# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Richard Jones' _publ_contact_author_email rajones@mail.utexas.edu _publ_section_title ; Synthesis and Structures of the Homoleptic Cations [M(PMe3)5]+ (M = Rh, Ir) ; loop_ _publ_author_name 'Richard Jones' 'Joseph Rivers' # Attachment '- Compound 1.CIF' data_RhP4B _database_code_depnum_ccdc_archive 'CCDC 772623' #TrackingRef '- Compound 1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; tetrakis(trimethylphosphine)rhodium(I) tetra(pentafluorophenyl)borate ; _chemical_name_common ;tetrakis(trimethylphosphine)rhodium(i) tetra(pentafluorophenyl)borate ; _chemical_melting_point 182 _chemical_formula_moiety 'C12 H36 P4 Rh, C24 B F20' _chemical_formula_sum 'C36 H36 B F20 P4 Rh' _chemical_formula_weight 1086.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.1222(9) _cell_length_b 12.6241(9) _cell_length_c 15.8420(11) _cell_angle_alpha 104.7118(17) _cell_angle_beta 109.8361(17) _cell_angle_gamma 98.4962(18) _cell_volume 2131.58(27) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 41317 _cell_measurement_theta_min 6.56 _cell_measurement_theta_max 55.03 _exptl_crystal_description chunk _exptl_crystal_colour orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.692 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1084 _exptl_absorpt_coefficient_mu 0.665 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8138 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ; Abscor. T. Higashi (2001). The Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC-12 with Saturn 724+CCD' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 52101 _diffrn_reflns_av_R_equivalents 0.0376 _diffrn_reflns_av_sigmaI/netI 0.0301 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.28 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9768 _reflns_number_gt 8420 _reflns_threshold_expression >2sigma(I) _publ_section_references ; Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838. An Integrated System of Windows Programs for the Solution, Refinement and Analysis of Single Crystal X-ray Diffraction Data. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'CIFTAB (Sheldrick, 2008)' _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^)+(0.0378P)^2^+5.9335P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9768 _refine_ls_number_parameters 571 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0544 _refine_ls_R_factor_gt 0.0450 _refine_ls_wR_factor_ref 0.1085 _refine_ls_wR_factor_gt 0.1020 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.10235(2) 0.775396(19) 0.214393(17) 0.02103(7) Uani 1 1 d . . . P2 P 0.16610(8) 0.87620(7) 0.13234(6) 0.02809(19) Uani 1 1 d . . . P3 P 0.10746(7) 0.61449(7) 0.25694(6) 0.02396(17) Uani 1 1 d . . . P4 P -0.09627(7) 0.72155(7) 0.11518(6) 0.02328(17) Uani 1 1 d . . . P1 P 0.22685(9) 0.89371(7) 0.36396(6) 0.02995(19) Uani 1 1 d . . . F16 F 0.66239(19) 0.44905(16) 0.12158(14) 0.0332(5) Uani 1 1 d . . . F5 F 0.85782(17) 0.44777(16) 0.41802(14) 0.0317(4) Uani 1 1 d . . . F19 F 0.37029(17) 0.02148(15) -0.05578(13) 0.0285(4) Uani 1 1 d . . . F1 F 0.50098(18) 0.50678(16) 0.21161(14) 0.0317(4) Uani 1 1 d . . . F14 F 0.16571(17) 0.28985(17) 0.21933(14) 0.0319(4) Uani 1 1 d . . . F15 F 0.32878(17) 0.28477(16) 0.14461(13) 0.0270(4) Uani 1 1 d . . . F20 F 0.44996(17) 0.10902(15) 0.13251(13) 0.0255(4) Uani 1 1 d . . . F6 F 0.83110(18) 0.33028(17) 0.23262(15) 0.0345(5) Uani 1 1 d . . . F10 F 0.55984(18) 0.12865(16) 0.32919(14) 0.0301(4) Uani 1 1 d . . . F4 F 0.94432(19) 0.66980(18) 0.50150(15) 0.0405(5) Uani 1 1 d . . . F9 F 0.6919(2) -0.01815(17) 0.34661(14) 0.0426(6) Uani 1 1 d . . . F17 F 0.5776(2) 0.36224(19) -0.06519(15) 0.0416(5) Uani 1 1 d . . . F11 F 0.63624(17) 0.36107(17) 0.45033(13) 0.0291(4) Uani 1 1 d . . . F18 F 0.42743(19) 0.14865(18) -0.15801(13) 0.0339(5) Uani 1 1 d . . . F12 F 0.4684(2) 0.36597(19) 0.52392(14) 0.0385(5) Uani 1 1 d . . . F2 F 0.5890(2) 0.73024(18) 0.30002(17) 0.0470(6) Uani 1 1 d . . . F13 F 0.2298(2) 0.3309(2) 0.40925(16) 0.0409(5) Uani 1 1 d . . . F8 F 0.8981(3) 0.0047(2) 0.31115(18) 0.0560(7) Uani 1 1 d . . . F7 F 0.9652(2) 0.1809(2) 0.25334(19) 0.0526(6) Uani 1 1 d . . . F3 F 0.8139(2) 0.81467(17) 0.44431(17) 0.0494(6) Uani 1 1 d . . . C32 C 0.5873(3) 0.3432(3) 0.0827(2) 0.0253(6) Uani 1 1 d . . . C25 C 0.4928(3) 0.3197(2) 0.2929(2) 0.0212(6) Uani 1 1 d . . . C34 C 0.4714(3) 0.1913(3) -0.0630(2) 0.0253(6) Uani 1 1 d . . . C36 C 0.4848(3) 0.1754(2) 0.0861(2) 0.0207(6) Uani 1 1 d . . . C29 C 0.2825(3) 0.3065(3) 0.2767(2) 0.0250(6) Uani 1 1 d . . . C24 C 0.6615(3) 0.1492(3) 0.3112(2) 0.0265(7) Uani 1 1 d . . . C19 C 0.6906(3) 0.2414(3) 0.2832(2) 0.0231(6) Uani 1 1 d . . . C28 C 0.3147(3) 0.3276(3) 0.3727(2) 0.0285(7) Uani 1 1 d . . . C20 C 0.7955(3) 0.2466(3) 0.2644(2) 0.0281(7) Uani 1 1 d . . . C16 C 0.7693(4) 0.7019(3) 0.3998(3) 0.0349(8) Uani 1 1 d . . . C26 C 0.5196(3) 0.3418(3) 0.3892(2) 0.0238(6) Uani 1 1 d . . . C33 C 0.5457(3) 0.2995(3) -0.0156(2) 0.0270(7) Uani 1 1 d . . . C17 C 0.8353(3) 0.6291(3) 0.4283(2) 0.0312(7) Uani 1 1 d . . . C23 C 0.7285(4) 0.0703(3) 0.3209(2) 0.0323(8) Uani 1 1 d . . . C18 C 0.7880(3) 0.5128(3) 0.3827(2) 0.0265(7) Uani 1 1 d . . . C21 C 0.8656(3) 0.1702(3) 0.2738(3) 0.0364(8) Uani 1 1 d . . . C27 C 0.4350(3) 0.3455(3) 0.4298(2) 0.0273(7) Uani 1 1 d . . . C35 C 0.4427(3) 0.1279(2) -0.0109(2) 0.0226(6) Uani 1 1 d . . . C14 C 0.6132(3) 0.5435(3) 0.2829(2) 0.0265(7) Uani 1 1 d . . . C22 C 0.8317(4) 0.0810(3) 0.3027(3) 0.0384(9) Uani 1 1 d . . . C15 C 0.6565(4) 0.6595(3) 0.3272(3) 0.0333(8) Uani 1 1 d . . . C31 C 0.5574(3) 0.2853(2) 0.1383(2) 0.0212(6) Uani 1 1 d . . . C13 C 0.6758(3) 0.4649(3) 0.3072(2) 0.0231(6) Uani 1 1 d . . . C30 C 0.3707(3) 0.3039(2) 0.2394(2) 0.0226(6) Uani 1 1 d . . . C11 C -0.1860(3) 0.7003(3) 0.1847(3) 0.0323(7) Uani 1 1 d . . . H11A H -0.1610 0.7679 0.2405 0.048 Uiso 1 1 calc R . . H11B H -0.1729 0.6346 0.2053 0.048 Uiso 1 1 calc R . . H11C H -0.2723 0.6869 0.1455 0.048 Uiso 1 1 calc R . . C6 C 0.3285(4) 0.8895(3) 0.1664(4) 0.0467(10) Uani 1 1 d . . . H6A H 0.3448 0.8153 0.1644 0.070 Uiso 1 1 calc R . . H6B H 0.3729 0.9432 0.2308 0.070 Uiso 1 1 calc R . . H6C H 0.3550 0.9170 0.1221 0.070 Uiso 1 1 calc R . . C7 C 0.0009(3) 0.4826(3) 0.1694(3) 0.0309(7) Uani 1 1 d . . . H7A H 0.0238 0.4181 0.1881 0.046 Uiso 1 1 calc R . . H7B H 0.0031 0.4760 0.1070 0.046 Uiso 1 1 calc R . . H7C H -0.0813 0.4828 0.1660 0.046 Uiso 1 1 calc R . . C8 C 0.1016(4) 0.5934(3) 0.3646(3) 0.0405(9) Uani 1 1 d . . . H8A H 0.0234 0.6006 0.3673 0.061 Uiso 1 1 calc R . . H8B H 0.1674 0.6506 0.4200 0.061 Uiso 1 1 calc R . . H8C H 0.1109 0.5176 0.3646 0.061 Uiso 1 1 calc R . . C2 C 0.3625(4) 0.8688(3) 0.4428(3) 0.0401(9) Uani 1 1 d . . . H2A H 0.4241 0.8707 0.4157 0.060 Uiso 1 1 calc R . . H2B H 0.3421 0.7945 0.4500 0.060 Uiso 1 1 calc R . . H2C H 0.3943 0.9279 0.5050 0.060 Uiso 1 1 calc R . . C5 C 0.1545(4) 1.0189(3) 0.1329(3) 0.0382(8) Uani 1 1 d . . . H5A H 0.1935 1.0424 0.0933 0.057 Uiso 1 1 calc R . . H5B H 0.1949 1.0716 0.1981 0.057 Uiso 1 1 calc R . . H5C H 0.0687 1.0193 0.1077 0.057 Uiso 1 1 calc R . . C4 C 0.1109(4) 0.8010(3) 0.0054(3) 0.0454(10) Uani 1 1 d . . . H4A H 0.0232 0.7919 -0.0240 0.068 Uiso 1 1 calc R . . H4B H 0.1276 0.7262 -0.0045 0.068 Uiso 1 1 calc R . . H4C H 0.1520 0.8445 -0.0234 0.068 Uiso 1 1 calc R . . C1 C 0.1294(4) 0.9002(3) 0.4310(3) 0.0387(8) Uani 1 1 d . . . H1A H 0.1105 0.8275 0.4412 0.058 Uiso 1 1 calc R . . H1B H 0.0539 0.9162 0.3951 0.058 Uiso 1 1 calc R . . H1C H 0.1716 0.9605 0.4925 0.058 Uiso 1 1 calc R . . C10 C -0.1757(3) 0.6013(3) 0.0046(3) 0.0336(8) Uani 1 1 d . . . H10A H -0.2622 0.5989 -0.0209 0.050 Uiso 1 1 calc R . . H10B H -0.1659 0.5306 0.0176 0.050 Uiso 1 1 calc R . . H10C H -0.1415 0.6101 -0.0418 0.050 Uiso 1 1 calc R . . C12 C -0.1492(3) 0.8357(3) 0.0760(3) 0.0344(8) Uani 1 1 d . . . H12A H -0.2380 0.8137 0.0453 0.052 Uiso 1 1 calc R . . H12B H -0.1154 0.8500 0.0306 0.052 Uiso 1 1 calc R . . H12C H -0.1226 0.9046 0.1309 0.052 Uiso 1 1 calc R . . C9 C 0.2523(3) 0.5867(3) 0.2597(3) 0.0404(9) Uani 1 1 d . . . H9A H 0.3191 0.6478 0.3108 0.061 Uiso 1 1 calc R . . H9B H 0.2578 0.5829 0.1988 0.061 Uiso 1 1 calc R . . H9C H 0.2575 0.5144 0.2710 0.061 Uiso 1 1 calc R . . B1 B 0.6053(3) 0.3286(3) 0.2560(2) 0.0212(7) Uani 1 1 d . . . C3 C 0.2815(4) 1.0447(3) 0.3829(3) 0.0448(10) Uani 1 1 d . . . H3A H 0.3220 1.0860 0.4512 0.067 Uiso 1 1 calc R . . H3B H 0.2126 1.0745 0.3550 0.067 Uiso 1 1 calc R . . H3C H 0.3390 1.0543 0.3528 0.067 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 0.02253(12) 0.01545(11) 0.01842(12) 0.00466(9) 0.00273(9) 0.00005(8) P2 0.0319(4) 0.0190(4) 0.0326(5) 0.0084(3) 0.0143(4) 0.0006(3) P3 0.0238(4) 0.0197(4) 0.0278(4) 0.0104(3) 0.0082(3) 0.0039(3) P4 0.0198(4) 0.0228(4) 0.0258(4) 0.0097(3) 0.0064(3) 0.0045(3) P1 0.0358(5) 0.0205(4) 0.0237(4) 0.0039(3) 0.0044(4) 0.0028(3) F16 0.0445(12) 0.0224(9) 0.0254(10) 0.0066(8) 0.0126(9) -0.0078(8) F5 0.0261(10) 0.0282(10) 0.0300(10) 0.0044(8) 0.0040(8) 0.0014(8) F19 0.0267(9) 0.0187(9) 0.0284(10) 0.0004(7) 0.0043(8) 0.0009(7) F1 0.0377(11) 0.0253(10) 0.0294(10) 0.0126(8) 0.0068(9) 0.0092(8) F14 0.0238(9) 0.0337(11) 0.0363(11) 0.0111(9) 0.0089(8) 0.0103(8) F15 0.0262(9) 0.0334(10) 0.0197(9) 0.0107(8) 0.0052(7) 0.0086(8) F20 0.0278(9) 0.0196(9) 0.0252(9) 0.0097(7) 0.0071(8) -0.0009(7) F6 0.0304(10) 0.0321(11) 0.0415(12) 0.0119(9) 0.0172(9) 0.0021(8) F10 0.0358(11) 0.0227(9) 0.0285(10) 0.0116(8) 0.0096(8) 0.0002(8) F4 0.0348(11) 0.0336(11) 0.0327(11) -0.0063(9) 0.0086(9) -0.0083(9) F9 0.0694(16) 0.0200(10) 0.0268(11) 0.0098(8) 0.0040(10) 0.0105(10) F17 0.0575(14) 0.0377(12) 0.0273(11) 0.0135(9) 0.0188(10) -0.0045(10) F11 0.0256(9) 0.0341(10) 0.0199(9) 0.0092(8) 0.0024(8) 0.0007(8) F18 0.0381(11) 0.0377(11) 0.0175(9) 0.0032(8) 0.0076(8) 0.0038(9) F12 0.0449(12) 0.0477(13) 0.0200(10) 0.0076(9) 0.0142(9) 0.0061(10) F2 0.0723(17) 0.0238(10) 0.0457(13) 0.0152(10) 0.0195(12) 0.0170(11) F13 0.0404(12) 0.0497(13) 0.0397(12) 0.0112(10) 0.0260(10) 0.0130(10) F8 0.0663(17) 0.0460(14) 0.0503(15) 0.0107(12) 0.0100(13) 0.0386(13) F7 0.0342(12) 0.0616(16) 0.0615(16) 0.0121(13) 0.0205(12) 0.0211(12) F3 0.0725(17) 0.0158(10) 0.0476(14) -0.0030(9) 0.0251(13) -0.0043(10) C32 0.0274(16) 0.0185(14) 0.0243(16) 0.0065(12) 0.0072(13) -0.0025(12) C25 0.0249(15) 0.0171(13) 0.0202(14) 0.0084(11) 0.0063(12) 0.0031(11) C34 0.0249(15) 0.0297(16) 0.0179(14) 0.0052(12) 0.0066(12) 0.0065(13) C36 0.0209(14) 0.0183(14) 0.0236(15) 0.0100(12) 0.0076(12) 0.0046(11) C29 0.0242(15) 0.0196(14) 0.0281(16) 0.0056(12) 0.0088(13) 0.0042(12) C24 0.0306(17) 0.0215(15) 0.0198(15) 0.0054(12) 0.0039(13) 0.0017(13) C19 0.0265(15) 0.0184(14) 0.0178(14) 0.0032(11) 0.0048(12) 0.0017(12) C28 0.0324(17) 0.0251(16) 0.0328(18) 0.0087(14) 0.0189(15) 0.0076(13) C20 0.0271(16) 0.0233(15) 0.0274(17) 0.0059(13) 0.0062(13) 0.0030(13) C16 0.052(2) 0.0172(15) 0.0327(19) 0.0007(13) 0.0226(17) -0.0008(15) C26 0.0243(15) 0.0219(14) 0.0215(15) 0.0079(12) 0.0065(12) 0.0004(12) C33 0.0313(17) 0.0270(16) 0.0244(16) 0.0105(13) 0.0137(14) 0.0020(13) C17 0.0326(18) 0.0265(16) 0.0246(16) 0.0003(13) 0.0105(14) -0.0047(14) C23 0.047(2) 0.0202(15) 0.0198(16) 0.0055(13) 0.0022(15) 0.0093(14) C18 0.0287(16) 0.0224(15) 0.0259(16) 0.0061(13) 0.0114(13) 0.0010(13) C21 0.0275(17) 0.039(2) 0.0320(19) 0.0009(15) 0.0066(15) 0.0089(15) C27 0.0350(18) 0.0228(15) 0.0224(15) 0.0056(13) 0.0121(14) 0.0038(13) C35 0.0195(14) 0.0183(14) 0.0247(15) 0.0038(12) 0.0051(12) 0.0042(11) C14 0.0344(17) 0.0211(15) 0.0219(15) 0.0063(12) 0.0115(14) 0.0014(13) C22 0.046(2) 0.0293(18) 0.0290(18) 0.0034(15) 0.0024(16) 0.0202(16) C15 0.055(2) 0.0199(15) 0.0330(18) 0.0125(14) 0.0241(17) 0.0085(15) C31 0.0220(14) 0.0185(14) 0.0212(15) 0.0061(12) 0.0070(12) 0.0035(11) C13 0.0280(16) 0.0185(14) 0.0208(15) 0.0054(12) 0.0102(13) 0.0007(12) C30 0.0274(15) 0.0174(13) 0.0213(15) 0.0071(12) 0.0079(12) 0.0039(12) C11 0.0285(17) 0.0294(17) 0.041(2) 0.0125(15) 0.0161(15) 0.0059(14) C6 0.038(2) 0.034(2) 0.069(3) 0.018(2) 0.024(2) 0.0045(17) C7 0.0280(16) 0.0189(15) 0.041(2) 0.0092(14) 0.0096(15) 0.0036(13) C8 0.046(2) 0.039(2) 0.037(2) 0.0173(17) 0.0151(18) 0.0069(17) C2 0.038(2) 0.036(2) 0.0297(19) 0.0086(16) 0.0000(16) -0.0012(16) C5 0.050(2) 0.0239(17) 0.040(2) 0.0146(15) 0.0161(18) 0.0048(16) C4 0.063(3) 0.037(2) 0.035(2) 0.0041(17) 0.028(2) -0.0009(19) C1 0.047(2) 0.0359(19) 0.0259(18) 0.0031(15) 0.0110(16) 0.0105(17) C10 0.0296(17) 0.0289(17) 0.0305(18) 0.0055(14) 0.0039(14) -0.0002(14) C12 0.0296(17) 0.0324(18) 0.041(2) 0.0162(16) 0.0088(15) 0.0114(15) C9 0.0283(18) 0.0253(17) 0.061(3) 0.0064(17) 0.0147(18) 0.0081(14) B1 0.0224(16) 0.0204(16) 0.0183(16) 0.0076(13) 0.0057(13) 0.0014(13) C3 0.057(3) 0.0209(17) 0.037(2) 0.0027(15) 0.0040(19) 0.0021(16) _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 P4 2.2660(12) . ? Rh1 P2 2.2666(10) . ? Rh1 P1 2.2874(10) . ? Rh1 P3 2.2997(11) . ? P2 C4 1.822(4) . ? P2 C6 1.825(4) . ? P2 C5 1.825(4) . ? P3 C8 1.814(4) . ? P3 C9 1.829(4) . ? P3 C7 1.828(3) . ? P4 C12 1.825(4) . ? P4 C11 1.829(4) . ? P4 C10 1.837(4) . ? P1 C2 1.822(4) . ? P1 C3 1.834(4) . ? P1 C1 1.835(4) . ? F16 C32 1.354(3) . ? F5 C18 1.350(4) . ? F19 C35 1.351(3) . ? F1 C14 1.359(4) . ? F14 C29 1.347(4) . ? F15 C30 1.355(4) . ? F20 C36 1.356(3) . ? F6 C20 1.357(4) . ? F10 C24 1.360(4) . ? F4 C17 1.346(4) . ? F9 C23 1.348(4) . ? F17 C33 1.351(4) . ? F11 C26 1.358(4) . ? F18 C34 1.341(4) . ? F12 C27 1.347(4) . ? F2 C15 1.350(4) . ? F13 C28 1.342(4) . ? F8 C22 1.347(4) . ? F7 C21 1.349(4) . ? F3 C16 1.350(4) . ? C32 C31 1.382(4) . ? C32 C33 1.391(5) . ? C25 C30 1.386(4) . ? C25 C26 1.391(4) . ? C25 B1 1.656(5) . ? C34 C35 1.375(5) . ? C34 C33 1.378(5) . ? C36 C35 1.376(4) . ? C36 C31 1.395(4) . ? C29 C28 1.378(5) . ? C29 C30 1.387(4) . ? C24 C23 1.380(5) . ? C24 C19 1.388(4) . ? C19 C20 1.396(5) . ? C19 B1 1.657(5) . ? C28 C27 1.378(5) . ? C20 C21 1.380(5) . ? C16 C17 1.368(5) . ? C16 C15 1.372(6) . ? C26 C27 1.384(5) . ? C17 C18 1.391(4) . ? C23 C22 1.371(6) . ? C18 C13 1.390(5) . ? C21 C22 1.378(6) . ? C14 C15 1.383(4) . ? C14 C13 1.388(5) . ? C31 B1 1.663(4) . ? C13 B1 1.653(4) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P4 Rh1 P2 95.79(4) . . ? P4 Rh1 P1 139.55(4) . . ? P2 Rh1 P1 97.71(4) . . ? P4 Rh1 P3 97.22(3) . . ? P2 Rh1 P3 144.26(3) . . ? P1 Rh1 P3 93.62(4) . . ? C4 P2 C6 100.2(2) . . ? C4 P2 C5 101.2(2) . . ? C6 P2 C5 102.45(19) . . ? C4 P2 Rh1 114.16(14) . . ? C6 P2 Rh1 107.64(15) . . ? C5 P2 Rh1 127.50(14) . . ? C8 P3 C9 103.1(2) . . ? C8 P3 C7 99.67(18) . . ? C9 P3 C7 100.99(17) . . ? C8 P3 Rh1 128.08(14) . . ? C9 P3 Rh1 104.62(13) . . ? C7 P3 Rh1 116.71(12) . . ? C12 P4 C11 100.38(17) . . ? C12 P4 C10 100.38(18) . . ? C11 P4 C10 102.66(17) . . ? C12 P4 Rh1 112.88(12) . . ? C11 P4 Rh1 107.83(13) . . ? C10 P4 Rh1 128.91(13) . . ? C2 P1 C3 100.26(19) . . ? C2 P1 C1 103.00(19) . . ? C3 P1 C1 100.6(2) . . ? C2 P1 Rh1 125.69(14) . . ? C3 P1 Rh1 119.10(14) . . ? C1 P1 Rh1 104.52(13) . . ? F16 C32 C31 121.4(3) . . ? F16 C32 C33 114.5(3) . . ? C31 C32 C33 124.1(3) . . ? C30 C25 C26 113.3(3) . . ? C30 C25 B1 127.2(3) . . ? C26 C25 B1 119.2(3) . . ? F18 C34 C35 120.6(3) . . ? F18 C34 C33 120.8(3) . . ? C35 C34 C33 118.7(3) . . ? F20 C36 C35 116.1(3) . . ? F20 C36 C31 118.9(3) . . ? C35 C36 C31 124.9(3) . . ? F14 C29 C28 120.0(3) . . ? F14 C29 C30 120.1(3) . . ? C28 C29 C30 119.8(3) . . ? F10 C24 C23 114.6(3) . . ? F10 C24 C19 121.0(3) . . ? C23 C24 C19 124.4(3) . . ? C24 C19 C20 113.0(3) . . ? C24 C19 B1 126.8(3) . . ? C20 C19 B1 119.6(3) . . ? F13 C28 C27 121.1(3) . . ? F13 C28 C29 120.1(3) . . ? C27 C28 C29 118.8(3) . . ? F6 C20 C21 116.6(3) . . ? F6 C20 C19 118.8(3) . . ? C21 C20 C19 124.6(3) . . ? F3 C16 C17 120.1(3) . . ? F3 C16 C15 120.2(3) . . ? C17 C16 C15 119.7(3) . . ? F11 C26 C27 115.6(3) . . ? F11 C26 C25 119.6(3) . . ? C27 C26 C25 124.8(3) . . ? F17 C33 C34 119.7(3) . . ? F17 C33 C32 120.6(3) . . ? C34 C33 C32 119.8(3) . . ? F4 C17 C16 120.0(3) . . ? F4 C17 C18 120.3(3) . . ? C16 C17 C18 119.7(3) . . ? F9 C23 C22 119.8(3) . . ? F9 C23 C24 120.4(3) . . ? C22 C23 C24 119.8(3) . . ? F5 C18 C13 121.3(3) . . ? F5 C18 C17 115.4(3) . . ? C13 C18 C17 123.4(3) . . ? F7 C21 C22 120.0(3) . . ? F7 C21 C20 120.7(4) . . ? C22 C21 C20 119.2(3) . . ? F12 C27 C28 119.8(3) . . ? F12 C27 C26 121.0(3) . . ? C28 C27 C26 119.2(3) . . ? F19 C35 C34 119.7(3) . . ? F19 C35 C36 120.9(3) . . ? C34 C35 C36 119.4(3) . . ? F1 C14 C15 116.1(3) . . ? F1 C14 C13 119.3(3) . . ? C15 C14 C13 124.5(3) . . ? F8 C22 C23 120.8(4) . . ? F8 C22 C21 120.2(4) . . ? C23 C22 C21 119.0(3) . . ? F2 C15 C16 120.3(3) . . ? F2 C15 C14 120.8(3) . . ? C16 C15 C14 118.9(3) . . ? C32 C31 C36 113.0(3) . . ? C32 C31 B1 127.6(3) . . ? C36 C31 B1 119.2(3) . . ? C14 C13 C18 113.8(3) . . ? C14 C13 B1 118.6(3) . . ? C18 C13 B1 127.0(3) . . ? F15 C30 C25 121.3(3) . . ? F15 C30 C29 114.6(3) . . ? C25 C30 C29 124.1(3) . . ? P4 C11 H11A 109.5 . . ? P4 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? P4 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? P2 C6 H6A 109.5 . . ? P2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? P2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? P3 C7 H7A 109.5 . . ? P3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? P3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? P3 C8 H8A 109.5 . . ? P3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? P3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? P1 C2 H2A 109.5 . . ? P1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? P1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? P2 C5 H5A 109.5 . . ? P2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? P2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? P2 C4 H4A 109.5 . . ? P2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? P2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? P1 C1 H1A 109.5 . . ? P1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? P1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? P4 C10 H10A 109.5 . . ? P4 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? P4 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? P4 C12 H12A 109.5 . . ? P4 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? P4 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? P3 C9 H9A 109.5 . . ? P3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? P3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C13 B1 C25 101.6(2) . . ? C13 B1 C19 114.9(3) . . ? C25 B1 C19 113.0(2) . . ? C13 B1 C31 113.7(2) . . ? C25 B1 C31 113.0(2) . . ? C19 B1 C31 101.1(2) . . ? P1 C3 H3A 109.5 . . ? P1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? P1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.633 _refine_diff_density_min -1.310 _refine_diff_density_rms 0.096 # Attachment '- Compound 2.CIF' data_RhP5B _database_code_depnum_ccdc_archive 'CCDC 772624' #TrackingRef '- Compound 2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; pentakis(trimethylphosphine)rhodium(I) tetra(pentafluorophenyl)borate ; _chemical_name_common ;pentakis(trimethylphosphine)rhodium(i) tetra(pentafluorophenyl)borate ; _chemical_melting_point ? _chemical_formula_moiety 'C15 H45 P5 Rh, C24 B F20' _chemical_formula_sum 'C39 H45 B F20 P5 Rh' _chemical_formula_weight 1162.32 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' F F 0.0171 0.0103 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.7999(8) _cell_length_b 13.4422(8) _cell_length_c 15.4812(9) _cell_angle_alpha 111.8790(10) _cell_angle_beta 99.044(2) _cell_angle_gamma 103.507(2) _cell_volume 2313.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 32533 _cell_measurement_theta_min 6.12 _cell_measurement_theta_max 55.10 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.087 _exptl_crystal_size_mid 0.075 _exptl_crystal_size_min 0.072 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.668 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1168 _exptl_absorpt_coefficient_mu 0.653 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.889 _exptl_absorpt_correction_T_max 0.968 _exptl_absorpt_process_details ; Abscor. T. Higashi (2001). The Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC-12 with Saturn 724+CCD' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47554 _diffrn_reflns_av_R_equivalents 0.0760 _diffrn_reflns_av_sigmaI/netI 0.0751 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 27.48 _reflns_number_total 10580 _reflns_number_gt 7709 _reflns_threshold_expression >2sigma(I) _publ_section_references ; Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838. An Integrated System of Windows Programs for the Solution, Refinement and Analysis of Single Crystal X-ray Diffraction Data. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _publ_section_acknowledgements ; The data were collected using instrumentation purchased with funds provided by the National Science Foundation Grant No. 0741973. ; _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'CIFTAB (Sheldrick, 2008)' _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^)+(0.0391P)^2^+9.8117P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10580 _refine_ls_number_parameters 610 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0937 _refine_ls_R_factor_gt 0.0609 _refine_ls_wR_factor_ref 0.1358 _refine_ls_wR_factor_gt 0.1209 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.78132(3) 0.12224(3) 0.19099(2) 0.01578(10) Uani 1 1 d . . . P1 P 0.97523(11) 0.16437(12) 0.26383(10) 0.0309(3) Uani 1 1 d . . . P2 P 0.75543(11) -0.07032(10) 0.12239(9) 0.0258(3) Uani 1 1 d . . . P3 P 0.79697(11) 0.31343(10) 0.25500(9) 0.0230(3) Uani 1 1 d . . . P4 P 0.67073(11) 0.09825(11) 0.29229(9) 0.0268(3) Uani 1 1 d . . . P5 P 0.75250(11) 0.12111(11) 0.03569(9) 0.0261(3) Uani 1 1 d . . . B1 B 0.3588(4) 0.6075(4) 0.2779(4) 0.0180(10) Uani 1 1 d . . . F1 F 0.5542(2) 0.5453(2) 0.24581(19) 0.0263(6) Uani 1 1 d . . . F2 F 0.7680(2) 0.6652(3) 0.3367(2) 0.0379(7) Uani 1 1 d . . . F3 F 0.8248(2) 0.8817(3) 0.4748(2) 0.0398(8) Uani 1 1 d . . . F4 F 0.6605(2) 0.9701(2) 0.5253(2) 0.0330(7) Uani 1 1 d . . . F5 F 0.4483(2) 0.8528(2) 0.43795(18) 0.0246(6) Uani 1 1 d . . . F6 F 0.4943(2) 0.6611(2) 0.14186(19) 0.0266(6) Uani 1 1 d . . . F7 F 0.4263(3) 0.5684(2) -0.04788(19) 0.0332(7) Uani 1 1 d . . . F8 F 0.2170(3) 0.4166(2) -0.14397(19) 0.0395(8) Uani 1 1 d . . . F9 F 0.0803(3) 0.3556(2) -0.0410(2) 0.0362(7) Uani 1 1 d . . . F10 F 0.1509(2) 0.4401(2) 0.15105(19) 0.0265(6) Uani 1 1 d . . . F11 F 0.3734(2) 0.6420(2) 0.47472(17) 0.0225(6) Uani 1 1 d . . . F12 F 0.3749(2) 0.4947(2) 0.55188(19) 0.0294(6) Uani 1 1 d . . . F13 F 0.3642(3) 0.2784(3) 0.4389(2) 0.0372(7) Uani 1 1 d . . . F14 F 0.3480(3) 0.2145(2) 0.2476(2) 0.0341(7) Uani 1 1 d . . . F15 F 0.3430(3) 0.3563(2) 0.16855(18) 0.0287(6) Uani 1 1 d . . . F16 F 0.3450(2) 0.7952(2) 0.23697(19) 0.0258(6) Uani 1 1 d . . . F17 F 0.1941(3) 0.9021(2) 0.2588(2) 0.0343(7) Uani 1 1 d . . . F18 F 0.0262(3) 0.8412(3) 0.3373(2) 0.0392(8) Uani 1 1 d . . . F19 F 0.0148(2) 0.6688(2) 0.3914(2) 0.0313(7) Uani 1 1 d . . . F20 F 0.1601(2) 0.5573(2) 0.36631(19) 0.0236(6) Uani 1 1 d . . . C1 C 1.0257(6) 0.0617(6) 0.2941(6) 0.059(2) Uani 1 1 d . . . H1A H 1.1070 0.0921 0.3206 0.089 Uiso 1 1 calc R . . H1B H 1.0059 -0.0090 0.2357 0.089 Uiso 1 1 calc R . . H1C H 0.9912 0.0471 0.3423 0.089 Uiso 1 1 calc R . . C2 C 1.0707(5) 0.1858(6) 0.1889(5) 0.0562(18) Uani 1 1 d . . . H2A H 1.1467 0.1954 0.2220 0.084 Uiso 1 1 calc R . . H2B H 1.0698 0.2534 0.1788 0.084 Uiso 1 1 calc R . . H2C H 1.0459 0.1197 0.1262 0.084 Uiso 1 1 calc R . . C3 C 1.0531(5) 0.2876(5) 0.3778(4) 0.0390(13) Uani 1 1 d . . . H3A H 1.0190 0.2830 0.4293 0.059 Uiso 1 1 calc R . . H3B H 1.0512 0.3567 0.3709 0.059 Uiso 1 1 calc R . . H3C H 1.1307 0.2889 0.3944 0.059 Uiso 1 1 calc R . . C4 C 0.8384(5) -0.1190(5) 0.0392(4) 0.0395(14) Uani 1 1 d . . . H4A H 0.8197 -0.2013 0.0142 0.059 Uiso 1 1 calc R . . H4B H 0.9179 -0.0833 0.0735 0.059 Uiso 1 1 calc R . . H4C H 0.8221 -0.0984 -0.0147 0.059 Uiso 1 1 calc R . . C5 C 0.7842(5) -0.1402(5) 0.2022(4) 0.0406(14) Uani 1 1 d . . . H5A H 0.7230 -0.2106 0.1814 0.061 Uiso 1 1 calc R . . H5B H 0.7908 -0.0897 0.2690 0.061 Uiso 1 1 calc R . . H5C H 0.8542 -0.1573 0.1985 0.061 Uiso 1 1 calc R . . C6 C 0.6156(5) -0.1662(5) 0.0466(4) 0.0409(14) Uani 1 1 d . . . H6A H 0.5854 -0.1357 0.0035 0.061 Uiso 1 1 calc R . . H6B H 0.5664 -0.1734 0.0880 0.061 Uiso 1 1 calc R . . H6C H 0.6204 -0.2408 0.0080 0.061 Uiso 1 1 calc R . . C7 C 0.9054(5) 0.4026(4) 0.2265(4) 0.0356(13) Uani 1 1 d . . . H7A H 0.8997 0.3668 0.1573 0.053 Uiso 1 1 calc R . . H7B H 0.9791 0.4118 0.2638 0.053 Uiso 1 1 calc R . . H7C H 0.8953 0.4770 0.2432 0.053 Uiso 1 1 calc R . . C8 C 0.8356(5) 0.3976(5) 0.3868(4) 0.0364(13) Uani 1 1 d . . . H8A H 0.8432 0.4767 0.4010 0.055 Uiso 1 1 calc R . . H8B H 0.9067 0.3927 0.4162 0.055 Uiso 1 1 calc R . . H8C H 0.7775 0.3682 0.4134 0.055 Uiso 1 1 calc R . . C9 C 0.6731(5) 0.3513(5) 0.2210(4) 0.0363(13) Uani 1 1 d . . . H9A H 0.6521 0.3918 0.2792 0.054 Uiso 1 1 calc R . . H9B H 0.6112 0.2824 0.1779 0.054 Uiso 1 1 calc R . . H9C H 0.6897 0.3999 0.1876 0.054 Uiso 1 1 calc R . . C10 C 0.5719(5) 0.1762(5) 0.3165(4) 0.0363(13) Uani 1 1 d . . . H10A H 0.5164 0.1547 0.2559 0.054 Uiso 1 1 calc R . . H10B H 0.6119 0.2576 0.3447 0.054 Uiso 1 1 calc R . . H10C H 0.5344 0.1585 0.3619 0.054 Uiso 1 1 calc R . . C11 C 0.5732(5) -0.0384(5) 0.2685(4) 0.0354(12) Uani 1 1 d . . . H11A H 0.5405 -0.0304 0.3229 0.053 Uiso 1 1 calc R . . H11B H 0.6131 -0.0938 0.2606 0.053 Uiso 1 1 calc R . . H11C H 0.5138 -0.0643 0.2092 0.053 Uiso 1 1 calc R . . C12 C 0.7498(5) 0.1363(5) 0.4157(4) 0.0415(14) Uani 1 1 d . . . H12A H 0.7967 0.2158 0.4450 0.062 Uiso 1 1 calc R . . H12B H 0.7971 0.0882 0.4139 0.062 Uiso 1 1 calc R . . H12C H 0.6978 0.1254 0.4541 0.062 Uiso 1 1 calc R . . C13 C 0.7042(5) 0.2262(5) 0.0076(4) 0.0404(14) Uani 1 1 d . . . H13A H 0.7553 0.3021 0.0512 0.061 Uiso 1 1 calc R . . H13B H 0.6291 0.2204 0.0161 0.061 Uiso 1 1 calc R . . H13C H 0.7025 0.2124 -0.0594 0.061 Uiso 1 1 calc R . . C14 C 0.8747(5) 0.1351(6) -0.0127(5) 0.0503(16) Uani 1 1 d . . . H14A H 0.8531 0.1344 -0.0765 0.076 Uiso 1 1 calc R . . H14B H 0.9029 0.0718 -0.0183 0.076 Uiso 1 1 calc R . . H14C H 0.9331 0.2065 0.0311 0.076 Uiso 1 1 calc R . . C15 C 0.6508(6) -0.0005(5) -0.0708(4) 0.0443(15) Uani 1 1 d . . . H15A H 0.5764 -0.0125 -0.0598 0.066 Uiso 1 1 calc R . . H15B H 0.6725 -0.0684 -0.0811 0.066 Uiso 1 1 calc R . . H15C H 0.6495 0.0149 -0.1280 0.066 Uiso 1 1 calc R . . C16 C 0.4890(4) 0.6931(4) 0.3332(3) 0.0194(9) Uani 1 1 d . . . C17 C 0.5771(4) 0.6518(4) 0.3136(3) 0.0206(10) Uani 1 1 d . . . C18 C 0.6881(4) 0.7122(4) 0.3593(3) 0.0257(11) Uani 1 1 d . . . C19 C 0.7167(4) 0.8208(4) 0.4295(3) 0.0267(11) Uani 1 1 d . . . C20 C 0.6344(4) 0.8657(4) 0.4538(3) 0.0240(10) Uani 1 1 d . . . C21 C 0.5229(4) 0.8020(4) 0.4067(3) 0.0201(9) Uani 1 1 d . . . C22 C 0.3280(4) 0.5543(4) 0.1588(3) 0.0181(9) Uani 1 1 d . . . C23 C 0.2223(4) 0.4764(4) 0.1043(3) 0.0221(10) Uani 1 1 d . . . C24 C 0.1841(4) 0.4301(4) 0.0051(3) 0.0253(10) Uani 1 1 d . . . C25 C 0.2524(5) 0.4604(4) -0.0466(3) 0.0269(11) Uani 1 1 d . . . C26 C 0.3570(4) 0.5367(4) 0.0015(3) 0.0247(11) Uani 1 1 d . . . C27 C 0.3918(4) 0.5830(4) 0.1012(3) 0.0220(10) Uani 1 1 d . . . C28 C 0.3533(4) 0.5078(4) 0.3170(3) 0.0187(9) Uani 1 1 d . . . C29 C 0.3648(4) 0.5355(4) 0.4151(3) 0.0193(9) Uani 1 1 d . . . C30 C 0.3674(4) 0.4616(4) 0.4570(3) 0.0218(10) Uani 1 1 d . . . C31 C 0.3626(4) 0.3533(4) 0.4006(4) 0.0251(10) Uani 1 1 d . . . C32 C 0.3551(4) 0.3216(4) 0.3042(3) 0.0247(10) Uani 1 1 d . . . C33 C 0.3500(4) 0.3970(4) 0.2642(3) 0.0207(10) Uani 1 1 d . . . C34 C 0.2638(4) 0.6718(4) 0.3023(3) 0.0179(9) Uani 1 1 d . . . C35 C 0.2639(4) 0.7598(4) 0.2750(3) 0.0207(9) Uani 1 1 d . . . C36 C 0.1866(4) 0.8169(4) 0.2858(3) 0.0250(10) Uani 1 1 d . . . C37 C 0.1014(4) 0.7863(4) 0.3249(3) 0.0250(10) Uani 1 1 d . . . C38 C 0.0956(4) 0.6989(4) 0.3517(3) 0.0233(10) Uani 1 1 d . . . C39 C 0.1750(4) 0.6436(4) 0.3390(3) 0.0197(9) 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 0.01869(18) 0.01508(18) 0.01529(17) 0.00683(14) 0.00606(13) 0.00684(13) P1 0.0243(7) 0.0318(7) 0.0333(7) 0.0121(6) 0.0012(6) 0.0105(6) P2 0.0320(7) 0.0174(6) 0.0312(7) 0.0107(5) 0.0148(6) 0.0092(5) P3 0.0274(7) 0.0184(6) 0.0219(6) 0.0066(5) 0.0052(5) 0.0093(5) P4 0.0291(7) 0.0286(7) 0.0254(7) 0.0121(6) 0.0131(6) 0.0091(6) P5 0.0331(7) 0.0275(7) 0.0194(6) 0.0104(5) 0.0082(5) 0.0114(6) B1 0.024(3) 0.017(2) 0.016(2) 0.008(2) 0.008(2) 0.009(2) F1 0.0320(16) 0.0281(15) 0.0236(14) 0.0099(12) 0.0112(12) 0.0176(13) F2 0.0264(16) 0.057(2) 0.0351(17) 0.0180(16) 0.0136(14) 0.0220(15) F3 0.0261(16) 0.049(2) 0.0364(17) 0.0179(15) 0.0028(14) 0.0021(14) F4 0.0375(17) 0.0187(14) 0.0288(15) 0.0047(12) -0.0025(13) 0.0011(13) F5 0.0286(15) 0.0205(14) 0.0237(14) 0.0063(12) 0.0071(12) 0.0115(12) F6 0.0298(15) 0.0307(15) 0.0237(14) 0.0161(12) 0.0111(12) 0.0074(13) F7 0.0491(19) 0.0377(17) 0.0226(14) 0.0175(13) 0.0177(14) 0.0180(15) F8 0.068(2) 0.0328(17) 0.0120(13) 0.0075(13) 0.0029(14) 0.0146(16) F9 0.0418(19) 0.0265(16) 0.0268(15) 0.0079(13) -0.0048(14) 0.0020(14) F10 0.0279(15) 0.0236(14) 0.0232(14) 0.0095(12) 0.0070(12) 0.0008(12) F11 0.0321(15) 0.0195(14) 0.0158(12) 0.0054(11) 0.0089(11) 0.0099(12) F12 0.0400(17) 0.0418(17) 0.0203(14) 0.0213(13) 0.0150(13) 0.0196(14) F13 0.056(2) 0.0356(17) 0.0420(18) 0.0314(15) 0.0201(16) 0.0243(16) F14 0.053(2) 0.0204(15) 0.0343(16) 0.0113(13) 0.0152(15) 0.0205(14) F15 0.0523(19) 0.0224(14) 0.0153(13) 0.0071(11) 0.0122(13) 0.0186(14) F16 0.0325(16) 0.0249(14) 0.0292(15) 0.0186(12) 0.0132(12) 0.0102(12) F17 0.0465(19) 0.0304(16) 0.0409(17) 0.0239(14) 0.0140(15) 0.0226(14) F18 0.0380(18) 0.0421(18) 0.0502(19) 0.0214(16) 0.0163(15) 0.0298(15) F19 0.0244(15) 0.0372(17) 0.0363(16) 0.0156(14) 0.0146(13) 0.0125(13) F20 0.0236(14) 0.0244(14) 0.0307(15) 0.0182(12) 0.0115(12) 0.0078(11) C1 0.042(4) 0.048(4) 0.078(5) 0.024(4) -0.010(3) 0.019(3) C2 0.033(3) 0.076(5) 0.046(4) 0.017(4) 0.014(3) 0.006(3) C3 0.031(3) 0.039(3) 0.039(3) 0.011(3) 0.007(3) 0.007(3) C4 0.046(4) 0.034(3) 0.045(3) 0.014(3) 0.023(3) 0.022(3) C5 0.050(4) 0.035(3) 0.057(4) 0.030(3) 0.025(3) 0.024(3) C6 0.045(4) 0.026(3) 0.041(3) 0.012(3) 0.012(3) -0.004(3) C7 0.046(3) 0.017(3) 0.037(3) 0.012(2) 0.005(3) 0.002(2) C8 0.042(3) 0.029(3) 0.027(3) 0.001(2) 0.006(2) 0.013(3) C9 0.044(3) 0.033(3) 0.037(3) 0.014(3) 0.010(3) 0.023(3) C10 0.032(3) 0.038(3) 0.030(3) 0.001(2) 0.016(2) 0.012(3) C11 0.034(3) 0.038(3) 0.037(3) 0.019(3) 0.015(2) 0.008(2) C12 0.039(3) 0.054(4) 0.032(3) 0.022(3) 0.011(3) 0.010(3) C13 0.056(4) 0.039(3) 0.031(3) 0.018(3) 0.006(3) 0.022(3) C14 0.051(4) 0.074(5) 0.050(4) 0.039(4) 0.031(3) 0.030(4) C15 0.061(4) 0.036(3) 0.028(3) 0.012(3) 0.004(3) 0.009(3) C16 0.028(2) 0.021(2) 0.016(2) 0.0125(19) 0.0097(19) 0.0096(19) C17 0.029(3) 0.021(2) 0.018(2) 0.0113(19) 0.0114(19) 0.010(2) C18 0.024(3) 0.041(3) 0.022(2) 0.020(2) 0.011(2) 0.015(2) C19 0.022(3) 0.033(3) 0.024(2) 0.016(2) 0.002(2) 0.005(2) C20 0.033(3) 0.020(2) 0.019(2) 0.010(2) 0.005(2) 0.005(2) C21 0.024(2) 0.022(2) 0.022(2) 0.015(2) 0.0075(19) 0.0088(19) C22 0.025(2) 0.017(2) 0.018(2) 0.0089(18) 0.0074(19) 0.0113(19) C23 0.031(3) 0.017(2) 0.022(2) 0.0103(19) 0.008(2) 0.010(2) C24 0.032(3) 0.017(2) 0.023(2) 0.009(2) 0.001(2) 0.006(2) C25 0.047(3) 0.017(2) 0.013(2) 0.0046(19) 0.004(2) 0.012(2) C26 0.044(3) 0.025(3) 0.017(2) 0.014(2) 0.016(2) 0.020(2) C27 0.029(3) 0.018(2) 0.022(2) 0.0099(19) 0.008(2) 0.010(2) C28 0.023(2) 0.019(2) 0.019(2) 0.0108(19) 0.0074(19) 0.0089(19) C29 0.020(2) 0.020(2) 0.021(2) 0.0111(19) 0.0066(19) 0.0071(19) C30 0.025(2) 0.031(3) 0.019(2) 0.015(2) 0.0087(19) 0.014(2) C31 0.032(3) 0.027(3) 0.031(3) 0.022(2) 0.015(2) 0.015(2) C32 0.030(3) 0.017(2) 0.029(3) 0.010(2) 0.008(2) 0.011(2) C33 0.030(3) 0.020(2) 0.016(2) 0.0095(19) 0.0074(19) 0.012(2) C34 0.022(2) 0.018(2) 0.014(2) 0.0079(18) 0.0047(18) 0.0067(18) C35 0.024(2) 0.018(2) 0.019(2) 0.0067(19) 0.0054(19) 0.0056(19) C36 0.033(3) 0.023(3) 0.023(2) 0.012(2) 0.005(2) 0.014(2) C37 0.028(3) 0.023(3) 0.025(2) 0.006(2) 0.007(2) 0.017(2) C38 0.020(2) 0.024(2) 0.022(2) 0.005(2) 0.0073(19) 0.006(2) C39 0.024(2) 0.015(2) 0.019(2) 0.0058(18) 0.0041(19) 0.0053(18) _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 P2 2.3189(13) . ? Rh1 P3 2.3294(13) . ? Rh1 P4 2.3299(13) . ? Rh1 P5 2.3682(13) . ? Rh1 P1 2.3959(14) . ? P1 C1 1.829(6) . ? P1 C3 1.830(6) . ? P1 C2 1.858(6) . ? P2 C4 1.828(5) . ? P2 C6 1.838(6) . ? P2 C5 1.852(5) . ? P3 C9 1.835(5) . ? P3 C7 1.835(5) . ? P3 C8 1.841(5) . ? P4 C10 1.820(5) . ? P4 C11 1.830(5) . ? P4 C12 1.832(6) . ? P5 C13 1.829(5) . ? P5 C14 1.837(6) . ? P5 C15 1.846(6) . ? B1 C22 1.651(6) . ? B1 C28 1.656(6) . ? B1 C16 1.659(7) . ? B1 C34 1.662(7) . ? F1 C17 1.351(5) . ? F2 C18 1.348(5) . ? F3 C19 1.347(6) . ? F4 C20 1.347(5) . ? F5 C21 1.347(5) . ? F6 C27 1.351(5) . ? F7 C26 1.354(5) . ? F8 C25 1.350(5) . ? F9 C24 1.351(6) . ? F10 C23 1.364(5) . ? F11 C29 1.350(5) . ? F12 C30 1.346(5) . ? F13 C31 1.348(5) . ? F14 C32 1.350(5) . ? F15 C33 1.353(5) . ? F16 C35 1.350(5) . ? F17 C36 1.347(5) . ? F18 C37 1.339(5) . ? F19 C38 1.342(5) . ? F20 C39 1.361(5) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C21 1.390(6) . ? C16 C17 1.395(6) . ? C17 C18 1.377(7) . ? C18 C19 1.373(7) . ? C19 C20 1.368(7) . ? C20 C21 1.392(7) . ? C22 C27 1.395(6) . ? C22 C23 1.400(7) . ? C23 C24 1.377(6) . ? C24 C25 1.367(7) . ? C25 C26 1.369(7) . ? C26 C27 1.381(6) . ? C28 C33 1.392(6) . ? C28 C29 1.397(6) . ? C29 C30 1.377(6) . ? C30 C31 1.372(7) . ? C31 C32 1.371(7) . ? C32 C33 1.380(6) . ? C34 C39 1.385(6) . ? C34 C35 1.397(6) . ? C35 C36 1.380(6) . ? C36 C37 1.381(7) . ? C37 C38 1.375(7) . ? C38 C39 1.390(6) . ? 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 P2 Rh1 P3 176.75(5) . . ? P2 Rh1 P4 90.13(5) . . ? P3 Rh1 P4 89.00(5) . . ? P2 Rh1 P5 90.22(5) . . ? P3 Rh1 P5 88.25(5) . . ? P4 Rh1 P5 136.47(5) . . ? P2 Rh1 P1 91.61(5) . . ? P3 Rh1 P1 91.62(5) . . ? P4 Rh1 P1 112.21(5) . . ? P5 Rh1 P1 111.29(5) . . ? C1 P1 C3 96.5(3) . . ? C1 P1 C2 97.1(4) . . ? C3 P1 C2 98.9(3) . . ? C1 P1 Rh1 120.9(2) . . ? C3 P1 Rh1 122.81(19) . . ? C2 P1 Rh1 115.5(2) . . ? C4 P2 C6 99.8(3) . . ? C4 P2 C5 99.8(3) . . ? C6 P2 C5 99.8(3) . . ? C4 P2 Rh1 116.77(19) . . ? C6 P2 Rh1 117.9(2) . . ? C5 P2 Rh1 119.2(2) . . ? C9 P3 C7 103.0(3) . . ? C9 P3 C8 99.2(3) . . ? C7 P3 C8 98.5(3) . . ? C9 P3 Rh1 117.56(19) . . ? C7 P3 Rh1 115.06(18) . . ? C8 P3 Rh1 120.33(19) . . ? C10 P4 C11 95.6(3) . . ? C10 P4 C12 100.7(3) . . ? C11 P4 C12 98.8(3) . . ? C10 P4 Rh1 120.0(2) . . ? C11 P4 Rh1 123.20(18) . . ? C12 P4 Rh1 114.2(2) . . ? C13 P5 C14 96.9(3) . . ? C13 P5 C15 94.1(3) . . ? C14 P5 C15 99.2(3) . . ? C13 P5 Rh1 123.24(19) . . ? C14 P5 Rh1 116.7(2) . . ? C15 P5 Rh1 121.16(19) . . ? C22 B1 C28 111.7(4) . . ? C22 B1 C16 114.1(4) . . ? C28 B1 C16 102.3(3) . . ? C22 B1 C34 102.5(3) . . ? C28 B1 C34 113.4(4) . . ? C16 B1 C34 113.3(4) . . ? P1 C1 H1A 109.5 . . ? P1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? P1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? P1 C2 H2A 109.5 . . ? P1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? P1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? P1 C3 H3A 109.5 . . ? P1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? P1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? P2 C4 H4A 109.5 . . ? P2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? P2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? P2 C5 H5A 109.5 . . ? P2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? P2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? P2 C6 H6A 109.5 . . ? P2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? P2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? P3 C7 H7A 109.5 . . ? P3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? P3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? P3 C8 H8A 109.5 . . ? P3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? P3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? P3 C9 H9A 109.5 . . ? P3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? P3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? P4 C10 H10A 109.5 . . ? P4 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? P4 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? P4 C11 H11A 109.5 . . ? P4 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? P4 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? P4 C12 H12A 109.5 . . ? P4 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? P4 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? P5 C13 H13A 109.5 . . ? P5 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? P5 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? P5 C14 H14A 109.5 . . ? P5 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? P5 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? P5 C15 H15A 109.5 . . ? P5 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? P5 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C21 C16 C17 113.6(4) . . ? C21 C16 B1 126.9(4) . . ? C17 C16 B1 119.2(4) . . ? F1 C17 C18 116.4(4) . . ? F1 C17 C16 119.0(4) . . ? C18 C17 C16 124.5(4) . . ? F2 C18 C19 120.2(4) . . ? F2 C18 C17 120.6(4) . . ? C19 C18 C17 119.2(4) . . ? F3 C19 C20 120.3(4) . . ? F3 C19 C18 120.3(4) . . ? C20 C19 C18 119.4(4) . . ? F4 C20 C19 120.2(4) . . ? F4 C20 C21 119.8(4) . . ? C19 C20 C21 119.9(4) . . ? F5 C21 C16 121.4(4) . . ? F5 C21 C20 115.3(4) . . ? C16 C21 C20 123.3(4) . . ? C27 C22 C23 112.4(4) . . ? C27 C22 B1 128.3(4) . . ? C23 C22 B1 119.2(4) . . ? F10 C23 C24 116.1(4) . . ? F10 C23 C22 118.9(4) . . ? C24 C23 C22 125.0(4) . . ? F9 C24 C25 120.2(4) . . ? F9 C24 C23 120.6(4) . . ? C25 C24 C23 119.2(5) . . ? F8 C25 C24 120.5(5) . . ? F8 C25 C26 120.3(4) . . ? C24 C25 C26 119.2(4) . . ? F7 C26 C25 120.5(4) . . ? F7 C26 C27 119.6(5) . . ? C25 C26 C27 119.9(4) . . ? F6 C27 C26 115.3(4) . . ? F6 C27 C22 120.6(4) . . ? C26 C27 C22 124.2(5) . . ? C33 C28 C29 113.1(4) . . ? C33 C28 B1 127.0(4) . . ? C29 C28 B1 119.5(4) . . ? F11 C29 C30 116.4(4) . . ? F11 C29 C28 118.7(4) . . ? C30 C29 C28 124.9(4) . . ? F12 C30 C31 120.2(4) . . ? F12 C30 C29 120.9(4) . . ? C31 C30 C29 118.9(4) . . ? F13 C31 C32 120.2(4) . . ? F13 C31 C30 120.6(4) . . ? C32 C31 C30 119.1(4) . . ? F14 C32 C31 119.6(4) . . ? F14 C32 C33 119.9(4) . . ? C31 C32 C33 120.4(4) . . ? F15 C33 C32 115.0(4) . . ? F15 C33 C28 121.4(4) . . ? C32 C33 C28 123.5(4) . . ? C39 C34 C35 113.1(4) . . ? C39 C34 B1 128.7(4) . . ? C35 C34 B1 117.9(4) . . ? F16 C35 C36 116.0(4) . . ? F16 C35 C34 119.5(4) . . ? C36 C35 C34 124.5(4) . . ? F17 C36 C35 120.5(4) . . ? F17 C36 C37 120.0(4) . . ? C35 C36 C37 119.5(4) . . ? F18 C37 C38 120.4(4) . . ? F18 C37 C36 120.8(4) . . ? C38 C37 C36 118.9(4) . . ? F19 C38 C37 120.0(4) . . ? F19 C38 C39 120.5(4) . . ? C37 C38 C39 119.5(4) . . ? F20 C39 C34 121.0(4) . . ? F20 C39 C38 114.5(4) . . ? C34 C39 C38 124.5(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.113 _refine_diff_density_min -0.845 _refine_diff_density_rms 0.123 # Attachment '- Compound 3.CIF' data_RhP5Pz _database_code_depnum_ccdc_archive 'CCDC 772625' #TrackingRef '- Compound 3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; pentakis(trimethylphosphine)rhodium(I) bis(3,5-trifluoromethyl)pyrazolate ; _chemical_name_common ;pentakis(trimethylphosphine)rhodium(i) bis(3,5- trifluoromethyl)pyrazolate ; _chemical_melting_point ? _chemical_formula_moiety 'C15 H45 P5 Rh, C5 H F6 N2' _chemical_formula_sum 'C20 H46 F6 N2 P5 Rh' _chemical_formula_weight 686.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4967(11) _cell_length_b 12.0818(14) _cell_length_c 14.6363(17) _cell_angle_alpha 88.422(4) _cell_angle_beta 75.798(3) _cell_angle_gamma 77.305(3) _cell_volume 1587.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 22713 _cell_measurement_theta_min 6.28 _cell_measurement_theta_max 54.92 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.436 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 708 _exptl_absorpt_coefficient_mu 0.837 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.66 _exptl_absorpt_correction_T_max 0.92 _exptl_absorpt_process_details ; Abscor. T. Higashi (2001). The Rigaku Corporation, Tokyo, Japan. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC-12 with Saturn 724+CCD' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27263 _diffrn_reflns_av_R_equivalents 0.0226 _diffrn_reflns_av_sigmaI/netI 0.0191 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 27.46 _reflns_number_total 7227 _reflns_number_gt 6910 _reflns_threshold_expression >2sigma(I) _publ_section_references ; Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838. An Integrated System of Windows Programs for the Solution, Refinement and Analysis of Single Crystal X-ray Diffraction Data. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'CIFTAB (Sheldrick, 2008)' _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^)+(0.0285P)^2^+2.2373P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7227 _refine_ls_number_parameters 486 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0309 _refine_ls_R_factor_gt 0.0294 _refine_ls_wR_factor_ref 0.0714 _refine_ls_wR_factor_gt 0.0703 _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_restrained_S_all 0.985 _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 0.957863(16) 0.800542(14) 0.767415(11) 0.02493(5) Uani 1 1 d . . . N1 N 0.4451(2) 0.28221(15) 0.81556(14) 0.0315(4) Uani 1 1 d . . . F1A F 0.7297(10) 0.3234(8) 0.8540(7) 0.099(4) Uani 0.56 1 d PD A 1 F2A F 0.5371(8) 0.4523(7) 0.9028(4) 0.0508(17) Uani 0.56 1 d PD A 1 F3A F 0.6837(6) 0.4807(4) 0.7769(3) 0.0636(13) Uani 0.56 1 d PD A 1 F1B F 0.6914(12) 0.3149(12) 0.8832(8) 0.063(2) Uani 0.44 1 d PD A 2 F2B F 0.5491(12) 0.4713(9) 0.8907(7) 0.085(4) Uani 0.44 1 d PD A 2 F3B F 0.7508(8) 0.4147(8) 0.7763(4) 0.090(3) Uani 0.44 1 d PD A 2 N2 N 0.3865(2) 0.24594(16) 0.74903(14) 0.0331(4) Uani 1 1 d . . . F4A F 0.4491(14) 0.3369(15) 0.5153(10) 0.080(4) Uani 0.36 1 d PD A 1 F5A F 0.4936(12) 0.1697(9) 0.5302(7) 0.116(5) Uani 0.36 1 d PD A 1 F6A F 0.2639(12) 0.2637(15) 0.5877(10) 0.065(4) Uani 0.36 1 d PD A 1 F5B F 0.4430(6) 0.1482(4) 0.5582(4) 0.0633(13) Uani 0.64 1 d PD A 2 F6B F 0.2604(8) 0.2863(10) 0.5917(7) 0.089(3) Uani 0.64 1 d PD A 2 F4B F 0.4580(10) 0.3160(9) 0.5056(5) 0.083(3) Uani 0.64 1 d PD A 2 C1 C 0.6252(3) 0.3944(2) 0.82672(17) 0.0427(6) Uani 1 1 d D . . C2 C 0.5425(2) 0.3441(2) 0.77184(16) 0.0334(5) Uani 1 1 d . A . C3 C 0.5484(3) 0.3514(2) 0.67624(17) 0.0435(6) Uani 1 1 d . . . H3 H 0.6059 0.3905 0.6295 0.052 Uiso 1 1 calc R A . C4 C 0.4486(2) 0.28674(19) 0.66668(16) 0.0321(5) Uani 1 1 d . A . C5 C 0.4064(3) 0.2608(3) 0.5805(2) 0.0462(6) Uani 1 1 d D . . C9 C 0.7824(3) 0.8389(3) 1.0084(2) 0.0561(8) Uani 1 1 d . . . H9A H 0.7110 0.8174 1.0627 0.084 Uiso 1 1 calc R B . H9B H 0.7490 0.9192 0.9956 0.084 Uiso 1 1 calc R . . H9C H 0.8805 0.8267 1.0222 0.084 Uiso 1 1 calc R . . C10 C 0.5954(2) 0.7595(2) 0.9148(2) 0.0419(6) Uani 1 1 d . . . H10A H 0.5464 0.7457 0.9800 0.063 Uiso 1 1 calc R B . H10B H 0.5852 0.7018 0.8726 0.063 Uiso 1 1 calc R . . H10C H 0.5488 0.8349 0.8970 0.063 Uiso 1 1 calc R . . C11 C 0.8227(2) 0.61126(18) 0.95694(16) 0.0308(4) Uani 1 1 d . . . H11A H 0.9227 0.5907 0.9680 0.046 Uiso 1 1 calc R B . H11B H 0.8117 0.5552 0.9135 0.046 Uiso 1 1 calc R . . H11C H 0.7483 0.6126 1.0169 0.046 Uiso 1 1 calc R . . C12 C 1.1856(3) 0.6670(2) 0.91890(18) 0.0432(6) Uani 1 1 d . . . H12A H 1.2630 0.6006 0.9250 0.065 Uiso 1 1 calc R B . H12B H 1.0937 0.6653 0.9668 0.065 Uiso 1 1 calc R . . H12C H 1.2188 0.7364 0.9278 0.065 Uiso 1 1 calc R . . C13 C 1.1415(3) 0.5152(2) 0.7907(2) 0.0546(8) Uani 1 1 d . . . H13A H 1.1350 0.4987 0.7269 0.082 Uiso 1 1 calc R B . H13B H 1.0533 0.5012 0.8366 0.082 Uiso 1 1 calc R . . H13C H 1.2311 0.4661 0.8034 0.082 Uiso 1 1 calc R . . C14 C 1.3412(3) 0.6600(2) 0.7285(2) 0.0458(6) Uani 1 1 d . . . H14A H 1.4137 0.6229 0.7634 0.069 Uiso 1 1 calc R B . H14B H 1.3537 0.7375 0.7142 0.069 Uiso 1 1 calc R . . H14C H 1.3573 0.6172 0.6696 0.069 Uiso 1 1 calc R . . P1A P 0.97084(18) 0.73593(15) 0.62412(10) 0.0287(3) Uani 0.50 1 d P B 1 C6A C 1.1486(7) 0.6541(6) 0.5517(4) 0.0492(15) Uani 0.50 1 d P B 1 H6A1 H 1.1351 0.6344 0.4904 0.074 Uiso 0.50 1 calc PR B 1 H6A2 H 1.1812 0.5845 0.5839 0.074 Uiso 0.50 1 calc PR B 1 H6A3 H 1.2241 0.6999 0.5424 0.074 Uiso 0.50 1 calc PR B 1 C7A C 0.8507(8) 0.6359(6) 0.6195(4) 0.0410(14) Uani 0.50 1 d P B 1 H7A1 H 0.7476 0.6704 0.6519 0.062 Uiso 0.50 1 calc PR B 1 H7A2 H 0.8848 0.5658 0.6506 0.062 Uiso 0.50 1 calc PR B 1 H7A3 H 0.8559 0.6185 0.5536 0.062 Uiso 0.50 1 calc PR B 1 C8A C 0.9291(8) 0.8321(6) 0.5293(4) 0.0471(14) Uani 0.50 1 d P B 1 H8A1 H 0.9449 0.7876 0.4713 0.071 Uiso 0.50 1 calc PR B 1 H8A2 H 0.9951 0.8857 0.5184 0.071 Uiso 0.50 1 calc PR B 1 H8A3 H 0.8253 0.8742 0.5480 0.071 Uiso 0.50 1 calc PR B 1 P1B P 1.01666(19) 0.68640(15) 0.61710(11) 0.0298(3) Uani 0.50 1 d P B 2 C7B C 0.9042(9) 0.5818(7) 0.6135(5) 0.0508(19) Uani 0.50 1 d P B 2 H7B1 H 0.7984 0.6194 0.6301 0.076 Uiso 0.50 1 calc PR B 2 H7B2 H 0.9234 0.5223 0.6586 0.076 Uiso 0.50 1 calc PR B 2 H7B3 H 0.9308 0.5478 0.5498 0.076 Uiso 0.50 1 calc PR B 2 C6B C 1.2030(7) 0.5980(5) 0.5640(4) 0.0415(13) Uani 0.50 1 d P B 2 H6B1 H 1.2309 0.5401 0.6084 0.062 Uiso 0.50 1 calc PR B 2 H6B2 H 1.2760 0.6460 0.5497 0.062 Uiso 0.50 1 calc PR B 2 H6B3 H 1.2009 0.5610 0.5057 0.062 Uiso 0.50 1 calc PR B 2 C8B C 0.9979(7) 0.7609(7) 0.5078(4) 0.0492(14) Uani 0.50 1 d P B 2 H8B1 H 1.0194 0.7052 0.4560 0.074 Uiso 0.50 1 calc PR B 2 H8B2 H 1.0682 0.8111 0.4929 0.074 Uiso 0.50 1 calc PR B 2 H8B3 H 0.8961 0.8060 0.5165 0.074 Uiso 0.50 1 calc PR B 2 P3 P 1.15085(6) 0.66465(4) 0.80070(4) 0.02699(11) Uani 1 1 d . B . P5A P 0.75331(13) 0.95488(12) 0.75885(11) 0.0288(3) Uani 0.51 1 d P B 1 C18A C 0.7869(5) 1.0683(4) 0.6738(4) 0.0366(10) Uani 0.51 1 d P B 1 H18A H 0.7032 1.1341 0.6897 0.055 Uiso 0.51 1 calc PR B 1 H18B H 0.7964 1.0401 0.6099 0.055 Uiso 0.51 1 calc PR B 1 H18C H 0.8789 1.0906 0.6767 0.055 Uiso 0.51 1 calc PR B 1 C19A C 0.6514(6) 1.0424(5) 0.8655(4) 0.0468(14) Uani 0.51 1 d P B 1 H19A H 0.7213 1.0744 0.8903 0.070 Uiso 0.51 1 calc PR B 1 H19B H 0.6030 0.9952 0.9132 0.070 Uiso 0.51 1 calc PR B 1 H19C H 0.5759 1.1040 0.8497 0.070 Uiso 0.51 1 calc PR B 1 C20A C 0.5989(5) 0.9165(6) 0.7209(5) 0.0520(16) Uani 0.51 1 d P B 1 H20A H 0.5609 0.8593 0.7627 0.078 Uiso 0.51 1 calc PR B 1 H20B H 0.6347 0.8855 0.6561 0.078 Uiso 0.51 1 calc PR B 1 H20C H 0.5190 0.9841 0.7236 0.078 Uiso 0.51 1 calc PR B 1 P5B P 0.76902(15) 0.91562(13) 0.71819(12) 0.0294(3) Uani 0.49 1 d P B 2 C18B C 0.6353(6) 0.8538(6) 0.6767(4) 0.0419(13) Uani 0.49 1 d P B 2 H18D H 0.5981 0.8002 0.7228 0.063 Uiso 0.49 1 calc PR B 2 H18E H 0.6845 0.8139 0.6160 0.063 Uiso 0.49 1 calc PR B 2 H18F H 0.5519 0.9144 0.6689 0.063 Uiso 0.49 1 calc PR B 2 C19B C 0.6438(6) 1.0194(4) 0.8077(5) 0.0415(12) Uani 0.49 1 d P B 2 H19D H 0.5648 1.0646 0.7813 0.062 Uiso 0.49 1 calc PR B 2 H19E H 0.7003 1.0696 0.8268 0.062 Uiso 0.49 1 calc PR B 2 H19F H 0.5994 0.9795 0.8627 0.062 Uiso 0.49 1 calc PR B 2 C20B C 0.8117(7) 1.0144(6) 0.6222(5) 0.0539(16) Uani 0.49 1 d P B 2 H20D H 0.7240 1.0759 0.6250 0.081 Uiso 0.49 1 calc PR B 2 H20E H 0.8389 0.9735 0.5613 0.081 Uiso 0.49 1 calc PR B 2 H20F H 0.8950 1.0463 0.6292 0.081 Uiso 0.49 1 calc PR B 2 P2 P 0.79499(5) 0.75220(4) 0.90525(4) 0.02254(10) Uani 1 1 d . B . P4A P 1.0880(6) 0.9472(3) 0.7774(3) 0.0228(5) Uani 0.64 1 d P B 1 C15A C 1.0004(5) 1.0904(3) 0.8257(4) 0.0451(10) Uani 0.64 1 d P B 1 H15A H 1.0763 1.1356 0.8183 0.068 Uiso 0.64 1 calc PR B 1 H15B H 0.9526 1.0866 0.8928 0.068 Uiso 0.64 1 calc PR B 1 H15C H 0.9254 1.1258 0.7920 0.068 Uiso 0.64 1 calc PR B 1 C17A C 1.2327(6) 0.9245(5) 0.8465(4) 0.0298(10) Uani 0.64 1 d P B 1 H17A H 1.2824 0.9884 0.8378 0.045 Uiso 0.64 1 calc PR B 1 H17B H 1.3062 0.8540 0.8245 0.045 Uiso 0.64 1 calc PR B 1 H17C H 1.1854 0.9192 0.9135 0.045 Uiso 0.64 1 calc PR B 1 C16A C 1.1990(7) 0.9807(5) 0.6628(4) 0.0363(11) Uani 0.64 1 d P B 1 H16A H 1.1329 1.0109 0.6218 0.054 Uiso 0.64 1 calc PR B 1 H16B H 1.2694 0.9117 0.6336 0.054 Uiso 0.64 1 calc PR B 1 H16C H 1.2541 1.0376 0.6720 0.054 Uiso 0.64 1 calc PR B 1 P4B P 1.0924(12) 0.9360(7) 0.7588(6) 0.0360(18) Uani 0.36 1 d P B 2 C15B C 0.9909(12) 1.0889(9) 0.7846(8) 0.058(3) Uiso 0.36 1 d P B 2 H15D H 0.9168 1.0948 0.8452 0.087 Uiso 0.36 1 calc PR B 2 H15E H 0.9408 1.1158 0.7345 0.087 Uiso 0.36 1 calc PR B 2 H15F H 1.0623 1.1353 0.7876 0.087 Uiso 0.36 1 calc PR B 2 C16B C 1.2257(14) 0.9522(10) 0.6476(9) 0.040(3) Uiso 0.36 1 d P B 2 H16D H 1.2717 1.0157 0.6543 0.060 Uiso 0.36 1 calc PR B 2 H16E H 1.1735 0.9674 0.5970 0.060 Uiso 0.36 1 calc PR B 2 H16F H 1.3029 0.8823 0.6323 0.060 Uiso 0.36 1 calc PR B 2 C17B C 1.2055(14) 0.9442(11) 0.8365(10) 0.041(4) Uiso 0.36 1 d P B 2 H17D H 1.2857 0.8759 0.8283 0.062 Uiso 0.36 1 calc PR B 2 H17E H 1.1452 0.9501 0.9016 0.062 Uiso 0.36 1 calc PR B 2 H17F H 1.2486 1.0113 0.8227 0.062 Uiso 0.36 1 calc PR B 2 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 0.01879(8) 0.03193(9) 0.02832(9) 0.01615(6) -0.01117(6) -0.01032(6) N1 0.0262(9) 0.0273(9) 0.0378(10) -0.0004(7) -0.0063(7) -0.0007(7) F1A 0.058(5) 0.068(5) 0.177(11) -0.069(6) -0.076(6) 0.032(4) F2A 0.050(3) 0.072(4) 0.0291(17) -0.0233(19) 0.0050(16) -0.025(3) F3A 0.082(3) 0.090(3) 0.0432(18) 0.016(2) -0.020(2) -0.067(3) F1B 0.043(4) 0.075(4) 0.076(4) -0.018(3) -0.031(3) -0.002(3) F2B 0.091(7) 0.041(3) 0.129(8) -0.050(4) -0.071(5) 0.026(4) F3B 0.097(5) 0.162(7) 0.048(3) 0.015(5) -0.020(3) -0.103(5) N2 0.0267(9) 0.0273(9) 0.0441(11) -0.0006(8) -0.0099(8) -0.0018(7) F4A 0.054(5) 0.145(11) 0.052(5) -0.029(5) -0.020(4) -0.032(5) F5A 0.098(7) 0.144(10) 0.082(7) -0.089(7) -0.057(6) 0.071(6) F6A 0.057(6) 0.112(8) 0.054(6) 0.027(6) -0.029(4) -0.064(6) F5B 0.089(3) 0.0553(19) 0.050(2) -0.0186(16) -0.0072(19) -0.034(2) F6B 0.047(3) 0.140(6) 0.087(4) -0.039(4) -0.033(3) -0.010(3) F4B 0.132(6) 0.120(5) 0.030(2) 0.013(3) -0.020(3) -0.097(5) C1 0.0389(13) 0.0543(15) 0.0357(12) -0.0100(11) -0.0032(10) -0.0175(11) C2 0.0255(10) 0.0396(12) 0.0314(11) -0.0109(9) 0.0024(8) -0.0085(9) C3 0.0339(12) 0.0654(17) 0.0299(11) -0.0137(11) 0.0069(9) -0.0233(12) C4 0.0224(9) 0.0348(11) 0.0352(11) -0.0111(9) -0.0023(8) -0.0020(8) C5 0.0387(13) 0.0573(16) 0.0437(14) -0.0121(13) -0.0090(11) -0.0126(12) C9 0.0575(17) 0.0544(16) 0.0507(16) -0.0255(13) 0.0170(13) -0.0310(14) C10 0.0217(10) 0.0401(13) 0.0605(16) 0.0213(11) -0.0056(10) -0.0070(9) C11 0.0291(10) 0.0270(10) 0.0336(11) 0.0112(8) -0.0053(8) -0.0046(8) C12 0.0308(11) 0.0584(16) 0.0448(14) 0.0255(12) -0.0190(10) -0.0108(11) C13 0.0417(14) 0.0230(11) 0.080(2) -0.0055(12) 0.0163(14) -0.0013(10) C14 0.0253(11) 0.0384(13) 0.0605(16) -0.0009(12) 0.0089(11) -0.0010(9) P1A 0.0320(8) 0.0401(9) 0.0183(6) -0.0023(6) -0.0040(5) -0.0191(6) C6A 0.042(3) 0.063(4) 0.038(3) -0.028(3) 0.009(3) -0.019(3) C7A 0.050(4) 0.055(4) 0.027(3) -0.007(3) -0.009(3) -0.031(3) C8A 0.066(4) 0.070(4) 0.022(2) 0.015(3) -0.017(2) -0.045(3) P1B 0.0381(9) 0.0369(8) 0.0186(6) -0.0004(6) -0.0022(6) -0.0225(7) C7B 0.058(5) 0.058(4) 0.040(3) -0.023(3) 0.008(3) -0.040(4) C6B 0.047(3) 0.040(3) 0.028(2) -0.017(2) 0.012(2) -0.011(3) C8B 0.054(4) 0.079(4) 0.024(2) 0.013(3) -0.013(2) -0.031(3) P3 0.0192(2) 0.0230(2) 0.0332(3) 0.0027(2) -0.0012(2) 0.00116(18) P5A 0.0163(5) 0.0329(7) 0.0324(7) 0.0168(5) -0.0029(5) -0.0004(5) C18A 0.025(2) 0.037(3) 0.040(3) 0.020(2) -0.0036(19) 0.0010(18) C19A 0.038(3) 0.031(3) 0.047(3) 0.012(2) 0.014(2) 0.016(2) C20A 0.020(2) 0.075(4) 0.066(4) 0.043(3) -0.019(2) -0.017(3) P5B 0.0219(6) 0.0333(7) 0.0369(8) 0.0196(6) -0.0141(6) -0.0086(5) C18B 0.029(3) 0.061(4) 0.043(3) 0.012(3) -0.019(2) -0.013(2) C19B 0.026(2) 0.022(2) 0.069(4) 0.009(3) -0.008(3) 0.0022(18) C20B 0.047(3) 0.057(4) 0.063(4) 0.045(3) -0.025(3) -0.016(3) P2 0.0187(2) 0.0194(2) 0.0271(2) 0.00298(18) -0.00257(18) -0.00277(17) P4A 0.0199(7) 0.0156(10) 0.0297(11) 0.0030(10) -0.0009(8) -0.0029(7) C15A 0.053(3) 0.0202(18) 0.054(3) -0.0001(18) -0.007(2) 0.0016(16) C17A 0.029(2) 0.029(2) 0.038(2) 0.0005(18) -0.017(2) -0.0113(18) C16A 0.037(3) 0.034(3) 0.038(3) 0.010(2) 0.001(2) -0.020(2) P4B 0.0225(13) 0.0260(16) 0.054(4) -0.0107(17) 0.002(2) -0.0063(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 P1A 2.2236(16) . ? Rh1 P5B 2.2697(15) . ? Rh1 P4B 2.271(10) . ? Rh1 P3 2.3160(9) . ? Rh1 P2 2.3673(8) . ? Rh1 P4A 2.399(5) . ? Rh1 P5A 2.4044(15) . ? Rh1 P1B 2.5059(17) . ? N1 C2 1.345(3) . ? N1 N2 1.359(3) . ? F1A C1 1.298(8) . ? F2A C1 1.325(5) . ? F3A C1 1.394(5) . ? F1B C1 1.395(10) . ? F2B C1 1.297(8) . ? F3B C1 1.309(6) . ? N2 C4 1.338(3) . ? F4A C5 1.359(11) . ? F5A C5 1.336(8) . ? F6A C5 1.324(10) . ? F5B C5 1.356(5) . ? F6B C5 1.322(7) . ? F4B C5 1.314(6) . ? C1 C2 1.476(3) . ? C2 C3 1.388(3) . ? C3 C4 1.387(3) . ? C3 H3 0.9500 . ? C4 C5 1.474(3) . ? C9 P2 1.826(3) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 P2 1.848(2) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 P2 1.836(2) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 P3 1.841(3) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 P3 1.838(3) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 P3 1.846(2) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? P1A C6A 1.843(6) . ? P1A C8A 1.847(6) . ? P1A C7A 1.848(6) . ? C6A H6A1 0.9800 . ? C6A H6A2 0.9800 . ? C6A H6A3 0.9800 . ? C7A H7A1 0.9800 . ? C7A H7A2 0.9800 . ? C7A H7A3 0.9800 . ? C8A H8A1 0.9800 . ? C8A H8A2 0.9800 . ? C8A H8A3 0.9800 . ? P1B C7B 1.834(7) . ? P1B C8B 1.841(6) . ? P1B C6B 1.848(6) . ? C7B H7B1 0.9800 . ? C7B H7B2 0.9800 . ? C7B H7B3 0.9800 . ? C6B H6B1 0.9800 . ? C6B H6B2 0.9800 . ? C6B H6B3 0.9800 . ? C8B H8B1 0.9800 . ? C8B H8B2 0.9800 . ? C8B H8B3 0.9800 . ? P5A C20A 1.841(6) . ? P5A C19A 1.841(6) . ? P5A C18A 1.853(5) . ? C18A H18A 0.9800 . ? C18A H18B 0.9800 . ? C18A H18C 0.9800 . ? C19A H19A 0.9800 . ? C19A H19B 0.9800 . ? C19A H19C 0.9800 . ? C20A H20A 0.9800 . ? C20A H20B 0.9800 . ? C20A H20C 0.9800 . ? P5B C18B 1.833(6) . ? P5B C19B 1.837(6) . ? P5B C20B 1.845(5) . ? C18B H18D 0.9800 . ? C18B H18E 0.9800 . ? C18B H18F 0.9800 . ? C19B H19D 0.9800 . ? C19B H19E 0.9800 . ? C19B H19F 0.9800 . ? C20B H20D 0.9800 . ? C20B H20E 0.9800 . ? C20B H20F 0.9800 . ? P4A C15A 1.825(6) . ? P4A C16A 1.835(7) . ? P4A C17A 1.868(8) . ? C15A H15A 0.9800 . ? C15A H15B 0.9800 . ? C15A H15C 0.9800 . ? C17A H17A 0.9800 . ? C17A H17B 0.9800 . ? C17A H17C 0.9800 . ? C16A H16A 0.9800 . ? C16A H16B 0.9800 . ? C16A H16C 0.9800 . ? P4B C17B 1.764(16) . ? P4B C16B 1.835(16) . ? P4B C15B 1.887(14) . ? C15B H15D 0.9800 . ? C15B H15E 0.9800 . ? C15B H15F 0.9800 . ? C16B H16D 0.9800 . ? C16B H16E 0.9800 . ? C16B H16F 0.9800 . ? C17B H17D 0.9800 . ? C17B H17E 0.9800 . ? C17B H17F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1A Rh1 P5B 74.06(7) . . ? P1A Rh1 P4B 110.7(2) . . ? P5B Rh1 P4B 94.3(2) . . ? P1A Rh1 P3 98.00(5) . . ? P5B Rh1 P3 171.65(5) . . ? P4B Rh1 P3 90.9(2) . . ? P1A Rh1 P2 123.02(5) . . ? P5B Rh1 P2 92.76(5) . . ? P4B Rh1 P2 125.7(2) . . ? P3 Rh1 P2 89.45(3) . . ? P1A Rh1 P4A 117.20(12) . . ? P5B Rh1 P4A 95.17(11) . . ? P3 Rh1 P4A 90.78(11) . . ? P2 Rh1 P4A 119.09(12) . . ? P1A Rh1 P5A 91.69(6) . . ? P4B Rh1 P5A 85.6(2) . . ? P3 Rh1 P5A 170.31(4) . . ? P2 Rh1 P5A 85.26(4) . . ? P4A Rh1 P5A 84.73(12) . . ? P5B Rh1 P1B 88.06(7) . . ? P4B Rh1 P1B 113.3(2) . . ? P3 Rh1 P1B 83.89(5) . . ? P2 Rh1 P1B 120.71(4) . . ? P4A Rh1 P1B 119.84(12) . . ? P5A Rh1 P1B 105.79(6) . . ? C2 N1 N2 107.35(19) . . ? C4 N2 N1 107.19(18) . . ? F2B C1 F3B 115.4(7) . . ? F1A C1 F2A 107.1(6) . . ? F1A C1 F3A 109.6(6) . . ? F2A C1 F3A 100.4(4) . . ? F2B C1 F1B 99.4(8) . . ? F3B C1 F1B 95.0(6) . . ? F2B C1 C2 117.6(6) . . ? F1A C1 C2 115.5(5) . . ? F3B C1 C2 113.8(3) . . ? F2A C1 C2 112.7(4) . . ? F3A C1 C2 110.5(3) . . ? F1B C1 C2 111.9(7) . . ? N1 C2 C3 111.5(2) . . ? N1 C2 C1 119.7(2) . . ? C3 C2 C1 128.8(2) . . ? C4 C3 C2 102.0(2) . . ? C4 C3 H3 129.0 . . ? C2 C3 H3 129.0 . . ? N2 C4 C3 112.0(2) . . ? N2 C4 C5 119.6(2) . . ? C3 C4 C5 128.4(2) . . ? F4B C5 F6B 104.6(6) . . ? F6A C5 F5A 111.2(10) . . ? F6B C5 F5B 102.9(6) . . ? F6A C5 F4A 108.1(8) . . ? F5A C5 F4A 95.1(10) . . ? F4B C5 C4 115.3(4) . . ? F6B C5 C4 111.8(5) . . ? F6A C5 C4 117.3(7) . . ? F5A C5 C4 115.3(5) . . ? F5B C5 C4 112.6(4) . . ? F4A C5 C4 107.1(7) . . ? P2 C9 H9A 109.5 . . ? P2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? P2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? P2 C10 H10A 109.5 . . ? P2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? P2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? P2 C11 H11A 109.5 . . ? P2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? P2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? P3 C12 H12A 109.5 . . ? P3 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? P3 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? P3 C13 H13A 109.5 . . ? P3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? P3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? P3 C14 H14A 109.5 . . ? P3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? P3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C6A P1A C8A 95.0(4) . . ? C6A P1A C7A 99.4(3) . . ? C8A P1A C7A 100.2(3) . . ? C6A P1A Rh1 120.3(2) . . ? C8A P1A Rh1 122.0(2) . . ? C7A P1A Rh1 115.4(2) . . ? C7B P1B C8B 99.3(3) . . ? C7B P1B C6B 99.0(3) . . ? C8B P1B C6B 94.6(3) . . ? C7B P1B Rh1 116.9(2) . . ? C8B P1B Rh1 118.8(3) . . ? C6B P1B Rh1 123.2(2) . . ? P1B C7B H7B1 109.5 . . ? P1B C7B H7B2 109.5 . . ? H7B1 C7B H7B2 109.5 . . ? P1B C7B H7B3 109.5 . . ? H7B1 C7B H7B3 109.5 . . ? H7B2 C7B H7B3 109.5 . . ? P1B C6B H6B1 109.5 . . ? P1B C6B H6B2 109.5 . . ? H6B1 C6B H6B2 109.5 . . ? P1B C6B H6B3 109.5 . . ? H6B1 C6B H6B3 109.5 . . ? H6B2 C6B H6B3 109.5 . . ? P1B C8B H8B1 109.5 . . ? P1B C8B H8B2 109.5 . . ? H8B1 C8B H8B2 109.5 . . ? P1B C8B H8B3 109.5 . . ? H8B1 C8B H8B3 109.5 . . ? H8B2 C8B H8B3 109.5 . . ? C13 P3 C12 100.23(15) . . ? C13 P3 C14 100.37(12) . . ? C12 P3 C14 99.25(13) . . ? C13 P3 Rh1 117.12(11) . . ? C12 P3 Rh1 118.47(9) . . ? C14 P3 Rh1 117.94(10) . . ? C20A P5A C19A 101.0(3) . . ? C20A P5A C18A 98.2(2) . . ? C19A P5A C18A 99.8(3) . . ? C20A P5A Rh1 115.9(2) . . ? C19A P5A Rh1 119.3(2) . . ? C18A P5A Rh1 118.88(16) . . ? C18B P5B C19B 101.2(3) . . ? C18B P5B C20B 99.6(3) . . ? C19B P5B C20B 98.3(3) . . ? C18B P5B Rh1 119.8(2) . . ? C19B P5B Rh1 114.6(2) . . ? C20B P5B Rh1 119.6(2) . . ? P5B C18B H18D 109.5 . . ? P5B C18B H18E 109.5 . . ? H18D C18B H18E 109.5 . . ? P5B C18B H18F 109.5 . . ? H18D C18B H18F 109.5 . . ? H18E C18B H18F 109.5 . . ? P5B C19B H19D 109.5 . . ? P5B C19B H19E 109.5 . . ? H19D C19B H19E 109.5 . . ? P5B C19B H19F 109.5 . . ? H19D C19B H19F 109.5 . . ? H19E C19B H19F 109.5 . . ? P5B C20B H20D 109.5 . . ? P5B C20B H20E 109.5 . . ? H20D C20B H20E 109.5 . . ? P5B C20B H20F 109.5 . . ? H20D C20B H20F 109.5 . . ? H20E C20B H20F 109.5 . . ? C9 P2 C11 99.31(14) . . ? C9 P2 C10 100.35(14) . . ? C11 P2 C10 92.95(10) . . ? C9 P2 Rh1 112.85(9) . . ? C11 P2 Rh1 123.44(7) . . ? C10 P2 Rh1 123.08(9) . . ? C15A P4A C16A 100.0(3) . . ? C15A P4A C17A 94.3(3) . . ? C16A P4A C17A 99.7(4) . . ? C15A P4A Rh1 125.0(3) . . ? C16A P4A Rh1 113.4(3) . . ? C17A P4A Rh1 119.8(3) . . ? C17B P4B C16B 98.4(8) . . ? C17B P4B C15B 92.0(7) . . ? C16B P4B C15B 99.6(7) . . ? C17B P4B Rh1 123.0(6) . . ? C16B P4B Rh1 119.2(6) . . ? C15B P4B Rh1 118.9(6) . . ? P4B C15B H15D 109.5 . . ? P4B C15B H15E 109.5 . . ? H15D C15B H15E 109.5 . . ? P4B C15B H15F 109.5 . . ? H15D C15B H15F 109.5 . . ? H15E C15B H15F 109.5 . . ? P4B C16B H16D 109.5 . . ? P4B C16B H16E 109.5 . . ? H16D C16B H16E 109.5 . . ? P4B C16B H16F 109.5 . . ? H16D C16B H16F 109.5 . . ? H16E C16B H16F 109.5 . . ? P4B C17B H17D 109.5 . . ? P4B C17B H17E 109.5 . . ? H17D C17B H17E 109.5 . . ? P4B C17B H17F 109.5 . . ? H17D C17B H17F 109.5 . . ? H17E C17B H17F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.802 _refine_diff_density_min -1.247 _refine_diff_density_rms 0.060 # Attachment '- Compound 4.CIF' data_IrP5Pz _database_code_depnum_ccdc_archive 'CCDC 772626' #TrackingRef '- Compound 4.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; pentakis(trimethylphosphine)iridium(I) bis(3,5-trifluoromethyl) pyrazolate ; _chemical_name_common ;pentakis(trimethylphosphine)iridium(i) bis(3,5- trifluoromethyl) pyrazolate ; _chemical_melting_point ? _chemical_formula_moiety 'C15 H45 Ir P5, C5 H1 F6 N2' _chemical_formula_sum 'C20 H46 F6 Ir N2 P5' _chemical_formula_weight 775.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4552(8) _cell_length_b 12.0860(10) _cell_length_c 14.5150(13) _cell_angle_alpha 88.571(3) _cell_angle_beta 75.866(2) _cell_angle_gamma 77.060(2) _cell_volume 1566.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 36337 _cell_measurement_theta_min 3.16 _cell_measurement_theta_max 27.7 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.077 _exptl_crystal_size_min 0.077 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.644 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 772 _exptl_absorpt_coefficient_mu 4.564 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.44 _exptl_absorpt_correction_T_max 0.7 _exptl_absorpt_process_details ; Abscor. T. Higashi (2001). The Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC-12 with Saturn 724+CCD' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43093 _diffrn_reflns_av_R_equivalents 0.0741 _diffrn_reflns_av_sigmaI/netI 0.0527 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7160 _reflns_number_gt 6381 _reflns_threshold_expression >2sigma(I) _publ_section_references ; Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838. An Integrated System of Windows Programs for the Solution, Refinement and Analysis of Single Crystal X-ray Diffraction Data. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'CIFTAB (Sheldrick, 2008)' _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^)+(0.0968P)^2^+17.5144P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7160 _refine_ls_number_parameters 393 _refine_ls_number_restraints 193 _refine_ls_R_factor_all 0.0839 _refine_ls_R_factor_gt 0.0759 _refine_ls_wR_factor_ref 0.1996 _refine_ls_wR_factor_gt 0.1897 _refine_ls_goodness_of_fit_ref 1.170 _refine_ls_restrained_S_all 1.171 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.54115(4) 0.20043(3) 0.73287(2) 0.03149(15) Uani 1 1 d . . . P2 P 0.7018(3) 0.2451(2) 0.59485(18) 0.0326(5) Uani 1 1 d . A . P3 P 0.3491(3) 0.3379(2) 0.6992(2) 0.0396(6) Uani 1 1 d . A . P4 P 0.4108(3) 0.0612(2) 0.7300(2) 0.0452(7) Uani 1 1 d . A . P1A P 0.4927(8) 0.3107(6) 0.8800(4) 0.0373(13) Uani 0.56 1 d PU A 1 C1A C 0.303(3) 0.398(2) 0.9320(16) 0.053(5) Uani 0.56 1 d PU A 1 H1A1 H 0.3092 0.4552 0.9766 0.080 Uiso 0.56 1 calc PR A 1 H1A2 H 0.2387 0.3490 0.9659 0.080 Uiso 0.56 1 calc PR A 1 H1A3 H 0.2605 0.4357 0.8812 0.080 Uiso 0.56 1 calc PR A 1 C2A C 0.510(3) 0.234(2) 0.9890(16) 0.053(5) Uani 0.56 1 d PU A 1 H2A1 H 0.4976 0.2889 1.0407 0.080 Uiso 0.56 1 calc PR A 1 H2A2 H 0.6090 0.1828 0.9783 0.080 Uiso 0.56 1 calc PR A 1 H2A3 H 0.4325 0.1902 1.0062 0.080 Uiso 0.56 1 calc PR A 1 C3A C 0.607(3) 0.409(2) 0.8833(17) 0.049(5) Uani 0.56 1 d PU A 1 H3A1 H 0.5828 0.4419 0.9477 0.073 Uiso 0.56 1 calc PR A 1 H3A2 H 0.5881 0.4692 0.8386 0.073 Uiso 0.56 1 calc PR A 1 H3A3 H 0.7126 0.3691 0.8653 0.073 Uiso 0.56 1 calc PR A 1 P1B P 0.5367(11) 0.2592(8) 0.8731(6) 0.0399(18) Uani 0.44 1 d PU A 2 C1B C 0.365(5) 0.340(4) 0.949(3) 0.076(9) Uani 0.44 1 d PU A 2 H1B1 H 0.3813 0.3525 1.0119 0.114 Uiso 0.44 1 calc PR A 2 H1B2 H 0.2862 0.2976 0.9559 0.114 Uiso 0.44 1 calc PR A 2 H1B3 H 0.3350 0.4132 0.9211 0.114 Uiso 0.44 1 calc PR A 2 C2B C 0.577(4) 0.162(3) 0.969(2) 0.057(7) Uani 0.44 1 d PU A 2 H2B1 H 0.6778 0.1135 0.9473 0.086 Uiso 0.44 1 calc PR A 2 H2B2 H 0.5034 0.1150 0.9842 0.086 Uiso 0.44 1 calc PR A 2 H2B3 H 0.5724 0.2069 1.0254 0.086 Uiso 0.44 1 calc PR A 2 C3B C 0.659(4) 0.354(3) 0.881(3) 0.059(8) Uani 0.44 1 d PU A 2 H3B1 H 0.6196 0.4294 0.8595 0.089 Uiso 0.44 1 calc PR A 2 H3B2 H 0.7601 0.3233 0.8418 0.089 Uiso 0.44 1 calc PR A 2 H3B3 H 0.6645 0.3609 0.9477 0.089 Uiso 0.44 1 calc PR A 2 C4 C 0.9016(12) 0.2400(12) 0.5868(11) 0.058(4) Uani 1 1 d . . . H4A H 0.9460 0.1695 0.6139 0.087 Uiso 1 1 calc R A . H4B H 0.9099 0.3052 0.6223 0.087 Uiso 1 1 calc R . . H4C H 0.9546 0.2426 0.5200 0.087 Uiso 1 1 calc R . . C5 C 0.722(2) 0.1558(17) 0.4913(11) 0.090(7) Uani 1 1 d . . . H5A H 0.6318 0.1776 0.4671 0.135 Uiso 1 1 calc R A . H5B H 0.7357 0.0761 0.5092 0.135 Uiso 1 1 calc R . . H5C H 0.8092 0.1656 0.4418 0.135 Uiso 1 1 calc R . . C6 C 0.6749(13) 0.3861(9) 0.5435(8) 0.042(2) Uani 1 1 d . . . H6A H 0.7471 0.3837 0.4819 0.063 Uiso 1 1 calc R A . H6B H 0.6901 0.4412 0.5865 0.063 Uiso 1 1 calc R . . H6C H 0.5730 0.4088 0.5346 0.063 Uiso 1 1 calc R . . C7 C 0.3591(17) 0.4851(11) 0.7101(14) 0.076(5) Uani 1 1 d . . . H7A H 0.4626 0.4923 0.6849 0.114 Uiso 1 1 calc R A . H7B H 0.3256 0.5099 0.7772 0.114 Uiso 1 1 calc R . . H7C H 0.2944 0.5326 0.6741 0.114 Uiso 1 1 calc R . . C8 C 0.3126(15) 0.3339(15) 0.5806(10) 0.066(4) Uani 1 1 d . . . H8A H 0.2377 0.4020 0.5734 0.098 Uiso 1 1 calc R A . H8B H 0.2752 0.2661 0.5734 0.098 Uiso 1 1 calc R . . H8C H 0.4056 0.3316 0.5319 0.098 Uiso 1 1 calc R . . C9 C 0.1565(14) 0.3438(13) 0.7720(12) 0.066(4) Uani 1 1 d . . . H9A H 0.1333 0.3989 0.8250 0.100 Uiso 1 1 calc R A . H9B H 0.1496 0.2686 0.7970 0.100 Uiso 1 1 calc R . . H9C H 0.0851 0.3670 0.7325 0.100 Uiso 1 1 calc R . . C10 C 0.2727(16) 0.0749(13) 0.6588(10) 0.057(3) Uani 1 1 d . . . H10A H 0.2231 0.0110 0.6707 0.086 Uiso 1 1 calc R A . H10B H 0.3231 0.0745 0.5912 0.086 Uiso 1 1 calc R . . H10C H 0.1980 0.1464 0.6764 0.086 Uiso 1 1 calc R . . C11 C 0.2911(18) 0.0313(14) 0.8446(10) 0.067(4) Uani 1 1 d . . . H11A H 0.2178 0.1010 0.8709 0.101 Uiso 1 1 calc R A . H11B H 0.3534 0.0041 0.8891 0.101 Uiso 1 1 calc R . . H11C H 0.2385 -0.0269 0.8346 0.101 Uiso 1 1 calc R . . C12 C 0.506(3) -0.0851(13) 0.6877(19) 0.115(9) Uani 1 1 d . . . H12A H 0.4316 -0.1262 0.6783 0.173 Uiso 1 1 calc R A . H12B H 0.5564 -0.1235 0.7348 0.173 Uiso 1 1 calc R . . H12C H 0.5792 -0.0837 0.6273 0.173 Uiso 1 1 calc R . . P5A P 0.7342(7) 0.0811(6) 0.7800(6) 0.0428(16) Uani 0.53 1 d PU A 1 C13A C 0.692(3) -0.014(2) 0.8766(18) 0.049(5) Uani 0.53 1 d PU A 1 H13A H 0.7725 -0.0829 0.8675 0.073 Uiso 0.53 1 calc PR A 1 H13B H 0.5973 -0.0350 0.8770 0.073 Uiso 0.53 1 calc PR A 1 H13C H 0.6830 0.0238 0.9372 0.073 Uiso 0.53 1 calc PR A 1 C14A C 0.867(2) 0.140(2) 0.8244(17) 0.045(5) Uani 0.53 1 d PU A 1 H14A H 0.8156 0.1829 0.8839 0.068 Uiso 0.53 1 calc PR A 1 H14B H 0.9109 0.1898 0.7772 0.068 Uiso 0.53 1 calc PR A 1 H14C H 0.9469 0.0775 0.8360 0.068 Uiso 0.53 1 calc PR A 1 C15A C 0.868(3) -0.020(2) 0.690(2) 0.051(5) Uani 0.53 1 d PU A 1 H15A H 0.9211 0.0224 0.6394 0.077 Uiso 0.53 1 calc PR A 1 H15B H 0.8136 -0.0651 0.6621 0.077 Uiso 0.53 1 calc PR A 1 H15C H 0.9399 -0.0698 0.7191 0.077 Uiso 0.53 1 calc PR A 1 P5B P 0.7428(9) 0.0424(8) 0.7377(7) 0.052(2) Uani 0.47 1 d PU A 2 C13B C 0.902(4) 0.075(3) 0.776(2) 0.064(5) Uani 0.47 1 d PU A 2 H13D H 0.9934 0.0531 0.7249 0.097 Uiso 0.47 1 calc PR A 2 H13E H 0.9154 0.0324 0.8328 0.097 Uiso 0.47 1 calc PR A 2 H13F H 0.8820 0.1565 0.7907 0.097 Uiso 0.47 1 calc PR A 2 C14B C 0.847(3) -0.041(2) 0.634(2) 0.057(5) Uani 0.47 1 d PU A 2 H14D H 0.8814 0.0093 0.5831 0.086 Uiso 0.47 1 calc PR A 2 H14E H 0.7841 -0.0843 0.6132 0.086 Uiso 0.47 1 calc PR A 2 H14F H 0.9344 -0.0931 0.6479 0.086 Uiso 0.47 1 calc PR A 2 C15B C 0.711(3) -0.069(2) 0.8261(19) 0.049(5) Uani 0.47 1 d PU A 2 H15D H 0.7542 -0.1441 0.7950 0.074 Uiso 0.47 1 calc PR A 2 H15E H 0.6033 -0.0607 0.8524 0.074 Uiso 0.47 1 calc PR A 2 H15F H 0.7590 -0.0605 0.8774 0.074 Uiso 0.47 1 calc PR A 2 C16 C 0.9058(7) 0.2566(6) 0.0792(4) 0.052(3) Uani 1 1 d G . . F1A F 0.9649(11) 0.3203(8) 0.0068(6) 0.078(3) Uani 0.78 1 d PG B 1 F2A F 0.7529(7) 0.2823(9) 0.0953(7) 0.073(3) Uani 0.78 1 d PG B 1 F3A F 0.9595(11) 0.1437(6) 0.0547(7) 0.071(3) Uani 0.78 1 d PG B 1 F1B F 0.8200(11) 0.1772(8) 0.0978(6) 0.078(3) Uani 0.22 1 d PG B 2 F2B F 1.0319(8) 0.2152(9) 0.0092(6) 0.073(3) Uani 0.22 1 d PG B 2 F3B F 0.8254(11) 0.3538(6) 0.0498(7) 0.071(3) Uani 0.22 1 d PG B 2 C17 C 0.9531(11) 0.2851(9) 0.1673(7) 0.036(2) Uani 1 1 d . B . C18 C 1.0521(15) 0.3450(13) 0.1777(9) 0.056(3) Uani 1 1 d . . . H18 H 1.1123 0.3813 0.1299 0.067 Uiso 1 1 calc R B . C19 C 1.0467(12) 0.3418(10) 0.2732(8) 0.042(2) Uani 1 1 d . B . C20 C 1.1318(8) 0.3932(6) 0.3309(5) 0.056(3) Uani 1 1 d G . . F4A F 1.2197(13) 0.4542(11) 0.2712(7) 0.111(4) Uani 0.80 1 d PGU B 1 F5A F 1.2204(11) 0.3088(7) 0.3697(8) 0.086(3) Uani 0.80 1 d PGU B 1 F6A F 1.0335(9) 0.4637(8) 0.4020(7) 0.070(3) Uani 0.80 1 d PGU B 1 F4B F 1.0960(12) 0.3636(8) 0.4240(6) 0.111(4) Uani 0.20 1 d PGU B 2 F5B F 1.0954(13) 0.5090(7) 0.3255(8) 0.086(3) Uani 0.20 1 d PGU B 2 F6B F 1.2822(8) 0.3541(11) 0.2932(8) 0.070(3) Uani 0.20 1 d PGU B 2 N1 N 0.8880(10) 0.2466(8) 0.2514(7) 0.042(2) Uani 1 1 d . . . N2 N 0.9472(11) 0.2834(8) 0.3170(7) 0.043(2) Uani 1 1 d . B . 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 0.0262(2) 0.0331(2) 0.0340(2) 0.01915(15) -0.01118(14) -0.00202(14) P2 0.0301(12) 0.0255(11) 0.0344(12) 0.0077(9) -0.0023(9) 0.0029(9) P3 0.0260(12) 0.0362(13) 0.0456(14) 0.0136(11) -0.0041(10) 0.0090(10) P4 0.0427(15) 0.0310(13) 0.0564(17) 0.0070(12) -0.0061(13) -0.0043(11) P1A 0.054(4) 0.040(3) 0.021(2) 0.002(3) -0.001(2) -0.023(3) C1A 0.062(9) 0.057(9) 0.035(7) -0.004(7) -0.002(7) -0.014(7) C2A 0.059(9) 0.063(9) 0.041(8) 0.012(7) -0.016(7) -0.015(7) C3A 0.053(9) 0.049(9) 0.047(8) -0.010(7) -0.012(7) -0.018(7) P1B 0.061(5) 0.042(4) 0.029(3) 0.002(3) -0.016(3) -0.031(4) C1B 0.077(12) 0.076(12) 0.075(12) -0.005(9) -0.019(9) -0.017(9) C2B 0.064(11) 0.061(10) 0.045(9) 0.013(8) -0.013(8) -0.013(8) C3B 0.058(11) 0.061(11) 0.059(11) 0.005(8) -0.011(8) -0.019(8) C4 0.025(5) 0.062(8) 0.077(9) 0.035(7) -0.003(5) -0.006(5) C5 0.121(15) 0.098(13) 0.048(8) -0.033(8) 0.031(9) -0.072(12) C6 0.042(6) 0.036(5) 0.044(6) 0.020(4) -0.009(4) -0.004(4) C7 0.057(8) 0.036(7) 0.112(13) 0.008(7) 0.012(8) 0.002(6) C8 0.043(7) 0.103(12) 0.060(8) 0.045(8) -0.033(6) -0.019(7) C9 0.037(6) 0.065(9) 0.078(10) 0.026(7) 0.002(6) 0.007(6) C10 0.058(8) 0.063(8) 0.058(8) -0.005(6) -0.011(6) -0.030(7) C11 0.080(10) 0.084(11) 0.058(8) 0.031(7) -0.018(7) -0.060(9) C12 0.122(17) 0.031(7) 0.15(2) 0.005(10) 0.026(15) -0.005(9) P5A 0.025(2) 0.045(4) 0.058(4) 0.040(3) -0.017(3) -0.004(2) C13A 0.047(8) 0.047(8) 0.049(8) 0.031(7) -0.016(7) -0.004(7) C14A 0.036(7) 0.054(9) 0.047(8) 0.013(7) -0.016(6) -0.009(7) C15A 0.043(8) 0.040(8) 0.064(9) 0.006(7) -0.014(7) 0.006(6) P5B 0.031(3) 0.050(4) 0.058(4) 0.029(3) 0.003(3) 0.011(3) C13B 0.058(9) 0.068(9) 0.065(9) 0.021(7) -0.015(7) -0.012(7) C14B 0.054(9) 0.049(9) 0.055(7) 0.016(6) -0.001(7) 0.001(7) C15B 0.051(9) 0.047(8) 0.044(7) 0.024(7) -0.013(7) 0.000(6) C16 0.055(7) 0.051(7) 0.047(6) -0.001(5) -0.012(5) -0.006(6) F1A 0.101(9) 0.114(10) 0.036(5) 0.021(5) -0.024(5) -0.054(8) F2A 0.052(6) 0.112(9) 0.067(6) 0.003(6) -0.031(5) -0.026(6) F3A 0.093(8) 0.058(6) 0.065(6) -0.022(5) -0.033(6) -0.005(6) F1B 0.101(9) 0.114(10) 0.036(5) 0.021(5) -0.024(5) -0.054(8) F2B 0.052(6) 0.112(9) 0.067(6) 0.003(6) -0.031(5) -0.026(6) F3B 0.093(8) 0.058(6) 0.065(6) -0.022(5) -0.033(6) -0.005(6) C17 0.030(5) 0.035(5) 0.035(5) 0.001(4) -0.001(4) 0.002(4) C18 0.054(7) 0.073(9) 0.037(6) 0.001(6) 0.004(5) -0.025(7) C19 0.034(5) 0.044(6) 0.039(5) 0.001(4) -0.003(4) 0.003(4) C20 0.053(7) 0.062(8) 0.051(7) 0.005(6) -0.008(6) -0.015(6) F4A 0.118(7) 0.130(7) 0.109(7) -0.002(5) -0.035(5) -0.072(6) F5A 0.075(5) 0.091(6) 0.103(6) -0.013(5) -0.051(5) -0.011(5) F6A 0.079(5) 0.064(5) 0.063(5) -0.019(4) -0.020(4) -0.007(4) F4B 0.118(7) 0.130(7) 0.109(7) -0.002(5) -0.035(5) -0.072(6) F5B 0.075(5) 0.091(6) 0.103(6) -0.013(5) -0.051(5) -0.011(5) F6B 0.079(5) 0.064(5) 0.063(5) -0.019(4) -0.020(4) -0.007(4) N1 0.035(4) 0.036(5) 0.051(5) 0.005(4) -0.009(4) -0.002(4) N2 0.041(5) 0.039(5) 0.040(5) 0.011(4) -0.007(4) 0.006(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 P1B 2.161(8) . ? Ir1 P5A 2.293(6) . ? Ir1 P4 2.305(3) . ? Ir1 P3 2.311(2) . ? Ir1 P2 2.332(2) . ? Ir1 P5B 2.391(7) . ? Ir1 P1A 2.437(6) . ? P2 C5 1.819(14) . ? P2 C6 1.833(10) . ? P2 C4 1.851(12) . ? P3 C7 1.815(15) . ? P3 C8 1.840(13) . ? P3 C9 1.855(13) . ? P4 C10 1.831(14) . ? P4 C12 1.839(16) . ? P4 C11 1.847(13) . ? P1A C3A 1.78(2) . ? P1A C2A 1.84(2) . ? P1A C1A 1.85(3) . ? C1A H1A1 0.9800 . ? C1A H1A2 0.9800 . ? C1A H1A3 0.9800 . ? C2A H2A1 0.9800 . ? C2A H2A2 0.9800 . ? C2A H2A3 0.9800 . ? C3A H3A1 0.9800 . ? C3A H3A2 0.9800 . ? C3A H3A3 0.9800 . ? P1B C1B 1.81(4) . ? P1B C3B 1.83(4) . ? P1B C2B 1.85(3) . ? C1B H1B1 0.9800 . ? C1B H1B2 0.9800 . ? C1B H1B3 0.9800 . ? C2B H2B1 0.9800 . ? C2B H2B2 0.9800 . ? C2B H2B3 0.9800 . ? C3B H3B1 0.9800 . ? C3B H3B2 0.9800 . ? C3B H3B3 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? P5A C13A 1.82(2) . ? P5A C14A 1.82(2) . ? P5A C15A 1.84(3) . ? C13A H13A 0.9800 . ? C13A H13B 0.9800 . ? C13A H13C 0.9800 . ? C14A H14A 0.9800 . ? C14A H14B 0.9800 . ? C14A H14C 0.9800 . ? C15A H15A 0.9800 . ? C15A H15B 0.9800 . ? C15A H15C 0.9800 . ? P5B C14B 1.78(3) . ? P5B C13B 1.85(4) . ? P5B C15B 1.86(2) . ? C13B H13D 0.9800 . ? C13B H13E 0.9800 . ? C13B H13F 0.9800 . ? C14B H14D 0.9800 . ? C14B H14E 0.9800 . ? C14B H14F 0.9800 . ? C15B H15D 0.9800 . ? C15B H15E 0.9800 . ? C15B H15F 0.9800 . ? C16 F2B 1.3674 . ? C16 F3A 1.3682 . ? C16 F3B 1.3696 . ? C16 F1A 1.3699 . ? C16 F2A 1.3711 . ? C16 F1B 1.3714 . ? C16 C17 1.525(12) . ? C17 C18 1.341(17) . ? C17 N1 1.348(14) . ? C18 C19 1.374(17) . ? C18 H18 0.9500 . ? C19 N2 1.330(15) . ? C19 C20 1.520(13) . ? C20 F5B 1.3700 . ? C20 F6A 1.3700 . ? C20 F4A 1.3700 . ? C20 F5A 1.3700 . ? C20 F4B 1.3700 . ? C20 F6B 1.3700 . ? N1 N2 1.346(14) . ? 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 P1B Ir1 P5A 73.2(4) . . ? P1B Ir1 P4 115.0(2) . . ? P5A Ir1 P4 94.3(2) . . ? P1B Ir1 P3 100.0(3) . . ? P5A Ir1 P3 172.5(2) . . ? P4 Ir1 P3 91.37(11) . . ? P1B Ir1 P2 123.1(2) . . ? P5A Ir1 P2 92.17(19) . . ? P4 Ir1 P2 120.74(11) . . ? P3 Ir1 P2 89.15(9) . . ? P1B Ir1 P5B 91.3(4) . . ? P5A Ir1 P5B 18.5(2) . . ? P4 Ir1 P5B 83.5(3) . . ? P3 Ir1 P5B 168.7(3) . . ? P2 Ir1 P5B 84.9(2) . . ? P1B Ir1 P1A 15.0(3) . . ? P5A Ir1 P1A 87.8(3) . . ? P4 Ir1 P1A 118.63(17) . . ? P3 Ir1 P1A 85.2(2) . . ? P2 Ir1 P1A 120.44(17) . . ? P5B Ir1 P1A 106.1(3) . . ? C5 P2 C6 100.7(8) . . ? C5 P2 C4 99.4(8) . . ? C6 P2 C4 92.0(6) . . ? C5 P2 Ir1 114.5(5) . . ? C6 P2 Ir1 123.0(4) . . ? C4 P2 Ir1 122.4(4) . . ? C7 P3 C8 101.4(9) . . ? C7 P3 C9 100.3(7) . . ? C8 P3 C9 98.6(7) . . ? C7 P3 Ir1 117.3(6) . . ? C8 P3 Ir1 118.2(5) . . ? C9 P3 Ir1 117.7(5) . . ? C10 P4 C12 94.5(11) . . ? C10 P4 C11 97.9(7) . . ? C12 P4 C11 99.4(9) . . ? C10 P4 Ir1 121.2(5) . . ? C12 P4 Ir1 122.1(8) . . ? C11 P4 Ir1 116.5(5) . . ? C3A P1A C2A 99.9(12) . . ? C3A P1A C1A 101.7(12) . . ? C2A P1A C1A 95.1(12) . . ? C3A P1A Ir1 117.5(8) . . ? C2A P1A Ir1 118.4(9) . . ? C1A P1A Ir1 120.0(9) . . ? C1B P1B C3B 98.6(19) . . ? C1B P1B C2B 92.9(19) . . ? C3B P1B C2B 98.4(17) . . ? C1B P1B Ir1 120.7(15) . . ? C3B P1B Ir1 117.4(12) . . ? C2B P1B Ir1 123.2(12) . . ? P1B C1B H1B1 109.5 . . ? P1B C1B H1B2 109.5 . . ? H1B1 C1B H1B2 109.5 . . ? P1B C1B H1B3 109.5 . . ? H1B1 C1B H1B3 109.5 . . ? H1B2 C1B H1B3 109.5 . . ? P1B C2B H2B1 109.5 . . ? P1B C2B H2B2 109.5 . . ? H2B1 C2B H2B2 109.5 . . ? P1B C2B H2B3 109.5 . . ? H2B1 C2B H2B3 109.5 . . ? H2B2 C2B H2B3 109.5 . . ? P1B C3B H3B1 109.5 . . ? P1B C3B H3B2 109.5 . . ? H3B1 C3B H3B2 109.5 . . ? P1B C3B H3B3 109.5 . . ? H3B1 C3B H3B3 109.5 . . ? H3B2 C3B H3B3 109.5 . . ? P2 C4 H4A 109.5 . . ? P2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? P2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? P2 C5 H5A 109.5 . . ? P2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? P2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? P2 C6 H6A 109.5 . . ? P2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? P2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? P3 C7 H7A 109.5 . . ? P3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? P3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? P3 C8 H8A 109.5 . . ? P3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? P3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? P3 C9 H9A 109.5 . . ? P3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? P3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? P4 C10 H10A 109.5 . . ? P4 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? P4 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? P4 C11 H11A 109.5 . . ? P4 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? P4 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? P4 C12 H12A 109.5 . . ? P4 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? P4 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C13A P5A C14A 97.4(12) . . ? C13A P5A C15A 100.4(12) . . ? C14A P5A C15A 98.7(12) . . ? C13A P5A Ir1 119.2(8) . . ? C14A P5A Ir1 120.0(8) . . ? C15A P5A Ir1 117.0(9) . . ? C14B P5B C13B 97.8(16) . . ? C14B P5B C15B 101.7(14) . . ? C13B P5B C15B 95.4(14) . . ? C14B P5B Ir1 121.6(11) . . ? C13B P5B Ir1 116.1(12) . . ? C15B P5B Ir1 119.3(9) . . ? P5B C13B H13D 109.5 . . ? P5B C13B H13E 109.5 . . ? H13D C13B H13E 109.5 . . ? P5B C13B H13F 109.5 . . ? H13D C13B H13F 109.5 . . ? H13E C13B H13F 109.5 . . ? P5B C14B H14D 109.5 . . ? P5B C14B H14E 109.5 . . ? H14D C14B H14E 109.5 . . ? P5B C14B H14F 109.5 . . ? H14D C14B H14F 109.5 . . ? H14E C14B H14F 109.5 . . ? P5B C15B H15D 109.5 . . ? P5B C15B H15E 109.5 . . ? H15D C15B H15E 109.5 . . ? P5B C15B H15F 109.5 . . ? H15D C15B H15F 109.5 . . ? H15E C15B H15F 109.5 . . ? F2B C16 F3A 56.4 . . ? F2B C16 F3B 109.4 . . ? F3A C16 F3B 140.9 . . ? F2B C16 F1A 56.2 . . ? F3A C16 F1A 109.6 . . ? F3B C16 F1A 56.2 . . ? F2B C16 F2A 140.9 . . ? F3A C16 F2A 109.3 . . ? F3B C16 F2A 56.3 . . ? F1A C16 F2A 109.4 . . ? F2B C16 F1B 109.5 . . ? F3A C16 F1B 56.2 . . ? F3B C16 F1B 109.4 . . ? F1A C16 F1B 141.0 . . ? F2A C16 F1B 56.1 . . ? F2B C16 C17 108.5(6) . . ? F3A C16 C17 110.3(6) . . ? F3B C16 C17 108.8(6) . . ? F1A C16 C17 107.7(6) . . ? F2A C16 C17 110.6(6) . . ? F1B C16 C17 111.3(6) . . ? C18 C17 N1 111.1(10) . . ? C18 C17 C16 130.9(10) . . ? N1 C17 C16 118.1(9) . . ? C17 C18 C19 104.4(11) . . ? C17 C18 H18 127.8 . . ? C19 C18 H18 127.8 . . ? N2 C19 C18 109.8(11) . . ? N2 C19 C20 119.4(9) . . ? C18 C19 C20 130.8(11) . . ? F5B C20 F6A 56.3 . . ? F5B C20 F4A 56.3 . . ? F6A C20 F4A 109.5 . . ? F5B C20 F5A 141.1 . . ? F6A C20 F5A 109.5 . . ? F4A C20 F5A 109.5 . . ? F5B C20 F4B 109.5 . . ? F6A C20 F4B 56.3 . . ? F4A C20 F4B 141.1 . . ? F5A C20 F4B 56.3 . . ? F5B C20 F6B 109.5 . . ? F6A C20 F6B 141.1 . . ? F4A C20 F6B 56.3 . . ? F5A C20 F6B 56.3 . . ? F4B C20 F6B 109.5 . . ? F5B C20 C19 108.9(7) . . ? F6A C20 C19 110.1(6) . . ? F4A C20 C19 108.2(7) . . ? F5A C20 C19 110.1(7) . . ? F4B C20 C19 110.7(7) . . ? F6B C20 C19 108.8(6) . . ? N2 N1 C17 106.5(9) . . ? C19 N2 N1 108.2(9) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 3.577 _refine_diff_density_min -4.503 _refine_diff_density_rms 0.272