# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'T Don Tilley' _publ_contact_author_email TDTILLEY@BERKELEY.EDU _publ_section_title ; Synthesis and reactivity of rhodium and iridium alkene, alkyl and silyl complexes supported by a phenyl-substituted PNP pincer ligand. ; loop_ _publ_author_name 'T Don Tilley' 'Elisa Calimano' # Attachment 'complex21.cif' data_ec29f _database_code_depnum_ccdc_archive 'CCDC 757516' #TrackingRef 'complex21.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H45 Ir N P2, C6 Cl2, C6 H4 Cl2, Cl' _chemical_formula_sum 'C58 H49 Cl5 Ir N P2' _chemical_formula_weight 1191.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -4.7710 6.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6344(14) _cell_length_b 10.6886(15) _cell_length_c 24.996(4) _cell_angle_alpha 88.097(4) _cell_angle_beta 81.884(4) _cell_angle_gamma 80.357(4) _cell_volume 2512.1(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 38976 _cell_measurement_theta_min 8.391 _cell_measurement_theta_max 136.574 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.575 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1192 _exptl_absorpt_coefficient_mu 8.501 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4836 _exptl_absorpt_correction_T_max 0.7845 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'microfocus rotating anode' _diffrn_radiation_monochromator 'HELIOS multilayer mirrors' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_reflns_number 37973 _diffrn_reflns_av_R_equivalents 0.0201 _diffrn_reflns_av_sigmaI/netI 0.0172 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 4.20 _diffrn_reflns_theta_max 68.57 _reflns_number_total 8775 _reflns_number_gt 8592 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v. 2009.1' _computing_cell_refinement 'Bruker APEX2 v. 2009.1' _computing_data_reduction 'Bruker APEX2 v. 2009.1' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Mercury _computing_publication_material CIFTAB _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^)+(0.0940P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8775 _refine_ls_number_parameters 642 _refine_ls_number_restraints 54 _refine_ls_R_factor_all 0.0361 _refine_ls_R_factor_gt 0.0349 _refine_ls_wR_factor_ref 0.1310 _refine_ls_wR_factor_gt 0.1231 _refine_ls_goodness_of_fit_ref 1.339 _refine_ls_restrained_S_all 1.336 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.132028(13) 0.244445(12) 0.268181(5) 0.01840(10) Uani 1 1 d . . . P1 P 0.05647(9) 0.20537(8) 0.18637(4) 0.01755(19) Uani 1 1 d . . . P2 P 0.13716(10) 0.06117(9) 0.31947(4) 0.0200(2) Uani 1 1 d . . . N1 N 0.3330(3) 0.1493(3) 0.22775(13) 0.0207(6) Uani 1 1 d . . . H1 H 0.380(5) 0.209(5) 0.2374(19) 0.025 Uiso 1 1 d . . . Cl1 Cl 0.59590(10) 0.22372(10) 0.26501(4) 0.0315(2) Uani 1 1 d . . . C1 C 0.2131(5) 0.4189(4) 0.2504(2) 0.0328(9) Uani 1 1 d . . . H1A H 0.2984 0.4096 0.2221 0.039 Uiso 1 1 calc R . . C2 C 0.2450(5) 0.3720(4) 0.30183(19) 0.0320(9) Uani 1 1 d . . . H2A H 0.3478 0.3386 0.3033 0.038 Uiso 1 1 calc R . . C3 C 0.1667(6) 0.4435(5) 0.3526(2) 0.0431(11) Uani 1 1 d . . . H3A H 0.2316 0.4370 0.3803 0.052 Uiso 1 1 calc R . . H3B H 0.1410 0.5344 0.3434 0.052 Uiso 1 1 calc R . . C4 C 0.0352(5) 0.3935(4) 0.37589(17) 0.0336(9) Uani 1 1 d . . . H4A H -0.0369 0.4649 0.3913 0.040 Uiso 1 1 calc R . . H4B H 0.0575 0.3338 0.4058 0.040 Uiso 1 1 calc R . . C5 C -0.0277(4) 0.3256(4) 0.33484(17) 0.0259(8) Uani 1 1 d . . . H5A H -0.0916 0.2658 0.3513 0.031 Uiso 1 1 calc R . . C6 C -0.0629(5) 0.3801(4) 0.28563(18) 0.0289(9) Uani 1 1 d . . . H6A H -0.1477 0.3522 0.2738 0.035 Uiso 1 1 calc R . . C7 C -0.0469(6) 0.5179(5) 0.2693(2) 0.0345(10) Uani 1 1 d . . . H7A H -0.0708 0.5710 0.3021 0.041 Uiso 1 1 calc R . . H7B H -0.1166 0.5499 0.2445 0.041 Uiso 1 1 calc R . . C8 C 0.1035(5) 0.5342(4) 0.2415(2) 0.0415(11) Uani 1 1 d . . . H8A H 0.1015 0.5479 0.2022 0.050 Uiso 1 1 calc R . . H8B H 0.1310 0.6101 0.2561 0.050 Uiso 1 1 calc R . . C9 C -0.0245(4) 0.0716(3) 0.16785(15) 0.0202(7) Uani 1 1 d . . . C10 C 0.0140(5) -0.0458(4) 0.19183(16) 0.0274(8) Uani 1 1 d . . . H10A H 0.0795 -0.0544 0.2173 0.033 Uiso 1 1 calc R . . C11 C -0.0425(5) -0.1511(4) 0.17892(18) 0.0324(9) Uani 1 1 d . . . H11A H -0.0161 -0.2308 0.1959 0.039 Uiso 1 1 calc R . . C12 C -0.1362(4) -0.1397(4) 0.14168(18) 0.0300(9) Uani 1 1 d . . . H12A H -0.1755 -0.2113 0.1333 0.036 Uiso 1 1 calc R . . C13 C -0.1740(4) -0.0226(4) 0.11604(17) 0.0276(8) Uani 1 1 d . . . H13A H -0.2368 -0.0149 0.0896 0.033 Uiso 1 1 calc R . . C14 C -0.1190(4) 0.0811(4) 0.12961(16) 0.0251(8) Uani 1 1 d . . . H14A H -0.1457 0.1606 0.1127 0.030 Uiso 1 1 calc R . . C15 C -0.0450(4) 0.3403(3) 0.15457(15) 0.0193(7) Uani 1 1 d . . . C16 C 0.0179(4) 0.4290(4) 0.12181(16) 0.0248(8) Uani 1 1 d . . . H16A H 0.1183 0.4182 0.1131 0.030 Uiso 1 1 calc R . . C17 C -0.0674(5) 0.5339(4) 0.10175(17) 0.0280(8) Uani 1 1 d . . . H17A H -0.0246 0.5940 0.0790 0.034 Uiso 1 1 calc R . . C18 C -0.2142(5) 0.5508(4) 0.11483(18) 0.0282(9) Uani 1 1 d . . . H18A H -0.2718 0.6211 0.1003 0.034 Uiso 1 1 calc R . . C19 C -0.2765(4) 0.4655(4) 0.14888(17) 0.0284(8) Uani 1 1 d . . . H19A H -0.3767 0.4785 0.1587 0.034 Uiso 1 1 calc R . . C20 C -0.1929(4) 0.3609(4) 0.16879(16) 0.0241(8) Uani 1 1 d . . . H20A H -0.2364 0.3025 0.1923 0.029 Uiso 1 1 calc R . . C21 C 0.3492(4) 0.1664(3) 0.16866(15) 0.0208(7) Uani 1 1 d . . . C22 C 0.2276(4) 0.1778(3) 0.14341(15) 0.0190(7) Uani 1 1 d . . . C23 C 0.2414(4) 0.1802(4) 0.08676(15) 0.0230(7) Uani 1 1 d . . . H23A H 0.1595 0.1835 0.0693 0.028 Uiso 1 1 calc R . . C24 C 0.3742(4) 0.1777(4) 0.05576(16) 0.0252(8) Uani 1 1 d . . . C25 C 0.4901(4) 0.1789(4) 0.08276(17) 0.0276(8) Uani 1 1 d . . . H25A H 0.5798 0.1845 0.0623 0.033 Uiso 1 1 calc R . . C26 C 0.4795(4) 0.1720(4) 0.13870(16) 0.0230(8) Uani 1 1 d . . . H26A H 0.5611 0.1712 0.1561 0.028 Uiso 1 1 calc R . . C27 C 0.3883(5) 0.1831(4) -0.00583(17) 0.0325(9) Uani 1 1 d . . . H27A H 0.4588 0.1115 -0.0208 0.049 Uiso 1 1 calc R . . H27B H 0.4191 0.2629 -0.0189 0.049 Uiso 1 1 calc R . . H27C H 0.2962 0.1784 -0.0173 0.049 Uiso 1 1 calc R . . C28 C 0.3708(4) 0.0124(4) 0.24182(15) 0.0204(7) Uani 1 1 d . . . C29 C 0.2850(4) -0.0434(4) 0.28224(16) 0.0230(8) Uani 1 1 d . . . C30 C 0.3236(4) -0.1711(4) 0.29551(16) 0.0247(8) Uani 1 1 d . . . H30A H 0.2641 -0.2086 0.3228 0.030 Uiso 1 1 calc R . . C31 C 0.4468(4) -0.2458(4) 0.27001(16) 0.0247(8) Uani 1 1 d . . . C32 C 0.5327(4) -0.1851(4) 0.23157(17) 0.0262(8) Uani 1 1 d . . . H32A H 0.6196 -0.2321 0.2148 0.031 Uiso 1 1 calc R . . C33 C 0.4967(4) -0.0602(4) 0.21696(16) 0.0232(7) Uani 1 1 d . . . H33A H 0.5572 -0.0229 0.1900 0.028 Uiso 1 1 calc R . . C34 C 0.4848(5) -0.3839(4) 0.28400(19) 0.0328(9) Uani 1 1 d . . . H34A H 0.5843 -0.4022 0.2903 0.049 Uiso 1 1 calc R . . H34B H 0.4714 -0.4356 0.2541 0.049 Uiso 1 1 calc R . . H34C H 0.4234 -0.4040 0.3168 0.049 Uiso 1 1 calc R . . C35 C 0.1937(5) 0.0661(4) 0.38587(16) 0.0262(8) Uani 1 1 d . . . C36 C 0.3371(5) 0.0589(5) 0.39126(18) 0.0328(10) Uani 1 1 d . . . H36A H 0.4073 0.0470 0.3603 0.039 Uiso 1 1 calc R . . C37 C 0.3768(5) 0.0691(5) 0.44201(19) 0.0382(10) Uani 1 1 d . . . H37A H 0.4749 0.0612 0.4455 0.046 Uiso 1 1 calc R . . C38 C 0.2775(5) 0.0903(4) 0.48722(18) 0.0344(10) Uani 1 1 d . . . H38A H 0.3062 0.0982 0.5216 0.041 Uiso 1 1 calc R . . C39 C 0.1345(5) 0.1002(4) 0.48210(17) 0.0318(9) Uani 1 1 d . . . H39A H 0.0648 0.1153 0.5131 0.038 Uiso 1 1 calc R . . C40 C 0.0931(5) 0.0880(4) 0.43187(16) 0.0280(8) Uani 1 1 d . . . H40A H -0.0050 0.0947 0.4288 0.034 Uiso 1 1 calc R . . C41 C -0.0105(4) -0.0278(4) 0.33430(16) 0.0234(8) Uani 1 1 d . . . C42 C -0.0027(4) -0.1358(4) 0.36826(15) 0.0250(8) Uani 1 1 d . . . H42A H 0.0796 -0.1627 0.3852 0.030 Uiso 1 1 calc R . . C43 C -0.1152(5) -0.2029(4) 0.37686(18) 0.0319(9) Uani 1 1 d . . . H43A H -0.1082 -0.2776 0.3986 0.038 Uiso 1 1 calc R . . C44 C -0.2373(5) -0.1619(5) 0.35407(19) 0.0350(9) Uani 1 1 d . . . H44A H -0.3147 -0.2074 0.3608 0.042 Uiso 1 1 calc R . . C45 C -0.2472(5) -0.0551(4) 0.32152(19) 0.0329(9) Uani 1 1 d . . . H45A H -0.3311 -0.0276 0.3056 0.039 Uiso 1 1 calc R . . C46 C -0.1347(4) 0.0126(4) 0.31187(16) 0.0246(8) Uani 1 1 d . . . H46A H -0.1428 0.0868 0.2898 0.030 Uiso 1 1 calc R . . Cl2 Cl 0.30328(15) 0.39424(12) 0.50254(5) 0.0478(3) Uani 1 1 d D . . Cl3 Cl 0.2350(2) 0.66930(16) 0.45225(6) 0.0704(5) Uani 1 1 d D . . C47 C 0.3265(5) 0.5268(4) 0.53575(19) 0.0351(9) Uani 1 1 d D . . C48 C 0.2933(5) 0.6476(5) 0.5151(2) 0.0402(11) Uani 1 1 d D . . C49 C 0.3092(6) 0.7528(5) 0.5430(2) 0.0433(11) Uani 1 1 d D . . H49A H 0.2868 0.8357 0.5284 0.052 Uiso 1 1 calc R . . C50 C 0.3587(5) 0.7347(5) 0.59281(19) 0.0389(10) Uani 1 1 d D . . H50A H 0.3691 0.8062 0.6125 0.047 Uiso 1 1 calc R . . C51 C 0.3923(5) 0.6163(5) 0.6137(2) 0.0392(10) Uani 1 1 d D . . H51A H 0.4268 0.6056 0.6476 0.047 Uiso 1 1 calc R . . C52 C 0.3762(5) 0.5114(5) 0.58570(19) 0.0396(10) Uani 1 1 d D . . H52A H 0.3990 0.4287 0.6005 0.048 Uiso 1 1 calc R . . Cl4A Cl 0.58305(15) 0.49993(13) 0.92105(6) 0.0379(4) Uani 0.799(4) 1 d PD A 1 Cl5A Cl 0.64361(15) 0.22686(14) 0.86802(5) 0.0370(4) Uani 0.799(4) 1 d PD A 1 C53A C 0.6933(10) 0.3754(5) 0.9469(3) 0.027(2) Uani 0.799(4) 1 d PD A 1 C54A C 0.7225(5) 0.2576(5) 0.92283(19) 0.0237(10) Uani 0.799(4) 1 d PD A 1 C55A C 0.8148(5) 0.1596(5) 0.9438(2) 0.0281(11) Uani 0.799(4) 1 d PD A 1 C56A C 0.8777(8) 0.1845(7) 0.9900(3) 0.0247(17) Uani 0.799(4) 1 d PD A 1 C57A C 0.8494(5) 0.3027(5) 1.01227(19) 0.0264(10) Uani 0.799(4) 1 d PD A 1 C58A C 0.7592(5) 0.3976(5) 0.9908(2) 0.0250(10) Uani 0.799(4) 1 d PD A 1 Cl4B Cl 0.7185(14) 0.4708(13) 1.0000(5) 0.089(3) Uiso 0.201(4) 1 d PD A 2 Cl5B Cl 0.884(3) 0.178(2) 0.9947(10) 0.124(9) Uiso 0.201(4) 1 d PD A 2 C53B C 0.727(4) 0.374(2) 0.9447(11) 0.031(12) Uiso 0.201(4) 1 d PD A 2 C54B C 0.779(3) 0.246(2) 0.9468(10) 0.062(8) Uiso 0.201(4) 1 d PD A 2 C55B C 0.775(6) 0.169(3) 0.9034(15) 0.118(19) Uiso 0.201(4) 1 d PD A 2 C56B C 0.719(7) 0.233(4) 0.8586(14) 0.13(2) Uiso 0.201(4) 1 d PD A 2 C57B C 0.627(3) 0.345(2) 0.8652(9) 0.045(6) Uiso 0.201(4) 1 d PD A 2 C58B C 0.640(3) 0.424(2) 0.9055(9) 0.047(6) Uiso 0.201(4) 1 d PD A 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 Ir1 0.01892(13) 0.01919(13) 0.01697(14) -0.00073(8) -0.00335(9) -0.00190(8) P1 0.0184(4) 0.0177(4) 0.0167(4) -0.0006(3) -0.0029(3) -0.0028(3) P2 0.0197(4) 0.0229(5) 0.0171(4) 0.0013(3) -0.0024(4) -0.0034(3) N1 0.0198(15) 0.0212(16) 0.0220(17) 0.0011(12) -0.0061(13) -0.0032(13) Cl1 0.0224(4) 0.0409(5) 0.0336(5) 0.0023(4) -0.0069(4) -0.0102(4) C1 0.030(2) 0.023(2) 0.049(3) 0.0001(17) -0.011(2) -0.0107(17) C2 0.029(2) 0.035(2) 0.035(2) -0.0098(18) -0.0074(19) -0.0088(18) C3 0.045(3) 0.048(3) 0.035(2) -0.024(2) -0.005(2) -0.003(2) C4 0.047(3) 0.030(2) 0.022(2) -0.0070(16) -0.0026(19) -0.0028(19) C5 0.0269(19) 0.0246(19) 0.020(2) -0.0092(15) 0.0099(17) 0.0043(15) C6 0.0255(19) 0.027(2) 0.032(2) -0.0057(16) -0.0074(18) 0.0047(16) C7 0.040(2) 0.028(2) 0.034(2) 0.0010(18) -0.011(2) 0.0044(19) C8 0.044(3) 0.025(2) 0.058(3) -0.001(2) -0.013(2) -0.0087(19) C9 0.0231(17) 0.0191(17) 0.0180(17) -0.0039(13) 0.0004(15) -0.0043(14) C10 0.034(2) 0.027(2) 0.0209(18) -0.0009(15) -0.0035(17) -0.0053(16) C11 0.045(2) 0.0216(19) 0.029(2) 0.0026(16) -0.0017(19) -0.0052(17) C12 0.0304(19) 0.0217(19) 0.039(2) -0.0061(16) -0.0018(18) -0.0085(16) C13 0.0222(17) 0.027(2) 0.035(2) -0.0054(16) -0.0088(17) -0.0035(15) C14 0.0274(18) 0.0214(18) 0.027(2) 0.0000(14) -0.0083(17) -0.0018(15) C15 0.0215(17) 0.0149(16) 0.0206(17) -0.0045(13) -0.0063(14) 0.0035(13) C16 0.0260(19) 0.0212(18) 0.027(2) -0.0008(15) -0.0042(17) -0.0034(15) C17 0.036(2) 0.0213(19) 0.028(2) 0.0009(15) -0.0046(18) -0.0072(16) C18 0.035(2) 0.0185(18) 0.031(2) -0.0047(15) -0.0143(19) 0.0063(16) C19 0.0275(19) 0.0241(19) 0.034(2) -0.0067(16) -0.0119(18) 0.0007(16) C20 0.0227(17) 0.0259(19) 0.0236(19) -0.0030(14) -0.0024(15) -0.0039(15) C21 0.0242(18) 0.0215(18) 0.0144(17) -0.0011(13) 0.0022(15) -0.0013(14) C22 0.0203(16) 0.0173(16) 0.0189(17) -0.0007(13) -0.0026(14) -0.0015(13) C23 0.0274(18) 0.0207(17) 0.0211(19) 0.0004(13) -0.0056(16) -0.0029(14) C24 0.0286(19) 0.0235(18) 0.0211(19) 0.0012(14) -0.0005(16) 0.0000(15) C25 0.0238(18) 0.028(2) 0.028(2) 0.0070(16) 0.0015(17) -0.0005(16) C26 0.0203(17) 0.0249(19) 0.0218(19) 0.0006(14) -0.0021(16) 0.0009(14) C27 0.039(2) 0.035(2) 0.021(2) 0.0035(16) -0.0007(18) -0.0019(19) C28 0.0214(17) 0.0207(18) 0.0202(18) 0.0015(14) -0.0076(15) -0.0028(14) C29 0.0238(18) 0.026(2) 0.0198(19) -0.0003(15) -0.0058(16) -0.0049(15) C30 0.0247(18) 0.027(2) 0.0214(19) 0.0035(15) -0.0007(16) -0.0037(15) C31 0.0243(17) 0.0243(19) 0.026(2) 0.0005(15) -0.0065(16) -0.0040(15) C32 0.0238(18) 0.026(2) 0.027(2) -0.0013(15) -0.0032(16) 0.0000(15) C33 0.0207(17) 0.0257(19) 0.0228(19) 0.0010(14) -0.0035(15) -0.0028(14) C34 0.032(2) 0.025(2) 0.037(2) 0.0037(17) -0.0022(19) 0.0031(16) C35 0.030(2) 0.030(2) 0.0214(19) 0.0030(15) -0.0065(17) -0.0090(16) C36 0.028(2) 0.047(3) 0.025(2) 0.0013(19) -0.0050(18) -0.0092(19) C37 0.035(2) 0.054(3) 0.030(2) 0.003(2) -0.011(2) -0.017(2) C38 0.051(3) 0.030(2) 0.028(2) 0.0030(16) -0.014(2) -0.0155(19) C39 0.043(2) 0.034(2) 0.0182(19) -0.0001(15) -0.0039(18) -0.0056(18) C40 0.0282(19) 0.034(2) 0.0201(19) -0.0038(15) 0.0021(17) -0.0048(16) C41 0.0238(19) 0.027(2) 0.0186(19) -0.0044(15) 0.0026(16) -0.0053(15) C42 0.0242(18) 0.030(2) 0.0179(18) -0.0040(15) 0.0052(15) -0.0011(15) C43 0.037(2) 0.026(2) 0.032(2) -0.0025(17) 0.0014(19) -0.0094(17) C44 0.033(2) 0.038(2) 0.037(2) -0.0070(18) -0.0017(19) -0.0153(19) C45 0.0253(19) 0.039(2) 0.036(2) -0.0070(18) -0.0057(18) -0.0071(17) C46 0.0220(18) 0.028(2) 0.0224(19) -0.0036(15) -0.0012(16) -0.0024(15) Cl2 0.0601(7) 0.0393(6) 0.0471(7) -0.0074(5) -0.0077(6) -0.0151(5) Cl3 0.0993(13) 0.0598(9) 0.0527(8) 0.0022(6) -0.0414(9) 0.0105(8) C47 0.032(2) 0.036(2) 0.035(2) -0.0026(18) -0.0025(19) -0.0032(18) C48 0.042(2) 0.040(3) 0.037(3) -0.002(2) -0.010(2) 0.000(2) C49 0.044(3) 0.031(2) 0.052(3) 0.008(2) -0.007(2) -0.001(2) C50 0.041(2) 0.040(2) 0.033(2) -0.0083(19) 0.008(2) -0.009(2) C51 0.038(2) 0.046(3) 0.033(2) -0.004(2) -0.003(2) -0.008(2) C52 0.042(2) 0.042(3) 0.032(2) 0.0052(19) -0.003(2) 0.002(2) Cl4A 0.0350(7) 0.0335(8) 0.0451(8) -0.0012(6) -0.0201(6) 0.0067(6) Cl5A 0.0349(7) 0.0508(8) 0.0274(7) -0.0148(5) -0.0112(5) -0.0043(6) C53A 0.014(3) 0.032(4) 0.034(4) 0.003(2) -0.003(2) -0.003(2) C54A 0.020(2) 0.033(3) 0.019(2) -0.0044(18) 0.0008(19) -0.0070(19) C55A 0.026(2) 0.034(3) 0.020(2) -0.0142(19) 0.005(2) 0.003(2) C56A 0.026(3) 0.022(3) 0.022(3) 0.0076(18) -0.007(2) 0.0093(19) C57A 0.027(2) 0.037(3) 0.016(2) 0.0015(19) -0.003(2) -0.008(2) C58A 0.021(2) 0.020(2) 0.032(3) 0.0009(19) -0.002(2) -0.0009(19) _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 C2 2.141(4) . ? Ir1 C1 2.149(4) . ? Ir1 N1 2.159(3) . ? Ir1 C6 2.172(4) . ? Ir1 C5 2.196(4) . ? Ir1 P2 2.3027(9) . ? Ir1 P1 2.3378(9) . ? P1 C22 1.821(4) . ? P1 C15 1.827(4) . ? P1 C9 1.840(4) . ? P2 C29 1.818(4) . ? P2 C35 1.823(4) . ? P2 C41 1.829(4) . ? N1 C21 1.472(5) . ? N1 C28 1.490(5) . ? N1 H1 0.90(6) . ? C1 C2 1.419(7) . ? C1 C8 1.515(6) . ? C1 H1A 1.0000 . ? C2 C3 1.538(6) . ? C2 H2A 1.0000 . ? C3 C4 1.492(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.523(6) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.404(6) . ? C5 H5A 1.0000 . ? C6 C7 1.541(6) . ? C6 H6A 1.0000 . ? C7 C8 1.551(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.388(5) . ? C9 C14 1.400(5) . ? C10 C11 1.395(6) . ? C10 H10A 0.9500 . ? C11 C12 1.375(7) . ? C11 H11A 0.9500 . ? C12 C13 1.404(6) . ? C12 H12A 0.9500 . ? C13 C14 1.377(6) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? C15 C16 1.391(5) . ? C15 C20 1.401(5) . ? C16 C17 1.398(6) . ? C16 H16A 0.9500 . ? C17 C18 1.389(6) . ? C17 H17A 0.9500 . ? C18 C19 1.379(6) . ? C18 H18A 0.9500 . ? C19 C20 1.386(6) . ? C19 H19A 0.9500 . ? C20 H20A 0.9500 . ? C21 C26 1.377(6) . ? C21 C22 1.393(5) . ? C22 C23 1.403(5) . ? C23 C24 1.395(6) . ? C23 H23A 0.9500 . ? C24 C25 1.386(6) . ? C24 C27 1.526(5) . ? C25 C26 1.388(6) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.396(6) . ? C28 C33 1.401(6) . ? C29 C30 1.395(6) . ? C30 C31 1.398(6) . ? C30 H30A 0.9500 . ? C31 C32 1.394(6) . ? C31 C34 1.502(5) . ? C32 C33 1.373(6) . ? C32 H32A 0.9500 . ? C33 H33A 0.9500 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C40 1.394(6) . ? C35 C36 1.396(6) . ? C36 C37 1.388(6) . ? C36 H36A 0.9500 . ? C37 C38 1.372(7) . ? C37 H37A 0.9500 . ? C38 C39 1.387(7) . ? C38 H38A 0.9500 . ? C39 C40 1.386(6) . ? C39 H39A 0.9500 . ? C40 H40A 0.9500 . ? C41 C46 1.390(6) . ? C41 C42 1.409(6) . ? C42 C43 1.385(6) . ? C42 H42A 0.9500 . ? C43 C44 1.378(7) . ? C43 H43A 0.9500 . ? C44 C45 1.378(7) . ? C44 H44A 0.9500 . ? C45 C46 1.390(6) . ? C45 H45A 0.9500 . ? C46 H46A 0.9500 . ? Cl2 C47 1.728(5) . ? Cl3 C48 1.738(5) . ? C47 C48 1.378(6) . ? C47 C52 1.394(6) . ? C48 C49 1.382(7) . ? C49 C50 1.392(7) . ? C49 H49A 0.9500 . ? C50 C51 1.358(7) . ? C50 H50A 0.9500 . ? C51 C52 1.384(7) . ? C51 H51A 0.9500 . ? C52 H52A 0.9500 . ? Cl4A C53A 1.726(7) . ? Cl5A C54A 1.724(5) . ? C53A C54A 1.383(7) . ? C53A C58A 1.389(8) . ? C54A C55A 1.394(7) . ? C55A C56A 1.430(8) . ? C56A C57A 1.367(9) . ? C57A C58A 1.369(7) . ? Cl4B C53B 1.735(16) . ? Cl5B C54B 1.740(15) . ? C53B C54B 1.379(15) . ? C53B C58B 1.413(16) . ? C54B C55B 1.395(16) . ? C55B C56B 1.413(17) . ? C56B C57B 1.366(18) . ? C57B C58B 1.374(16) . ? 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 C2 Ir1 C1 38.62(18) . . ? C2 Ir1 N1 88.43(15) . . ? C1 Ir1 N1 86.86(16) . . ? C2 Ir1 C6 89.50(17) . . ? C1 Ir1 C6 79.90(18) . . ? N1 Ir1 C6 161.15(17) . . ? C2 Ir1 C5 79.10(17) . . ? C1 Ir1 C5 93.88(17) . . ? N1 Ir1 C5 158.57(16) . . ? C6 Ir1 C5 37.49(16) . . ? C2 Ir1 P2 109.91(13) . . ? C1 Ir1 P2 147.58(12) . . ? N1 Ir1 P2 84.05(9) . . ? C6 Ir1 P2 114.19(13) . . ? C5 Ir1 P2 83.94(11) . . ? C2 Ir1 P1 139.91(13) . . ? C1 Ir1 P1 101.74(13) . . ? N1 Ir1 P1 82.04(9) . . ? C6 Ir1 P1 87.55(12) . . ? C5 Ir1 P1 118.59(12) . . ? P2 Ir1 P1 107.68(3) . . ? C22 P1 C15 104.22(17) . . ? C22 P1 C9 101.32(16) . . ? C15 P1 C9 102.36(17) . . ? C22 P1 Ir1 99.58(12) . . ? C15 P1 Ir1 116.46(12) . . ? C9 P1 Ir1 129.16(12) . . ? C29 P2 C35 102.52(19) . . ? C29 P2 C41 107.36(19) . . ? C35 P2 C41 101.52(18) . . ? C29 P2 Ir1 101.77(14) . . ? C35 P2 Ir1 116.55(13) . . ? C41 P2 Ir1 124.85(14) . . ? C21 N1 C28 110.0(3) . . ? C21 N1 Ir1 113.4(2) . . ? C28 N1 Ir1 115.5(2) . . ? C21 N1 H1 101(3) . . ? C28 N1 H1 123(3) . . ? Ir1 N1 H1 93(3) . . ? C2 C1 C8 124.7(4) . . ? C2 C1 Ir1 70.4(2) . . ? C8 C1 Ir1 115.7(3) . . ? C2 C1 H1A 113.1 . . ? C8 C1 H1A 113.1 . . ? Ir1 C1 H1A 113.1 . . ? C1 C2 C3 118.7(4) . . ? C1 C2 Ir1 71.0(2) . . ? C3 C2 Ir1 115.9(3) . . ? C1 C2 H2A 114.7 . . ? C3 C2 H2A 114.7 . . ? Ir1 C2 H2A 114.7 . . ? C4 C3 C2 113.0(4) . . ? C4 C3 H3A 109.0 . . ? C2 C3 H3A 109.0 . . ? C4 C3 H3B 109.0 . . ? C2 C3 H3B 109.0 . . ? H3A C3 H3B 107.8 . . ? C3 C4 C5 113.5(4) . . ? C3 C4 H4A 108.9 . . ? C5 C4 H4A 108.9 . . ? C3 C4 H4B 108.9 . . ? C5 C4 H4B 108.9 . . ? H4A C4 H4B 107.7 . . ? C6 C5 C4 123.9(4) . . ? C6 C5 Ir1 70.3(2) . . ? C4 C5 Ir1 112.8(3) . . ? C6 C5 H5A 114.1 . . ? C4 C5 H5A 114.1 . . ? Ir1 C5 H5A 114.1 . . ? C5 C6 C7 122.5(4) . . ? C5 C6 Ir1 72.2(2) . . ? C7 C6 Ir1 114.0(3) . . ? C5 C6 H6A 113.8 . . ? C7 C6 H6A 113.8 . . ? Ir1 C6 H6A 113.8 . . ? C6 C7 C8 114.5(4) . . ? C6 C7 H7A 108.6 . . ? C8 C7 H7A 108.6 . . ? C6 C7 H7B 108.6 . . ? C8 C7 H7B 108.6 . . ? H7A C7 H7B 107.6 . . ? C1 C8 C7 111.5(4) . . ? C1 C8 H8A 109.3 . . ? C7 C8 H8A 109.3 . . ? C1 C8 H8B 109.3 . . ? C7 C8 H8B 109.3 . . ? H8A C8 H8B 108.0 . . ? C10 C9 C14 118.4(3) . . ? C10 C9 P1 118.1(3) . . ? C14 C9 P1 123.5(3) . . ? C9 C10 C11 120.7(4) . . ? C9 C10 H10A 119.6 . . ? C11 C10 H10A 119.6 . . ? C12 C11 C10 120.0(4) . . ? C12 C11 H11A 120.0 . . ? C10 C11 H11A 120.0 . . ? C11 C12 C13 120.1(4) . . ? C11 C12 H12A 119.9 . . ? C13 C12 H12A 119.9 . . ? C14 C13 C12 119.3(4) . . ? C14 C13 H13A 120.4 . . ? C12 C13 H13A 120.4 . . ? C13 C14 C9 121.4(4) . . ? C13 C14 H14A 119.3 . . ? C9 C14 H14A 119.3 . . ? C16 C15 C20 119.2(3) . . ? C16 C15 P1 123.4(3) . . ? C20 C15 P1 117.2(3) . . ? C15 C16 C17 119.8(4) . . ? C15 C16 H16A 120.1 . . ? C17 C16 H16A 120.1 . . ? C18 C17 C16 120.3(4) . . ? C18 C17 H17A 119.8 . . ? C16 C17 H17A 119.8 . . ? C19 C18 C17 120.0(4) . . ? C19 C18 H18A 120.0 . . ? C17 C18 H18A 120.0 . . ? C18 C19 C20 120.1(4) . . ? C18 C19 H19A 120.0 . . ? C20 C19 H19A 120.0 . . ? C19 C20 C15 120.6(4) . . ? C19 C20 H20A 119.7 . . ? C15 C20 H20A 119.7 . . ? C26 C21 C22 120.3(4) . . ? C26 C21 N1 121.8(4) . . ? C22 C21 N1 117.9(3) . . ? C21 C22 C23 119.2(3) . . ? C21 C22 P1 117.4(3) . . ? C23 C22 P1 123.1(3) . . ? C24 C23 C22 120.8(4) . . ? C24 C23 H23A 119.6 . . ? C22 C23 H23A 119.6 . . ? C25 C24 C23 117.8(4) . . ? C25 C24 C27 121.5(4) . . ? C23 C24 C27 120.6(4) . . ? C24 C25 C26 122.2(4) . . ? C24 C25 H25A 118.9 . . ? C26 C25 H25A 118.9 . . ? C21 C26 C25 119.2(4) . . ? C21 C26 H26A 120.4 . . ? C25 C26 H26A 120.4 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 C33 119.0(4) . . ? C29 C28 N1 120.3(4) . . ? C33 C28 N1 120.6(3) . . ? C30 C29 C28 119.4(4) . . ? C30 C29 P2 123.5(3) . . ? C28 C29 P2 116.8(3) . . ? C29 C30 C31 122.2(4) . . ? C29 C30 H30A 118.9 . . ? C31 C30 H30A 118.9 . . ? C32 C31 C30 116.6(4) . . ? C32 C31 C34 122.0(4) . . ? C30 C31 C34 121.4(4) . . ? C33 C32 C31 122.6(4) . . ? C33 C32 H32A 118.7 . . ? C31 C32 H32A 118.7 . . ? C32 C33 C28 120.1(4) . . ? C32 C33 H33A 120.0 . . ? C28 C33 H33A 120.0 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C40 C35 C36 118.6(4) . . ? C40 C35 P2 120.3(3) . . ? C36 C35 P2 120.9(3) . . ? C37 C36 C35 119.8(4) . . ? C37 C36 H36A 120.1 . . ? C35 C36 H36A 120.1 . . ? C38 C37 C36 121.4(4) . . ? C38 C37 H37A 119.3 . . ? C36 C37 H37A 119.3 . . ? C37 C38 C39 119.2(4) . . ? C37 C38 H38A 120.4 . . ? C39 C38 H38A 120.4 . . ? C40 C39 C38 120.2(4) . . ? C40 C39 H39A 119.9 . . ? C38 C39 H39A 119.9 . . ? C39 C40 C35 120.8(4) . . ? C39 C40 H40A 119.6 . . ? C35 C40 H40A 119.6 . . ? C46 C41 C42 118.7(4) . . ? C46 C41 P2 119.3(3) . . ? C42 C41 P2 121.9(3) . . ? C43 C42 C41 119.9(4) . . ? C43 C42 H42A 120.0 . . ? C41 C42 H42A 120.0 . . ? C44 C43 C42 120.5(4) . . ? C44 C43 H43A 119.8 . . ? C42 C43 H43A 119.8 . . ? C45 C44 C43 120.1(4) . . ? C45 C44 H44A 119.9 . . ? C43 C44 H44A 119.9 . . ? C44 C45 C46 120.2(4) . . ? C44 C45 H45A 119.9 . . ? C46 C45 H45A 119.9 . . ? C45 C46 C41 120.4(4) . . ? C45 C46 H46A 119.8 . . ? C41 C46 H46A 119.8 . . ? C48 C47 C52 119.0(4) . . ? C48 C47 Cl2 122.0(4) . . ? C52 C47 Cl2 118.9(4) . . ? C47 C48 C49 121.1(4) . . ? C47 C48 Cl3 119.9(4) . . ? C49 C48 Cl3 118.9(4) . . ? C48 C49 C50 118.6(4) . . ? C48 C49 H49A 120.7 . . ? C50 C49 H49A 120.7 . . ? C51 C50 C49 121.1(5) . . ? C51 C50 H50A 119.5 . . ? C49 C50 H50A 119.5 . . ? C50 C51 C52 120.0(5) . . ? C50 C51 H51A 120.0 . . ? C52 C51 H51A 120.0 . . ? C51 C52 C47 120.0(4) . . ? C51 C52 H52A 120.0 . . ? C47 C52 H52A 120.0 . . ? C54A C53A C58A 120.1(6) . . ? C54A C53A Cl4A 121.2(5) . . ? C58A C53A Cl4A 118.6(4) . . ? C53A C54A C55A 120.0(5) . . ? C53A C54A Cl5A 121.4(4) . . ? C55A C54A Cl5A 118.6(4) . . ? C54A C55A C56A 118.5(5) . . ? C57A C56A C55A 120.3(5) . . ? C56A C57A C58A 120.1(5) . . ? C57A C58A C53A 120.9(5) . . ? C54B C53B C58B 120.7(16) . . ? C54B C53B Cl4B 121.2(16) . . ? C58B C53B Cl4B 115.4(14) . . ? C53B C54B C55B 120.0(16) . . ? C53B C54B Cl5B 123.1(17) . . ? C55B C54B Cl5B 115.5(16) . . ? C54B C55B C56B 115(2) . . ? C57B C56B C55B 121(2) . . ? C56B C57B C58B 118(2) . . ? C57B C58B C53B 117.5(16) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 Cl1 0.90(6) 2.31(5) 3.051(3) 139(4) . _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 68.57 _diffrn_measured_fraction_theta_full 0.947 _refine_diff_density_max 1.962 _refine_diff_density_min -1.426 _refine_diff_density_rms 0.161 # Attachment 'complex31.cif' data_ec20s _database_code_depnum_ccdc_archive 'CCDC 757517' #TrackingRef 'complex31.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H44 Ir N P2' _chemical_formula_sum 'C46 H44 Ir N P2' _chemical_formula_weight 864.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.230(2) _cell_length_b 10.663(2) _cell_length_c 17.091(3) _cell_angle_alpha 88.76(3) _cell_angle_beta 89.08(3) _cell_angle_gamma 73.16(3) _cell_volume 1783.9(6) _cell_formula_units_Z 2 _cell_measurement_temperature 144(2) _cell_measurement_reflns_used 9035 _cell_measurement_theta_min 6.535 _cell_measurement_theta_max 49.371 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.610 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 868 _exptl_absorpt_coefficient_mu 3.868 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5269 _exptl_absorpt_correction_T_max 0.7735 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 144(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_reflns_number 9035 _diffrn_reflns_av_R_equivalents 0.0185 _diffrn_reflns_av_sigmaI/netI 0.0345 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.27 _diffrn_reflns_theta_max 24.73 _reflns_number_total 5839 _reflns_number_gt 5179 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART v5.054d' _computing_cell_refinement 'Bruker SAINT v7.07' _computing_data_reduction 'Bruker SAINT v7.07' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0310P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5839 _refine_ls_number_parameters 453 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0317 _refine_ls_R_factor_gt 0.0253 _refine_ls_wR_factor_ref 0.0598 _refine_ls_wR_factor_gt 0.0581 _refine_ls_goodness_of_fit_ref 1.156 _refine_ls_restrained_S_all 1.156 _refine_ls_shift/su_max 0.009 _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 -0.017148(15) 0.246767(14) 0.312124(9) 0.01400(6) Uani 1 1 d . . . P1 P -0.04992(10) 0.34920(10) 0.19232(6) 0.0148(2) Uani 1 1 d . . . P2 P 0.21113(10) 0.11564(9) 0.31944(6) 0.0142(2) Uani 1 1 d . . . N1 N -0.0228(3) 0.0843(3) 0.24602(18) 0.0148(7) Uani 1 1 d . . . C1 C -0.2059(4) 0.2343(4) 0.3588(2) 0.0207(9) Uani 1 1 d . . . H1A H -0.2467 0.1758 0.3287 0.025 Uiso 1 1 calc R . . C2 C -0.0982(4) 0.1643(4) 0.4102(2) 0.0170(8) Uani 1 1 d . . . H2A H -0.0781 0.0668 0.4096 0.020 Uiso 1 1 calc R . . C3 C -0.0798(4) 0.2190(4) 0.4891(2) 0.0243(10) Uani 1 1 d . . . H3A H -0.0353 0.1453 0.5249 0.029 Uiso 1 1 calc R . . H3B H -0.1710 0.2635 0.5113 0.029 Uiso 1 1 calc R . . C4 C 0.0049(4) 0.3155(4) 0.4861(2) 0.0224(9) Uani 1 1 d . . . H4A H -0.0377 0.3890 0.5213 0.027 Uiso 1 1 calc R . . H4B H 0.0973 0.2709 0.5061 0.027 Uiso 1 1 calc R . . C5 C 0.0186(4) 0.3708(4) 0.4047(2) 0.0199(9) Uani 1 1 d . . . H5A H 0.1012 0.4018 0.3965 0.024 Uiso 1 1 calc R . . C6 C -0.0960(4) 0.4409(4) 0.3620(2) 0.0210(9) Uani 1 1 d . . . H6A H -0.0800 0.5129 0.3282 0.025 Uiso 1 1 calc R . . C7 C -0.2413(4) 0.4704(4) 0.3946(3) 0.0315(11) Uani 1 1 d . . . H7A H -0.2395 0.4838 0.4516 0.038 Uiso 1 1 calc R . . H7B H -0.2977 0.5533 0.3705 0.038 Uiso 1 1 calc R . . C8 C -0.3081(4) 0.3637(4) 0.3803(3) 0.0328(11) Uani 1 1 d . . . H8A H -0.3748 0.3924 0.3374 0.039 Uiso 1 1 calc R . . H8B H -0.3589 0.3505 0.4280 0.039 Uiso 1 1 calc R . . C9 C 0.3453(4) 0.1053(4) 0.2449(2) 0.0165(8) Uani 1 1 d . . . C10 C 0.3054(4) 0.0978(4) 0.1678(2) 0.0184(9) Uani 1 1 d . . . H10A H 0.2142 0.0987 0.1573 0.022 Uiso 1 1 calc R . . C11 C 0.3976(4) 0.0889(4) 0.1064(2) 0.0219(9) Uani 1 1 d . . . H11A H 0.3701 0.0822 0.0542 0.026 Uiso 1 1 calc R . . C12 C 0.5287(4) 0.0899(4) 0.1212(3) 0.0254(10) Uani 1 1 d . . . H12A H 0.5915 0.0854 0.0791 0.030 Uiso 1 1 calc R . . C13 C 0.5698(4) 0.0975(4) 0.1973(3) 0.0259(10) Uani 1 1 d . . . H13A H 0.6608 0.0981 0.2072 0.031 Uiso 1 1 calc R . . C14 C 0.4790(4) 0.1042(4) 0.2592(2) 0.0217(9) Uani 1 1 d . . . H14A H 0.5081 0.1081 0.3114 0.026 Uiso 1 1 calc R . . C15 C 0.2933(4) 0.1154(4) 0.4133(2) 0.0167(8) Uani 1 1 d . . . C16 C 0.3549(4) 0.2128(4) 0.4279(2) 0.0201(9) Uani 1 1 d . . . H16A H 0.3664 0.2697 0.3865 0.024 Uiso 1 1 calc R . . C17 C 0.3999(4) 0.2280(4) 0.5024(2) 0.0242(10) Uani 1 1 d . . . H17A H 0.4444 0.2930 0.5115 0.029 Uiso 1 1 calc R . . C18 C 0.3795(4) 0.1479(4) 0.5634(2) 0.0249(10) Uani 1 1 d . . . H18A H 0.4077 0.1597 0.6147 0.030 Uiso 1 1 calc R . . C19 C 0.3184(4) 0.0511(4) 0.5496(2) 0.0222(9) Uani 1 1 d . . . H19A H 0.3063 -0.0049 0.5914 0.027 Uiso 1 1 calc R . . C20 C 0.2744(4) 0.0349(4) 0.4749(2) 0.0194(9) Uani 1 1 d . . . H20A H 0.2313 -0.0312 0.4660 0.023 Uiso 1 1 calc R . . C21 C 0.1831(4) -0.0447(4) 0.3092(2) 0.0156(8) Uani 1 1 d . . . C22 C 0.2721(4) -0.1638(4) 0.3326(2) 0.0177(8) Uani 1 1 d . . . H22A H 0.3587 -0.1657 0.3527 0.021 Uiso 1 1 calc R . . C23 C 0.2386(4) -0.2797(4) 0.3275(2) 0.0179(9) Uani 1 1 d . . . C24 C 0.1104(4) -0.2730(4) 0.2987(2) 0.0197(9) Uani 1 1 d . . . H24A H 0.0832 -0.3508 0.2969 0.024 Uiso 1 1 calc R . . C25 C 0.0211(4) -0.1557(4) 0.2725(2) 0.0186(9) Uani 1 1 d . . . H25A H -0.0659 -0.1543 0.2533 0.022 Uiso 1 1 calc R . . C26 C 0.0584(4) -0.0388(4) 0.2742(2) 0.0143(8) Uani 1 1 d . . . C27 C 0.3350(4) -0.4082(4) 0.3560(3) 0.0261(10) Uani 1 1 d . . . H27A H 0.4205 -0.3938 0.3730 0.039 Uiso 1 1 calc R . . H27B H 0.3541 -0.4712 0.3134 0.039 Uiso 1 1 calc R . . H27C H 0.2927 -0.4427 0.4001 0.039 Uiso 1 1 calc R . . C28 C -0.0992(4) 0.2306(4) 0.1354(2) 0.0165(8) Uani 1 1 d . . . C29 C -0.0666(4) 0.1023(4) 0.1692(2) 0.0150(8) Uani 1 1 d . . . C30 C -0.0810(4) 0.0034(4) 0.1199(2) 0.0162(8) Uani 1 1 d . . . H30A H -0.0514 -0.0854 0.1375 0.019 Uiso 1 1 calc R . . C31 C -0.1372(4) 0.0326(4) 0.0465(2) 0.0180(9) Uani 1 1 d . . . H31A H -0.1456 -0.0372 0.0152 0.022 Uiso 1 1 calc R . . C32 C -0.1824(4) 0.1608(4) 0.0163(2) 0.0196(9) Uani 1 1 d . . . C33 C -0.1585(4) 0.2576(4) 0.0615(2) 0.0183(9) Uani 1 1 d . . . H33A H -0.1830 0.3451 0.0417 0.022 Uiso 1 1 calc R . . C34 C -0.2526(4) 0.1917(4) -0.0617(2) 0.0281(10) Uani 1 1 d . . . H34A H -0.3476 0.1904 -0.0559 0.042 Uiso 1 1 calc R . . H34B H -0.2053 0.1260 -0.0997 0.042 Uiso 1 1 calc R . . H34C H -0.2503 0.2787 -0.0801 0.042 Uiso 1 1 calc R . . C35 C -0.1868(4) 0.5033(4) 0.1802(2) 0.0173(8) Uani 1 1 d . . . C36 C -0.3223(4) 0.5013(4) 0.1825(2) 0.0210(9) Uani 1 1 d . . . H36A H -0.3429 0.4200 0.1857 0.025 Uiso 1 1 calc R . . C37 C -0.4278(4) 0.6182(4) 0.1803(3) 0.0254(10) Uani 1 1 d . . . H37A H -0.5200 0.6162 0.1808 0.030 Uiso 1 1 calc R . . C38 C -0.3991(4) 0.7371(4) 0.1772(3) 0.0267(10) Uani 1 1 d . . . H38A H -0.4713 0.8167 0.1765 0.032 Uiso 1 1 calc R . . C39 C -0.2655(4) 0.7393(4) 0.1753(3) 0.0267(10) Uani 1 1 d . . . H39A H -0.2457 0.8210 0.1735 0.032 Uiso 1 1 calc R . . C40 C -0.1589(4) 0.6235(4) 0.1761(2) 0.0235(9) Uani 1 1 d . . . H40A H -0.0670 0.6265 0.1738 0.028 Uiso 1 1 calc R . . C41 C 0.0946(4) 0.3863(4) 0.1414(2) 0.0171(9) Uani 1 1 d . . . C42 C 0.1167(4) 0.3806(4) 0.0614(2) 0.0258(10) Uani 1 1 d . . . H42A H 0.0500 0.3638 0.0284 0.031 Uiso 1 1 calc R . . C43 C 0.2348(4) 0.3988(4) 0.0284(2) 0.0266(10) Uani 1 1 d . . . H43A H 0.2481 0.3944 -0.0267 0.032 Uiso 1 1 calc R . . C44 C 0.3327(5) 0.4232(4) 0.0751(3) 0.0292(10) Uani 1 1 d . . . H44A H 0.4140 0.4348 0.0526 0.035 Uiso 1 1 calc R . . C45 C 0.3108(4) 0.4305(4) 0.1553(3) 0.0264(10) Uani 1 1 d . . . H45A H 0.3771 0.4487 0.1880 0.032 Uiso 1 1 calc R . . C46 C 0.1938(4) 0.4118(4) 0.1881(2) 0.0200(9) Uani 1 1 d . . . H46A H 0.1808 0.4163 0.2432 0.024 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.01479(9) 0.01254(9) 0.01469(9) -0.00021(6) -0.00079(6) -0.00394(6) P1 0.0166(5) 0.0125(5) 0.0152(5) 0.0013(4) -0.0023(4) -0.0043(4) P2 0.0137(5) 0.0133(5) 0.0155(5) -0.0003(4) -0.0014(4) -0.0039(4) N1 0.0203(17) 0.0119(16) 0.0127(17) 0.0002(14) -0.0025(13) -0.0053(14) C1 0.015(2) 0.028(2) 0.021(2) -0.0011(19) 0.0038(17) -0.0087(18) C2 0.018(2) 0.017(2) 0.016(2) -0.0012(17) 0.0024(16) -0.0068(17) C3 0.024(2) 0.026(2) 0.021(2) 0.0030(19) 0.0035(18) -0.0063(19) C4 0.027(2) 0.020(2) 0.018(2) -0.0038(18) -0.0047(18) -0.0037(18) C5 0.023(2) 0.015(2) 0.023(2) -0.0052(18) -0.0008(18) -0.0068(17) C6 0.030(2) 0.014(2) 0.018(2) -0.0048(17) 0.0040(18) -0.0052(18) C7 0.028(3) 0.026(2) 0.032(3) -0.009(2) -0.003(2) 0.006(2) C8 0.025(2) 0.032(3) 0.033(3) 0.010(2) 0.007(2) 0.005(2) C9 0.015(2) 0.0107(19) 0.024(2) -0.0005(17) 0.0011(17) -0.0037(16) C10 0.014(2) 0.017(2) 0.025(2) -0.0001(18) -0.0009(17) -0.0060(16) C11 0.026(2) 0.019(2) 0.019(2) -0.0006(18) -0.0003(18) -0.0056(18) C12 0.022(2) 0.024(2) 0.028(2) -0.002(2) 0.0090(19) -0.0041(18) C13 0.014(2) 0.027(2) 0.036(3) -0.003(2) -0.0008(19) -0.0052(18) C14 0.019(2) 0.022(2) 0.023(2) -0.0020(19) 0.0005(17) -0.0058(18) C15 0.017(2) 0.017(2) 0.016(2) -0.0015(17) -0.0039(16) -0.0047(16) C16 0.017(2) 0.020(2) 0.022(2) -0.0020(18) 0.0008(17) -0.0043(17) C17 0.021(2) 0.023(2) 0.030(3) -0.005(2) -0.0015(19) -0.0082(18) C18 0.020(2) 0.032(2) 0.021(2) -0.005(2) -0.0053(18) -0.0046(19) C19 0.021(2) 0.027(2) 0.016(2) 0.0058(18) -0.0038(17) -0.0035(18) C20 0.017(2) 0.018(2) 0.024(2) -0.0014(18) -0.0017(17) -0.0050(17) C21 0.016(2) 0.016(2) 0.015(2) -0.0001(17) 0.0019(16) -0.0041(16) C22 0.015(2) 0.022(2) 0.016(2) 0.0001(17) -0.0022(16) -0.0058(17) C23 0.023(2) 0.014(2) 0.015(2) 0.0003(17) 0.0007(17) -0.0028(17) C24 0.027(2) 0.015(2) 0.019(2) -0.0024(17) 0.0001(18) -0.0098(18) C25 0.019(2) 0.019(2) 0.020(2) -0.0008(18) -0.0037(17) -0.0075(17) C26 0.016(2) 0.0136(19) 0.0130(19) -0.0041(16) 0.0014(16) -0.0042(16) C27 0.031(2) 0.018(2) 0.026(2) 0.0006(19) -0.0022(19) -0.0001(19) C28 0.0127(19) 0.018(2) 0.018(2) -0.0009(17) -0.0018(16) -0.0047(16) C29 0.0077(18) 0.019(2) 0.018(2) -0.0009(17) 0.0017(15) -0.0035(16) C30 0.013(2) 0.019(2) 0.017(2) -0.0016(17) 0.0003(15) -0.0064(16) C31 0.0128(19) 0.020(2) 0.022(2) -0.0065(18) -0.0009(16) -0.0054(16) C32 0.016(2) 0.025(2) 0.017(2) -0.0008(18) 0.0010(16) -0.0059(17) C33 0.016(2) 0.019(2) 0.019(2) 0.0031(17) -0.0023(16) -0.0034(17) C34 0.031(3) 0.029(2) 0.024(2) 0.000(2) -0.0104(19) -0.009(2) C35 0.022(2) 0.017(2) 0.011(2) -0.0010(17) -0.0045(16) -0.0034(17) C36 0.022(2) 0.017(2) 0.026(2) 0.0023(19) -0.0005(18) -0.0087(18) C37 0.019(2) 0.025(2) 0.033(3) 0.005(2) -0.0042(18) -0.0062(18) C38 0.023(2) 0.019(2) 0.034(3) 0.003(2) -0.0078(19) 0.0002(18) C39 0.027(2) 0.015(2) 0.040(3) -0.001(2) -0.009(2) -0.0094(18) C40 0.021(2) 0.023(2) 0.028(2) 0.0029(19) -0.0079(18) -0.0090(18) C41 0.021(2) 0.013(2) 0.017(2) 0.0031(17) 0.0011(17) -0.0042(17) C42 0.027(2) 0.028(2) 0.022(2) 0.008(2) -0.0043(18) -0.008(2) C43 0.030(2) 0.028(2) 0.019(2) 0.008(2) 0.0015(19) -0.005(2) C44 0.030(3) 0.025(2) 0.035(3) 0.005(2) 0.006(2) -0.012(2) C45 0.027(2) 0.022(2) 0.034(3) 0.000(2) -0.002(2) -0.0135(19) C46 0.026(2) 0.015(2) 0.020(2) 0.0005(18) 0.0002(18) -0.0089(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 Ir1 N1 2.104(3) . ? Ir1 C1 2.116(4) . ? Ir1 C2 2.142(4) . ? Ir1 C6 2.179(4) . ? Ir1 C5 2.185(4) . ? Ir1 P1 2.2827(12) . ? Ir1 P2 2.3525(13) . ? P1 C28 1.799(4) . ? P1 C35 1.835(4) . ? P1 C41 1.839(4) . ? P2 C15 1.822(4) . ? P2 C21 1.826(4) . ? P2 C9 1.839(4) . ? N1 C29 1.385(5) . ? N1 C26 1.414(5) . ? C1 C2 1.439(6) . ? C1 C8 1.518(6) . ? C1 H1A 1.0000 . ? C2 C3 1.515(5) . ? C2 H2A 1.0000 . ? C3 C4 1.525(6) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.519(6) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.400(6) . ? C5 H5A 1.0000 . ? C6 C7 1.526(6) . ? C6 H6A 1.0000 . ? C7 C8 1.513(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C14 1.390(5) . ? C9 C10 1.397(5) . ? C10 C11 1.386(5) . ? C10 H10A 0.9500 . ? C11 C12 1.372(6) . ? C11 H11A 0.9500 . ? C12 C13 1.384(6) . ? C12 H12A 0.9500 . ? C13 C14 1.386(6) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? C15 C20 1.391(6) . ? C15 C16 1.391(5) . ? C16 C17 1.389(6) . ? C16 H16A 0.9500 . ? C17 C18 1.384(6) . ? C17 H17A 0.9500 . ? C18 C19 1.379(6) . ? C18 H18A 0.9500 . ? C19 C20 1.392(5) . ? C19 H19A 0.9500 . ? C20 H20A 0.9500 . ? C21 C22 1.386(5) . ? C21 C26 1.403(5) . ? C22 C23 1.380(5) . ? C22 H22A 0.9500 . ? C23 C24 1.390(6) . ? C23 C27 1.513(5) . ? C24 C25 1.388(5) . ? C24 H24A 0.9500 . ? C25 C26 1.405(5) . ? C25 H25A 0.9500 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C33 1.398(5) . ? C28 C29 1.423(5) . ? C29 C30 1.405(5) . ? C30 C31 1.380(5) . ? C30 H30A 0.9500 . ? C31 C32 1.400(6) . ? C31 H31A 0.9500 . ? C32 C33 1.381(6) . ? C32 C34 1.508(5) . ? C33 H33A 0.9500 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C40 1.392(6) . ? C35 C36 1.392(5) . ? C36 C37 1.392(6) . ? C36 H36A 0.9500 . ? C37 C38 1.381(6) . ? C37 H37A 0.9500 . ? C38 C39 1.374(6) . ? C38 H38A 0.9500 . ? C39 C40 1.390(6) . ? C39 H39A 0.9500 . ? C40 H40A 0.9500 . ? C41 C42 1.383(6) . ? C41 C46 1.392(6) . ? C42 C43 1.387(6) . ? C42 H42A 0.9500 . ? C43 C44 1.375(6) . ? C43 H43A 0.9500 . ? C44 C45 1.386(6) . ? C44 H44A 0.9500 . ? C45 C46 1.378(6) . ? C45 H45A 0.9500 . ? C46 H46A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ir1 C1 84.58(14) . . ? N1 Ir1 C2 88.98(13) . . ? C1 Ir1 C2 39.51(15) . . ? N1 Ir1 C6 156.41(14) . . ? C1 Ir1 C6 79.60(16) . . ? C2 Ir1 C6 89.85(15) . . ? N1 Ir1 C5 163.37(13) . . ? C1 Ir1 C5 94.95(16) . . ? C2 Ir1 C5 80.36(15) . . ? C6 Ir1 C5 37.42(15) . . ? N1 Ir1 P1 82.25(9) . . ? C1 Ir1 P1 109.91(12) . . ? C2 Ir1 P1 149.14(11) . . ? C6 Ir1 P1 86.79(11) . . ? C5 Ir1 P1 113.29(11) . . ? N1 Ir1 P2 78.54(9) . . ? C1 Ir1 P2 135.17(11) . . ? C2 Ir1 P2 98.53(11) . . ? C6 Ir1 P2 124.90(11) . . ? C5 Ir1 P2 90.39(11) . . ? P1 Ir1 P2 108.50(5) . . ? C28 P1 C35 105.87(18) . . ? C28 P1 C41 107.57(18) . . ? C35 P1 C41 102.23(18) . . ? C28 P1 Ir1 101.19(13) . . ? C35 P1 Ir1 119.39(13) . . ? C41 P1 Ir1 119.49(13) . . ? C15 P2 C21 107.53(18) . . ? C15 P2 C9 105.63(18) . . ? C21 P2 C9 100.37(17) . . ? C15 P2 Ir1 115.38(13) . . ? C21 P2 Ir1 98.72(13) . . ? C9 P2 Ir1 126.34(13) . . ? C29 N1 C26 121.4(3) . . ? C29 N1 Ir1 119.9(2) . . ? C26 N1 Ir1 115.6(2) . . ? C2 C1 C8 122.7(4) . . ? C2 C1 Ir1 71.2(2) . . ? C8 C1 Ir1 115.7(3) . . ? C2 C1 H1A 113.5 . . ? C8 C1 H1A 113.5 . . ? Ir1 C1 H1A 113.5 . . ? C1 C2 C3 120.8(4) . . ? C1 C2 Ir1 69.3(2) . . ? C3 C2 Ir1 115.3(3) . . ? C1 C2 H2A 114.6 . . ? C3 C2 H2A 114.6 . . ? Ir1 C2 H2A 114.6 . . ? C2 C3 C4 114.1(3) . . ? C2 C3 H3A 108.7 . . ? C4 C3 H3A 108.7 . . ? C2 C3 H3B 108.7 . . ? C4 C3 H3B 108.7 . . ? H3A C3 H3B 107.6 . . ? C5 C4 C3 113.9(3) . . ? C5 C4 H4A 108.8 . . ? C3 C4 H4A 108.8 . . ? C5 C4 H4B 108.8 . . ? C3 C4 H4B 108.8 . . ? H4A C4 H4B 107.7 . . ? C6 C5 C4 121.6(4) . . ? C6 C5 Ir1 71.1(2) . . ? C4 C5 Ir1 112.7(3) . . ? C6 C5 H5A 114.7 . . ? C4 C5 H5A 114.7 . . ? Ir1 C5 H5A 114.7 . . ? C5 C6 C7 122.7(4) . . ? C5 C6 Ir1 71.5(2) . . ? C7 C6 Ir1 114.2(3) . . ? C5 C6 H6A 113.9 . . ? C7 C6 H6A 113.9 . . ? Ir1 C6 H6A 113.9 . . ? C8 C7 C6 113.9(3) . . ? C8 C7 H7A 108.8 . . ? C6 C7 H7A 108.8 . . ? C8 C7 H7B 108.8 . . ? C6 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? C7 C8 C1 112.8(4) . . ? C7 C8 H8A 109.0 . . ? C1 C8 H8A 109.0 . . ? C7 C8 H8B 109.0 . . ? C1 C8 H8B 109.0 . . ? H8A C8 H8B 107.8 . . ? C14 C9 C10 119.0(3) . . ? C14 C9 P2 125.9(3) . . ? C10 C9 P2 115.2(3) . . ? C11 C10 C9 120.6(4) . . ? C11 C10 H10A 119.7 . . ? C9 C10 H10A 119.7 . . ? C12 C11 C10 119.8(4) . . ? C12 C11 H11A 120.1 . . ? C10 C11 H11A 120.1 . . ? C11 C12 C13 120.3(4) . . ? C11 C12 H12A 119.8 . . ? C13 C12 H12A 119.8 . . ? C12 C13 C14 120.3(4) . . ? C12 C13 H13A 119.8 . . ? C14 C13 H13A 119.8 . . ? C13 C14 C9 120.0(4) . . ? C13 C14 H14A 120.0 . . ? C9 C14 H14A 120.0 . . ? C20 C15 C16 118.9(4) . . ? C20 C15 P2 120.9(3) . . ? C16 C15 P2 119.2(3) . . ? C17 C16 C15 120.8(4) . . ? C17 C16 H16A 119.6 . . ? C15 C16 H16A 119.6 . . ? C18 C17 C16 119.7(4) . . ? C18 C17 H17A 120.1 . . ? C16 C17 H17A 120.1 . . ? C19 C18 C17 120.0(4) . . ? C19 C18 H18A 120.0 . . ? C17 C18 H18A 120.0 . . ? C18 C19 C20 120.3(4) . . ? C18 C19 H19A 119.8 . . ? C20 C19 H19A 119.8 . . ? C15 C20 C19 120.2(4) . . ? C15 C20 H20A 119.9 . . ? C19 C20 H20A 119.9 . . ? C22 C21 C26 120.8(4) . . ? C22 C21 P2 125.8(3) . . ? C26 C21 P2 113.4(3) . . ? C23 C22 C21 121.9(4) . . ? C23 C22 H22A 119.0 . . ? C21 C22 H22A 119.0 . . ? C22 C23 C24 117.4(4) . . ? C22 C23 C27 121.2(4) . . ? C24 C23 C27 121.3(4) . . ? C25 C24 C23 121.8(4) . . ? C25 C24 H24A 119.1 . . ? C23 C24 H24A 119.1 . . ? C24 C25 C26 120.6(4) . . ? C24 C25 H25A 119.7 . . ? C26 C25 H25A 119.7 . . ? C21 C26 C25 117.1(3) . . ? C21 C26 N1 118.0(3) . . ? C25 C26 N1 124.8(3) . . ? C23 C27 H27A 109.5 . . ? C23 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C23 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C33 C28 C29 121.1(4) . . ? C33 C28 P1 123.8(3) . . ? C29 C28 P1 115.0(3) . . ? N1 C29 C30 125.6(3) . . ? N1 C29 C28 118.6(3) . . ? C30 C29 C28 115.8(3) . . ? C31 C30 C29 121.4(4) . . ? C31 C30 H30A 119.3 . . ? C29 C30 H30A 119.3 . . ? C30 C31 C32 122.7(4) . . ? C30 C31 H31A 118.6 . . ? C32 C31 H31A 118.6 . . ? C33 C32 C31 116.4(4) . . ? C33 C32 C34 121.7(4) . . ? C31 C32 C34 121.9(4) . . ? C32 C33 C28 122.0(4) . . ? C32 C33 H33A 119.0 . . ? C28 C33 H33A 119.0 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C40 C35 C36 119.0(4) . . ? C40 C35 P1 121.4(3) . . ? C36 C35 P1 119.4(3) . . ? C37 C36 C35 120.2(4) . . ? C37 C36 H36A 119.9 . . ? C35 C36 H36A 119.9 . . ? C38 C37 C36 120.4(4) . . ? C38 C37 H37A 119.8 . . ? C36 C37 H37A 119.8 . . ? C39 C38 C37 119.5(4) . . ? C39 C38 H38A 120.3 . . ? C37 C38 H38A 120.3 . . ? C38 C39 C40 120.9(4) . . ? C38 C39 H39A 119.6 . . ? C40 C39 H39A 119.6 . . ? C39 C40 C35 120.0(4) . . ? C39 C40 H40A 120.0 . . ? C35 C40 H40A 120.0 . . ? C42 C41 C46 118.1(4) . . ? C42 C41 P1 124.9(3) . . ? C46 C41 P1 116.8(3) . . ? C41 C42 C43 121.1(4) . . ? C41 C42 H42A 119.4 . . ? C43 C42 H42A 119.4 . . ? C44 C43 C42 120.4(4) . . ? C44 C43 H43A 119.8 . . ? C42 C43 H43A 119.8 . . ? C43 C44 C45 119.0(4) . . ? C43 C44 H44A 120.5 . . ? C45 C44 H44A 120.5 . . ? C46 C45 C44 120.6(4) . . ? C46 C45 H45A 119.7 . . ? C44 C45 H45A 119.7 . . ? C45 C46 C41 120.8(4) . . ? C45 C46 H46A 119.6 . . ? C41 C46 H46A 119.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Ir1 P1 C28 13.92(15) . . . . ? C1 Ir1 P1 C28 -67.42(18) . . . . ? C2 Ir1 P1 C28 -60.8(2) . . . . ? C6 Ir1 P1 C28 -145.14(17) . . . . ? C5 Ir1 P1 C28 -172.24(17) . . . . ? P2 Ir1 P1 C28 89.02(13) . . . . ? N1 Ir1 P1 C35 129.47(17) . . . . ? C1 Ir1 P1 C35 48.14(19) . . . . ? C2 Ir1 P1 C35 54.7(3) . . . . ? C6 Ir1 P1 C35 -29.59(18) . . . . ? C5 Ir1 P1 C35 -56.69(19) . . . . ? P2 Ir1 P1 C35 -155.42(15) . . . . ? N1 Ir1 P1 C41 -103.82(17) . . . . ? C1 Ir1 P1 C41 174.85(19) . . . . ? C2 Ir1 P1 C41 -178.6(2) . . . . ? C6 Ir1 P1 C41 97.12(18) . . . . ? C5 Ir1 P1 C41 70.02(19) . . . . ? P2 Ir1 P1 C41 -28.72(15) . . . . ? N1 Ir1 P2 C15 -142.19(17) . . . . ? C1 Ir1 P2 C15 -72.1(2) . . . . ? C2 Ir1 P2 C15 -54.99(18) . . . . ? C6 Ir1 P2 C15 40.8(2) . . . . ? C5 Ir1 P2 C15 25.32(18) . . . . ? P1 Ir1 P2 C15 140.11(14) . . . . ? N1 Ir1 P2 C21 -27.98(15) . . . . ? C1 Ir1 P2 C21 42.1(2) . . . . ? C2 Ir1 P2 C21 59.22(16) . . . . ? C6 Ir1 P2 C21 155.04(18) . . . . ? C5 Ir1 P2 C21 139.53(16) . . . . ? P1 Ir1 P2 C21 -105.68(13) . . . . ? N1 Ir1 P2 C9 81.83(18) . . . . ? C1 Ir1 P2 C9 151.9(2) . . . . ? C2 Ir1 P2 C9 169.03(19) . . . . ? C6 Ir1 P2 C9 -95.2(2) . . . . ? C5 Ir1 P2 C9 -110.66(19) . . . . ? P1 Ir1 P2 C9 4.13(16) . . . . ? C1 Ir1 N1 C29 99.0(3) . . . . ? C2 Ir1 N1 C29 138.3(3) . . . . ? C6 Ir1 N1 C29 51.0(5) . . . . ? C5 Ir1 N1 C29 -171.9(4) . . . . ? P1 Ir1 N1 C29 -12.0(2) . . . . ? P2 Ir1 N1 C29 -122.8(3) . . . . ? C1 Ir1 N1 C26 -100.6(3) . . . . ? C2 Ir1 N1 C26 -61.3(3) . . . . ? C6 Ir1 N1 C26 -148.5(3) . . . . ? C5 Ir1 N1 C26 -11.4(6) . . . . ? P1 Ir1 N1 C26 148.4(3) . . . . ? P2 Ir1 N1 C26 37.7(2) . . . . ? N1 Ir1 C1 C2 95.0(2) . . . . ? C6 Ir1 C1 C2 -102.6(2) . . . . ? C5 Ir1 C1 C2 -68.3(2) . . . . ? P1 Ir1 C1 C2 174.70(19) . . . . ? P2 Ir1 C1 C2 27.2(3) . . . . ? N1 Ir1 C1 C8 -147.0(3) . . . . ? C2 Ir1 C1 C8 118.0(4) . . . . ? C6 Ir1 C1 C8 15.4(3) . . . . ? C5 Ir1 C1 C8 49.7(3) . . . . ? P1 Ir1 C1 C8 -67.3(3) . . . . ? P2 Ir1 C1 C8 145.2(3) . . . . ? C8 C1 C2 C3 -1.2(6) . . . . ? Ir1 C1 C2 C3 107.8(3) . . . . ? C8 C1 C2 Ir1 -109.0(4) . . . . ? N1 Ir1 C2 C1 -82.7(2) . . . . ? C6 Ir1 C2 C1 73.7(3) . . . . ? C5 Ir1 C2 C1 110.1(2) . . . . ? P1 Ir1 C2 C1 -9.7(4) . . . . ? P2 Ir1 C2 C1 -161.0(2) . . . . ? N1 Ir1 C2 C3 162.0(3) . . . . ? C1 Ir1 C2 C3 -115.3(4) . . . . ? C6 Ir1 C2 C3 -41.6(3) . . . . ? C5 Ir1 C2 C3 -5.2(3) . . . . ? P1 Ir1 C2 C3 -125.0(3) . . . . ? P2 Ir1 C2 C3 83.8(3) . . . . ? C1 C2 C3 C4 -85.2(4) . . . . ? Ir1 C2 C3 C4 -5.2(5) . . . . ? C2 C3 C4 C5 17.7(5) . . . . ? C3 C4 C5 C6 59.3(5) . . . . ? C3 C4 C5 Ir1 -21.7(4) . . . . ? N1 Ir1 C5 C6 -153.4(4) . . . . ? C1 Ir1 C5 C6 -65.7(3) . . . . ? C2 Ir1 C5 C6 -102.6(3) . . . . ? P1 Ir1 C5 C6 48.5(2) . . . . ? P2 Ir1 C5 C6 158.9(2) . . . . ? N1 Ir1 C5 C4 -36.2(6) . . . . ? C1 Ir1 C5 C4 51.5(3) . . . . ? C2 Ir1 C5 C4 14.6(3) . . . . ? C6 Ir1 C5 C4 117.2(4) . . . . ? P1 Ir1 C5 C4 165.6(2) . . . . ? P2 Ir1 C5 C4 -84.0(3) . . . . ? C4 C5 C6 C7 1.9(6) . . . . ? Ir1 C5 C6 C7 107.4(4) . . . . ? C4 C5 C6 Ir1 -105.5(4) . . . . ? N1 Ir1 C6 C5 161.3(3) . . . . ? C1 Ir1 C6 C5 112.6(3) . . . . ? C2 Ir1 C6 C5 74.2(2) . . . . ? P1 Ir1 C6 C5 -136.5(2) . . . . ? P2 Ir1 C6 C5 -26.1(3) . . . . ? N1 Ir1 C6 C7 43.0(5) . . . . ? C1 Ir1 C6 C7 -5.7(3) . . . . ? C2 Ir1 C6 C7 -44.1(3) . . . . ? C5 Ir1 C6 C7 -118.3(4) . . . . ? P1 Ir1 C6 C7 105.2(3) . . . . ? P2 Ir1 C6 C7 -144.4(3) . . . . ? C5 C6 C7 C8 -87.5(5) . . . . ? Ir1 C6 C7 C8 -4.7(5) . . . . ? C6 C7 C8 C1 17.1(6) . . . . ? C2 C1 C8 C7 60.9(5) . . . . ? Ir1 C1 C8 C7 -22.5(5) . . . . ? C15 P2 C9 C14 -2.8(4) . . . . ? C21 P2 C9 C14 -114.5(4) . . . . ? Ir1 P2 C9 C14 136.5(3) . . . . ? C15 P2 C9 C10 177.1(3) . . . . ? C21 P2 C9 C10 65.4(3) . . . . ? Ir1 P2 C9 C10 -43.6(3) . . . . ? C14 C9 C10 C11 0.2(6) . . . . ? P2 C9 C10 C11 -179.7(3) . . . . ? C9 C10 C11 C12 -1.2(6) . . . . ? C10 C11 C12 C13 1.1(6) . . . . ? C11 C12 C13 C14 0.0(6) . . . . ? C12 C13 C14 C9 -0.9(6) . . . . ? C10 C9 C14 C13 0.8(6) . . . . ? P2 C9 C14 C13 -179.3(3) . . . . ? C21 P2 C15 C20 -26.6(4) . . . . ? C9 P2 C15 C20 -133.1(3) . . . . ? Ir1 P2 C15 C20 82.4(3) . . . . ? C21 P2 C15 C16 165.0(3) . . . . ? C9 P2 C15 C16 58.5(3) . . . . ? Ir1 P2 C15 C16 -86.0(3) . . . . ? C20 C15 C16 C17 1.4(6) . . . . ? P2 C15 C16 C17 170.1(3) . . . . ? C15 C16 C17 C18 -1.9(6) . . . . ? C16 C17 C18 C19 1.9(6) . . . . ? C17 C18 C19 C20 -1.3(6) . . . . ? C16 C15 C20 C19 -0.8(6) . . . . ? P2 C15 C20 C19 -169.3(3) . . . . ? C18 C19 C20 C15 0.8(6) . . . . ? C15 P2 C21 C22 -38.5(4) . . . . ? C9 P2 C21 C22 71.7(4) . . . . ? Ir1 P2 C21 C22 -158.7(3) . . . . ? C15 P2 C21 C26 141.5(3) . . . . ? C9 P2 C21 C26 -108.3(3) . . . . ? Ir1 P2 C21 C26 21.3(3) . . . . ? C26 C21 C22 C23 -4.5(6) . . . . ? P2 C21 C22 C23 175.5(3) . . . . ? C21 C22 C23 C24 -0.7(6) . . . . ? C21 C22 C23 C27 -177.8(4) . . . . ? C22 C23 C24 C25 2.9(6) . . . . ? C27 C23 C24 C25 179.9(4) . . . . ? C23 C24 C25 C26 0.2(6) . . . . ? C22 C21 C26 C25 7.4(5) . . . . ? P2 C21 C26 C25 -172.6(3) . . . . ? C22 C21 C26 N1 -175.0(3) . . . . ? P2 C21 C26 N1 5.0(4) . . . . ? C24 C25 C26 C21 -5.2(6) . . . . ? C24 C25 C26 N1 177.3(3) . . . . ? C29 N1 C26 C21 125.1(4) . . . . ? Ir1 N1 C26 C21 -35.0(4) . . . . ? C29 N1 C26 C25 -57.5(5) . . . . ? Ir1 N1 C26 C25 142.4(3) . . . . ? C35 P1 C28 C33 40.8(4) . . . . ? C41 P1 C28 C33 -67.9(4) . . . . ? Ir1 P1 C28 C33 166.0(3) . . . . ? C35 P1 C28 C29 -142.5(3) . . . . ? C41 P1 C28 C29 108.7(3) . . . . ? Ir1 P1 C28 C29 -17.4(3) . . . . ? C26 N1 C29 C30 23.7(5) . . . . ? Ir1 N1 C29 C30 -177.0(3) . . . . ? C26 N1 C29 C28 -155.6(3) . . . . ? Ir1 N1 C29 C28 3.7(4) . . . . ? C33 C28 C29 N1 -172.7(3) . . . . ? P1 C28 C29 N1 10.6(4) . . . . ? C33 C28 C29 C30 8.0(5) . . . . ? P1 C28 C29 C30 -168.8(3) . . . . ? N1 C29 C30 C31 174.0(3) . . . . ? C28 C29 C30 C31 -6.7(5) . . . . ? C29 C30 C31 C32 0.4(6) . . . . ? C30 C31 C32 C33 4.8(6) . . . . ? C30 C31 C32 C34 -175.6(4) . . . . ? C31 C32 C33 C28 -3.5(6) . . . . ? C34 C32 C33 C28 177.0(4) . . . . ? C29 C28 C33 C32 -3.0(6) . . . . ? P1 C28 C33 C32 173.4(3) . . . . ? C28 P1 C35 C40 -143.9(3) . . . . ? C41 P1 C35 C40 -31.4(4) . . . . ? Ir1 P1 C35 C40 103.1(3) . . . . ? C28 P1 C35 C36 42.3(4) . . . . ? C41 P1 C35 C36 154.8(3) . . . . ? Ir1 P1 C35 C36 -70.8(3) . . . . ? C40 C35 C36 C37 0.4(6) . . . . ? P1 C35 C36 C37 174.4(3) . . . . ? C35 C36 C37 C38 -1.3(6) . . . . ? C36 C37 C38 C39 0.9(7) . . . . ? C37 C38 C39 C40 0.3(7) . . . . ? C38 C39 C40 C35 -1.1(7) . . . . ? C36 C35 C40 C39 0.7(6) . . . . ? P1 C35 C40 C39 -173.1(3) . . . . ? C28 P1 C41 C42 29.3(4) . . . . ? C35 P1 C41 C42 -81.9(4) . . . . ? Ir1 P1 C41 C42 143.7(3) . . . . ? C28 P1 C41 C46 -145.3(3) . . . . ? C35 P1 C41 C46 103.5(3) . . . . ? Ir1 P1 C41 C46 -30.9(3) . . . . ? C46 C41 C42 C43 0.4(6) . . . . ? P1 C41 C42 C43 -174.2(3) . . . . ? C41 C42 C43 C44 0.0(7) . . . . ? C42 C43 C44 C45 -0.7(7) . . . . ? C43 C44 C45 C46 1.0(6) . . . . ? C44 C45 C46 C41 -0.6(6) . . . . ? C42 C41 C46 C45 -0.1(6) . . . . ? P1 C41 C46 C45 175.0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 24.73 _diffrn_measured_fraction_theta_full 0.957 _refine_diff_density_max 2.135 _refine_diff_density_min -0.614 _refine_diff_density_rms 0.105 # Attachment 'complex161.cif' data_ec27 _database_code_depnum_ccdc_archive 'CCDC 757518' #TrackingRef 'complex161.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H47 Ir N P2 Si, C6 F' _chemical_formula_sum 'C62 H47 F Ir N P2 Si' _chemical_formula_weight 1107.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -4.7710 6.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/ c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.1135(8) _cell_length_b 15.3247(9) _cell_length_c 25.2279(16) _cell_angle_alpha 90.00 _cell_angle_beta 98.463(4) _cell_angle_gamma 90.00 _cell_volume 5014.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 48183 _cell_measurement_theta_min 6.769 _cell_measurement_theta_max 135.244 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.467 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2224 _exptl_absorpt_coefficient_mu 6.334 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.3640 _exptl_absorpt_correction_T_max 0.7857 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'microfocus rotating anode' _diffrn_radiation_monochromator 'HELIOS multilayer mirrors' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_reflns_number 46231 _diffrn_reflns_av_R_equivalents 0.0675 _diffrn_reflns_av_sigmaI/netI 0.0499 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.38 _diffrn_reflns_theta_max 67.70 _reflns_number_total 8821 _reflns_number_gt 6991 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v. 2009.1' _computing_cell_refinement 'Bruker APEX2 v. 2009.1' _computing_data_reduction 'Bruker APEX2 v. 2009.1' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Mercury _computing_publication_material CIFTAB _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^)+(0.0490P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8821 _refine_ls_number_parameters 580 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0562 _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_ref 0.0987 _refine_ls_wR_factor_gt 0.0918 _refine_ls_goodness_of_fit_ref 1.192 _refine_ls_restrained_S_all 1.193 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.329271(13) 0.904453(14) 0.844193(7) 0.01192(7) Uani 1 1 d . . . Si1 Si 0.23624(9) 0.89856(9) 0.91563(5) 0.0141(3) Uani 1 1 d . . . P1 P 0.23848(9) 1.01043(9) 0.79430(5) 0.0139(3) Uani 1 1 d . . . P2 P 0.44492(8) 0.79323(8) 0.86702(5) 0.0134(2) Uani 1 1 d . . . N1 N 0.3302(3) 0.8495(3) 0.76942(15) 0.0131(8) Uani 1 1 d . . . C1 C 0.2699(3) 0.9846(3) 0.72805(18) 0.0144(10) Uani 1 1 d . . . C2 C 0.2533(3) 1.0414(3) 0.68433(19) 0.0163(10) Uani 1 1 d . . . H2A H 0.2217 1.0963 0.6884 0.020 Uiso 1 1 calc R . . C3 C 0.2816(4) 1.0199(4) 0.6352(2) 0.0193(11) Uani 1 1 d . . . C4 C 0.3291(4) 0.9384(3) 0.6318(2) 0.0188(11) Uani 1 1 d . . . H4A H 0.3515 0.9223 0.5990 0.023 Uiso 1 1 calc R . . C5 C 0.3444(4) 0.8809(3) 0.67405(19) 0.0175(11) Uani 1 1 d . . . H5A H 0.3763 0.8262 0.6698 0.021 Uiso 1 1 calc R . . C6 C 0.3134(3) 0.9019(3) 0.72345(19) 0.0158(10) Uani 1 1 d . . . C7 C 0.3540(3) 0.7594(3) 0.76593(19) 0.0142(10) Uani 1 1 d . . . C8 C 0.4141(3) 0.7200(3) 0.80992(19) 0.0140(10) Uani 1 1 d . . . C9 C 0.5750(3) 0.8342(3) 0.86496(18) 0.0140(10) Uani 1 1 d . . . C10 C 0.6034(4) 0.9142(3) 0.88837(19) 0.0186(10) Uani 1 1 d . . . H10A H 0.5533 0.9490 0.9021 0.022 Uiso 1 1 calc R . . C11 C 0.7040(4) 0.9441(4) 0.8920(2) 0.0218(11) Uani 1 1 d . . . H11A H 0.7235 0.9980 0.9091 0.026 Uiso 1 1 calc R . . C12 C 0.7754(4) 0.8943(4) 0.8703(2) 0.0250(12) Uani 1 1 d . . . H12A H 0.8446 0.9140 0.8729 0.030 Uiso 1 1 calc R . . C13 C 0.7469(4) 0.8161(4) 0.8449(2) 0.0278(13) Uani 1 1 d . . . H13A H 0.7961 0.7835 0.8291 0.033 Uiso 1 1 calc R . . C14 C 0.6468(4) 0.7851(4) 0.8425(2) 0.0194(11) Uani 1 1 d . . . H14A H 0.6277 0.7308 0.8258 0.023 Uiso 1 1 calc R . . C15 C 0.4625(4) 0.7213(3) 0.9256(2) 0.0192(11) Uani 1 1 d . . . C16 C 0.5483(5) 0.7291(4) 0.9642(2) 0.0262(12) Uani 1 1 d . . . H16A H 0.5993 0.7716 0.9601 0.031 Uiso 1 1 calc R . . C17 C 0.5610(5) 0.6754(4) 1.0092(2) 0.0363(15) Uani 1 1 d . . . H17A H 0.6203 0.6814 1.0355 0.044 Uiso 1 1 calc R . . C18 C 0.4887(5) 0.6146(4) 1.0154(2) 0.0392(17) Uani 1 1 d . . . H18A H 0.4976 0.5778 1.0461 0.047 Uiso 1 1 calc R . . C19 C 0.4022(5) 0.6059(5) 0.9774(3) 0.050(2) Uani 1 1 d . . . H19A H 0.3515 0.5633 0.9819 0.060 Uiso 1 1 calc R . . C20 C 0.3893(4) 0.6595(5) 0.9326(3) 0.0385(16) Uani 1 1 d . . . H20A H 0.3295 0.6535 0.9065 0.046 Uiso 1 1 calc R . . C21 C 0.4403(4) 0.6319(3) 0.8085(2) 0.0196(11) Uani 1 1 d . . . H21A H 0.4826 0.6067 0.8384 0.023 Uiso 1 1 calc R . . C22 C 0.4055(4) 0.5802(3) 0.7642(2) 0.0198(11) Uani 1 1 d . . . C23 C 0.4349(4) 0.4861(4) 0.7610(2) 0.0290(13) Uani 1 1 d . . . H23A H 0.4660 0.4658 0.7966 0.044 Uiso 1 1 calc R . . H23B H 0.4847 0.4796 0.7359 0.044 Uiso 1 1 calc R . . H23C H 0.3733 0.4514 0.7486 0.044 Uiso 1 1 calc R . . C24 C 0.3411(4) 0.6199(3) 0.7216(2) 0.0194(11) Uani 1 1 d . . . H24A H 0.3145 0.5856 0.6913 0.023 Uiso 1 1 calc R . . C25 C 0.3153(3) 0.7071(4) 0.7223(2) 0.0186(11) Uani 1 1 d . . . H25A H 0.2708 0.7316 0.6930 0.022 Uiso 1 1 calc R . . C26 C 0.2643(5) 1.0803(4) 0.5878(2) 0.0296(13) Uani 1 1 d . . . H26A H 0.3208 1.0737 0.5666 0.044 Uiso 1 1 calc R . . H26B H 0.2620 1.1407 0.6003 0.044 Uiso 1 1 calc R . . H26C H 0.1988 1.0657 0.5655 0.044 Uiso 1 1 calc R . . C27 C 0.2739(4) 1.1237(3) 0.8079(2) 0.0189(11) Uani 1 1 d . . . C28 C 0.2287(5) 1.1711(4) 0.8451(2) 0.0283(13) Uani 1 1 d . . . H28A H 0.1754 1.1455 0.8616 0.034 Uiso 1 1 calc R . . C29 C 0.2607(5) 1.2554(4) 0.8582(2) 0.0353(15) Uani 1 1 d . . . H29A H 0.2295 1.2870 0.8840 0.042 Uiso 1 1 calc R . . C30 C 0.3379(5) 1.2948(4) 0.8341(2) 0.0390(16) Uani 1 1 d . . . H30A H 0.3577 1.3536 0.8420 0.047 Uiso 1 1 calc R . . C31 C 0.3854(4) 1.2460(4) 0.7983(2) 0.0280(13) Uani 1 1 d . . . H31A H 0.4402 1.2709 0.7827 0.034 Uiso 1 1 calc R . . C32 C 0.3542(4) 1.1620(4) 0.78530(19) 0.0192(11) Uani 1 1 d . . . H32A H 0.3876 1.1297 0.7607 0.023 Uiso 1 1 calc R . . C33 C 0.0979(4) 1.0047(4) 0.78289(19) 0.0202(11) Uani 1 1 d . . . C34 C 0.0327(4) 1.0766(4) 0.7754(2) 0.0296(13) Uani 1 1 d . . . H34A H 0.0606 1.1339 0.7759 0.036 Uiso 1 1 calc R . . C35 C -0.0731(5) 1.0642(5) 0.7673(2) 0.0387(17) Uani 1 1 d . . . H35A H -0.1176 1.1134 0.7632 0.046 Uiso 1 1 calc R . . C36 C -0.1139(4) 0.9826(6) 0.7651(2) 0.0447(19) Uani 1 1 d . . . H36A H -0.1866 0.9752 0.7596 0.054 Uiso 1 1 calc R . . C37 C -0.0501(4) 0.9101(5) 0.7710(3) 0.0415(16) Uani 1 1 d . . . H37A H -0.0789 0.8531 0.7685 0.050 Uiso 1 1 calc R . . C38 C 0.0563(4) 0.9212(4) 0.7804(2) 0.0273(13) Uani 1 1 d . . . H38A H 0.1004 0.8718 0.7852 0.033 Uiso 1 1 calc R . . C39 C 0.3118(4) 0.8701(3) 0.9842(2) 0.0179(10) Uani 1 1 d . . . C40 C 0.2651(5) 0.8220(4) 1.0206(2) 0.0309(13) Uani 1 1 d . . . H40A H 0.1973 0.8002 1.0103 0.037 Uiso 1 1 calc R . . C41 C 0.3162(5) 0.8051(4) 1.0720(2) 0.0367(15) Uani 1 1 d . . . H41A H 0.2824 0.7725 1.0962 0.044 Uiso 1 1 calc R . . C42 C 0.4144(5) 0.8346(4) 1.0881(2) 0.0313(14) Uani 1 1 d . . . H42A H 0.4488 0.8228 1.1232 0.038 Uiso 1 1 calc R . . C43 C 0.4625(4) 0.8819(4) 1.0523(2) 0.0256(13) Uani 1 1 d . . . H43A H 0.5308 0.9026 1.0626 0.031 Uiso 1 1 calc R . . C44 C 0.4111(4) 0.8993(4) 1.0012(2) 0.0221(11) Uani 1 1 d . . . H44A H 0.4452 0.9323 0.9772 0.027 Uiso 1 1 calc R . . C45 C 0.1350(4) 0.8100(3) 0.90067(19) 0.0170(10) Uani 1 1 d . . . C46 C 0.0478(4) 0.8067(4) 0.9271(2) 0.0229(12) Uani 1 1 d . . . H46A H 0.0363 0.8523 0.9510 0.027 Uiso 1 1 calc R . . C47 C -0.0216(4) 0.7382(4) 0.9188(2) 0.0301(13) Uani 1 1 d . . . H47A H -0.0802 0.7374 0.9369 0.036 Uiso 1 1 calc R . . C48 C -0.0060(4) 0.6711(4) 0.8843(3) 0.0350(15) Uani 1 1 d . . . H48A H -0.0532 0.6238 0.8791 0.042 Uiso 1 1 calc R . . C49 C 0.0775(4) 0.6730(4) 0.8578(2) 0.0307(14) Uani 1 1 d . . . H49A H 0.0880 0.6271 0.8339 0.037 Uiso 1 1 calc R . . C50 C 0.1469(4) 0.7414(4) 0.8656(2) 0.0224(12) Uani 1 1 d . . . H50A H 0.2043 0.7418 0.8465 0.027 Uiso 1 1 calc R . . C51 C 0.1643(4) 1.0016(4) 0.93085(18) 0.0187(11) Uani 1 1 d . . . C52 C 0.2149(4) 1.0654(4) 0.9650(2) 0.0243(12) Uani 1 1 d . . . H52A H 0.2843 1.0555 0.9808 0.029 Uiso 1 1 calc R . . C53 C 0.1671(4) 1.1421(4) 0.9765(2) 0.0321(14) Uani 1 1 d . . . H53A H 0.2034 1.1840 0.9998 0.039 Uiso 1 1 calc R . . C54 C 0.0654(5) 1.1574(4) 0.9537(2) 0.0352(15) Uani 1 1 d . . . H54A H 0.0323 1.2102 0.9611 0.042 Uiso 1 1 calc R . . C55 C 0.0126(4) 1.0957(4) 0.9202(2) 0.0321(14) Uani 1 1 d . . . H55A H -0.0569 1.1059 0.9048 0.039 Uiso 1 1 calc R . . C56 C 0.0618(4) 1.0184(4) 0.90905(19) 0.0213(11) Uani 1 1 d . . . H56A H 0.0249 0.9763 0.8862 0.026 Uiso 1 1 calc R . . C57 C 0.1051(10) 0.4407(10) 0.9071(6) 0.127(5) Uiso 1 1 d D . . C58 C 0.0336(11) 0.4203(9) 0.8664(5) 0.124(5) Uiso 1 1 d D . . C59 C -0.0567(10) 0.3805(9) 0.8765(5) 0.117(5) Uiso 1 1 d D . . C60 C -0.0784(9) 0.3776(9) 0.9277(6) 0.109(4) Uiso 1 1 d D . . C61 C -0.0057(14) 0.4045(13) 0.9689(6) 0.219(10) Uiso 1 1 d D . . C62 C 0.0896(12) 0.4280(12) 0.9583(6) 0.176(8) Uiso 1 1 d D . . F1 F 0.2010(9) 0.4728(7) 0.8986(4) 0.197(4) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.01163(10) 0.01421(12) 0.00953(10) 0.00039(9) 0.00026(6) 0.00241(9) Si1 0.0140(5) 0.0197(7) 0.0082(6) -0.0005(5) 0.0002(4) 0.0016(5) P1 0.0140(5) 0.0159(7) 0.0115(6) 0.0018(5) 0.0005(4) 0.0050(5) P2 0.0124(5) 0.0147(6) 0.0123(5) 0.0006(5) -0.0008(4) 0.0024(5) N1 0.0132(17) 0.015(2) 0.0101(19) -0.0015(16) -0.0018(14) 0.0007(16) C1 0.014(2) 0.018(3) 0.012(2) 0.000(2) 0.0025(17) -0.0012(19) C2 0.018(2) 0.013(3) 0.018(2) 0.000(2) 0.0019(18) 0.0020(19) C3 0.023(2) 0.021(3) 0.014(2) 0.002(2) 0.0020(19) -0.003(2) C4 0.019(2) 0.024(3) 0.014(2) -0.004(2) 0.0036(18) 0.001(2) C5 0.018(2) 0.020(3) 0.015(2) -0.005(2) 0.0012(18) -0.0011(19) C6 0.0128(19) 0.020(3) 0.014(2) -0.003(2) -0.0011(17) -0.001(2) C7 0.0119(19) 0.014(3) 0.017(2) -0.002(2) 0.0035(17) -0.0028(18) C8 0.0122(19) 0.015(3) 0.016(2) -0.002(2) 0.0029(17) 0.0021(19) C9 0.012(2) 0.015(3) 0.013(2) 0.0035(19) -0.0021(17) 0.0007(19) C10 0.020(2) 0.021(3) 0.013(2) 0.001(2) -0.0026(18) 0.004(2) C11 0.024(2) 0.019(3) 0.020(3) -0.002(2) -0.005(2) -0.005(2) C12 0.016(2) 0.029(3) 0.028(3) 0.005(2) -0.003(2) -0.003(2) C13 0.020(2) 0.026(3) 0.038(3) -0.006(3) 0.007(2) 0.000(2) C14 0.020(2) 0.018(3) 0.020(2) -0.003(2) 0.0041(19) 0.004(2) C15 0.025(2) 0.017(3) 0.016(2) 0.001(2) 0.0055(19) 0.008(2) C16 0.042(3) 0.022(3) 0.014(2) -0.002(2) -0.001(2) 0.004(3) C17 0.057(4) 0.035(4) 0.014(3) 0.003(3) -0.003(3) 0.013(3) C18 0.053(4) 0.041(4) 0.027(3) 0.019(3) 0.019(3) 0.029(3) C19 0.039(3) 0.051(5) 0.062(5) 0.034(4) 0.017(3) 0.008(3) C20 0.026(3) 0.047(4) 0.042(4) 0.023(3) 0.007(3) 0.003(3) C21 0.016(2) 0.018(3) 0.023(3) 0.003(2) -0.0038(19) 0.003(2) C22 0.015(2) 0.011(3) 0.032(3) -0.003(2) 0.002(2) -0.0011(19) C23 0.022(2) 0.020(3) 0.042(3) -0.004(3) -0.005(2) 0.000(2) C24 0.015(2) 0.019(3) 0.023(3) -0.002(2) -0.0005(19) -0.003(2) C25 0.016(2) 0.021(3) 0.018(2) 0.001(2) -0.0013(18) -0.001(2) C26 0.048(3) 0.028(4) 0.013(2) 0.006(2) 0.006(2) 0.005(3) C27 0.021(2) 0.018(3) 0.017(2) 0.001(2) -0.0006(19) 0.003(2) C28 0.042(3) 0.025(3) 0.020(3) 0.002(2) 0.011(2) 0.008(3) C29 0.068(4) 0.018(3) 0.022(3) -0.003(2) 0.016(3) 0.005(3) C30 0.070(4) 0.021(3) 0.028(3) 0.002(3) 0.014(3) -0.007(3) C31 0.031(3) 0.029(3) 0.022(3) 0.002(2) -0.003(2) -0.001(2) C32 0.017(2) 0.026(3) 0.014(2) 0.001(2) -0.0008(18) 0.006(2) C33 0.019(2) 0.033(3) 0.010(2) 0.001(2) 0.0039(18) 0.006(2) C34 0.026(3) 0.040(4) 0.024(3) 0.009(3) 0.006(2) 0.013(3) C35 0.025(3) 0.062(5) 0.030(3) 0.017(3) 0.007(2) 0.019(3) C36 0.014(2) 0.087(6) 0.031(3) 0.015(4) -0.001(2) 0.005(3) C37 0.024(3) 0.059(5) 0.039(4) 0.002(3) -0.001(3) -0.005(3) C38 0.023(3) 0.038(4) 0.021(3) 0.000(3) 0.003(2) 0.002(2) C39 0.023(2) 0.014(3) 0.017(2) -0.002(2) 0.0017(19) 0.005(2) C40 0.040(3) 0.035(4) 0.016(3) 0.000(3) -0.004(2) -0.004(3) C41 0.055(4) 0.035(4) 0.018(3) 0.007(3) -0.003(3) -0.006(3) C42 0.051(3) 0.026(3) 0.013(3) 0.002(2) -0.008(2) 0.013(3) C43 0.026(3) 0.027(3) 0.021(3) -0.011(2) -0.006(2) 0.012(2) C44 0.026(2) 0.027(3) 0.013(2) -0.004(2) 0.0018(19) 0.007(2) C45 0.018(2) 0.018(3) 0.015(2) 0.000(2) -0.0017(18) -0.001(2) C46 0.020(2) 0.032(3) 0.017(2) -0.005(2) 0.0049(19) -0.002(2) C47 0.026(3) 0.034(4) 0.031(3) -0.005(3) 0.008(2) -0.007(2) C48 0.024(3) 0.043(4) 0.038(3) -0.016(3) 0.008(2) -0.012(3) C49 0.027(3) 0.035(4) 0.030(3) -0.018(3) 0.002(2) -0.006(3) C50 0.022(2) 0.030(3) 0.015(2) -0.002(2) 0.0031(19) 0.001(2) C51 0.018(2) 0.032(3) 0.006(2) 0.003(2) 0.0030(17) 0.001(2) C52 0.029(3) 0.027(3) 0.017(3) 0.001(2) 0.001(2) 0.007(2) C53 0.034(3) 0.037(4) 0.026(3) -0.005(3) 0.004(2) 0.011(3) C54 0.047(3) 0.038(4) 0.023(3) 0.002(3) 0.014(3) 0.022(3) C55 0.029(3) 0.046(4) 0.022(3) 0.004(3) 0.007(2) 0.021(3) C56 0.020(2) 0.032(3) 0.013(2) 0.001(2) 0.0056(19) 0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 N1 2.067(4) . ? Ir1 P1 2.2800(12) . ? Ir1 P2 2.2978(12) . ? Ir1 Si1 2.3220(13) . ? Si1 C45 1.897(5) . ? Si1 C51 1.907(6) . ? Si1 C39 1.913(5) . ? P1 C27 1.816(5) . ? P1 C1 1.823(5) . ? P1 C33 1.825(5) . ? P2 C8 1.824(5) . ? P2 C9 1.825(5) . ? P2 C15 1.830(5) . ? N1 C6 1.402(6) . ? N1 C7 1.421(6) . ? C1 C2 1.396(7) . ? C1 C6 1.402(7) . ? C2 C3 1.385(7) . ? C2 H2A 0.9500 . ? C3 C4 1.404(7) . ? C3 C26 1.502(7) . ? C4 C5 1.375(7) . ? C4 H4A 0.9500 . ? C5 C6 1.404(7) . ? C5 H5A 0.9500 . ? C7 C25 1.395(7) . ? C7 C8 1.400(6) . ? C8 C21 1.395(7) . ? C9 C10 1.388(7) . ? C9 C14 1.389(7) . ? C10 C11 1.386(7) . ? C10 H10A 0.9500 . ? C11 C12 1.382(8) . ? C11 H11A 0.9500 . ? C12 C13 1.385(8) . ? C12 H12A 0.9500 . ? C13 C14 1.389(7) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? C15 C20 1.379(8) . ? C15 C16 1.382(7) . ? C16 C17 1.390(8) . ? C16 H16A 0.9500 . ? C17 C18 1.355(9) . ? C17 H17A 0.9500 . ? C18 C19 1.381(10) . ? C18 H18A 0.9500 . ? C19 C20 1.387(8) . ? C19 H19A 0.9500 . ? C20 H20A 0.9500 . ? C21 C22 1.392(7) . ? C21 H21A 0.9500 . ? C22 C24 1.404(7) . ? C22 C23 1.497(7) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.380(7) . ? C24 H24A 0.9500 . ? C25 H25A 0.9500 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.387(7) . ? C27 C32 1.399(7) . ? C28 C29 1.384(8) . ? C28 H28A 0.9500 . ? C29 C30 1.393(9) . ? C29 H29A 0.9500 . ? C30 C31 1.388(8) . ? C30 H30A 0.9500 . ? C31 C32 1.375(8) . ? C31 H31A 0.9500 . ? C32 H32A 0.9500 . ? C33 C38 1.388(8) . ? C33 C34 1.391(7) . ? C34 C35 1.385(8) . ? C34 H34A 0.9500 . ? C35 C36 1.359(10) . ? C35 H35A 0.9500 . ? C36 C37 1.385(10) . ? C36 H36A 0.9500 . ? C37 C38 1.391(8) . ? C37 H37A 0.9500 . ? C38 H38A 0.9500 . ? C39 C44 1.384(7) . ? C39 C40 1.388(8) . ? C40 C41 1.392(7) . ? C40 H40A 0.9500 . ? C41 C42 1.369(9) . ? C41 H41A 0.9500 . ? C42 C43 1.380(8) . ? C42 H42A 0.9500 . ? C43 C44 1.389(7) . ? C43 H43A 0.9500 . ? C44 H44A 0.9500 . ? C45 C50 1.398(7) . ? C45 C46 1.406(7) . ? C46 C47 1.385(8) . ? C46 H46A 0.9500 . ? C47 C48 1.381(8) . ? C47 H47A 0.9500 . ? C48 C49 1.365(8) . ? C48 H48A 0.9500 . ? C49 C50 1.384(8) . ? C49 H49A 0.9500 . ? C50 H50A 0.9500 . ? C51 C56 1.399(6) . ? C51 C52 1.404(7) . ? C52 C53 1.382(8) . ? C52 H52A 0.9500 . ? C53 C54 1.393(8) . ? C53 H53A 0.9500 . ? C54 C55 1.383(9) . ? C54 H54A 0.9500 . ? C55 C56 1.398(8) . ? C55 H55A 0.9500 . ? C56 H56A 0.9500 . ? C57 C58 1.323(11) . ? C57 C62 1.350(12) . ? C57 F1 1.395(13) . ? C58 C59 1.389(11) . ? C59 C60 1.362(11) . ? C60 C61 1.367(12) . ? C61 C62 1.363(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ir1 P1 81.90(11) . . ? N1 Ir1 P2 80.46(11) . . ? P1 Ir1 P2 159.81(4) . . ? N1 Ir1 Si1 140.04(11) . . ? P1 Ir1 Si1 99.49(4) . . ? P2 Ir1 Si1 100.33(5) . . ? C45 Si1 C51 106.3(2) . . ? C45 Si1 C39 105.7(2) . . ? C51 Si1 C39 102.2(2) . . ? C45 Si1 Ir1 107.79(16) . . ? C51 Si1 Ir1 117.11(16) . . ? C39 Si1 Ir1 116.71(16) . . ? C27 P1 C1 107.1(2) . . ? C27 P1 C33 107.5(2) . . ? C1 P1 C33 101.8(2) . . ? C27 P1 Ir1 118.59(16) . . ? C1 P1 Ir1 100.46(16) . . ? C33 P1 Ir1 119.06(18) . . ? C8 P2 C9 106.7(2) . . ? C8 P2 C15 104.7(2) . . ? C9 P2 C15 102.9(2) . . ? C8 P2 Ir1 101.37(15) . . ? C9 P2 Ir1 108.83(16) . . ? C15 P2 Ir1 130.49(16) . . ? C6 N1 C7 121.0(4) . . ? C6 N1 Ir1 120.0(3) . . ? C7 N1 Ir1 118.9(3) . . ? C2 C1 C6 121.0(5) . . ? C2 C1 P1 124.0(4) . . ? C6 C1 P1 114.9(4) . . ? C3 C2 C1 121.9(5) . . ? C3 C2 H2A 119.1 . . ? C1 C2 H2A 119.1 . . ? C2 C3 C4 116.5(5) . . ? C2 C3 C26 122.5(5) . . ? C4 C3 C26 121.0(5) . . ? C5 C4 C3 122.6(5) . . ? C5 C4 H4A 118.7 . . ? C3 C4 H4A 118.7 . . ? C4 C5 C6 120.9(5) . . ? C4 C5 H5A 119.6 . . ? C6 C5 H5A 119.6 . . ? N1 C6 C1 117.8(4) . . ? N1 C6 C5 124.9(5) . . ? C1 C6 C5 117.1(5) . . ? C25 C7 C8 118.3(5) . . ? C25 C7 N1 123.4(4) . . ? C8 C7 N1 118.2(4) . . ? C21 C8 C7 120.6(5) . . ? C21 C8 P2 126.1(4) . . ? C7 C8 P2 113.2(4) . . ? C10 C9 C14 119.7(4) . . ? C10 C9 P2 119.0(4) . . ? C14 C9 P2 121.2(4) . . ? C11 C10 C9 120.9(5) . . ? C11 C10 H10A 119.5 . . ? C9 C10 H10A 119.5 . . ? C12 C11 C10 119.0(5) . . ? C12 C11 H11A 120.5 . . ? C10 C11 H11A 120.5 . . ? C11 C12 C13 120.6(5) . . ? C11 C12 H12A 119.7 . . ? C13 C12 H12A 119.7 . . ? C12 C13 C14 120.3(5) . . ? C12 C13 H13A 119.8 . . ? C14 C13 H13A 119.8 . . ? C13 C14 C9 119.3(5) . . ? C13 C14 H14A 120.3 . . ? C9 C14 H14A 120.3 . . ? C20 C15 C16 118.6(5) . . ? C20 C15 P2 120.7(4) . . ? C16 C15 P2 120.7(4) . . ? C15 C16 C17 120.7(6) . . ? C15 C16 H16A 119.6 . . ? C17 C16 H16A 119.6 . . ? C18 C17 C16 120.0(6) . . ? C18 C17 H17A 120.0 . . ? C16 C17 H17A 120.0 . . ? C17 C18 C19 120.2(6) . . ? C17 C18 H18A 119.9 . . ? C19 C18 H18A 119.9 . . ? C18 C19 C20 119.9(7) . . ? C18 C19 H19A 120.0 . . ? C20 C19 H19A 120.0 . . ? C15 C20 C19 120.5(6) . . ? C15 C20 H20A 119.8 . . ? C19 C20 H20A 119.8 . . ? C22 C21 C8 121.3(5) . . ? C22 C21 H21A 119.4 . . ? C8 C21 H21A 119.4 . . ? C21 C22 C24 117.2(5) . . ? C21 C22 C23 122.3(5) . . ? C24 C22 C23 120.5(5) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C22 122.0(5) . . ? C25 C24 H24A 119.0 . . ? C22 C24 H24A 119.0 . . ? C24 C25 C7 120.4(5) . . ? C24 C25 H25A 119.8 . . ? C7 C25 H25A 119.8 . . ? C3 C26 H26A 109.5 . . ? C3 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C3 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C32 118.5(5) . . ? C28 C27 P1 120.4(4) . . ? C32 C27 P1 120.8(4) . . ? C29 C28 C27 120.4(6) . . ? C29 C28 H28A 119.8 . . ? C27 C28 H28A 119.8 . . ? C28 C29 C30 120.9(6) . . ? C28 C29 H29A 119.5 . . ? C30 C29 H29A 119.5 . . ? C31 C30 C29 118.4(6) . . ? C31 C30 H30A 120.8 . . ? C29 C30 H30A 120.8 . . ? C32 C31 C30 120.9(6) . . ? C32 C31 H31A 119.5 . . ? C30 C31 H31A 119.5 . . ? C31 C32 C27 120.7(5) . . ? C31 C32 H32A 119.6 . . ? C27 C32 H32A 119.6 . . ? C38 C33 C34 119.6(5) . . ? C38 C33 P1 115.7(4) . . ? C34 C33 P1 124.7(5) . . ? C35 C34 C33 119.6(6) . . ? C35 C34 H34A 120.2 . . ? C33 C34 H34A 120.2 . . ? C36 C35 C34 120.8(6) . . ? C36 C35 H35A 119.6 . . ? C34 C35 H35A 119.6 . . ? C35 C36 C37 120.4(5) . . ? C35 C36 H36A 119.8 . . ? C37 C36 H36A 119.8 . . ? C36 C37 C38 119.7(7) . . ? C36 C37 H37A 120.2 . . ? C38 C37 H37A 120.2 . . ? C33 C38 C37 119.9(6) . . ? C33 C38 H38A 120.1 . . ? C37 C38 H38A 120.1 . . ? C44 C39 C40 116.8(5) . . ? C44 C39 Si1 123.1(4) . . ? C40 C39 Si1 120.0(4) . . ? C39 C40 C41 121.1(6) . . ? C39 C40 H40A 119.5 . . ? C41 C40 H40A 119.5 . . ? C42 C41 C40 121.2(6) . . ? C42 C41 H41A 119.4 . . ? C40 C41 H41A 119.4 . . ? C41 C42 C43 118.6(5) . . ? C41 C42 H42A 120.7 . . ? C43 C42 H42A 120.7 . . ? C42 C43 C44 120.1(5) . . ? C42 C43 H43A 119.9 . . ? C44 C43 H43A 119.9 . . ? C39 C44 C43 122.2(5) . . ? C39 C44 H44A 118.9 . . ? C43 C44 H44A 118.9 . . ? C50 C45 C46 116.6(5) . . ? C50 C45 Si1 121.6(4) . . ? C46 C45 Si1 121.7(4) . . ? C47 C46 C45 121.3(5) . . ? C47 C46 H46A 119.4 . . ? C45 C46 H46A 119.4 . . ? C48 C47 C46 120.2(5) . . ? C48 C47 H47A 119.9 . . ? C46 C47 H47A 119.9 . . ? C49 C48 C47 119.8(6) . . ? C49 C48 H48A 120.1 . . ? C47 C48 H48A 120.1 . . ? C48 C49 C50 120.3(6) . . ? C48 C49 H49A 119.8 . . ? C50 C49 H49A 119.8 . . ? C49 C50 C45 121.8(5) . . ? C49 C50 H50A 119.1 . . ? C45 C50 H50A 119.1 . . ? C56 C51 C52 117.0(5) . . ? C56 C51 Si1 123.2(4) . . ? C52 C51 Si1 119.8(4) . . ? C53 C52 C51 122.1(5) . . ? C53 C52 H52A 118.9 . . ? C51 C52 H52A 118.9 . . ? C52 C53 C54 119.6(6) . . ? C52 C53 H53A 120.2 . . ? C54 C53 H53A 120.2 . . ? C55 C54 C53 120.0(6) . . ? C55 C54 H54A 120.0 . . ? C53 C54 H54A 120.0 . . ? C54 C55 C56 119.8(5) . . ? C54 C55 H55A 120.1 . . ? C56 C55 H55A 120.1 . . ? C55 C56 C51 121.5(5) . . ? C55 C56 H56A 119.3 . . ? C51 C56 H56A 119.3 . . ? C58 C57 C62 121.3(9) . . ? C58 C57 F1 121.0(13) . . ? C62 C57 F1 117.7(13) . . ? C57 C58 C59 119.1(9) . . ? C60 C59 C58 119.5(9) . . ? C59 C60 C61 119.4(9) . . ? C62 C61 C60 119.2(10) . . ? C57 C62 C61 119.8(10) . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 67.70 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 2.035 _refine_diff_density_min -0.973 _refine_diff_density_rms 0.129 # Attachment 'complex181.cif' data_ec28sqz _database_code_depnum_ccdc_archive 'CCDC 757519' #TrackingRef 'complex181.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H48 N P2 Rh Si' _chemical_formula_sum 'C56 H48 N P2 Rh Si' _chemical_formula_weight 927.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh 0.0927 3.6045 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/ c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.1126(5) _cell_length_b 15.3957(6) _cell_length_c 25.2088(10) _cell_angle_alpha 90.00 _cell_angle_beta 98.327(2) _cell_angle_gamma 90.00 _cell_volume 5035.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 26182 _cell_measurement_theta_min 6.747 _cell_measurement_theta_max 135.871 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.224 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1920 _exptl_absorpt_coefficient_mu 3.834 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.5453 _exptl_absorpt_correction_T_max 0.7004 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'microfocus rotating anode' _diffrn_radiation_monochromator 'HELIOS multilayer mirrors' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_reflns_number 25446 _diffrn_reflns_av_R_equivalents 0.0487 _diffrn_reflns_av_sigmaI/netI 0.0494 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.37 _diffrn_reflns_theta_max 68.08 _reflns_number_total 8114 _reflns_number_gt 6261 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v. 2009.1' _computing_cell_refinement 'Bruker APEX2 v. 2009.1' _computing_data_reduction 'Bruker APEX2 v. 2009.1' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Mercury _computing_publication_material CIFTAB _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^)+(0.0460P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8114 _refine_ls_number_parameters 555 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0511 _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_ref 0.0823 _refine_ls_wR_factor_gt 0.0773 _refine_ls_goodness_of_fit_ref 0.969 _refine_ls_restrained_S_all 0.969 _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 0.670609(16) 0.094707(14) 0.155182(9) 0.01768(7) Uani 1 1 d . . . H1 H 0.654(2) 0.0409(19) 0.1055(12) 0.021 Uiso 1 1 d . . . Si1 Si 0.76133(6) 0.09880(5) 0.08299(3) 0.02040(17) Uani 1 1 d . . . P1 P 0.76093(6) -0.01102(5) 0.20536(3) 0.01996(17) Uani 1 1 d . . . P2 P 0.55493(6) 0.20564(5) 0.13225(3) 0.01900(16) Uani 1 1 d . . . N1 N 0.66746(18) 0.14963(15) 0.22983(10) 0.0184(5) Uani 1 1 d . . . C1 C 0.6861(2) 0.12879(19) 0.01492(13) 0.0245(7) Uani 1 1 d . . . C2 C 0.7333(3) 0.1760(2) -0.02208(15) 0.0410(9) Uani 1 1 d . . . H2A H 0.8017 0.1965 -0.0121 0.049 Uiso 1 1 calc R . . C3 C 0.6826(4) 0.1936(3) -0.07278(16) 0.0513(11) Uani 1 1 d . . . H3A H 0.7164 0.2259 -0.0972 0.062 Uiso 1 1 calc R . . C4 C 0.5834(3) 0.1646(2) -0.08819(15) 0.0412(9) Uani 1 1 d . . . H4A H 0.5489 0.1764 -0.1232 0.049 Uiso 1 1 calc R . . C5 C 0.5350(3) 0.1185(2) -0.05254(14) 0.0360(9) Uani 1 1 d . . . H5A H 0.4661 0.0991 -0.0627 0.043 Uiso 1 1 calc R . . C6 C 0.5862(2) 0.1001(2) -0.00183(14) 0.0301(7) Uani 1 1 d . . . H6A H 0.5521 0.0670 0.0221 0.036 Uiso 1 1 calc R . . C7 C 0.8334(2) -0.0026(2) 0.06769(13) 0.0235(7) Uani 1 1 d . . . C8 C 0.9365(2) -0.0191(2) 0.08983(14) 0.0292(7) Uani 1 1 d . . . H8A H 0.9732 0.0226 0.1130 0.035 Uiso 1 1 calc R . . C9 C 0.9856(3) -0.0960(2) 0.07824(15) 0.0385(9) Uani 1 1 d . . . H9A H 1.0552 -0.1060 0.0935 0.046 Uiso 1 1 calc R . . C10 C 0.9336(3) -0.1575(2) 0.04473(15) 0.0404(9) Uani 1 1 d . . . H10A H 0.9670 -0.2099 0.0373 0.049 Uiso 1 1 calc R . . C11 C 0.8323(3) -0.1424(2) 0.02200(15) 0.0363(8) Uani 1 1 d . . . H11A H 0.7963 -0.1844 -0.0012 0.044 Uiso 1 1 calc R . . C12 C 0.7841(3) -0.0663(2) 0.03310(14) 0.0293(7) Uani 1 1 d . . . H12A H 0.7151 -0.0566 0.0168 0.035 Uiso 1 1 calc R . . C13 C 0.8620(2) 0.1875(2) 0.09948(13) 0.0252(7) Uani 1 1 d . . . C14 C 0.9492(2) 0.1915(2) 0.07361(14) 0.0313(8) Uani 1 1 d . . . H14A H 0.9608 0.1469 0.0491 0.038 Uiso 1 1 calc R . . C15 C 1.0192(3) 0.2591(2) 0.08285(16) 0.0380(9) Uani 1 1 d . . . H15A H 1.0773 0.2611 0.0643 0.046 Uiso 1 1 calc R . . C16 C 1.0047(3) 0.3234(3) 0.11885(16) 0.0434(10) Uani 1 1 d . . . H16A H 1.0525 0.3698 0.1251 0.052 Uiso 1 1 calc R . . C17 C 0.9207(3) 0.3203(3) 0.14580(16) 0.0413(9) Uani 1 1 d . . . H17A H 0.9109 0.3646 0.1708 0.050 Uiso 1 1 calc R . . C18 C 0.8503(3) 0.2526(2) 0.13655(14) 0.0330(8) Uani 1 1 d . . . H18A H 0.7932 0.2506 0.1558 0.040 Uiso 1 1 calc R . . C19 C 0.5872(2) 0.27800(19) 0.18917(12) 0.0197(6) Uani 1 1 d . . . C20 C 0.6844(2) 0.0973(2) 0.27573(12) 0.0216(6) Uani 1 1 d . . . C21 C 0.7287(2) 0.01486(19) 0.27134(13) 0.0213(7) Uani 1 1 d . . . C22 C 0.7471(2) -0.0405(2) 0.31519(13) 0.0258(7) Uani 1 1 d . . . H22A H 0.7798 -0.0947 0.3112 0.031 Uiso 1 1 calc R . . C23 C 0.7195(3) -0.0194(2) 0.36456(13) 0.0280(7) Uani 1 1 d . . . C24 C 0.7404(3) -0.0786(2) 0.41252(15) 0.0416(9) Uani 1 1 d . . . H24A H 0.6816 -0.0772 0.4325 0.062 Uiso 1 1 calc R . . H24B H 0.8025 -0.0589 0.4358 0.062 Uiso 1 1 calc R . . H24C H 0.7508 -0.1380 0.4005 0.062 Uiso 1 1 calc R . . C25 C 0.6710(3) 0.0605(2) 0.36804(14) 0.0288(7) Uani 1 1 d . . . H25A H 0.6487 0.0764 0.4009 0.035 Uiso 1 1 calc R . . C26 C 0.6541(2) 0.11752(19) 0.32549(13) 0.0245(7) Uani 1 1 d . . . H26A H 0.6214 0.1715 0.3299 0.029 Uiso 1 1 calc R . . C27 C 0.7237(2) -0.12362(19) 0.19212(13) 0.0233(7) Uani 1 1 d . . . C28 C 0.7685(3) -0.1706(2) 0.15428(15) 0.0342(8) Uani 1 1 d . . . H28A H 0.8213 -0.1450 0.1373 0.041 Uiso 1 1 calc R . . C29 C 0.7360(3) -0.2545(2) 0.14137(16) 0.0440(10) Uani 1 1 d . . . H29A H 0.7672 -0.2865 0.1158 0.053 Uiso 1 1 calc R . . C30 C 0.6580(3) -0.2922(2) 0.16566(15) 0.0425(10) Uani 1 1 d . . . H30A H 0.6361 -0.3499 0.1570 0.051 Uiso 1 1 calc R . . C31 C 0.6134(3) -0.2454(2) 0.20201(15) 0.0369(8) Uani 1 1 d . . . H31A H 0.5597 -0.2708 0.2184 0.044 Uiso 1 1 calc R . . C32 C 0.6449(2) -0.1620(2) 0.21534(13) 0.0280(7) Uani 1 1 d . . . H32A H 0.6126 -0.1303 0.2406 0.034 Uiso 1 1 calc R . . C33 C 0.9012(2) -0.0078(2) 0.21694(13) 0.0264(7) Uani 1 1 d . . . C34 C 0.9442(3) 0.0756(2) 0.22079(14) 0.0357(8) Uani 1 1 d . . . H34A H 0.9007 0.1252 0.2168 0.043 Uiso 1 1 calc R . . C35 C 1.0508(3) 0.0859(3) 0.23040(16) 0.0499(11) Uani 1 1 d . . . H35A H 1.0800 0.1425 0.2338 0.060 Uiso 1 1 calc R . . C36 C 1.1139(3) 0.0137(3) 0.23499(17) 0.0544(12) Uani 1 1 d . . . H36A H 1.1867 0.0206 0.2409 0.065 Uiso 1 1 calc R . . C37 C 1.0718(3) -0.0682(3) 0.23101(17) 0.0526(12) Uani 1 1 d . . . H37A H 1.1157 -0.1176 0.2340 0.063 Uiso 1 1 calc R . . C38 C 0.9656(3) -0.0793(3) 0.22270(15) 0.0394(9) Uani 1 1 d . . . H38A H 0.9371 -0.1361 0.2210 0.047 Uiso 1 1 calc R . . C39 C 0.6453(2) 0.2383(2) 0.23383(13) 0.0216(7) Uani 1 1 d . . . C40 C 0.6830(2) 0.2912(2) 0.27697(13) 0.0241(7) Uani 1 1 d . . . H40A H 0.7269 0.2672 0.3066 0.029 Uiso 1 1 calc R . . C41 C 0.6576(2) 0.3782(2) 0.27729(14) 0.0256(7) Uani 1 1 d . . . H41A H 0.6833 0.4122 0.3077 0.031 Uiso 1 1 calc R . . C42 C 0.5958(2) 0.4177(2) 0.23467(14) 0.0261(7) Uani 1 1 d . . . C43 C 0.5617(2) 0.36670(19) 0.19034(14) 0.0238(7) Uani 1 1 d . . . H43A H 0.5205 0.3921 0.1602 0.029 Uiso 1 1 calc R . . C44 C 0.5667(3) 0.5116(2) 0.23793(15) 0.0336(8) Uani 1 1 d . . . H44A H 0.5370 0.5323 0.2023 0.050 Uiso 1 1 calc R . . H44B H 0.6282 0.5458 0.2511 0.050 Uiso 1 1 calc R . . H44C H 0.5159 0.5180 0.2626 0.050 Uiso 1 1 calc R . . C45 C 0.4261(2) 0.16438(19) 0.13584(12) 0.0204(6) Uani 1 1 d . . . C46 C 0.3968(2) 0.08401(19) 0.11291(13) 0.0233(7) Uani 1 1 d . . . H46A H 0.4464 0.0490 0.0990 0.028 Uiso 1 1 calc R . . C47 C 0.2970(2) 0.0548(2) 0.11022(13) 0.0274(7) Uani 1 1 d . . . H47A H 0.2778 0.0004 0.0939 0.033 Uiso 1 1 calc R . . C48 C 0.2251(2) 0.1045(2) 0.13119(14) 0.0305(8) Uani 1 1 d . . . H48A H 0.1558 0.0850 0.1285 0.037 Uiso 1 1 calc R . . C49 C 0.2534(2) 0.1826(2) 0.15611(15) 0.0321(8) Uani 1 1 d . . . H49A H 0.2045 0.2151 0.1722 0.039 Uiso 1 1 calc R . . C50 C 0.3527(2) 0.2136(2) 0.15771(13) 0.0257(7) Uani 1 1 d . . . H50A H 0.3711 0.2683 0.1737 0.031 Uiso 1 1 calc R . . C51 C 0.5339(2) 0.27586(19) 0.07358(13) 0.0239(7) Uani 1 1 d . . . C52 C 0.4457(3) 0.2699(2) 0.03639(14) 0.0355(8) Uani 1 1 d . . . H52A H 0.3941 0.2286 0.0414 0.043 Uiso 1 1 calc R . . C53 C 0.4318(3) 0.3234(3) -0.00808(15) 0.0443(10) Uani 1 1 d . . . H53A H 0.3703 0.3190 -0.0330 0.053 Uiso 1 1 calc R . . C54 C 0.5052(3) 0.3826(2) -0.01666(16) 0.0423(10) Uani 1 1 d . . . H54A H 0.4948 0.4195 -0.0471 0.051 Uiso 1 1 calc R . . C55 C 0.5936(3) 0.3881(3) 0.01891(18) 0.0525(11) Uani 1 1 d . . . H55A H 0.6454 0.4284 0.0127 0.063 Uiso 1 1 calc R . . C56 C 0.6091(3) 0.3357(2) 0.06401(17) 0.0450(10) Uani 1 1 d . . . H56A H 0.6711 0.3406 0.0885 0.054 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.01620(10) 0.02179(10) 0.01577(13) -0.00020(11) 0.00473(8) 0.00200(10) Si1 0.0197(4) 0.0260(4) 0.0161(4) -0.0009(4) 0.0048(3) 0.0000(4) P1 0.0184(4) 0.0252(4) 0.0171(4) 0.0016(3) 0.0055(3) 0.0040(3) P2 0.0175(3) 0.0210(3) 0.0190(4) 0.0001(3) 0.0041(3) 0.0012(3) N1 0.0183(12) 0.0237(12) 0.0137(14) -0.0035(11) 0.0040(10) 0.0024(11) C1 0.0294(17) 0.0262(14) 0.0177(18) -0.0017(14) 0.0024(13) 0.0035(14) C2 0.053(2) 0.043(2) 0.025(2) 0.0060(18) 0.0000(17) -0.0108(19) C3 0.075(3) 0.050(2) 0.027(2) 0.012(2) 0.001(2) -0.007(2) C4 0.061(3) 0.042(2) 0.018(2) 0.0005(17) -0.0031(17) 0.018(2) C5 0.0338(19) 0.046(2) 0.026(2) -0.0110(17) -0.0042(15) 0.0131(17) C6 0.0303(17) 0.0372(17) 0.0229(18) -0.0051(17) 0.0041(13) 0.0080(17) C7 0.0247(15) 0.0308(15) 0.0171(17) 0.0036(15) 0.0100(13) 0.0032(14) C8 0.0246(16) 0.0428(18) 0.0217(19) 0.0003(16) 0.0082(13) 0.0016(16) C9 0.0300(18) 0.050(2) 0.038(2) 0.008(2) 0.0127(16) 0.0166(19) C10 0.051(2) 0.043(2) 0.031(2) -0.0006(19) 0.0187(18) 0.019(2) C11 0.038(2) 0.0405(19) 0.032(2) -0.0049(18) 0.0085(16) 0.0106(18) C12 0.0279(17) 0.0361(17) 0.0251(19) -0.0012(16) 0.0077(14) 0.0035(15) C13 0.0217(15) 0.0351(16) 0.0191(18) 0.0019(15) 0.0035(13) -0.0008(15) C14 0.0285(17) 0.0372(17) 0.030(2) 0.0004(17) 0.0098(14) -0.0016(16) C15 0.0297(18) 0.047(2) 0.040(2) -0.0037(19) 0.0150(16) -0.0095(17) C16 0.0310(19) 0.053(2) 0.047(3) -0.013(2) 0.0074(17) -0.0183(19) C17 0.039(2) 0.047(2) 0.038(2) -0.0174(19) 0.0070(17) -0.0115(19) C18 0.0275(17) 0.0421(18) 0.031(2) -0.0072(17) 0.0091(15) -0.0043(16) C19 0.0168(14) 0.0256(14) 0.0178(17) -0.0013(14) 0.0062(12) -0.0003(13) C20 0.0159(13) 0.0298(15) 0.0194(17) -0.0041(15) 0.0041(12) -0.0041(14) C21 0.0168(14) 0.0261(14) 0.0218(18) -0.0024(14) 0.0056(12) -0.0003(13) C22 0.0259(16) 0.0292(15) 0.0230(19) -0.0028(15) 0.0053(14) -0.0012(14) C23 0.0346(18) 0.0310(16) 0.0196(19) 0.0022(15) 0.0083(14) -0.0040(15) C24 0.063(3) 0.0395(19) 0.025(2) 0.0077(17) 0.0149(18) 0.0044(19) C25 0.0316(17) 0.0374(17) 0.0197(19) -0.0076(16) 0.0111(14) -0.0033(16) C26 0.0256(16) 0.0261(15) 0.0224(19) -0.0049(14) 0.0060(13) -0.0030(14) C27 0.0267(16) 0.0249(14) 0.0184(17) 0.0032(14) 0.0036(13) 0.0037(14) C28 0.045(2) 0.0298(16) 0.031(2) 0.0021(16) 0.0159(17) 0.0002(17) C29 0.066(3) 0.0339(18) 0.035(2) -0.0041(18) 0.016(2) 0.0024(19) C30 0.062(3) 0.0306(17) 0.035(2) -0.0022(17) 0.0083(19) -0.0097(19) C31 0.039(2) 0.0410(19) 0.030(2) 0.0039(18) 0.0024(16) -0.0110(18) C32 0.0265(16) 0.0357(17) 0.0211(18) 0.0008(15) 0.0008(13) 0.0038(15) C33 0.0199(15) 0.0445(18) 0.0161(17) 0.0038(16) 0.0068(12) 0.0035(16) C34 0.0279(17) 0.052(2) 0.028(2) 0.0032(18) 0.0056(14) 0.0011(17) C35 0.0316(19) 0.077(3) 0.042(2) -0.001(2) 0.0051(17) -0.016(2) C36 0.0177(17) 0.098(4) 0.048(3) 0.016(3) 0.0054(16) 0.004(2) C37 0.032(2) 0.084(3) 0.043(3) 0.020(2) 0.0113(18) 0.023(2) C38 0.0289(18) 0.056(2) 0.036(2) 0.0116(19) 0.0113(15) 0.0151(18) C39 0.0157(14) 0.0278(15) 0.0230(18) -0.0035(15) 0.0082(12) -0.0020(13) C40 0.0202(15) 0.0295(15) 0.0226(18) -0.0024(15) 0.0034(13) -0.0036(14) C41 0.0196(15) 0.0298(15) 0.0282(19) -0.0095(15) 0.0059(13) -0.0071(14) C42 0.0205(15) 0.0260(16) 0.033(2) -0.0071(16) 0.0090(13) -0.0030(14) C43 0.0189(15) 0.0248(14) 0.0287(19) -0.0015(15) 0.0064(13) -0.0014(14) C44 0.0279(17) 0.0242(15) 0.047(2) -0.0089(16) 0.0009(16) 0.0019(15) C45 0.0185(14) 0.0260(14) 0.0173(17) 0.0052(14) 0.0050(12) 0.0000(13) C46 0.0240(15) 0.0245(14) 0.0217(17) 0.0016(14) 0.0036(12) 0.0031(14) C47 0.0289(17) 0.0308(15) 0.0213(19) 0.0022(15) -0.0002(14) -0.0050(15) C48 0.0195(15) 0.0366(17) 0.035(2) 0.0086(17) 0.0015(13) -0.0037(16) C49 0.0234(16) 0.0324(16) 0.042(2) -0.0017(17) 0.0101(15) 0.0008(15) C50 0.0251(16) 0.0288(15) 0.0242(19) -0.0017(15) 0.0063(13) 0.0032(14) C51 0.0289(16) 0.0227(14) 0.0222(18) -0.0017(14) 0.0107(14) 0.0044(14) C52 0.046(2) 0.0419(19) 0.0181(19) 0.0068(17) 0.0018(15) -0.0018(18) C53 0.048(2) 0.056(2) 0.028(2) 0.007(2) 0.0009(17) 0.010(2) C54 0.058(3) 0.0406(19) 0.031(2) 0.0127(18) 0.0151(19) 0.019(2) C55 0.058(3) 0.050(2) 0.053(3) 0.028(2) 0.020(2) -0.002(2) C56 0.034(2) 0.049(2) 0.051(3) 0.018(2) 0.0054(18) -0.0046(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 N1 2.069(2) . ? Rh1 P1 2.2844(8) . ? Rh1 P2 2.3017(8) . ? Rh1 Si1 2.3148(8) . ? Rh1 H1 1.49(3) . ? Si1 C7 1.893(3) . ? Si1 C13 1.903(3) . ? Si1 C1 1.908(3) . ? Si1 H1 1.83(3) . ? P1 C21 1.818(3) . ? P1 C27 1.819(3) . ? P1 C33 1.821(3) . ? P2 C19 1.817(3) . ? P2 C45 1.819(3) . ? P2 C51 1.820(3) . ? N1 C20 1.401(4) . ? N1 C39 1.402(4) . ? C1 C6 1.389(4) . ? C1 C2 1.395(5) . ? C2 C3 1.379(5) . ? C2 H2A 0.9500 . ? C3 C4 1.377(6) . ? C3 H3A 0.9500 . ? C4 C5 1.371(5) . ? C4 H4A 0.9500 . ? C5 C6 1.384(5) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 C12 1.406(5) . ? C7 C8 1.409(4) . ? C8 C9 1.399(5) . ? C8 H8A 0.9500 . ? C9 C10 1.382(5) . ? C9 H9A 0.9500 . ? C10 C11 1.387(5) . ? C10 H10A 0.9500 . ? C11 C12 1.379(4) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C13 C18 1.394(4) . ? C13 C14 1.397(4) . ? C14 C15 1.385(5) . ? C14 H14A 0.9500 . ? C15 C16 1.374(5) . ? C15 H15A 0.9500 . ? C16 C17 1.375(5) . ? C16 H16A 0.9500 . ? C17 C18 1.391(5) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C19 C39 1.405(4) . ? C19 C43 1.407(4) . ? C20 C26 1.404(4) . ? C20 C21 1.407(4) . ? C21 C22 1.389(4) . ? C22 C23 1.384(4) . ? C22 H22A 0.9500 . ? C23 C25 1.394(4) . ? C23 C24 1.507(5) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.378(5) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? C27 C32 1.391(4) . ? C27 C28 1.393(4) . ? C28 C29 1.384(5) . ? C28 H28A 0.9500 . ? C29 C30 1.393(5) . ? C29 H29A 0.9500 . ? C30 C31 1.362(5) . ? C30 H30A 0.9500 . ? C31 C32 1.376(5) . ? C31 H31A 0.9500 . ? C32 H32A 0.9500 . ? C33 C38 1.382(5) . ? C33 C34 1.400(5) . ? C34 C35 1.392(5) . ? C34 H34A 0.9500 . ? C35 C36 1.382(6) . ? C35 H35A 0.9500 . ? C36 C37 1.375(6) . ? C36 H36A 0.9500 . ? C37 C38 1.388(5) . ? C37 H37A 0.9500 . ? C38 H38A 0.9500 . ? C39 C40 1.391(4) . ? C40 C41 1.380(4) . ? C40 H40A 0.9500 . ? C41 C42 1.389(5) . ? C41 H41A 0.9500 . ? C42 C43 1.386(5) . ? C42 C44 1.500(4) . ? C43 H43A 0.9500 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C46 1.396(4) . ? C45 C50 1.399(4) . ? C46 C47 1.376(4) . ? C46 H46A 0.9500 . ? C47 C48 1.378(4) . ? C47 H47A 0.9500 . ? C48 C49 1.383(5) . ? C48 H48A 0.9500 . ? C49 C50 1.382(4) . ? C49 H49A 0.9500 . ? C50 H50A 0.9500 . ? C51 C52 1.382(5) . ? C51 C56 1.396(4) . ? C52 C53 1.382(5) . ? C52 H52A 0.9500 . ? C53 C54 1.365(5) . ? C53 H53A 0.9500 . ? C54 C55 1.361(6) . ? C54 H54A 0.9500 . ? C55 C56 1.384(5) . ? C55 H55A 0.9500 . ? C56 H56A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Rh1 P1 82.22(7) . . ? N1 Rh1 P2 79.98(7) . . ? P1 Rh1 P2 159.68(3) . . ? N1 Rh1 Si1 141.65(7) . . ? P1 Rh1 Si1 99.82(3) . . ? P2 Rh1 Si1 100.22(3) . . ? N1 Rh1 H1 166.1(11) . . ? P1 Rh1 H1 94.1(12) . . ? P2 Rh1 H1 100.9(12) . . ? Si1 Rh1 H1 52.2(11) . . ? C7 Si1 C13 106.55(14) . . ? C7 Si1 C1 102.98(14) . . ? C13 Si1 C1 105.95(14) . . ? C7 Si1 Rh1 117.79(10) . . ? C13 Si1 Rh1 105.49(10) . . ? C1 Si1 Rh1 117.14(10) . . ? C7 Si1 H1 95.3(9) . . ? C13 Si1 H1 145.5(9) . . ? C1 Si1 H1 94.3(10) . . ? Rh1 Si1 H1 40.0(9) . . ? C21 P1 C27 106.56(14) . . ? C21 P1 C33 102.14(14) . . ? C27 P1 C33 107.08(15) . . ? C21 P1 Rh1 100.37(10) . . ? C27 P1 Rh1 118.27(11) . . ? C33 P1 Rh1 119.99(11) . . ? C19 P2 C45 106.63(13) . . ? C19 P2 C51 105.54(14) . . ? C45 P2 C51 102.42(14) . . ? C19 P2 Rh1 100.78(10) . . ? C45 P2 Rh1 108.14(10) . . ? C51 P2 Rh1 131.42(10) . . ? C20 N1 C39 120.7(2) . . ? C20 N1 Rh1 119.64(19) . . ? C39 N1 Rh1 119.7(2) . . ? C6 C1 C2 116.9(3) . . ? C6 C1 Si1 122.6(2) . . ? C2 C1 Si1 120.4(3) . . ? C3 C2 C1 121.4(4) . . ? C3 C2 H2A 119.3 . . ? C1 C2 H2A 119.3 . . ? C4 C3 C2 120.4(4) . . ? C4 C3 H3A 119.8 . . ? C2 C3 H3A 119.8 . . ? C5 C4 C3 119.4(4) . . ? C5 C4 H4A 120.3 . . ? C3 C4 H4A 120.3 . . ? C4 C5 C6 120.1(4) . . ? C4 C5 H5A 119.9 . . ? C6 C5 H5A 119.9 . . ? C5 C6 C1 121.7(3) . . ? C5 C6 H6A 119.1 . . ? C1 C6 H6A 119.1 . . ? C12 C7 C8 116.7(3) . . ? C12 C7 Si1 120.2(2) . . ? C8 C7 Si1 123.1(3) . . ? C9 C8 C7 120.9(3) . . ? C9 C8 H8A 119.5 . . ? C7 C8 H8A 119.5 . . ? C10 C9 C8 120.4(3) . . ? C10 C9 H9A 119.8 . . ? C8 C9 H9A 119.8 . . ? C9 C10 C11 119.8(3) . . ? C9 C10 H10A 120.1 . . ? C11 C10 H10A 120.1 . . ? C12 C11 C10 119.8(4) . . ? C12 C11 H11A 120.1 . . ? C10 C11 H11A 120.1 . . ? C11 C12 C7 122.4(3) . . ? C11 C12 H12A 118.8 . . ? C7 C12 H12A 118.8 . . ? C18 C13 C14 117.3(3) . . ? C18 C13 Si1 121.4(2) . . ? C14 C13 Si1 121.3(3) . . ? C15 C14 C13 121.5(3) . . ? C15 C14 H14A 119.2 . . ? C13 C14 H14A 119.2 . . ? C16 C15 C14 120.0(3) . . ? C16 C15 H15A 120.0 . . ? C14 C15 H15A 120.0 . . ? C15 C16 C17 120.0(3) . . ? C15 C16 H16A 120.0 . . ? C17 C16 H16A 120.0 . . ? C16 C17 C18 120.2(3) . . ? C16 C17 H17A 119.9 . . ? C18 C17 H17A 119.9 . . ? C17 C18 C13 121.1(3) . . ? C17 C18 H18A 119.5 . . ? C13 C18 H18A 119.5 . . ? C39 C19 C43 120.6(3) . . ? C39 C19 P2 113.8(2) . . ? C43 C19 P2 125.6(2) . . ? N1 C20 C26 125.4(3) . . ? N1 C20 C21 118.1(3) . . ? C26 C20 C21 116.3(3) . . ? C22 C21 C20 121.1(3) . . ? C22 C21 P1 123.9(2) . . ? C20 C21 P1 115.0(2) . . ? C23 C22 C21 122.3(3) . . ? C23 C22 H22A 118.9 . . ? C21 C22 H22A 118.9 . . ? C22 C23 C25 116.4(3) . . ? C22 C23 C24 122.6(3) . . ? C25 C23 C24 121.0(3) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C23 122.4(3) . . ? C26 C25 H25A 118.8 . . ? C23 C25 H25A 118.8 . . ? C25 C26 C20 121.3(3) . . ? C25 C26 H26A 119.3 . . ? C20 C26 H26A 119.3 . . ? C32 C27 C28 118.7(3) . . ? C32 C27 P1 121.6(2) . . ? C28 C27 P1 119.5(2) . . ? C29 C28 C27 120.0(3) . . ? C29 C28 H28A 120.0 . . ? C27 C28 H28A 120.0 . . ? C28 C29 C30 120.4(3) . . ? C28 C29 H29A 119.8 . . ? C30 C29 H29A 119.8 . . ? C31 C30 C29 119.3(3) . . ? C31 C30 H30A 120.3 . . ? C29 C30 H30A 120.3 . . ? C30 C31 C32 121.0(3) . . ? C30 C31 H31A 119.5 . . ? C32 C31 H31A 119.5 . . ? C31 C32 C27 120.6(3) . . ? C31 C32 H32A 119.7 . . ? C27 C32 H32A 119.7 . . ? C38 C33 C34 119.3(3) . . ? C38 C33 P1 125.6(3) . . ? C34 C33 P1 115.1(2) . . ? C35 C34 C33 120.0(4) . . ? C35 C34 H34A 120.0 . . ? C33 C34 H34A 120.0 . . ? C36 C35 C34 119.8(4) . . ? C36 C35 H35A 120.1 . . ? C34 C35 H35A 120.1 . . ? C37 C36 C35 120.2(4) . . ? C37 C36 H36A 119.9 . . ? C35 C36 H36A 119.9 . . ? C36 C37 C38 120.5(4) . . ? C36 C37 H37A 119.8 . . ? C38 C37 H37A 119.8 . . ? C33 C38 C37 120.1(4) . . ? C33 C38 H38A 119.9 . . ? C37 C38 H38A 119.9 . . ? C40 C39 N1 124.9(3) . . ? C40 C39 C19 117.5(3) . . ? N1 C39 C19 117.4(3) . . ? C41 C40 C39 120.9(3) . . ? C41 C40 H40A 119.5 . . ? C39 C40 H40A 119.5 . . ? C40 C41 C42 122.3(3) . . ? C40 C41 H41A 118.8 . . ? C42 C41 H41A 118.8 . . ? C43 C42 C41 117.3(3) . . ? C43 C42 C44 122.4(3) . . ? C41 C42 C44 120.3(3) . . ? C42 C43 C19 121.2(3) . . ? C42 C43 H43A 119.4 . . ? C19 C43 H43A 119.4 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C46 C45 C50 118.7(3) . . ? C46 C45 P2 119.4(2) . . ? C50 C45 P2 121.8(2) . . ? C47 C46 C45 120.9(3) . . ? C47 C46 H46A 119.6 . . ? C45 C46 H46A 119.6 . . ? C46 C47 C48 119.9(3) . . ? C46 C47 H47A 120.1 . . ? C48 C47 H47A 120.1 . . ? C47 C48 C49 120.2(3) . . ? C47 C48 H48A 119.9 . . ? C49 C48 H48A 119.9 . . ? C50 C49 C48 120.3(3) . . ? C50 C49 H49A 119.9 . . ? C48 C49 H49A 119.9 . . ? C49 C50 C45 120.0(3) . . ? C49 C50 H50A 120.0 . . ? C45 C50 H50A 120.0 . . ? C52 C51 C56 118.0(3) . . ? C52 C51 P2 121.7(2) . . ? C56 C51 P2 120.3(3) . . ? C53 C52 C51 120.6(3) . . ? C53 C52 H52A 119.7 . . ? C51 C52 H52A 119.7 . . ? C54 C53 C52 120.9(4) . . ? C54 C53 H53A 119.6 . . ? C52 C53 H53A 119.6 . . ? C55 C54 C53 119.3(4) . . ? C55 C54 H54A 120.3 . . ? C53 C54 H54A 120.3 . . ? C54 C55 C56 121.0(4) . . ? C54 C55 H55A 119.5 . . ? C56 C55 H55A 119.5 . . ? C55 C56 C51 120.2(4) . . ? C55 C56 H56A 119.9 . . ? C51 C56 H56A 119.9 . . ? _diffrn_measured_fraction_theta_max 0.881 _diffrn_reflns_theta_full 68.08 _diffrn_measured_fraction_theta_full 0.881 _refine_diff_density_max 0.481 _refine_diff_density_min -0.292 _refine_diff_density_rms 0.067 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.500 408 101 ' ' 2 0.000 0.500 1.000 408 101 ' ' _platon_squeeze_details ; ;