# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Johnson, Kevin' 'Hannon, Matt' 'Ritch, Jamie' 'Hayes, Paul' _publ_contact_author_name 'Hayes, Paul' _publ_contact_author_email p.hayes@uleth.ca _publ_section_title ; Thermally stable rare earth dialkyl complexes supported by a novel bis(phosphinimine)pyrrole ligand ; # Attachment '- Dalton Structures - Paul G Hayes.cif' data_ph11018a _database_code_depnum_ccdc_archive 'CCDC 861266' #TrackingRef '- Dalton Structures - Paul G Hayes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H45 N3 P2' _chemical_formula_weight 701.79 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.9263(2) _cell_length_b 14.5326(2) _cell_length_c 14.8331(3) _cell_angle_alpha 112.5870(10) _cell_angle_beta 103.5210(10) _cell_angle_gamma 108.7700(10) _cell_volume 2223.03(8) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9997 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 25.66 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.048 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 744 _exptl_absorpt_coefficient_mu 0.129 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9623 _exptl_absorpt_correction_T_max 0.9872 _exptl_absorpt_process_details 'Otwinowski & Minor, 1997' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 APEX II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36845 _diffrn_reflns_av_R_equivalents 0.0344 _diffrn_reflns_av_sigmaI/netI 0.0435 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 27.54 _reflns_number_total 10171 _reflns_number_gt 7370 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0610P)^2^+2.5948P] 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 10171 _refine_ls_number_parameters 439 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.0950 _refine_ls_R_factor_gt 0.0709 _refine_ls_wR_factor_ref 0.1821 _refine_ls_wR_factor_gt 0.1723 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.050 _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 N1 N 0.50654(18) 0.14634(17) -0.06576(16) 0.0294(4) Uani 1 1 d . . . H1A H 0.5296 0.0935 -0.0809 0.035 Uiso 1 1 calc R . . C1 C 0.5385(2) 0.2299(2) -0.0902(2) 0.0353(6) Uani 1 1 d . A . C2 C 0.4852(3) 0.2960(2) -0.0531(3) 0.0472(7) Uani 1 1 d . . . H2A H 0.4922 0.3602 -0.0592 0.057 Uiso 1 1 calc R . . C3 C 0.4188(3) 0.2511(2) -0.0048(2) 0.0390(6) Uani 1 1 d . . . H3A H 0.3726 0.2794 0.0280 0.047 Uiso 1 1 calc R . . C4 C 0.4329(2) 0.1580(2) -0.0139(2) 0.0310(5) Uani 1 1 d . . . C5A C 0.7065(5) 0.3830(5) -0.1224(5) 0.0384(17) Uiso 0.60 1 d PD A 1 C6A C 0.8236(5) 0.4306(5) -0.0478(5) 0.0602(15) Uiso 0.60 1 d PD A 1 H6AA H 0.8530 0.3855 -0.0291 0.072 Uiso 0.60 1 calc PR A 1 C7A C 0.8969(7) 0.5453(5) -0.0011(6) 0.0777(19) Uiso 0.60 1 d PD A 1 H7AA H 0.9769 0.5778 0.0493 0.093 Uiso 0.60 1 calc PR A 1 C8A C 0.8548(6) 0.6138(6) -0.0270(6) 0.0610(18) Uiso 0.60 1 d PD A 1 H8AA H 0.9037 0.6925 0.0086 0.073 Uiso 0.60 1 calc PR A 1 C9A C 0.7428(5) 0.5652(4) -0.1039(4) 0.0524(14) Uiso 0.60 1 d PD A 1 H9AA H 0.7148 0.6089 -0.1265 0.063 Uiso 0.60 1 calc PR A 1 C10A C 0.6696(5) 0.4516(4) -0.1492(4) 0.0427(12) Uiso 0.60 1 d PD A 1 H10A H 0.5906 0.4196 -0.2010 0.051 Uiso 0.60 1 calc PR A 1 C5B C 0.7238(8) 0.3962(7) -0.0981(6) 0.030(2) Uiso 0.40 1 d PD A 2 C6B C 0.8073(6) 0.4534(6) 0.0051(6) 0.0479(18) Uiso 0.40 1 d PD A 2 H6BA H 0.8128 0.4132 0.0421 0.058 Uiso 0.40 1 calc PR A 2 C7B C 0.8829(8) 0.5651(7) 0.0571(8) 0.066(2) Uiso 0.40 1 d PD A 2 H7BA H 0.9358 0.6026 0.1304 0.079 Uiso 0.40 1 calc PR A 2 C8B C 0.8818(10) 0.6208(8) 0.0047(8) 0.061(3) Uiso 0.40 1 d PD A 2 H8BA H 0.9412 0.6963 0.0375 0.073 Uiso 0.40 1 calc PR A 2 C9B C 0.7961(10) 0.5710(8) -0.0961(8) 0.069(3) Uiso 0.40 1 d PD A 2 H9BA H 0.7903 0.6141 -0.1297 0.083 Uiso 0.40 1 calc PR A 2 C10B C 0.7166(9) 0.4561(7) -0.1500(7) 0.060(3) Uiso 0.40 1 d PD A 2 H10B H 0.6588 0.4203 -0.2212 0.073 Uiso 0.40 1 calc PR A 2 P1 P 0.62459(7) 0.23957(6) -0.16747(6) 0.03579(18) Uani 1 1 d . . . C11A C 0.5078(6) 0.1777(6) -0.3108(6) 0.032(2) Uiso 0.50 1 d PD A 1 C12A C 0.5365(5) 0.2161(5) -0.3788(4) 0.0432(13) Uiso 0.50 1 d PD A 1 H12A H 0.6125 0.2767 -0.3538 0.052 Uiso 0.50 1 calc PR A 1 C13A C 0.4533(6) 0.1653(5) -0.4836(5) 0.0561(16) Uiso 0.50 1 d PD A 1 H13A H 0.4702 0.1910 -0.5310 0.067 Uiso 0.50 1 calc PR A 1 C14A C 0.3446(7) 0.0755(7) -0.5159(7) 0.055(3) Uiso 0.50 1 d PD A 1 H14A H 0.2882 0.0384 -0.5878 0.065 Uiso 0.50 1 calc PR A 1 C15A C 0.3146(6) 0.0382(5) -0.4516(4) 0.0490(14) Uiso 0.50 1 d PD A 1 H15A H 0.2384 -0.0224 -0.4768 0.059 Uiso 0.50 1 calc PR A 1 C16A C 0.3973(5) 0.0900(5) -0.3476(4) 0.0444(13) Uiso 0.50 1 d PD A 1 H16A H 0.3776 0.0646 -0.3007 0.053 Uiso 0.50 1 calc PR A 1 C11B C 0.5288(7) 0.1951(6) -0.2910(6) 0.033(2) Uiso 0.50 1 d PD A 2 C12B C 0.5303(5) 0.1109(4) -0.3775(4) 0.0372(12) Uiso 0.50 1 d PD A 2 H12B H 0.5869 0.0838 -0.3652 0.045 Uiso 0.50 1 calc PR A 2 C13B C 0.4496(5) 0.0672(5) -0.4809(5) 0.0483(14) Uiso 0.50 1 d PD A 2 H13B H 0.4514 0.0094 -0.5383 0.058 Uiso 0.50 1 calc PR A 2 C14B C 0.3662(8) 0.1050(8) -0.5034(7) 0.054(2) Uiso 0.50 1 d PD A 2 H14B H 0.3155 0.0793 -0.5747 0.065 Uiso 0.50 1 calc PR A 2 C15B C 0.3611(6) 0.1827(6) -0.4152(5) 0.0583(17) Uiso 0.50 1 d PD A 2 H15B H 0.2994 0.2042 -0.4269 0.070 Uiso 0.50 1 calc PR A 2 C16B C 0.4419(5) 0.2296(5) -0.3116(5) 0.0477(14) Uiso 0.50 1 d PD A 2 H16B H 0.4381 0.2856 -0.2543 0.057 Uiso 0.50 1 calc PR A 2 P2 P 0.37190(6) 0.06655(5) 0.03434(5) 0.02885(16) Uani 1 1 d . B . C17 C 0.2673(2) -0.0688(2) -0.0826(2) 0.0321(5) Uani 1 1 d . . . C18 C 0.2221(2) -0.1623(2) -0.0711(2) 0.0362(6) Uani 1 1 d . . . H18A H 0.2505 -0.1560 -0.0028 0.043 Uiso 1 1 calc R . . C19 C 0.1363(3) -0.2640(2) -0.1584(2) 0.0448(7) Uani 1 1 d . . . H19A H 0.1057 -0.3279 -0.1503 0.054 Uiso 1 1 calc R . . C20 C 0.0943(3) -0.2735(3) -0.2586(2) 0.0499(8) Uani 1 1 d . . . H20A H 0.0347 -0.3436 -0.3187 0.060 Uiso 1 1 calc R . . C21 C 0.1390(3) -0.1815(3) -0.2703(2) 0.0451(7) Uani 1 1 d . . . H21A H 0.1106 -0.1883 -0.3388 0.054 Uiso 1 1 calc R . . C22 C 0.2255(2) -0.0785(2) -0.1829(2) 0.0382(6) Uani 1 1 d . . . H22A H 0.2560 -0.0150 -0.1914 0.046 Uiso 1 1 calc R . . C23 C 0.2799(2) 0.1233(2) 0.0894(2) 0.0325(5) Uani 1 1 d . . . C24 C 0.1699(3) 0.1020(3) 0.0235(2) 0.0428(7) Uani 1 1 d . . . H24A H 0.1429 0.0591 -0.0519 0.051 Uiso 1 1 calc R . . C25 C 0.0984(3) 0.1421(3) 0.0654(3) 0.0501(8) Uani 1 1 d . . . H25A H 0.0233 0.1272 0.0188 0.060 Uiso 1 1 calc R . . C26 C 0.1351(3) 0.2026(3) 0.1728(3) 0.0582(9) Uani 1 1 d . . . H26A H 0.0857 0.2295 0.2017 0.070 Uiso 1 1 calc R . . C27 C 0.2426(4) 0.2242(4) 0.2385(3) 0.0830(14) Uani 1 1 d . . . H27A H 0.2685 0.2668 0.3138 0.100 Uiso 1 1 calc R . . C28 C 0.3159(3) 0.1851(3) 0.1978(3) 0.0669(11) Uani 1 1 d . . . H28A H 0.3912 0.2014 0.2453 0.080 Uiso 1 1 calc R . . N2 N 0.6958(2) 0.17277(19) -0.15682(19) 0.0381(5) Uani 1 1 d . A . C29 C 0.7786(3) 0.1584(2) -0.1987(2) 0.0395(6) Uani 1 1 d . . . C30 C 0.8254(3) 0.0878(3) -0.1829(2) 0.0417(7) Uani 1 1 d . A . H30A H 0.7987 0.0515 -0.1455 0.050 Uiso 1 1 calc R . . C31 C 0.9096(3) 0.0706(3) -0.2208(2) 0.0474(7) Uani 1 1 d . . . H31A H 0.9404 0.0237 -0.2074 0.057 Uiso 1 1 calc R A . C32 C 0.9506(3) 0.1195(3) -0.2780(3) 0.0492(8) Uani 1 1 d . A . C33 C 0.9043(3) 0.1889(3) -0.2932(3) 0.0607(10) Uani 1 1 d . . . H33A H 0.9306 0.2241 -0.3315 0.073 Uiso 1 1 calc R A . C34 C 0.8217(3) 0.2086(3) -0.2550(3) 0.0560(9) Uani 1 1 d . A . H34A H 0.7933 0.2573 -0.2671 0.067 Uiso 1 1 calc R . . C35 C 1.0081(4) -0.0223(4) -0.3833(3) 0.0740(12) Uani 1 1 d . A . H35A H 0.9281 -0.0610 -0.4411 0.111 Uiso 1 1 calc R . . H35B H 1.0076 -0.0549 -0.3364 0.111 Uiso 1 1 calc R . . H35C H 1.0661 -0.0309 -0.4140 0.111 Uiso 1 1 calc R . . C36 C 1.0424(3) 0.0998(4) -0.3198(3) 0.0617(10) Uani 1 1 d . . . H36A H 1.0467 0.1314 -0.3688 0.074 Uiso 1 1 calc R A . C37 C 1.1659(4) 0.1620(4) -0.2293(3) 0.0778(12) Uani 1 1 d . A . H37A H 1.1868 0.2416 -0.1890 0.117 Uiso 1 1 calc R . . H37B H 1.2248 0.1542 -0.2590 0.117 Uiso 1 1 calc R . . H37C H 1.1658 0.1305 -0.1816 0.117 Uiso 1 1 calc R . . N3 N 0.45873(19) 0.04807(17) 0.11147(16) 0.0325(5) Uani 1 1 d . . . C38A C 0.5447(7) 0.1273(6) 0.2191(6) 0.031(2) Uiso 0.50 1 d PD B 1 C39A C 0.6135(6) 0.2410(5) 0.2534(5) 0.038(2) Uiso 0.50 1 d PD B 1 H39A H 0.6046 0.2672 0.2039 0.046 Uiso 0.50 1 calc PR B 1 C40A C 0.6943(6) 0.3152(5) 0.3593(5) 0.0396(16) Uiso 0.50 1 d PD B 1 H40A H 0.7370 0.3923 0.3815 0.047 Uiso 0.50 1 calc PR B 1 C41A C 0.7145(6) 0.2802(5) 0.4333(5) 0.0466(16) Uiso 0.50 1 d PD B 1 C42A C 0.6528(5) 0.1681(5) 0.3966(5) 0.0466(15) Uiso 0.50 1 d PD B 1 H42A H 0.6682 0.1402 0.4439 0.056 Uiso 0.50 1 calc PR B 1 C43A C 0.5699(6) 0.0955(5) 0.2944(4) 0.0395(15) Uiso 0.50 1 d PD B 1 H43A H 0.5272 0.0189 0.2738 0.047 Uiso 0.50 1 calc PR B 1 C44A C 0.9332(7) 0.4022(7) 0.5593(6) 0.0647(19) Uiso 0.50 1 d PD B 1 H44A H 0.9892 0.4405 0.6344 0.097 Uiso 0.50 1 calc PR B 1 H44B H 0.9488 0.4542 0.5316 0.097 Uiso 0.50 1 calc PR B 1 H44C H 0.9439 0.3377 0.5172 0.097 Uiso 0.50 1 calc PR B 1 C45A C 0.8027(7) 0.3610(7) 0.5511(6) 0.066(2) Uiso 0.50 1 d PD B 1 H45A H 0.7944 0.3155 0.5876 0.080 Uiso 0.50 1 calc PR B 1 C46A C 0.7777(9) 0.4531(8) 0.6086(8) 0.071(2) Uiso 0.50 1 d PD B 1 H46A H 0.8315 0.4948 0.6847 0.107 Uiso 0.50 1 calc PR B 1 H46B H 0.6945 0.4225 0.6006 0.107 Uiso 0.50 1 calc PR B 1 H46C H 0.7904 0.5036 0.5791 0.107 Uiso 0.50 1 calc PR B 1 C38B C 0.5439(7) 0.1402(6) 0.2121(6) 0.031(2) Uiso 0.50 1 d PD B 2 C39B C 0.6190(6) 0.2449(5) 0.2329(5) 0.0354(18) Uiso 0.50 1 d PD B 2 H39B H 0.6161 0.2599 0.1756 0.042 Uiso 0.50 1 calc PR B 2 C40B C 0.6976(6) 0.3272(5) 0.3351(5) 0.0391(16) Uiso 0.50 1 d PD B 2 H40B H 0.7477 0.3987 0.3471 0.047 Uiso 0.50 1 calc PR B 2 C41B C 0.7073(6) 0.3108(5) 0.4224(5) 0.0438(15) Uiso 0.50 1 d PD B 2 C42B C 0.6323(6) 0.2049(5) 0.4012(5) 0.0501(16) Uiso 0.50 1 d PD B 2 H42B H 0.6376 0.1901 0.4588 0.060 Uiso 0.50 1 calc PR B 2 C43B C 0.5492(6) 0.1197(6) 0.2979(5) 0.0453(17) Uiso 0.50 1 d PD B 2 H43B H 0.4969 0.0488 0.2857 0.054 Uiso 0.50 1 calc PR B 2 C44B C 0.8849(14) 0.3781(13) 0.5856(12) 0.140(5) Uiso 0.50 1 d PD B 2 H44D H 0.9210 0.3494 0.5372 0.209 Uiso 0.50 1 calc PR B 2 H44E H 0.8447 0.3207 0.6020 0.209 Uiso 0.50 1 calc PR B 2 H44F H 0.9474 0.4456 0.6520 0.209 Uiso 0.50 1 calc PR B 2 C45B C 0.7957(7) 0.4063(7) 0.5333(6) 0.066(2) Uiso 0.50 1 d PD B 2 H45B H 0.8442 0.4650 0.5202 0.079 Uiso 0.50 1 calc PR B 2 C46B C 0.7348(15) 0.4599(15) 0.5947(14) 0.159(7) Uiso 0.50 1 d PD B 2 H46D H 0.6775 0.4707 0.5486 0.239 Uiso 0.50 1 calc PR B 2 H46E H 0.7947 0.5327 0.6570 0.239 Uiso 0.50 1 calc PR B 2 H46F H 0.6924 0.4113 0.6187 0.239 Uiso 0.50 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0307(11) 0.0318(10) 0.0328(11) 0.0172(9) 0.0169(9) 0.0181(9) C1 0.0377(14) 0.0361(13) 0.0460(15) 0.0250(12) 0.0257(12) 0.0208(12) C2 0.061(2) 0.0438(16) 0.074(2) 0.0404(16) 0.0482(18) 0.0360(15) C3 0.0471(16) 0.0413(15) 0.0515(17) 0.0281(13) 0.0347(14) 0.0291(13) C4 0.0318(13) 0.0332(13) 0.0329(13) 0.0167(11) 0.0169(11) 0.0173(11) P1 0.0393(4) 0.0392(4) 0.0469(4) 0.0276(3) 0.0284(3) 0.0228(3) P2 0.0311(3) 0.0309(3) 0.0303(3) 0.0161(3) 0.0168(3) 0.0165(3) C17 0.0270(13) 0.0388(14) 0.0330(13) 0.0165(11) 0.0141(10) 0.0183(11) C18 0.0341(14) 0.0397(14) 0.0369(14) 0.0175(12) 0.0175(12) 0.0188(12) C19 0.0383(16) 0.0392(15) 0.0504(17) 0.0175(13) 0.0195(14) 0.0153(13) C20 0.0366(16) 0.0461(17) 0.0418(17) 0.0049(14) 0.0103(13) 0.0163(14) C21 0.0411(16) 0.0549(18) 0.0338(15) 0.0157(13) 0.0102(12) 0.0273(15) C22 0.0398(15) 0.0445(15) 0.0349(14) 0.0199(12) 0.0154(12) 0.0242(13) C23 0.0343(14) 0.0327(13) 0.0384(14) 0.0189(11) 0.0223(11) 0.0175(11) C24 0.0411(16) 0.0512(17) 0.0456(16) 0.0254(14) 0.0220(13) 0.0269(14) C25 0.0395(17) 0.0545(18) 0.071(2) 0.0349(17) 0.0293(16) 0.0281(15) C26 0.049(2) 0.058(2) 0.074(2) 0.0250(18) 0.0413(18) 0.0309(17) C27 0.077(3) 0.110(3) 0.048(2) 0.012(2) 0.033(2) 0.056(3) C28 0.051(2) 0.094(3) 0.0420(18) 0.0130(18) 0.0204(16) 0.043(2) N2 0.0431(13) 0.0463(13) 0.0476(13) 0.0314(11) 0.0303(11) 0.0274(11) C29 0.0410(15) 0.0496(16) 0.0466(16) 0.0302(14) 0.0277(13) 0.0267(13) C30 0.0528(18) 0.0549(17) 0.0449(16) 0.0345(14) 0.0307(14) 0.0355(15) C31 0.0586(19) 0.069(2) 0.0512(17) 0.0412(16) 0.0329(15) 0.0492(18) C32 0.0520(18) 0.074(2) 0.0530(18) 0.0418(17) 0.0348(16) 0.0416(17) C33 0.068(2) 0.092(3) 0.091(3) 0.074(2) 0.061(2) 0.057(2) C34 0.067(2) 0.075(2) 0.088(3) 0.065(2) 0.058(2) 0.052(2) C35 0.090(3) 0.113(3) 0.069(2) 0.053(2) 0.055(2) 0.076(3) C36 0.072(2) 0.105(3) 0.066(2) 0.061(2) 0.051(2) 0.066(2) C37 0.067(3) 0.120(4) 0.084(3) 0.058(3) 0.049(2) 0.063(3) N3 0.0331(11) 0.0312(11) 0.0302(11) 0.0130(9) 0.0126(9) 0.0144(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C1 1.364(3) . ? N1 C4 1.369(3) . ? C1 C2 1.377(4) . ? C1 P1 1.787(3) . ? C2 C3 1.400(4) . ? C3 C4 1.384(4) . ? C4 P2 1.794(3) . ? C5A C10A 1.380(6) . ? C5A C6A 1.396(7) . ? C5A P1 1.758(6) . ? C6A C7A 1.394(7) . ? C7A C8A 1.407(7) . ? C8A C9A 1.359(7) . ? C9A C10A 1.384(6) . ? C5B C6B 1.368(8) . ? C5B C10B 1.376(8) . ? C5B P1 1.895(8) . ? C6B C7B 1.359(8) . ? C7B C8B 1.322(8) . ? C8B C9B 1.366(9) . ? C9B C10B 1.402(8) . ? P1 N2 1.562(2) . ? P1 C11B 1.680(7) . ? P1 C11A 1.940(7) . ? C11A C16A 1.376(7) . ? C11A C12A 1.392(7) . ? C12A C13A 1.394(7) . ? C13A C14A 1.391(8) . ? C14A C15A 1.337(7) . ? C15A C16A 1.381(6) . ? C11B C16B 1.388(7) . ? C11B C12B 1.401(7) . ? C12B C13B 1.386(6) . ? C13B C14B 1.389(7) . ? C14B C15B 1.394(7) . ? C15B C16B 1.379(7) . ? P2 N3 1.572(2) . ? P2 C17 1.810(3) . ? P2 C23 1.826(3) . ? C17 C18 1.390(4) . ? C17 C22 1.392(4) . ? C18 C19 1.377(4) . ? C19 C20 1.392(4) . ? C20 C21 1.372(5) . ? C21 C22 1.387(4) . ? C23 C28 1.371(4) . ? C23 C24 1.381(4) . ? C24 C25 1.386(4) . ? C25 C26 1.356(5) . ? C26 C27 1.353(5) . ? C27 C28 1.391(5) . ? N2 C29 1.390(3) . ? C29 C34 1.401(4) . ? C29 C30 1.411(4) . ? C30 C31 1.385(4) . ? C31 C32 1.392(4) . ? C32 C33 1.387(4) . ? C32 C36 1.517(4) . ? C33 C34 1.378(4) . ? C35 C36 1.499(6) . ? C36 C37 1.518(5) . ? N3 C38B 1.408(8) . ? N3 C38A 1.430(8) . ? C38A C43A 1.374(7) . ? C38A C39A 1.405(7) . ? C39A C40A 1.388(7) . ? C40A C41A 1.383(7) . ? C41A C42A 1.366(7) . ? C41A C45A 1.537(9) . ? C42A C43A 1.358(6) . ? C44A C45A 1.555(10) . ? C45A C46A 1.468(11) . ? C38B C39B 1.379(7) . ? C38B C43B 1.406(7) . ? C39B C40B 1.367(7) . ? C40B C41B 1.388(7) . ? C41B C42B 1.390(7) . ? C41B C45B 1.512(9) . ? C42B C43B 1.398(7) . ? C44B C45B 1.494(13) . ? C45B C46B 1.496(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 N1 C4 109.0(2) . . ? N1 C1 C2 108.3(2) . . ? N1 C1 P1 123.66(19) . . ? C2 C1 P1 127.8(2) . . ? C1 C2 C3 107.4(2) . . ? C4 C3 C2 107.3(2) . . ? N1 C4 C3 107.9(2) . . ? N1 C4 P2 123.62(18) . . ? C3 C4 P2 128.42(19) . . ? C10A C5A C6A 118.0(6) . . ? C10A C5A P1 128.9(5) . . ? C6A C5A P1 113.1(4) . . ? C7A C6A C5A 119.2(6) . . ? C6A C7A C8A 121.3(7) . . ? C9A C8A C7A 118.8(6) . . ? C8A C9A C10A 119.7(6) . . ? C5A C10A C9A 122.8(6) . . ? C6B C5B C10B 117.6(8) . . ? C6B C5B P1 120.9(6) . . ? C10B C5B P1 121.5(6) . . ? C7B C6B C5B 123.1(8) . . ? C8B C7B C6B 119.3(9) . . ? C7B C8B C9B 120.6(10) . . ? C8B C9B C10B 120.2(9) . . ? C5B C10B C9B 118.9(9) . . ? N2 P1 C11B 117.2(2) . . ? N2 P1 C5A 118.0(2) . . ? C11B P1 C5A 100.8(3) . . ? N2 P1 C1 106.27(12) . . ? C11B P1 C1 107.0(3) . . ? C5A P1 C1 106.7(2) . . ? N2 P1 C5B 113.2(3) . . ? C11B P1 C5B 109.6(3) . . ? C1 P1 C5B 102.2(3) . . ? N2 P1 C11A 115.0(2) . . ? C5A P1 C11A 104.9(3) . . ? C1 P1 C11A 104.9(2) . . ? C5B P1 C11A 113.7(3) . . ? C16A C11A C12A 119.7(6) . . ? C16A C11A P1 119.1(5) . . ? C12A C11A P1 121.2(5) . . ? C11A C12A C13A 119.9(6) . . ? C14A C13A C12A 117.2(6) . . ? C15A C14A C13A 123.8(8) . . ? C14A C15A C16A 118.3(6) . . ? C11A C16A C15A 121.0(6) . . ? C16B C11B C12B 118.3(6) . . ? C16B C11B P1 123.9(5) . . ? C12B C11B P1 117.6(5) . . ? C13B C12B C11B 120.3(6) . . ? C12B C13B C14B 122.2(6) . . ? C13B C14B C15B 116.0(7) . . ? C16B C15B C14B 122.8(7) . . ? C15B C16B C11B 120.1(6) . . ? N3 P2 C4 119.37(12) . . ? N3 P2 C17 108.00(12) . . ? C4 P2 C17 106.50(12) . . ? N3 P2 C23 114.66(12) . . ? C4 P2 C23 101.75(11) . . ? C17 P2 C23 105.49(12) . . ? C18 C17 C22 119.7(2) . . ? C18 C17 P2 119.7(2) . . ? C22 C17 P2 120.5(2) . . ? C19 C18 C17 120.1(3) . . ? C18 C19 C20 120.1(3) . . ? C21 C20 C19 119.9(3) . . ? C20 C21 C22 120.6(3) . . ? C21 C22 C17 119.6(3) . . ? C28 C23 C24 117.9(3) . . ? C28 C23 P2 121.0(2) . . ? C24 C23 P2 121.1(2) . . ? C23 C24 C25 121.1(3) . . ? C26 C25 C24 120.3(3) . . ? C27 C26 C25 119.4(3) . . ? C26 C27 C28 121.2(3) . . ? C23 C28 C27 120.2(3) . . ? C29 N2 P1 128.82(19) . . ? N2 C29 C34 126.1(3) . . ? N2 C29 C30 117.7(2) . . ? C34 C29 C30 116.2(2) . . ? C31 C30 C29 121.2(3) . . ? C30 C31 C32 122.2(3) . . ? C33 C32 C31 116.3(3) . . ? C33 C32 C36 121.7(3) . . ? C31 C32 C36 121.9(3) . . ? C34 C33 C32 122.6(3) . . ? C33 C34 C29 121.5(3) . . ? C35 C36 C32 112.6(3) . . ? C35 C36 C37 110.7(3) . . ? C32 C36 C37 111.0(3) . . ? C38B N3 P2 119.1(4) . . ? C38A N3 P2 128.1(3) . . ? C43A C38A C39A 115.6(6) . . ? C43A C38A N3 121.8(6) . . ? C39A C38A N3 122.5(6) . . ? C40A C39A C38A 120.5(7) . . ? C41A C40A C39A 122.0(6) . . ? C42A C41A C40A 116.7(6) . . ? C42A C41A C45A 120.5(6) . . ? C40A C41A C45A 122.9(6) . . ? C43A C42A C41A 121.8(6) . . ? C42A C43A C38A 123.3(6) . . ? C46A C45A C41A 114.8(8) . . ? C46A C45A C44A 113.0(7) . . ? C41A C45A C44A 109.7(6) . . ? C39B C38B C43B 119.0(7) . . ? C39B C38B N3 126.7(6) . . ? C43B C38B N3 114.4(5) . . ? C40B C39B C38B 120.5(7) . . ? C39B C40B C41B 122.8(6) . . ? C40B C41B C42B 116.7(6) . . ? C40B C41B C45B 119.7(6) . . ? C42B C41B C45B 123.6(6) . . ? C41B C42B C43B 122.0(6) . . ? C42B C43B C38B 119.1(6) . . ? C44B C45B C46B 119.6(11) . . ? C44B C45B C41B 112.2(9) . . ? C46B C45B C41B 111.5(9) . . ? 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 H1A N3 0.88 1.99 2.851(3) 164.3 2_655 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.491 _refine_diff_density_min -0.431 _refine_diff_density_rms 0.054 # 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 0.500 0.500 0.500 386 100 ' ' _platon_squeeze_details ; 'A heavily disordered molecule of toluene was present in the unit cell, for which no suitable model could be found. The electron density associated with this fragment was removed using SQUEEZE (PLATON), leaving a void of ca. 386 A^3.' ; data_ph11025 _database_code_depnum_ccdc_archive 'CCDC 861267' #TrackingRef '- Dalton Structures - Paul G Hayes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H66 Er N3 P2 Si2' _chemical_formula_weight 1042.48 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' Si Si 0.0817 0.0704 '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' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.729(5) _cell_length_b 12.188(6) _cell_length_c 24.287(11) _cell_angle_alpha 84.796(5) _cell_angle_beta 78.920(5) _cell_angle_gamma 69.550(5) _cell_volume 2647(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9980 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 27.31 _exptl_crystal_description needle _exptl_crystal_colour pink _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.308 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1074 _exptl_absorpt_coefficient_mu 1.727 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.4955 _exptl_absorpt_correction_T_max 0.8945 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 34897 _diffrn_reflns_av_R_equivalents 0.0345 _diffrn_reflns_av_sigmaI/netI 0.0382 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 26.37 _reflns_number_total 10778 _reflns_number_gt 9128 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0399P)^2^+3.1446P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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 10778 _refine_ls_number_parameters 548 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0484 _refine_ls_R_factor_gt 0.0365 _refine_ls_wR_factor_ref 0.0868 _refine_ls_wR_factor_gt 0.0818 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 Er1 Er 0.955100(19) 0.959536(13) 0.751073(7) 0.03448(6) Uani 1 1 d . B . C29 C 1.1428(4) 1.0047(3) 0.62979(16) 0.0388(9) Uani 1 1 d . B . C4 C 0.7578(4) 1.2046(3) 0.82083(15) 0.0366(8) Uani 1 1 d . B . C1 C 0.9011(4) 1.2455(3) 0.74733(15) 0.0357(8) Uani 1 1 d . B . C5 C 0.9500(5) 1.2993(3) 0.62788(16) 0.0454(10) Uani 1 1 d . . . C3 C 0.7426(5) 1.3213(3) 0.82456(17) 0.0464(10) Uani 1 1 d . . . H3 H 0.6816 1.3733 0.8534 0.056 Uiso 1 1 calc R . . C30 C 1.0902(5) 1.0233(4) 0.57986(18) 0.0501(10) Uani 1 1 d . . . H30 H 0.9953 1.0804 0.5776 0.060 Uiso 1 1 calc R . . C2 C 0.8341(5) 1.3473(3) 0.77765(17) 0.0466(10) Uani 1 1 d . . . H2 H 0.8480 1.4205 0.7682 0.056 Uiso 1 1 calc R . . C31 C 1.1736(5) 0.9600(4) 0.53235(19) 0.0552(11) Uani 1 1 d . . . H31 H 1.1365 0.9771 0.4980 0.066 Uiso 1 1 calc R . . C32 C 1.3087(5) 0.8731(4) 0.53451(18) 0.0474(10) Uani 1 1 d . . . C34 C 1.2765(5) 0.9169(4) 0.63258(18) 0.0490(10) Uani 1 1 d . . . H34 H 1.3139 0.9005 0.6669 0.059 Uiso 1 1 calc R . . C11 C 1.1969(4) 1.2366(3) 0.68808(16) 0.0419(9) Uani 1 1 d . . . C10 C 1.0382(6) 1.3056(4) 0.57574(19) 0.0655(14) Uani 1 1 d . . . H10 H 1.1427 1.2656 0.5703 0.079 Uiso 1 1 calc R . . C12 C 1.3171(5) 1.1490(4) 0.7049(2) 0.0565(11) Uani 1 1 d . . . H12 H 1.3138 1.0720 0.7123 0.068 Uiso 1 1 calc R . . C33 C 1.3587(5) 0.8510(4) 0.5849(2) 0.0555(12) Uani 1 1 d . . . H33 H 1.4504 0.7902 0.5877 0.067 Uiso 1 1 calc R . . C6 C 0.7989(5) 1.3626(4) 0.6348(2) 0.0573(11) Uani 1 1 d . . . H6 H 0.7378 1.3603 0.6702 0.069 Uiso 1 1 calc R . . C13 C 1.4425(6) 1.1728(5) 0.7110(2) 0.0742(15) Uani 1 1 d . . . H13 H 1.5254 1.1120 0.7223 0.089 Uiso 1 1 calc R . . C14 C 1.4467(7) 1.2837(6) 0.7009(3) 0.0854(19) Uani 1 1 d . . . H14 H 1.5316 1.3005 0.7060 0.102 Uiso 1 1 calc R . . C9 C 0.9725(8) 1.3703(5) 0.5323(2) 0.089(2) Uani 1 1 d . . . H9 H 1.0322 1.3731 0.4966 0.106 Uiso 1 1 calc R . . C7 C 0.7355(7) 1.4291(5) 0.5910(2) 0.0772(15) Uani 1 1 d . . . H7 H 0.6321 1.4734 0.5965 0.093 Uiso 1 1 calc R . . C8 C 0.8224(8) 1.4308(5) 0.5398(2) 0.0851(18) Uani 1 1 d . . . H8 H 0.7787 1.4740 0.5092 0.102 Uiso 1 1 calc R . . C15 C 1.3291(7) 1.3706(5) 0.6834(3) 0.0872(19) Uani 1 1 d . . . H15 H 1.3339 1.4472 0.6758 0.105 Uiso 1 1 calc R . . C16 C 1.2035(6) 1.3486(4) 0.6767(2) 0.0644(13) Uani 1 1 d . . . H16 H 1.1224 1.4095 0.6645 0.077 Uiso 1 1 calc R . . C17 C 0.4885(5) 1.1471(4) 0.86298(17) 0.0470(10) Uani 1 1 d . C . C47 C 1.1678(5) 0.8454(4) 0.7922(2) 0.0559(11) Uani 1 1 d . . . H47A H 1.2391 0.8883 0.7820 0.067 Uiso 1 1 calc R A 1 H47B H 1.1335 0.8541 0.8332 0.067 Uiso 1 1 calc R A 1 C51 C 0.8351(5) 0.8932(4) 0.69139(19) 0.0506(10) Uani 1 1 d . . . H51A H 0.7344 0.9064 0.7137 0.061 Uiso 1 1 calc R B . H51B H 0.8208 0.9540 0.6611 0.061 Uiso 1 1 calc R . . C54 C 1.0714(5) 0.6915(4) 0.6223(2) 0.0636(13) Uani 1 1 d . . . H54A H 1.1010 0.7474 0.5954 0.095 Uiso 1 1 calc R B . H54B H 1.0857 0.6202 0.6030 0.095 Uiso 1 1 calc R . . H54C H 1.1326 0.6720 0.6519 0.095 Uiso 1 1 calc R . . C52 C 0.7608(7) 0.7826(6) 0.5964(3) 0.093(2) Uani 1 1 d . . . H52A H 0.6558 0.8250 0.6109 0.139 Uiso 1 1 calc R B . H52B H 0.7707 0.7069 0.5823 0.139 Uiso 1 1 calc R . . H52C H 0.7979 0.8287 0.5659 0.139 Uiso 1 1 calc R . . C53 C 0.8198(6) 0.6459(4) 0.7034(2) 0.0743(15) Uani 1 1 d . . . H53A H 0.8873 0.6197 0.7308 0.111 Uiso 1 1 calc R B . H53B H 0.8275 0.5788 0.6821 0.111 Uiso 1 1 calc R . . H53C H 0.7172 0.6805 0.7230 0.111 Uiso 1 1 calc R . . Si2 Si 0.87194(13) 0.75795(10) 0.65417(5) 0.0479(3) Uani 1 1 d . B . P2 P 0.68565(11) 1.10579(8) 0.86407(4) 0.0382(2) Uani 1 1 d . . . P1 P 1.02993(11) 1.20549(8) 0.68393(4) 0.0366(2) Uani 1 1 d . B . N2 N 0.8545(3) 1.1576(2) 0.77362(12) 0.0345(7) Uani 1 1 d . . . N1 N 1.0569(3) 1.0685(3) 0.67998(13) 0.0384(7) Uani 1 1 d . . . N3 N 0.7840(4) 0.9798(3) 0.83796(13) 0.0430(8) Uani 1 1 d . B . C18 C 0.3978(5) 1.2609(4) 0.8672(3) 0.0740(16) Uani 1 1 d . . . H18 H 0.4378 1.3193 0.8724 0.089 Uiso 1 1 calc R C . C22 C 0.4270(6) 1.0661(5) 0.8529(3) 0.0767(15) Uani 1 1 d . . . H22 H 0.4884 0.9866 0.8472 0.092 Uiso 1 1 calc R C . C20 C 0.1879(6) 1.2118(6) 0.8567(3) 0.0795(16) Uani 1 1 d . . . H20 H 0.0845 1.2345 0.8557 0.095 Uiso 1 1 calc R C . C19 C 0.2484(6) 1.2931(5) 0.8641(3) 0.093(2) Uani 1 1 d . C . H19 H 0.1873 1.3731 0.8672 0.112 Uiso 1 1 calc R . . C21 C 0.2746(7) 1.1000(6) 0.8509(3) 0.096(2) Uani 1 1 d . C . H21 H 0.2330 1.0429 0.8453 0.116 Uiso 1 1 calc R . . C35 C 1.4009(5) 0.8066(4) 0.4818(2) 0.0616(12) Uani 1 1 d . . . H35 H 1.3306 0.8083 0.4564 0.074 Uiso 1 1 calc R . . C36 C 1.4869(8) 0.6808(5) 0.4934(3) 0.099(2) Uani 1 1 d . . . H36A H 1.5316 0.6406 0.4578 0.148 Uiso 1 1 calc R . . H36B H 1.4197 0.6432 0.5157 0.148 Uiso 1 1 calc R . . H36C H 1.5656 0.6765 0.5142 0.148 Uiso 1 1 calc R . . C37 C 1.5054(8) 0.8679(6) 0.4513(3) 0.100(2) Uani 1 1 d . . . H37A H 1.5827 0.8598 0.4735 0.150 Uiso 1 1 calc R . . H37B H 1.4494 0.9511 0.4459 0.150 Uiso 1 1 calc R . . H37C H 1.5520 0.8325 0.4146 0.150 Uiso 1 1 calc R . . Si1 Si 1.2826(4) 0.6896(2) 0.78344(16) 0.0462(8) Uiso 0.614(11) 1 d P B 1 C48 C 1.4031(8) 0.6513(6) 0.7135(4) 0.0465(19) Uiso 0.614(11) 1 d P B 1 H48A H 1.4594 0.5671 0.7130 0.070 Uiso 0.614(11) 1 calc PR B 1 H48B H 1.4725 0.6951 0.7064 0.070 Uiso 0.614(11) 1 calc PR B 1 H48C H 1.3408 0.6717 0.6843 0.070 Uiso 0.614(11) 1 calc PR B 1 C49 C 1.4088(14) 0.6303(10) 0.8361(5) 0.097(4) Uiso 0.614(11) 1 d P B 1 H49A H 1.4666 0.5476 0.8289 0.146 Uiso 0.614(11) 1 calc PR B 1 H49B H 1.3494 0.6374 0.8740 0.146 Uiso 0.614(11) 1 calc PR B 1 H49C H 1.4768 0.6747 0.8333 0.146 Uiso 0.614(11) 1 calc PR B 1 C50 C 1.1574(15) 0.6005(11) 0.7988(6) 0.091(4) Uiso 0.614(11) 1 d P B 1 H50A H 1.2168 0.5174 0.7937 0.136 Uiso 0.614(11) 1 calc PR B 1 H50B H 1.0851 0.6249 0.7731 0.136 Uiso 0.614(11) 1 calc PR B 1 H50C H 1.1045 0.6124 0.8376 0.136 Uiso 0.614(11) 1 calc PR B 1 C38 C 0.7916(10) 0.8727(7) 0.8729(4) 0.028(2) Uiso 0.513(11) 1 d P B 1 C39 C 0.8269(13) 0.8468(10) 0.9257(5) 0.049(3) Uiso 0.513(11) 1 d P B 1 H39 H 0.8507 0.9020 0.9438 0.059 Uiso 0.513(11) 1 calc PR B 1 C40 C 0.8285(13) 0.7428(10) 0.9527(5) 0.059(3) Uiso 0.513(11) 1 d P B 1 H40 H 0.8547 0.7274 0.9890 0.071 Uiso 0.513(11) 1 calc PR B 1 C41 C 0.7929(11) 0.6589(8) 0.9288(4) 0.049(2) Uiso 0.513(11) 1 d P B 1 C42 C 0.7600(11) 0.6818(8) 0.8749(4) 0.045(2) Uiso 0.513(11) 1 d P B 1 H42 H 0.7379 0.6254 0.8570 0.054 Uiso 0.513(11) 1 calc PR B 1 C43 C 0.7590(10) 0.7875(7) 0.8468(4) 0.036(2) Uiso 0.513(11) 1 d P B 1 H43 H 0.7362 0.8022 0.8100 0.043 Uiso 0.513(11) 1 calc PR B 1 C44 C 0.7910(15) 0.5463(10) 0.9625(6) 0.078(4) Uiso 0.513(11) 1 d P B 1 H44 H 0.8336 0.5368 0.9977 0.094 Uiso 0.513(11) 1 calc PR B 1 C45 C 0.8685(15) 0.4524(11) 0.9251(6) 0.079(4) Uiso 0.513(11) 1 d P B 1 H45A H 0.9729 0.4475 0.9144 0.119 Uiso 0.513(11) 1 calc PR B 1 H45B H 0.8225 0.4665 0.8914 0.119 Uiso 0.513(11) 1 calc PR B 1 H45C H 0.8635 0.3787 0.9436 0.119 Uiso 0.513(11) 1 calc PR B 1 C46 C 0.6408(14) 0.5343(11) 0.9723(6) 0.085(4) Uiso 0.513(11) 1 d P B 1 H46A H 0.5732 0.5911 1.0000 0.127 Uiso 0.513(11) 1 calc PR B 1 H46B H 0.6485 0.4548 0.9864 0.127 Uiso 0.513(11) 1 calc PR B 1 H46C H 0.6022 0.5490 0.9369 0.127 Uiso 0.513(11) 1 calc PR B 1 C23 C 0.7234(16) 1.1294(9) 0.9378(5) 0.028(3) Uiso 0.383(14) 1 d P C 1 C24 C 0.6061(15) 1.1547(13) 0.9821(5) 0.051(3) Uiso 0.383(14) 1 d P C 1 H24 H 0.5081 1.1624 0.9777 0.061 Uiso 0.383(14) 1 calc PR C 1 C25 C 0.6407(19) 1.1684(14) 1.0343(6) 0.067(4) Uiso 0.383(14) 1 d P C 1 H25 H 0.5688 1.1806 1.0677 0.080 Uiso 0.383(14) 1 calc PR C 1 C26 C 0.7871(19) 1.1631(13) 1.0340(8) 0.067(4) Uiso 0.383(14) 1 d P C 1 H26 H 0.8106 1.1801 1.0677 0.081 Uiso 0.383(14) 1 calc PR C 1 C27 C 0.897(2) 1.1353(13) 0.9888(6) 0.062(4) Uiso 0.383(14) 1 d P C 1 H27 H 0.9960 1.1279 0.9914 0.074 Uiso 0.383(14) 1 calc PR C 1 C28 C 0.8634(19) 1.1189(13) 0.9414(6) 0.048(4) Uiso 0.383(14) 1 d P C 1 H28 H 0.9390 1.0993 0.9091 0.058 Uiso 0.383(14) 1 calc PR C 1 Si1B Si 1.2469(6) 0.6822(3) 0.8006(3) 0.0526(13) Uiso 0.386(11) 1 d P B 2 C48B C 1.4076(17) 0.6367(14) 0.7419(8) 0.074(4) Uiso 0.386(11) 1 d P B 2 H48D H 1.4552 0.5514 0.7434 0.111 Uiso 0.386(11) 1 calc PR B 2 H48E H 1.4798 0.6740 0.7454 0.111 Uiso 0.386(11) 1 calc PR B 2 H48F H 1.3723 0.6607 0.7060 0.111 Uiso 0.386(11) 1 calc PR B 2 C49B C 1.3246(19) 0.6179(14) 0.8635(7) 0.079(5) Uiso 0.386(11) 1 d P B 2 H49D H 1.3613 0.5323 0.8616 0.118 Uiso 0.386(11) 1 calc PR B 2 H49E H 1.2472 0.6422 0.8968 0.118 Uiso 0.386(11) 1 calc PR B 2 H49F H 1.4071 0.6447 0.8661 0.118 Uiso 0.386(11) 1 calc PR B 2 C50B C 1.1157(16) 0.6084(12) 0.7899(6) 0.046(3) Uiso 0.386(11) 1 d P B 2 H50D H 1.1619 0.5234 0.7948 0.069 Uiso 0.386(11) 1 calc PR B 2 H50E H 1.0924 0.6265 0.7519 0.069 Uiso 0.386(11) 1 calc PR B 2 H50F H 1.0237 0.6363 0.8174 0.069 Uiso 0.386(11) 1 calc PR B 2 C38B C 0.7629(11) 0.8735(8) 0.8616(4) 0.034(3) Uiso 0.487(11) 1 d P B 2 C39B C 0.8082(14) 0.8392(10) 0.9135(6) 0.049(3) Uiso 0.487(11) 1 d P B 2 H39B H 0.8472 0.8862 0.9307 0.059 Uiso 0.487(11) 1 calc PR B 2 C40B C 0.7957(13) 0.7320(10) 0.9412(5) 0.056(3) Uiso 0.487(11) 1 d P B 2 H40B H 0.8221 0.7092 0.9773 0.067 Uiso 0.487(11) 1 calc PR B 2 C41B C 0.7442(12) 0.6634(8) 0.9136(5) 0.051(3) Uiso 0.487(11) 1 d P B 2 C42B C 0.7075(13) 0.6974(9) 0.8622(5) 0.054(3) Uiso 0.487(11) 1 d P B 2 H42B H 0.6754 0.6480 0.8434 0.065 Uiso 0.487(11) 1 calc PR B 2 C43B C 0.7150(13) 0.8013(9) 0.8358(5) 0.049(3) Uiso 0.487(11) 1 d P B 2 H43B H 0.6870 0.8225 0.7999 0.059 Uiso 0.487(11) 1 calc PR B 2 C44B C 0.7360(13) 0.5440(9) 0.9413(5) 0.062(3) Uiso 0.487(11) 1 d P B 2 H44B H 0.6789 0.5089 0.9224 0.074 Uiso 0.487(11) 1 calc PR B 2 C45B C 0.9085(19) 0.4520(15) 0.9468(8) 0.106(5) Uiso 0.487(11) 1 d P B 2 H45D H 0.9028 0.3774 0.9639 0.159 Uiso 0.487(11) 1 calc PR B 2 H45E H 0.9529 0.4868 0.9703 0.159 Uiso 0.487(11) 1 calc PR B 2 H45F H 0.9700 0.4384 0.9094 0.159 Uiso 0.487(11) 1 calc PR B 2 C46B C 0.6784(14) 0.5573(11) 1.0078(5) 0.078(4) Uiso 0.487(11) 1 d P B 2 H46D H 0.6716 0.4826 1.0244 0.117 Uiso 0.487(11) 1 calc PR B 2 H46E H 0.5800 0.6182 1.0147 0.117 Uiso 0.487(11) 1 calc PR B 2 H46F H 0.7485 0.5791 1.0247 0.117 Uiso 0.487(11) 1 calc PR B 2 C23B C 0.6887(10) 1.1248(6) 0.9327(3) 0.033(2) Uiso 0.617(14) 1 d P C 2 C24B C 0.5794(8) 1.1172(7) 0.9781(3) 0.0429(19) Uiso 0.617(14) 1 d P C 2 H24B H 0.4922 1.1063 0.9712 0.052 Uiso 0.617(14) 1 calc PR C 2 C25B C 0.5955(10) 1.1252(8) 1.0331(4) 0.063(3) Uiso 0.617(14) 1 d P C 2 H25B H 0.5195 1.1197 1.0632 0.076 Uiso 0.617(14) 1 calc PR C 2 C26B C 0.7236(11) 1.1415(7) 1.0447(4) 0.057(2) Uiso 0.617(14) 1 d P C 2 H26B H 0.7321 1.1503 1.0822 0.069 Uiso 0.617(14) 1 calc PR C 2 C27B C 0.8358(13) 1.1446(8) 1.0014(4) 0.059(2) Uiso 0.617(14) 1 d P C 2 H27B H 0.9251 1.1509 1.0088 0.071 Uiso 0.617(14) 1 calc PR C 2 C28B C 0.8169(13) 1.1382(8) 0.9458(4) 0.049(3) Uiso 0.617(14) 1 d P C 2 H28B H 0.8937 1.1432 0.9159 0.059 Uiso 0.617(14) 1 calc PR C 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 Er1 0.03728(10) 0.02292(8) 0.03830(10) -0.00487(6) 0.00679(7) -0.01010(6) C29 0.039(2) 0.0360(19) 0.040(2) -0.0099(16) 0.0100(17) -0.0184(17) C4 0.040(2) 0.0284(17) 0.034(2) -0.0026(15) 0.0091(16) -0.0106(15) C1 0.043(2) 0.0261(17) 0.0328(19) -0.0010(14) 0.0070(16) -0.0129(15) C5 0.059(3) 0.036(2) 0.037(2) -0.0036(16) 0.0066(19) -0.0171(19) C3 0.057(3) 0.0287(18) 0.042(2) -0.0088(16) 0.0175(19) -0.0131(18) C30 0.048(2) 0.049(2) 0.045(2) -0.0100(19) -0.0005(19) -0.008(2) C2 0.061(3) 0.0257(18) 0.046(2) -0.0043(16) 0.0140(19) -0.0171(18) C31 0.061(3) 0.057(3) 0.042(2) -0.014(2) -0.001(2) -0.014(2) C32 0.044(2) 0.055(2) 0.044(2) -0.0173(19) 0.0069(19) -0.022(2) C34 0.043(2) 0.055(2) 0.047(2) -0.015(2) 0.0007(19) -0.015(2) C11 0.044(2) 0.039(2) 0.039(2) -0.0108(17) 0.0150(17) -0.0194(18) C10 0.076(3) 0.050(3) 0.047(3) 0.006(2) 0.018(2) -0.010(2) C12 0.059(3) 0.053(3) 0.060(3) -0.007(2) -0.006(2) -0.022(2) C33 0.035(2) 0.055(3) 0.072(3) -0.024(2) 0.003(2) -0.011(2) C6 0.058(3) 0.069(3) 0.048(3) 0.007(2) -0.007(2) -0.027(2) C13 0.057(3) 0.080(4) 0.086(4) -0.017(3) -0.007(3) -0.022(3) C14 0.063(4) 0.101(5) 0.106(5) -0.031(4) 0.015(3) -0.054(4) C9 0.123(5) 0.068(4) 0.044(3) 0.014(3) 0.013(3) -0.011(4) C7 0.070(4) 0.085(4) 0.073(4) 0.008(3) -0.018(3) -0.020(3) C8 0.113(5) 0.076(4) 0.054(3) 0.010(3) -0.023(3) -0.014(4) C15 0.083(4) 0.066(4) 0.125(5) -0.019(3) 0.009(4) -0.051(3) C16 0.060(3) 0.044(2) 0.087(4) -0.012(2) 0.015(3) -0.027(2) C17 0.047(2) 0.043(2) 0.048(2) 0.0008(18) 0.0055(19) -0.0189(19) C47 0.057(3) 0.039(2) 0.069(3) -0.004(2) -0.013(2) -0.011(2) C51 0.051(3) 0.042(2) 0.060(3) -0.0036(19) -0.002(2) -0.019(2) C54 0.058(3) 0.064(3) 0.070(3) -0.008(2) -0.002(2) -0.025(2) C52 0.079(4) 0.098(5) 0.106(5) -0.030(4) -0.043(4) -0.014(3) C53 0.077(4) 0.058(3) 0.095(4) -0.009(3) 0.005(3) -0.040(3) Si2 0.0443(6) 0.0443(6) 0.0602(8) -0.0046(5) -0.0107(6) -0.0196(5) P2 0.0421(5) 0.0292(5) 0.0357(5) -0.0007(4) 0.0112(4) -0.0122(4) P1 0.0428(5) 0.0296(5) 0.0330(5) -0.0042(4) 0.0100(4) -0.0148(4) N2 0.0389(17) 0.0240(14) 0.0343(16) -0.0028(12) 0.0088(13) -0.0105(13) N1 0.0445(18) 0.0299(15) 0.0364(17) -0.0089(13) 0.0108(14) -0.0145(14) N3 0.0492(19) 0.0267(15) 0.0444(19) -0.0016(13) 0.0136(15) -0.0130(14) C18 0.047(3) 0.049(3) 0.122(5) 0.020(3) -0.011(3) -0.020(2) C22 0.062(3) 0.071(3) 0.101(4) -0.016(3) -0.007(3) -0.027(3) C20 0.052(3) 0.100(5) 0.085(4) 0.008(3) -0.007(3) -0.028(3) C19 0.051(3) 0.066(3) 0.148(6) 0.042(4) -0.013(3) -0.015(3) C21 0.077(4) 0.103(5) 0.125(6) -0.021(4) -0.015(4) -0.046(4) C35 0.054(3) 0.069(3) 0.053(3) -0.027(2) 0.009(2) -0.014(2) C36 0.122(5) 0.067(4) 0.081(4) -0.035(3) 0.005(4) -0.003(4) C37 0.110(5) 0.106(5) 0.074(4) -0.040(4) 0.052(4) -0.050(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Er1 N2 2.338(3) . ? Er1 N1 2.361(3) . ? Er1 C51 2.375(4) . ? Er1 N3 2.396(3) . ? Er1 C47 2.398(4) . ? C29 C34 1.375(6) . ? C29 C30 1.375(6) . ? C29 N1 1.454(4) . ? C4 N2 1.362(4) . ? C4 C3 1.388(5) . ? C4 P2 1.768(4) . ? C1 N2 1.365(4) . ? C1 C2 1.387(5) . ? C1 P1 1.774(4) . ? C5 C6 1.386(6) . ? C5 C10 1.399(6) . ? C5 P1 1.808(4) . ? C3 C2 1.390(5) . ? C3 H3 0.9500 . ? C30 C31 1.397(6) . ? C30 H30 0.9500 . ? C2 H2 0.9500 . ? C31 C32 1.377(6) . ? C31 H31 0.9500 . ? C32 C33 1.372(6) . ? C32 C35 1.529(6) . ? C34 C33 1.411(6) . ? C34 H34 0.9500 . ? C11 C12 1.381(6) . ? C11 C16 1.389(5) . ? C11 P1 1.814(4) . ? C10 C9 1.379(7) . ? C10 H10 0.9500 . ? C12 C13 1.386(7) . ? C12 H12 0.9500 . ? C33 H33 0.9500 . ? C6 C7 1.385(7) . ? C6 H6 0.9500 . ? C13 C14 1.365(8) . ? C13 H13 0.9500 . ? C14 C15 1.368(9) . ? C14 H14 0.9500 . ? C9 C8 1.371(8) . ? C9 H9 0.9500 . ? C7 C8 1.366(8) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C15 C16 1.380(7) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C18 1.360(6) . ? C17 C22 1.381(6) . ? C17 P2 1.810(4) . ? C47 Si1 1.843(5) . ? C47 Si1B 1.873(6) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C51 Si2 1.842(4) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C54 Si2 1.860(5) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C52 Si2 1.872(5) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 Si2 1.873(5) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? P2 N3 1.610(3) . ? P2 C23B 1.712(8) . ? P2 C23 1.960(13) . ? P1 N1 1.606(3) . ? N3 C38B 1.434(9) . ? N3 C38 1.478(9) . ? C18 C19 1.383(7) . ? C18 H18 0.9500 . ? C22 C21 1.403(8) . ? C22 H22 0.9500 . ? C20 C21 1.332(8) . ? C20 C19 1.356(8) . ? C20 H20 0.9500 . ? C19 H19 0.9500 . ? C21 H21 0.9500 . ? C35 C36 1.498(7) . ? C35 C37 1.510(7) . ? C35 H35 1.0000 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? Si1 C48 1.864(8) . ? Si1 C50 1.866(12) . ? Si1 C49 1.867(11) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C38 C39 1.370(15) . ? C38 C43 1.417(12) . ? C39 C40 1.371(15) . ? C39 H39 0.9500 . ? C40 C41 1.391(15) . ? C40 H40 0.9500 . ? C41 C42 1.387(14) . ? C41 C44 1.537(15) . ? C42 C43 1.400(12) . ? C42 H42 0.9500 . ? C43 H43 0.9500 . ? C44 C45 1.424(17) . ? C44 C46 1.491(19) . ? C44 H44 1.0000 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C23 C28 1.34(2) . ? C23 C24 1.378(17) . ? C24 C25 1.410(19) . ? C24 H24 0.9500 . ? C25 C26 1.40(2) . ? C25 H25 0.9500 . ? C26 C27 1.35(2) . ? C26 H26 0.9500 . ? C27 C28 1.30(2) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? Si1B C49B 1.827(15) . ? Si1B C48B 1.861(16) . ? Si1B C50B 1.865(14) . ? C48B H48D 0.9800 . ? C48B H48E 0.9800 . ? C48B H48F 0.9800 . ? C49B H49D 0.9800 . ? C49B H49E 0.9800 . ? C49B H49F 0.9800 . ? C50B H50D 0.9800 . ? C50B H50E 0.9800 . ? C50B H50F 0.9800 . ? C38B C43B 1.373(14) . ? C38B C39B 1.395(16) . ? C39B C40B 1.447(17) . ? C39B H39B 0.9500 . ? C40B C41B 1.387(16) . ? C40B H40B 0.9500 . ? C41B C42B 1.354(16) . ? C41B C44B 1.568(14) . ? C42B C43B 1.385(14) . ? C42B H42B 0.9500 . ? C43B H43B 0.9500 . ? C44B C46B 1.608(18) . ? C44B C45B 1.68(2) . ? C44B H44B 1.0000 . ? C45B H45D 0.9800 . ? C45B H45E 0.9800 . ? C45B H45F 0.9800 . ? C46B H46D 0.9800 . ? C46B H46E 0.9800 . ? C46B H46F 0.9800 . ? C23B C24B 1.398(10) . ? C23B C28B 1.410(12) . ? C24B C25B 1.391(11) . ? C24B H24B 0.9500 . ? C25B C26B 1.411(13) . ? C25B H25B 0.9500 . ? C26B C27B 1.371(14) . ? C26B H26B 0.9500 . ? C27B C28B 1.410(13) . ? C27B H27B 0.9500 . ? C28B H28B 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 N2 Er1 N1 71.09(10) . . ? N2 Er1 C51 116.97(13) . . ? N1 Er1 C51 94.98(14) . . ? N2 Er1 N3 71.32(10) . . ? N1 Er1 N3 142.41(10) . . ? C51 Er1 N3 101.57(14) . . ? N2 Er1 C47 115.74(13) . . ? N1 Er1 C47 102.27(15) . . ? C51 Er1 C47 127.28(15) . . ? N3 Er1 C47 94.14(15) . . ? C34 C29 C30 118.0(4) . . ? C34 C29 N1 119.7(4) . . ? C30 C29 N1 122.2(4) . . ? N2 C4 C3 110.6(3) . . ? N2 C4 P2 114.9(2) . . ? C3 C4 P2 134.4(3) . . ? N2 C1 C2 110.4(3) . . ? N2 C1 P1 114.7(2) . . ? C2 C1 P1 134.9(3) . . ? C6 C5 C10 118.5(4) . . ? C6 C5 P1 120.8(3) . . ? C10 C5 P1 120.7(4) . . ? C4 C3 C2 106.4(3) . . ? C4 C3 H3 126.8 . . ? C2 C3 H3 126.8 . . ? C29 C30 C31 121.3(4) . . ? C29 C30 H30 119.4 . . ? C31 C30 H30 119.4 . . ? C1 C2 C3 106.6(3) . . ? C1 C2 H2 126.7 . . ? C3 C2 H2 126.7 . . ? C32 C31 C30 121.1(4) . . ? C32 C31 H31 119.5 . . ? C30 C31 H31 119.5 . . ? C33 C32 C31 117.7(4) . . ? C33 C32 C35 121.7(4) . . ? C31 C32 C35 120.6(4) . . ? C29 C34 C33 120.5(4) . . ? C29 C34 H34 119.7 . . ? C33 C34 H34 119.7 . . ? C12 C11 C16 119.3(4) . . ? C12 C11 P1 119.7(3) . . ? C16 C11 P1 121.0(4) . . ? C9 C10 C5 119.6(5) . . ? C9 C10 H10 120.2 . . ? C5 C10 H10 120.2 . . ? C11 C12 C13 120.4(5) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C32 C33 C34 121.3(4) . . ? C32 C33 H33 119.3 . . ? C34 C33 H33 119.3 . . ? C7 C6 C5 121.0(5) . . ? C7 C6 H6 119.5 . . ? C5 C6 H6 119.5 . . ? C14 C13 C12 119.8(5) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C13 C14 C15 120.2(5) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C8 C9 C10 120.9(5) . . ? C8 C9 H9 119.5 . . ? C10 C9 H9 119.5 . . ? C8 C7 C6 119.6(5) . . ? C8 C7 H7 120.2 . . ? C6 C7 H7 120.2 . . ? C7 C8 C9 120.2(5) . . ? C7 C8 H8 119.9 . . ? C9 C8 H8 119.9 . . ? C14 C15 C16 120.8(5) . . ? C14 C15 H15 119.6 . . ? C16 C15 H15 119.6 . . ? C15 C16 C11 119.4(5) . . ? C15 C16 H16 120.3 . . ? C11 C16 H16 120.3 . . ? C18 C17 C22 117.4(5) . . ? C18 C17 P2 121.1(3) . . ? C22 C17 P2 121.3(4) . . ? Si1 C47 Si1B 15.82(16) . . ? Si1 C47 Er1 129.4(2) . . ? Si1B C47 Er1 128.1(2) . . ? Si1 C47 H47A 104.9 . . ? Si1B C47 H47A 117.4 . . ? Er1 C47 H47A 104.9 . . ? Si1 C47 H47B 104.9 . . ? Si1B C47 H47B 91.5 . . ? Er1 C47 H47B 104.9 . . ? H47A C47 H47B 105.8 . . ? Si2 C51 Er1 136.6(2) . . ? Si2 C51 H51A 103.0 . . ? Er1 C51 H51A 103.0 . . ? Si2 C51 H51B 103.0 . . ? Er1 C51 H51B 103.0 . . ? H51A C51 H51B 105.1 . . ? Si2 C54 H54A 109.5 . . ? Si2 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? Si2 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? Si2 C52 H52A 109.5 . . ? Si2 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? Si2 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? Si2 C53 H53A 109.5 . . ? Si2 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? Si2 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C51 Si2 C54 112.3(2) . . ? C51 Si2 C52 112.5(2) . . ? C54 Si2 C52 107.2(3) . . ? C51 Si2 C53 110.6(2) . . ? C54 Si2 C53 107.7(2) . . ? C52 Si2 C53 106.2(3) . . ? N3 P2 C23B 117.3(3) . . ? N3 P2 C4 103.98(16) . . ? C23B P2 C4 109.4(3) . . ? N3 P2 C17 114.10(19) . . ? C23B P2 C17 102.6(3) . . ? C4 P2 C17 109.44(19) . . ? N3 P2 C23 114.5(4) . . ? C23B P2 C23 9.9(4) . . ? C4 P2 C23 101.9(4) . . ? C17 P2 C23 111.8(4) . . ? N1 P1 C1 103.21(15) . . ? N1 P1 C5 116.19(18) . . ? C1 P1 C5 108.17(18) . . ? N1 P1 C11 113.73(18) . . ? C1 P1 C11 109.46(18) . . ? C5 P1 C11 105.88(19) . . ? C4 N2 C1 106.0(3) . . ? C4 N2 Er1 126.8(2) . . ? C1 N2 Er1 126.3(2) . . ? C29 N1 P1 120.7(2) . . ? C29 N1 Er1 115.6(2) . . ? P1 N1 Er1 123.69(16) . . ? C38B N3 C38 16.7(5) . . ? C38B N3 P2 122.2(4) . . ? C38 N3 P2 119.3(4) . . ? C38B N3 Er1 115.3(4) . . ? C38 N3 Er1 117.6(4) . . ? P2 N3 Er1 122.12(16) . . ? C17 C18 C19 121.1(5) . . ? C17 C18 H18 119.5 . . ? C19 C18 H18 119.5 . . ? C17 C22 C21 120.7(5) . . ? C17 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C21 C20 C19 119.5(6) . . ? C21 C20 H20 120.3 . . ? C19 C20 H20 120.3 . . ? C20 C19 C18 120.9(6) . . ? C20 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? C20 C21 C22 120.4(6) . . ? C20 C21 H21 119.8 . . ? C22 C21 H21 119.8 . . ? C36 C35 C37 109.9(5) . . ? C36 C35 C32 113.6(4) . . ? C37 C35 C32 110.0(4) . . ? C36 C35 H35 107.7 . . ? C37 C35 H35 107.7 . . ? C32 C35 H35 107.7 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C47 Si1 C48 115.7(3) . . ? C47 Si1 C50 108.5(5) . . ? C48 Si1 C50 109.6(5) . . ? C47 Si1 C49 113.9(4) . . ? C48 Si1 C49 105.8(5) . . ? C50 Si1 C49 102.5(6) . . ? Si1 C48 H48A 109.5 . . ? Si1 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? Si1 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? Si1 C49 H49A 109.5 . . ? Si1 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? Si1 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? Si1 C50 H50A 109.5 . . ? Si1 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? Si1 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C39 C38 C43 117.7(9) . . ? C39 C38 N3 128.4(8) . . ? C43 C38 N3 113.8(8) . . ? C38 C39 C40 121.3(11) . . ? C38 C39 H39 119.4 . . ? C40 C39 H39 119.4 . . ? C39 C40 C41 122.3(11) . . ? C39 C40 H40 118.9 . . ? C41 C40 H40 118.9 . . ? C42 C41 C40 117.6(9) . . ? C42 C41 C44 123.0(10) . . ? C40 C41 C44 119.4(10) . . ? C41 C42 C43 120.5(8) . . ? C41 C42 H42 119.7 . . ? C43 C42 H42 119.7 . . ? C42 C43 C38 120.6(8) . . ? C42 C43 H43 119.7 . . ? C38 C43 H43 119.7 . . ? C45 C44 C46 98.9(12) . . ? C45 C44 C41 106.1(10) . . ? C46 C44 C41 111.9(11) . . ? C45 C44 H44 113.0 . . ? C46 C44 H44 113.0 . . ? C41 C44 H44 113.0 . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C44 C46 H46A 109.5 . . ? C44 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C44 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C28 C23 C24 124.5(14) . . ? C28 C23 P2 117.1(9) . . ? C24 C23 P2 118.3(11) . . ? C23 C24 C25 115.8(13) . . ? C23 C24 H24 122.1 . . ? C25 C24 H24 122.1 . . ? C26 C25 C24 116.2(14) . . ? C26 C25 H25 121.9 . . ? C24 C25 H25 121.9 . . ? C27 C26 C25 124.2(16) . . ? C27 C26 H26 117.9 . . ? C25 C26 H26 117.9 . . ? C28 C27 C26 118.3(16) . . ? C28 C27 H27 120.9 . . ? C26 C27 H27 120.9 . . ? C27 C28 C23 120.8(16) . . ? C27 C28 H28 119.6 . . ? C23 C28 H28 119.6 . . ? C49B Si1B C48B 104.7(8) . . ? C49B Si1B C50B 108.2(7) . . ? C48B Si1B C50B 106.2(7) . . ? C49B Si1B C47 119.4(6) . . ? C48B Si1B C47 104.6(6) . . ? C50B Si1B C47 112.6(5) . . ? Si1B C48B H48D 109.5 . . ? Si1B C48B H48E 109.5 . . ? H48D C48B H48E 109.5 . . ? Si1B C48B H48F 109.5 . . ? H48D C48B H48F 109.5 . . ? H48E C48B H48F 109.5 . . ? Si1B C49B H49D 109.5 . . ? Si1B C49B H49E 109.5 . . ? H49D C49B H49E 109.5 . . ? Si1B C49B H49F 109.5 . . ? H49D C49B H49F 109.5 . . ? H49E C49B H49F 109.5 . . ? Si1B C50B H50D 109.5 . . ? Si1B C50B H50E 109.5 . . ? H50D C50B H50E 109.5 . . ? Si1B C50B H50F 109.5 . . ? H50D C50B H50F 109.5 . . ? H50E C50B H50F 109.5 . . ? C43B C38B C39B 119.3(9) . . ? C43B C38B N3 125.8(9) . . ? C39B C38B N3 114.7(9) . . ? C38B C39B C40B 120.0(11) . . ? C38B C39B H39B 120.0 . . ? C40B C39B H39B 120.0 . . ? C41B C40B C39B 118.1(11) . . ? C41B C40B H40B 120.9 . . ? C39B C40B H40B 120.9 . . ? C42B C41B C40B 119.9(10) . . ? C42B C41B C44B 120.6(9) . . ? C40B C41B C44B 119.4(11) . . ? C41B C42B C43B 122.6(10) . . ? C41B C42B H42B 118.7 . . ? C43B C42B H42B 118.7 . . ? C38B C43B C42B 119.9(10) . . ? C38B C43B H43B 120.1 . . ? C42B C43B H43B 120.1 . . ? C41B C44B C46B 110.3(9) . . ? C41B C44B C45B 109.8(10) . . ? C46B C44B C45B 95.2(11) . . ? C41B C44B H44B 113.4 . . ? C46B C44B H44B 113.4 . . ? C45B C44B H44B 113.4 . . ? C44B C45B H45D 109.5 . . ? C44B C45B H45E 109.5 . . ? H45D C45B H45E 109.5 . . ? C44B C45B H45F 109.5 . . ? H45D C45B H45F 109.5 . . ? H45E C45B H45F 109.5 . . ? C44B C46B H46D 109.5 . . ? C44B C46B H46E 109.5 . . ? H46D C46B H46E 109.5 . . ? C44B C46B H46F 109.5 . . ? H46D C46B H46F 109.5 . . ? H46E C46B H46F 109.5 . . ? C24B C23B C28B 116.6(7) . . ? C24B C23B P2 125.0(6) . . ? C28B C23B P2 118.2(6) . . ? C25B C24B C23B 121.4(8) . . ? C25B C24B H24B 119.3 . . ? C23B C24B H24B 119.3 . . ? C24B C25B C26B 120.6(8) . . ? C24B C25B H25B 119.7 . . ? C26B C25B H25B 119.7 . . ? C27B C26B C25B 119.5(9) . . ? C27B C26B H26B 120.2 . . ? C25B C26B H26B 120.2 . . ? C26B C27B C28B 119.2(9) . . ? C26B C27B H27B 120.4 . . ? C28B C27B H27B 120.4 . . ? C23B C28B C27B 122.6(9) . . ? C23B C28B H28B 118.7 . . ? C27B C28B H28B 118.7 . . ? 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 N2 C4 C3 C2 -0.1(5) . . . . ? P2 C4 C3 C2 177.4(4) . . . . ? C34 C29 C30 C31 -3.7(6) . . . . ? N1 C29 C30 C31 -179.1(4) . . . . ? N2 C1 C2 C3 0.0(5) . . . . ? P1 C1 C2 C3 -179.9(4) . . . . ? C4 C3 C2 C1 0.1(5) . . . . ? C29 C30 C31 C32 2.8(7) . . . . ? C30 C31 C32 C33 -0.1(7) . . . . ? C30 C31 C32 C35 -178.4(4) . . . . ? C30 C29 C34 C33 2.0(6) . . . . ? N1 C29 C34 C33 177.6(4) . . . . ? C6 C5 C10 C9 -2.5(7) . . . . ? P1 C5 C10 C9 174.8(4) . . . . ? C16 C11 C12 C13 0.8(7) . . . . ? P1 C11 C12 C13 -176.7(4) . . . . ? C31 C32 C33 C34 -1.6(6) . . . . ? C35 C32 C33 C34 176.7(4) . . . . ? C29 C34 C33 C32 0.6(7) . . . . ? C10 C5 C6 C7 1.1(7) . . . . ? P1 C5 C6 C7 -176.1(4) . . . . ? C11 C12 C13 C14 0.6(8) . . . . ? C12 C13 C14 C15 -1.6(9) . . . . ? C5 C10 C9 C8 1.5(9) . . . . ? C5 C6 C7 C8 1.3(8) . . . . ? C6 C7 C8 C9 -2.3(9) . . . . ? C10 C9 C8 C7 1.0(10) . . . . ? C13 C14 C15 C16 1.2(10) . . . . ? C14 C15 C16 C11 0.2(9) . . . . ? C12 C11 C16 C15 -1.1(7) . . . . ? P1 C11 C16 C15 176.3(4) . . . . ? N2 Er1 C47 Si1 -177.7(3) . . . . ? N1 Er1 C47 Si1 -103.0(4) . . . . ? C51 Er1 C47 Si1 3.1(5) . . . . ? N3 Er1 C47 Si1 111.1(4) . . . . ? N2 Er1 C47 Si1B 162.0(4) . . . . ? N1 Er1 C47 Si1B -123.2(4) . . . . ? C51 Er1 C47 Si1B -17.1(5) . . . . ? N3 Er1 C47 Si1B 90.8(4) . . . . ? N2 Er1 C51 Si2 171.8(3) . . . . ? N1 Er1 C51 Si2 100.5(3) . . . . ? N3 Er1 C51 Si2 -113.4(3) . . . . ? C47 Er1 C51 Si2 -9.0(4) . . . . ? Er1 C51 Si2 C54 -40.5(4) . . . . ? Er1 C51 Si2 C52 -161.6(3) . . . . ? Er1 C51 Si2 C53 79.8(4) . . . . ? N2 C4 P2 N3 10.0(3) . . . . ? C3 C4 P2 N3 -167.5(4) . . . . ? N2 C4 P2 C23B 136.1(4) . . . . ? C3 C4 P2 C23B -41.4(6) . . . . ? N2 C4 P2 C17 -112.3(3) . . . . ? C3 C4 P2 C17 70.2(5) . . . . ? N2 C4 P2 C23 129.2(5) . . . . ? C3 C4 P2 C23 -48.2(6) . . . . ? C18 C17 P2 N3 -160.0(4) . . . . ? C22 C17 P2 N3 14.2(5) . . . . ? C18 C17 P2 C23B 72.0(5) . . . . ? C22 C17 P2 C23B -113.8(5) . . . . ? C18 C17 P2 C4 -44.0(5) . . . . ? C22 C17 P2 C4 130.2(4) . . . . ? C18 C17 P2 C23 68.1(6) . . . . ? C22 C17 P2 C23 -117.7(5) . . . . ? N2 C1 P1 N1 -3.0(3) . . . . ? C2 C1 P1 N1 177.0(4) . . . . ? N2 C1 P1 C5 120.7(3) . . . . ? C2 C1 P1 C5 -59.3(5) . . . . ? N2 C1 P1 C11 -124.4(3) . . . . ? C2 C1 P1 C11 55.6(5) . . . . ? C6 C5 P1 N1 98.6(4) . . . . ? C10 C5 P1 N1 -78.6(4) . . . . ? C6 C5 P1 C1 -16.8(4) . . . . ? C10 C5 P1 C1 165.9(4) . . . . ? C6 C5 P1 C11 -134.1(4) . . . . ? C10 C5 P1 C11 48.7(4) . . . . ? C12 C11 P1 N1 -20.0(4) . . . . ? C16 C11 P1 N1 162.6(3) . . . . ? C12 C11 P1 C1 94.9(3) . . . . ? C16 C11 P1 C1 -82.5(4) . . . . ? C12 C11 P1 C5 -148.7(3) . . . . ? C16 C11 P1 C5 33.8(4) . . . . ? C3 C4 N2 C1 0.2(5) . . . . ? P2 C4 N2 C1 -177.9(3) . . . . ? C3 C4 N2 Er1 169.5(3) . . . . ? P2 C4 N2 Er1 -8.5(4) . . . . ? C2 C1 N2 C4 -0.1(4) . . . . ? P1 C1 N2 C4 179.8(3) . . . . ? C2 C1 N2 Er1 -169.6(3) . . . . ? P1 C1 N2 Er1 10.4(4) . . . . ? N1 Er1 N2 C4 -177.3(3) . . . . ? C51 Er1 N2 C4 96.8(3) . . . . ? N3 Er1 N2 C4 3.0(3) . . . . ? C47 Er1 N2 C4 -82.5(3) . . . . ? N1 Er1 N2 C1 -10.0(3) . . . . ? C51 Er1 N2 C1 -96.0(3) . . . . ? N3 Er1 N2 C1 170.3(3) . . . . ? C47 Er1 N2 C1 84.8(3) . . . . ? C34 C29 N1 P1 114.5(4) . . . . ? C30 C29 N1 P1 -70.1(4) . . . . ? C34 C29 N1 Er1 -68.0(4) . . . . ? C30 C29 N1 Er1 107.4(4) . . . . ? C1 P1 N1 C29 172.3(3) . . . . ? C5 P1 N1 C29 54.1(4) . . . . ? C11 P1 N1 C29 -69.3(3) . . . . ? C1 P1 N1 Er1 -5.0(3) . . . . ? C5 P1 N1 Er1 -123.2(2) . . . . ? C11 P1 N1 Er1 113.5(2) . . . . ? N2 Er1 N1 C29 -169.9(3) . . . . ? C51 Er1 N1 C29 -53.1(3) . . . . ? N3 Er1 N1 C29 -169.4(2) . . . . ? C47 Er1 N1 C29 76.8(3) . . . . ? N2 Er1 N1 P1 7.46(19) . . . . ? C51 Er1 N1 P1 124.3(2) . . . . ? N3 Er1 N1 P1 8.0(3) . . . . ? C47 Er1 N1 P1 -105.8(2) . . . . ? C23B P2 N3 C38B 58.0(7) . . . . ? C4 P2 N3 C38B 178.9(6) . . . . ? C17 P2 N3 C38B -61.9(6) . . . . ? C23 P2 N3 C38B 68.6(8) . . . . ? C23B P2 N3 C38 38.9(6) . . . . ? C4 P2 N3 C38 159.8(5) . . . . ? C17 P2 N3 C38 -81.1(5) . . . . ? C23 P2 N3 C38 49.5(7) . . . . ? C23B P2 N3 Er1 -129.3(4) . . . . ? C4 P2 N3 Er1 -8.4(3) . . . . ? C17 P2 N3 Er1 110.8(2) . . . . ? C23 P2 N3 Er1 -118.7(5) . . . . ? N2 Er1 N3 C38B 177.4(6) . . . . ? N1 Er1 N3 C38B 176.8(5) . . . . ? C51 Er1 N3 C38B 62.6(6) . . . . ? C47 Er1 N3 C38B -66.8(6) . . . . ? N2 Er1 N3 C38 -164.1(5) . . . . ? N1 Er1 N3 C38 -164.7(5) . . . . ? C51 Er1 N3 C38 81.1(5) . . . . ? C47 Er1 N3 C38 -48.3(5) . . . . ? N2 Er1 N3 P2 4.2(2) . . . . ? N1 Er1 N3 P2 3.7(3) . . . . ? C51 Er1 N3 P2 -110.6(2) . . . . ? C47 Er1 N3 P2 120.0(2) . . . . ? C22 C17 C18 C19 3.0(8) . . . . ? P2 C17 C18 C19 177.4(5) . . . . ? C18 C17 C22 C21 -4.1(8) . . . . ? P2 C17 C22 C21 -178.5(5) . . . . ? C21 C20 C19 C18 -1.8(10) . . . . ? C17 C18 C19 C20 -0.1(10) . . . . ? C19 C20 C21 C22 0.6(11) . . . . ? C17 C22 C21 C20 2.4(10) . . . . ? C33 C32 C35 C36 35.8(7) . . . . ? C31 C32 C35 C36 -146.0(5) . . . . ? C33 C32 C35 C37 -87.9(6) . . . . ? C31 C32 C35 C37 90.3(6) . . . . ? Si1B C47 Si1 C48 162.2(7) . . . . ? Er1 C47 Si1 C48 70.5(5) . . . . ? Si1B C47 Si1 C50 38.5(7) . . . . ? Er1 C47 Si1 C50 -53.1(6) . . . . ? Si1B C47 Si1 C49 -74.9(7) . . . . ? Er1 C47 Si1 C49 -166.6(5) . . . . ? C38B N3 C38 C39 -157(3) . . . . ? P2 N3 C38 C39 -52.1(11) . . . . ? Er1 N3 C38 C39 116.6(9) . . . . ? C38B N3 C38 C43 23.7(17) . . . . ? P2 N3 C38 C43 128.6(6) . . . . ? Er1 N3 C38 C43 -62.7(8) . . . . ? C43 C38 C39 C40 -1.0(15) . . . . ? N3 C38 C39 C40 179.8(9) . . . . ? C38 C39 C40 C41 -0.8(17) . . . . ? C39 C40 C41 C42 2.2(16) . . . . ? C39 C40 C41 C44 -177.6(10) . . . . ? C40 C41 C42 C43 -1.7(14) . . . . ? C44 C41 C42 C43 178.0(9) . . . . ? C41 C42 C43 C38 0.0(14) . . . . ? C39 C38 C43 C42 1.4(13) . . . . ? N3 C38 C43 C42 -179.3(7) . . . . ? C42 C41 C44 C45 46.0(16) . . . . ? C40 C41 C44 C45 -134.3(12) . . . . ? C42 C41 C44 C46 -60.8(14) . . . . ? C40 C41 C44 C46 118.9(12) . . . . ? N3 P2 C23 C28 58.2(11) . . . . ? C23B P2 C23 C28 167(3) . . . . ? C4 P2 C23 C28 -53.4(10) . . . . ? C17 P2 C23 C28 -170.1(9) . . . . ? N3 P2 C23 C24 -121.5(9) . . . . ? C23B P2 C23 C24 -12(2) . . . . ? C4 P2 C23 C24 127.0(9) . . . . ? C17 P2 C23 C24 10.2(10) . . . . ? C28 C23 C24 C25 -0.8(19) . . . . ? P2 C23 C24 C25 178.8(9) . . . . ? C23 C24 C25 C26 4.5(19) . . . . ? C24 C25 C26 C27 -6(2) . . . . ? C25 C26 C27 C28 4(2) . . . . ? C26 C27 C28 C23 0(2) . . . . ? C24 C23 C28 C27 -2(2) . . . . ? P2 C23 C28 C27 178.8(11) . . . . ? Si1 C47 Si1B C49B 115.4(9) . . . . ? Er1 C47 Si1B C49B -143.5(7) . . . . ? Si1 C47 Si1B C48B -1.1(7) . . . . ? Er1 C47 Si1B C48B 100.0(7) . . . . ? Si1 C47 Si1B C50B -116.0(9) . . . . ? Er1 C47 Si1B C50B -14.9(8) . . . . ? C38 N3 C38B C43B -160(3) . . . . ? P2 N3 C38B C43B 115.4(9) . . . . ? Er1 N3 C38B C43B -57.8(10) . . . . ? C38 N3 C38B C39B 14.7(17) . . . . ? P2 N3 C38B C39B -70.2(10) . . . . ? Er1 N3 C38B C39B 116.6(8) . . . . ? C43B C38B C39B C40B -3.8(16) . . . . ? N3 C38B C39B C40B -178.6(9) . . . . ? C38B C39B C40B C41B 2.7(17) . . . . ? C39B C40B C41B C42B 0.1(16) . . . . ? C39B C40B C41B C44B 177.4(10) . . . . ? C40B C41B C42B C43B -1.9(17) . . . . ? C44B C41B C42B C43B -179.2(10) . . . . ? C39B C38B C43B C42B 2.1(15) . . . . ? N3 C38B C43B C42B 176.3(9) . . . . ? C41B C42B C43B C38B 0.9(17) . . . . ? C42B C41B C44B C46B -142.9(11) . . . . ? C40B C41B C44B C46B 39.9(14) . . . . ? C42B C41B C44B C45B 113.5(13) . . . . ? C40B C41B C44B C45B -63.7(15) . . . . ? N3 P2 C23B C24B -99.0(7) . . . . ? C4 P2 C23B C24B 142.9(6) . . . . ? C17 P2 C23B C24B 26.8(7) . . . . ? C23 P2 C23B C24B -175(3) . . . . ? N3 P2 C23B C28B 74.6(7) . . . . ? C4 P2 C23B C28B -43.4(7) . . . . ? C17 P2 C23B C28B -159.5(6) . . . . ? C23 P2 C23B C28B -1(3) . . . . ? C28B C23B C24B C25B 1.4(11) . . . . ? P2 C23B C24B C25B 175.2(6) . . . . ? C23B C24B C25B C26B 0.1(12) . . . . ? C24B C25B C26B C27B -2.7(13) . . . . ? C25B C26B C27B C28B 3.7(13) . . . . ? C24B C23B C28B C27B -0.4(12) . . . . ? P2 C23B C28B C27B -174.6(7) . . . . ? C26B C27B C28B C23B -2.2(13) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.827 _refine_diff_density_min -0.814 _refine_diff_density_rms 0.082 # start Validation Reply Form _vrf_PLAT201_ph11025 ; PROBLEM: Isotropic non-H Atoms in Main Residue RESPONSE: Various moieties (one phenyl ring, C23; one 4-isopropylphenyl ring, C38; and one TMS group, Si1) were disordered over two positions. Disordered atoms were held isotropic. ; # end Validation Reply Form data_ph11026 _database_code_depnum_ccdc_archive 'CCDC 861268' #TrackingRef '- Dalton Structures - Paul G Hayes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H66 Lu N3 P2 Si2' _chemical_formula_weight 1050.19 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' Si Si 0.0817 0.0704 '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' Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7163(6) _cell_length_b 12.1266(7) _cell_length_c 24.2569(14) _cell_angle_alpha 84.9530(10) _cell_angle_beta 78.9220(10) _cell_angle_gamma 69.4640(10) _cell_volume 2625.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9907 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 27.50 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.328 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1080 _exptl_absorpt_coefficient_mu 2.023 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.5728 _exptl_absorpt_correction_T_max 0.7775 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 37480 _diffrn_reflns_av_R_equivalents 0.0210 _diffrn_reflns_av_sigmaI/netI 0.0221 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 27.10 _reflns_number_total 11526 _reflns_number_gt 10485 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0361P)^2^+3.2112P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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 11526 _refine_ls_number_parameters 548 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0346 _refine_ls_R_factor_gt 0.0300 _refine_ls_wR_factor_ref 0.0746 _refine_ls_wR_factor_gt 0.0721 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _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 Lu1 Lu 0.953745(14) 0.961337(10) 0.751409(5) 0.03292(5) Uani 1 1 d . B . C38 C 1.1432(3) 1.0024(3) 0.63056(13) 0.0380(7) Uani 1 1 d . C . C1 C 0.7574(3) 1.2051(2) 0.82070(12) 0.0370(6) Uani 1 1 d . B . C4 C 0.9015(3) 1.2453(2) 0.74733(12) 0.0350(6) Uani 1 1 d . C . C23 C 0.9511(4) 1.2976(3) 0.62785(13) 0.0435(7) Uani 1 1 d . . . C41 C 1.3100(4) 0.8707(3) 0.53483(14) 0.0458(8) Uani 1 1 d . . . C43 C 1.0898(4) 1.0203(3) 0.58051(14) 0.0483(8) Uani 1 1 d . . . H43 H 0.9943 1.0772 0.5784 0.058 Uiso 1 1 calc R . . C42 C 1.1734(4) 0.9563(3) 0.53304(15) 0.0534(9) Uani 1 1 d . . . H42 H 1.1353 0.9722 0.4988 0.064 Uiso 1 1 calc R . . C2 C 0.7418(4) 1.3224(3) 0.82434(14) 0.0468(8) Uani 1 1 d . . . H2 H 0.6804 1.3749 0.8532 0.056 Uiso 1 1 calc R . . C11 C 0.4886(4) 1.1470(3) 0.86220(14) 0.0476(8) Uani 1 1 d . . . C3 C 0.8338(4) 1.3481(3) 0.77730(14) 0.0460(8) Uani 1 1 d . . . H3 H 0.8474 1.4217 0.7677 0.055 Uiso 1 1 calc R . . C51 C 1.1632(4) 0.8475(3) 0.79150(17) 0.0533(9) Uani 1 1 d . . . H51A H 1.2343 0.8908 0.7813 0.064 Uiso 1 1 calc R A 1 H51B H 1.1286 0.8564 0.8325 0.064 Uiso 1 1 calc R A 1 C17 C 1.1967(4) 1.2357(3) 0.68780(13) 0.0412(7) Uani 1 1 d . . . C39 C 1.2786(4) 0.9150(3) 0.63281(15) 0.0471(8) Uani 1 1 d . . . H39 H 1.3169 0.8990 0.6670 0.056 Uiso 1 1 calc R . . C47 C 0.8349(4) 0.8949(3) 0.69255(15) 0.0485(8) Uani 1 1 d . . . H47A H 0.7346 0.9074 0.7152 0.058 Uiso 1 1 calc R C . H47B H 0.8191 0.9565 0.6625 0.058 Uiso 1 1 calc R . . C24 C 1.0396(5) 1.3029(3) 0.57602(16) 0.0655(11) Uani 1 1 d . . . H24 H 1.1442 1.2623 0.5707 0.079 Uiso 1 1 calc R . . C18 C 1.3173(4) 1.1481(3) 0.70457(16) 0.0543(9) Uani 1 1 d . . . H18 H 1.3144 1.0707 0.7120 0.065 Uiso 1 1 calc R . . C28 C 0.7998(4) 1.3615(4) 0.63478(16) 0.0567(9) Uani 1 1 d . . . H28 H 0.7384 1.3597 0.6702 0.068 Uiso 1 1 calc R . . C40 C 1.3604(4) 0.8497(3) 0.58514(16) 0.0516(8) Uani 1 1 d . . . H40 H 1.4530 0.7892 0.5877 0.062 Uiso 1 1 calc R . . C48 C 1.0720(4) 0.6911(4) 0.62316(18) 0.0590(9) Uani 1 1 d . . . H48A H 1.1032 0.7471 0.5966 0.089 Uiso 1 1 calc R C . H48B H 1.0854 0.6201 0.6033 0.089 Uiso 1 1 calc R . . H48C H 1.1328 0.6699 0.6529 0.089 Uiso 1 1 calc R . . C19 C 1.4428(5) 1.1721(4) 0.7107(2) 0.0707(11) Uani 1 1 d . . . H19 H 1.5259 1.1112 0.7220 0.085 Uiso 1 1 calc R . . C20 C 1.4465(5) 1.2839(5) 0.7005(2) 0.0795(14) Uani 1 1 d . . . H20 H 1.5312 1.3011 0.7058 0.095 Uiso 1 1 calc R . . C25 C 0.9737(6) 1.3681(4) 0.53213(17) 0.0845(16) Uani 1 1 d . . . H25 H 1.0335 1.3700 0.4964 0.101 Uiso 1 1 calc R . . C49 C 0.7617(6) 0.7870(5) 0.5965(2) 0.0893(17) Uani 1 1 d . . . H49A H 0.6566 0.8309 0.6108 0.134 Uiso 1 1 calc R C . H49B H 0.7702 0.7115 0.5821 0.134 Uiso 1 1 calc R . . H49C H 0.8005 0.8329 0.5662 0.134 Uiso 1 1 calc R . . C50 C 0.8179(5) 0.6470(4) 0.7032(2) 0.0736(13) Uani 1 1 d . . . H50A H 0.8843 0.6202 0.7311 0.110 Uiso 1 1 calc R C . H50B H 0.8264 0.5798 0.6815 0.110 Uiso 1 1 calc R . . H50C H 0.7146 0.6820 0.7225 0.110 Uiso 1 1 calc R . . C27 C 0.7369(6) 1.4277(4) 0.5908(2) 0.0764(13) Uani 1 1 d . . . H27 H 0.6332 1.4719 0.5962 0.092 Uiso 1 1 calc R . . C26 C 0.8243(7) 1.4294(4) 0.53974(19) 0.0840(15) Uani 1 1 d . . . H26 H 0.7808 1.4736 0.5093 0.101 Uiso 1 1 calc R . . C21 C 1.3287(6) 1.3709(4) 0.6829(2) 0.0829(15) Uani 1 1 d . . . H21 H 1.3334 1.4478 0.6750 0.100 Uiso 1 1 calc R . . C22 C 1.2031(5) 1.3484(3) 0.67619(19) 0.0621(11) Uani 1 1 d . . . H22 H 1.1218 1.4093 0.6638 0.075 Uiso 1 1 calc R . . N2 N 0.8553(3) 1.1571(2) 0.77360(10) 0.0353(5) Uani 1 1 d . . . N3 N 1.0573(3) 1.0661(2) 0.68044(10) 0.0368(6) Uani 1 1 d . . . N1 N 0.7848(3) 0.9788(2) 0.83716(11) 0.0439(6) Uani 1 1 d . . . P1 P 0.68571(9) 1.10528(7) 0.86348(3) 0.03844(18) Uani 1 1 d . B . P2 P 1.03049(9) 1.20411(6) 0.68405(3) 0.03512(16) Uani 1 1 d . C . Si1 Si 0.87195(11) 0.75985(8) 0.65477(4) 0.0467(2) Uani 1 1 d . C . C44 C 1.4025(4) 0.8045(4) 0.48193(16) 0.0574(9) Uani 1 1 d . . . H44 H 1.3323 0.8064 0.4563 0.069 Uiso 1 1 calc R . . C12 C 0.3978(5) 1.2613(4) 0.8672(2) 0.0742(13) Uani 1 1 d . . . H12 H 0.4383 1.3196 0.8725 0.089 Uiso 1 1 calc R . . C16 C 0.4267(5) 1.0655(4) 0.8516(2) 0.0736(12) Uani 1 1 d . . . H16 H 0.4882 0.9856 0.8457 0.088 Uiso 1 1 calc R . . C14 C 0.1879(5) 1.2129(5) 0.8567(2) 0.0797(14) Uani 1 1 d . . . H14 H 0.0840 1.2359 0.8563 0.096 Uiso 1 1 calc R . . C13 C 0.2480(5) 1.2946(5) 0.8646(3) 0.0906(18) Uani 1 1 d . . . H13 H 0.1866 1.3751 0.8683 0.109 Uiso 1 1 calc R . . C45 C 1.4891(7) 0.6783(4) 0.4931(2) 0.0948(18) Uani 1 1 d . . . H45A H 1.5643 0.6740 0.5158 0.142 Uiso 1 1 calc R . . H45B H 1.5386 0.6391 0.4574 0.142 Uiso 1 1 calc R . . H45C H 1.4212 0.6391 0.5135 0.142 Uiso 1 1 calc R . . C15 C 0.2748(6) 1.1001(6) 0.8497(2) 0.0901(16) Uani 1 1 d . . . H15 H 0.2329 1.0433 0.8433 0.108 Uiso 1 1 calc R . . C46 C 1.5077(6) 0.8669(5) 0.4517(2) 0.0945(18) Uani 1 1 d . . . H46A H 1.5797 0.8643 0.4756 0.142 Uiso 1 1 calc R . . H46B H 1.4502 0.9491 0.4438 0.142 Uiso 1 1 calc R . . H46C H 1.5612 0.8275 0.4164 0.142 Uiso 1 1 calc R . . C29 C 0.7944(8) 0.8710(5) 0.8726(3) 0.0277(16) Uiso 0.487(9) 1 d P B 1 C30 C 0.8356(11) 0.8442(8) 0.9238(4) 0.047(2) Uiso 0.487(9) 1 d P B 1 H30 H 0.8645 0.8981 0.9410 0.057 Uiso 0.487(9) 1 calc PR B 1 C31 C 0.8359(11) 0.7394(8) 0.9510(4) 0.057(2) Uiso 0.487(9) 1 d P B 1 H31 H 0.8663 0.7229 0.9867 0.068 Uiso 0.487(9) 1 calc PR B 1 C32 C 0.7943(10) 0.6577(7) 0.9291(4) 0.051(2) Uiso 0.487(9) 1 d P B 1 C33 C 0.7597(10) 0.6795(7) 0.8750(4) 0.0475(19) Uiso 0.487(9) 1 d P B 1 H33 H 0.7361 0.6228 0.8575 0.057 Uiso 0.487(9) 1 calc PR B 1 C34 C 0.7599(9) 0.7854(6) 0.8463(3) 0.0380(17) Uiso 0.487(9) 1 d P B 1 H34 H 0.7371 0.8001 0.8094 0.046 Uiso 0.487(9) 1 calc PR B 1 C35 C 0.7934(13) 0.5458(9) 0.9633(5) 0.078(3) Uiso 0.487(9) 1 d P B 1 H35 H 0.8097 0.5587 1.0013 0.093 Uiso 0.487(9) 1 calc PR B 1 C36 C 0.9097(16) 0.4480(12) 0.9441(6) 0.097(4) Uiso 0.487(9) 1 d P B 1 H36A H 0.9032 0.3797 0.9679 0.145 Uiso 0.487(9) 1 calc PR B 1 H36B H 1.0039 0.4596 0.9453 0.145 Uiso 0.487(9) 1 calc PR B 1 H36C H 0.9057 0.4344 0.9053 0.145 Uiso 0.487(9) 1 calc PR B 1 C37 C 0.6414(12) 0.5330(10) 0.9730(5) 0.081(3) Uiso 0.487(9) 1 d P B 1 H37A H 0.5656 0.6061 0.9883 0.122 Uiso 0.487(9) 1 calc PR B 1 H37B H 0.6402 0.4677 0.9997 0.122 Uiso 0.487(9) 1 calc PR B 1 H37C H 0.6197 0.5169 0.9373 0.122 Uiso 0.487(9) 1 calc PR B 1 Si2 Si 1.2811(3) 0.69008(17) 0.78310(13) 0.0445(7) Uiso 0.575(9) 1 d P C 1 C52 C 1.4012(7) 0.6513(6) 0.7138(3) 0.0456(15) Uiso 0.575(9) 1 d P C 1 H52A H 1.4581 0.5666 0.7135 0.068 Uiso 0.575(9) 1 calc PR C 1 H52B H 1.4702 0.6956 0.7067 0.068 Uiso 0.575(9) 1 calc PR C 1 H52C H 1.3390 0.6709 0.6846 0.068 Uiso 0.575(9) 1 calc PR C 1 C53 C 1.4059(12) 0.6341(9) 0.8365(4) 0.090(3) Uiso 0.575(9) 1 d P C 1 H53A H 1.3469 0.6528 0.8742 0.134 Uiso 0.575(9) 1 calc PR C 1 H53B H 1.4823 0.6716 0.8299 0.134 Uiso 0.575(9) 1 calc PR C 1 H53C H 1.4542 0.5486 0.8334 0.134 Uiso 0.575(9) 1 calc PR C 1 C54 C 1.1588(13) 0.5998(10) 0.7969(5) 0.086(3) Uiso 0.575(9) 1 d P C 1 H54A H 1.0945 0.6190 0.8337 0.129 Uiso 0.575(9) 1 calc PR C 1 H54B H 1.2202 0.5161 0.7967 0.129 Uiso 0.575(9) 1 calc PR C 1 H54C H 1.0968 0.6163 0.7677 0.129 Uiso 0.575(9) 1 calc PR C 1 C5 C 0.6888(8) 1.1237(5) 0.9326(3) 0.0339(16) Uiso 0.624(12) 1 d P B 1 C6 C 0.8172(11) 1.1380(7) 0.9456(3) 0.049(2) Uiso 0.624(12) 1 d P B 1 H6 H 0.8939 1.1435 0.9157 0.059 Uiso 0.624(12) 1 calc PR B 1 C7 C 0.8352(10) 1.1443(6) 1.0016(3) 0.0580(19) Uiso 0.624(12) 1 d P B 1 H7 H 0.9227 1.1535 1.0093 0.070 Uiso 0.624(12) 1 calc PR B 1 C8 C 0.7244(9) 1.1369(6) 1.0444(3) 0.0597(19) Uiso 0.624(12) 1 d P B 1 H8 H 0.7347 1.1412 1.0823 0.072 Uiso 0.624(12) 1 calc PR B 1 C9 C 0.5968(8) 1.1232(7) 1.0329(3) 0.060(2) Uiso 0.624(12) 1 d P B 1 H9 H 0.5202 1.1189 1.0630 0.072 Uiso 0.624(12) 1 calc PR B 1 C10 C 0.5791(7) 1.1156(6) 0.9776(2) 0.0458(15) Uiso 0.624(12) 1 d P B 1 H10 H 0.4917 1.1049 0.9707 0.055 Uiso 0.624(12) 1 calc PR B 1 C29B C 0.7629(8) 0.8724(6) 0.8609(3) 0.0346(17) Uiso 0.513(9) 1 d P B 2 C30B C 0.8065(10) 0.8390(8) 0.9134(4) 0.049(2) Uiso 0.513(9) 1 d P B 2 H30B H 0.8452 0.8866 0.9305 0.059 Uiso 0.513(9) 1 calc PR B 2 C31B C 0.7931(10) 0.7336(8) 0.9414(4) 0.055(2) Uiso 0.513(9) 1 d P B 2 H31B H 0.8186 0.7119 0.9777 0.066 Uiso 0.513(9) 1 calc PR B 2 C32B C 0.7419(10) 0.6641(7) 0.9141(4) 0.052(2) Uiso 0.513(9) 1 d P B 2 C33B C 0.7050(11) 0.6972(7) 0.8627(4) 0.056(2) Uiso 0.513(9) 1 d P B 2 H33B H 0.6728 0.6476 0.8439 0.067 Uiso 0.513(9) 1 calc PR B 2 C34B C 0.7128(10) 0.8015(7) 0.8367(3) 0.0475(19) Uiso 0.513(9) 1 d P B 2 H34B H 0.6824 0.8234 0.8012 0.057 Uiso 0.513(9) 1 calc PR B 2 C35B C 0.7328(11) 0.5455(8) 0.9425(4) 0.065(2) Uiso 0.513(9) 1 d P B 2 H35B H 0.6534 0.5302 0.9268 0.078 Uiso 0.513(9) 1 calc PR B 2 C36B C 0.8596(14) 0.4534(11) 0.9261(6) 0.091(3) Uiso 0.513(9) 1 d P B 2 H36D H 0.8499 0.3808 0.9447 0.136 Uiso 0.513(9) 1 calc PR B 2 H36E H 0.9447 0.4674 0.9364 0.136 Uiso 0.513(9) 1 calc PR B 2 H36F H 0.8758 0.4457 0.8852 0.136 Uiso 0.513(9) 1 calc PR B 2 C37B C 0.6731(12) 0.5589(9) 1.0078(4) 0.081(3) Uiso 0.513(9) 1 d P B 2 H37D H 0.5824 0.6283 1.0145 0.121 Uiso 0.513(9) 1 calc PR B 2 H37E H 0.7495 0.5683 1.0263 0.121 Uiso 0.513(9) 1 calc PR B 2 H37F H 0.6506 0.4884 1.0231 0.121 Uiso 0.513(9) 1 calc PR B 2 Si2B Si 1.2418(5) 0.6852(2) 0.7993(2) 0.0515(9) Uiso 0.425(9) 1 d P C 2 C52B C 1.4028(14) 0.6399(12) 0.7409(6) 0.080(4) Uiso 0.425(9) 1 d P C 2 H52D H 1.4500 0.5540 0.7419 0.120 Uiso 0.425(9) 1 calc PR C 2 H52E H 1.4755 0.6766 0.7449 0.120 Uiso 0.425(9) 1 calc PR C 2 H52F H 1.3682 0.6651 0.7049 0.120 Uiso 0.425(9) 1 calc PR C 2 C53B C 1.3226(15) 0.6203(11) 0.8624(5) 0.081(4) Uiso 0.425(9) 1 d P C 2 H53D H 1.3592 0.5342 0.8605 0.121 Uiso 0.425(9) 1 calc PR C 2 H53E H 1.2460 0.6451 0.8960 0.121 Uiso 0.425(9) 1 calc PR C 2 H53F H 1.4056 0.6472 0.8644 0.121 Uiso 0.425(9) 1 calc PR C 2 C54B C 1.1092(12) 0.6091(9) 0.7913(4) 0.048(2) Uiso 0.425(9) 1 d P C 2 H54D H 1.1576 0.5238 0.7954 0.072 Uiso 0.425(9) 1 calc PR C 2 H54E H 1.0806 0.6279 0.7541 0.072 Uiso 0.425(9) 1 calc PR C 2 H54F H 1.0199 0.6359 0.8203 0.072 Uiso 0.425(9) 1 calc PR C 2 C5B C 0.7225(13) 1.1281(8) 0.9373(4) 0.032(3) Uiso 0.376(12) 1 d P B 2 C6B C 0.8606(16) 1.1197(12) 0.9408(5) 0.048(3) Uiso 0.376(12) 1 d P B 2 H6B H 0.9353 1.1032 0.9081 0.057 Uiso 0.376(12) 1 calc PR B 2 C7B C 0.8957(17) 1.1339(11) 0.9888(5) 0.061(3) Uiso 0.376(12) 1 d P B 2 H7B H 0.9954 1.1246 0.9916 0.073 Uiso 0.376(12) 1 calc PR B 2 C8B C 0.7827(16) 1.1629(11) 1.0349(6) 0.066(4) Uiso 0.376(12) 1 d P B 2 H8B H 0.8042 1.1815 1.0688 0.079 Uiso 0.376(12) 1 calc PR B 2 C9B C 0.6404(16) 1.1659(13) 1.0340(5) 0.068(4) Uiso 0.376(12) 1 d P B 2 H9B H 0.5684 1.1777 1.0675 0.081 Uiso 0.376(12) 1 calc PR B 2 C10B C 0.6029(13) 1.1511(11) 0.9817(4) 0.051(3) Uiso 0.376(12) 1 d P B 2 H10B H 0.5054 1.1565 0.9777 0.061 Uiso 0.376(12) 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Lu1 0.03697(7) 0.02261(6) 0.03572(7) -0.00149(4) 0.00437(5) -0.01128(5) C38 0.0416(16) 0.0326(14) 0.0388(16) -0.0062(12) 0.0091(13) -0.0187(13) C1 0.0433(17) 0.0278(13) 0.0335(14) -0.0016(11) 0.0095(12) -0.0125(12) C4 0.0422(16) 0.0271(13) 0.0322(14) 0.0013(11) 0.0054(12) -0.0140(12) C23 0.058(2) 0.0332(15) 0.0351(15) 0.0025(12) 0.0039(14) -0.0169(14) C41 0.0464(18) 0.0472(18) 0.0442(18) -0.0127(14) 0.0080(14) -0.0220(15) C43 0.0487(19) 0.0447(18) 0.0429(18) -0.0086(14) 0.0012(15) -0.0085(15) C42 0.061(2) 0.052(2) 0.0404(18) -0.0109(15) -0.0020(16) -0.0122(17) C2 0.058(2) 0.0300(15) 0.0431(17) -0.0069(12) 0.0153(15) -0.0150(14) C11 0.0485(19) 0.0478(18) 0.0445(18) 0.0032(14) 0.0059(15) -0.0222(16) C3 0.061(2) 0.0261(14) 0.0448(17) -0.0037(12) 0.0135(15) -0.0186(14) C51 0.058(2) 0.0352(17) 0.065(2) -0.0002(15) -0.0156(18) -0.0118(16) C17 0.0455(18) 0.0375(16) 0.0388(16) -0.0077(12) 0.0122(13) -0.0206(14) C39 0.0439(18) 0.0506(19) 0.0444(18) -0.0115(14) -0.0007(14) -0.0146(15) C47 0.0486(19) 0.0408(17) 0.056(2) -0.0013(15) -0.0031(16) -0.0187(15) C24 0.077(3) 0.051(2) 0.045(2) 0.0097(16) 0.0130(18) -0.0079(19) C18 0.058(2) 0.051(2) 0.058(2) -0.0044(16) -0.0056(17) -0.0241(18) C28 0.059(2) 0.068(2) 0.047(2) 0.0097(17) -0.0074(17) -0.030(2) C40 0.0342(17) 0.054(2) 0.061(2) -0.0172(17) 0.0021(15) -0.0101(15) C48 0.053(2) 0.057(2) 0.067(2) -0.0071(18) -0.0026(18) -0.0215(18) C19 0.058(2) 0.077(3) 0.077(3) -0.008(2) -0.010(2) -0.022(2) C20 0.060(3) 0.096(4) 0.098(4) -0.023(3) 0.008(2) -0.051(3) C25 0.112(4) 0.068(3) 0.042(2) 0.0156(19) 0.010(2) -0.009(3) C49 0.079(3) 0.089(4) 0.106(4) -0.026(3) -0.047(3) -0.013(3) C50 0.077(3) 0.057(2) 0.095(3) -0.009(2) 0.007(2) -0.043(2) C27 0.072(3) 0.083(3) 0.071(3) 0.009(2) -0.022(2) -0.020(2) C26 0.111(4) 0.075(3) 0.054(3) 0.016(2) -0.023(3) -0.016(3) C21 0.076(3) 0.063(3) 0.120(4) -0.011(3) 0.009(3) -0.048(3) C22 0.057(2) 0.0419(19) 0.086(3) -0.0064(18) 0.011(2) -0.0261(17) N2 0.0409(14) 0.0262(11) 0.0330(12) -0.0006(9) 0.0093(10) -0.0126(10) N3 0.0445(14) 0.0272(11) 0.0348(13) -0.0043(9) 0.0093(11) -0.0150(11) N1 0.0538(16) 0.0282(12) 0.0434(14) 0.0000(10) 0.0137(12) -0.0179(12) P1 0.0441(4) 0.0304(4) 0.0346(4) 0.0011(3) 0.0103(3) -0.0145(3) P2 0.0422(4) 0.0280(3) 0.0317(4) -0.0014(3) 0.0086(3) -0.0154(3) Si1 0.0433(5) 0.0431(5) 0.0590(6) -0.0035(4) -0.0106(4) -0.0199(4) C44 0.056(2) 0.060(2) 0.049(2) -0.0219(17) 0.0051(17) -0.0148(18) C12 0.050(2) 0.050(2) 0.122(4) 0.024(2) -0.016(2) -0.0220(19) C16 0.069(3) 0.072(3) 0.083(3) -0.021(2) -0.002(2) -0.030(2) C14 0.056(3) 0.103(4) 0.082(3) 0.014(3) -0.011(2) -0.034(3) C13 0.054(3) 0.073(3) 0.139(5) 0.044(3) -0.018(3) -0.024(2) C45 0.122(5) 0.062(3) 0.075(3) -0.032(2) 0.007(3) -0.004(3) C15 0.075(3) 0.110(4) 0.101(4) -0.019(3) -0.014(3) -0.048(3) C46 0.103(4) 0.097(4) 0.072(3) -0.033(3) 0.049(3) -0.046(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Lu1 N2 2.297(2) . ? Lu1 N3 2.332(2) . ? Lu1 C47 2.347(4) . ? Lu1 C51 2.355(4) . ? Lu1 N1 2.364(2) . ? C38 C39 1.376(5) . ? C38 C43 1.381(5) . ? C38 N3 1.443(4) . ? C1 N2 1.364(3) . ? C1 C2 1.385(4) . ? C1 P1 1.767(3) . ? C4 N2 1.363(3) . ? C4 C3 1.384(4) . ? C4 P2 1.770(3) . ? C23 C28 1.385(5) . ? C23 C24 1.390(5) . ? C23 P2 1.805(3) . ? C41 C40 1.371(5) . ? C41 C42 1.374(5) . ? C41 C44 1.527(4) . ? C43 C42 1.394(5) . ? C43 H43 0.9500 . ? C42 H42 0.9500 . ? C2 C3 1.393(4) . ? C2 H2 0.9500 . ? C11 C12 1.359(5) . ? C11 C16 1.387(5) . ? C11 P1 1.807(4) . ? C3 H3 0.9500 . ? C51 Si2B 1.851(4) . ? C51 Si2 1.855(4) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C17 C18 1.379(5) . ? C17 C22 1.392(5) . ? C17 P2 1.805(3) . ? C39 C40 1.401(5) . ? C39 H39 0.9500 . ? C47 Si1 1.837(3) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C24 C25 1.388(6) . ? C24 H24 0.9500 . ? C18 C19 1.386(6) . ? C18 H18 0.9500 . ? C28 C27 1.383(6) . ? C28 H28 0.9500 . ? C40 H40 0.9500 . ? C48 Si1 1.861(4) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C19 C20 1.368(7) . ? C19 H19 0.9500 . ? C20 C21 1.367(7) . ? C20 H20 0.9500 . ? C25 C26 1.364(7) . ? C25 H25 0.9500 . ? C49 Si1 1.872(5) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 Si1 1.875(4) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C27 C26 1.364(7) . ? C27 H27 0.9500 . ? C26 H26 0.9500 . ? C21 C22 1.381(6) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? N3 P2 1.608(2) . ? N1 C29B 1.434(7) . ? N1 C29 1.485(7) . ? N1 P1 1.608(3) . ? P1 C5 1.719(6) . ? P1 C5B 1.953(11) . ? C44 C45 1.495(6) . ? C44 C46 1.521(6) . ? C44 H44 1.0000 . ? C12 C13 1.380(6) . ? C12 H12 0.9500 . ? C16 C15 1.395(7) . ? C16 H16 0.9500 . ? C14 C15 1.338(7) . ? C14 C13 1.356(7) . ? C14 H14 0.9500 . ? C13 H13 0.9500 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C15 H15 0.9500 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C29 C30 1.353(12) . ? C29 C34 1.429(10) . ? C30 C31 1.380(13) . ? C30 H30 0.9500 . ? C31 C32 1.373(13) . ? C31 H31 0.9500 . ? C32 C33 1.397(12) . ? C32 C35 1.528(13) . ? C33 C34 1.407(10) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 C36 1.362(16) . ? C35 C37 1.510(16) . ? C35 H35 1.0000 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? Si2 C52 1.846(7) . ? Si2 C54 1.849(11) . ? Si2 C53 1.865(10) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C5 C10 1.394(8) . ? C5 C6 1.413(10) . ? C6 C7 1.415(11) . ? C6 H6 0.9500 . ? C7 C8 1.366(11) . ? C7 H7 0.9500 . ? C8 C9 1.389(11) . ? C8 H8 0.9500 . ? C9 C10 1.398(9) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C29B C34B 1.348(11) . ? C29B C30B 1.399(11) . ? C30B C31B 1.428(12) . ? C30B H30B 0.9500 . ? C31B C32B 1.385(12) . ? C31B H31B 0.9500 . ? C32B C33B 1.351(12) . ? C32B C35B 1.563(12) . ? C33B C34B 1.382(11) . ? C33B H33B 0.9500 . ? C34B H34B 0.9500 . ? C35B C36B 1.360(14) . ? C35B C37B 1.580(15) . ? C35B H35B 1.0000 . ? C36B H36D 0.9800 . ? C36B H36E 0.9800 . ? C36B H36F 0.9800 . ? C37B H37D 0.9800 . ? C37B H37E 0.9800 . ? C37B H37F 0.9800 . ? Si2B C53B 1.844(12) . ? Si2B C52B 1.855(13) . ? Si2B C54B 1.873(11) . ? C52B H52D 0.9800 . ? C52B H52E 0.9800 . ? C52B H52F 0.9800 . ? C53B H53D 0.9800 . ? C53B H53E 0.9800 . ? C53B H53F 0.9800 . ? C54B H54D 0.9800 . ? C54B H54E 0.9800 . ? C54B H54F 0.9800 . ? C5B C6B 1.328(17) . ? C5B C10B 1.391(14) . ? C6B C7B 1.315(17) . ? C6B H6B 0.9500 . ? C7B C8B 1.382(19) . ? C7B H7B 0.9500 . ? C8B C9B 1.374(19) . ? C8B H8B 0.9500 . ? C9B C10B 1.426(17) . ? C9B H9B 0.9500 . ? C10B H10B 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 N2 Lu1 N3 71.94(8) . . ? N2 Lu1 C47 117.16(11) . . ? N3 Lu1 C47 94.82(11) . . ? N2 Lu1 C51 116.04(11) . . ? N3 Lu1 C51 101.85(12) . . ? C47 Lu1 C51 126.79(12) . . ? N2 Lu1 N1 72.34(8) . . ? N3 Lu1 N1 144.27(8) . . ? C47 Lu1 N1 100.92(11) . . ? C51 Lu1 N1 94.04(13) . . ? C39 C38 C43 117.7(3) . . ? C39 C38 N3 120.1(3) . . ? C43 C38 N3 122.1(3) . . ? N2 C1 C2 110.6(2) . . ? N2 C1 P1 114.3(2) . . ? C2 C1 P1 135.0(2) . . ? N2 C4 C3 110.7(2) . . ? N2 C4 P2 114.4(2) . . ? C3 C4 P2 135.0(2) . . ? C28 C23 C24 118.7(3) . . ? C28 C23 P2 120.6(2) . . ? C24 C23 P2 120.6(3) . . ? C40 C41 C42 117.6(3) . . ? C40 C41 C44 121.9(3) . . ? C42 C41 C44 120.5(3) . . ? C38 C43 C42 121.2(3) . . ? C38 C43 H43 119.4 . . ? C42 C43 H43 119.4 . . ? C41 C42 C43 121.2(3) . . ? C41 C42 H42 119.4 . . ? C43 C42 H42 119.4 . . ? C1 C2 C3 106.4(3) . . ? C1 C2 H2 126.8 . . ? C3 C2 H2 126.8 . . ? C12 C11 C16 117.5(4) . . ? C12 C11 P1 120.9(3) . . ? C16 C11 P1 121.4(3) . . ? C4 C3 C2 106.4(3) . . ? C4 C3 H3 126.8 . . ? C2 C3 H3 126.8 . . ? Si2B C51 Si2 15.73(11) . . ? Si2B C51 Lu1 128.3(2) . . ? Si2 C51 Lu1 130.7(2) . . ? Si2B C51 H51A 117.6 . . ? Si2 C51 H51A 104.6 . . ? Lu1 C51 H51A 104.6 . . ? Si2B C51 H51B 91.8 . . ? Si2 C51 H51B 104.6 . . ? Lu1 C51 H51B 104.6 . . ? H51A C51 H51B 105.7 . . ? C18 C17 C22 119.3(3) . . ? C18 C17 P2 119.7(2) . . ? C22 C17 P2 121.0(3) . . ? C38 C39 C40 120.6(3) . . ? C38 C39 H39 119.7 . . ? C40 C39 H39 119.7 . . ? Si1 C47 Lu1 136.91(19) . . ? Si1 C47 H47A 102.9 . . ? Lu1 C47 H47A 102.9 . . ? Si1 C47 H47B 102.9 . . ? Lu1 C47 H47B 102.9 . . ? H47A C47 H47B 105.1 . . ? C25 C24 C23 119.5(4) . . ? C25 C24 H24 120.3 . . ? C23 C24 H24 120.3 . . ? C17 C18 C19 120.6(4) . . ? C17 C18 H18 119.7 . . ? C19 C18 H18 119.7 . . ? C27 C28 C23 120.8(4) . . ? C27 C28 H28 119.6 . . ? C23 C28 H28 119.6 . . ? C41 C40 C39 121.6(3) . . ? C41 C40 H40 119.2 . . ? C39 C40 H40 119.2 . . ? Si1 C48 H48A 109.5 . . ? Si1 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? Si1 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C20 C19 C18 119.7(4) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C21 C20 C19 120.2(4) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C26 C25 C24 120.8(4) . . ? C26 C25 H25 119.6 . . ? C24 C25 H25 119.6 . . ? Si1 C49 H49A 109.5 . . ? Si1 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? Si1 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? Si1 C50 H50A 109.5 . . ? Si1 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? Si1 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C26 C27 C28 119.8(5) . . ? C26 C27 H27 120.1 . . ? C28 C27 H27 120.1 . . ? C27 C26 C25 120.4(4) . . ? C27 C26 H26 119.8 . . ? C25 C26 H26 119.8 . . ? C20 C21 C22 120.8(4) . . ? C20 C21 H21 119.6 . . ? C22 C21 H21 119.6 . . ? C21 C22 C17 119.4(4) . . ? C21 C22 H22 120.3 . . ? C17 C22 H22 120.3 . . ? C4 N2 C1 105.8(2) . . ? C4 N2 Lu1 126.50(18) . . ? C1 N2 Lu1 126.83(18) . . ? C38 N3 P2 120.18(19) . . ? C38 N3 Lu1 116.67(17) . . ? P2 N3 Lu1 123.09(12) . . ? C29B N1 C29 17.7(3) . . ? C29B N1 P1 121.7(3) . . ? C29 N1 P1 119.0(3) . . ? C29B N1 Lu1 116.5(3) . . ? C29 N1 Lu1 118.3(3) . . ? P1 N1 Lu1 121.47(13) . . ? N1 P1 C5 117.1(2) . . ? N1 P1 C1 104.17(13) . . ? C5 P1 C1 109.3(3) . . ? N1 P1 C11 114.23(16) . . ? C5 P1 C11 102.7(3) . . ? C1 P1 C11 109.21(15) . . ? N1 P1 C5B 114.3(3) . . ? C5 P1 C5B 9.7(4) . . ? C1 P1 C5B 102.1(3) . . ? C11 P1 C5B 111.7(4) . . ? N3 P2 C4 103.15(13) . . ? N3 P2 C23 116.30(15) . . ? C4 P2 C23 108.23(15) . . ? N3 P2 C17 113.95(15) . . ? C4 P2 C17 109.53(14) . . ? C23 P2 C17 105.49(16) . . ? C47 Si1 C48 112.85(17) . . ? C47 Si1 C49 112.1(2) . . ? C48 Si1 C49 107.1(2) . . ? C47 Si1 C50 110.72(19) . . ? C48 Si1 C50 107.3(2) . . ? C49 Si1 C50 106.4(3) . . ? C45 C44 C46 109.8(4) . . ? C45 C44 C41 113.5(4) . . ? C46 C44 C41 109.9(3) . . ? C45 C44 H44 107.8 . . ? C46 C44 H44 107.8 . . ? C41 C44 H44 107.8 . . ? C11 C12 C13 121.4(4) . . ? C11 C12 H12 119.3 . . ? C13 C12 H12 119.3 . . ? C11 C16 C15 120.5(5) . . ? C11 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C15 C14 C13 120.1(5) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C14 C13 C12 120.3(5) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C14 C15 C16 120.1(5) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C44 C46 H46A 109.5 . . ? C44 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C44 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C30 C29 C34 118.5(7) . . ? C30 C29 N1 128.7(6) . . ? C34 C29 N1 112.8(6) . . ? C29 C30 C31 120.6(9) . . ? C29 C30 H30 119.7 . . ? C31 C30 H30 119.7 . . ? C32 C31 C30 123.1(9) . . ? C32 C31 H31 118.4 . . ? C30 C31 H31 118.4 . . ? C31 C32 C33 117.7(8) . . ? C31 C32 C35 119.4(9) . . ? C33 C32 C35 122.9(8) . . ? C32 C33 C34 120.0(7) . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? C33 C34 C29 120.0(7) . . ? C33 C34 H34 120.0 . . ? C29 C34 H34 120.0 . . ? C36 C35 C37 115.3(11) . . ? C36 C35 C32 113.4(10) . . ? C37 C35 C32 111.5(9) . . ? C36 C35 H35 105.2 . . ? C37 C35 H35 105.2 . . ? C32 C35 H35 105.2 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C52 Si2 C54 108.4(4) . . ? C52 Si2 C51 115.7(3) . . ? C54 Si2 C51 108.7(4) . . ? C52 Si2 C53 106.4(4) . . ? C54 Si2 C53 103.6(5) . . ? C51 Si2 C53 113.3(4) . . ? Si2 C52 H52A 109.5 . . ? Si2 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? Si2 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? Si2 C53 H53A 109.5 . . ? Si2 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? Si2 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? Si2 C54 H54A 109.5 . . ? Si2 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? Si2 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C10 C5 C6 117.2(6) . . ? C10 C5 P1 124.6(5) . . ? C6 C5 P1 117.9(5) . . ? C5 C6 C7 122.0(8) . . ? C5 C6 H6 119.0 . . ? C7 C6 H6 119.0 . . ? C8 C7 C6 118.9(8) . . ? C8 C7 H7 120.6 . . ? C6 C7 H7 120.6 . . ? C7 C8 C9 120.2(7) . . ? C7 C8 H8 119.9 . . ? C9 C8 H8 119.9 . . ? C8 C9 C10 121.2(7) . . ? C8 C9 H9 119.4 . . ? C10 C9 H9 119.4 . . ? C5 C10 C9 120.5(6) . . ? C5 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C34B C29B C30B 118.7(7) . . ? C34B C29B N1 126.6(7) . . ? C30B C29B N1 114.6(7) . . ? C29B C30B C31B 120.5(8) . . ? C29B C30B H30B 119.8 . . ? C31B C30B H30B 119.8 . . ? C32B C31B C30B 117.9(8) . . ? C32B C31B H31B 121.0 . . ? C30B C31B H31B 121.0 . . ? C33B C32B C31B 120.0(8) . . ? C33B C32B C35B 120.8(8) . . ? C31B C32B C35B 119.2(8) . . ? C32B C33B C34B 121.7(8) . . ? C32B C33B H33B 119.1 . . ? C34B C33B H33B 119.1 . . ? C29B C34B C33B 121.1(8) . . ? C29B C34B H34B 119.5 . . ? C33B C34B H34B 119.5 . . ? C36B C35B C32B 111.8(9) . . ? C36B C35B C37B 116.9(9) . . ? C32B C35B C37B 111.4(7) . . ? C36B C35B H35B 105.2 . . ? C32B C35B H35B 105.2 . . ? C37B C35B H35B 105.2 . . ? C35B C36B H36D 109.5 . . ? C35B C36B H36E 109.5 . . ? H36D C36B H36E 109.5 . . ? C35B C36B H36F 109.5 . . ? H36D C36B H36F 109.5 . . ? H36E C36B H36F 109.5 . . ? C35B C37B H37D 109.5 . . ? C35B C37B H37E 109.5 . . ? H37D C37B H37E 109.5 . . ? C35B C37B H37F 109.5 . . ? H37D C37B H37F 109.5 . . ? H37E C37B H37F 109.5 . . ? C53B Si2B C51 119.1(4) . . ? C53B Si2B C52B 103.9(6) . . ? C51 Si2B C52B 104.6(5) . . ? C53B Si2B C54B 106.8(5) . . ? C51 Si2B C54B 113.5(4) . . ? C52B Si2B C54B 108.0(5) . . ? Si2B C52B H52D 109.5 . . ? Si2B C52B H52E 109.5 . . ? H52D C52B H52E 109.5 . . ? Si2B C52B H52F 109.5 . . ? H52D C52B H52F 109.5 . . ? H52E C52B H52F 109.5 . . ? Si2B C53B H53D 109.5 . . ? Si2B C53B H53E 109.5 . . ? H53D C53B H53E 109.5 . . ? Si2B C53B H53F 109.5 . . ? H53D C53B H53F 109.5 . . ? H53E C53B H53F 109.5 . . ? Si2B C54B H54D 109.5 . . ? Si2B C54B H54E 109.5 . . ? H54D C54B H54E 109.5 . . ? Si2B C54B H54F 109.5 . . ? H54D C54B H54F 109.5 . . ? H54E C54B H54F 109.5 . . ? C6B C5B C10B 125.5(12) . . ? C6B C5B P1 116.9(8) . . ? C10B C5B P1 117.6(9) . . ? C7B C6B C5B 121.2(13) . . ? C7B C6B H6B 119.4 . . ? C5B C6B H6B 119.4 . . ? C6B C7B C8B 117.7(14) . . ? C6B C7B H7B 121.1 . . ? C8B C7B H7B 121.1 . . ? C9B C8B C7B 122.9(13) . . ? C9B C8B H8B 118.6 . . ? C7B C8B H8B 118.6 . . ? C8B C9B C10B 118.8(12) . . ? C8B C9B H9B 120.6 . . ? C10B C9B H9B 120.6 . . ? C5B C10B C9B 113.6(11) . . ? C5B C10B H10B 123.2 . . ? C9B C10B H10B 123.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C39 C38 C43 C42 -3.2(5) . . . . ? N3 C38 C43 C42 -178.9(3) . . . . ? C40 C41 C42 C43 0.6(6) . . . . ? C44 C41 C42 C43 -177.9(3) . . . . ? C38 C43 C42 C41 2.0(6) . . . . ? N2 C1 C2 C3 0.2(4) . . . . ? P1 C1 C2 C3 177.6(3) . . . . ? N2 C4 C3 C2 0.2(4) . . . . ? P2 C4 C3 C2 179.8(3) . . . . ? C1 C2 C3 C4 -0.2(4) . . . . ? N2 Lu1 C51 Si2B 162.4(3) . . . . ? N3 Lu1 C51 Si2B -122.0(3) . . . . ? C47 Lu1 C51 Si2B -16.7(4) . . . . ? N1 Lu1 C51 Si2B 90.1(3) . . . . ? N2 Lu1 C51 Si2 -177.3(3) . . . . ? N3 Lu1 C51 Si2 -101.8(3) . . . . ? C47 Lu1 C51 Si2 3.5(4) . . . . ? N1 Lu1 C51 Si2 110.3(3) . . . . ? C43 C38 C39 C40 1.9(5) . . . . ? N3 C38 C39 C40 177.7(3) . . . . ? N2 Lu1 C47 Si1 171.0(2) . . . . ? N3 Lu1 C47 Si1 98.8(3) . . . . ? C51 Lu1 C47 Si1 -9.9(3) . . . . ? N1 Lu1 C47 Si1 -113.4(3) . . . . ? C28 C23 C24 C25 -2.4(6) . . . . ? P2 C23 C24 C25 174.9(4) . . . . ? C22 C17 C18 C19 1.0(6) . . . . ? P2 C17 C18 C19 -176.4(3) . . . . ? C24 C23 C28 C27 1.1(6) . . . . ? P2 C23 C28 C27 -176.1(3) . . . . ? C42 C41 C40 C39 -1.9(5) . . . . ? C44 C41 C40 C39 176.6(3) . . . . ? C38 C39 C40 C41 0.7(5) . . . . ? C17 C18 C19 C20 0.6(6) . . . . ? C18 C19 C20 C21 -1.8(7) . . . . ? C23 C24 C25 C26 1.8(8) . . . . ? C23 C28 C27 C26 0.7(7) . . . . ? C28 C27 C26 C25 -1.4(8) . . . . ? C24 C25 C26 C27 0.1(9) . . . . ? C19 C20 C21 C22 1.5(8) . . . . ? C20 C21 C22 C17 0.1(7) . . . . ? C18 C17 C22 C21 -1.4(6) . . . . ? P2 C17 C22 C21 176.0(3) . . . . ? C3 C4 N2 C1 -0.1(4) . . . . ? P2 C4 N2 C1 -179.8(2) . . . . ? C3 C4 N2 Lu1 -170.2(2) . . . . ? P2 C4 N2 Lu1 10.1(4) . . . . ? C2 C1 N2 C4 -0.1(4) . . . . ? P1 C1 N2 C4 -178.1(2) . . . . ? C2 C1 N2 Lu1 170.0(2) . . . . ? P1 C1 N2 Lu1 -8.0(4) . . . . ? N3 Lu1 N2 C4 -9.7(2) . . . . ? C47 Lu1 N2 C4 -95.8(3) . . . . ? C51 Lu1 N2 C4 84.9(3) . . . . ? N1 Lu1 N2 C4 170.7(3) . . . . ? N3 Lu1 N2 C1 -177.9(3) . . . . ? C47 Lu1 N2 C1 96.0(3) . . . . ? C51 Lu1 N2 C1 -83.2(3) . . . . ? N1 Lu1 N2 C1 2.6(3) . . . . ? C39 C38 N3 P2 113.7(3) . . . . ? C43 C38 N3 P2 -70.8(4) . . . . ? C39 C38 N3 Lu1 -69.2(3) . . . . ? C43 C38 N3 Lu1 106.4(3) . . . . ? N2 Lu1 N3 C38 -170.0(2) . . . . ? C47 Lu1 N3 C38 -53.0(2) . . . . ? C51 Lu1 N3 C38 76.2(2) . . . . ? N1 Lu1 N3 C38 -169.3(2) . . . . ? N2 Lu1 N3 P2 7.08(16) . . . . ? C47 Lu1 N3 P2 124.10(18) . . . . ? C51 Lu1 N3 P2 -106.71(18) . . . . ? N1 Lu1 N3 P2 7.8(3) . . . . ? N2 Lu1 N1 C29B 177.5(4) . . . . ? N3 Lu1 N1 C29B 176.7(4) . . . . ? C47 Lu1 N1 C29B 62.2(4) . . . . ? C51 Lu1 N1 C29B -66.5(4) . . . . ? N2 Lu1 N1 C29 -162.7(4) . . . . ? N3 Lu1 N1 C29 -163.5(4) . . . . ? C47 Lu1 N1 C29 82.0(4) . . . . ? C51 Lu1 N1 C29 -46.7(4) . . . . ? N2 Lu1 N1 P1 4.36(17) . . . . ? N3 Lu1 N1 P1 3.6(3) . . . . ? C47 Lu1 N1 P1 -110.89(19) . . . . ? C51 Lu1 N1 P1 120.4(2) . . . . ? C29B N1 P1 C5 58.1(6) . . . . ? C29 N1 P1 C5 37.8(5) . . . . ? Lu1 N1 P1 C5 -129.2(3) . . . . ? C29B N1 P1 C1 178.9(5) . . . . ? C29 N1 P1 C1 158.6(4) . . . . ? Lu1 N1 P1 C1 -8.4(2) . . . . ? C29B N1 P1 C11 -62.0(5) . . . . ? C29 N1 P1 C11 -82.3(4) . . . . ? Lu1 N1 P1 C11 110.69(18) . . . . ? C29B N1 P1 C5B 68.4(6) . . . . ? C29 N1 P1 C5B 48.1(6) . . . . ? Lu1 N1 P1 C5B -118.9(4) . . . . ? N2 C1 P1 N1 9.7(3) . . . . ? C2 C1 P1 N1 -167.7(4) . . . . ? N2 C1 P1 C5 135.5(3) . . . . ? C2 C1 P1 C5 -41.8(5) . . . . ? N2 C1 P1 C11 -112.8(3) . . . . ? C2 C1 P1 C11 69.9(4) . . . . ? N2 C1 P1 C5B 128.9(4) . . . . ? C2 C1 P1 C5B -48.5(5) . . . . ? C12 C11 P1 N1 -160.6(3) . . . . ? C16 C11 P1 N1 14.1(4) . . . . ? C12 C11 P1 C5 71.5(4) . . . . ? C16 C11 P1 C5 -113.7(4) . . . . ? C12 C11 P1 C1 -44.5(4) . . . . ? C16 C11 P1 C1 130.3(3) . . . . ? C12 C11 P1 C5B 67.7(5) . . . . ? C16 C11 P1 C5B -117.6(5) . . . . ? C38 N3 P2 C4 172.4(2) . . . . ? Lu1 N3 P2 C4 -4.6(2) . . . . ? C38 N3 P2 C23 54.1(3) . . . . ? Lu1 N3 P2 C23 -122.90(17) . . . . ? C38 N3 P2 C17 -69.0(3) . . . . ? Lu1 N3 P2 C17 114.04(17) . . . . ? N2 C4 P2 N3 -2.9(3) . . . . ? C3 C4 P2 N3 177.5(4) . . . . ? N2 C4 P2 C23 120.8(2) . . . . ? C3 C4 P2 C23 -58.7(4) . . . . ? N2 C4 P2 C17 -124.6(2) . . . . ? C3 C4 P2 C17 55.8(4) . . . . ? C28 C23 P2 N3 98.5(3) . . . . ? C24 C23 P2 N3 -78.7(3) . . . . ? C28 C23 P2 C4 -16.9(3) . . . . ? C24 C23 P2 C4 165.9(3) . . . . ? C28 C23 P2 C17 -134.1(3) . . . . ? C24 C23 P2 C17 48.7(3) . . . . ? C18 C17 P2 N3 -19.9(3) . . . . ? C22 C17 P2 N3 162.7(3) . . . . ? C18 C17 P2 C4 95.1(3) . . . . ? C22 C17 P2 C4 -82.3(3) . . . . ? C18 C17 P2 C23 -148.6(3) . . . . ? C22 C17 P2 C23 34.0(3) . . . . ? Lu1 C47 Si1 C48 -39.1(3) . . . . ? Lu1 C47 Si1 C49 -160.2(3) . . . . ? Lu1 C47 Si1 C50 81.2(3) . . . . ? C40 C41 C44 C45 36.6(6) . . . . ? C42 C41 C44 C45 -144.9(4) . . . . ? C40 C41 C44 C46 -86.7(5) . . . . ? C42 C41 C44 C46 91.7(5) . . . . ? C16 C11 C12 C13 3.1(7) . . . . ? P1 C11 C12 C13 178.1(4) . . . . ? C12 C11 C16 C15 -3.8(7) . . . . ? P1 C11 C16 C15 -178.7(4) . . . . ? C15 C14 C13 C12 -2.2(9) . . . . ? C11 C12 C13 C14 -0.2(9) . . . . ? C13 C14 C15 C16 1.5(9) . . . . ? C11 C16 C15 C14 1.5(8) . . . . ? C29B N1 C29 C30 -158.3(19) . . . . ? P1 N1 C29 C30 -54.5(9) . . . . ? Lu1 N1 C29 C30 112.9(7) . . . . ? C29B N1 C29 C34 24.3(12) . . . . ? P1 N1 C29 C34 128.1(5) . . . . ? Lu1 N1 C29 C34 -64.5(6) . . . . ? C34 C29 C30 C31 -3.6(12) . . . . ? N1 C29 C30 C31 179.1(7) . . . . ? C29 C30 C31 C32 -0.6(14) . . . . ? C30 C31 C32 C33 4.3(14) . . . . ? C30 C31 C32 C35 -178.0(9) . . . . ? C31 C32 C33 C34 -3.6(13) . . . . ? C35 C32 C33 C34 178.7(8) . . . . ? C32 C33 C34 C29 -0.4(12) . . . . ? C30 C29 C34 C33 4.1(11) . . . . ? N1 C29 C34 C33 -178.2(6) . . . . ? C31 C32 C35 C36 -105.2(12) . . . . ? C33 C32 C35 C36 72.3(14) . . . . ? C31 C32 C35 C37 122.6(11) . . . . ? C33 C32 C35 C37 -59.8(13) . . . . ? Si2B C51 Si2 C52 158.2(6) . . . . ? Lu1 C51 Si2 C52 70.1(4) . . . . ? Si2B C51 Si2 C54 36.0(6) . . . . ? Lu1 C51 Si2 C54 -52.1(5) . . . . ? Si2B C51 Si2 C53 -78.5(6) . . . . ? Lu1 C51 Si2 C53 -166.7(4) . . . . ? N1 P1 C5 C10 -99.2(6) . . . . ? C1 P1 C5 C10 142.7(5) . . . . ? C11 P1 C5 C10 26.8(6) . . . . ? C5B P1 C5 C10 -175(3) . . . . ? N1 P1 C5 C6 75.1(6) . . . . ? C1 P1 C5 C6 -43.0(6) . . . . ? C11 P1 C5 C6 -158.9(5) . . . . ? C5B P1 C5 C6 -1(2) . . . . ? C10 C5 C6 C7 -0.1(10) . . . . ? P1 C5 C6 C7 -174.9(6) . . . . ? C5 C6 C7 C8 -0.3(11) . . . . ? C6 C7 C8 C9 0.1(11) . . . . ? C7 C8 C9 C10 0.6(11) . . . . ? C6 C5 C10 C9 0.8(9) . . . . ? P1 C5 C10 C9 175.2(5) . . . . ? C8 C9 C10 C5 -1.1(11) . . . . ? C29 N1 C29B C34B -160(2) . . . . ? P1 N1 C29B C34B 113.8(7) . . . . ? Lu1 N1 C29B C34B -59.2(8) . . . . ? C29 N1 C29B C30B 16.9(12) . . . . ? P1 N1 C29B C30B -69.7(7) . . . . ? Lu1 N1 C29B C30B 117.3(6) . . . . ? C34B C29B C30B C31B -2.1(12) . . . . ? N1 C29B C30B C31B -179.0(7) . . . . ? C29B C30B C31B C32B 2.6(13) . . . . ? C30B C31B C32B C33B -0.6(13) . . . . ? C30B C31B C32B C35B 177.3(8) . . . . ? C31B C32B C33B C34B -1.8(13) . . . . ? C35B C32B C33B C34B -179.7(8) . . . . ? C30B C29B C34B C33B -0.3(12) . . . . ? N1 C29B C34B C33B 176.1(7) . . . . ? C32B C33B C34B C29B 2.4(13) . . . . ? C33B C32B C35B C36B 85.7(12) . . . . ? C31B C32B C35B C36B -92.2(11) . . . . ? C33B C32B C35B C37B -141.5(9) . . . . ? C31B C32B C35B C37B 40.6(11) . . . . ? Si2 C51 Si2B C53B 110.9(7) . . . . ? Lu1 C51 Si2B C53B -144.3(5) . . . . ? Si2 C51 Si2B C52B -4.5(6) . . . . ? Lu1 C51 Si2B C52B 100.3(6) . . . . ? Si2 C51 Si2B C54B -122.0(7) . . . . ? Lu1 C51 Si2B C54B -17.2(6) . . . . ? N1 P1 C5B C6B 59.5(10) . . . . ? C5 P1 C5B C6B 168(3) . . . . ? C1 P1 C5B C6B -52.2(9) . . . . ? C11 P1 C5B C6B -168.8(8) . . . . ? N1 P1 C5B C10B -120.2(8) . . . . ? C5 P1 C5B C10B -11(2) . . . . ? C1 P1 C5B C10B 128.0(8) . . . . ? C11 P1 C5B C10B 11.4(9) . . . . ? C10B C5B C6B C7B -0.4(19) . . . . ? P1 C5B C6B C7B 179.9(10) . . . . ? C5B C6B C7B C8B -2.7(19) . . . . ? C6B C7B C8B C9B 6.5(19) . . . . ? C7B C8B C9B C10B -7(2) . . . . ? C6B C5B C10B C9B 0.0(17) . . . . ? P1 C5B C10B C9B 179.7(8) . . . . ? C8B C9B C10B C5B 3.5(17) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.124 _refine_diff_density_min -0.853 _refine_diff_density_rms 0.074 # start Validation Reply Form _vrf_PLAT201_ph11026 ; PROBLEM: Isotropic non-H Atoms in Main Residue RESPONSE: Various moieties (one phenyl ring, C5; one 4-isopropylphenyl ring, C29; and one TMS group, Si2) were disordered over two positions. Disordered atoms were held isotropic. ; # end Validation Reply Form