.1374 0.0316 0.1548 0.032 Uiso 1 1 calc R . . C44 C 0.08429(5) 0.05936(3) 0.0333(3) 0.0201(3) Uani 1 1 d . . . C45 C 0.06330(5) 0.04125(3) 0.1117(3) 0.0235(4) Uani 1 1 d . . . H45 H 0.0633 0.0407 0.2282 0.028 Uiso 1 1 calc R . . C46 C 0.04267(5) 0.02426(3) 0.0270(3) 0.0276(4) Uani 1 1 d . . . H46 H 0.0298 0.0120 0.0854 0.033 Uiso 1 1 calc R . . C47 C 0.04057(6) 0.02502(4) -0.1430(3) 0.0308(5) Uani 1 1 d . . . H47 H 0.0262 0.0134 -0.2016 0.037 Uiso 1 1 calc R . . C48 C 0.05987(5) 0.04297(3) -0.2257(3) 0.0293(4) Uani 1 1 d . . . H48 H 0.0583 0.0440 -0.3419 0.035 Uiso 1 1 calc R . . C49 C 0.08166(6) 0.05952(4) -0.1384(2) 0.0249(4) Uani 1 1 d . . . H49 H 0.0953 0.0714 -0.1977 0.030 Uiso 1 1 calc R . . B1 B 0.10950(6) 0.07886(4) 0.1411(3) 0.0197(4) 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 0.01522(6) 0.01848(6) 0.01731(6) -0.00148(6) -0.00021(6) -0.00095(5) P1 0.0159(2) 0.0201(2) 0.0209(2) -0.00259(19) 0.00006(19) -0.00127(18) N1 0.0187(8) 0.0231(8) 0.0205(7) -0.0019(6) -0.0016(6) -0.0009(6) N2 0.0196(7) 0.0220(7) 0.0211(7) -0.0023(7) -0.0008(7) 0.0005(6) C1 0.0164(9) 0.0271(10) 0.0228(10) -0.0045(8) -0.0040(8) 0.0004(7) C2 0.0163(9) 0.0296(10) 0.0193(9) -0.0010(8) 0.0011(7) -0.0033(8) C3 0.0233(10) 0.0242(10) 0.0273(10) -0.0023(8) -0.0017(8) -0.0037(8) C4 0.0250(10) 0.0215(10) 0.0299(11) -0.0035(8) 0.0012(8) -0.0002(7) C5 0.0176(9) 0.0252(10) 0.0226(10) -0.0057(8) 0.0017(8) 0.0001(7) C6 0.0219(9) 0.0253(9) 0.0203(9) -0.0042(8) 0.0047(9) -0.0022(7) C7 0.0333(11) 0.0317(11) 0.0201(10) 0.0004(8) 0.0004(9) -0.0050(9) C8 0.0288(11) 0.0296(11) 0.0228(10) 0.0015(8) -0.0058(8) -0.0012(9) C9 0.0197(8) 0.0302(9) 0.0207(9) 0.0014(9) -0.0010(8) -0.0009(7) C10 0.0197(9) 0.0353(11) 0.0182(9) -0.0014(8) -0.0009(8) 0.0052(8) C11 0.0243(10) 0.0289(10) 0.0198(9) -0.0054(8) -0.0035(8) 0.0069(8) C12 0.0241(10) 0.0192(9) 0.0241(9) -0.0023(7) 0.0018(8) -0.0026(7) C13 0.0205(9) 0.0182(8) 0.0261(11) -0.0064(8) -0.0006(8) -0.0026(6) C14 0.0179(8) 0.0291(9) 0.0232(9) -0.0069(10) 0.0003(9) -0.0043(7) C15 0.0279(11) 0.0321(11) 0.0342(11) 0.0000(9) 0.0045(9) -0.0061(9) C16 0.0396(12) 0.0478(13) 0.0346(14) -0.0031(10) 0.0106(10) -0.0186(10) C17 0.0237(11) 0.0708(16) 0.0356(14) -0.0172(12) 0.0077(10) -0.0147(11) C18 0.0219(11) 0.0560(15) 0.0384(13) -0.0165(12) 0.0014(10) 0.0047(10) C19 0.0241(9) 0.0354(10) 0.0279(10) -0.0064(10) -0.0023(9) 0.0025(8) C20 0.0194(8) 0.0232(9) 0.0192(11) -0.0016(7) 0.0009(7) 0.0034(7) C21 0.0212(9) 0.0265(10) 0.0240(10) -0.0022(7) -0.0029(7) -0.0024(7) C22 0.0315(11) 0.0266(10) 0.0286(11) 0.0019(8) 0.0027(9) -0.0036(9) C23 0.0366(11) 0.0339(11) 0.0234(11) 0.0035(9) 0.0021(9) 0.0078(9) C24 0.0327(11) 0.0473(12) 0.0283(11) 0.0021(11) -0.0108(10) 0.0012(9) C25 0.0263(10) 0.0324(11) 0.0305(11) -0.0025(9) -0.0061(9) -0.0028(8) C26 0.0200(8) 0.0164(8) 0.0256(9) -0.0005(8) -0.0013(8) -0.0022(6) C27 0.0293(10) 0.0256(10) 0.0256(10) 0.0045(8) 0.0021(8) 0.0062(8) C28 0.0385(11) 0.0338(10) 0.0227(10) 0.0018(10) 0.0085(10) 0.0035(9) C29 0.0286(10) 0.0248(10) 0.0370(11) -0.0037(8) 0.0100(9) 0.0012(8) C30 0.0201(9) 0.0280(10) 0.0393(13) -0.0034(9) -0.0015(9) 0.0011(8) C31 0.0207(9) 0.0272(10) 0.0279(10) -0.0047(8) -0.0026(8) -0.0005(8) C32 0.0270(10) 0.0218(9) 0.0253(9) -0.0015(7) -0.0088(8) -0.0030(8) C33 0.0430(13) 0.0250(10) 0.0299(11) 0.0073(8) -0.0154(10) -0.0074(9) C34 0.0447(12) 0.0413(12) 0.0227(10) 0.0073(10) -0.0059(11) -0.0208(9) C35 0.0327(11) 0.0427(12) 0.0236(11) -0.0018(9) 0.0031(9) -0.0113(9) C36 0.0270(10) 0.0267(10) 0.0261(10) -0.0022(8) 0.0002(8) -0.0027(8) C37 0.0197(8) 0.0206(8) 0.0187(10) -0.0012(7) -0.0045(7) -0.0039(7) C38 0.0181(8) 0.0222(9) 0.0195(9) 0.0014(7) 0.0029(7) 0.0010(7) C39 0.0297(11) 0.0309(11) 0.0311(11) -0.0076(9) -0.0045(9) 0.0066(9) C40 0.0281(11) 0.0517(14) 0.0281(11) -0.0070(10) -0.0077(9) 0.0038(10) C41 0.0213(10) 0.0475(13) 0.0338(11) 0.0151(11) 0.0004(9) 0.0086(9) C42 0.0230(10) 0.0235(10) 0.0562(16) 0.0116(10) 0.0036(10) 0.0044(8) C43 0.0208(10) 0.0232(10) 0.0365(11) 0.0023(8) 0.0019(8) -0.0023(7) C44 0.0175(8) 0.0181(8) 0.0248(9) -0.0001(8) -0.0033(8) 0.0024(6) C45 0.0201(9) 0.0224(10) 0.0279(10) 0.0002(8) 0.0007(8) 0.0023(7) C46 0.0190(8) 0.0234(9) 0.0405(11) -0.0016(10) 0.0031(10) -0.0006(7) C47 0.0220(10) 0.0300(11) 0.0404(12) -0.0136(9) -0.0057(9) -0.0009(8) C48 0.0302(10) 0.0324(10) 0.0254(10) -0.0079(9) -0.0082(9) 0.0035(8) C49 0.0254(10) 0.0234(10) 0.0259(10) -0.0004(8) -0.0018(8) 0.0000(8) B1 0.0190(10) 0.0186(10) 0.0215(10) -0.0001(8) -0.0003(8) -0.0004(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 N1 2.1053(16) . ? Rh1 C6 2.139(2) . ? Rh1 C5 2.1524(18) . ? Rh1 C1 2.2476(19) . ? Rh1 C2 2.2504(19) . ? Rh1 P1 2.2885(6) . ? P1 C20 1.8221(19) . ? P1 C14 1.826(2) . ? P1 C13 1.8522(18) . ? N1 C9 1.343(2) . ? N1 N2 1.364(2) . ? N2 C11 1.352(2) . ? N2 C12 1.463(2) . ? C1 C2 1.371(3) . ? C1 C8 1.512(3) . ? C1 H1 0.946(8) . ? C2 C3 1.517(3) . ? C2 H2 0.95(2) . ? C3 C4 1.533(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.511(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.396(3) . ? C5 H5 0.92(2) . ? C6 C7 1.526(3) . ? C6 H6 0.944(19) . ? C7 C8 1.543(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.387(3) . ? C9 H9 0.9500 . ? C10 C11 1.371(3) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C13 1.530(2) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C19 1.394(3) . ? C14 C15 1.400(3) . ? C15 C16 1.392(3) . ? C15 H15 0.9500 . ? C16 C17 1.387(4) . ? C16 H16 0.9500 . ? C17 C18 1.375(4) . ? C17 H17 0.9500 . ? C18 C19 1.391(3) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C21 1.394(3) . ? C20 C25 1.395(3) . ? C21 C22 1.387(3) . ? C21 H21 0.9500 . ? C22 C23 1.386(3) . ? C22 H22 0.9500 . ? C23 C24 1.384(3) . ? C23 H23 0.9500 . ? C24 C25 1.386(3) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C27 1.402(3) . ? C26 C31 1.409(3) . ? C26 B1 1.655(3) . ? C27 C28 1.401(3) . ? C27 H27 0.9500 . ? C28 C29 1.383(3) . ? C28 H28 0.9500 . ? C29 C30 1.389(3) . ? C29 H29 0.9500 . ? C30 C31 1.389(3) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 C37 1.399(3) . ? C32 C33 1.406(3) . ? C32 H32 0.9500 . ? C33 C34 1.375(3) . ? C33 H33 0.9500 . ? C34 C35 1.379(3) . ? C34 H34 0.9500 . ? C35 C36 1.389(3) . ? C35 H35 0.9500 . ? C36 C37 1.408(3) . ? C36 H36 0.9500 . ? C37 B1 1.653(3) . ? C38 C43 1.393(3) . ? C38 C39 1.409(3) . ? C38 B1 1.659(3) . ? C39 C40 1.390(3) . ? C39 H39 0.9500 . ? C40 C41 1.389(3) . ? C40 H40 0.9500 . ? C41 C42 1.376(3) . ? C41 H41 0.9500 . ? C42 C43 1.392(3) . ? C42 H42 0.9500 . ? C43 H43 0.9500 . ? C44 C49 1.402(3) . ? C44 C45 1.406(3) . ? C44 B1 1.656(3) . ? C45 C46 1.380(3) . ? C45 H45 0.9500 . ? C46 C47 1.388(3) . ? C46 H46 0.9500 . ? C47 C48 1.386(3) . ? C47 H47 0.9500 . ? C48 C49 1.395(3) . ? 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 Rh1 C6 154.65(7) . . ? N1 Rh1 C5 167.38(7) . . ? C6 Rh1 C5 37.95(7) . . ? N1 Rh1 C1 87.85(7) . . ? C6 Rh1 C1 81.69(7) . . ? C5 Rh1 C1 96.57(7) . . ? N1 Rh1 C2 96.86(7) . . ? C6 Rh1 C2 87.94(7) . . ? C5 Rh1 C2 80.38(7) . . ? C1 Rh1 C2 35.48(7) . . ? N1 Rh1 P1 88.86(4) . . ? C6 Rh1 P1 97.57(5) . . ? C5 Rh1 P1 88.58(5) . . ? C1 Rh1 P1 170.20(5) . . ? C2 Rh1 P1 154.28(5) . . ? C20 P1 C14 105.48(9) . . ? C20 P1 C13 104.88(9) . . ? C14 P1 C13 103.82(8) . . ? C20 P1 Rh1 110.83(6) . . ? C14 P1 Rh1 118.81(7) . . ? C13 P1 Rh1 111.88(6) . . ? C9 N1 N2 105.23(15) . . ? C9 N1 Rh1 130.57(13) . . ? N2 N1 Rh1 124.11(11) . . ? C11 N2 N1 110.62(15) . . ? C11 N2 C12 126.82(16) . . ? N1 N2 C12 122.56(15) . . ? C2 C1 C8 124.85(18) . . ? C2 C1 Rh1 72.37(11) . . ? C8 C1 Rh1 106.73(13) . . ? C2 C1 H1 116.4(14) . . ? C8 C1 H1 117.1(14) . . ? Rh1 C1 H1 103.6(14) . . ? C1 C2 C3 124.24(18) . . ? C1 C2 Rh1 72.15(11) . . ? C3 C2 Rh1 111.05(12) . . ? C1 C2 H2 115.4(12) . . ? C3 C2 H2 118.5(12) . . ? Rh1 C2 H2 99.6(11) . . ? C2 C3 C4 112.99(15) . . ? C2 C3 H3A 109.0 . . ? C4 C3 H3A 109.0 . . ? C2 C3 H3B 109.0 . . ? C4 C3 H3B 109.0 . . ? H3A C3 H3B 107.8 . . ? C5 C4 C3 113.08(16) . . ? C5 C4 H4A 109.0 . . ? C3 C4 H4A 109.0 . . ? C5 C4 H4B 109.0 . . ? C3 C4 H4B 109.0 . . ? H4A C4 H4B 107.8 . . ? C6 C5 C4 125.70(17) . . ? C6 C5 Rh1 70.51(11) . . ? C4 C5 Rh1 110.64(12) . . ? C6 C5 H5 121.9(13) . . ? C4 C5 H5 108.3(12) . . ? Rh1 C5 H5 111.3(13) . . ? C5 C6 C7 124.82(17) . . ? C5 C6 Rh1 71.54(11) . . ? C7 C6 Rh1 113.13(13) . . ? C5 C6 H6 116.4(12) . . ? C7 C6 H6 115.1(13) . . ? Rh1 C6 H6 104.0(13) . . ? C6 C7 C8 113.78(17) . . ? C6 C7 H7A 108.8 . . ? C8 C7 H7A 108.8 . . ? C6 C7 H7B 108.8 . . ? C8 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? C1 C8 C7 114.10(17) . . ? C1 C8 H8A 108.7 . . ? C7 C8 H8A 108.7 . . ? C1 C8 H8B 108.7 . . ? C7 C8 H8B 108.7 . . ? H8A C8 H8B 107.6 . . ? N1 C9 C10 111.06(16) . . ? N1 C9 H9 124.5 . . ? C10 C9 H9 124.5 . . ? C11 C10 C9 105.35(17) . . ? C11 C10 H10 127.3 . . ? C9 C10 H10 127.3 . . ? N2 C11 C10 107.74(17) . . ? N2 C11 H11 126.1 . . ? C10 C11 H11 126.1 . . ? N2 C12 C13 112.17(15) . . ? N2 C12 H12A 109.2 . . ? C13 C12 H12A 109.2 . . ? N2 C12 H12B 109.2 . . ? C13 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? C12 C13 P1 111.64(13) . . ? C12 C13 H13A 109.3 . . ? P1 C13 H13A 109.3 . . ? C12 C13 H13B 109.3 . . ? P1 C13 H13B 109.3 . . ? H13A C13 H13B 108.0 . . ? C19 C14 C15 119.03(19) . . ? C19 C14 P1 122.90(16) . . ? C15 C14 P1 117.93(14) . . ? C16 C15 C14 120.3(2) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C17 C16 C15 120.0(2) . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C18 C17 C16 120.0(2) . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C17 C18 C19 120.7(2) . . ? C17 C18 H18 119.7 . . ? C19 C18 H18 119.7 . . ? C18 C19 C14 120.0(2) . . ? C18 C19 H19 120.0 . . ? C14 C19 H19 120.0 . . ? C21 C20 C25 118.80(17) . . ? C21 C20 P1 119.70(14) . . ? C25 C20 P1 121.50(15) . . ? C22 C21 C20 120.70(18) . . ? C22 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? C23 C22 C21 119.92(19) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C24 C23 C22 119.9(2) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C23 C24 C25 120.3(2) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C24 C25 C20 120.38(19) . . ? C24 C25 H25 119.8 . . ? C20 C25 H25 119.8 . . ? C27 C26 C31 114.97(18) . . ? C27 C26 B1 125.80(16) . . ? C31 C26 B1 119.20(18) . . ? C28 C27 C26 122.57(19) . . ? C28 C27 H27 118.7 . . ? C26 C27 H27 118.7 . . ? C29 C28 C27 120.4(2) . . ? C29 C28 H28 119.8 . . ? C27 C28 H28 119.8 . . ? C28 C29 C30 118.76(19) . . ? C28 C29 H29 120.6 . . ? C30 C29 H29 120.6 . . ? C31 C30 C29 120.20(19) . . ? C31 C30 H30 119.9 . . ? C29 C30 H30 119.9 . . ? C30 C31 C26 123.05(19) . . ? C30 C31 H31 118.5 . . ? C26 C31 H31 118.5 . . ? C37 C32 C33 122.2(2) . . ? C37 C32 H32 118.9 . . ? C33 C32 H32 118.9 . . ? C34 C33 C32 120.5(2) . . ? C34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C33 C34 C35 119.0(2) . . ? C33 C34 H34 120.5 . . ? C35 C34 H34 120.5 . . ? C34 C35 C36 120.2(2) . . ? C34 C35 H35 119.9 . . ? C36 C35 H35 119.9 . . ? C35 C36 C37 122.96(19) . . ? C35 C36 H36 118.5 . . ? C37 C36 H36 118.5 . . ? C32 C37 C36 115.03(18) . . ? C32 C37 B1 125.83(17) . . ? C36 C37 B1 119.08(16) . . ? C43 C38 C39 114.45(17) . . ? C43 C38 B1 124.13(16) . . ? C39 C38 B1 121.41(17) . . ? C40 C39 C38 123.0(2) . . ? C40 C39 H39 118.5 . . ? C38 C39 H39 118.5 . . ? C41 C40 C39 120.3(2) . . ? C41 C40 H40 119.8 . . ? C39 C40 H40 119.8 . . ? C42 C41 C40 118.24(19) . . ? C42 C41 H41 120.9 . . ? C40 C41 H41 120.9 . . ? C41 C42 C43 120.7(2) . . ? C41 C42 H42 119.6 . . ? C43 C42 H42 119.6 . . ? C42 C43 C38 123.23(19) . . ? C42 C43 H43 118.4 . . ? C38 C43 H43 118.4 . . ? C49 C44 C45 115.06(17) . . ? C49 C44 B1 124.06(17) . . ? C45 C44 B1 120.88(18) . . ? C46 C45 C44 123.0(2) . . ? C46 C45 H45 118.5 . . ? C44 C45 H45 118.5 . . ? C45 C46 C47 120.37(19) . . ? C45 C46 H46 119.8 . . ? C47 C46 H46 119.8 . . ? C48 C47 C46 118.83(19) . . ? C48 C47 H47 120.6 . . ? C46 C47 H47 120.6 . . ? C47 C48 C49 120.0(2) . . ? C47 C48 H48 120.0 . . ? C49 C48 H48 120.0 . . ? C48 C49 C44 122.73(19) . . ? C48 C49 H49 118.6 . . ? C44 C49 H49 118.6 . . ? C37 B1 C26 112.53(15) . . ? C37 B1 C44 108.17(15) . . ? C26 B1 C44 106.65(14) . . ? C37 B1 C38 107.91(15) . . ? C26 B1 C38 111.28(15) . . ? C44 B1 C38 110.26(15) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Rh1 P1 C20 -88.30(8) . . . . ? C6 Rh1 P1 C20 116.30(8) . . . . ? C5 Rh1 P1 C20 79.33(8) . . . . ? C1 Rh1 P1 C20 -158.7(3) . . . . ? C2 Rh1 P1 C20 15.23(14) . . . . ? N1 Rh1 P1 C14 149.34(8) . . . . ? C6 Rh1 P1 C14 -6.05(8) . . . . ? C5 Rh1 P1 C14 -43.02(9) . . . . ? C1 Rh1 P1 C14 78.9(3) . . . . ? C2 Rh1 P1 C14 -107.12(14) . . . . ? N1 Rh1 P1 C13 28.37(9) . . . . ? C6 Rh1 P1 C13 -127.03(9) . . . . ? C5 Rh1 P1 C13 -163.99(9) . . . . ? C1 Rh1 P1 C13 -42.0(3) . . . . ? C2 Rh1 P1 C13 131.90(14) . . . . ? C6 Rh1 N1 C9 -113.0(2) . . . . ? C5 Rh1 N1 C9 63.2(4) . . . . ? C1 Rh1 N1 C9 -47.69(17) . . . . ? C2 Rh1 N1 C9 -13.30(18) . . . . ? P1 Rh1 N1 C9 141.55(17) . . . . ? C6 Rh1 N1 N2 62.9(2) . . . . ? C5 Rh1 N1 N2 -120.9(3) . . . . ? C1 Rh1 N1 N2 128.21(14) . . . . ? C2 Rh1 N1 N2 162.59(14) . . . . ? P1 Rh1 N1 N2 -42.56(13) . . . . ? C9 N1 N2 C11 0.3(2) . . . . ? Rh1 N1 N2 C11 -176.45(12) . . . . ? C9 N1 N2 C12 179.90(16) . . . . ? Rh1 N1 N2 C12 3.1(2) . . . . ? N1 Rh1 C1 C2 104.98(12) . . . . ? C6 Rh1 C1 C2 -98.18(13) . . . . ? C5 Rh1 C1 C2 -63.16(13) . . . . ? P1 Rh1 C1 C2 175.5(3) . . . . ? N1 Rh1 C1 C8 -132.97(13) . . . . ? C6 Rh1 C1 C8 23.87(13) . . . . ? C5 Rh1 C1 C8 58.89(14) . . . . ? C2 Rh1 C1 C8 122.05(19) . . . . ? P1 Rh1 C1 C8 -62.5(4) . . . . ? C8 C1 C2 C3 5.3(3) . . . . ? Rh1 C1 C2 C3 103.72(17) . . . . ? C8 C1 C2 Rh1 -98.45(19) . . . . ? N1 Rh1 C2 C1 -76.48(12) . . . . ? C6 Rh1 C2 C1 78.54(13) . . . . ? C5 Rh1 C2 C1 115.97(13) . . . . ? P1 Rh1 C2 C1 -178.23(10) . . . . ? N1 Rh1 C2 C3 162.90(13) . . . . ? C6 Rh1 C2 C3 -42.08(14) . . . . ? C5 Rh1 C2 C3 -4.66(13) . . . . ? C1 Rh1 C2 C3 -120.63(19) . . . . ? P1 Rh1 C2 C3 61.1(2) . . . . ? C1 C2 C3 C4 -96.5(2) . . . . ? Rh1 C2 C3 C4 -14.3(2) . . . . ? C2 C3 C4 C5 34.7(2) . . . . ? C3 C4 C5 C6 42.2(3) . . . . ? C3 C4 C5 Rh1 -38.1(2) . . . . ? N1 Rh1 C5 C6 -177.4(3) . . . . ? C1 Rh1 C5 C6 -67.40(11) . . . . ? C2 Rh1 C5 C6 -99.09(12) . . . . ? P1 Rh1 C5 C6 104.24(10) . . . . ? N1 Rh1 C5 C4 -55.5(4) . . . . ? C6 Rh1 C5 C4 121.88(19) . . . . ? C1 Rh1 C5 C4 54.48(14) . . . . ? C2 Rh1 C5 C4 22.79(14) . . . . ? P1 Rh1 C5 C4 -133.87(13) . . . . ? C4 C5 C6 C7 3.9(3) . . . . ? Rh1 C5 C6 C7 105.79(19) . . . . ? C4 C5 C6 Rh1 -101.90(18) . . . . ? N1 Rh1 C6 C5 178.67(13) . . . . ? C1 Rh1 C6 C5 112.05(11) . . . . ? C2 Rh1 C6 C5 76.95(11) . . . . ? P1 Rh1 C6 C5 -77.82(10) . . . . ? N1 Rh1 C6 C7 57.9(2) . . . . ? C5 Rh1 C6 C7 -120.80(18) . . . . ? C1 Rh1 C6 C7 -8.75(13) . . . . ? C2 Rh1 C6 C7 -43.84(14) . . . . ? P1 Rh1 C6 C7 161.39(12) . . . . ? C5 C6 C7 C8 -91.3(2) . . . . ? Rh1 C6 C7 C8 -8.3(2) . . . . ? C2 C1 C8 C7 44.2(3) . . . . ? Rh1 C1 C8 C7 -35.6(2) . . . . ? C6 C7 C8 C1 30.5(2) . . . . ? N2 N1 C9 C10 -0.3(2) . . . . ? Rh1 N1 C9 C10 176.18(13) . . . . ? N1 C9 C10 C11 0.2(2) . . . . ? N1 N2 C11 C10 -0.2(2) . . . . ? C12 N2 C11 C10 -179.78(17) . . . . ? C9 C10 C11 N2 0.0(2) . . . . ? C11 N2 C12 C13 -115.6(2) . . . . ? N1 N2 C12 C13 64.9(2) . . . . ? N2 C12 C13 P1 -67.86(19) . . . . ? C20 P1 C13 C12 134.71(14) . . . . ? C14 P1 C13 C12 -114.82(15) . . . . ? Rh1 P1 C13 C12 14.50(16) . . . . ? C20 P1 C14 C19 -19.93(19) . . . . ? C13 P1 C14 C19 -129.96(17) . . . . ? Rh1 P1 C14 C19 105.06(17) . . . . ? C20 P1 C14 C15 164.30(16) . . . . ? C13 P1 C14 C15 54.27(18) . . . . ? Rh1 P1 C14 C15 -70.71(16) . . . . ? C19 C14 C15 C16 -0.9(3) . . . . ? P1 C14 C15 C16 175.01(17) . . . . ? C14 C15 C16 C17 0.8(3) . . . . ? C15 C16 C17 C18 -0.5(3) . . . . ? C16 C17 C18 C19 0.3(3) . . . . ? C17 C18 C19 C14 -0.4(3) . . . . ? C15 C14 C19 C18 0.8(3) . . . . ? P1 C14 C19 C18 -174.97(16) . . . . ? C14 P1 C20 C21 118.92(15) . . . . ? C13 P1 C20 C21 -131.81(15) . . . . ? Rh1 P1 C20 C21 -10.90(16) . . . . ? C14 P1 C20 C25 -61.90(17) . . . . ? C13 P1 C20 C25 47.37(17) . . . . ? Rh1 P1 C20 C25 168.28(14) . . . . ? C25 C20 C21 C22 0.6(3) . . . . ? P1 C20 C21 C22 179.84(15) . . . . ? C20 C21 C22 C23 -0.1(3) . . . . ? C21 C22 C23 C24 -0.3(3) . . . . ? C22 C23 C24 C25 0.1(3) . . . . ? C23 C24 C25 C20 0.5(3) . . . . ? C21 C20 C25 C24 -0.9(3) . . . . ? P1 C20 C25 C24 179.95(17) . . . . ? C31 C26 C27 C28 -1.9(3) . . . . ? B1 C26 C27 C28 179.89(18) . . . . ? C26 C27 C28 C29 1.4(3) . . . . ? C27 C28 C29 C30 0.0(3) . . . . ? C28 C29 C30 C31 -0.9(3) . . . . ? C29 C30 C31 C26 0.3(3) . . . . ? C27 C26 C31 C30 1.0(3) . . . . ? B1 C26 C31 C30 179.40(17) . . . . ? C37 C32 C33 C34 0.8(3) . . . . ? C32 C33 C34 C35 0.8(3) . . . . ? C33 C34 C35 C36 -0.9(3) . . . . ? C34 C35 C36 C37 -0.4(3) . . . . ? C33 C32 C37 C36 -2.0(3) . . . . ? C33 C32 C37 B1 -179.14(17) . . . . ? C35 C36 C37 C32 1.9(3) . . . . ? C35 C36 C37 B1 179.19(18) . . . . ? C43 C38 C39 C40 -2.7(3) . . . . ? B1 C38 C39 C40 178.5(2) . . . . ? C38 C39 C40 C41 1.4(3) . . . . ? C39 C40 C41 C42 0.4(3) . . . . ? C40 C41 C42 C43 -0.8(3) . . . . ? C41 C42 C43 C38 -0.6(3) . . . . ? C39 C38 C43 C42 2.3(3) . . . . ? B1 C38 C43 C42 -178.91(19) . . . . ? C49 C44 C45 C46 2.3(3) . . . . ? B1 C44 C45 C46 -178.36(17) . . . . ? C44 C45 C46 C47 -2.7(3) . . . . ? C45 C46 C47 C48 0.7(3) . . . . ? C46 C47 C48 C49 1.5(3) . . . . ? C47 C48 C49 C44 -1.9(3) . . . . ? C45 C44 C49 C48 0.0(3) . . . . ? B1 C44 C49 C48 -179.37(18) . . . . ? C32 C37 B1 C26 -17.6(3) . . . . ? C36 C37 B1 C26 165.39(16) . . . . ? C32 C37 B1 C44 99.9(2) . . . . ? C36 C37 B1 C44 -77.1(2) . . . . ? C32 C37 B1 C38 -140.77(18) . . . . ? C36 C37 B1 C38 42.2(2) . . . . ? C27 C26 B1 C37 -117.1(2) . . . . ? C31 C26 B1 C37 64.8(2) . . . . ? C27 C26 B1 C44 124.47(19) . . . . ? C31 C26 B1 C44 -53.7(2) . . . . ? C27 C26 B1 C38 4.2(2) . . . . ? C31 C26 B1 C38 -173.99(16) . . . . ? C49 C44 B1 C37 2.3(2) . . . . ? C45 C44 B1 C37 -177.07(16) . . . . ? C49 C44 B1 C26 123.53(19) . . . . ? C45 C44 B1 C26 -55.8(2) . . . . ? C49 C44 B1 C38 -115.5(2) . . . . ? C45 C44 B1 C38 65.1(2) . . . . ? C43 C38 B1 C37 -115.86(19) . . . . ? C39 C38 B1 C37 62.8(2) . . . . ? C43 C38 B1 C26 120.22(18) . . . . ? C39 C38 B1 C26 -61.1(2) . . . . ? C43 C38 B1 C44 2.1(2) . . . . ? C39 C38 B1 C44 -179.24(17) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.593 _refine_diff_density_min -0.240 _refine_diff_density_rms 0.050 #===END data_bam8 _database_code_CSD 207602 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H17 Cl Ir N2 O P' _chemical_formula_weight 535.96 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' 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' 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' _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 11.912(3) _cell_length_b 13.040(3) _cell_length_c 12.137(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.564(4) _cell_angle_gamma 90.00 _cell_volume 1868.8(7) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 947 _cell_measurement_theta_min 3.008 _cell_measurement_theta_max 28.129 _exptl_crystal_description blade _exptl_crystal_colour yellow _exptl_crystal_size_max 0.408 _exptl_crystal_size_mid 0.144 _exptl_crystal_size_min 0.058 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.905 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1024 _exptl_absorpt_coefficient_mu 7.380 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.172 _exptl_absorpt_correction_T_max 0.657 _exptl_absorpt_process_details ; Gaussian (Coppens et al., 1965) XPREP (Bruker, 1995) ; _diffrn_crystal_treatment ; attached to a thin glass fibre ; _diffrn_ambient_temperature 295(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 242 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.1 _diffrn_reflns_number 18392 _diffrn_reflns_av_R_equivalents 0.0323 _diffrn_reflns_av_sigmaI/netI 0.0156 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 28.27 _reflns_number_total 4469 _reflns_number_gt 3924 _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 4469 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0213 _refine_ls_R_factor_gt 0.0167 _refine_ls_wR_factor_ref 0.0407 _refine_ls_wR_factor_gt 0.0397 _refine_ls_goodness_of_fit_ref 1.165 _refine_ls_restrained_S_all 1.165 _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 Ir1 Ir 0.198284(8) 0.578943(6) 0.260420(7) 0.03281(4) Uani 1 1 d . . . Cl1 Cl 0.15642(6) 0.49060(5) 0.08745(5) 0.05027(16) Uani 1 1 d . . . P1 P 0.24306(5) 0.66009(5) 0.42061(5) 0.03713(14) Uani 1 1 d . . . O1 O 0.3722(2) 0.42322(17) 0.3348(2) 0.0872(9) Uani 1 1 d . . . N1 N 0.06137(17) 0.67891(14) 0.20812(15) 0.0362(4) Uani 1 1 d . . . N2 N 0.03786(19) 0.77212(16) 0.25052(19) 0.0478(5) Uani 1 1 d . . . C1 C 0.3071(2) 0.4853(2) 0.3049(2) 0.0501(7) Uani 1 1 d . . . C2 C -0.0264(2) 0.6596(2) 0.1299(2) 0.0432(6) Uani 1 1 d . . . H2 H -0.0343 0.6001 0.0874 0.052 Uiso 1 1 calc R . . C3 C -0.1032(2) 0.7388(2) 0.1203(2) 0.0533(7) Uani 1 1 d . . . H3 H -0.1700 0.7436 0.0715 0.064 Uiso 1 1 calc R . . C4 C -0.0597(3) 0.8090(2) 0.1984(3) 0.0584(8) Uani 1 1 d . . . H4 H -0.0923 0.8715 0.2128 0.070 Uiso 1 1 calc R . . C5 C 0.1122(3) 0.8228(2) 0.3402(2) 0.0557(7) Uani 1 1 d . . . H5A H 0.0766 0.8856 0.3606 0.067 Uiso 1 1 calc R . . H5B H 0.1829 0.8408 0.3137 0.067 Uiso 1 1 calc R . . C6 C 0.1367(2) 0.7554(2) 0.4415(2) 0.0518(7) Uani 1 1 d . . . H6A H 0.0676 0.7214 0.4559 0.062 Uiso 1 1 calc R . . H6B H 0.1635 0.7973 0.5057 0.062 Uiso 1 1 calc R . . C7 C 0.3747(2) 0.73340(19) 0.4361(2) 0.0407(6) Uani 1 1 d . . . C8 C 0.4548(3) 0.7154(2) 0.3656(3) 0.0605(8) Uani 1 1 d . . . H8 H 0.4412 0.6663 0.3099 0.073 Uiso 1 1 calc R . . C9 C 0.5559(3) 0.7703(3) 0.3778(3) 0.0794(11) Uani 1 1 d . . . H9 H 0.6095 0.7570 0.3303 0.095 Uiso 1 1 calc R . . C10 C 0.5773(3) 0.8424(3) 0.4572(3) 0.0785(11) Uani 1 1 d . . . H10 H 0.6454 0.8781 0.4654 0.094 Uiso 1 1 calc R . . C11 C 0.4969(3) 0.8628(3) 0.5262(3) 0.0796(11) Uani 1 1 d . . . H11 H 0.5107 0.9136 0.5801 0.095 Uiso 1 1 calc R . . C12 C 0.3970(3) 0.8092(2) 0.5168(2) 0.0598(8) Uani 1 1 d . . . H12 H 0.3440 0.8236 0.5645 0.072 Uiso 1 1 calc R . . C13 C 0.2527(2) 0.57988(19) 0.5447(2) 0.0447(6) Uani 1 1 d . . . C14 C 0.3426(3) 0.5823(2) 0.6279(3) 0.0637(9) Uani 1 1 d . . . H14 H 0.4031 0.6261 0.6220 0.076 Uiso 1 1 calc R . . C15 C 0.3442(3) 0.5200(3) 0.7208(3) 0.0791(11) Uani 1 1 d . . . H15 H 0.4048 0.5236 0.7773 0.095 Uiso 1 1 calc R . . C16 C 0.2577(4) 0.4538(3) 0.7297(3) 0.0755(10) Uani 1 1 d . . . H16 H 0.2600 0.4108 0.7910 0.091 Uiso 1 1 calc R . . C17 C 0.1681(4) 0.4511(3) 0.6483(3) 0.1000(15) Uani 1 1 d . . . H17 H 0.1077 0.4074 0.6550 0.120 Uiso 1 1 calc R . . C18 C 0.1659(3) 0.5126(3) 0.5561(3) 0.0900(14) Uani 1 1 d . . . H18 H 0.1046 0.5087 0.5003 0.108 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.03247(6) 0.03458(6) 0.03129(5) -0.00504(3) 0.00393(4) -0.00286(4) Cl1 0.0585(4) 0.0509(4) 0.0393(3) -0.0152(3) -0.0014(3) 0.0055(3) P1 0.0345(3) 0.0439(4) 0.0333(3) -0.0077(3) 0.0052(3) -0.0079(3) O1 0.0749(18) 0.0842(18) 0.0949(19) -0.0144(13) -0.0177(15) 0.0384(14) N1 0.0377(12) 0.0361(11) 0.0356(10) -0.0017(8) 0.0072(9) 0.0003(9) N2 0.0444(13) 0.0415(12) 0.0563(13) -0.0095(10) 0.0029(11) 0.0042(10) C1 0.0452(16) 0.0543(17) 0.0487(15) -0.0125(13) -0.0019(13) 0.0066(14) C2 0.0449(15) 0.0493(15) 0.0349(12) -0.0003(11) 0.0030(11) -0.0027(12) C3 0.0413(16) 0.0638(18) 0.0530(16) 0.0038(14) -0.0007(13) 0.0095(14) C4 0.0506(18) 0.0512(17) 0.072(2) -0.0017(15) 0.0032(15) 0.0170(14) C5 0.0521(18) 0.0404(15) 0.0721(19) -0.0202(14) -0.0005(15) 0.0029(13) C6 0.0449(16) 0.0606(17) 0.0504(15) -0.0260(13) 0.0084(13) -0.0025(13) C7 0.0389(14) 0.0442(14) 0.0379(12) -0.0019(11) 0.0009(10) -0.0102(11) C8 0.0477(18) 0.067(2) 0.069(2) -0.0107(16) 0.0154(15) -0.0176(15) C9 0.051(2) 0.088(3) 0.103(3) 0.004(2) 0.0239(19) -0.0224(19) C10 0.055(2) 0.070(2) 0.105(3) 0.016(2) -0.011(2) -0.0324(19) C11 0.082(3) 0.069(2) 0.081(2) -0.0117(19) -0.015(2) -0.034(2) C12 0.063(2) 0.0574(18) 0.0580(18) -0.0134(14) 0.0023(15) -0.0163(16) C13 0.0479(16) 0.0516(16) 0.0353(13) -0.0071(11) 0.0079(12) -0.0120(12) C14 0.0514(19) 0.069(2) 0.067(2) 0.0226(15) -0.0034(16) -0.0108(15) C15 0.072(2) 0.087(3) 0.072(2) 0.0307(19) -0.0131(19) -0.007(2) C16 0.093(3) 0.075(2) 0.059(2) 0.0177(17) 0.011(2) -0.017(2) C17 0.106(3) 0.123(3) 0.069(2) 0.026(2) 0.006(2) -0.067(3) C18 0.084(3) 0.130(3) 0.0506(18) 0.018(2) -0.0092(18) -0.064(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 C1 1.811(3) . ? Ir1 N1 2.119(2) . ? Ir1 P1 2.2161(7) . ? Ir1 Cl1 2.3890(7) . ? P1 C6 1.817(3) . ? P1 C7 1.825(3) . ? P1 C13 1.825(3) . ? O1 C1 1.146(3) . ? N1 C2 1.340(3) . ? N1 N2 1.363(3) . ? N2 C4 1.337(3) . ? N2 C5 1.467(3) . ? C2 C3 1.374(4) . ? C2 H2 0.9300 . ? C3 C4 1.370(4) . ? C3 H3 0.9300 . ? C4 H4 0.9300 . ? C5 C6 1.507(4) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.383(4) . ? C7 C12 1.393(4) . ? C8 C9 1.392(4) . ? C8 H8 0.9300 . ? C9 C10 1.347(5) . ? C9 H9 0.9300 . ? C10 C11 1.378(5) . ? C10 H10 0.9300 . ? C11 C12 1.372(4) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.372(4) . ? C13 C18 1.377(4) . ? C14 C15 1.387(4) . ? C14 H14 0.9300 . ? C15 C16 1.358(5) . ? C15 H15 0.9300 . ? C16 C17 1.356(5) . ? C16 H16 0.9300 . ? C17 C18 1.374(5) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? 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 Ir1 N1 175.40(10) . . ? C1 Ir1 P1 88.88(8) . . ? N1 Ir1 P1 93.21(5) . . ? C1 Ir1 Cl1 89.72(8) . . ? N1 Ir1 Cl1 88.28(5) . . ? P1 Ir1 Cl1 178.14(2) . . ? C6 P1 C7 103.46(13) . . ? C6 P1 C13 104.27(13) . . ? C7 P1 C13 104.79(12) . . ? C6 P1 Ir1 110.95(9) . . ? C7 P1 Ir1 116.41(8) . . ? C13 P1 Ir1 115.61(8) . . ? C2 N1 N2 104.8(2) . . ? C2 N1 Ir1 126.49(17) . . ? N2 N1 Ir1 128.59(15) . . ? C4 N2 N1 110.6(2) . . ? C4 N2 C5 126.2(2) . . ? N1 N2 C5 123.2(2) . . ? O1 C1 Ir1 176.9(3) . . ? N1 C2 C3 111.6(2) . . ? N1 C2 H2 124.2 . . ? C3 C2 H2 124.2 . . ? C4 C3 C2 104.8(3) . . ? C4 C3 H3 127.6 . . ? C2 C3 H3 127.6 . . ? N2 C4 C3 108.3(2) . . ? N2 C4 H4 125.9 . . ? C3 C4 H4 125.9 . . ? N2 C5 C6 112.1(2) . . ? N2 C5 H5A 109.2 . . ? C6 C5 H5A 109.2 . . ? N2 C5 H5B 109.2 . . ? C6 C5 H5B 109.2 . . ? H5A C5 H5B 107.9 . . ? C5 C6 P1 110.38(19) . . ? C5 C6 H6A 109.6 . . ? P1 C6 H6A 109.6 . . ? C5 C6 H6B 109.6 . . ? P1 C6 H6B 109.6 . . ? H6A C6 H6B 108.1 . . ? C8 C7 C12 118.1(3) . . ? C8 C7 P1 120.1(2) . . ? C12 C7 P1 121.8(2) . . ? C7 C8 C9 120.4(3) . . ? C7 C8 H8 119.8 . . ? C9 C8 H8 119.8 . . ? C10 C9 C8 120.9(3) . . ? C10 C9 H9 119.5 . . ? C8 C9 H9 119.5 . . ? C9 C10 C11 119.3(3) . . ? C9 C10 H10 120.4 . . ? C11 C10 H10 120.4 . . ? C12 C11 C10 121.0(3) . . ? C12 C11 H11 119.5 . . ? C10 C11 H11 119.5 . . ? C11 C12 C7 120.2(3) . . ? C11 C12 H12 119.9 . . ? C7 C12 H12 119.9 . . ? C14 C13 C18 117.6(3) . . ? C14 C13 P1 123.6(2) . . ? C18 C13 P1 118.8(2) . . ? C13 C14 C15 120.7(3) . . ? C13 C14 H14 119.6 . . ? C15 C14 H14 119.6 . . ? C16 C15 C14 120.5(3) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C17 C16 C15 119.4(3) . . ? C17 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? C16 C17 C18 120.4(3) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C17 C18 C13 121.3(3) . . ? C17 C18 H18 119.3 . . ? C13 C18 H18 119.3 . . ? 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 Ir1 P1 C6 -167.62(14) . . . . ? N1 Ir1 P1 C6 8.28(12) . . . . ? Cl1 Ir1 P1 C6 151.3(7) . . . . ? C1 Ir1 P1 C7 74.46(14) . . . . ? N1 Ir1 P1 C7 -109.64(11) . . . . ? Cl1 Ir1 P1 C7 33.4(8) . . . . ? C1 Ir1 P1 C13 -49.18(14) . . . . ? N1 Ir1 P1 C13 126.72(12) . . . . ? Cl1 Ir1 P1 C13 -90.2(7) . . . . ? C1 Ir1 N1 C2 -42.9(12) . . . . ? P1 Ir1 N1 C2 -159.72(19) . . . . ? Cl1 Ir1 N1 C2 21.40(19) . . . . ? C1 Ir1 N1 N2 131.8(12) . . . . ? P1 Ir1 N1 N2 14.94(19) . . . . ? Cl1 Ir1 N1 N2 -163.94(19) . . . . ? C2 N1 N2 C4 -1.1(3) . . . . ? Ir1 N1 N2 C4 -176.69(18) . . . . ? C2 N1 N2 C5 179.4(2) . . . . ? Ir1 N1 N2 C5 3.8(3) . . . . ? N1 Ir1 C1 O1 -22(6) . . . . ? P1 Ir1 C1 O1 95(5) . . . . ? Cl1 Ir1 C1 O1 -87(5) . . . . ? N2 N1 C2 C3 1.2(3) . . . . ? Ir1 N1 C2 C3 176.92(17) . . . . ? N1 C2 C3 C4 -0.9(3) . . . . ? N1 N2 C4 C3 0.6(3) . . . . ? C5 N2 C4 C3 -179.9(3) . . . . ? C2 C3 C4 N2 0.1(3) . . . . ? C4 N2 C5 C6 125.6(3) . . . . ? N1 N2 C5 C6 -55.0(3) . . . . ? N2 C5 C6 P1 78.1(3) . . . . ? C7 P1 C6 C5 75.3(2) . . . . ? C13 P1 C6 C5 -175.29(19) . . . . ? Ir1 P1 C6 C5 -50.2(2) . . . . ? C6 P1 C7 C8 -139.2(2) . . . . ? C13 P1 C7 C8 111.8(2) . . . . ? Ir1 P1 C7 C8 -17.2(3) . . . . ? C6 P1 C7 C12 39.9(3) . . . . ? C13 P1 C7 C12 -69.1(3) . . . . ? Ir1 P1 C7 C12 161.9(2) . . . . ? C12 C7 C8 C9 1.5(5) . . . . ? P1 C7 C8 C9 -179.3(3) . . . . ? C7 C8 C9 C10 -0.6(6) . . . . ? C8 C9 C10 C11 -0.9(6) . . . . ? C9 C10 C11 C12 1.5(6) . . . . ? C10 C11 C12 C7 -0.5(5) . . . . ? C8 C7 C12 C11 -1.0(5) . . . . ? P1 C7 C12 C11 179.9(3) . . . . ? C6 P1 C13 C14 -107.0(3) . . . . ? C7 P1 C13 C14 1.4(3) . . . . ? Ir1 P1 C13 C14 130.9(2) . . . . ? C6 P1 C13 C18 73.3(3) . . . . ? C7 P1 C13 C18 -178.3(3) . . . . ? Ir1 P1 C13 C18 -48.7(3) . . . . ? C18 C13 C14 C15 -1.0(5) . . . . ? P1 C13 C14 C15 179.3(3) . . . . ? C13 C14 C15 C16 1.5(6) . . . . ? C14 C15 C16 C17 -1.9(7) . . . . ? C15 C16 C17 C18 1.8(7) . . . . ? C16 C17 C18 C13 -1.4(7) . . . . ? C14 C13 C18 C17 1.0(6) . . . . ? P1 C13 C18 C17 -179.3(4) . . . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 0.308 _refine_diff_density_min -0.652 _refine_diff_density_rms 0.082 #===END data_bam9 _database_code_CSD 207603 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H17 Cl N2 O P Rh' _chemical_formula_weight 446.67 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 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 11.908(3) _cell_length_b 13.063(3) _cell_length_c 12.087(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.498(4) _cell_angle_gamma 90.00 _cell_volume 1864.2(8) _cell_formula_units_Z 4 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 884 _cell_measurement_theta_min 2.306 _cell_measurement_theta_max 24.406 _exptl_crystal_description blade _exptl_crystal_colour yellow _exptl_crystal_size_max 0.442 _exptl_crystal_size_mid 0.045 _exptl_crystal_size_min 0.032 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.591 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 1.152 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.760 _exptl_absorpt_correction_T_max 0.964 _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 294(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 126 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.01 _diffrn_reflns_number 18974 _diffrn_reflns_av_R_equivalents 0.0432 _diffrn_reflns_av_sigmaI/netI 0.0440 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 28.32 _reflns_number_total 4519 _reflns_number_gt 3157 _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^)+(0.01P)^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 4519 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0502 _refine_ls_R_factor_gt 0.0263 _refine_ls_wR_factor_ref 0.0436 _refine_ls_wR_factor_gt 0.0406 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _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 0.199054(15) 0.579097(14) 0.260579(14) 0.03410(6) Uani 1 1 d . . . Cl1 Cl 0.16045(5) 0.49050(5) 0.08647(5) 0.05000(17) Uani 1 1 d . . . P1 P 0.24432(5) 0.65865(5) 0.42207(5) 0.03766(15) Uani 1 1 d . . . O1 O 0.37131(17) 0.42323(16) 0.33370(17) 0.0883(7) Uani 1 1 d . . . N1 N 0.06168(15) 0.67959(14) 0.21047(14) 0.0363(4) Uani 1 1 d . . . N2 N 0.03668(17) 0.77142(15) 0.25418(16) 0.0467(5) Uani 1 1 d . . . C1 C 0.3063(2) 0.4855(2) 0.3048(2) 0.0504(7) Uani 1 1 d . . . C2 C -0.02500(19) 0.66103(18) 0.13107(18) 0.0424(6) Uani 1 1 d . . . H2 H -0.0317 0.6025 0.0869 0.051 Uiso 1 1 calc R . . C3 C -0.1031(2) 0.7391(2) 0.1228(2) 0.0545(7) Uani 1 1 d . . . H3 H -0.1699 0.7438 0.0739 0.065 Uiso 1 1 calc R . . C4 C -0.0612(2) 0.8081(2) 0.2019(2) 0.0606(8) Uani 1 1 d . . . H4 H -0.0947 0.8699 0.2170 0.073 Uiso 1 1 calc R . . C5 C 0.1098(2) 0.82166(19) 0.3444(2) 0.0570(7) Uani 1 1 d . . . H5A H 0.0725 0.8829 0.3666 0.068 Uiso 1 1 calc R . . H5B H 0.1796 0.8424 0.3174 0.068 Uiso 1 1 calc R . . C6 C 0.1378(2) 0.75264(18) 0.44534(19) 0.0516(7) Uani 1 1 d . . . H6A H 0.0697 0.7178 0.4608 0.062 Uiso 1 1 calc R . . H6B H 0.1653 0.7939 0.5099 0.062 Uiso 1 1 calc R . . C7 C 0.37538(19) 0.73183(17) 0.43700(18) 0.0402(6) Uani 1 1 d . . . C8 C 0.4567(2) 0.7115(2) 0.3685(2) 0.0629(8) Uani 1 1 d . . . H8 H 0.4440 0.6607 0.3144 0.076 Uiso 1 1 calc R . . C9 C 0.5574(2) 0.7664(2) 0.3798(3) 0.0812(10) Uani 1 1 d . . . H9 H 0.6116 0.7519 0.3332 0.097 Uiso 1 1 calc R . . C10 C 0.5775(3) 0.8408(2) 0.4581(3) 0.0790(10) Uani 1 1 d . . . H10 H 0.6456 0.8766 0.4659 0.095 Uiso 1 1 calc R . . C11 C 0.4973(3) 0.8627(2) 0.5250(3) 0.0814(10) Uani 1 1 d . . . H11 H 0.5104 0.9144 0.5780 0.098 Uiso 1 1 calc R . . C12 C 0.3968(2) 0.8088(2) 0.5150(2) 0.0597(7) Uani 1 1 d . . . H12 H 0.3429 0.8247 0.5615 0.072 Uiso 1 1 calc R . . C13 C 0.2542(2) 0.57885(18) 0.54654(18) 0.0427(6) Uani 1 1 d . . . C14 C 0.3414(2) 0.5837(2) 0.6322(2) 0.0603(7) Uani 1 1 d . . . H14 H 0.4008 0.6289 0.6273 0.072 Uiso 1 1 calc R . . C15 C 0.3429(3) 0.5231(2) 0.7255(2) 0.0757(9) Uani 1 1 d . . . H15 H 0.4023 0.5285 0.7833 0.091 Uiso 1 1 calc R . . C16 C 0.2575(3) 0.4549(2) 0.7334(2) 0.0747(9) Uani 1 1 d . . . H16 H 0.2591 0.4132 0.7959 0.090 Uiso 1 1 calc R . . C17 C 0.1709(3) 0.4485(3) 0.6500(3) 0.0975(12) Uani 1 1 d . . . H17 H 0.1119 0.4029 0.6554 0.117 Uiso 1 1 calc R . . C18 C 0.1697(3) 0.5096(3) 0.5566(2) 0.0847(11) Uani 1 1 d . . . H18 H 0.1101 0.5036 0.4991 0.102 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 0.03247(10) 0.03727(10) 0.03233(9) -0.00492(9) 0.00339(7) -0.00214(10) Cl1 0.0560(4) 0.0525(4) 0.0393(3) -0.0145(3) -0.0022(3) 0.0060(3) P1 0.0343(4) 0.0448(4) 0.0340(3) -0.0071(3) 0.0048(3) -0.0068(3) O1 0.0737(15) 0.0829(15) 0.1008(16) -0.0114(13) -0.0166(13) 0.0365(13) N1 0.0386(12) 0.0361(11) 0.0346(10) -0.0023(9) 0.0058(9) 0.0002(9) N2 0.0413(13) 0.0430(13) 0.0545(13) -0.0078(10) 0.0016(11) 0.0051(10) C1 0.0478(17) 0.0555(18) 0.0457(15) -0.0125(13) -0.0017(13) 0.0023(14) C2 0.0421(15) 0.0501(16) 0.0343(13) -0.0002(12) 0.0023(11) -0.0023(13) C3 0.0411(16) 0.0650(19) 0.0549(16) 0.0037(15) -0.0033(13) 0.0052(15) C4 0.0491(18) 0.0548(18) 0.076(2) 0.0007(16) 0.0020(16) 0.0178(15) C5 0.0521(17) 0.0432(16) 0.0735(19) -0.0216(15) -0.0006(15) 0.0036(14) C6 0.0432(15) 0.0624(18) 0.0495(15) -0.0246(14) 0.0072(13) -0.0018(13) C7 0.0369(14) 0.0439(15) 0.0382(13) -0.0001(12) -0.0012(11) -0.0071(12) C8 0.0476(18) 0.069(2) 0.0742(19) -0.0135(16) 0.0162(16) -0.0179(15) C9 0.052(2) 0.089(3) 0.106(3) 0.002(2) 0.0229(19) -0.0201(19) C10 0.053(2) 0.077(2) 0.101(3) 0.020(2) -0.013(2) -0.0308(19) C11 0.083(3) 0.069(2) 0.085(2) -0.0058(19) -0.014(2) -0.038(2) C12 0.0577(19) 0.0608(18) 0.0593(17) -0.0122(15) 0.0026(15) -0.0171(15) C13 0.0438(15) 0.0490(15) 0.0361(12) -0.0051(12) 0.0075(11) -0.0114(13) C14 0.0497(17) 0.0657(19) 0.0623(17) 0.0165(16) -0.0047(14) -0.0105(15) C15 0.070(2) 0.086(2) 0.066(2) 0.0262(18) -0.0127(17) -0.0065(19) C16 0.088(3) 0.079(2) 0.0578(19) 0.0194(16) 0.0103(19) -0.0129(19) C17 0.102(3) 0.126(3) 0.063(2) 0.025(2) 0.001(2) -0.069(2) C18 0.078(2) 0.122(3) 0.0487(17) 0.0164(18) -0.0110(16) -0.055(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C1 1.798(3) . ? Rh1 N1 2.1231(18) . ? Rh1 P1 2.2149(7) . ? Rh1 Cl1 2.3932(7) . ? P1 C6 1.813(2) . ? P1 C7 1.819(2) . ? P1 C13 1.821(2) . ? O1 C1 1.146(3) . ? N1 C2 1.337(2) . ? N1 N2 1.359(2) . ? N2 C4 1.340(3) . ? N2 C5 1.460(3) . ? C2 C3 1.375(3) . ? C2 H2 0.9300 . ? C3 C4 1.359(3) . ? C3 H3 0.9300 . ? C4 H4 0.9300 . ? C5 C6 1.519(3) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.379(3) . ? C7 C12 1.380(3) . ? C8 C9 1.388(3) . ? C8 H8 0.9300 . ? C9 C10 1.356(4) . ? C9 H9 0.9300 . ? C10 C11 1.360(4) . ? C10 H10 0.9300 . ? C11 C12 1.380(3) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.369(3) . ? C13 C18 1.370(3) . ? C14 C15 1.376(3) . ? C14 H14 0.9300 . ? C15 C16 1.364(4) . ? C15 H15 0.9300 . ? C16 C17 1.347(4) . ? C16 H16 0.9300 . ? C17 C18 1.381(4) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? 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 174.93(10) . . ? C1 Rh1 P1 88.59(8) . . ? N1 Rh1 P1 92.93(5) . . ? C1 Rh1 Cl1 88.86(8) . . ? N1 Rh1 Cl1 89.76(5) . . ? P1 Rh1 Cl1 176.96(2) . . ? C6 P1 C7 103.72(11) . . ? C6 P1 C13 103.33(11) . . ? C7 P1 C13 104.87(10) . . ? C6 P1 Rh1 111.08(8) . . ? C7 P1 Rh1 116.17(8) . . ? C13 P1 Rh1 116.20(8) . . ? C2 N1 N2 104.56(18) . . ? C2 N1 Rh1 125.92(16) . . ? N2 N1 Rh1 129.38(14) . . ? C4 N2 N1 110.7(2) . . ? C4 N2 C5 126.1(2) . . ? N1 N2 C5 123.20(19) . . ? O1 C1 Rh1 177.4(3) . . ? N1 C2 C3 111.6(2) . . ? N1 C2 H2 124.2 . . ? C3 C2 H2 124.2 . . ? C4 C3 C2 105.0(2) . . ? C4 C3 H3 127.5 . . ? C2 C3 H3 127.5 . . ? N2 C4 C3 108.2(2) . . ? N2 C4 H4 125.9 . . ? C3 C4 H4 125.9 . . ? N2 C5 C6 112.4(2) . . ? N2 C5 H5A 109.1 . . ? C6 C5 H5A 109.1 . . ? N2 C5 H5B 109.1 . . ? C6 C5 H5B 109.1 . . ? H5A C5 H5B 107.9 . . ? C5 C6 P1 111.23(16) . . ? C5 C6 H6A 109.4 . . ? P1 C6 H6A 109.4 . . ? C5 C6 H6B 109.4 . . ? P1 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? C8 C7 C12 117.9(2) . . ? C8 C7 P1 119.99(18) . . ? C12 C7 P1 122.07(19) . . ? C7 C8 C9 120.4(3) . . ? C7 C8 H8 119.8 . . ? C9 C8 H8 119.8 . . ? C10 C9 C8 120.7(3) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C9 C10 C11 119.5(3) . . ? C9 C10 H10 120.3 . . ? C11 C10 H10 120.3 . . ? C10 C11 C12 120.6(3) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C11 C12 C7 120.8(3) . . ? C11 C12 H12 119.6 . . ? C7 C12 H12 119.6 . . ? C14 C13 C18 117.2(2) . . ? C14 C13 P1 124.02(19) . . ? C18 C13 P1 118.8(2) . . ? C13 C14 C15 121.4(3) . . ? C13 C14 H14 119.3 . . ? C15 C14 H14 119.3 . . ? C16 C15 C14 120.2(3) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C17 C16 C15 119.5(3) . . ? C17 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? C16 C17 C18 120.1(3) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C13 C18 C17 121.6(3) . . ? C13 C18 H18 119.2 . . ? C17 C18 H18 119.2 . . ? 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 -166.51(12) . . . . ? N1 Rh1 P1 C6 8.65(10) . . . . ? Cl1 Rh1 P1 C6 160.7(4) . . . . ? C1 Rh1 P1 C7 75.29(12) . . . . ? N1 Rh1 P1 C7 -109.55(10) . . . . ? Cl1 Rh1 P1 C7 42.5(5) . . . . ? C1 Rh1 P1 C13 -48.79(12) . . . . ? N1 Rh1 P1 C13 126.36(10) . . . . ? Cl1 Rh1 P1 C13 -81.6(5) . . . . ? C1 Rh1 N1 C2 -53.6(10) . . . . ? P1 Rh1 N1 C2 -160.89(17) . . . . ? Cl1 Rh1 N1 C2 20.54(17) . . . . ? C1 Rh1 N1 N2 121.4(10) . . . . ? P1 Rh1 N1 N2 14.15(17) . . . . ? Cl1 Rh1 N1 N2 -164.42(17) . . . . ? C2 N1 N2 C4 -0.9(2) . . . . ? Rh1 N1 N2 C4 -176.72(16) . . . . ? C2 N1 N2 C5 -179.8(2) . . . . ? Rh1 N1 N2 C5 4.4(3) . . . . ? N1 Rh1 C1 O1 -2(6) . . . . ? P1 Rh1 C1 O1 105(5) . . . . ? Cl1 Rh1 C1 O1 -76(5) . . . . ? N2 N1 C2 C3 0.7(2) . . . . ? Rh1 N1 C2 C3 176.72(15) . . . . ? N1 C2 C3 C4 -0.3(3) . . . . ? N1 N2 C4 C3 0.7(3) . . . . ? C5 N2 C4 C3 179.6(2) . . . . ? C2 C3 C4 N2 -0.3(3) . . . . ? C4 N2 C5 C6 127.4(3) . . . . ? N1 N2 C5 C6 -53.9(3) . . . . ? N2 C5 C6 P1 76.8(2) . . . . ? C7 P1 C6 C5 75.78(18) . . . . ? C13 P1 C6 C5 -174.99(17) . . . . ? Rh1 P1 C6 C5 -49.72(18) . . . . ? C6 P1 C7 C8 -142.2(2) . . . . ? C13 P1 C7 C8 109.7(2) . . . . ? Rh1 P1 C7 C8 -20.0(2) . . . . ? C6 P1 C7 C12 37.3(2) . . . . ? C13 P1 C7 C12 -70.8(2) . . . . ? Rh1 P1 C7 C12 159.50(18) . . . . ? C12 C7 C8 C9 1.0(4) . . . . ? P1 C7 C8 C9 -179.5(2) . . . . ? C7 C8 C9 C10 -0.1(5) . . . . ? C8 C9 C10 C11 -0.9(5) . . . . ? C9 C10 C11 C12 1.0(5) . . . . ? C10 C11 C12 C7 -0.1(5) . . . . ? C8 C7 C12 C11 -0.9(4) . . . . ? P1 C7 C12 C11 179.6(2) . . . . ? C6 P1 C13 C14 -104.3(2) . . . . ? C7 P1 C13 C14 4.1(2) . . . . ? Rh1 P1 C13 C14 133.8(2) . . . . ? C6 P1 C13 C18 75.4(2) . . . . ? C7 P1 C13 C18 -176.2(2) . . . . ? Rh1 P1 C13 C18 -46.5(2) . . . . ? C18 C13 C14 C15 -1.3(4) . . . . ? P1 C13 C14 C15 178.4(2) . . . . ? C13 C14 C15 C16 1.2(5) . . . . ? C14 C15 C16 C17 -1.0(5) . . . . ? C15 C16 C17 C18 0.9(5) . . . . ? C14 C13 C18 C17 1.2(5) . . . . ? P1 C13 C18 C17 -178.5(3) . . . . ? C16 C17 C18 C13 -1.1(6) . . . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.535 _refine_diff_density_min -0.394 _refine_diff_density_rms 0.062