# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_complex1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H80 N5 Si2 Sm' _chemical_formula_sum 'C48 H80 N5 Si2 Sm' _chemical_formula_weight 933.70 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' Sm Sm -0.1638 3.4418 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.5601(11) _cell_length_b 12.3884(15) _cell_length_c 17.6788(17) _cell_angle_alpha 84.091(7) _cell_angle_beta 81.737(6) _cell_angle_gamma 86.887(9) _cell_volume 2490.2(5) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 12195 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.245 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 986 _exptl_absorpt_coefficient_mu 1.263 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.541 _exptl_absorpt_correction_T_max 0.804 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20400 _diffrn_reflns_av_R_equivalents 0.0559 _diffrn_reflns_av_unetI/netI 0.0858 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 25.50 _reflns_number_total 9189 _reflns_number_gt 7960 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _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^)+(0.0255P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9189 _refine_ls_number_parameters 520 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0653 _refine_ls_R_factor_gt 0.0529 _refine_ls_wR_factor_ref 0.0917 _refine_ls_wR_factor_gt 0.0866 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.117 _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 Sm1 Sm 0.70064(2) 0.758976(17) 0.732440(13) 0.03151(9) Uani 1 1 d . . . Si1 Si 0.55469(12) 0.57123(10) 0.65146(8) 0.0429(3) Uani 1 1 d . . . Si2 Si 0.60748(13) 0.78401(10) 0.55577(8) 0.0424(3) Uani 1 1 d . . . N1 N 0.8076(3) 0.9105(2) 0.75283(19) 0.0296(8) Uani 1 1 d . . . N2 N 0.8265(3) 0.6491(3) 0.7934(2) 0.0312(8) Uani 1 1 d . . . N3 N 0.6128(3) 0.6974(3) 0.6366(2) 0.0346(9) Uani 1 1 d . . . N4 N 0.6136(3) 0.7972(3) 0.8567(2) 0.0330(9) Uani 1 1 d . . . N5 N 0.6612(3) 0.7484(3) 0.9807(2) 0.0386(9) Uani 1 1 d D . . H5 H 0.5868 0.7435 0.9970 0.046 Uiso 1 1 calc RD . . C1 C 0.8859(4) 0.9895(3) 0.8548(3) 0.0461(13) Uani 1 1 d . . . H1A H 0.8997 1.0565 0.8256 0.055 Uiso 1 1 calc R . . H1B H 0.9044 0.9786 0.9052 0.055 Uiso 1 1 calc R . . C2 C 0.8379(4) 0.9061(3) 0.8234(2) 0.0272(10) Uani 1 1 d . . . C3 C 0.8202(4) 0.7994(3) 0.8756(2) 0.0272(10) Uani 1 1 d . . . H3 H 0.8574 0.8096 0.9213 0.033 Uiso 1 1 calc R . . C4 C 0.8843(4) 0.6992(3) 0.8428(2) 0.0298(10) Uani 1 1 d . . . C5 C 0.9875(4) 0.6681(3) 0.8648(3) 0.0429(12) Uani 1 1 d . . . H5A H 1.0285 0.6064 0.8464 0.051 Uiso 1 1 calc R . . H5B H 1.0194 0.7079 0.8988 0.051 Uiso 1 1 calc R . . C6 C 0.8247(4) 1.0109(3) 0.7034(2) 0.0321(11) Uani 1 1 d . . . C7 C 0.9331(4) 1.0292(3) 0.6585(2) 0.0368(11) Uani 1 1 d . . . C8 C 0.9420(5) 1.1207(4) 0.6050(3) 0.0464(13) Uani 1 1 d . . . H8 H 1.0141 1.1345 0.5744 0.056 Uiso 1 1 calc R . . C9 C 0.8482(5) 1.1904(4) 0.5963(3) 0.0507(14) Uani 1 1 d . . . H9 H 0.8553 1.2498 0.5585 0.061 Uiso 1 1 calc R . . C10 C 0.7435(5) 1.1738(4) 0.6428(3) 0.0487(13) Uani 1 1 d . . . H10 H 0.6801 1.2234 0.6375 0.058 Uiso 1 1 calc R . . C11 C 0.7300(4) 1.0846(3) 0.6974(2) 0.0378(11) Uani 1 1 d . . . C12 C 1.0398(4) 0.9550(4) 0.6663(3) 0.0439(13) Uani 1 1 d . . . H12 H 1.0179 0.8975 0.7083 0.053 Uiso 1 1 calc R . . C13 C 1.0789(5) 0.8998(4) 0.5927(3) 0.0598(15) Uani 1 1 d . . . H13A H 1.0156 0.8582 0.5817 0.090 Uiso 1 1 calc R . . H13B H 1.1464 0.8515 0.5995 0.090 Uiso 1 1 calc R . . H13C H 1.0996 0.9545 0.5503 0.090 Uiso 1 1 calc R . . C14 C 1.1419(5) 1.0143(5) 0.6873(3) 0.0685(17) Uani 1 1 d . . . H14A H 1.1680 1.0688 0.6458 0.103 Uiso 1 1 calc R . . H14B H 1.2059 0.9626 0.6956 0.103 Uiso 1 1 calc R . . H14C H 1.1165 1.0493 0.7339 0.103 Uiso 1 1 calc R . . C15 C 0.6152(4) 1.0728(4) 0.7505(3) 0.0483(13) Uani 1 1 d . . . H15 H 0.6146 0.9976 0.7757 0.058 Uiso 1 1 calc R . . C16 C 0.5062(5) 1.0904(5) 0.7094(4) 0.0770(19) Uani 1 1 d . . . H16A H 0.5036 1.1638 0.6845 0.116 Uiso 1 1 calc R . . H16B H 0.4365 1.0794 0.7466 0.116 Uiso 1 1 calc R . . H16C H 0.5096 1.0391 0.6712 0.116 Uiso 1 1 calc R . . C17 C 0.6073(5) 1.1494(4) 0.8139(3) 0.0723(18) Uani 1 1 d . . . H17A H 0.6741 1.1352 0.8415 0.108 Uiso 1 1 calc R . . H17B H 0.5358 1.1375 0.8492 0.108 Uiso 1 1 calc R . . H17C H 0.6071 1.2241 0.7912 0.108 Uiso 1 1 calc R . . C18 C 0.8635(4) 0.5392(3) 0.7792(3) 0.0316(10) Uani 1 1 d . . . C19 C 0.8321(4) 0.4531(3) 0.8360(3) 0.0356(11) Uani 1 1 d . . . C20 C 0.8570(4) 0.3475(4) 0.8171(3) 0.0471(13) Uani 1 1 d . . . H20 H 0.8367 0.2894 0.8544 0.056 Uiso 1 1 calc R . . C21 C 0.9105(5) 0.3253(4) 0.7456(3) 0.0529(14) Uani 1 1 d . . . H21 H 0.9242 0.2530 0.7338 0.063 Uiso 1 1 calc R . . C22 C 0.9439(4) 0.4098(4) 0.6913(3) 0.0486(13) Uani 1 1 d . . . H22 H 0.9816 0.3945 0.6426 0.058 Uiso 1 1 calc R . . C23 C 0.9227(4) 0.5177(3) 0.7071(3) 0.0379(11) Uani 1 1 d . . . C24 C 0.7753(4) 0.4712(3) 0.9167(3) 0.0402(12) Uani 1 1 d . . . H24 H 0.7660 0.5506 0.9200 0.048 Uiso 1 1 calc R . . C25 C 0.6532(4) 0.4240(4) 0.9358(3) 0.0520(14) Uani 1 1 d . . . H25A H 0.6012 0.4625 0.9028 0.078 Uiso 1 1 calc R . . H25B H 0.6228 0.4322 0.9890 0.078 Uiso 1 1 calc R . . H25C H 0.6585 0.3476 0.9275 0.078 Uiso 1 1 calc R . . C26 C 0.8542(5) 0.4245(4) 0.9759(3) 0.0519(14) Uani 1 1 d . . . H26A H 0.8651 0.3466 0.9739 0.078 Uiso 1 1 calc R . . H26B H 0.8178 0.4396 1.0269 0.078 Uiso 1 1 calc R . . H26C H 0.9295 0.4579 0.9644 0.078 Uiso 1 1 calc R . . C27 C 0.9714(4) 0.6079(4) 0.6479(3) 0.0444(13) Uani 1 1 d . . . H27 H 0.9505 0.6779 0.6698 0.053 Uiso 1 1 calc R . . C28 C 0.9226(5) 0.6128(4) 0.5723(3) 0.0605(15) Uani 1 1 d . . . H28A H 0.9412 0.5448 0.5497 0.091 Uiso 1 1 calc R . . H28B H 0.9570 0.6719 0.5374 0.091 Uiso 1 1 calc R . . H28C H 0.8384 0.6250 0.5813 0.091 Uiso 1 1 calc R . . C29 C 1.1041(5) 0.5958(5) 0.6336(4) 0.088(2) Uani 1 1 d . . . H29A H 1.1270 0.5264 0.6139 0.132 Uiso 1 1 calc R . . H29B H 1.1352 0.5994 0.6813 0.132 Uiso 1 1 calc R . . H29C H 1.1346 0.6540 0.5963 0.132 Uiso 1 1 calc R . . C30 C 0.7122(5) 0.8931(4) 0.5599(3) 0.0595(15) Uani 1 1 d . . . H30A H 0.6908 0.9275 0.6070 0.089 Uiso 1 1 calc R . . H30B H 0.7091 0.9470 0.5162 0.089 Uiso 1 1 calc R . . H30C H 0.7910 0.8613 0.5584 0.089 Uiso 1 1 calc R . . C31 C 0.6533(6) 0.7233(4) 0.4639(3) 0.0679(17) Uani 1 1 d . . . H31A H 0.7333 0.6945 0.4623 0.102 Uiso 1 1 calc R . . H31B H 0.6484 0.7785 0.4213 0.102 Uiso 1 1 calc R . . H31C H 0.6023 0.6651 0.4601 0.102 Uiso 1 1 calc R . . C32 C 0.4592(5) 0.8500(4) 0.5501(4) 0.0752(19) Uani 1 1 d . . . H32A H 0.4044 0.7954 0.5452 0.113 Uiso 1 1 calc R . . H32B H 0.4630 0.9035 0.5058 0.113 Uiso 1 1 calc R . . H32C H 0.4332 0.8855 0.5964 0.113 Uiso 1 1 calc R . . C33 C 0.5644(5) 0.5140(4) 0.7532(3) 0.0624(16) Uani 1 1 d . . . H33A H 0.6457 0.5080 0.7615 0.094 Uiso 1 1 calc R . . H33B H 0.5315 0.4427 0.7622 0.094 Uiso 1 1 calc R . . H33C H 0.5211 0.5618 0.7883 0.094 Uiso 1 1 calc R . . C34 C 0.6324(5) 0.4705(4) 0.5890(3) 0.0718(18) Uani 1 1 d . . . H34A H 0.6358 0.4992 0.5356 0.108 Uiso 1 1 calc R . . H34B H 0.5908 0.4035 0.5975 0.108 Uiso 1 1 calc R . . H34C H 0.7112 0.4564 0.6014 0.108 Uiso 1 1 calc R . . C35 C 0.3977(5) 0.5752(4) 0.6384(3) 0.0667(17) Uani 1 1 d . . . H35A H 0.3537 0.6242 0.6724 0.100 Uiso 1 1 calc R . . H35B H 0.3677 0.5029 0.6505 0.100 Uiso 1 1 calc R . . H35C H 0.3897 0.6006 0.5856 0.100 Uiso 1 1 calc R . . C36 C 0.6904(4) 0.7810(3) 0.9068(2) 0.0317(10) Uani 1 1 d . . . C37 C 0.4874(4) 0.7906(4) 0.8853(3) 0.0375(11) Uani 1 1 d . . . H37 H 0.4743 0.7219 0.9187 0.045 Uiso 1 1 calc R . . C38 C 0.4408(4) 0.8862(4) 0.9313(3) 0.0436(12) Uani 1 1 d . . . H38A H 0.4811 0.8850 0.9765 0.052 Uiso 1 1 calc R . . H38B H 0.4573 0.9546 0.8995 0.052 Uiso 1 1 calc R . . C39 C 0.3095(5) 0.8803(4) 0.9568(3) 0.0592(16) Uani 1 1 d . . . H39A H 0.2935 0.8149 0.9922 0.071 Uiso 1 1 calc R . . H39B H 0.2813 0.9436 0.9841 0.071 Uiso 1 1 calc R . . C40 C 0.2450(5) 0.8774(4) 0.8882(4) 0.0674(18) Uani 1 1 d . . . H40A H 0.1614 0.8696 0.9062 0.081 Uiso 1 1 calc R . . H40B H 0.2543 0.9463 0.8557 0.081 Uiso 1 1 calc R . . C41 C 0.2903(4) 0.7845(4) 0.8411(3) 0.0619(16) Uani 1 1 d . . . H41A H 0.2510 0.7884 0.7953 0.074 Uiso 1 1 calc R . . H41B H 0.2723 0.7152 0.8715 0.074 Uiso 1 1 calc R . . C42 C 0.4217(4) 0.7897(4) 0.8172(3) 0.0473(13) Uani 1 1 d . . . H42A H 0.4496 0.7269 0.7892 0.057 Uiso 1 1 calc R . . H42B H 0.4384 0.8555 0.7823 0.057 Uiso 1 1 calc R . . C43 C 0.7405(4) 0.7197(3) 1.0374(3) 0.0369(11) Uani 1 1 d . . . H43 H 0.8146 0.6881 1.0118 0.044 Uiso 1 1 calc R . . C44 C 0.7673(5) 0.8187(4) 1.0766(3) 0.0528(14) Uani 1 1 d . . . H44A H 0.8071 0.8720 1.0382 0.063 Uiso 1 1 calc R . . H44B H 0.6938 0.8529 1.0994 0.063 Uiso 1 1 calc R . . C45 C 0.8440(5) 0.7862(5) 1.1388(3) 0.0661(16) Uani 1 1 d . . . H45A H 0.8574 0.8504 1.1639 0.079 Uiso 1 1 calc R . . H45B H 0.9201 0.7578 1.1153 0.079 Uiso 1 1 calc R . . C46 C 0.7881(6) 0.7001(5) 1.1989(3) 0.0753(19) Uani 1 1 d . . . H46A H 0.7160 0.7306 1.2264 0.090 Uiso 1 1 calc R . . H46B H 0.8417 0.6775 1.2363 0.090 Uiso 1 1 calc R . . C47 C 0.7603(5) 0.6021(5) 1.1599(3) 0.0618(16) Uani 1 1 d . . . H47A H 0.8335 0.5677 1.1368 0.074 Uiso 1 1 calc R . . H47B H 0.7207 0.5489 1.1985 0.074 Uiso 1 1 calc R . . C48 C 0.6828(4) 0.6347(4) 1.0980(3) 0.0488(13) Uani 1 1 d . . . H48A H 0.6074 0.6643 1.1215 0.059 Uiso 1 1 calc R . . H48B H 0.6682 0.5704 1.0733 0.059 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.03343(15) 0.03236(14) 0.02958(15) -0.00008(10) -0.00936(10) -0.00124(10) Si1 0.0420(8) 0.0424(8) 0.0467(9) 0.0039(6) -0.0174(7) -0.0086(7) Si2 0.0501(9) 0.0390(7) 0.0419(8) 0.0028(6) -0.0212(7) -0.0083(7) N1 0.037(2) 0.0226(18) 0.028(2) -0.0007(15) 0.0001(17) -0.0033(16) N2 0.029(2) 0.0276(19) 0.038(2) 0.0013(16) -0.0126(17) 0.0011(16) N3 0.034(2) 0.038(2) 0.033(2) -0.0002(16) -0.0108(17) -0.0002(17) N4 0.027(2) 0.036(2) 0.037(2) 0.0031(17) -0.0089(17) -0.0015(17) N5 0.031(2) 0.047(2) 0.034(2) 0.0060(18) -0.0020(18) 0.0013(18) C1 0.070(4) 0.036(3) 0.035(3) -0.001(2) -0.013(3) -0.015(3) C2 0.026(2) 0.031(2) 0.024(2) -0.0050(18) -0.0012(19) 0.0008(19) C3 0.027(2) 0.027(2) 0.027(2) 0.0026(18) -0.0077(19) -0.0019(19) C4 0.026(2) 0.028(2) 0.038(3) 0.0010(19) -0.013(2) -0.004(2) C5 0.039(3) 0.034(3) 0.058(3) -0.003(2) -0.017(3) 0.000(2) C6 0.046(3) 0.024(2) 0.028(2) -0.0011(18) -0.010(2) -0.009(2) C7 0.048(3) 0.036(3) 0.028(3) -0.006(2) -0.004(2) -0.012(2) C8 0.065(4) 0.039(3) 0.034(3) -0.002(2) 0.002(3) -0.016(3) C9 0.076(4) 0.035(3) 0.040(3) 0.008(2) -0.006(3) -0.012(3) C10 0.070(4) 0.033(3) 0.043(3) 0.003(2) -0.014(3) 0.001(3) C11 0.051(3) 0.031(2) 0.031(3) 0.004(2) -0.008(2) -0.004(2) C12 0.044(3) 0.047(3) 0.037(3) -0.004(2) 0.008(2) -0.009(3) C13 0.051(4) 0.068(4) 0.062(4) -0.021(3) -0.001(3) -0.002(3) C14 0.060(4) 0.086(4) 0.064(4) -0.015(3) -0.016(3) -0.015(3) C15 0.051(3) 0.029(3) 0.062(4) 0.004(2) -0.006(3) 0.005(2) C16 0.052(4) 0.091(5) 0.087(5) -0.002(4) -0.014(4) 0.006(3) C17 0.066(4) 0.068(4) 0.080(5) -0.020(3) 0.011(3) -0.006(3) C18 0.027(2) 0.024(2) 0.046(3) -0.003(2) -0.016(2) 0.0011(19) C19 0.041(3) 0.028(2) 0.040(3) 0.000(2) -0.017(2) -0.001(2) C20 0.053(3) 0.034(3) 0.057(4) 0.002(2) -0.019(3) -0.008(2) C21 0.065(4) 0.038(3) 0.060(4) -0.015(3) -0.020(3) 0.005(3) C22 0.051(3) 0.047(3) 0.050(3) -0.014(3) -0.011(3) 0.002(3) C23 0.034(3) 0.038(3) 0.042(3) -0.004(2) -0.008(2) -0.003(2) C24 0.049(3) 0.032(2) 0.040(3) 0.005(2) -0.011(2) 0.000(2) C25 0.049(3) 0.062(3) 0.044(3) 0.010(3) -0.012(3) -0.009(3) C26 0.059(4) 0.056(3) 0.043(3) 0.004(2) -0.015(3) -0.010(3) C27 0.039(3) 0.041(3) 0.051(3) -0.004(2) 0.001(2) -0.003(2) C28 0.059(4) 0.076(4) 0.043(3) 0.004(3) -0.003(3) -0.002(3) C29 0.047(4) 0.099(5) 0.109(6) 0.030(4) -0.005(4) -0.012(4) C30 0.063(4) 0.048(3) 0.070(4) 0.001(3) -0.019(3) -0.011(3) C31 0.101(5) 0.068(4) 0.038(3) 0.005(3) -0.025(3) -0.015(3) C32 0.065(4) 0.055(4) 0.109(5) 0.021(3) -0.043(4) -0.005(3) C33 0.053(4) 0.070(4) 0.063(4) 0.025(3) -0.023(3) -0.015(3) C34 0.091(5) 0.044(3) 0.083(5) -0.015(3) -0.009(4) -0.007(3) C35 0.052(4) 0.069(4) 0.082(4) 0.015(3) -0.034(3) -0.017(3) C36 0.034(3) 0.028(2) 0.032(3) -0.0003(19) -0.003(2) -0.001(2) C37 0.032(3) 0.042(3) 0.036(3) 0.006(2) -0.004(2) 0.001(2) C38 0.039(3) 0.047(3) 0.043(3) -0.005(2) -0.002(2) 0.006(2) C39 0.044(3) 0.051(3) 0.072(4) 0.008(3) 0.010(3) 0.014(3) C40 0.031(3) 0.064(4) 0.100(5) 0.010(3) 0.002(3) 0.006(3) C41 0.031(3) 0.065(4) 0.088(5) 0.009(3) -0.012(3) -0.008(3) C42 0.035(3) 0.057(3) 0.049(3) -0.001(2) -0.007(2) -0.004(3) C43 0.035(3) 0.043(3) 0.031(3) 0.001(2) -0.004(2) 0.001(2) C44 0.066(4) 0.052(3) 0.042(3) -0.010(2) -0.012(3) 0.006(3) C45 0.079(4) 0.073(4) 0.051(4) -0.015(3) -0.021(3) 0.006(3) C46 0.075(5) 0.115(5) 0.034(3) -0.002(3) -0.017(3) 0.021(4) C47 0.061(4) 0.078(4) 0.040(3) 0.018(3) -0.007(3) 0.008(3) C48 0.048(3) 0.054(3) 0.040(3) 0.014(2) -0.007(3) 0.005(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 Sm1 N2 2.251(3) . ? Sm1 N3 2.308(4) . ? Sm1 N4 2.364(3) . ? Sm1 N1 2.387(3) . ? Sm1 Si2 3.4266(14) . ? Si1 N3 1.716(3) . ? Si1 C35 1.860(5) . ? Si1 C34 1.860(5) . ? Si1 C33 1.880(5) . ? Si2 N3 1.703(4) . ? Si2 C31 1.856(5) . ? Si2 C32 1.870(6) . ? Si2 C30 1.877(5) . ? N1 C2 1.338(5) . ? N1 C6 1.451(5) . ? N2 C4 1.384(5) . ? N2 C18 1.441(5) . ? N4 C36 1.335(5) . ? N4 C37 1.478(5) . ? N5 C36 1.328(5) . ? N5 C43 1.459(6) . ? N5 H5 0.8700 . ? C1 C2 1.398(5) . ? C1 H1A 0.9400 . ? C1 H1B 0.9400 . ? C2 C3 1.538(5) . ? C3 C4 1.533(5) . ? C3 C36 1.543(5) . ? C3 H3 0.9900 . ? C4 C5 1.333(6) . ? C5 H5A 0.9400 . ? C5 H5B 0.9400 . ? C6 C11 1.396(6) . ? C6 C7 1.399(6) . ? C7 C8 1.398(6) . ? C7 C12 1.512(7) . ? C8 C9 1.365(7) . ? C8 H8 0.9400 . ? C9 C10 1.375(7) . ? C9 H9 0.9400 . ? C10 C11 1.391(6) . ? C10 H10 0.9400 . ? C11 C15 1.516(6) . ? C12 C13 1.532(6) . ? C12 C14 1.532(7) . ? C12 H12 0.9900 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 H13C 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 C17 1.532(7) . ? C15 C16 1.538(8) . ? C15 H15 0.9900 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 C23 1.401(6) . ? C18 C19 1.412(6) . ? C19 C20 1.388(6) . ? C19 C24 1.516(6) . ? C20 C21 1.372(6) . ? C20 H20 0.9400 . ? C21 C22 1.378(6) . ? C21 H21 0.9400 . ? C22 C23 1.395(6) . ? C22 H22 0.9400 . ? C23 C27 1.523(6) . ? C24 C26 1.534(7) . ? C24 C25 1.536(6) . ? C24 H24 0.9900 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C25 H25C 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C26 H26C 0.9700 . ? C27 C28 1.519(7) . ? C27 C29 1.520(7) . ? C27 H27 0.9900 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 H28C 0.9700 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C29 H29C 0.9700 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C30 H30C 0.9700 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 H31C 0.9700 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C32 H32C 0.9700 . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C33 H33C 0.9700 . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C34 H34C 0.9700 . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C35 H35C 0.9700 . ? C37 C42 1.515(6) . ? C37 C38 1.535(6) . ? C37 H37 0.9900 . ? C38 C39 1.523(6) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C39 C40 1.516(8) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C40 C41 1.516(7) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C41 C42 1.521(6) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C43 C48 1.530(6) . ? C43 C44 1.535(6) . ? C43 H43 0.9900 . ? C44 C45 1.519(7) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C45 C46 1.525(7) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C46 C47 1.526(7) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C47 C48 1.522(7) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Sm1 N3 120.17(12) . . ? N2 Sm1 N4 85.47(12) . . ? N3 Sm1 N4 128.24(12) . . ? N2 Sm1 N1 88.77(12) . . ? N3 Sm1 N1 139.03(12) . . ? N4 Sm1 N1 78.28(11) . . ? N2 Sm1 Si2 136.57(9) . . ? N3 Sm1 Si2 26.38(9) . . ? N4 Sm1 Si2 134.18(9) . . ? N1 Sm1 Si2 112.77(9) . . ? N3 Si1 C35 112.6(2) . . ? N3 Si1 C34 114.2(2) . . ? C35 Si1 C34 107.3(3) . . ? N3 Si1 C33 108.9(2) . . ? C35 Si1 C33 107.1(3) . . ? C34 Si1 C33 106.2(3) . . ? N3 Si2 C31 115.3(2) . . ? N3 Si2 C32 113.0(2) . . ? C31 Si2 C32 106.8(3) . . ? N3 Si2 C30 106.3(2) . . ? C31 Si2 C30 106.9(3) . . ? C32 Si2 C30 108.1(2) . . ? N3 Si2 Sm1 37.04(12) . . ? C31 Si2 Sm1 135.3(2) . . ? C32 Si2 Sm1 116.4(2) . . ? C30 Si2 Sm1 70.42(17) . . ? C2 N1 C6 117.9(3) . . ? C2 N1 Sm1 113.9(2) . . ? C6 N1 Sm1 127.4(3) . . ? C4 N2 C18 117.5(3) . . ? C4 N2 Sm1 114.7(3) . . ? C18 N2 Sm1 127.3(3) . . ? Si2 N3 Si1 124.4(2) . . ? Si2 N3 Sm1 116.58(17) . . ? Si1 N3 Sm1 119.02(18) . . ? C36 N4 C37 119.0(4) . . ? C36 N4 Sm1 111.2(3) . . ? C37 N4 Sm1 124.5(3) . . ? C36 N5 C43 127.0(4) . . ? C36 N5 H5 116.5 . . ? C43 N5 H5 116.5 . . ? C2 C1 H1A 120.0 . . ? C2 C1 H1B 120.0 . . ? H1A C1 H1B 120.0 . . ? N1 C2 C1 126.3(4) . . ? N1 C2 C3 117.9(3) . . ? C1 C2 C3 115.9(4) . . ? C4 C3 C2 114.9(3) . . ? C4 C3 C36 113.1(3) . . ? C2 C3 C36 112.7(3) . . ? C4 C3 H3 105.0 . . ? C2 C3 H3 105.0 . . ? C36 C3 H3 105.0 . . ? C5 C4 N2 126.7(4) . . ? C5 C4 C3 117.9(4) . . ? N2 C4 C3 115.5(4) . . ? C4 C5 H5A 120.0 . . ? C4 C5 H5B 120.0 . . ? H5A C5 H5B 120.0 . . ? C11 C6 C7 120.9(4) . . ? C11 C6 N1 119.1(4) . . ? C7 C6 N1 119.8(4) . . ? C8 C7 C6 118.0(5) . . ? C8 C7 C12 119.3(4) . . ? C6 C7 C12 122.7(4) . . ? C9 C8 C7 121.4(5) . . ? C9 C8 H8 119.3 . . ? C7 C8 H8 119.3 . . ? C8 C9 C10 120.0(5) . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? C9 C10 C11 121.0(5) . . ? C9 C10 H10 119.5 . . ? C11 C10 H10 119.5 . . ? C10 C11 C6 118.6(4) . . ? C10 C11 C15 119.2(4) . . ? C6 C11 C15 122.2(4) . . ? C7 C12 C13 111.0(4) . . ? C7 C12 C14 112.5(4) . . ? C13 C12 C14 109.9(4) . . ? C7 C12 H12 107.7 . . ? C13 C12 H12 107.7 . . ? C14 C12 H12 107.7 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 C17 110.5(4) . . ? C11 C15 C16 114.2(4) . . ? C17 C15 C16 109.8(5) . . ? C11 C15 H15 107.3 . . ? C17 C15 H15 107.3 . . ? C16 C15 H15 107.3 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C23 C18 C19 120.3(4) . . ? C23 C18 N2 119.7(4) . . ? C19 C18 N2 119.8(4) . . ? C20 C19 C18 118.1(4) . . ? C20 C19 C24 119.0(4) . . ? C18 C19 C24 122.9(4) . . ? C21 C20 C19 122.0(4) . . ? C21 C20 H20 119.0 . . ? C19 C20 H20 119.0 . . ? C20 C21 C22 119.4(5) . . ? C20 C21 H21 120.3 . . ? C22 C21 H21 120.3 . . ? C21 C22 C23 121.2(5) . . ? C21 C22 H22 119.4 . . ? C23 C22 H22 119.4 . . ? C22 C23 C18 118.7(4) . . ? C22 C23 C27 119.2(4) . . ? C18 C23 C27 122.0(4) . . ? C19 C24 C26 110.8(4) . . ? C19 C24 C25 112.2(4) . . ? C26 C24 C25 110.7(4) . . ? C19 C24 H24 107.7 . . ? C26 C24 H24 107.7 . . ? C25 C24 H24 107.7 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C29 109.7(4) . . ? C28 C27 C23 113.8(4) . . ? C29 C27 C23 109.8(4) . . ? C28 C27 H27 107.7 . . ? C29 C27 H27 107.7 . . ? C23 C27 H27 107.7 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? Si2 C30 H30A 109.5 . . ? Si2 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si2 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? Si2 C31 H31A 109.5 . . ? Si2 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si2 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Si2 C32 H32A 109.5 . . ? Si2 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si2 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Si1 C33 H33A 109.5 . . ? Si1 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Si1 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? Si1 C34 H34A 109.5 . . ? Si1 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? Si1 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? Si1 C35 H35A 109.5 . . ? Si1 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? Si1 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N5 C36 N4 123.7(4) . . ? N5 C36 C3 119.0(4) . . ? N4 C36 C3 117.3(4) . . ? N4 C37 C42 108.5(4) . . ? N4 C37 C38 112.1(4) . . ? C42 C37 C38 109.4(4) . . ? N4 C37 H37 108.9 . . ? C42 C37 H37 108.9 . . ? C38 C37 H37 108.9 . . ? C39 C38 C37 111.0(4) . . ? C39 C38 H38A 109.4 . . ? C37 C38 H38A 109.4 . . ? C39 C38 H38B 109.4 . . ? C37 C38 H38B 109.4 . . ? H38A C38 H38B 108.0 . . ? C40 C39 C38 110.7(4) . . ? C40 C39 H39A 109.5 . . ? C38 C39 H39A 109.5 . . ? C40 C39 H39B 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 108.1 . . ? C41 C40 C39 111.7(5) . . ? C41 C40 H40A 109.3 . . ? C39 C40 H40A 109.3 . . ? C41 C40 H40B 109.3 . . ? C39 C40 H40B 109.3 . . ? H40A C40 H40B 107.9 . . ? C40 C41 C42 110.6(4) . . ? C40 C41 H41A 109.5 . . ? C42 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? C42 C41 H41B 109.5 . . ? H41A C41 H41B 108.1 . . ? C37 C42 C41 112.3(4) . . ? C37 C42 H42A 109.2 . . ? C41 C42 H42A 109.2 . . ? C37 C42 H42B 109.2 . . ? C41 C42 H42B 109.2 . . ? H42A C42 H42B 107.9 . . ? N5 C43 C48 108.1(4) . . ? N5 C43 C44 111.9(4) . . ? C48 C43 C44 109.3(4) . . ? N5 C43 H43 109.1 . . ? C48 C43 H43 109.1 . . ? C44 C43 H43 109.1 . . ? C45 C44 C43 111.2(4) . . ? C45 C44 H44A 109.4 . . ? C43 C44 H44A 109.4 . . ? C45 C44 H44B 109.4 . . ? C43 C44 H44B 109.4 . . ? H44A C44 H44B 108.0 . . ? C44 C45 C46 111.7(5) . . ? C44 C45 H45A 109.3 . . ? C46 C45 H45A 109.3 . . ? C44 C45 H45B 109.3 . . ? C46 C45 H45B 109.3 . . ? H45A C45 H45B 108.0 . . ? C45 C46 C47 109.8(5) . . ? C45 C46 H46A 109.7 . . ? C47 C46 H46A 109.7 . . ? C45 C46 H46B 109.7 . . ? C47 C46 H46B 109.7 . . ? H46A C46 H46B 108.2 . . ? C48 C47 C46 111.5(5) . . ? C48 C47 H47A 109.3 . . ? C46 C47 H47A 109.3 . . ? C48 C47 H47B 109.3 . . ? C46 C47 H47B 109.3 . . ? H47A C47 H47B 108.0 . . ? C47 C48 C43 110.9(4) . . ? C47 C48 H48A 109.4 . . ? C43 C48 H48A 109.4 . . ? C47 C48 H48B 109.4 . . ? C43 C48 H48B 109.4 . . ? H48A C48 H48B 108.0 . . ? 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 Sm1 Si2 N3 61.0(2) . . . . ? N4 Sm1 Si2 N3 -89.0(2) . . . . ? N1 Sm1 Si2 N3 175.2(2) . . . . ? N2 Sm1 Si2 C31 -9.6(3) . . . . ? N3 Sm1 Si2 C31 -70.6(3) . . . . ? N4 Sm1 Si2 C31 -159.7(3) . . . . ? N1 Sm1 Si2 C31 104.5(3) . . . . ? N2 Sm1 Si2 C32 154.8(2) . . . . ? N3 Sm1 Si2 C32 93.8(3) . . . . ? N4 Sm1 Si2 C32 4.8(2) . . . . ? N1 Sm1 Si2 C32 -91.0(2) . . . . ? N2 Sm1 Si2 C30 -104.1(2) . . . . ? N3 Sm1 Si2 C30 -165.2(3) . . . . ? N4 Sm1 Si2 C30 105.8(2) . . . . ? N1 Sm1 Si2 C30 10.0(2) . . . . ? N2 Sm1 N1 C2 -43.2(3) . . . . ? N3 Sm1 N1 C2 178.9(3) . . . . ? N4 Sm1 N1 C2 42.4(3) . . . . ? Si2 Sm1 N1 C2 175.6(2) . . . . ? N2 Sm1 N1 C6 147.9(3) . . . . ? N3 Sm1 N1 C6 10.0(4) . . . . ? N4 Sm1 N1 C6 -126.5(3) . . . . ? Si2 Sm1 N1 C6 6.7(3) . . . . ? N3 Sm1 N2 C4 172.4(3) . . . . ? N4 Sm1 N2 C4 -55.4(3) . . . . ? N1 Sm1 N2 C4 22.9(3) . . . . ? Si2 Sm1 N2 C4 145.6(2) . . . . ? N3 Sm1 N2 C18 1.0(4) . . . . ? N4 Sm1 N2 C18 133.3(3) . . . . ? N1 Sm1 N2 C18 -148.4(3) . . . . ? Si2 Sm1 N2 C18 -25.7(4) . . . . ? C31 Si2 N3 Si1 -48.9(4) . . . . ? C32 Si2 N3 Si1 74.4(3) . . . . ? C30 Si2 N3 Si1 -167.1(3) . . . . ? Sm1 Si2 N3 Si1 178.3(4) . . . . ? C31 Si2 N3 Sm1 132.8(3) . . . . ? C32 Si2 N3 Sm1 -103.9(3) . . . . ? C30 Si2 N3 Sm1 14.6(3) . . . . ? C35 Si1 N3 Si2 -54.0(3) . . . . ? C34 Si1 N3 Si2 68.8(3) . . . . ? C33 Si1 N3 Si2 -172.6(3) . . . . ? C35 Si1 N3 Sm1 124.3(3) . . . . ? C34 Si1 N3 Sm1 -112.9(3) . . . . ? C33 Si1 N3 Sm1 5.6(3) . . . . ? N2 Sm1 N3 Si2 -135.92(19) . . . . ? N4 Sm1 N3 Si2 114.1(2) . . . . ? N1 Sm1 N3 Si2 -6.8(3) . . . . ? N2 Sm1 N3 Si1 45.7(2) . . . . ? N4 Sm1 N3 Si1 -64.3(2) . . . . ? N1 Sm1 N3 Si1 174.82(16) . . . . ? Si2 Sm1 N3 Si1 -178.4(4) . . . . ? N2 Sm1 N4 C36 25.1(3) . . . . ? N3 Sm1 N4 C36 150.5(3) . . . . ? N1 Sm1 N4 C36 -64.6(3) . . . . ? Si2 Sm1 N4 C36 -175.0(2) . . . . ? N2 Sm1 N4 C37 -128.8(3) . . . . ? N3 Sm1 N4 C37 -3.4(4) . . . . ? N1 Sm1 N4 C37 141.5(3) . . . . ? Si2 Sm1 N4 C37 31.0(3) . . . . ? C6 N1 C2 C1 -0.4(6) . . . . ? Sm1 N1 C2 C1 -170.4(4) . . . . ? C6 N1 C2 C3 -179.7(3) . . . . ? Sm1 N1 C2 C3 10.3(4) . . . . ? N1 C2 C3 C4 57.8(5) . . . . ? C1 C2 C3 C4 -121.6(4) . . . . ? N1 C2 C3 C36 -73.7(5) . . . . ? C1 C2 C3 C36 106.9(4) . . . . ? C18 N2 C4 C5 17.2(6) . . . . ? Sm1 N2 C4 C5 -155.0(4) . . . . ? C18 N2 C4 C3 -161.9(3) . . . . ? Sm1 N2 C4 C3 25.9(4) . . . . ? C2 C3 C4 C5 96.9(5) . . . . ? C36 C3 C4 C5 -131.8(4) . . . . ? C2 C3 C4 N2 -84.0(4) . . . . ? C36 C3 C4 N2 47.3(5) . . . . ? C2 N1 C6 C11 -98.0(5) . . . . ? Sm1 N1 C6 C11 70.4(5) . . . . ? C2 N1 C6 C7 86.3(5) . . . . ? Sm1 N1 C6 C7 -105.2(4) . . . . ? C11 C6 C7 C8 -3.0(6) . . . . ? N1 C6 C7 C8 172.5(4) . . . . ? C11 C6 C7 C12 176.4(4) . . . . ? N1 C6 C7 C12 -8.1(6) . . . . ? C6 C7 C8 C9 -0.1(7) . . . . ? C12 C7 C8 C9 -179.6(4) . . . . ? C7 C8 C9 C10 2.6(7) . . . . ? C8 C9 C10 C11 -2.0(7) . . . . ? C9 C10 C11 C6 -1.1(7) . . . . ? C9 C10 C11 C15 176.6(4) . . . . ? C7 C6 C11 C10 3.6(6) . . . . ? N1 C6 C11 C10 -172.0(4) . . . . ? C7 C6 C11 C15 -174.0(4) . . . . ? N1 C6 C11 C15 10.5(6) . . . . ? C8 C7 C12 C13 -65.0(5) . . . . ? C6 C7 C12 C13 115.6(5) . . . . ? C8 C7 C12 C14 58.7(6) . . . . ? C6 C7 C12 C14 -120.8(5) . . . . ? C10 C11 C15 C17 -77.1(6) . . . . ? C6 C11 C15 C17 100.5(5) . . . . ? C10 C11 C15 C16 47.3(6) . . . . ? C6 C11 C15 C16 -135.1(5) . . . . ? C4 N2 C18 C23 -109.8(5) . . . . ? Sm1 N2 C18 C23 61.4(5) . . . . ? C4 N2 C18 C19 75.1(5) . . . . ? Sm1 N2 C18 C19 -113.8(4) . . . . ? C23 C18 C19 C20 -2.7(6) . . . . ? N2 C18 C19 C20 172.5(4) . . . . ? C23 C18 C19 C24 175.8(4) . . . . ? N2 C18 C19 C24 -9.1(6) . . . . ? C18 C19 C20 C21 -0.1(7) . . . . ? C24 C19 C20 C21 -178.6(5) . . . . ? C19 C20 C21 C22 1.9(8) . . . . ? C20 C21 C22 C23 -1.0(8) . . . . ? C21 C22 C23 C18 -1.8(7) . . . . ? C21 C22 C23 C27 174.3(5) . . . . ? C19 C18 C23 C22 3.6(7) . . . . ? N2 C18 C23 C22 -171.5(4) . . . . ? C19 C18 C23 C27 -172.3(4) . . . . ? N2 C18 C23 C27 12.5(7) . . . . ? C20 C19 C24 C26 61.2(5) . . . . ? C18 C19 C24 C26 -117.3(5) . . . . ? C20 C19 C24 C25 -63.1(6) . . . . ? C18 C19 C24 C25 118.5(5) . . . . ? C22 C23 C27 C28 62.8(6) . . . . ? C18 C23 C27 C28 -121.3(5) . . . . ? C22 C23 C27 C29 -60.7(6) . . . . ? C18 C23 C27 C29 115.2(5) . . . . ? C43 N5 C36 N4 174.2(4) . . . . ? C43 N5 C36 C3 -4.4(6) . . . . ? C37 N4 C36 N5 7.0(6) . . . . ? Sm1 N4 C36 N5 -148.6(3) . . . . ? C37 N4 C36 C3 -174.3(3) . . . . ? Sm1 N4 C36 C3 30.1(4) . . . . ? C4 C3 C36 N5 93.0(4) . . . . ? C2 C3 C36 N5 -134.6(4) . . . . ? C4 C3 C36 N4 -85.7(4) . . . . ? C2 C3 C36 N4 46.7(5) . . . . ? C36 N4 C37 C42 -169.0(4) . . . . ? Sm1 N4 C37 C42 -16.9(5) . . . . ? C36 N4 C37 C38 70.0(5) . . . . ? Sm1 N4 C37 C38 -137.9(3) . . . . ? N4 C37 C38 C39 177.3(4) . . . . ? C42 C37 C38 C39 56.8(5) . . . . ? C37 C38 C39 C40 -56.8(5) . . . . ? C38 C39 C40 C41 55.9(6) . . . . ? C39 C40 C41 C42 -54.9(6) . . . . ? N4 C37 C42 C41 -179.2(4) . . . . ? C38 C37 C42 C41 -56.6(5) . . . . ? C40 C41 C42 C37 55.9(6) . . . . ? C36 N5 C43 C48 -150.4(4) . . . . ? C36 N5 C43 C44 89.2(5) . . . . ? N5 C43 C44 C45 176.6(4) . . . . ? C48 C43 C44 C45 56.8(6) . . . . ? C43 C44 C45 C46 -57.1(6) . . . . ? C44 C45 C46 C47 55.7(6) . . . . ? C45 C46 C47 C48 -56.1(6) . . . . ? C46 C47 C48 C43 57.8(6) . . . . ? N5 C43 C48 C47 -179.2(4) . . . . ? C44 C43 C48 C47 -57.1(6) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.479 _refine_diff_density_min -0.690 _refine_diff_density_rms 0.091 _database_code_depnum_ccdc_archive 'CCDC 976986' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_complex2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H80 N5 Si2 Yb, 0.5(C6 H14)' _chemical_formula_sum 'C51 H87 N5 Si2 Yb' _chemical_formula_weight 999.48 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' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.4354(3) _cell_length_b 12.4814(3) _cell_length_c 19.2857(5) _cell_angle_alpha 99.150(2) _cell_angle_beta 101.425(2) _cell_angle_gamma 92.695(2) _cell_volume 2654.97(13) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 12511 _cell_measurement_theta_min 3.1490 _cell_measurement_theta_max 29.4346 _exptl_crystal_description chip _exptl_crystal_colour red _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.250 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1052 _exptl_absorpt_coefficient_mu 1.842 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.25144 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.4692 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25731 _diffrn_reflns_av_R_equivalents 0.0625 _diffrn_reflns_av_sigmaI/netI 0.0603 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 25.50 _reflns_number_total 9854 _reflns_number_gt 9090 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro, Agilent Technologies' _computing_cell_refinement 'CrysAlisPro, Agilent Technologies' _computing_data_reduction 'CrysAlisPro, Agilent Technologies' _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.Due to the disorder of the free hexane molecular, four restraints were done(C52 C53, C51 C52, C50 C51 C53, C49 C50). The restraint of N4-H4 was also done. ; _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^)+(0.0418P)^2^+2.2078P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9854 _refine_ls_number_parameters 494 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0416 _refine_ls_R_factor_gt 0.0374 _refine_ls_wR_factor_ref 0.0904 _refine_ls_wR_factor_gt 0.0878 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.043 _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 Yb1 Yb 0.729661(12) 0.831188(11) 0.744614(7) 0.02086(7) Uani 1 1 d . . . Si1 Si 0.57611(11) 1.04151(10) 0.80774(7) 0.0393(3) Uani 1 1 d . . . Si2 Si 0.64303(10) 0.87565(9) 0.90143(6) 0.0320(2) Uani 1 1 d . . . N1 N 0.8401(3) 0.9244(2) 0.69119(15) 0.0228(6) Uani 1 1 d . . . N2 N 0.8316(2) 0.6852(2) 0.73759(15) 0.0210(6) Uani 1 1 d . . . N3 N 0.6261(2) 0.7489(2) 0.63167(15) 0.0229(6) Uani 1 1 d . . . N4 N 0.6684(3) 0.7493(3) 0.51801(16) 0.0291(7) Uani 1 1 d D . . H4 H 0.5948(14) 0.752(3) 0.4988(19) 0.031(11) Uiso 1 1 d D . . N5 N 0.6441(3) 0.9261(2) 0.82365(16) 0.0275(7) Uani 1 1 d . . . C1 C 0.9983(3) 0.8807(3) 0.6254(2) 0.0311(9) Uani 1 1 d . . . H1A H 1.0377 0.9509 0.6404 0.037 Uiso 1 1 calc R . . H1B H 1.0296 0.8279 0.5953 0.037 Uiso 1 1 calc R . . C2 C 0.8975(3) 0.8561(3) 0.64705(18) 0.0216(7) Uani 1 1 d . . . C3 C 0.8348(3) 0.7412(3) 0.61904(18) 0.0207(7) Uani 1 1 d . . . H3 H 0.8690 0.7123 0.5772 0.025 Uiso 1 1 calc R . . C4 C 0.8575(3) 0.6568(3) 0.66996(19) 0.0237(8) Uani 1 1 d . . . C5 C 0.9006(4) 0.5643(3) 0.6444(2) 0.0336(9) Uani 1 1 d . . . H5A H 0.9163 0.5105 0.6733 0.040 Uiso 1 1 calc R . . H5B H 0.9151 0.5530 0.5976 0.040 Uiso 1 1 calc R . . C6 C 0.8758(3) 1.0378(3) 0.70535(19) 0.0235(7) Uani 1 1 d . . . C7 C 0.9379(3) 1.0876(3) 0.7746(2) 0.0293(8) Uani 1 1 d . . . C8 C 0.9606(4) 1.2001(3) 0.7897(2) 0.0399(10) Uani 1 1 d . . . H8 H 1.0000 1.2335 0.8361 0.048 Uiso 1 1 calc R . . C9 C 0.9263(4) 1.2642(3) 0.7379(2) 0.0427(11) Uani 1 1 d . . . H9 H 0.9417 1.3403 0.7491 0.051 Uiso 1 1 calc R . . C10 C 0.8695(4) 1.2148(3) 0.6696(2) 0.0340(9) Uani 1 1 d . . . H10 H 0.8478 1.2580 0.6341 0.041 Uiso 1 1 calc R . . C11 C 0.8434(3) 1.1027(3) 0.65203(19) 0.0260(8) Uani 1 1 d . . . C12 C 0.9877(5) 1.0197(5) 0.8306(3) 0.0581(8) Uani 1 1 d . . . H12 H 0.9402 0.9484 0.8180 0.070 Uiso 1 1 calc R . . C13 C 1.1152(4) 0.9987(5) 0.8254(3) 0.0581(8) Uani 1 1 d . . . H13A H 1.1162 0.9592 0.7780 0.087 Uiso 1 1 calc R . . H13B H 1.1482 0.9559 0.8613 0.087 Uiso 1 1 calc R . . H13C H 1.1630 1.0675 0.8336 0.087 Uiso 1 1 calc R . . C14 C 0.9809(5) 1.0672(5) 0.9068(2) 0.0581(8) Uani 1 1 d . . . H14A H 1.0314 1.1348 0.9222 0.087 Uiso 1 1 calc R . . H14B H 1.0080 1.0160 0.9383 0.087 Uiso 1 1 calc R . . H14C H 0.8988 1.0812 0.9088 0.087 Uiso 1 1 calc R . . C15 C 0.7820(4) 1.0546(4) 0.5750(2) 0.0383(6) Uani 1 1 d . . . H15 H 0.7713 0.9746 0.5714 0.046 Uiso 1 1 calc R . . C16 C 0.8607(4) 1.0787(4) 0.5233(2) 0.0383(6) Uani 1 1 d . . . H16A H 0.8736 1.1569 0.5264 0.057 Uiso 1 1 calc R . . H16B H 0.8215 1.0462 0.4746 0.057 Uiso 1 1 calc R . . H16C H 0.9371 1.0485 0.5358 0.057 Uiso 1 1 calc R . . C17 C 0.6581(4) 1.0959(3) 0.5525(2) 0.0383(6) Uani 1 1 d . . . H17A H 0.6045 1.0707 0.5808 0.057 Uiso 1 1 calc R . . H17B H 0.6264 1.0683 0.5020 0.057 Uiso 1 1 calc R . . H17C H 0.6652 1.1749 0.5605 0.057 Uiso 1 1 calc R . . C18 C 0.8520(3) 0.6049(3) 0.78376(18) 0.0245(8) Uani 1 1 d . . . C19 C 0.7585(4) 0.5261(3) 0.7825(2) 0.0316(9) Uani 1 1 d . . . C20 C 0.7751(4) 0.4565(3) 0.8331(2) 0.0443(11) Uani 1 1 d . . . H20 H 0.7125 0.4052 0.8334 0.053 Uiso 1 1 calc R . . C21 C 0.8801(5) 0.4612(4) 0.8819(2) 0.0481(12) Uani 1 1 d . . . H21 H 0.8894 0.4140 0.9157 0.058 Uiso 1 1 calc R . . C22 C 0.9718(5) 0.5353(3) 0.8813(2) 0.0442(11) Uani 1 1 d . . . H22 H 1.0446 0.5369 0.9143 0.053 Uiso 1 1 calc R . . C23 C 0.9606(4) 0.6088(3) 0.8330(2) 0.0355(9) Uani 1 1 d . . . C24 C 0.6397(4) 0.5141(4) 0.7281(3) 0.0525(7) Uani 1 1 d . . . H24 H 0.6379 0.5775 0.7031 0.063 Uiso 1 1 calc R . . C25 C 0.6298(4) 0.4121(4) 0.6715(3) 0.0525(7) Uani 1 1 d . . . H25A H 0.6948 0.4159 0.6462 0.079 Uiso 1 1 calc R . . H25B H 0.5538 0.4071 0.6377 0.079 Uiso 1 1 calc R . . H25C H 0.6344 0.3484 0.6946 0.079 Uiso 1 1 calc R . . C26 C 0.5320(4) 0.5148(4) 0.7634(3) 0.0525(7) Uani 1 1 d . . . H26A H 0.5276 0.4503 0.7852 0.079 Uiso 1 1 calc R . . H26B H 0.4596 0.5152 0.7274 0.079 Uiso 1 1 calc R . . H26C H 0.5401 0.5793 0.8000 0.079 Uiso 1 1 calc R . . C27 C 1.0648(5) 0.6890(5) 0.8347(3) 0.0688(9) Uani 1 1 d . . . H27 H 1.0338 0.7471 0.8084 0.083 Uiso 1 1 calc R . . C28 C 1.1584(5) 0.6347(5) 0.7972(3) 0.0688(9) Uani 1 1 d . . . H28A H 1.1893 0.5765 0.8217 0.103 Uiso 1 1 calc R . . H28B H 1.2235 0.6882 0.7985 0.103 Uiso 1 1 calc R . . H28C H 1.1216 0.6049 0.7477 0.103 Uiso 1 1 calc R . . C29 C 1.1257(5) 0.7425(5) 0.9112(3) 0.0688(9) Uani 1 1 d . . . H29A H 1.0665 0.7756 0.9356 0.103 Uiso 1 1 calc R . . H29B H 1.1868 0.7980 0.9094 0.103 Uiso 1 1 calc R . . H29C H 1.1622 0.6878 0.9370 0.103 Uiso 1 1 calc R . . C30 C 0.7001(3) 0.7459(3) 0.58845(18) 0.0232(7) Uani 1 1 d . . . C31 C 0.4952(3) 0.7433(3) 0.60343(19) 0.0268(8) Uani 1 1 d . . . H31 H 0.4782 0.7995 0.5727 0.032 Uiso 1 1 calc R . . C32 C 0.4462(4) 0.6320(3) 0.5589(2) 0.0355(9) Uani 1 1 d . . . H32A H 0.4650 0.5753 0.5882 0.043 Uiso 1 1 calc R . . H32B H 0.4846 0.6174 0.5176 0.043 Uiso 1 1 calc R . . C33 C 0.3099(4) 0.6287(4) 0.5324(2) 0.0458(11) Uani 1 1 d . . . H33A H 0.2918 0.6809 0.4996 0.055 Uiso 1 1 calc R . . H33B H 0.2798 0.5559 0.5058 0.055 Uiso 1 1 calc R . . C34 C 0.2468(4) 0.6560(4) 0.5944(3) 0.0526(12) Uani 1 1 d . . . H34A H 0.2568 0.5990 0.6242 0.063 Uiso 1 1 calc R . . H34B H 0.1609 0.6581 0.5755 0.063 Uiso 1 1 calc R . . C35 C 0.2963(4) 0.7651(4) 0.6404(3) 0.0464(11) Uani 1 1 d . . . H35A H 0.2587 0.7779 0.6821 0.056 Uiso 1 1 calc R . . H35B H 0.2774 0.8234 0.6124 0.056 Uiso 1 1 calc R . . C36 C 0.4322(3) 0.7672(4) 0.6658(2) 0.0364(9) Uani 1 1 d . . . H36A H 0.4628 0.8390 0.6939 0.044 Uiso 1 1 calc R . . H36B H 0.4503 0.7130 0.6972 0.044 Uiso 1 1 calc R . . C37 C 0.7440(3) 0.7577(3) 0.46589(19) 0.0287(8) Uani 1 1 d . . . H37 H 0.8206 0.7992 0.4911 0.034 Uiso 1 1 calc R . . C38 C 0.6808(4) 0.8203(4) 0.4096(2) 0.0405(10) Uani 1 1 d . . . H38A H 0.6679 0.8931 0.4330 0.049 Uiso 1 1 calc R . . H38B H 0.6025 0.7824 0.3865 0.049 Uiso 1 1 calc R . . C39 C 0.7550(5) 0.8303(5) 0.3530(2) 0.0552(13) Uani 1 1 d . . . H39A H 0.7113 0.8684 0.3165 0.066 Uiso 1 1 calc R . . H39B H 0.8305 0.8735 0.3756 0.066 Uiso 1 1 calc R . . C40 C 0.7811(5) 0.7196(5) 0.3174(2) 0.0646(16) Uani 1 1 d . . . H40A H 0.8322 0.7286 0.2832 0.078 Uiso 1 1 calc R . . H40B H 0.7060 0.6789 0.2907 0.078 Uiso 1 1 calc R . . C41 C 0.8433(5) 0.6556(4) 0.3730(3) 0.0602(14) Uani 1 1 d . . . H41A H 0.9225 0.6922 0.3958 0.072 Uiso 1 1 calc R . . H41B H 0.8548 0.5827 0.3490 0.072 Uiso 1 1 calc R . . C42 C 0.7708(4) 0.6457(3) 0.4303(2) 0.0402(10) Uani 1 1 d . . . H42A H 0.8156 0.6083 0.4668 0.048 Uiso 1 1 calc R . . H42B H 0.6954 0.6018 0.4084 0.048 Uiso 1 1 calc R . . C43 C 0.5677(5) 1.0566(5) 0.7122(3) 0.0665(16) Uani 1 1 d . . . H43A H 0.6434 1.0410 0.6990 0.100 Uiso 1 1 calc R . . H43B H 0.5508 1.1304 0.7065 0.100 Uiso 1 1 calc R . . H43C H 0.5044 1.0060 0.6815 0.100 Uiso 1 1 calc R . . C44 C 0.4196(5) 1.0387(5) 0.8227(3) 0.0628(15) Uani 1 1 d . . . H44A H 0.3738 0.9739 0.7937 0.094 Uiso 1 1 calc R . . H44B H 0.3830 1.1028 0.8090 0.094 Uiso 1 1 calc R . . H44C H 0.4208 1.0378 0.8730 0.094 Uiso 1 1 calc R . . C45 C 0.6579(6) 1.1701(4) 0.8630(4) 0.0777(19) Uani 1 1 d . . . H45A H 0.6656 1.1667 0.9135 0.117 Uiso 1 1 calc R . . H45B H 0.6137 1.2317 0.8516 0.117 Uiso 1 1 calc R . . H45C H 0.7369 1.1786 0.8523 0.117 Uiso 1 1 calc R . . C46 C 0.7652(5) 0.7809(4) 0.9119(3) 0.0586(14) Uani 1 1 d . . . H46A H 0.7465 0.7187 0.8733 0.088 Uiso 1 1 calc R . . H46B H 0.7720 0.7561 0.9577 0.088 Uiso 1 1 calc R . . H46C H 0.8404 0.8187 0.9103 0.088 Uiso 1 1 calc R . . C47 C 0.4980(5) 0.7986(4) 0.8995(3) 0.0585(14) Uani 1 1 d . . . H47A H 0.4355 0.8485 0.8999 0.088 Uiso 1 1 calc R . . H47B H 0.5056 0.7634 0.9414 0.088 Uiso 1 1 calc R . . H47C H 0.4775 0.7440 0.8564 0.088 Uiso 1 1 calc R . . C48 C 0.6731(5) 0.9813(4) 0.9838(2) 0.0501(12) Uani 1 1 d . . . H48A H 0.7502 1.0206 0.9883 0.075 Uiso 1 1 calc R . . H48B H 0.6739 0.9467 1.0255 0.075 Uiso 1 1 calc R . . H48C H 0.6110 1.0317 0.9806 0.075 Uiso 1 1 calc R . . C49 C 0.301(2) 0.352(2) -0.0941(16) 0.158(4) Uiso 0.50 1 d PD . . C50 C 0.339(2) 0.432(2) -0.0262(13) 0.158(4) Uiso 0.50 1 d PD . . C51 C 0.461(2) 0.443(3) -0.0405(15) 0.158(4) Uiso 0.50 1 d PD . . C52 C 0.525(2) 0.535(3) 0.0184(17) 0.158(4) Uiso 0.50 1 d PD . . C53 C 0.658(2) 0.543(2) 0.0581(13) 0.158(4) Uiso 0.50 1 d PD . . C54 C 0.743(2) 0.642(2) 0.0948(17) 0.158(4) Uiso 0.50 1 d PD . . 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 Yb1 0.02197(10) 0.02320(10) 0.02008(10) 0.00606(6) 0.00826(7) 0.00443(6) Si1 0.0374(7) 0.0452(7) 0.0456(7) 0.0171(5) 0.0232(6) 0.0152(5) Si2 0.0385(6) 0.0350(6) 0.0259(5) 0.0037(4) 0.0154(5) 0.0052(5) N1 0.0240(15) 0.0207(15) 0.0268(15) 0.0064(12) 0.0113(13) 0.0003(12) N2 0.0188(14) 0.0239(15) 0.0208(15) 0.0034(11) 0.0057(12) 0.0018(11) N3 0.0179(15) 0.0304(16) 0.0223(15) 0.0082(12) 0.0057(12) 0.0021(12) N4 0.0229(17) 0.0452(19) 0.0202(16) 0.0106(13) 0.0030(13) 0.0012(14) N5 0.0285(16) 0.0289(17) 0.0279(16) 0.0047(13) 0.0128(13) 0.0019(13) C1 0.026(2) 0.031(2) 0.041(2) 0.0103(17) 0.0140(17) 0.0028(16) C2 0.0208(17) 0.0268(18) 0.0193(17) 0.0090(14) 0.0044(14) 0.0054(14) C3 0.0201(17) 0.0267(18) 0.0179(16) 0.0054(13) 0.0082(14) 0.0038(14) C4 0.0201(17) 0.0242(18) 0.0263(18) 0.0051(14) 0.0033(15) -0.0003(14) C5 0.048(2) 0.032(2) 0.0241(19) 0.0073(16) 0.0113(18) 0.0109(18) C6 0.0192(17) 0.0267(19) 0.0278(18) 0.0069(14) 0.0095(15) 0.0057(14) C7 0.0228(19) 0.035(2) 0.031(2) 0.0064(16) 0.0097(16) -0.0026(16) C8 0.038(2) 0.043(2) 0.036(2) -0.0025(19) 0.0095(19) -0.0067(19) C9 0.052(3) 0.025(2) 0.051(3) -0.0009(19) 0.018(2) -0.0031(19) C10 0.040(2) 0.028(2) 0.041(2) 0.0144(17) 0.0170(19) 0.0065(17) C11 0.0239(19) 0.030(2) 0.0290(19) 0.0093(15) 0.0132(15) 0.0081(15) C12 0.0515(17) 0.085(2) 0.0399(15) 0.0214(14) 0.0043(14) 0.0111(15) C13 0.0515(17) 0.085(2) 0.0399(15) 0.0214(14) 0.0043(14) 0.0111(15) C14 0.0515(17) 0.085(2) 0.0399(15) 0.0214(14) 0.0043(14) 0.0111(15) C15 0.0405(14) 0.0454(14) 0.0333(12) 0.0148(10) 0.0105(11) 0.0081(11) C16 0.0405(14) 0.0454(14) 0.0333(12) 0.0148(10) 0.0105(11) 0.0081(11) C17 0.0405(14) 0.0454(14) 0.0333(12) 0.0148(10) 0.0105(11) 0.0081(11) C18 0.033(2) 0.0197(18) 0.0211(17) 0.0021(14) 0.0058(15) 0.0083(15) C19 0.044(2) 0.0202(18) 0.032(2) 0.0087(15) 0.0069(18) 0.0069(16) C20 0.058(3) 0.032(2) 0.047(3) 0.0153(19) 0.015(2) 0.001(2) C21 0.075(4) 0.041(3) 0.035(2) 0.0222(19) 0.014(2) 0.014(2) C22 0.060(3) 0.039(2) 0.032(2) 0.0118(18) -0.003(2) 0.014(2) C23 0.043(2) 0.033(2) 0.031(2) 0.0080(17) 0.0025(18) 0.0127(18) C24 0.0440(16) 0.0476(16) 0.0639(19) 0.0080(13) 0.0084(14) 0.0013(13) C25 0.0440(16) 0.0476(16) 0.0639(19) 0.0080(13) 0.0084(14) 0.0013(13) C26 0.0440(16) 0.0476(16) 0.0639(19) 0.0080(13) 0.0084(14) 0.0013(13) C27 0.0531(19) 0.078(2) 0.065(2) 0.0085(17) -0.0061(15) -0.0063(16) C28 0.0531(19) 0.078(2) 0.065(2) 0.0085(17) -0.0061(15) -0.0063(16) C29 0.0531(19) 0.078(2) 0.065(2) 0.0085(17) -0.0061(15) -0.0063(16) C30 0.0236(18) 0.0221(18) 0.0241(18) 0.0065(14) 0.0036(15) 0.0012(14) C31 0.0232(19) 0.031(2) 0.0267(19) 0.0109(15) 0.0017(15) 0.0042(15) C32 0.033(2) 0.036(2) 0.036(2) 0.0063(17) 0.0038(18) -0.0059(17) C33 0.034(2) 0.047(3) 0.051(3) 0.012(2) -0.005(2) -0.0093(19) C34 0.024(2) 0.058(3) 0.076(3) 0.020(3) 0.006(2) -0.003(2) C35 0.025(2) 0.053(3) 0.068(3) 0.022(2) 0.015(2) 0.0098(19) C36 0.025(2) 0.049(3) 0.037(2) 0.0088(18) 0.0082(17) 0.0060(18) C37 0.030(2) 0.035(2) 0.0215(18) 0.0078(15) 0.0062(16) -0.0025(16) C38 0.039(2) 0.058(3) 0.026(2) 0.0184(19) 0.0023(18) 0.002(2) C39 0.050(3) 0.088(4) 0.032(2) 0.030(2) 0.007(2) -0.009(3) C40 0.061(3) 0.106(5) 0.027(2) 0.006(3) 0.019(2) -0.014(3) C41 0.069(4) 0.064(3) 0.051(3) -0.004(3) 0.032(3) 0.000(3) C42 0.047(3) 0.037(2) 0.036(2) 0.0003(18) 0.013(2) -0.0035(19) C43 0.063(3) 0.096(4) 0.066(4) 0.053(3) 0.035(3) 0.037(3) C44 0.050(3) 0.093(4) 0.068(3) 0.038(3) 0.041(3) 0.038(3) C45 0.093(5) 0.034(3) 0.113(5) 0.013(3) 0.035(4) 0.012(3) C46 0.070(4) 0.059(3) 0.056(3) 0.015(2) 0.026(3) 0.031(3) C47 0.068(3) 0.048(3) 0.070(3) 0.011(2) 0.041(3) -0.005(2) C48 0.059(3) 0.062(3) 0.027(2) -0.003(2) 0.013(2) 0.008(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 N1 2.183(3) . ? Yb1 N5 2.192(3) . ? Yb1 N2 2.210(3) . ? Yb1 N3 2.314(3) . ? Yb1 C30 2.977(3) . ? Yb1 C2 2.980(4) . ? Yb1 C3 2.998(3) . ? Yb1 C4 3.014(3) . ? Yb1 Si1 3.4235(11) . ? Si1 N5 1.711(3) . ? Si1 C43 1.865(5) . ? Si1 C44 1.868(5) . ? Si1 C45 1.873(6) . ? Si2 N5 1.719(3) . ? Si2 C48 1.859(4) . ? Si2 C47 1.869(5) . ? Si2 C46 1.874(5) . ? N1 C2 1.388(4) . ? N1 C6 1.422(4) . ? N2 C4 1.389(4) . ? N2 C18 1.440(4) . ? N3 C30 1.298(5) . ? N3 C31 1.483(4) . ? N4 C30 1.343(5) . ? N4 C37 1.463(5) . ? N4 H4 0.854(10) . ? C1 C2 1.340(5) . ? C1 H1A 0.9400 . ? C1 H1B 0.9400 . ? C2 C3 1.538(5) . ? C3 C30 1.544(5) . ? C3 C4 1.547(5) . ? C3 H3 0.9900 . ? C4 C5 1.336(5) . ? C5 H5A 0.9400 . ? C5 H5B 0.9400 . ? C6 C7 1.411(5) . ? C6 C11 1.412(5) . ? C7 C8 1.389(6) . ? C7 C12 1.518(6) . ? C8 C9 1.386(6) . ? C8 H8 0.9400 . ? C9 C10 1.379(6) . ? C9 H9 0.9400 . ? C10 C11 1.390(5) . ? C10 H10 0.9400 . ? C11 C15 1.524(5) . ? C12 C13 1.513(7) . ? C12 C14 1.513(7) . ? C12 H12 0.9900 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 H13C 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 C16 1.524(6) . ? C15 C17 1.536(6) . ? C15 H15 0.9900 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 C23 1.400(5) . ? C18 C19 1.412(6) . ? C19 C20 1.397(6) . ? C19 C24 1.528(6) . ? C20 C21 1.364(7) . ? C20 H20 0.9400 . ? C21 C22 1.368(7) . ? C21 H21 0.9400 . ? C22 C23 1.400(6) . ? C22 H22 0.9400 . ? C23 C27 1.512(7) . ? C24 C26 1.520(7) . ? C24 C25 1.523(6) . ? C24 H24 0.9900 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C25 H25C 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C26 H26C 0.9700 . ? C27 C29 1.530(7) . ? C27 C28 1.532(8) . ? C27 H27 0.9900 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 H28C 0.9700 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C29 H29C 0.9700 . ? C31 C36 1.518(5) . ? C31 C32 1.529(5) . ? C31 H31 0.9900 . ? C32 C33 1.538(6) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C33 C34 1.517(7) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C34 C35 1.518(6) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C35 C36 1.532(5) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C37 C38 1.523(5) . ? C37 C42 1.530(5) . ? C37 H37 0.9900 . ? C38 C39 1.526(6) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C39 C40 1.513(8) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C40 C41 1.522(8) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C41 C42 1.524(7) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C43 H43C 0.9700 . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C44 H44C 0.9700 . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C45 H45C 0.9700 . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C46 H46C 0.9700 . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C47 H47C 0.9700 . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C48 H48C 0.9700 . ? C49 C54 0.51(4) 2_665 ? C49 C53 1.39(4) 2_665 ? C49 C50 1.495(18) . ? C50 C53 0.73(4) 2_665 ? C50 C51 1.469(18) . ? C50 C52 1.55(5) 2_665 ? C50 C54 1.59(4) 2_665 ? C51 C52 0.46(5) 2_665 ? C51 C53 1.35(4) 2_665 ? C51 C52 1.528(15) . ? C51 C51 1.97(5) 2_665 ? C52 C51 0.46(5) 2_665 ? C52 C52 1.09(5) 2_665 ? C52 C53 1.550(18) . ? C52 C50 1.55(5) 2_665 ? C53 C50 0.73(4) 2_665 ? C53 C51 1.35(4) 2_665 ? C53 C49 1.39(4) 2_665 ? C53 C54 1.516(18) . ? C54 C49 0.51(4) 2_665 ? C54 C50 1.59(4) 2_665 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Yb1 N5 116.20(11) . . ? N1 Yb1 N2 95.54(11) . . ? N5 Yb1 N2 137.37(11) . . ? N1 Yb1 N3 87.53(10) . . ? N5 Yb1 N3 123.03(11) . . ? N2 Yb1 N3 83.72(10) . . ? N1 Yb1 C30 66.55(10) . . ? N5 Yb1 C30 142.92(10) . . ? N2 Yb1 C30 74.35(10) . . ? N3 Yb1 C30 24.55(10) . . ? N1 Yb1 C2 25.74(10) . . ? N5 Yb1 C2 141.80(10) . . ? N2 Yb1 C2 72.13(10) . . ? N3 Yb1 C2 74.83(10) . . ? C30 Yb1 C2 50.54(9) . . ? N1 Yb1 C3 54.28(10) . . ? N5 Yb1 C3 167.60(11) . . ? N2 Yb1 C3 54.92(10) . . ? N3 Yb1 C3 53.08(9) . . ? C30 Yb1 C3 29.95(9) . . ? C2 Yb1 C3 29.82(9) . . ? N1 Yb1 C4 77.59(10) . . ? N5 Yb1 C4 162.56(11) . . ? N2 Yb1 C4 25.36(10) . . ? N3 Yb1 C4 65.48(9) . . ? C30 Yb1 C4 50.66(9) . . ? C2 Yb1 C4 52.03(9) . . ? C3 Yb1 C4 29.83(9) . . ? N1 Yb1 Si1 97.19(8) . . ? N5 Yb1 Si1 25.05(8) . . ? N2 Yb1 Si1 162.36(8) . . ? N3 Yb1 Si1 108.95(7) . . ? C30 Yb1 Si1 122.11(7) . . ? C2 Yb1 Si1 122.28(7) . . ? C3 Yb1 Si1 142.60(7) . . ? C4 Yb1 Si1 172.27(7) . . ? N5 Si1 C43 109.5(2) . . ? N5 Si1 C44 112.8(2) . . ? C43 Si1 C44 106.9(2) . . ? N5 Si1 C45 114.1(2) . . ? C43 Si1 C45 105.8(3) . . ? C44 Si1 C45 107.2(3) . . ? N5 Si1 Yb1 32.86(10) . . ? C43 Si1 Yb1 76.99(17) . . ? C44 Si1 Yb1 129.1(2) . . ? C45 Si1 Yb1 120.7(2) . . ? N5 Si2 C48 114.1(2) . . ? N5 Si2 C47 112.7(2) . . ? C48 Si2 C47 106.8(2) . . ? N5 Si2 C46 107.3(2) . . ? C48 Si2 C46 107.1(2) . . ? C47 Si2 C46 108.6(3) . . ? C2 N1 C6 118.3(3) . . ? C2 N1 Yb1 111.1(2) . . ? C6 N1 Yb1 129.4(2) . . ? C4 N2 C18 115.8(3) . . ? C4 N2 Yb1 111.7(2) . . ? C18 N2 Yb1 131.0(2) . . ? C30 N3 C31 120.6(3) . . ? C30 N3 Yb1 107.7(2) . . ? C31 N3 Yb1 127.1(2) . . ? C30 N4 C37 129.4(3) . . ? C30 N4 H4 120(3) . . ? C37 N4 H4 111(3) . . ? Si1 N5 Si2 121.20(18) . . ? Si1 N5 Yb1 122.09(17) . . ? Si2 N5 Yb1 116.65(16) . . ? C2 C1 H1A 120.0 . . ? C2 C1 H1B 120.0 . . ? H1A C1 H1B 120.0 . . ? C1 C2 N1 127.0(3) . . ? C1 C2 C3 117.7(3) . . ? N1 C2 C3 115.2(3) . . ? C1 C2 Yb1 159.9(3) . . ? N1 C2 Yb1 43.11(16) . . ? C3 C2 Yb1 75.75(18) . . ? C2 C3 C30 111.2(3) . . ? C2 C3 C4 116.9(3) . . ? C30 C3 C4 112.0(3) . . ? C2 C3 Yb1 74.43(17) . . ? C30 C3 Yb1 74.27(18) . . ? C4 C3 Yb1 75.66(18) . . ? C2 C3 H3 105.2 . . ? C30 C3 H3 105.2 . . ? C4 C3 H3 105.2 . . ? Yb1 C3 H3 179.1 . . ? C5 C4 N2 126.7(3) . . ? C5 C4 C3 116.6(3) . . ? N2 C4 C3 116.7(3) . . ? C5 C4 Yb1 166.7(3) . . ? N2 C4 Yb1 42.93(15) . . ? C3 C4 Yb1 74.51(18) . . ? C4 C5 H5A 120.0 . . ? C4 C5 H5B 120.0 . . ? H5A C5 H5B 120.0 . . ? C7 C6 C11 119.3(3) . . ? C7 C6 N1 119.9(3) . . ? C11 C6 N1 120.6(3) . . ? C8 C7 C6 119.2(4) . . ? C8 C7 C12 119.7(4) . . ? C6 C7 C12 121.0(4) . . ? C9 C8 C7 121.5(4) . . ? C9 C8 H8 119.2 . . ? C7 C8 H8 119.2 . . ? C10 C9 C8 119.1(4) . . ? C10 C9 H9 120.4 . . ? C8 C9 H9 120.4 . . ? C9 C10 C11 121.6(4) . . ? C9 C10 H10 119.2 . . ? C11 C10 H10 119.2 . . ? C10 C11 C6 119.2(3) . . ? C10 C11 C15 118.2(3) . . ? C6 C11 C15 122.6(3) . . ? C13 C12 C14 110.8(4) . . ? C13 C12 C7 108.8(4) . . ? C14 C12 C7 115.0(4) . . ? C13 C12 H12 107.3 . . ? C14 C12 H12 107.3 . . ? C7 C12 H12 107.3 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 C16 110.3(3) . . ? C11 C15 C17 112.9(3) . . ? C16 C15 C17 109.6(3) . . ? C11 C15 H15 107.9 . . ? C16 C15 H15 107.9 . . ? C17 C15 H15 107.9 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C23 C18 C19 119.8(4) . . ? C23 C18 N2 120.6(3) . . ? C19 C18 N2 119.5(3) . . ? C20 C19 C18 118.8(4) . . ? C20 C19 C24 118.7(4) . . ? C18 C19 C24 122.5(4) . . ? C21 C20 C19 121.6(4) . . ? C21 C20 H20 119.2 . . ? C19 C20 H20 119.2 . . ? C20 C21 C22 119.4(4) . . ? C20 C21 H21 120.3 . . ? C22 C21 H21 120.3 . . ? C21 C22 C23 122.1(4) . . ? C21 C22 H22 119.0 . . ? C23 C22 H22 119.0 . . ? C22 C23 C18 118.4(4) . . ? C22 C23 C27 119.9(4) . . ? C18 C23 C27 121.8(4) . . ? C26 C24 C25 110.2(4) . . ? C26 C24 C19 112.7(4) . . ? C25 C24 C19 111.5(4) . . ? C26 C24 H24 107.4 . . ? C25 C24 H24 107.4 . . ? C19 C24 H24 107.4 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 C29 112.5(5) . . ? C23 C27 C28 111.3(5) . . ? C29 C27 C28 109.0(4) . . ? C23 C27 H27 108.0 . . ? C29 C27 H27 108.0 . . ? C28 C27 H27 108.0 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N3 C30 N4 124.5(3) . . ? N3 C30 C3 118.9(3) . . ? N4 C30 C3 116.6(3) . . ? N3 C30 Yb1 47.78(17) . . ? N4 C30 Yb1 155.4(2) . . ? C3 C30 Yb1 75.79(18) . . ? N3 C31 C36 109.2(3) . . ? N3 C31 C32 112.2(3) . . ? C36 C31 C32 109.2(3) . . ? N3 C31 H31 108.7 . . ? C36 C31 H31 108.7 . . ? C32 C31 H31 108.7 . . ? C31 C32 C33 110.6(3) . . ? C31 C32 H32A 109.5 . . ? C33 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? C33 C32 H32B 109.5 . . ? H32A C32 H32B 108.1 . . ? C34 C33 C32 111.5(4) . . ? C34 C33 H33A 109.3 . . ? C32 C33 H33A 109.3 . . ? C34 C33 H33B 109.3 . . ? C32 C33 H33B 109.3 . . ? H33A C33 H33B 108.0 . . ? C33 C34 C35 111.3(4) . . ? C33 C34 H34A 109.4 . . ? C35 C34 H34A 109.4 . . ? C33 C34 H34B 109.4 . . ? C35 C34 H34B 109.4 . . ? H34A C34 H34B 108.0 . . ? C34 C35 C36 110.5(4) . . ? C34 C35 H35A 109.6 . . ? C36 C35 H35A 109.6 . . ? C34 C35 H35B 109.6 . . ? C36 C35 H35B 109.6 . . ? H35A C35 H35B 108.1 . . ? C31 C36 C35 112.0(3) . . ? C31 C36 H36A 109.2 . . ? C35 C36 H36A 109.2 . . ? C31 C36 H36B 109.2 . . ? C35 C36 H36B 109.2 . . ? H36A C36 H36B 107.9 . . ? N4 C37 C38 108.4(3) . . ? N4 C37 C42 111.7(3) . . ? C38 C37 C42 110.5(3) . . ? N4 C37 H37 108.7 . . ? C38 C37 H37 108.7 . . ? C42 C37 H37 108.7 . . ? C37 C38 C39 110.8(4) . . ? C37 C38 H38A 109.5 . . ? C39 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? C39 C38 H38B 109.5 . . ? H38A C38 H38B 108.1 . . ? C40 C39 C38 111.3(4) . . ? C40 C39 H39A 109.4 . . ? C38 C39 H39A 109.4 . . ? C40 C39 H39B 109.4 . . ? C38 C39 H39B 109.4 . . ? H39A C39 H39B 108.0 . . ? C39 C40 C41 110.9(4) . . ? C39 C40 H40A 109.5 . . ? C41 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? C41 C40 H40B 109.5 . . ? H40A C40 H40B 108.1 . . ? C40 C41 C42 111.5(4) . . ? C40 C41 H41A 109.3 . . ? C42 C41 H41A 109.3 . . ? C40 C41 H41B 109.3 . . ? C42 C41 H41B 109.3 . . ? H41A C41 H41B 108.0 . . ? C41 C42 C37 111.1(4) . . ? C41 C42 H42A 109.4 . . ? C37 C42 H42A 109.4 . . ? C41 C42 H42B 109.4 . . ? C37 C42 H42B 109.4 . . ? H42A C42 H42B 108.0 . . ? Si1 C43 H43A 109.5 . . ? Si1 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? Si1 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? Si1 C44 H44A 109.5 . . ? Si1 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? Si1 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? Si1 C45 H45A 109.5 . . ? Si1 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? Si1 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? Si2 C46 H46A 109.5 . . ? Si2 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? Si2 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? Si2 C47 H47A 109.5 . . ? Si2 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? Si2 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? Si2 C48 H48A 109.5 . . ? Si2 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? Si2 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C54 C49 C53 94(5) 2_665 2_665 ? C54 C49 C50 91(5) 2_665 . ? C53 C49 C50 29.1(15) 2_665 . ? C53 C50 C51 66(3) 2_665 . ? C53 C50 C49 68(3) 2_665 . ? C51 C50 C49 90(2) . . ? C53 C50 C52 76(3) 2_665 2_665 ? C51 C50 C52 17(2) . 2_665 ? C49 C50 C52 107(2) . 2_665 ? C53 C50 C54 71(3) 2_665 2_665 ? C51 C50 C54 107(2) . 2_665 ? C49 C50 C54 18.7(17) . 2_665 ? C52 C50 C54 125(3) 2_665 2_665 ? C52 C51 C53 106(7) 2_665 2_665 ? C52 C51 C50 92(7) 2_665 . ? C53 C51 C50 29.8(15) 2_665 . ? C52 C51 C52 17(9) 2_665 . ? C53 C51 C52 111(2) 2_665 . ? C50 C51 C52 103.8(18) . . ? C52 C51 C51 13(7) 2_665 2_665 ? C53 C51 C51 110(3) 2_665 2_665 ? C50 C51 C51 101(2) . 2_665 ? C52 C51 C51 4(2) . 2_665 ? C51 C52 C52 155(10) 2_665 2_665 ? C51 C52 C51 163(9) 2_665 . ? C52 C52 C51 7(4) 2_665 . ? C51 C52 C53 57(6) 2_665 . ? C52 C52 C53 127(4) 2_665 . ? C51 C52 C53 127(2) . . ? C51 C52 C50 71(6) 2_665 2_665 ? C52 C52 C50 125(4) 2_665 2_665 ? C51 C52 C50 121(2) . 2_665 ? C53 C52 C50 27.3(13) . 2_665 ? C50 C53 C51 84(3) 2_665 2_665 ? C50 C53 C49 83(3) 2_665 2_665 ? C51 C53 C49 99(2) 2_665 2_665 ? C50 C53 C54 82(4) 2_665 . ? C51 C53 C54 118(2) 2_665 . ? C49 C53 C54 19.6(18) 2_665 . ? C50 C53 C52 77(4) 2_665 . ? C51 C53 C52 17(2) 2_665 . ? C49 C53 C52 113(2) 2_665 . ? C54 C53 C52 131(2) . . ? C49 C54 C53 67(5) 2_665 . ? C49 C54 C50 70(5) 2_665 2_665 ? C53 C54 C50 27.2(14) . 2_665 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Yb1 Si1 N5 -141.4(2) . . . . ? N2 Yb1 Si1 N5 -5.5(3) . . . . ? N3 Yb1 Si1 N5 128.8(2) . . . . ? C30 Yb1 Si1 N5 151.9(2) . . . . ? C2 Yb1 Si1 N5 -147.5(2) . . . . ? C3 Yb1 Si1 N5 -177.8(2) . . . . ? C4 Yb1 Si1 N5 171.6(5) . . . . ? N1 Yb1 Si1 C43 47.0(2) . . . . ? N5 Yb1 Si1 C43 -171.7(3) . . . . ? N2 Yb1 Si1 C43 -177.1(3) . . . . ? N3 Yb1 Si1 C43 -42.9(2) . . . . ? C30 Yb1 Si1 C43 -19.8(2) . . . . ? C2 Yb1 Si1 C43 40.8(2) . . . . ? C3 Yb1 Si1 C43 10.5(2) . . . . ? C4 Yb1 Si1 C43 0.0(6) . . . . ? N1 Yb1 Si1 C44 148.4(2) . . . . ? N5 Yb1 Si1 C44 -70.3(3) . . . . ? N2 Yb1 Si1 C44 -75.8(3) . . . . ? N3 Yb1 Si1 C44 58.5(2) . . . . ? C30 Yb1 Si1 C44 81.6(2) . . . . ? C2 Yb1 Si1 C44 142.2(2) . . . . ? C3 Yb1 Si1 C44 111.9(2) . . . . ? C4 Yb1 Si1 C44 101.3(5) . . . . ? N1 Yb1 Si1 C45 -53.9(3) . . . . ? N5 Yb1 Si1 C45 87.5(3) . . . . ? N2 Yb1 Si1 C45 82.0(4) . . . . ? N3 Yb1 Si1 C45 -143.7(3) . . . . ? C30 Yb1 Si1 C45 -120.6(3) . . . . ? C2 Yb1 Si1 C45 -60.1(3) . . . . ? C3 Yb1 Si1 C45 -90.4(3) . . . . ? C4 Yb1 Si1 C45 -100.9(6) . . . . ? N5 Yb1 N1 C2 175.0(2) . . . . ? N2 Yb1 N1 C2 24.3(2) . . . . ? N3 Yb1 N1 C2 -59.1(2) . . . . ? C30 Yb1 N1 C2 -45.9(2) . . . . ? C3 Yb1 N1 C2 -14.31(19) . . . . ? C4 Yb1 N1 C2 6.3(2) . . . . ? Si1 Yb1 N1 C2 -167.9(2) . . . . ? N5 Yb1 N1 C6 7.6(3) . . . . ? N2 Yb1 N1 C6 -143.1(3) . . . . ? N3 Yb1 N1 C6 133.5(3) . . . . ? C30 Yb1 N1 C6 146.6(3) . . . . ? C2 Yb1 N1 C6 -167.4(4) . . . . ? C3 Yb1 N1 C6 178.3(3) . . . . ? C4 Yb1 N1 C6 -161.1(3) . . . . ? Si1 Yb1 N1 C6 24.7(3) . . . . ? N1 Yb1 N2 C4 -44.9(2) . . . . ? N5 Yb1 N2 C4 175.7(2) . . . . ? N3 Yb1 N2 C4 42.0(2) . . . . ? C30 Yb1 N2 C4 18.9(2) . . . . ? C2 Yb1 N2 C4 -34.0(2) . . . . ? C3 Yb1 N2 C4 -6.6(2) . . . . ? Si1 Yb1 N2 C4 179.09(18) . . . . ? N1 Yb1 N2 C18 150.1(3) . . . . ? N5 Yb1 N2 C18 10.6(4) . . . . ? N3 Yb1 N2 C18 -123.0(3) . . . . ? C30 Yb1 N2 C18 -146.2(3) . . . . ? C2 Yb1 N2 C18 160.9(3) . . . . ? C3 Yb1 N2 C18 -171.6(3) . . . . ? C4 Yb1 N2 C18 -165.1(4) . . . . ? Si1 Yb1 N2 C18 14.0(5) . . . . ? N1 Yb1 N3 C30 30.2(2) . . . . ? N5 Yb1 N3 C30 150.1(2) . . . . ? N2 Yb1 N3 C30 -65.7(2) . . . . ? C2 Yb1 N3 C30 7.5(2) . . . . ? C3 Yb1 N3 C30 -15.5(2) . . . . ? C4 Yb1 N3 C30 -47.3(2) . . . . ? Si1 Yb1 N3 C30 126.9(2) . . . . ? N1 Yb1 N3 C31 -125.2(3) . . . . ? N5 Yb1 N3 C31 -5.3(3) . . . . ? N2 Yb1 N3 C31 138.9(3) . . . . ? C30 Yb1 N3 C31 -155.4(4) . . . . ? C2 Yb1 N3 C31 -147.9(3) . . . . ? C3 Yb1 N3 C31 -170.9(3) . . . . ? C4 Yb1 N3 C31 157.3(3) . . . . ? Si1 Yb1 N3 C31 -28.4(3) . . . . ? C43 Si1 N5 Si2 -168.6(3) . . . . ? C44 Si1 N5 Si2 -49.6(3) . . . . ? C45 Si1 N5 Si2 73.0(3) . . . . ? Yb1 Si1 N5 Si2 -177.2(3) . . . . ? C43 Si1 N5 Yb1 8.6(3) . . . . ? C44 Si1 N5 Yb1 127.6(2) . . . . ? C45 Si1 N5 Yb1 -109.8(3) . . . . ? C48 Si2 N5 Si1 -43.2(3) . . . . ? C47 Si2 N5 Si1 78.8(3) . . . . ? C46 Si2 N5 Si1 -161.7(2) . . . . ? C48 Si2 N5 Yb1 139.4(2) . . . . ? C47 Si2 N5 Yb1 -98.5(2) . . . . ? C46 Si2 N5 Yb1 21.0(3) . . . . ? N1 Yb1 N5 Si1 43.7(2) . . . . ? N2 Yb1 N5 Si1 177.56(14) . . . . ? N3 Yb1 N5 Si1 -61.6(2) . . . . ? C30 Yb1 N5 Si1 -41.5(3) . . . . ? C2 Yb1 N5 Si1 47.2(3) . . . . ? C3 Yb1 N5 Si1 6.1(6) . . . . ? C4 Yb1 N5 Si1 -176.3(2) . . . . ? N1 Yb1 N5 Si2 -139.00(16) . . . . ? N2 Yb1 N5 Si2 -5.1(3) . . . . ? N3 Yb1 N5 Si2 115.78(17) . . . . ? C30 Yb1 N5 Si2 135.85(16) . . . . ? C2 Yb1 N5 Si2 -135.47(15) . . . . ? C3 Yb1 N5 Si2 -176.5(4) . . . . ? C4 Yb1 N5 Si2 1.1(5) . . . . ? Si1 Yb1 N5 Si2 177.3(3) . . . . ? C6 N1 C2 C1 12.8(5) . . . . ? Yb1 N1 C2 C1 -156.2(3) . . . . ? C6 N1 C2 C3 -165.4(3) . . . . ? Yb1 N1 C2 C3 25.6(3) . . . . ? C6 N1 C2 Yb1 169.0(4) . . . . ? N1 Yb1 C2 C1 69.3(8) . . . . ? N5 Yb1 C2 C1 62.0(8) . . . . ? N2 Yb1 C2 C1 -85.2(8) . . . . ? N3 Yb1 C2 C1 -173.3(8) . . . . ? C30 Yb1 C2 C1 -169.3(8) . . . . ? C3 Yb1 C2 C1 -134.5(8) . . . . ? C4 Yb1 C2 C1 -102.8(8) . . . . ? Si1 Yb1 C2 C1 83.6(8) . . . . ? N5 Yb1 C2 N1 -7.3(3) . . . . ? N2 Yb1 C2 N1 -154.5(2) . . . . ? N3 Yb1 C2 N1 117.3(2) . . . . ? C30 Yb1 C2 N1 121.4(2) . . . . ? C3 Yb1 C2 N1 156.2(3) . . . . ? C4 Yb1 C2 N1 -172.2(3) . . . . ? Si1 Yb1 C2 N1 14.2(2) . . . . ? N1 Yb1 C2 C3 -156.2(3) . . . . ? N5 Yb1 C2 C3 -163.52(18) . . . . ? N2 Yb1 C2 C3 49.32(17) . . . . ? N3 Yb1 C2 C3 -38.86(17) . . . . ? C30 Yb1 C2 C3 -34.84(17) . . . . ? C4 Yb1 C2 C3 31.63(17) . . . . ? Si1 Yb1 C2 C3 -141.96(15) . . . . ? C1 C2 C3 C30 -130.3(3) . . . . ? N1 C2 C3 C30 48.1(4) . . . . ? Yb1 C2 C3 C30 65.8(2) . . . . ? C1 C2 C3 C4 99.3(4) . . . . ? N1 C2 C3 C4 -82.3(4) . . . . ? Yb1 C2 C3 C4 -64.6(3) . . . . ? C1 C2 C3 Yb1 163.9(3) . . . . ? N1 C2 C3 Yb1 -17.7(2) . . . . ? N1 Yb1 C3 C2 12.46(17) . . . . ? N5 Yb1 C3 C2 54.8(5) . . . . ? N2 Yb1 C3 C2 -118.1(2) . . . . ? N3 Yb1 C3 C2 130.8(2) . . . . ? C30 Yb1 C3 C2 117.9(3) . . . . ? C4 Yb1 C3 C2 -123.8(3) . . . . ? Si1 Yb1 C3 C2 59.1(2) . . . . ? N1 Yb1 C3 C30 -105.5(2) . . . . ? N5 Yb1 C3 C30 -63.1(5) . . . . ? N2 Yb1 C3 C30 124.0(2) . . . . ? N3 Yb1 C3 C30 12.84(18) . . . . ? C2 Yb1 C3 C30 -117.9(3) . . . . ? C4 Yb1 C3 C30 118.3(3) . . . . ? Si1 Yb1 C3 C30 -58.8(2) . . . . ? N1 Yb1 C3 C4 136.2(2) . . . . ? N5 Yb1 C3 C4 178.6(4) . . . . ? N2 Yb1 C3 C4 5.65(17) . . . . ? N3 Yb1 C3 C4 -105.5(2) . . . . ? C30 Yb1 C3 C4 -118.3(3) . . . . ? C2 Yb1 C3 C4 123.8(3) . . . . ? Si1 Yb1 C3 C4 -177.17(14) . . . . ? C18 N2 C4 C5 -1.1(5) . . . . ? Yb1 N2 C4 C5 -168.6(3) . . . . ? C18 N2 C4 C3 179.2(3) . . . . ? Yb1 N2 C4 C3 11.7(4) . . . . ? C18 N2 C4 Yb1 167.5(4) . . . . ? C2 C3 C4 C5 -124.1(4) . . . . ? C30 C3 C4 C5 106.0(4) . . . . ? Yb1 C3 C4 C5 172.1(3) . . . . ? C2 C3 C4 N2 55.6(4) . . . . ? C30 C3 C4 N2 -74.3(4) . . . . ? Yb1 C3 C4 N2 -8.2(2) . . . . ? C2 C3 C4 Yb1 63.9(3) . . . . ? C30 C3 C4 Yb1 -66.1(2) . . . . ? N1 Yb1 C4 C5 177.3(12) . . . . ? N5 Yb1 C4 C5 33.4(13) . . . . ? N2 Yb1 C4 C5 43.2(11) . . . . ? N3 Yb1 C4 C5 -89.8(11) . . . . ? C30 Yb1 C4 C5 -113.0(12) . . . . ? C2 Yb1 C4 C5 -179.2(12) . . . . ? C3 Yb1 C4 C5 -147.6(12) . . . . ? Si1 Yb1 C4 C5 -134.7(10) . . . . ? N1 Yb1 C4 N2 134.0(2) . . . . ? N5 Yb1 C4 N2 -9.8(5) . . . . ? N3 Yb1 C4 N2 -133.0(2) . . . . ? C30 Yb1 C4 N2 -156.2(3) . . . . ? C2 Yb1 C4 N2 137.5(3) . . . . ? C3 Yb1 C4 N2 169.2(3) . . . . ? Si1 Yb1 C4 N2 -177.9(4) . . . . ? N1 Yb1 C4 C3 -35.11(18) . . . . ? N5 Yb1 C4 C3 -179.0(3) . . . . ? N2 Yb1 C4 C3 -169.2(3) . . . . ? N3 Yb1 C4 C3 57.87(18) . . . . ? C30 Yb1 C4 C3 34.63(17) . . . . ? C2 Yb1 C4 C3 -31.63(17) . . . . ? Si1 Yb1 C4 C3 12.9(6) . . . . ? C2 N1 C6 C7 -110.2(4) . . . . ? Yb1 N1 C6 C7 56.5(4) . . . . ? C2 N1 C6 C11 73.7(4) . . . . ? Yb1 N1 C6 C11 -119.7(3) . . . . ? C11 C6 C7 C8 3.2(5) . . . . ? N1 C6 C7 C8 -173.0(3) . . . . ? C11 C6 C7 C12 -172.4(4) . . . . ? N1 C6 C7 C12 11.4(5) . . . . ? C6 C7 C8 C9 -1.7(6) . . . . ? C12 C7 C8 C9 173.9(4) . . . . ? C7 C8 C9 C10 -0.6(7) . . . . ? C8 C9 C10 C11 1.4(6) . . . . ? C9 C10 C11 C6 0.1(6) . . . . ? C9 C10 C11 C15 -179.1(4) . . . . ? C7 C6 C11 C10 -2.4(5) . . . . ? N1 C6 C11 C10 173.8(3) . . . . ? C7 C6 C11 C15 176.8(3) . . . . ? N1 C6 C11 C15 -7.1(5) . . . . ? C8 C7 C12 C13 -84.1(5) . . . . ? C6 C7 C12 C13 91.4(5) . . . . ? C8 C7 C12 C14 40.9(6) . . . . ? C6 C7 C12 C14 -143.6(4) . . . . ? C10 C11 C15 C16 61.3(5) . . . . ? C6 C11 C15 C16 -117.8(4) . . . . ? C10 C11 C15 C17 -61.7(5) . . . . ? C6 C11 C15 C17 119.1(4) . . . . ? C4 N2 C18 C23 94.2(4) . . . . ? Yb1 N2 C18 C23 -101.2(4) . . . . ? C4 N2 C18 C19 -90.1(4) . . . . ? Yb1 N2 C18 C19 74.5(4) . . . . ? C23 C18 C19 C20 2.8(6) . . . . ? N2 C18 C19 C20 -173.0(3) . . . . ? C23 C18 C19 C24 -177.3(4) . . . . ? N2 C18 C19 C24 6.9(5) . . . . ? C18 C19 C20 C21 -1.7(6) . . . . ? C24 C19 C20 C21 178.3(4) . . . . ? C19 C20 C21 C22 -0.4(7) . . . . ? C20 C21 C22 C23 1.6(7) . . . . ? C21 C22 C23 C18 -0.5(6) . . . . ? C21 C22 C23 C27 180.0(5) . . . . ? C19 C18 C23 C22 -1.7(6) . . . . ? N2 C18 C23 C22 174.1(3) . . . . ? C19 C18 C23 C27 177.8(4) . . . . ? N2 C18 C23 C27 -6.4(6) . . . . ? C20 C19 C24 C26 51.6(5) . . . . ? C18 C19 C24 C26 -128.3(4) . . . . ? C20 C19 C24 C25 -72.9(6) . . . . ? C18 C19 C24 C25 107.2(5) . . . . ? C22 C23 C27 C29 -44.1(7) . . . . ? C18 C23 C27 C29 136.5(5) . . . . ? C22 C23 C27 C28 78.6(6) . . . . ? C18 C23 C27 C28 -100.8(5) . . . . ? C31 N3 C30 N4 7.3(5) . . . . ? Yb1 N3 C30 N4 -150.0(3) . . . . ? C31 N3 C30 C3 -174.4(3) . . . . ? Yb1 N3 C30 C3 28.3(4) . . . . ? C31 N3 C30 Yb1 157.3(4) . . . . ? C37 N4 C30 N3 173.0(4) . . . . ? C37 N4 C30 C3 -5.4(5) . . . . ? C37 N4 C30 Yb1 110.2(6) . . . . ? C2 C3 C30 N3 -87.1(4) . . . . ? C4 C3 C30 N3 45.7(4) . . . . ? Yb1 C3 C30 N3 -21.2(3) . . . . ? C2 C3 C30 N4 91.3(4) . . . . ? C4 C3 C30 N4 -135.9(3) . . . . ? Yb1 C3 C30 N4 157.2(3) . . . . ? C2 C3 C30 Yb1 -65.9(2) . . . . ? C4 C3 C30 Yb1 66.9(2) . . . . ? N1 Yb1 C30 N3 -146.8(3) . . . . ? N5 Yb1 C30 N3 -43.8(3) . . . . ? N2 Yb1 C30 N3 109.9(2) . . . . ? C2 Yb1 C30 N3 -170.6(3) . . . . ? C3 Yb1 C30 N3 154.7(3) . . . . ? C4 Yb1 C30 N3 120.2(3) . . . . ? Si1 Yb1 C30 N3 -63.2(2) . . . . ? N1 Yb1 C30 N4 -65.1(6) . . . . ? N5 Yb1 C30 N4 37.8(7) . . . . ? N2 Yb1 C30 N4 -168.5(6) . . . . ? N3 Yb1 C30 N4 81.7(6) . . . . ? C2 Yb1 C30 N4 -89.0(6) . . . . ? C3 Yb1 C30 N4 -123.7(7) . . . . ? C4 Yb1 C30 N4 -158.2(7) . . . . ? Si1 Yb1 C30 N4 18.5(6) . . . . ? N1 Yb1 C30 C3 58.53(19) . . . . ? N5 Yb1 C30 C3 161.48(19) . . . . ? N2 Yb1 C30 C3 -44.81(18) . . . . ? N3 Yb1 C30 C3 -154.7(3) . . . . ? C2 Yb1 C30 C3 34.69(17) . . . . ? C4 Yb1 C30 C3 -34.48(18) . . . . ? Si1 Yb1 C30 C3 142.15(16) . . . . ? C30 N3 C31 C36 -170.7(3) . . . . ? Yb1 N3 C31 C36 -18.1(4) . . . . ? C30 N3 C31 C32 68.0(4) . . . . ? Yb1 N3 C31 C32 -139.4(3) . . . . ? N3 C31 C32 C33 178.4(3) . . . . ? C36 C31 C32 C33 57.2(4) . . . . ? C31 C32 C33 C34 -56.6(5) . . . . ? C32 C33 C34 C35 55.2(5) . . . . ? C33 C34 C35 C36 -54.6(5) . . . . ? N3 C31 C36 C35 178.8(3) . . . . ? C32 C31 C36 C35 -58.1(4) . . . . ? C34 C35 C36 C31 57.0(5) . . . . ? C30 N4 C37 C38 -148.3(4) . . . . ? C30 N4 C37 C42 89.6(5) . . . . ? N4 C37 C38 C39 -179.2(4) . . . . ? C42 C37 C38 C39 -56.4(5) . . . . ? C37 C38 C39 C40 57.0(5) . . . . ? C38 C39 C40 C41 -56.2(6) . . . . ? C39 C40 C41 C42 55.5(6) . . . . ? C40 C41 C42 C37 -55.4(5) . . . . ? N4 C37 C42 C41 176.6(4) . . . . ? C38 C37 C42 C41 55.7(5) . . . . ? C54 C49 C50 C53 -95(8) 2_665 . . 2_665 ? C54 C49 C50 C51 -160(7) 2_665 . . . ? C53 C49 C50 C51 -64(3) 2_665 . . . ? C54 C49 C50 C52 -162(7) 2_665 . . 2_665 ? C53 C49 C50 C52 -66(3) 2_665 . . 2_665 ? C53 C49 C50 C54 95(8) 2_665 . . 2_665 ? C53 C50 C51 C52 121(10) 2_665 . . 2_665 ? C49 C50 C51 C52 -174(9) . . . 2_665 ? C54 C50 C51 C52 180(9) 2_665 . . 2_665 ? C49 C50 C51 C53 66(3) . . . 2_665 ? C52 C50 C51 C53 -121(10) 2_665 . . 2_665 ? C54 C50 C51 C53 59(3) 2_665 . . 2_665 ? C53 C50 C51 C52 108(3) 2_665 . . . ? C49 C50 C51 C52 173.5(19) . . . . ? C52 C50 C51 C52 -13(9) 2_665 . . . ? C54 C50 C51 C52 167(2) 2_665 . . . ? C53 C50 C51 C51 111(4) 2_665 . . 2_665 ? C49 C50 C51 C51 176(3) . . . 2_665 ? C52 C50 C51 C51 -10(7) 2_665 . . 2_665 ? C54 C50 C51 C51 170(3) 2_665 . . 2_665 ? C52 C51 C52 C51 0.00(16) 2_665 . . 2_665 ? C53 C51 C52 C51 78(24) 2_665 . . 2_665 ? C50 C51 C52 C51 48(23) . . . 2_665 ? C53 C51 C52 C52 78(23) 2_665 . . 2_665 ? C50 C51 C52 C52 48(23) . . . 2_665 ? C51 C51 C52 C52 0.0(2) 2_665 . . 2_665 ? C52 C51 C52 C53 95(25) 2_665 . . . ? C53 C51 C52 C53 174(3) 2_665 . . . ? C50 C51 C52 C53 143(4) . . . . ? C51 C51 C52 C53 95(25) 2_665 . . . ? C52 C51 C52 C50 128(25) 2_665 . . 2_665 ? C53 C51 C52 C50 -154(4) 2_665 . . 2_665 ? C50 C51 C52 C50 176(3) . . . 2_665 ? C51 C51 C52 C50 128(25) 2_665 . . 2_665 ? C51 C52 C53 C50 -114(10) 2_665 . . 2_665 ? C52 C52 C53 C50 96(8) 2_665 . . 2_665 ? C51 C52 C53 C50 87(4) . . . 2_665 ? C52 C52 C53 C51 -150(16) 2_665 . . 2_665 ? C51 C52 C53 C51 -159(11) . . . 2_665 ? C50 C52 C53 C51 114(10) 2_665 . . 2_665 ? C51 C52 C53 C49 -37(11) 2_665 . . 2_665 ? C52 C52 C53 C49 173(6) 2_665 . . 2_665 ? C51 C52 C53 C49 164(3) . . . 2_665 ? C50 C52 C53 C49 76(3) 2_665 . . 2_665 ? C51 C52 C53 C54 -47(11) 2_665 . . . ? C52 C52 C53 C54 163(6) 2_665 . . . ? C51 C52 C53 C54 154(3) . . . . ? C50 C52 C53 C54 67(4) 2_665 . . . ? C50 C53 C54 C49 91(8) 2_665 . . 2_665 ? C51 C53 C54 C49 13(8) 2_665 . . 2_665 ? C52 C53 C54 C49 27(9) . . . 2_665 ? C51 C53 C54 C50 -79(4) 2_665 . . 2_665 ? C49 C53 C54 C50 -91(8) 2_665 . . 2_665 ? C52 C53 C54 C50 -65(4) . . . 2_665 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.144 _refine_diff_density_min -1.142 _refine_diff_density_rms 0.104 _database_code_depnum_ccdc_archive 'CCDC 976987' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_complex3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H80 N5 Si2 Y' _chemical_formula_sum 'C48 H80 N5 Si2 Y' _chemical_formula_weight 872.26 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' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.4805(7) _cell_length_b 12.4211(12) _cell_length_c 17.5400(9) _cell_angle_alpha 84.532(6) _cell_angle_beta 82.510(5) _cell_angle_gamma 87.367(6) _cell_volume 2467.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 5372 _cell_measurement_theta_min 3.2905 _cell_measurement_theta_max 29.4327 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.78 _exptl_crystal_size_mid 0.75 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.174 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 940 _exptl_absorpt_coefficient_mu 1.266 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.67853 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'xcalibur, Atlas, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.4692 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22943 _diffrn_reflns_av_R_equivalents 0.0637 _diffrn_reflns_av_unetI/netI 0.0741 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.30 _diffrn_reflns_theta_max 25.50 _reflns_number_total 9141 _reflns_number_gt 7407 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro, Agilent Technologies' _computing_cell_refinement 'CrysAlisPro, Agilent Technologies' _computing_data_reduction 'CrysAlisPro, Agilent Technologies' _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^)+(0.0382P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9141 _refine_ls_number_parameters 523 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0617 _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_ref 0.0940 _refine_ls_wR_factor_gt 0.0888 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _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 H4 H 0.5889(10) 0.7334(19) 0.9964(13) 0.022(7) Uiso 1 1 d D . . Y1 Y 0.702439(19) 0.762972(19) 0.734204(12) 0.02119(8) Uani 1 1 d . . . Si1 Si 0.55584(6) 0.57763(6) 0.65420(4) 0.03269(19) Uani 1 1 d . . . Si2 Si 0.60806(6) 0.78535(6) 0.55636(4) 0.03188(19) Uani 1 1 d . . . N1 N 0.82026(16) 0.64885(16) 0.79477(11) 0.0227(5) Uani 1 1 d . . . N2 N 0.80252(16) 0.90864(15) 0.75070(11) 0.0224(5) Uani 1 1 d . . . N3 N 0.60872(16) 0.79757(16) 0.85729(11) 0.0246(5) Uani 1 1 d . . . N4 N 0.65944(17) 0.74948(18) 0.98146(11) 0.0293(5) Uani 1 1 d D . . N5 N 0.61617(16) 0.70283(16) 0.63994(11) 0.0246(5) Uani 1 1 d . . . C1 C 0.9829(2) 0.6683(2) 0.86834(15) 0.0336(6) Uani 1 1 d . . . H1A H 1.0242 0.6056 0.8505 0.040 Uiso 1 1 calc R . . H1B H 1.0152 0.7093 0.9030 0.040 Uiso 1 1 calc R . . C2 C 0.87916(19) 0.69889(19) 0.84463(13) 0.0227(5) Uani 1 1 d . . . C3 C 0.81602(19) 0.80086(19) 0.87642(13) 0.0213(5) Uani 1 1 d . . . H3 H 0.8532 0.8115 0.9235 0.026 Uiso 1 1 calc R . . C4 C 0.83459(19) 0.9076(2) 0.82419(13) 0.0215(5) Uani 1 1 d . . . C5 C 0.8799(2) 0.9885(2) 0.85419(14) 0.0328(6) Uani 1 1 d . . . H5A H 0.8932 1.0556 0.8242 0.039 Uiso 1 1 calc R . . H5B H 0.8989 0.9791 0.9056 0.039 Uiso 1 1 calc R . . C6 C 0.85778(19) 0.5401(2) 0.78025(14) 0.0240(6) Uani 1 1 d . . . C7 C 0.9197(2) 0.5184(2) 0.70858(14) 0.0282(6) Uani 1 1 d . . . C8 C 0.9413(2) 0.4113(2) 0.69242(16) 0.0367(7) Uani 1 1 d . . . H8 H 0.9811 0.3961 0.6435 0.044 Uiso 1 1 calc R . . C9 C 0.9062(2) 0.3268(2) 0.74584(17) 0.0414(7) Uani 1 1 d . . . H9 H 0.9200 0.2542 0.7333 0.050 Uiso 1 1 calc R . . C10 C 0.8513(2) 0.3483(2) 0.81724(16) 0.0346(7) Uani 1 1 d . . . H10 H 0.8298 0.2897 0.8546 0.042 Uiso 1 1 calc R . . C11 C 0.8262(2) 0.4538(2) 0.83631(14) 0.0273(6) Uani 1 1 d . . . C12 C 0.9702(2) 0.6086(2) 0.65038(15) 0.0372(7) Uani 1 1 d . . . H12 H 0.9477 0.6792 0.6723 0.045 Uiso 1 1 calc R . . C13 C 1.1035(3) 0.5973(3) 0.6394(2) 0.0742(12) Uani 1 1 d . . . H13A H 1.1329 0.6014 0.6890 0.111 Uiso 1 1 calc R . . H13B H 1.1359 0.6558 0.6024 0.111 Uiso 1 1 calc R . . H13C H 1.1278 0.5274 0.6198 0.111 Uiso 1 1 calc R . . C14 C 0.9237(3) 0.6115(3) 0.57220(16) 0.0528(9) Uani 1 1 d . . . H14A H 0.9462 0.5436 0.5490 0.079 Uiso 1 1 calc R . . H14B H 0.9573 0.6723 0.5379 0.079 Uiso 1 1 calc R . . H14C H 0.8378 0.6204 0.5796 0.079 Uiso 1 1 calc R . . C15 C 0.7686(2) 0.4716(2) 0.91764(14) 0.0308(6) Uani 1 1 d . . . H15 H 0.7569 0.5513 0.9210 0.037 Uiso 1 1 calc R . . C16 C 0.8505(2) 0.4283(2) 0.97640(16) 0.0425(7) Uani 1 1 d . . . H16A H 0.8145 0.4429 1.0284 0.064 Uiso 1 1 calc R . . H16B H 0.9258 0.4641 0.9644 0.064 Uiso 1 1 calc R . . H16C H 0.8636 0.3501 0.9741 0.064 Uiso 1 1 calc R . . C17 C 0.6483(2) 0.4204(2) 0.93798(16) 0.0431(8) Uani 1 1 d . . . H17A H 0.5926 0.4573 0.9056 0.065 Uiso 1 1 calc R . . H17B H 0.6197 0.4275 0.9924 0.065 Uiso 1 1 calc R . . H17C H 0.6557 0.3436 0.9289 0.065 Uiso 1 1 calc R . . C18 C 0.8197(2) 1.0090(2) 0.70309(13) 0.0245(6) Uani 1 1 d . . . C19 C 0.7244(2) 1.0843(2) 0.69716(14) 0.0294(6) Uani 1 1 d . . . C20 C 0.7387(2) 1.1731(2) 0.64270(15) 0.0373(7) Uani 1 1 d . . . H20 H 0.6747 1.2234 0.6376 0.045 Uiso 1 1 calc R . . C21 C 0.8431(3) 1.1898(2) 0.59614(15) 0.0414(7) Uani 1 1 d . . . H21 H 0.8500 1.2492 0.5577 0.050 Uiso 1 1 calc R . . C22 C 0.9376(3) 1.1203(2) 0.60530(14) 0.0368(7) Uani 1 1 d . . . H22 H 1.0107 1.1345 0.5746 0.044 Uiso 1 1 calc R . . C23 C 0.9290(2) 1.0293(2) 0.65850(13) 0.0281(6) Uani 1 1 d . . . C24 C 0.6092(2) 1.0722(2) 0.75056(15) 0.0353(7) Uani 1 1 d . . . H24 H 0.6090 0.9971 0.7768 0.042 Uiso 1 1 calc R . . C25 C 0.6024(3) 1.1510(3) 0.81328(19) 0.0588(9) Uani 1 1 d . . . H25A H 0.6677 1.1349 0.8438 0.088 Uiso 1 1 calc R . . H25B H 0.5276 1.1431 0.8470 0.088 Uiso 1 1 calc R . . H25C H 0.6074 1.2254 0.7891 0.088 Uiso 1 1 calc R . . C26 C 0.5010(3) 1.0874(3) 0.7084(2) 0.0639(10) Uani 1 1 d . . . H26A H 0.4960 1.1620 0.6849 0.096 Uiso 1 1 calc R . . H26B H 0.4304 1.0726 0.7451 0.096 Uiso 1 1 calc R . . H26C H 0.5069 1.0373 0.6680 0.096 Uiso 1 1 calc R . . C27 C 1.0355(2) 0.9548(2) 0.66654(14) 0.0327(6) Uani 1 1 d . . . H27 H 1.0135 0.8970 0.7090 0.039 Uiso 1 1 calc R . . C28 C 1.1382(3) 1.0155(3) 0.68791(18) 0.0565(9) Uani 1 1 d . . . H28A H 1.1636 1.0704 0.6458 0.085 Uiso 1 1 calc R . . H28B H 1.2037 0.9643 0.6963 0.085 Uiso 1 1 calc R . . H28C H 1.1128 1.0508 0.7352 0.085 Uiso 1 1 calc R . . C29 C 1.0747(3) 0.9007(3) 0.59309(16) 0.0474(8) Uani 1 1 d . . . H29A H 1.0115 0.8565 0.5819 0.071 Uiso 1 1 calc R . . H29B H 1.1448 0.8545 0.5997 0.071 Uiso 1 1 calc R . . H29C H 1.0931 0.9562 0.5501 0.071 Uiso 1 1 calc R . . C30 C 0.6861(2) 0.78244(19) 0.90599(13) 0.0233(6) Uani 1 1 d . . . C31 C 0.4819(2) 0.7919(2) 0.88519(14) 0.0271(6) Uani 1 1 d . . . H31 H 0.4673 0.7223 0.9180 0.033 Uiso 1 1 calc R . . C32 C 0.4369(2) 0.8862(2) 0.93244(15) 0.0345(7) Uani 1 1 d . . . H32A H 0.4779 0.8833 0.9789 0.041 Uiso 1 1 calc R . . H32B H 0.4552 0.9554 0.9012 0.041 Uiso 1 1 calc R . . C33 C 0.3049(2) 0.8825(3) 0.95707(17) 0.0471(8) Uani 1 1 d . . . H33A H 0.2872 0.8169 0.9926 0.057 Uiso 1 1 calc R . . H33B H 0.2784 0.9465 0.9852 0.057 Uiso 1 1 calc R . . C34 C 0.2381(2) 0.8814(3) 0.8880(2) 0.0554(9) Uani 1 1 d . . . H34A H 0.1534 0.8730 0.9062 0.066 Uiso 1 1 calc R . . H34B H 0.2473 0.9512 0.8559 0.066 Uiso 1 1 calc R . . C35 C 0.2827(2) 0.7900(3) 0.83975(19) 0.0495(8) Uani 1 1 d . . . H35A H 0.2422 0.7946 0.7930 0.059 Uiso 1 1 calc R . . H35B H 0.2641 0.7199 0.8697 0.059 Uiso 1 1 calc R . . C36 C 0.4147(2) 0.7942(2) 0.81583(15) 0.0359(7) Uani 1 1 d . . . H36A H 0.4413 0.7318 0.7861 0.043 Uiso 1 1 calc R . . H36B H 0.4324 0.8612 0.7817 0.043 Uiso 1 1 calc R . . C37 C 0.7400(2) 0.7203(2) 1.03956(13) 0.0277(6) Uani 1 1 d . . . H37 H 0.8137 0.6868 1.0137 0.033 Uiso 1 1 calc R . . C38 C 0.6810(2) 0.6367(2) 1.09991(14) 0.0361(7) Uani 1 1 d . . . H38A H 0.6644 0.5721 1.0747 0.043 Uiso 1 1 calc R . . H38B H 0.6052 0.6674 1.1236 0.043 Uiso 1 1 calc R . . C39 C 0.7596(3) 0.6037(3) 1.16256(17) 0.0498(9) Uani 1 1 d . . . H39A H 0.7181 0.5521 1.2023 0.060 Uiso 1 1 calc R . . H39B H 0.8321 0.5667 1.1395 0.060 Uiso 1 1 calc R . . C40 C 0.7918(3) 0.7008(3) 1.20007(17) 0.0635(11) Uani 1 1 d . . . H40A H 0.8459 0.6776 1.2385 0.076 Uiso 1 1 calc R . . H40B H 0.7201 0.7339 1.2274 0.076 Uiso 1 1 calc R . . C41 C 0.8506(3) 0.7840(3) 1.13987(17) 0.0542(9) Uani 1 1 d . . . H41A H 0.9260 0.7530 1.1159 0.065 Uiso 1 1 calc R . . H41B H 0.8678 0.8484 1.1651 0.065 Uiso 1 1 calc R . . C42 C 0.7715(2) 0.8179(2) 1.07740(15) 0.0378(7) Uani 1 1 d . . . H42A H 0.6988 0.8543 1.1007 0.045 Uiso 1 1 calc R . . H42B H 0.8127 0.8700 1.0378 0.045 Uiso 1 1 calc R . . C43 C 0.5544(3) 0.5251(3) 0.75828(17) 0.0536(9) Uani 1 1 d . . . H43A H 0.6291 0.5405 0.7758 0.080 Uiso 1 1 calc R . . H43B H 0.5439 0.4468 0.7638 0.080 Uiso 1 1 calc R . . H43C H 0.4895 0.5606 0.7896 0.080 Uiso 1 1 calc R . . C44 C 0.4012(2) 0.5806(3) 0.63375(19) 0.0523(9) Uani 1 1 d . . . H44A H 0.3547 0.6332 0.6644 0.078 Uiso 1 1 calc R . . H44B H 0.3689 0.5087 0.6473 0.078 Uiso 1 1 calc R . . H44C H 0.3984 0.6016 0.5787 0.078 Uiso 1 1 calc R . . C45 C 0.6381(3) 0.4726(3) 0.5976(2) 0.0603(9) Uani 1 1 d . . . H45A H 0.6512 0.4998 0.5429 0.090 Uiso 1 1 calc R . . H45B H 0.5924 0.4069 0.6033 0.090 Uiso 1 1 calc R . . H45C H 0.7140 0.4558 0.6166 0.090 Uiso 1 1 calc R . . C46 C 0.7161(3) 0.8938(2) 0.55395(18) 0.0476(8) Uani 1 1 d . . . H46A H 0.6955 0.9352 0.5989 0.071 Uiso 1 1 calc R . . H46B H 0.7143 0.9422 0.5066 0.071 Uiso 1 1 calc R . . H46C H 0.7952 0.8609 0.5551 0.071 Uiso 1 1 calc R . . C47 C 0.4589(3) 0.8519(3) 0.5513(2) 0.0589(10) Uani 1 1 d . . . H47A H 0.4034 0.7979 0.5427 0.088 Uiso 1 1 calc R . . H47B H 0.4634 0.9091 0.5086 0.088 Uiso 1 1 calc R . . H47C H 0.4318 0.8834 0.5999 0.088 Uiso 1 1 calc R . . C48 C 0.6479(3) 0.7172(3) 0.46544(16) 0.0566(9) Uani 1 1 d . . . H48A H 0.7270 0.6838 0.4649 0.085 Uiso 1 1 calc R . . H48B H 0.6463 0.7708 0.4208 0.085 Uiso 1 1 calc R . . H48C H 0.5913 0.6613 0.4630 0.085 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y1 0.02166(13) 0.02119(14) 0.02141(13) 0.00001(10) -0.00630(9) -0.00179(9) Si1 0.0313(4) 0.0311(4) 0.0378(4) 0.0028(4) -0.0153(3) -0.0062(3) Si2 0.0374(4) 0.0294(4) 0.0311(4) 0.0011(3) -0.0149(3) -0.0035(3) N1 0.0205(10) 0.0198(11) 0.0286(11) -0.0019(9) -0.0072(8) 0.0006(9) N2 0.0252(11) 0.0177(11) 0.0246(11) -0.0024(9) -0.0031(8) -0.0016(9) N3 0.0188(10) 0.0270(12) 0.0273(11) 0.0028(10) -0.0035(8) -0.0012(9) N4 0.0201(12) 0.0404(14) 0.0250(12) 0.0076(10) -0.0011(9) -0.0029(10) N5 0.0233(11) 0.0255(12) 0.0266(11) -0.0035(9) -0.0088(8) -0.0013(9) C1 0.0247(14) 0.0308(16) 0.0478(16) -0.0056(13) -0.0123(12) 0.0002(12) C2 0.0224(13) 0.0205(14) 0.0243(13) 0.0031(11) -0.0021(10) -0.0026(10) C3 0.0204(12) 0.0249(14) 0.0189(12) 0.0007(11) -0.0045(9) -0.0037(10) C4 0.0185(12) 0.0250(14) 0.0208(12) -0.0042(11) -0.0003(9) 0.0003(11) C5 0.0460(17) 0.0291(15) 0.0242(13) -0.0008(12) -0.0051(11) -0.0102(13) C6 0.0191(12) 0.0229(14) 0.0322(14) -0.0024(12) -0.0119(10) -0.0003(11) C7 0.0200(13) 0.0312(16) 0.0348(14) -0.0043(12) -0.0075(10) 0.0005(11) C8 0.0370(16) 0.0360(17) 0.0392(16) -0.0124(14) -0.0076(12) 0.0043(13) C9 0.0493(18) 0.0255(16) 0.0528(19) -0.0099(15) -0.0183(14) 0.0078(14) C10 0.0385(16) 0.0250(16) 0.0420(17) 0.0011(13) -0.0134(13) -0.0026(13) C11 0.0260(14) 0.0239(14) 0.0339(14) -0.0013(12) -0.0120(11) -0.0001(11) C12 0.0311(15) 0.0407(18) 0.0379(16) -0.0032(14) 0.0016(12) -0.0001(13) C13 0.0353(19) 0.086(3) 0.095(3) 0.025(2) -0.0049(18) -0.0129(18) C14 0.059(2) 0.058(2) 0.0384(17) 0.0015(16) -0.0014(15) -0.0054(17) C15 0.0356(15) 0.0229(14) 0.0334(14) 0.0058(12) -0.0085(11) -0.0020(12) C16 0.0460(17) 0.0451(19) 0.0386(16) 0.0012(15) -0.0152(13) -0.0067(14) C17 0.0375(16) 0.0473(19) 0.0429(17) 0.0097(15) -0.0081(13) -0.0054(14) C18 0.0342(14) 0.0202(13) 0.0196(12) -0.0026(11) -0.0036(10) -0.0045(11) C19 0.0368(15) 0.0235(14) 0.0284(14) -0.0019(12) -0.0066(11) -0.0014(12) C20 0.0510(18) 0.0232(15) 0.0368(16) 0.0025(13) -0.0073(13) 0.0035(13) C21 0.065(2) 0.0283(16) 0.0288(15) 0.0099(13) -0.0034(14) -0.0076(15) C22 0.0522(18) 0.0346(17) 0.0221(14) -0.0034(13) 0.0050(12) -0.0126(14) C23 0.0365(15) 0.0303(15) 0.0184(12) -0.0062(11) -0.0015(10) -0.0082(12) C24 0.0315(15) 0.0270(15) 0.0455(17) 0.0028(13) -0.0030(12) 0.0012(12) C25 0.052(2) 0.057(2) 0.063(2) -0.0158(18) 0.0161(16) -0.0037(17) C26 0.0425(19) 0.074(3) 0.075(2) -0.001(2) -0.0133(17) 0.0030(18) C27 0.0306(15) 0.0386(17) 0.0270(14) 0.0001(13) 0.0035(11) -0.0062(12) C28 0.0460(19) 0.074(3) 0.0538(19) -0.0173(18) -0.0124(15) -0.0081(17) C29 0.0415(18) 0.052(2) 0.0491(18) -0.0149(16) -0.0015(14) -0.0016(15) C30 0.0260(13) 0.0198(13) 0.0232(13) 0.0000(11) -0.0011(10) -0.0006(11) C31 0.0201(13) 0.0273(15) 0.0319(14) 0.0060(12) -0.0014(10) -0.0016(11) C32 0.0311(15) 0.0364(17) 0.0336(15) 0.0030(13) -0.0015(11) 0.0042(13) C33 0.0350(16) 0.0439(19) 0.0551(19) 0.0062(16) 0.0105(14) 0.0093(14) C34 0.0244(16) 0.056(2) 0.082(2) 0.0080(19) -0.0021(15) 0.0029(15) C35 0.0260(15) 0.048(2) 0.074(2) 0.0049(18) -0.0141(14) -0.0029(14) C36 0.0262(14) 0.0391(17) 0.0428(16) 0.0006(14) -0.0073(12) -0.0044(12) C37 0.0267(14) 0.0318(15) 0.0237(13) 0.0008(12) -0.0035(10) 0.0039(12) C38 0.0328(15) 0.0439(18) 0.0293(14) 0.0071(13) -0.0025(11) -0.0013(13) C39 0.0436(18) 0.065(2) 0.0357(16) 0.0217(17) -0.0069(13) 0.0050(16) C40 0.056(2) 0.104(3) 0.0306(17) -0.003(2) -0.0159(15) 0.017(2) C41 0.059(2) 0.069(2) 0.0401(18) -0.0140(17) -0.0212(15) 0.0002(18) C42 0.0455(17) 0.0379(17) 0.0305(15) -0.0056(13) -0.0060(12) 0.0022(14) C43 0.0514(19) 0.055(2) 0.054(2) 0.0217(17) -0.0213(15) -0.0175(16) C44 0.0395(17) 0.055(2) 0.066(2) 0.0097(18) -0.0255(15) -0.0154(15) C45 0.069(2) 0.0333(19) 0.081(2) -0.0109(18) -0.0150(19) 0.0001(17) C46 0.0490(18) 0.0386(18) 0.057(2) -0.0004(16) -0.0138(15) -0.0127(14) C47 0.052(2) 0.047(2) 0.079(2) 0.0144(19) -0.0312(17) -0.0005(16) C48 0.085(2) 0.055(2) 0.0317(16) 0.0007(16) -0.0196(16) -0.0077(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y1 N1 2.2088(17) . ? Y1 N5 2.237(2) . ? Y1 N2 2.248(2) . ? Y1 N3 2.3520(19) . ? Y1 C2 3.014(2) . ? Y1 C30 3.027(2) . ? Y1 C3 3.045(2) . ? Y1 Si2 3.4162(7) . ? Y1 Si1 3.4190(9) . ? Si1 N5 1.715(2) . ? Si1 C44 1.854(3) . ? Si1 C45 1.863(3) . ? Si1 C43 1.877(3) . ? Si2 N5 1.7172(19) . ? Si2 C46 1.867(3) . ? Si2 C48 1.871(3) . ? Si2 C47 1.876(3) . ? N1 C2 1.380(3) . ? N1 C6 1.435(3) . ? N2 C4 1.385(3) . ? N2 C18 1.439(3) . ? N3 C30 1.306(3) . ? N3 C31 1.477(3) . ? N4 C30 1.348(3) . ? N4 C37 1.473(3) . ? N4 H4 0.845(10) . ? C1 C2 1.339(3) . ? C1 H1A 0.9500 . ? C1 H1B 0.9500 . ? C2 C3 1.545(3) . ? C3 C30 1.534(3) . ? C3 C4 1.545(3) . ? C3 H3 1.0000 . ? C4 C5 1.334(4) . ? C5 H5A 0.9500 . ? C5 H5B 0.9500 . ? C6 C7 1.404(3) . ? C6 C11 1.410(3) . ? C7 C8 1.391(4) . ? C7 C12 1.524(4) . ? C8 C9 1.376(4) . ? C8 H8 0.9500 . ? C9 C10 1.371(4) . ? C9 H9 0.9500 . ? C10 C11 1.392(4) . ? C10 H10 0.9500 . ? C11 C15 1.524(4) . ? C12 C13 1.519(4) . ? C12 C14 1.532(4) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.528(3) . ? C15 C17 1.532(4) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C23 1.409(3) . ? C18 C19 1.414(3) . ? C19 C20 1.389(3) . ? C19 C24 1.523(3) . ? C20 C21 1.372(4) . ? C20 H20 0.9500 . ? C21 C22 1.371(4) . ? C21 H21 0.9500 . ? C22 C23 1.394(3) . ? C22 H22 0.9500 . ? C23 C27 1.512(3) . ? C24 C26 1.522(4) . ? C24 C25 1.533(4) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C29 1.516(4) . ? C27 C28 1.534(4) . ? C27 H27 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C31 C36 1.520(3) . ? C31 C32 1.531(4) . ? C31 H31 1.0000 . ? C32 C33 1.522(4) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.516(4) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.512(5) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.520(4) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C42 1.515(4) . ? C37 C38 1.525(3) . ? C37 H37 1.0000 . ? C38 C39 1.526(3) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.511(5) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.519(4) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.529(4) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Y1 N5 117.74(7) . . ? N1 Y1 N2 93.59(7) . . ? N5 Y1 N2 137.04(7) . . ? N1 Y1 N3 86.59(7) . . ? N5 Y1 N3 125.78(7) . . ? N2 Y1 N3 81.67(7) . . ? N1 Y1 C2 25.09(7) . . ? N5 Y1 C2 142.53(7) . . ? N2 Y1 C2 70.55(7) . . ? N3 Y1 C2 74.03(6) . . ? N1 Y1 C30 65.67(7) . . ? N5 Y1 C30 145.56(7) . . ? N2 Y1 C30 72.36(7) . . ? N3 Y1 C30 24.20(6) . . ? C2 Y1 C30 50.04(6) . . ? N1 Y1 C3 53.28(7) . . ? N5 Y1 C3 169.11(7) . . ? N2 Y1 C3 53.52(6) . . ? N3 Y1 C3 52.06(6) . . ? C2 Y1 C3 29.53(6) . . ? C30 Y1 C3 29.26(6) . . ? N1 Y1 Si2 135.00(5) . . ? N5 Y1 Si2 26.09(5) . . ? N2 Y1 Si2 111.05(5) . . ? N3 Y1 Si2 132.44(5) . . ? C2 Y1 Si2 153.40(5) . . ? C30 Y1 Si2 156.54(4) . . ? C3 Y1 Si2 164.55(5) . . ? N1 Y1 Si1 98.08(6) . . ? N5 Y1 Si1 25.96(5) . . ? N2 Y1 Si1 162.87(5) . . ? N3 Y1 Si1 111.41(5) . . ? C2 Y1 Si1 122.70(5) . . ? C30 Y1 Si1 124.01(5) . . ? C3 Y1 Si1 143.31(4) . . ? Si2 Y1 Si1 52.043(18) . . ? N5 Si1 C44 112.87(12) . . ? N5 Si1 C45 114.74(13) . . ? C44 Si1 C45 107.42(17) . . ? N5 Si1 C43 109.09(13) . . ? C44 Si1 C43 106.53(14) . . ? C45 Si1 C43 105.65(15) . . ? N5 Si1 Y1 34.82(6) . . ? C44 Si1 Y1 129.90(12) . . ? C45 Si1 Y1 120.65(12) . . ? C43 Si1 Y1 74.72(11) . . ? N5 Si2 C46 107.26(12) . . ? N5 Si2 C48 114.79(12) . . ? C46 Si2 C48 106.42(16) . . ? N5 Si2 C47 112.97(12) . . ? C46 Si2 C47 108.07(15) . . ? C48 Si2 C47 106.97(16) . . ? N5 Si2 Y1 34.95(7) . . ? C46 Si2 Y1 73.70(9) . . ? C48 Si2 Y1 135.26(10) . . ? C47 Si2 Y1 115.52(12) . . ? C2 N1 C6 117.08(18) . . ? C2 N1 Y1 112.16(14) . . ? C6 N1 Y1 129.77(15) . . ? C4 N2 C18 115.3(2) . . ? C4 N2 Y1 113.29(15) . . ? C18 N2 Y1 130.35(15) . . ? C30 N3 C31 120.28(19) . . ? C30 N3 Y1 108.23(14) . . ? C31 N3 Y1 127.08(15) . . ? C30 N4 C37 128.5(2) . . ? C30 N4 H4 116.5(16) . . ? C37 N4 H4 114.2(15) . . ? Si1 N5 Si2 121.79(12) . . ? Si1 N5 Y1 119.23(10) . . ? Si2 N5 Y1 118.95(11) . . ? C2 C1 H1A 120.0 . . ? C2 C1 H1B 120.0 . . ? H1A C1 H1B 120.0 . . ? C1 C2 N1 127.3(2) . . ? C1 C2 C3 117.4(2) . . ? N1 C2 C3 115.23(18) . . ? C1 C2 Y1 158.47(18) . . ? N1 C2 Y1 42.75(10) . . ? C3 C2 Y1 76.35(12) . . ? C30 C3 C4 112.63(17) . . ? C30 C3 C2 112.2(2) . . ? C4 C3 C2 115.94(17) . . ? C30 C3 Y1 74.70(12) . . ? C4 C3 Y1 76.33(12) . . ? C2 C3 Y1 74.11(12) . . ? C30 C3 H3 104.9 . . ? C4 C3 H3 104.9 . . ? C2 C3 H3 104.9 . . ? Y1 C3 H3 178.7 . . ? C5 C4 N2 126.9(2) . . ? C5 C4 C3 117.0(2) . . ? N2 C4 C3 116.1(2) . . ? C4 C5 H5A 120.0 . . ? C4 C5 H5B 120.0 . . ? H5A C5 H5B 120.0 . . ? C7 C6 C11 119.7(2) . . ? C7 C6 N1 120.3(2) . . ? C11 C6 N1 119.9(2) . . ? C8 C7 C6 118.9(2) . . ? C8 C7 C12 119.2(2) . . ? C6 C7 C12 121.7(2) . . ? C9 C8 C7 121.4(3) . . ? C9 C8 H8 119.3 . . ? C7 C8 H8 119.3 . . ? C10 C9 C8 119.5(3) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? C9 C10 C11 121.6(3) . . ? C9 C10 H10 119.2 . . ? C11 C10 H10 119.2 . . ? C10 C11 C6 118.7(2) . . ? C10 C11 C15 118.7(2) . . ? C6 C11 C15 122.6(2) . . ? C13 C12 C7 109.6(2) . . ? C13 C12 C14 110.0(2) . . ? C7 C12 C14 113.2(2) . . ? C13 C12 H12 107.9 . . ? C7 C12 H12 107.9 . . ? C14 C12 H12 107.9 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 C16 109.8(2) . . ? C11 C15 C17 113.2(2) . . ? C16 C15 C17 110.1(2) . . ? C11 C15 H15 107.8 . . ? C16 C15 H15 107.8 . . ? C17 C15 H15 107.8 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C23 C18 C19 119.9(2) . . ? C23 C18 N2 120.2(2) . . ? C19 C18 N2 119.8(2) . . ? C20 C19 C18 118.6(2) . . ? C20 C19 C24 119.7(2) . . ? C18 C19 C24 121.6(2) . . ? C21 C20 C19 121.5(2) . . ? C21 C20 H20 119.3 . . ? C19 C20 H20 119.3 . . ? C22 C21 C20 119.7(2) . . ? C22 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? C21 C22 C23 121.6(2) . . ? C21 C22 H22 119.2 . . ? C23 C22 H22 119.2 . . ? C22 C23 C18 118.4(2) . . ? C22 C23 C27 119.8(2) . . ? C18 C23 C27 121.8(2) . . ? C26 C24 C19 113.5(2) . . ? C26 C24 C25 110.3(3) . . ? C19 C24 C25 110.1(2) . . ? C26 C24 H24 107.6 . . ? C19 C24 H24 107.6 . . ? C25 C24 H24 107.6 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 C29 111.5(2) . . ? C23 C27 C28 111.4(2) . . ? C29 C27 C28 109.4(2) . . ? C23 C27 H27 108.1 . . ? C29 C27 H27 108.1 . . ? C28 C27 H27 108.1 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N3 C30 N4 124.0(2) . . ? N3 C30 C3 118.93(19) . . ? N4 C30 C3 117.1(2) . . ? N3 C30 Y1 47.57(11) . . ? N4 C30 Y1 155.36(18) . . ? C3 C30 Y1 76.03(12) . . ? N3 C31 C36 108.63(19) . . ? N3 C31 C32 112.3(2) . . ? C36 C31 C32 108.9(2) . . ? N3 C31 H31 109.0 . . ? C36 C31 H31 109.0 . . ? C32 C31 H31 109.0 . . ? C33 C32 C31 111.6(2) . . ? C33 C32 H32A 109.3 . . ? C31 C32 H32A 109.3 . . ? C33 C32 H32B 109.3 . . ? C31 C32 H32B 109.3 . . ? H32A C32 H32B 108.0 . . ? C34 C33 C32 111.4(2) . . ? C34 C33 H33A 109.3 . . ? C32 C33 H33A 109.3 . . ? C34 C33 H33B 109.3 . . ? C32 C33 H33B 109.3 . . ? H33A C33 H33B 108.0 . . ? C35 C34 C33 111.1(2) . . ? C35 C34 H34A 109.4 . . ? C33 C34 H34A 109.4 . . ? C35 C34 H34B 109.4 . . ? C33 C34 H34B 109.4 . . ? H34A C34 H34B 108.0 . . ? C34 C35 C36 111.4(3) . . ? C34 C35 H35A 109.3 . . ? C36 C35 H35A 109.3 . . ? C34 C35 H35B 109.3 . . ? C36 C35 H35B 109.3 . . ? H35A C35 H35B 108.0 . . ? C31 C36 C35 111.9(2) . . ? C31 C36 H36A 109.2 . . ? C35 C36 H36A 109.2 . . ? C31 C36 H36B 109.2 . . ? C35 C36 H36B 109.2 . . ? H36A C36 H36B 107.9 . . ? N4 C37 C42 112.1(2) . . ? N4 C37 C38 108.0(2) . . ? C42 C37 C38 110.5(2) . . ? N4 C37 H37 108.7 . . ? C42 C37 H37 108.7 . . ? C38 C37 H37 108.7 . . ? C37 C38 C39 110.7(2) . . ? C37 C38 H38A 109.5 . . ? C39 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? C39 C38 H38B 109.5 . . ? H38A C38 H38B 108.1 . . ? C40 C39 C38 111.3(2) . . ? C40 C39 H39A 109.4 . . ? C38 C39 H39A 109.4 . . ? C40 C39 H39B 109.4 . . ? C38 C39 H39B 109.4 . . ? H39A C39 H39B 108.0 . . ? C39 C40 C41 110.6(3) . . ? C39 C40 H40A 109.5 . . ? C41 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? C41 C40 H40B 109.5 . . ? H40A C40 H40B 108.1 . . ? C40 C41 C42 110.9(3) . . ? C40 C41 H41A 109.5 . . ? C42 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? C42 C41 H41B 109.5 . . ? H41A C41 H41B 108.0 . . ? C37 C42 C41 110.7(2) . . ? C37 C42 H42A 109.5 . . ? C41 C42 H42A 109.5 . . ? C37 C42 H42B 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 108.1 . . ? Si1 C43 H43A 109.5 . . ? Si1 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? Si1 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? Si1 C44 H44A 109.5 . . ? Si1 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? Si1 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? Si1 C45 H45A 109.5 . . ? Si1 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? Si1 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? Si2 C46 H46A 109.5 . . ? Si2 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? Si2 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? Si2 C47 H47A 109.5 . . ? Si2 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? Si2 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? Si2 C48 H48A 109.5 . . ? Si2 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? Si2 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Y1 Si1 N5 -141.50(12) . . . . ? N2 Y1 Si1 N5 -9.0(2) . . . . ? N3 Y1 Si1 N5 129.00(12) . . . . ? C2 Y1 Si1 N5 -146.71(12) . . . . ? C30 Y1 Si1 N5 152.46(12) . . . . ? C3 Y1 Si1 N5 -176.38(13) . . . . ? Si2 Y1 Si1 N5 1.16(11) . . . . ? N1 Y1 Si1 C44 146.86(14) . . . . ? N5 Y1 Si1 C44 -71.63(17) . . . . ? N2 Y1 Si1 C44 -80.7(2) . . . . ? N3 Y1 Si1 C44 57.37(14) . . . . ? C2 Y1 Si1 C44 141.66(14) . . . . ? C30 Y1 Si1 C44 80.83(14) . . . . ? C3 Y1 Si1 C44 111.99(14) . . . . ? Si2 Y1 Si1 C44 -70.47(13) . . . . ? N1 Y1 Si1 C45 -51.51(13) . . . . ? N5 Y1 Si1 C45 90.00(16) . . . . ? N2 Y1 Si1 C45 81.0(2) . . . . ? N3 Y1 Si1 C45 -141.00(13) . . . . ? C2 Y1 Si1 C45 -56.71(13) . . . . ? C30 Y1 Si1 C45 -117.54(13) . . . . ? C3 Y1 Si1 C45 -86.38(14) . . . . ? Si2 Y1 Si1 C45 91.16(12) . . . . ? N1 Y1 Si1 C43 47.89(12) . . . . ? N5 Y1 Si1 C43 -170.61(16) . . . . ? N2 Y1 Si1 C43 -179.64(19) . . . . ? N3 Y1 Si1 C43 -41.60(11) . . . . ? C2 Y1 Si1 C43 42.68(12) . . . . ? C30 Y1 Si1 C43 -18.14(12) . . . . ? C3 Y1 Si1 C43 13.01(13) . . . . ? Si2 Y1 Si1 C43 -169.45(11) . . . . ? N1 Y1 Si2 N5 56.97(13) . . . . ? N2 Y1 Si2 N5 175.64(12) . . . . ? N3 Y1 Si2 N5 -86.22(13) . . . . ? C2 Y1 Si2 N5 87.27(15) . . . . ? C30 Y1 Si2 N5 -90.27(16) . . . . ? C3 Y1 Si2 N5 173.33(19) . . . . ? Si1 Y1 Si2 N5 -1.16(11) . . . . ? N1 Y1 Si2 C46 -106.30(13) . . . . ? N5 Y1 Si2 C46 -163.26(15) . . . . ? N2 Y1 Si2 C46 12.38(12) . . . . ? N3 Y1 Si2 C46 110.51(12) . . . . ? C2 Y1 Si2 C46 -75.99(15) . . . . ? C30 Y1 Si2 C46 106.46(16) . . . . ? C3 Y1 Si2 C46 10.1(2) . . . . ? Si1 Y1 Si2 C46 -164.42(11) . . . . ? N1 Y1 Si2 C48 -9.21(18) . . . . ? N5 Y1 Si2 C48 -66.17(19) . . . . ? N2 Y1 Si2 C48 109.47(17) . . . . ? N3 Y1 Si2 C48 -152.39(17) . . . . ? C2 Y1 Si2 C48 21.1(2) . . . . ? C30 Y1 Si2 C48 -156.44(19) . . . . ? C3 Y1 Si2 C48 107.2(2) . . . . ? Si1 Y1 Si2 C48 -67.33(16) . . . . ? N1 Y1 Si2 C47 151.08(14) . . . . ? N5 Y1 Si2 C47 94.11(16) . . . . ? N2 Y1 Si2 C47 -90.25(13) . . . . ? N3 Y1 Si2 C47 7.89(14) . . . . ? C2 Y1 Si2 C47 -178.62(15) . . . . ? C30 Y1 Si2 C47 3.84(17) . . . . ? C3 Y1 Si2 C47 -92.6(2) . . . . ? Si1 Y1 Si2 C47 92.96(12) . . . . ? N5 Y1 N1 C2 172.44(14) . . . . ? N2 Y1 N1 C2 22.94(15) . . . . ? N3 Y1 N1 C2 -58.48(15) . . . . ? C30 Y1 N1 C2 -45.86(14) . . . . ? C3 Y1 N1 C2 -14.86(13) . . . . ? Si2 Y1 N1 C2 147.81(12) . . . . ? Si1 Y1 N1 C2 -169.63(14) . . . . ? N5 Y1 N1 C6 4.3(2) . . . . ? N2 Y1 N1 C6 -145.20(19) . . . . ? N3 Y1 N1 C6 133.37(19) . . . . ? C2 Y1 N1 C6 -168.1(3) . . . . ? C30 Y1 N1 C6 146.0(2) . . . . ? C3 Y1 N1 C6 177.0(2) . . . . ? Si2 Y1 N1 C6 -20.3(2) . . . . ? Si1 Y1 N1 C6 22.22(19) . . . . ? N1 Y1 N2 C4 -43.32(15) . . . . ? N5 Y1 N2 C4 177.92(13) . . . . ? N3 Y1 N2 C4 42.70(14) . . . . ? C2 Y1 N2 C4 -33.22(14) . . . . ? C30 Y1 N2 C4 19.73(14) . . . . ? C3 Y1 N2 C4 -5.66(13) . . . . ? Si2 Y1 N2 C4 175.11(13) . . . . ? Si1 Y1 N2 C4 -176.29(12) . . . . ? N1 Y1 N2 C18 149.11(18) . . . . ? N5 Y1 N2 C18 10.4(2) . . . . ? N3 Y1 N2 C18 -124.87(18) . . . . ? C2 Y1 N2 C18 159.21(19) . . . . ? C30 Y1 N2 C18 -147.84(19) . . . . ? C3 Y1 N2 C18 -173.2(2) . . . . ? Si2 Y1 N2 C18 7.54(19) . . . . ? Si1 Y1 N2 C18 16.1(3) . . . . ? N1 Y1 N3 C30 29.05(17) . . . . ? N5 Y1 N3 C30 151.18(15) . . . . ? N2 Y1 N3 C30 -65.09(16) . . . . ? C2 Y1 N3 C30 6.96(16) . . . . ? C3 Y1 N3 C30 -15.47(15) . . . . ? Si2 Y1 N3 C30 -176.07(13) . . . . ? Si1 Y1 N3 C30 126.39(15) . . . . ? N1 Y1 N3 C31 -127.04(18) . . . . ? N5 Y1 N3 C31 -4.9(2) . . . . ? N2 Y1 N3 C31 138.82(18) . . . . ? C2 Y1 N3 C31 -149.13(19) . . . . ? C30 Y1 N3 C31 -156.1(3) . . . . ? C3 Y1 N3 C31 -171.6(2) . . . . ? Si2 Y1 N3 C31 27.8(2) . . . . ? Si1 Y1 N3 C31 -29.70(18) . . . . ? C44 Si1 N5 Si2 -50.06(18) . . . . ? C45 Si1 N5 Si2 73.45(17) . . . . ? C43 Si1 N5 Si2 -168.26(14) . . . . ? Y1 Si1 N5 Si2 -177.9(2) . . . . ? C44 Si1 N5 Y1 127.80(14) . . . . ? C45 Si1 N5 Y1 -108.70(15) . . . . ? C43 Si1 N5 Y1 9.59(16) . . . . ? C46 Si2 N5 Si1 -165.32(14) . . . . ? C48 Si2 N5 Si1 -47.31(19) . . . . ? C47 Si2 N5 Si1 75.71(18) . . . . ? Y1 Si2 N5 Si1 177.9(2) . . . . ? C46 Si2 N5 Y1 16.82(15) . . . . ? C48 Si2 N5 Y1 134.83(15) . . . . ? C47 Si2 N5 Y1 -102.15(16) . . . . ? N1 Y1 N5 Si1 44.13(13) . . . . ? N2 Y1 N5 Si1 176.11(9) . . . . ? N3 Y1 N5 Si1 -63.10(13) . . . . ? C2 Y1 N5 Si1 49.40(16) . . . . ? C30 Y1 N5 Si1 -42.65(18) . . . . ? C3 Y1 N5 Si1 11.5(4) . . . . ? Si2 Y1 N5 Si1 -177.9(2) . . . . ? N1 Y1 N5 Si2 -137.95(10) . . . . ? N2 Y1 N5 Si2 -5.98(17) . . . . ? N3 Y1 N5 Si2 114.82(11) . . . . ? C2 Y1 N5 Si2 -132.69(10) . . . . ? C30 Y1 N5 Si2 135.27(11) . . . . ? C3 Y1 N5 Si2 -170.6(3) . . . . ? Si1 Y1 N5 Si2 177.9(2) . . . . ? C6 N1 C2 C1 15.8(3) . . . . ? Y1 N1 C2 C1 -154.0(2) . . . . ? C6 N1 C2 C3 -163.60(18) . . . . ? Y1 N1 C2 C3 26.6(2) . . . . ? C6 N1 C2 Y1 169.8(2) . . . . ? N1 Y1 C2 C1 72.1(5) . . . . ? N5 Y1 C2 C1 61.0(5) . . . . ? N2 Y1 C2 C1 -83.6(5) . . . . ? N3 Y1 C2 C1 -170.2(5) . . . . ? C30 Y1 C2 C1 -166.5(5) . . . . ? C3 Y1 C2 C1 -132.6(6) . . . . ? Si2 Y1 C2 C1 14.8(6) . . . . ? Si1 Y1 C2 C1 84.3(5) . . . . ? N5 Y1 C2 N1 -11.0(2) . . . . ? N2 Y1 C2 N1 -155.63(16) . . . . ? N3 Y1 C2 N1 117.73(16) . . . . ? C30 Y1 C2 N1 121.45(17) . . . . ? C3 Y1 C2 N1 155.3(2) . . . . ? Si2 Y1 C2 N1 -57.28(19) . . . . ? Si1 Y1 C2 N1 12.22(16) . . . . ? N1 Y1 C2 C3 -155.3(2) . . . . ? N5 Y1 C2 C3 -166.39(12) . . . . ? N2 Y1 C2 C3 49.02(12) . . . . ? N3 Y1 C2 C3 -37.62(12) . . . . ? C30 Y1 C2 C3 -33.90(11) . . . . ? Si2 Y1 C2 C3 147.38(10) . . . . ? Si1 Y1 C2 C3 -143.13(10) . . . . ? C1 C2 C3 C30 -132.1(2) . . . . ? N1 C2 C3 C30 47.4(3) . . . . ? Y1 C2 C3 C30 65.65(16) . . . . ? C1 C2 C3 C4 96.6(3) . . . . ? N1 C2 C3 C4 -83.9(2) . . . . ? Y1 C2 C3 C4 -65.68(17) . . . . ? C1 C2 C3 Y1 162.3(2) . . . . ? N1 C2 C3 Y1 -18.24(15) . . . . ? N1 Y1 C3 C30 -106.25(14) . . . . ? N5 Y1 C3 C30 -69.7(4) . . . . ? N2 Y1 C3 C30 123.29(14) . . . . ? N3 Y1 C3 C30 12.92(12) . . . . ? C2 Y1 C3 C30 -119.00(18) . . . . ? Si2 Y1 C3 C30 125.97(16) . . . . ? Si1 Y1 C3 C30 -61.32(15) . . . . ? N1 Y1 C3 C4 135.25(13) . . . . ? N5 Y1 C3 C4 171.8(3) . . . . ? N2 Y1 C3 C4 4.79(11) . . . . ? N3 Y1 C3 C4 -105.57(13) . . . . ? C2 Y1 C3 C4 122.50(17) . . . . ? C30 Y1 C3 C4 -118.49(17) . . . . ? Si2 Y1 C3 C4 7.5(2) . . . . ? Si1 Y1 C3 C4 -179.81(8) . . . . ? N1 Y1 C3 C2 12.75(11) . . . . ? N5 Y1 C3 C2 49.3(4) . . . . ? N2 Y1 C3 C2 -117.71(14) . . . . ? N3 Y1 C3 C2 131.92(14) . . . . ? C30 Y1 C3 C2 119.00(18) . . . . ? Si2 Y1 C3 C2 -115.03(17) . . . . ? Si1 Y1 C3 C2 57.69(14) . . . . ? C18 N2 C4 C5 -0.7(3) . . . . ? Y1 N2 C4 C5 -170.2(2) . . . . ? C18 N2 C4 C3 179.57(17) . . . . ? Y1 N2 C4 C3 10.0(2) . . . . ? C30 C3 C4 C5 106.6(2) . . . . ? C2 C3 C4 C5 -122.3(2) . . . . ? Y1 C3 C4 C5 173.3(2) . . . . ? C30 C3 C4 N2 -73.7(2) . . . . ? C2 C3 C4 N2 57.5(3) . . . . ? Y1 C3 C4 N2 -6.98(15) . . . . ? C2 N1 C6 C7 -107.8(2) . . . . ? Y1 N1 C6 C7 59.8(3) . . . . ? C2 N1 C6 C11 76.1(3) . . . . ? Y1 N1 C6 C11 -116.3(2) . . . . ? C11 C6 C7 C8 4.5(3) . . . . ? N1 C6 C7 C8 -171.6(2) . . . . ? C11 C6 C7 C12 -171.6(2) . . . . ? N1 C6 C7 C12 12.3(3) . . . . ? C6 C7 C8 C9 -1.8(4) . . . . ? C12 C7 C8 C9 174.4(2) . . . . ? C7 C8 C9 C10 -1.6(4) . . . . ? C8 C9 C10 C11 2.3(4) . . . . ? C9 C10 C11 C6 0.4(4) . . . . ? C9 C10 C11 C15 -178.0(2) . . . . ? C7 C6 C11 C10 -3.8(3) . . . . ? N1 C6 C11 C10 172.3(2) . . . . ? C7 C6 C11 C15 174.5(2) . . . . ? N1 C6 C11 C15 -9.4(3) . . . . ? C8 C7 C12 C13 -61.2(4) . . . . ? C6 C7 C12 C13 114.9(3) . . . . ? C8 C7 C12 C14 62.1(3) . . . . ? C6 C7 C12 C14 -121.8(3) . . . . ? C10 C11 C15 C16 62.9(3) . . . . ? C6 C11 C15 C16 -115.4(3) . . . . ? C10 C11 C15 C17 -60.6(3) . . . . ? C6 C11 C15 C17 121.0(3) . . . . ? C4 N2 C18 C23 87.1(3) . . . . ? Y1 N2 C18 C23 -105.6(2) . . . . ? C4 N2 C18 C19 -97.1(3) . . . . ? Y1 N2 C18 C19 70.3(3) . . . . ? C23 C18 C19 C20 4.9(4) . . . . ? N2 C18 C19 C20 -171.0(2) . . . . ? C23 C18 C19 C24 -173.0(2) . . . . ? N2 C18 C19 C24 11.1(4) . . . . ? C18 C19 C20 C21 -1.2(4) . . . . ? C24 C19 C20 C21 176.7(3) . . . . ? C19 C20 C21 C22 -2.8(5) . . . . ? C20 C21 C22 C23 3.2(4) . . . . ? C21 C22 C23 C18 0.5(4) . . . . ? C21 C22 C23 C27 179.9(3) . . . . ? C19 C18 C23 C22 -4.5(4) . . . . ? N2 C18 C23 C22 171.3(2) . . . . ? C19 C18 C23 C27 176.1(2) . . . . ? N2 C18 C23 C27 -8.1(4) . . . . ? C20 C19 C24 C26 48.8(4) . . . . ? C18 C19 C24 C26 -133.3(3) . . . . ? C20 C19 C24 C25 -75.3(3) . . . . ? C18 C19 C24 C25 102.5(3) . . . . ? C22 C23 C27 C29 -64.2(3) . . . . ? C18 C23 C27 C29 115.2(3) . . . . ? C22 C23 C27 C28 58.4(3) . . . . ? C18 C23 C27 C28 -122.3(3) . . . . ? C31 N3 C30 N4 7.7(4) . . . . ? Y1 N3 C30 N4 -150.3(2) . . . . ? C31 N3 C30 C3 -173.5(2) . . . . ? Y1 N3 C30 C3 28.5(3) . . . . ? C31 N3 C30 Y1 158.0(3) . . . . ? C37 N4 C30 N3 173.8(2) . . . . ? C37 N4 C30 C3 -5.1(4) . . . . ? C37 N4 C30 Y1 112.6(4) . . . . ? C4 C3 C30 N3 46.4(3) . . . . ? C2 C3 C30 N3 -86.6(3) . . . . ? Y1 C3 C30 N3 -21.3(2) . . . . ? C4 C3 C30 N4 -134.7(2) . . . . ? C2 C3 C30 N4 92.3(3) . . . . ? Y1 C3 C30 N4 157.6(2) . . . . ? C4 C3 C30 Y1 67.69(17) . . . . ? C2 C3 C30 Y1 -65.29(15) . . . . ? N1 Y1 C30 N3 -147.87(18) . . . . ? N5 Y1 C30 N3 -43.7(2) . . . . ? N2 Y1 C30 N3 109.66(17) . . . . ? C2 Y1 C30 N3 -171.3(2) . . . . ? C3 Y1 C30 N3 154.5(2) . . . . ? Si2 Y1 C30 N3 7.3(2) . . . . ? Si1 Y1 C30 N3 -64.70(17) . . . . ? N1 Y1 C30 N4 -68.0(4) . . . . ? N5 Y1 C30 N4 36.1(4) . . . . ? N2 Y1 C30 N4 -170.5(4) . . . . ? N3 Y1 C30 N4 79.8(4) . . . . ? C2 Y1 C30 N4 -91.4(4) . . . . ? C3 Y1 C30 N4 -125.7(4) . . . . ? Si2 Y1 C30 N4 87.1(4) . . . . ? Si1 Y1 C30 N4 15.1(4) . . . . ? N1 Y1 C30 C3 57.62(12) . . . . ? N5 Y1 C30 C3 161.74(13) . . . . ? N2 Y1 C30 C3 -44.85(12) . . . . ? N3 Y1 C30 C3 -154.5(2) . . . . ? C2 Y1 C30 C3 34.22(12) . . . . ? Si2 Y1 C30 C3 -147.21(11) . . . . ? Si1 Y1 C30 C3 140.78(11) . . . . ? C30 N3 C31 C36 -170.9(2) . . . . ? Y1 N3 C31 C36 -17.4(3) . . . . ? C30 N3 C31 C32 68.6(3) . . . . ? Y1 N3 C31 C32 -137.85(17) . . . . ? N3 C31 C32 C33 176.92(19) . . . . ? C36 C31 C32 C33 56.6(3) . . . . ? C31 C32 C33 C34 -56.3(3) . . . . ? C32 C33 C34 C35 54.5(3) . . . . ? C33 C34 C35 C36 -54.5(3) . . . . ? N3 C31 C36 C35 -179.3(2) . . . . ? C32 C31 C36 C35 -56.8(3) . . . . ? C34 C35 C36 C31 56.7(3) . . . . ? C30 N4 C37 C42 87.4(3) . . . . ? C30 N4 C37 C38 -150.7(3) . . . . ? N4 C37 C38 C39 -179.4(2) . . . . ? C42 C37 C38 C39 -56.4(3) . . . . ? C37 C38 C39 C40 56.4(3) . . . . ? C38 C39 C40 C41 -56.4(3) . . . . ? C39 C40 C41 C42 56.6(3) . . . . ? N4 C37 C42 C41 177.4(2) . . . . ? C38 C37 C42 C41 56.8(3) . . . . ? C40 C41 C42 C37 -57.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.366 _refine_diff_density_min -0.443 _refine_diff_density_rms 0.059 _database_code_depnum_ccdc_archive 'CCDC 976988' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_complex4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H80 Gd N5 Si2' _chemical_formula_sum 'C48 H80 Gd N5 Si2' _chemical_formula_weight 940.60 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' Gd Gd -0.1653 3.9035 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.5232(2) _cell_length_b 12.4364(2) _cell_length_c 17.5822(3) _cell_angle_alpha 84.5038(14) _cell_angle_beta 82.1385(15) _cell_angle_gamma 87.1562(14) _cell_volume 2482.80(8) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 49629 _cell_measurement_theta_min 3.3280 _cell_measurement_theta_max 29.4100 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.258 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 990 _exptl_absorpt_coefficient_mu 1.419 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.62055 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.4692 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 95541 _diffrn_reflns_av_R_equivalents 0.0256 _diffrn_reflns_av_unetI/netI 0.0116 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 25.50 _reflns_number_total 9195 _reflns_number_gt 8786 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro, Agilent Technologies' _computing_cell_refinement 'CrysAlisPro, Agilent Technologies' _computing_data_reduction 'CrysAlisPro, Agilent Technologies' _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^)+(0.0333P)^2^+2.1299P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9195 _refine_ls_number_parameters 523 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0224 _refine_ls_R_factor_gt 0.0210 _refine_ls_wR_factor_ref 0.0623 _refine_ls_wR_factor_gt 0.0617 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.087 _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 Gd1 Gd 0.703430(9) 0.762158(8) 0.733152(6) 0.02441(5) Uani 1 1 d . . . Si1 Si 0.55647(6) 0.57585(5) 0.65240(4) 0.03281(15) Uani 1 1 d . . . Si2 Si 0.60910(6) 0.78480(5) 0.55545(4) 0.03263(15) Uani 1 1 d . . . N1 N 0.82217(15) 0.64806(14) 0.79564(10) 0.0230(4) Uani 1 1 d . . . N2 N 0.80444(15) 0.90929(14) 0.75083(10) 0.0220(4) Uani 1 1 d . . . N3 N 0.60987(15) 0.79773(15) 0.85800(10) 0.0241(4) Uani 1 1 d . . . N4 N 0.66008(16) 0.74969(17) 0.98147(11) 0.0299(4) Uani 1 1 d D . . H4 H 0.5885(11) 0.740(2) 0.9983(15) 0.034(7) Uiso 1 1 d D . . N5 N 0.61591(16) 0.70083(15) 0.63803(11) 0.0268(4) Uani 1 1 d . . . C1 C 0.9839(2) 0.6678(2) 0.86828(15) 0.0349(5) Uani 1 1 d . . . H1A H 1.0241 0.6052 0.8509 0.042 Uiso 1 1 calc R . . H1B H 1.0163 0.7084 0.9021 0.042 Uiso 1 1 calc R . . C2 C 0.88037(18) 0.69912(17) 0.84485(12) 0.0231(4) Uani 1 1 d . . . C3 C 0.81692(17) 0.80088(17) 0.87652(11) 0.0215(4) Uani 1 1 d . . . H3 H 0.8534 0.8117 0.9229 0.026 Uiso 1 1 calc R . . C4 C 0.83515(18) 0.90727(17) 0.82408(12) 0.0224(4) Uani 1 1 d . . . C5 C 0.8804(2) 0.9884(2) 0.85451(14) 0.0345(5) Uani 1 1 d . . . H5A H 0.8940 1.0547 0.8250 0.041 Uiso 1 1 calc R . . H5B H 0.8984 0.9788 0.9053 0.041 Uiso 1 1 calc R . . C6 C 0.85979(18) 0.53969(17) 0.78094(13) 0.0247(4) Uani 1 1 d . . . C7 C 0.92124(19) 0.51823(19) 0.70901(14) 0.0303(5) Uani 1 1 d . . . C8 C 0.9423(2) 0.4106(2) 0.69274(16) 0.0404(6) Uani 1 1 d . . . H8 H 0.9811 0.3955 0.6441 0.048 Uiso 1 1 calc R . . C9 C 0.9078(3) 0.3265(2) 0.74609(17) 0.0432(6) Uani 1 1 d . . . H9 H 0.9213 0.2548 0.7336 0.052 Uiso 1 1 calc R . . C10 C 0.8533(2) 0.34775(19) 0.81783(16) 0.0370(6) Uani 1 1 d . . . H10 H 0.8324 0.2898 0.8547 0.044 Uiso 1 1 calc R . . C11 C 0.82830(19) 0.45333(18) 0.83716(14) 0.0282(5) Uani 1 1 d . . . C12 C 0.9715(2) 0.6080(2) 0.65100(15) 0.0368(5) Uani 1 1 d . . . H12 H 0.9491 0.6777 0.6729 0.044 Uiso 1 1 calc R . . C13 C 1.1044(3) 0.5973(4) 0.6392(3) 0.0801(13) Uani 1 1 d . . . H13A H 1.1336 0.6014 0.6880 0.120 Uiso 1 1 calc R . . H13B H 1.1356 0.6554 0.6025 0.120 Uiso 1 1 calc R . . H13C H 1.1288 0.5283 0.6196 0.120 Uiso 1 1 calc R . . C14 C 0.9245(3) 0.6115(3) 0.57419(17) 0.0546(8) Uani 1 1 d . . . H14A H 0.9448 0.5438 0.5516 0.082 Uiso 1 1 calc R . . H14B H 0.9588 0.6706 0.5398 0.082 Uiso 1 1 calc R . . H14C H 0.8400 0.6223 0.5822 0.082 Uiso 1 1 calc R . . C15 C 0.7700(2) 0.47120(19) 0.91790(14) 0.0317(5) Uani 1 1 d . . . H15 H 0.7591 0.5501 0.9214 0.038 Uiso 1 1 calc R . . C16 C 0.8501(3) 0.4266(2) 0.97713(16) 0.0442(6) Uani 1 1 d . . . H16A H 0.8601 0.3488 0.9761 0.066 Uiso 1 1 calc R . . H16B H 0.8151 0.4435 1.0282 0.066 Uiso 1 1 calc R . . H16C H 0.9259 0.4592 0.9646 0.066 Uiso 1 1 calc R . . C17 C 0.6492(2) 0.4214(2) 0.93750(16) 0.0441(6) Uani 1 1 d . . . H17A H 0.5964 0.4561 0.9034 0.066 Uiso 1 1 calc R . . H17B H 0.6181 0.4318 0.9905 0.066 Uiso 1 1 calc R . . H17C H 0.6567 0.3446 0.9310 0.066 Uiso 1 1 calc R . . C18 C 0.8211(2) 1.00928(17) 0.70345(12) 0.0246(4) Uani 1 1 d . . . C19 C 0.7260(2) 1.08411(18) 0.69796(13) 0.0302(5) Uani 1 1 d . . . C20 C 0.7396(3) 1.1737(2) 0.64345(15) 0.0400(6) Uani 1 1 d . . . H20 H 0.6763 1.2234 0.6386 0.048 Uiso 1 1 calc R . . C21 C 0.8444(3) 1.1902(2) 0.59690(15) 0.0439(7) Uani 1 1 d . . . H21 H 0.8514 1.2491 0.5591 0.053 Uiso 1 1 calc R . . C22 C 0.9388(3) 1.1206(2) 0.60575(14) 0.0385(6) Uani 1 1 d . . . H22 H 1.0109 1.1346 0.5753 0.046 Uiso 1 1 calc R . . C23 C 0.9303(2) 1.02941(18) 0.65890(12) 0.0290(5) Uani 1 1 d . . . C24 C 0.6110(2) 1.0724(2) 0.75131(16) 0.0367(5) Uani 1 1 d . . . H24 H 0.6109 0.9981 0.7773 0.044 Uiso 1 1 calc R . . C25 C 0.6026(3) 1.1507(3) 0.8137(2) 0.0590(8) Uani 1 1 d . . . H25A H 0.6671 1.1356 0.8436 0.089 Uiso 1 1 calc R . . H25B H 0.5289 1.1420 0.8472 0.089 Uiso 1 1 calc R . . H25C H 0.6063 1.2242 0.7898 0.089 Uiso 1 1 calc R . . C26 C 0.5034(3) 1.0872(3) 0.7092(2) 0.0658(9) Uani 1 1 d . . . H26A H 0.4991 1.1605 0.6850 0.099 Uiso 1 1 calc R . . H26B H 0.4334 1.0740 0.7458 0.099 Uiso 1 1 calc R . . H26C H 0.5091 1.0366 0.6701 0.099 Uiso 1 1 calc R . . C27 C 1.0367(2) 0.9548(2) 0.66654(14) 0.0348(5) Uani 1 1 d . . . H27 H 1.0152 0.8978 0.7086 0.042 Uiso 1 1 calc R . . C28 C 1.1393(3) 1.0153(3) 0.68737(19) 0.0573(8) Uani 1 1 d . . . H28A H 1.1623 1.0714 0.6466 0.086 Uiso 1 1 calc R . . H28B H 1.2051 0.9650 0.6934 0.086 Uiso 1 1 calc R . . H28C H 1.1153 1.0479 0.7353 0.086 Uiso 1 1 calc R . . C29 C 1.0758(3) 0.9003(3) 0.59264(17) 0.0479(7) Uani 1 1 d . . . H29A H 1.0128 0.8578 0.5815 0.072 Uiso 1 1 calc R . . H29B H 1.1442 0.8534 0.5992 0.072 Uiso 1 1 calc R . . H29C H 1.0953 0.9550 0.5503 0.072 Uiso 1 1 calc R . . C30 C 0.68707(18) 0.78226(17) 0.90652(12) 0.0230(4) Uani 1 1 d . . . C31 C 0.48342(18) 0.79177(19) 0.88586(13) 0.0281(5) Uani 1 1 d . . . H31 H 0.4693 0.7231 0.9186 0.034 Uiso 1 1 calc R . . C32 C 0.4371(2) 0.8862(2) 0.93263(15) 0.0357(5) Uani 1 1 d . . . H32A H 0.4767 0.8839 0.9787 0.043 Uiso 1 1 calc R . . H32B H 0.4550 0.9545 0.9016 0.043 Uiso 1 1 calc R . . C33 C 0.3049(2) 0.8819(2) 0.95690(18) 0.0489(7) Uani 1 1 d . . . H33A H 0.2877 0.8170 0.9921 0.059 Uiso 1 1 calc R . . H33B H 0.2776 0.9451 0.9846 0.059 Uiso 1 1 calc R . . C34 C 0.2398(2) 0.8800(3) 0.8878(2) 0.0564(8) Uani 1 1 d . . . H34A H 0.1560 0.8720 0.9055 0.068 Uiso 1 1 calc R . . H34B H 0.2492 0.9488 0.8558 0.068 Uiso 1 1 calc R . . C35 C 0.2848(2) 0.7885(3) 0.8402(2) 0.0518(7) Uani 1 1 d . . . H35A H 0.2454 0.7928 0.7939 0.062 Uiso 1 1 calc R . . H35B H 0.2663 0.7194 0.8700 0.062 Uiso 1 1 calc R . . C36 C 0.4176(2) 0.7928(2) 0.81635(15) 0.0377(6) Uani 1 1 d . . . H36A H 0.4447 0.7305 0.7876 0.045 Uiso 1 1 calc R . . H36B H 0.4352 0.8585 0.7822 0.045 Uiso 1 1 calc R . . C37 C 0.7399(2) 0.72054(19) 1.03942(12) 0.0283(5) Uani 1 1 d . . . H37 H 0.8132 0.6877 1.0137 0.034 Uiso 1 1 calc R . . C38 C 0.6812(2) 0.6366(2) 1.09940(14) 0.0393(6) Uani 1 1 d . . . H38A H 0.6659 0.5727 1.0743 0.047 Uiso 1 1 calc R . . H38B H 0.6058 0.6665 1.1227 0.047 Uiso 1 1 calc R . . C39 C 0.7589(3) 0.6036(3) 1.16239(16) 0.0531(8) Uani 1 1 d . . . H39A H 0.7176 0.5526 1.2016 0.064 Uiso 1 1 calc R . . H39B H 0.8309 0.5670 1.1398 0.064 Uiso 1 1 calc R . . C40 C 0.7903(3) 0.7009(3) 1.19998(17) 0.0651(10) Uani 1 1 d . . . H40A H 0.8434 0.6779 1.2380 0.078 Uiso 1 1 calc R . . H40B H 0.7191 0.7334 1.2270 0.078 Uiso 1 1 calc R . . C41 C 0.8491(3) 0.7843(3) 1.13977(18) 0.0569(8) Uani 1 1 d . . . H41A H 0.9238 0.7538 1.1159 0.068 Uiso 1 1 calc R . . H41B H 0.8657 0.8479 1.1648 0.068 Uiso 1 1 calc R . . C42 C 0.7705(2) 0.8184(2) 1.07751(15) 0.0409(6) Uani 1 1 d . . . H42A H 0.6984 0.8541 1.1007 0.049 Uiso 1 1 calc R . . H42B H 0.8110 0.8701 1.0385 0.049 Uiso 1 1 calc R . . C43 C 0.5595(3) 0.5218(3) 0.75560(18) 0.0551(8) Uani 1 1 d . . . H43A H 0.6366 0.5309 0.7699 0.083 Uiso 1 1 calc R . . H43B H 0.5424 0.4456 0.7616 0.083 Uiso 1 1 calc R . . H43C H 0.5011 0.5609 0.7886 0.083 Uiso 1 1 calc R . . C44 C 0.4003(3) 0.5788(3) 0.6349(2) 0.0549(8) Uani 1 1 d . . . H44A H 0.3548 0.6293 0.6669 0.082 Uiso 1 1 calc R . . H44B H 0.3695 0.5072 0.6477 0.082 Uiso 1 1 calc R . . H44C H 0.3953 0.6013 0.5811 0.082 Uiso 1 1 calc R . . C45 C 0.6382(3) 0.4722(2) 0.5936(2) 0.0633(9) Uani 1 1 d . . . H45A H 0.6461 0.4987 0.5395 0.095 Uiso 1 1 calc R . . H45B H 0.5956 0.4059 0.6014 0.095 Uiso 1 1 calc R . . H45C H 0.7154 0.4583 0.6093 0.095 Uiso 1 1 calc R . . C46 C 0.7153(3) 0.8936(2) 0.55567(18) 0.0493(7) Uani 1 1 d . . . H46A H 0.6916 0.9348 0.5997 0.074 Uiso 1 1 calc R . . H46B H 0.7163 0.9413 0.5086 0.074 Uiso 1 1 calc R . . H46C H 0.7930 0.8613 0.5588 0.074 Uiso 1 1 calc R . . C47 C 0.4603(3) 0.8505(3) 0.5501(2) 0.0647(10) Uani 1 1 d . . . H47A H 0.4055 0.7963 0.5440 0.097 Uiso 1 1 calc R . . H47B H 0.4642 0.9048 0.5065 0.097 Uiso 1 1 calc R . . H47C H 0.4343 0.8846 0.5972 0.097 Uiso 1 1 calc R . . C48 C 0.6522(4) 0.7196(3) 0.46403(17) 0.0613(9) Uani 1 1 d . . . H48A H 0.7305 0.6869 0.4638 0.092 Uiso 1 1 calc R . . H48B H 0.6513 0.7737 0.4205 0.092 Uiso 1 1 calc R . . H48C H 0.5973 0.6643 0.4603 0.092 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.02587(7) 0.02450(7) 0.02345(7) 0.00065(4) -0.00685(4) -0.00225(4) Si1 0.0323(3) 0.0312(3) 0.0374(4) 0.0034(3) -0.0158(3) -0.0074(3) Si2 0.0405(4) 0.0293(3) 0.0308(3) 0.0023(3) -0.0164(3) -0.0056(3) N1 0.0214(9) 0.0204(9) 0.0279(9) -0.0002(7) -0.0071(7) -0.0015(7) N2 0.0262(9) 0.0192(8) 0.0204(9) 0.0008(7) -0.0033(7) -0.0030(7) N3 0.0200(9) 0.0269(9) 0.0244(9) 0.0027(7) -0.0026(7) -0.0021(7) N4 0.0229(10) 0.0419(11) 0.0225(9) 0.0065(8) -0.0008(7) -0.0023(8) N5 0.0286(9) 0.0278(10) 0.0261(9) -0.0019(7) -0.0110(7) -0.0024(8) C1 0.0268(12) 0.0308(12) 0.0502(15) -0.0061(11) -0.0153(10) 0.0003(9) C2 0.0201(10) 0.0204(10) 0.0281(11) 0.0025(8) -0.0033(8) -0.0032(8) C3 0.0217(10) 0.0248(10) 0.0178(10) 0.0015(8) -0.0040(8) -0.0030(8) C4 0.0211(10) 0.0238(10) 0.0214(10) -0.0012(8) 0.0000(8) -0.0010(8) C5 0.0492(15) 0.0309(12) 0.0242(11) -0.0022(9) -0.0050(10) -0.0105(11) C6 0.0214(10) 0.0233(10) 0.0314(11) -0.0026(9) -0.0099(8) -0.0010(8) C7 0.0251(11) 0.0329(12) 0.0340(12) -0.0042(10) -0.0081(9) 0.0011(9) C8 0.0414(14) 0.0405(14) 0.0409(14) -0.0140(11) -0.0073(11) 0.0076(11) C9 0.0532(16) 0.0267(13) 0.0539(17) -0.0124(12) -0.0188(13) 0.0067(11) C10 0.0433(14) 0.0236(12) 0.0463(15) 0.0006(10) -0.0161(11) -0.0021(10) C11 0.0275(11) 0.0248(11) 0.0341(12) -0.0006(9) -0.0118(9) -0.0009(9) C12 0.0320(13) 0.0396(14) 0.0365(13) -0.0030(11) 0.0033(10) -0.0007(10) C13 0.0348(17) 0.094(3) 0.103(3) 0.031(2) -0.0045(18) -0.0114(17) C14 0.0603(19) 0.063(2) 0.0382(16) 0.0023(14) -0.0014(13) -0.0037(15) C15 0.0379(13) 0.0253(11) 0.0316(12) 0.0054(9) -0.0081(10) -0.0039(9) C16 0.0494(16) 0.0474(16) 0.0383(14) 0.0035(12) -0.0183(12) -0.0061(12) C17 0.0405(14) 0.0510(16) 0.0391(14) 0.0114(12) -0.0077(11) -0.0075(12) C18 0.0352(12) 0.0212(10) 0.0182(10) -0.0022(8) -0.0052(8) -0.0049(9) C19 0.0407(13) 0.0215(11) 0.0289(12) -0.0003(9) -0.0075(10) -0.0033(9) C20 0.0557(16) 0.0246(12) 0.0387(14) 0.0049(10) -0.0086(12) 0.0004(11) C21 0.074(2) 0.0282(13) 0.0278(13) 0.0073(10) -0.0040(12) -0.0091(13) C22 0.0546(16) 0.0358(13) 0.0229(12) -0.0007(10) 0.0052(11) -0.0139(12) C23 0.0404(13) 0.0285(11) 0.0183(10) -0.0036(9) -0.0010(9) -0.0084(10) C24 0.0357(13) 0.0250(12) 0.0470(15) 0.0024(10) -0.0027(11) 0.0025(10) C25 0.0540(18) 0.0581(19) 0.061(2) -0.0170(16) 0.0136(15) -0.0046(15) C26 0.0437(17) 0.080(2) 0.074(2) 0.0017(19) -0.0144(16) 0.0029(16) C27 0.0345(13) 0.0405(14) 0.0271(12) -0.0003(10) 0.0041(10) -0.0070(10) C28 0.0473(17) 0.077(2) 0.0523(18) -0.0156(16) -0.0129(14) -0.0123(16) C29 0.0430(15) 0.0530(17) 0.0474(16) -0.0165(13) 0.0044(12) -0.0034(13) C30 0.0230(10) 0.0219(10) 0.0229(10) 0.0004(8) -0.0008(8) -0.0001(8) C31 0.0203(10) 0.0302(12) 0.0312(12) 0.0066(9) -0.0007(9) -0.0010(9) C32 0.0315(13) 0.0369(13) 0.0363(13) 0.0005(10) -0.0002(10) 0.0046(10) C33 0.0347(14) 0.0446(16) 0.0586(18) 0.0074(13) 0.0118(12) 0.0110(12) C34 0.0250(13) 0.0538(18) 0.086(2) 0.0079(16) -0.0038(14) 0.0041(12) C35 0.0271(13) 0.0552(18) 0.074(2) 0.0049(15) -0.0146(13) -0.0066(12) C36 0.0280(12) 0.0445(14) 0.0412(14) 0.0016(11) -0.0095(10) -0.0045(10) C37 0.0285(11) 0.0338(12) 0.0211(11) 0.0029(9) -0.0035(9) 0.0036(9) C38 0.0375(13) 0.0470(15) 0.0292(13) 0.0123(11) -0.0010(10) -0.0005(11) C39 0.0494(17) 0.069(2) 0.0348(15) 0.0227(14) -0.0062(12) 0.0069(14) C40 0.064(2) 0.103(3) 0.0285(15) -0.0007(16) -0.0176(14) 0.0172(19) C41 0.063(2) 0.071(2) 0.0433(17) -0.0162(15) -0.0230(15) 0.0008(16) C42 0.0491(15) 0.0417(14) 0.0330(13) -0.0077(11) -0.0079(11) 0.0044(12) C43 0.0543(18) 0.0588(19) 0.0526(18) 0.0241(15) -0.0224(14) -0.0192(15) C44 0.0406(16) 0.0577(19) 0.070(2) 0.0104(15) -0.0259(14) -0.0175(14) C45 0.077(2) 0.0319(15) 0.083(2) -0.0123(15) -0.0131(19) -0.0024(15) C46 0.0543(17) 0.0398(15) 0.0560(18) 0.0039(13) -0.0159(14) -0.0142(13) C47 0.0558(19) 0.0513(19) 0.089(3) 0.0171(17) -0.0361(18) -0.0001(15) C48 0.096(3) 0.060(2) 0.0320(15) -0.0017(14) -0.0202(16) -0.0111(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 N1 2.2389(17) . ? Gd1 N5 2.2756(18) . ? Gd1 N2 2.2844(17) . ? Gd1 N3 2.3807(18) . ? Gd1 C2 3.045(2) . ? Gd1 Si2 3.4282(6) . ? Gd1 Si1 3.4539(7) . ? Si1 N5 1.7123(19) . ? Si1 C44 1.865(3) . ? Si1 C45 1.867(3) . ? Si1 C43 1.878(3) . ? Si2 N5 1.7139(19) . ? Si2 C48 1.865(3) . ? Si2 C46 1.870(3) . ? Si2 C47 1.872(3) . ? N1 C2 1.381(3) . ? N1 C6 1.432(3) . ? N2 C4 1.379(3) . ? N2 C18 1.435(3) . ? N3 C30 1.310(3) . ? N3 C31 1.476(3) . ? N4 C30 1.340(3) . ? N4 C37 1.473(3) . ? N4 H4 0.848(10) . ? C1 C2 1.343(3) . ? C1 H1A 0.9400 . ? C1 H1B 0.9400 . ? C2 C3 1.542(3) . ? C3 C30 1.538(3) . ? C3 C4 1.544(3) . ? C3 H3 0.9900 . ? C4 C5 1.344(3) . ? C5 H5A 0.9400 . ? C5 H5B 0.9400 . ? C6 C7 1.405(3) . ? C6 C11 1.414(3) . ? C7 C8 1.398(3) . ? C7 C12 1.519(3) . ? C8 C9 1.372(4) . ? C8 H8 0.9400 . ? C9 C10 1.373(4) . ? C9 H9 0.9400 . ? C10 C11 1.394(3) . ? C10 H10 0.9400 . ? C11 C15 1.517(3) . ? C12 C13 1.518(4) . ? C12 C14 1.518(4) . ? C12 H12 0.9900 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 H13C 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 C16 1.532(3) . ? C15 C17 1.534(4) . ? C15 H15 0.9900 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 C23 1.409(3) . ? C18 C19 1.409(3) . ? C19 C20 1.399(3) . ? C19 C24 1.520(3) . ? C20 C21 1.376(4) . ? C20 H20 0.9400 . ? C21 C22 1.372(4) . ? C21 H21 0.9400 . ? C22 C23 1.397(3) . ? C22 H22 0.9400 . ? C23 C27 1.514(4) . ? C24 C26 1.524(4) . ? C24 C25 1.525(4) . ? C24 H24 0.9900 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C25 H25C 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C26 H26C 0.9700 . ? C27 C29 1.526(4) . ? C27 C28 1.535(4) . ? C27 H27 0.9900 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 H28C 0.9700 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C29 H29C 0.9700 . ? C31 C36 1.523(3) . ? C31 C32 1.531(3) . ? C31 H31 0.9900 . ? C32 C33 1.526(3) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C33 C34 1.515(5) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C34 C35 1.507(5) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C35 C36 1.532(4) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C37 C42 1.522(4) . ? C37 C38 1.525(3) . ? C37 H37 0.9900 . ? C38 C39 1.532(4) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C39 C40 1.514(5) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C40 C41 1.524(5) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C41 C42 1.531(4) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C43 H43C 0.9700 . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C44 H44C 0.9700 . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C45 H45C 0.9700 . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C46 H46C 0.9700 . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C47 H47C 0.9700 . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C48 H48C 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Gd1 N5 118.53(7) . . ? N1 Gd1 N2 92.65(6) . . ? N5 Gd1 N2 137.78(6) . . ? N1 Gd1 N3 85.57(6) . . ? N5 Gd1 N3 126.08(6) . . ? N2 Gd1 N3 80.84(6) . . ? N1 Gd1 C2 24.81(6) . . ? N5 Gd1 C2 143.04(6) . . ? N2 Gd1 C2 69.74(6) . . ? N3 Gd1 C2 73.21(6) . . ? N1 Gd1 Si2 135.96(5) . . ? N5 Gd1 Si2 26.25(5) . . ? N2 Gd1 Si2 111.63(4) . . ? N3 Gd1 Si2 132.74(4) . . ? C2 Gd1 Si2 153.96(4) . . ? N1 Gd1 Si1 98.92(5) . . ? N5 Gd1 Si1 25.60(5) . . ? N2 Gd1 Si1 163.25(4) . . ? N3 Gd1 Si1 111.96(4) . . ? C2 Gd1 Si1 123.30(4) . . ? Si2 Gd1 Si1 51.842(16) . . ? N5 Si1 C44 113.03(12) . . ? N5 Si1 C45 114.38(13) . . ? C44 Si1 C45 107.70(17) . . ? N5 Si1 C43 108.96(12) . . ? C44 Si1 C43 106.71(15) . . ? C45 Si1 C43 105.53(17) . . ? N5 Si1 Gd1 35.05(6) . . ? C44 Si1 Gd1 129.39(12) . . ? C45 Si1 Gd1 120.98(12) . . ? C43 Si1 Gd1 74.23(10) . . ? N5 Si2 C48 114.93(13) . . ? N5 Si2 C46 107.04(12) . . ? C48 Si2 C46 106.46(16) . . ? N5 Si2 C47 112.93(14) . . ? C48 Si2 C47 107.05(18) . . ? C46 Si2 C47 108.06(15) . . ? N5 Si2 Gd1 35.96(6) . . ? C48 Si2 Gd1 135.11(12) . . ? C46 Si2 Gd1 72.33(10) . . ? C47 Si2 Gd1 116.03(13) . . ? C2 N1 C6 117.72(17) . . ? C2 N1 Gd1 112.33(13) . . ? C6 N1 Gd1 128.83(13) . . ? C4 N2 C18 115.95(17) . . ? C4 N2 Gd1 113.22(13) . . ? C18 N2 Gd1 129.74(13) . . ? C30 N3 C31 120.44(18) . . ? C30 N3 Gd1 108.61(13) . . ? C31 N3 Gd1 126.32(14) . . ? C30 N4 C37 128.47(19) . . ? C30 N4 H4 117.6(19) . . ? C37 N4 H4 113.8(18) . . ? Si1 N5 Si2 122.83(11) . . ? Si1 N5 Gd1 119.35(10) . . ? Si2 N5 Gd1 117.80(10) . . ? C2 C1 H1A 120.0 . . ? C2 C1 H1B 120.0 . . ? H1A C1 H1B 120.0 . . ? C1 C2 N1 126.6(2) . . ? C1 C2 C3 117.9(2) . . ? N1 C2 C3 115.51(17) . . ? C1 C2 Gd1 158.07(18) . . ? N1 C2 Gd1 42.86(9) . . ? C3 C2 Gd1 76.73(11) . . ? C30 C3 C2 112.14(17) . . ? C30 C3 C4 112.70(16) . . ? C2 C3 C4 115.89(17) . . ? C30 C3 H3 105.0 . . ? C2 C3 H3 105.0 . . ? C4 C3 H3 105.0 . . ? C5 C4 N2 126.6(2) . . ? C5 C4 C3 116.43(19) . . ? N2 C4 C3 116.95(18) . . ? C4 C5 H5A 120.0 . . ? C4 C5 H5B 120.0 . . ? H5A C5 H5B 120.0 . . ? C7 C6 C11 119.9(2) . . ? C7 C6 N1 120.2(2) . . ? C11 C6 N1 119.8(2) . . ? C8 C7 C6 118.6(2) . . ? C8 C7 C12 119.4(2) . . ? C6 C7 C12 121.8(2) . . ? C9 C8 C7 121.5(2) . . ? C9 C8 H8 119.2 . . ? C7 C8 H8 119.2 . . ? C8 C9 C10 119.7(2) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? C9 C10 C11 121.5(2) . . ? C9 C10 H10 119.3 . . ? C11 C10 H10 119.3 . . ? C10 C11 C6 118.6(2) . . ? C10 C11 C15 118.8(2) . . ? C6 C11 C15 122.6(2) . . ? C13 C12 C14 110.3(3) . . ? C13 C12 C7 110.1(2) . . ? C14 C12 C7 113.1(2) . . ? C13 C12 H12 107.7 . . ? C14 C12 H12 107.7 . . ? C7 C12 H12 107.7 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 C16 110.0(2) . . ? C11 C15 C17 113.1(2) . . ? C16 C15 C17 110.1(2) . . ? C11 C15 H15 107.8 . . ? C16 C15 H15 107.8 . . ? C17 C15 H15 107.8 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C23 C18 C19 120.2(2) . . ? C23 C18 N2 119.9(2) . . ? C19 C18 N2 119.8(2) . . ? C20 C19 C18 118.8(2) . . ? C20 C19 C24 119.2(2) . . ? C18 C19 C24 122.0(2) . . ? C21 C20 C19 120.9(2) . . ? C21 C20 H20 119.5 . . ? C19 C20 H20 119.5 . . ? C22 C21 C20 119.9(2) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C21 C22 C23 121.7(2) . . ? C21 C22 H22 119.2 . . ? C23 C22 H22 119.2 . . ? C22 C23 C18 118.3(2) . . ? C22 C23 C27 119.8(2) . . ? C18 C23 C27 122.0(2) . . ? C19 C24 C26 113.4(2) . . ? C19 C24 C25 110.5(2) . . ? C26 C24 C25 110.1(3) . . ? C19 C24 H24 107.5 . . ? C26 C24 H24 107.5 . . ? C25 C24 H24 107.5 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 C29 111.4(2) . . ? C23 C27 C28 111.5(2) . . ? C29 C27 C28 109.5(2) . . ? C23 C27 H27 108.1 . . ? C29 C27 H27 108.1 . . ? C28 C27 H27 108.1 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N3 C30 N4 123.84(19) . . ? N3 C30 C3 118.83(18) . . ? N4 C30 C3 117.33(18) . . ? N3 C31 C36 108.42(18) . . ? N3 C31 C32 112.40(19) . . ? C36 C31 C32 109.09(19) . . ? N3 C31 H31 109.0 . . ? C36 C31 H31 109.0 . . ? C32 C31 H31 109.0 . . ? C33 C32 C31 111.5(2) . . ? C33 C32 H32A 109.3 . . ? C31 C32 H32A 109.3 . . ? C33 C32 H32B 109.3 . . ? C31 C32 H32B 109.3 . . ? H32A C32 H32B 108.0 . . ? C34 C33 C32 111.4(2) . . ? C34 C33 H33A 109.3 . . ? C32 C33 H33A 109.3 . . ? C34 C33 H33B 109.3 . . ? C32 C33 H33B 109.3 . . ? H33A C33 H33B 108.0 . . ? C35 C34 C33 111.3(2) . . ? C35 C34 H34A 109.4 . . ? C33 C34 H34A 109.4 . . ? C35 C34 H34B 109.4 . . ? C33 C34 H34B 109.4 . . ? H34A C34 H34B 108.0 . . ? C34 C35 C36 111.2(2) . . ? C34 C35 H35A 109.4 . . ? C36 C35 H35A 109.4 . . ? C34 C35 H35B 109.4 . . ? C36 C35 H35B 109.4 . . ? H35A C35 H35B 108.0 . . ? C31 C36 C35 111.8(2) . . ? C31 C36 H36A 109.2 . . ? C35 C36 H36A 109.2 . . ? C31 C36 H36B 109.2 . . ? C35 C36 H36B 109.2 . . ? H36A C36 H36B 107.9 . . ? N4 C37 C42 112.10(19) . . ? N4 C37 C38 107.99(19) . . ? C42 C37 C38 110.6(2) . . ? N4 C37 H37 108.7 . . ? C42 C37 H37 108.7 . . ? C38 C37 H37 108.7 . . ? C37 C38 C39 110.8(2) . . ? C37 C38 H38A 109.5 . . ? C39 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? C39 C38 H38B 109.5 . . ? H38A C38 H38B 108.1 . . ? C40 C39 C38 111.4(3) . . ? C40 C39 H39A 109.4 . . ? C38 C39 H39A 109.4 . . ? C40 C39 H39B 109.4 . . ? C38 C39 H39B 109.4 . . ? H39A C39 H39B 108.0 . . ? C39 C40 C41 110.6(2) . . ? C39 C40 H40A 109.5 . . ? C41 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? C41 C40 H40B 109.5 . . ? H40A C40 H40B 108.1 . . ? C40 C41 C42 110.8(3) . . ? C40 C41 H41A 109.5 . . ? C42 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? C42 C41 H41B 109.5 . . ? H41A C41 H41B 108.1 . . ? C37 C42 C41 110.6(2) . . ? C37 C42 H42A 109.5 . . ? C41 C42 H42A 109.5 . . ? C37 C42 H42B 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 108.1 . . ? Si1 C43 H43A 109.5 . . ? Si1 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? Si1 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? Si1 C44 H44A 109.5 . . ? Si1 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? Si1 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? Si1 C45 H45A 109.5 . . ? Si1 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? Si1 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? Si2 C46 H46A 109.5 . . ? Si2 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? Si2 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? Si2 C47 H47A 109.5 . . ? Si2 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? Si2 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? Si2 C48 H48A 109.5 . . ? Si2 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? Si2 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Gd1 Si1 N5 -142.32(12) . . . . ? N2 Gd1 Si1 N5 -9.2(2) . . . . ? N3 Gd1 Si1 N5 128.88(12) . . . . ? C2 Gd1 Si1 N5 -147.30(12) . . . . ? Si2 Gd1 Si1 N5 1.02(11) . . . . ? N1 Gd1 Si1 C44 144.47(14) . . . . ? N5 Gd1 Si1 C44 -73.20(18) . . . . ? N2 Gd1 Si1 C44 -82.4(2) . . . . ? N3 Gd1 Si1 C44 55.68(15) . . . . ? C2 Gd1 Si1 C44 139.50(14) . . . . ? Si2 Gd1 Si1 C44 -72.19(14) . . . . ? N1 Gd1 Si1 C45 -53.34(15) . . . . ? N5 Gd1 Si1 C45 88.99(18) . . . . ? N2 Gd1 Si1 C45 79.8(2) . . . . ? N3 Gd1 Si1 C45 -142.13(14) . . . . ? C2 Gd1 Si1 C45 -58.32(15) . . . . ? Si2 Gd1 Si1 C45 90.00(14) . . . . ? N1 Gd1 Si1 C43 45.58(13) . . . . ? N5 Gd1 Si1 C43 -172.10(17) . . . . ? N2 Gd1 Si1 C43 178.70(19) . . . . ? N3 Gd1 Si1 C43 -43.22(13) . . . . ? C2 Gd1 Si1 C43 40.60(13) . . . . ? Si2 Gd1 Si1 C43 -171.08(12) . . . . ? N1 Gd1 Si2 N5 57.07(13) . . . . ? N2 Gd1 Si2 N5 175.86(12) . . . . ? N3 Gd1 Si2 N5 -86.49(13) . . . . ? C2 Gd1 Si2 N5 88.00(14) . . . . ? Si1 Gd1 Si2 N5 -0.99(11) . . . . ? N1 Gd1 Si2 C48 -11.42(18) . . . . ? N5 Gd1 Si2 C48 -68.5(2) . . . . ? N2 Gd1 Si2 C48 107.37(17) . . . . ? N3 Gd1 Si2 C48 -154.98(17) . . . . ? C2 Gd1 Si2 C48 19.50(19) . . . . ? Si1 Gd1 Si2 C48 -69.48(16) . . . . ? N1 Gd1 Si2 C46 -107.26(13) . . . . ? N5 Gd1 Si2 C46 -164.33(16) . . . . ? N2 Gd1 Si2 C46 11.52(12) . . . . ? N3 Gd1 Si2 C46 109.18(12) . . . . ? C2 Gd1 Si2 C46 -76.34(14) . . . . ? Si1 Gd1 Si2 C46 -165.32(11) . . . . ? N1 Gd1 Si2 C47 150.82(14) . . . . ? N5 Gd1 Si2 C47 93.75(16) . . . . ? N2 Gd1 Si2 C47 -90.40(13) . . . . ? N3 Gd1 Si2 C47 7.26(14) . . . . ? C2 Gd1 Si2 C47 -178.26(15) . . . . ? Si1 Gd1 Si2 C47 92.76(12) . . . . ? N5 Gd1 N1 C2 172.46(13) . . . . ? N2 Gd1 N1 C2 22.11(14) . . . . ? N3 Gd1 N1 C2 -58.48(14) . . . . ? Si2 Gd1 N1 C2 147.47(12) . . . . ? Si1 Gd1 N1 C2 -170.05(13) . . . . ? N5 Gd1 N1 C6 5.0(2) . . . . ? N2 Gd1 N1 C6 -145.36(18) . . . . ? N3 Gd1 N1 C6 134.05(18) . . . . ? C2 Gd1 N1 C6 -167.5(3) . . . . ? Si2 Gd1 N1 C6 -20.0(2) . . . . ? Si1 Gd1 N1 C6 22.49(18) . . . . ? N1 Gd1 N2 C4 -42.77(14) . . . . ? N5 Gd1 N2 C4 177.54(13) . . . . ? N3 Gd1 N2 C4 42.31(14) . . . . ? C2 Gd1 N2 C4 -33.08(13) . . . . ? Si2 Gd1 N2 C4 174.81(12) . . . . ? Si1 Gd1 N2 C4 -176.56(11) . . . . ? N1 Gd1 N2 C18 149.89(18) . . . . ? N5 Gd1 N2 C18 10.2(2) . . . . ? N3 Gd1 N2 C18 -125.03(18) . . . . ? C2 Gd1 N2 C18 159.59(19) . . . . ? Si2 Gd1 N2 C18 7.47(19) . . . . ? Si1 Gd1 N2 C18 16.1(3) . . . . ? N1 Gd1 N3 C30 28.42(14) . . . . ? N5 Gd1 N3 C30 150.85(13) . . . . ? N2 Gd1 N3 C30 -64.99(14) . . . . ? C2 Gd1 N3 C30 6.48(13) . . . . ? Si2 Gd1 N3 C30 -176.05(11) . . . . ? Si1 Gd1 N3 C30 126.26(13) . . . . ? N1 Gd1 N3 C31 -127.23(17) . . . . ? N5 Gd1 N3 C31 -4.80(19) . . . . ? N2 Gd1 N3 C31 139.36(17) . . . . ? C2 Gd1 N3 C31 -149.17(17) . . . . ? Si2 Gd1 N3 C31 28.30(19) . . . . ? Si1 Gd1 N3 C31 -29.40(17) . . . . ? C44 Si1 N5 Si2 -51.61(19) . . . . ? C45 Si1 N5 Si2 72.13(19) . . . . ? C43 Si1 N5 Si2 -170.06(15) . . . . ? Gd1 Si1 N5 Si2 -178.1(2) . . . . ? C44 Si1 N5 Gd1 126.49(15) . . . . ? C45 Si1 N5 Gd1 -109.77(16) . . . . ? C43 Si1 N5 Gd1 8.04(17) . . . . ? C48 Si2 N5 Si1 -48.3(2) . . . . ? C46 Si2 N5 Si1 -166.26(15) . . . . ? C47 Si2 N5 Si1 74.94(19) . . . . ? Gd1 Si2 N5 Si1 178.1(2) . . . . ? C48 Si2 N5 Gd1 133.61(15) . . . . ? C46 Si2 N5 Gd1 15.61(16) . . . . ? C47 Si2 N5 Gd1 -103.19(16) . . . . ? N1 Gd1 N5 Si1 43.42(13) . . . . ? N2 Gd1 N5 Si1 176.07(8) . . . . ? N3 Gd1 N5 Si1 -63.28(13) . . . . ? C2 Gd1 N5 Si1 48.67(17) . . . . ? Si2 Gd1 N5 Si1 -178.2(2) . . . . ? N1 Gd1 N5 Si2 -138.39(10) . . . . ? N2 Gd1 N5 Si2 -5.74(17) . . . . ? N3 Gd1 N5 Si2 114.91(11) . . . . ? C2 Gd1 N5 Si2 -133.13(10) . . . . ? Si1 Gd1 N5 Si2 178.2(2) . . . . ? C6 N1 C2 C1 15.0(3) . . . . ? Gd1 N1 C2 C1 -154.0(2) . . . . ? C6 N1 C2 C3 -163.67(18) . . . . ? Gd1 N1 C2 C3 27.3(2) . . . . ? C6 N1 C2 Gd1 169.0(2) . . . . ? N1 Gd1 C2 C1 70.7(4) . . . . ? N5 Gd1 C2 C1 59.6(5) . . . . ? N2 Gd1 C2 C1 -85.7(4) . . . . ? N3 Gd1 C2 C1 -171.9(4) . . . . ? Si2 Gd1 C2 C1 12.3(5) . . . . ? Si1 Gd1 C2 C1 82.5(4) . . . . ? N5 Gd1 C2 N1 -11.06(19) . . . . ? N2 Gd1 C2 N1 -156.37(15) . . . . ? N3 Gd1 C2 N1 117.41(15) . . . . ? Si2 Gd1 C2 N1 -58.37(18) . . . . ? Si1 Gd1 C2 N1 11.79(16) . . . . ? N1 Gd1 C2 C3 -154.8(2) . . . . ? N5 Gd1 C2 C3 -165.85(11) . . . . ? N2 Gd1 C2 C3 48.83(11) . . . . ? N3 Gd1 C2 C3 -37.39(11) . . . . ? Si2 Gd1 C2 C3 146.84(9) . . . . ? Si1 Gd1 C2 C3 -143.01(9) . . . . ? C1 C2 C3 C30 -131.7(2) . . . . ? N1 C2 C3 C30 47.1(2) . . . . ? Gd1 C2 C3 C30 65.80(14) . . . . ? C1 C2 C3 C4 96.9(2) . . . . ? N1 C2 C3 C4 -84.3(2) . . . . ? Gd1 C2 C3 C4 -65.54(15) . . . . ? C18 N2 C4 C5 -1.2(3) . . . . ? Gd1 N2 C4 C5 -170.4(2) . . . . ? C18 N2 C4 C3 179.41(17) . . . . ? Gd1 N2 C4 C3 10.2(2) . . . . ? C30 C3 C4 C5 106.7(2) . . . . ? C2 C3 C4 C5 -122.3(2) . . . . ? C30 C3 C4 N2 -73.9(2) . . . . ? C2 C3 C4 N2 57.2(2) . . . . ? C2 N1 C6 C7 -107.8(2) . . . . ? Gd1 N1 C6 C7 59.1(3) . . . . ? C2 N1 C6 C11 76.4(3) . . . . ? Gd1 N1 C6 C11 -116.7(2) . . . . ? C11 C6 C7 C8 4.6(3) . . . . ? N1 C6 C7 C8 -171.2(2) . . . . ? C11 C6 C7 C12 -171.5(2) . . . . ? N1 C6 C7 C12 12.7(3) . . . . ? C6 C7 C8 C9 -2.1(4) . . . . ? C12 C7 C8 C9 174.1(2) . . . . ? C7 C8 C9 C10 -1.4(4) . . . . ? C8 C9 C10 C11 2.3(4) . . . . ? C9 C10 C11 C6 0.3(4) . . . . ? C9 C10 C11 C15 -178.9(2) . . . . ? C7 C6 C11 C10 -3.8(3) . . . . ? N1 C6 C11 C10 172.1(2) . . . . ? C7 C6 C11 C15 175.4(2) . . . . ? N1 C6 C11 C15 -8.8(3) . . . . ? C8 C7 C12 C13 -61.5(3) . . . . ? C6 C7 C12 C13 114.6(3) . . . . ? C8 C7 C12 C14 62.3(3) . . . . ? C6 C7 C12 C14 -121.6(3) . . . . ? C10 C11 C15 C16 62.6(3) . . . . ? C6 C11 C15 C16 -116.5(2) . . . . ? C10 C11 C15 C17 -60.9(3) . . . . ? C6 C11 C15 C17 119.9(2) . . . . ? C4 N2 C18 C23 87.2(2) . . . . ? Gd1 N2 C18 C23 -105.7(2) . . . . ? C4 N2 C18 C19 -96.7(2) . . . . ? Gd1 N2 C18 C19 70.3(2) . . . . ? C23 C18 C19 C20 4.9(3) . . . . ? N2 C18 C19 C20 -171.1(2) . . . . ? C23 C18 C19 C24 -172.9(2) . . . . ? N2 C18 C19 C24 11.1(3) . . . . ? C18 C19 C20 C21 -1.3(4) . . . . ? C24 C19 C20 C21 176.5(2) . . . . ? C19 C20 C21 C22 -2.6(4) . . . . ? C20 C21 C22 C23 3.0(4) . . . . ? C21 C22 C23 C18 0.6(4) . . . . ? C21 C22 C23 C27 179.9(2) . . . . ? C19 C18 C23 C22 -4.6(3) . . . . ? N2 C18 C23 C22 171.5(2) . . . . ? C19 C18 C23 C27 176.2(2) . . . . ? N2 C18 C23 C27 -7.8(3) . . . . ? C20 C19 C24 C26 49.1(3) . . . . ? C18 C19 C24 C26 -133.1(3) . . . . ? C20 C19 C24 C25 -75.0(3) . . . . ? C18 C19 C24 C25 102.7(3) . . . . ? C22 C23 C27 C29 -64.5(3) . . . . ? C18 C23 C27 C29 114.7(2) . . . . ? C22 C23 C27 C28 58.2(3) . . . . ? C18 C23 C27 C28 -122.6(2) . . . . ? C31 N3 C30 N4 7.1(3) . . . . ? Gd1 N3 C30 N4 -150.22(18) . . . . ? C31 N3 C30 C3 -173.64(18) . . . . ? Gd1 N3 C30 C3 29.0(2) . . . . ? C37 N4 C30 N3 174.0(2) . . . . ? C37 N4 C30 C3 -5.2(3) . . . . ? C2 C3 C30 N3 -87.0(2) . . . . ? C4 C3 C30 N3 45.9(3) . . . . ? C2 C3 C30 N4 92.3(2) . . . . ? C4 C3 C30 N4 -134.8(2) . . . . ? C30 N3 C31 C36 -169.9(2) . . . . ? Gd1 N3 C31 C36 -16.9(2) . . . . ? C30 N3 C31 C32 69.4(3) . . . . ? Gd1 N3 C31 C32 -137.57(16) . . . . ? N3 C31 C32 C33 176.7(2) . . . . ? C36 C31 C32 C33 56.5(3) . . . . ? C31 C32 C33 C34 -56.4(3) . . . . ? C32 C33 C34 C35 55.0(3) . . . . ? C33 C34 C35 C36 -54.6(3) . . . . ? N3 C31 C36 C35 -179.1(2) . . . . ? C32 C31 C36 C35 -56.4(3) . . . . ? C34 C35 C36 C31 56.3(3) . . . . ? C30 N4 C37 C42 87.7(3) . . . . ? C30 N4 C37 C38 -150.2(2) . . . . ? N4 C37 C38 C39 -179.2(2) . . . . ? C42 C37 C38 C39 -56.2(3) . . . . ? C37 C38 C39 C40 56.0(3) . . . . ? C38 C39 C40 C41 -56.2(3) . . . . ? C39 C40 C41 C42 56.7(4) . . . . ? N4 C37 C42 C41 177.5(2) . . . . ? C38 C37 C42 C41 56.9(3) . . . . ? C40 C41 C42 C37 -57.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.427 _refine_diff_density_min -0.319 _refine_diff_density_rms 0.061 _database_code_depnum_ccdc_archive 'CCDC 976989' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_complex5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H91 N5 Na O4 Si2 Sm' _chemical_formula_sum 'C50 H91 N5 Na O4 Si2 Sm' _chemical_formula_weight 1055.80 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' O O 0.0106 0.0060 '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' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, z' 'x, -y+1/2, z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, -z' '-x, y-1/2, -z-1/2' 'x-1/2, y, -z-1/2' _cell_length_a 12.3799(10) _cell_length_b 23.828(2) _cell_length_c 39.619(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11687.4(17) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 48823 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description chip _exptl_crystal_colour yellow _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.200 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4472 _exptl_absorpt_coefficient_mu 1.095 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.430 _exptl_absorpt_correction_T_max 0.848 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53353 _diffrn_reflns_av_R_equivalents 0.1379 _diffrn_reflns_av_sigmaI/netI 0.0998 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 47 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10077 _reflns_number_gt 8338 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _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. The size of the crystal is relatively big and it is not in good shape, furthermore,the diffraction of the crystal is relatively weak,that cause the internal R-factor high. Due to the disorder of c45, c46, c47, the Si1-C45,Si1-C46, Si1-C47 and Si1-C45', Si1-C46', Si1-C47' bonds were restrainted.Due to the disorder of C41, C42, the C41-C42 and C41'-C42'bonds were restrainted. Due to the disorder of C41, C42, the O3-C41,O3-C41'and O4-C42,O4-C42' bonds were restrainted. ; _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^)+(0.0000P)^2^+57.9778P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10077 _refine_ls_number_parameters 467 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1469 _refine_ls_R_factor_gt 0.1198 _refine_ls_wR_factor_ref 0.1822 _refine_ls_wR_factor_gt 0.1727 _refine_ls_goodness_of_fit_ref 1.344 _refine_ls_restrained_S_all 1.344 _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 Sm1 Sm 0.37544(4) 0.84252(2) 0.607659(12) 0.03618(16) Uani 1 1 d . A . Si1 Si 0.3776(3) 0.76894(13) 0.53235(8) 0.0564(9) Uani 1 1 d D . . Si2 Si 0.5454(2) 0.73404(12) 0.58328(7) 0.0433(7) Uani 1 1 d . . . Na1 Na 0.6758(3) 1.03348(18) 0.64840(11) 0.0541(11) Uani 1 1 d . A . O1 O 0.5740(6) 1.0972(3) 0.6142(2) 0.066(2) Uani 1 1 d . . . O2 O 0.7750(7) 1.0505(3) 0.5959(2) 0.067(2) Uani 1 1 d . . . O3 O 0.8478(7) 1.0120(4) 0.6733(2) 0.087(3) Uani 1 1 d D . . O4 O 0.7484(8) 1.1175(4) 0.6740(2) 0.079(3) Uani 1 1 d D . . N1 N 0.2325(6) 0.9041(3) 0.6066(2) 0.043(2) Uani 1 1 d . . . N2 N 0.3631(6) 0.8298(3) 0.66432(19) 0.0361(19) Uani 1 1 d . . . N3 N 0.4790(6) 0.9217(3) 0.61782(19) 0.0329(18) Uani 1 1 d . . . N4 N 0.5143(6) 0.9801(3) 0.66446(19) 0.040(2) Uani 1 1 d . . . N5 N 0.4385(6) 0.7747(3) 0.57071(19) 0.041(2) Uani 1 1 d . A . C1 C 0.1799(9) 0.9885(5) 0.6368(3) 0.070(4) Uani 1 1 d . . . H1A H 0.1215 0.9955 0.6222 0.084 Uiso 1 1 calc R B . H1B H 0.1941 1.0130 0.6548 0.084 Uiso 1 1 calc R . . C2 C 0.2431(8) 0.9434(4) 0.6318(3) 0.040(2) Uani 1 1 d . A . C3 C 0.3322(8) 0.9332(4) 0.6593(3) 0.038(2) Uani 1 1 d . . . H3 H 0.318(7) 0.966(4) 0.671(2) 0.046 Uiso 1 1 d . . . C4 C 0.3204(7) 0.8775(4) 0.6788(3) 0.039(2) Uani 1 1 d . A . C5 C 0.2695(8) 0.8803(5) 0.7092(2) 0.050(3) Uani 1 1 d . . . H5A H 0.2610 0.8477 0.7223 0.060 Uiso 1 1 calc R A . H5B H 0.2429 0.9148 0.7171 0.060 Uiso 1 1 calc R . . C6 C 0.1477(10) 0.9132(5) 0.5824(3) 0.0714(17) Uani 1 1 d . B . C7 C 0.1655(10) 0.9532(5) 0.5560(3) 0.0714(17) Uani 1 1 d . . . C8 C 0.0899(10) 0.9568(5) 0.5298(3) 0.0714(17) Uani 1 1 d . B . H8 H 0.1008 0.9824 0.5121 0.086 Uiso 1 1 calc R . . C9 C -0.0001(10) 0.9232(5) 0.5298(3) 0.0714(17) Uani 1 1 d . . . H9 H -0.0501 0.9258 0.5121 0.086 Uiso 1 1 calc R B . C10 C -0.0180(10) 0.8850(5) 0.5561(3) 0.0714(17) Uani 1 1 d . B . H10 H -0.0806 0.8626 0.5561 0.086 Uiso 1 1 calc R . . C11 C 0.0557(10) 0.8800(5) 0.5822(3) 0.0714(17) Uani 1 1 d . . . C12 C 0.2629(13) 0.9907(6) 0.5540(4) 0.097(3) Uani 1 1 d . B . H12 H 0.3092 0.9827 0.5738 0.116 Uiso 1 1 calc R . . C13 C 0.3287(12) 0.9791(6) 0.5224(3) 0.097(3) Uani 1 1 d . . . H13A H 0.3436 0.9392 0.5208 0.145 Uiso 1 1 calc R B . H13B H 0.3962 0.9997 0.5235 0.145 Uiso 1 1 calc R . . H13C H 0.2882 0.9910 0.5027 0.145 Uiso 1 1 calc R . . C14 C 0.2324(12) 1.0523(6) 0.5550(4) 0.097(3) Uani 1 1 d . . . H14A H 0.1814 1.0604 0.5371 0.145 Uiso 1 1 calc R B . H14B H 0.2967 1.0751 0.5520 0.145 Uiso 1 1 calc R . . H14C H 0.1997 1.0609 0.5767 0.145 Uiso 1 1 calc R . . C15 C 0.0387(12) 0.8375(7) 0.6091(4) 0.098(3) Uani 1 1 d . B . H15 H 0.1097 0.8201 0.6138 0.118 Uiso 1 1 calc R . . C16 C -0.0382(11) 0.7906(6) 0.6000(4) 0.098(3) Uani 1 1 d . . . H16A H -0.1107 0.8056 0.5976 0.147 Uiso 1 1 calc R B . H16B H -0.0376 0.7624 0.6176 0.147 Uiso 1 1 calc R . . H16C H -0.0157 0.7737 0.5788 0.147 Uiso 1 1 calc R . . C17 C -0.0006(11) 0.8633(7) 0.6419(4) 0.098(3) Uani 1 1 d . . . H17A H 0.0436 0.8956 0.6474 0.147 Uiso 1 1 calc R B . H17B H 0.0045 0.8358 0.6599 0.147 Uiso 1 1 calc R . . H17C H -0.0752 0.8750 0.6394 0.147 Uiso 1 1 calc R . . C18 C 0.3753(10) 0.7829(5) 0.6861(3) 0.0582(13) Uani 1 1 d . B . C19 C 0.3121(10) 0.7344(5) 0.6830(3) 0.0582(13) Uani 1 1 d . . . C20 C 0.3338(10) 0.6863(5) 0.7007(3) 0.0582(13) Uani 1 1 d . B . H20 H 0.2912 0.6540 0.6976 0.070 Uiso 1 1 calc R . . C21 C 0.4180(9) 0.6856(5) 0.7230(3) 0.0582(13) Uani 1 1 d . . . H21 H 0.4337 0.6526 0.7351 0.070 Uiso 1 1 calc R B . C22 C 0.4801(10) 0.7329(4) 0.7280(3) 0.0582(13) Uani 1 1 d . B . H22 H 0.5358 0.7323 0.7442 0.070 Uiso 1 1 calc R . . C23 C 0.4615(10) 0.7809(5) 0.7098(3) 0.0582(13) Uani 1 1 d . . . C24 C 0.2148(11) 0.7359(7) 0.6596(4) 0.091(3) Uani 1 1 d . B . H24 H 0.2060 0.7752 0.6519 0.109 Uiso 1 1 calc R . . C25 C 0.2313(11) 0.7001(6) 0.6283(3) 0.091(3) Uani 1 1 d . . . H25A H 0.2328 0.6608 0.6346 0.136 Uiso 1 1 calc R B . H25B H 0.2993 0.7100 0.6176 0.136 Uiso 1 1 calc R . . H25C H 0.1726 0.7065 0.6125 0.136 Uiso 1 1 calc R . . C26 C 0.1113(11) 0.7194(6) 0.6774(3) 0.091(3) Uani 1 1 d . . . H26A H 0.0515 0.7213 0.6616 0.136 Uiso 1 1 calc R B . H26B H 0.0981 0.7450 0.6960 0.136 Uiso 1 1 calc R . . H26C H 0.1179 0.6814 0.6860 0.136 Uiso 1 1 calc R . . C27 C 0.5318(9) 0.8322(5) 0.7166(3) 0.062(2) Uani 1 1 d . B . H27 H 0.5108 0.8615 0.7001 0.074 Uiso 1 1 calc R . . C28 C 0.6536(9) 0.8199(5) 0.7113(3) 0.062(2) Uani 1 1 d . . . H28A H 0.6771 0.7919 0.7275 0.093 Uiso 1 1 calc R B . H28B H 0.6946 0.8542 0.7146 0.093 Uiso 1 1 calc R . . H28C H 0.6652 0.8060 0.6886 0.093 Uiso 1 1 calc R . . C29 C 0.5112(10) 0.8559(5) 0.7521(3) 0.062(2) Uani 1 1 d . . . H29A H 0.4357 0.8660 0.7543 0.093 Uiso 1 1 calc R B . H29B H 0.5557 0.8889 0.7555 0.093 Uiso 1 1 calc R . . H29C H 0.5294 0.8277 0.7688 0.093 Uiso 1 1 calc R . . C30 C 0.4506(7) 0.9463(4) 0.6474(2) 0.034(2) Uani 1 1 d . A . C31 C 0.5873(8) 0.9338(4) 0.6044(3) 0.047(3) Uani 1 1 d . B . H31 H 0.5984 0.9749 0.6058 0.057 Uiso 1 1 calc R . . C32 C 0.6772(9) 0.9063(5) 0.6238(3) 0.064(3) Uani 1 1 d . . . H32A H 0.6672 0.9130 0.6478 0.095 Uiso 1 1 calc R B . H32B H 0.7459 0.9219 0.6167 0.095 Uiso 1 1 calc R . . H32C H 0.6765 0.8662 0.6195 0.095 Uiso 1 1 calc R . . C33 C 0.5890(9) 0.9178(5) 0.5674(3) 0.064(3) Uani 1 1 d . . . H33A H 0.5748 0.8780 0.5651 0.096 Uiso 1 1 calc R B . H33B H 0.6593 0.9264 0.5579 0.096 Uiso 1 1 calc R . . H33C H 0.5339 0.9389 0.5554 0.096 Uiso 1 1 calc R . . C34 C 0.4807(10) 1.0016(5) 0.6973(3) 0.0618(19) Uani 1 1 d . A . H34 H 0.429(6) 0.976(3) 0.710(2) 0.03(2) Uiso 1 1 d . . . C35 C 0.5800(9) 1.0071(5) 0.7200(3) 0.0618(19) Uani 1 1 d . . . H35A H 0.6203 0.9722 0.7197 0.093 Uiso 1 1 calc R A . H35B H 0.5572 1.0153 0.7429 0.093 Uiso 1 1 calc R . . H35C H 0.6255 1.0373 0.7118 0.093 Uiso 1 1 calc R . . C36 C 0.4258(9) 1.0576(5) 0.6948(3) 0.0618(19) Uani 1 1 d . . . H36A H 0.4751 1.0847 0.6850 0.093 Uiso 1 1 calc R A . H36B H 0.4047 1.0701 0.7172 0.093 Uiso 1 1 calc R . . H36C H 0.3622 1.0543 0.6806 0.093 Uiso 1 1 calc R . . C37 C 0.6467(11) 1.1244(5) 0.5921(3) 0.077(4) Uani 1 1 d . . . H37A H 0.6949 1.1488 0.6052 0.093 Uiso 1 1 calc R . . H37B H 0.6062 1.1481 0.5763 0.093 Uiso 1 1 calc R . . C38 C 0.7130(11) 1.0824(5) 0.5726(3) 0.072(4) Uani 1 1 d . . . H38A H 0.6653 1.0576 0.5597 0.086 Uiso 1 1 calc R . . H38B H 0.7609 1.1019 0.5568 0.086 Uiso 1 1 calc R . . C39 C 0.4749(10) 1.0824(6) 0.5982(4) 0.083(4) Uani 1 1 d . . . H39A H 0.4360 1.1162 0.5920 0.125 Uiso 1 1 calc R . . H39B H 0.4313 1.0603 0.6136 0.125 Uiso 1 1 calc R . . H39C H 0.4899 1.0606 0.5780 0.125 Uiso 1 1 calc R . . C40 C 0.8510(12) 1.0147(6) 0.5798(4) 0.104(6) Uani 1 1 d . . . H40A H 0.8129 0.9861 0.5670 0.155 Uiso 1 1 calc R . . H40B H 0.8961 0.9969 0.5967 0.155 Uiso 1 1 calc R . . H40C H 0.8958 1.0366 0.5646 0.155 Uiso 1 1 calc R . . C41 C 0.907(3) 1.0628(12) 0.6655(9) 0.119(7) Uani 0.50 1 d PD A 1 H41A H 0.8978 1.0745 0.6420 0.142 Uiso 0.50 1 calc PR A 1 H41B H 0.9843 1.0594 0.6708 0.142 Uiso 0.50 1 calc PR A 1 C41' C 0.911(3) 1.0605(11) 0.6831(10) 0.119(7) Uani 0.50 1 d PD A 2 H41C H 0.9703 1.0643 0.6668 0.142 Uiso 0.50 1 calc PR A 2 H41D H 0.9442 1.0521 0.7050 0.142 Uiso 0.50 1 calc PR A 2 C42 C 0.849(2) 1.1005(14) 0.6896(12) 0.119(7) Uani 0.50 1 d PD A 1 H42A H 0.8349 1.0807 0.7108 0.142 Uiso 0.50 1 calc PR A 1 H42B H 0.8935 1.1336 0.6946 0.142 Uiso 0.50 1 calc PR A 1 C42' C 0.858(2) 1.1160(14) 0.6859(14) 0.119(7) Uani 0.50 1 d PD A 2 H42C H 0.8584 1.1276 0.7097 0.142 Uiso 0.50 1 calc PR A 2 H42D H 0.9001 1.1435 0.6732 0.142 Uiso 0.50 1 calc PR A 2 C43 C 0.8758(12) 0.9718(6) 0.6974(4) 0.094(5) Uani 1 1 d . A . H43A H 0.9505 0.9607 0.6942 0.141 Uiso 1 1 calc R . . H43B H 0.8295 0.9392 0.6950 0.141 Uiso 1 1 calc R . . H43C H 0.8669 0.9875 0.7199 0.141 Uiso 1 1 calc R . . C44 C 0.6961(13) 1.1645(7) 0.6869(5) 0.129(7) Uani 1 1 d . A . H44A H 0.6713 1.1567 0.7096 0.194 Uiso 1 1 calc R . . H44B H 0.6347 1.1737 0.6727 0.194 Uiso 1 1 calc R . . H44C H 0.7459 1.1960 0.6873 0.194 Uiso 1 1 calc R . . C45 C 0.2676(18) 0.8222(10) 0.5290(8) 0.074(3) Uiso 0.50 1 d PD B 2 H45D H 0.2325 0.8188 0.5072 0.111 Uiso 0.50 1 calc PR B 2 H45E H 0.2980 0.8595 0.5313 0.111 Uiso 0.50 1 calc PR B 2 H45F H 0.2150 0.8159 0.5468 0.111 Uiso 0.50 1 calc PR B 2 C45' C 0.2419(15) 0.8030(10) 0.5375(8) 0.074(3) Uiso 0.50 1 d PD B 1 H45A H 0.1969 0.7941 0.5182 0.111 Uiso 0.50 1 calc PR B 1 H45B H 0.2509 0.8434 0.5391 0.111 Uiso 0.50 1 calc PR B 1 H45C H 0.2078 0.7892 0.5579 0.111 Uiso 0.50 1 calc PR B 1 C46 C 0.313(2) 0.6984(8) 0.5254(7) 0.074(3) Uiso 0.50 1 d PD B 2 H46D H 0.3242 0.6866 0.5022 0.111 Uiso 0.50 1 calc PR B 2 H46E H 0.2358 0.7011 0.5298 0.111 Uiso 0.50 1 calc PR B 2 H46F H 0.3447 0.6711 0.5406 0.111 Uiso 0.50 1 calc PR B 2 C46' C 0.366(2) 0.6971(8) 0.5155(7) 0.074(3) Uiso 0.50 1 d PD B 1 H46A H 0.3729 0.6980 0.4911 0.111 Uiso 0.50 1 calc PR B 1 H46B H 0.2956 0.6817 0.5214 0.111 Uiso 0.50 1 calc PR B 1 H46C H 0.4220 0.6737 0.5250 0.111 Uiso 0.50 1 calc PR B 1 C47 C 0.461(2) 0.7815(11) 0.4943(5) 0.074(3) Uiso 0.50 1 d PD B 2 H47D H 0.4437 0.7536 0.4773 0.111 Uiso 0.50 1 calc PR B 2 H47E H 0.5368 0.7787 0.5002 0.111 Uiso 0.50 1 calc PR B 2 H47F H 0.4460 0.8187 0.4855 0.111 Uiso 0.50 1 calc PR B 2 C47' C 0.459(2) 0.8100(10) 0.4999(6) 0.074(3) Uiso 0.50 1 d PD B 1 H47A H 0.4604 0.7896 0.4787 0.111 Uiso 0.50 1 calc PR B 1 H47B H 0.5328 0.8147 0.5080 0.111 Uiso 0.50 1 calc PR B 1 H47C H 0.4268 0.8466 0.4965 0.111 Uiso 0.50 1 calc PR B 1 C48 C 0.5197(10) 0.6574(5) 0.5811(4) 0.088(5) Uani 1 1 d . B . H48A H 0.4568 0.6483 0.5946 0.132 Uiso 1 1 calc R . . H48B H 0.5820 0.6373 0.5897 0.132 Uiso 1 1 calc R . . H48C H 0.5067 0.6467 0.5578 0.132 Uiso 1 1 calc R . . C49 C 0.5770(9) 0.7494(5) 0.6282(3) 0.065(4) Uani 1 1 d . B . H49A H 0.5712 0.7894 0.6322 0.098 Uiso 1 1 calc R . . H49B H 0.6500 0.7370 0.6333 0.098 Uiso 1 1 calc R . . H49C H 0.5264 0.7296 0.6427 0.098 Uiso 1 1 calc R . . C50 C 0.6726(9) 0.7492(6) 0.5592(3) 0.077(4) Uani 1 1 d . B . H50A H 0.6613 0.7411 0.5355 0.115 Uiso 1 1 calc R . . H50B H 0.7306 0.7259 0.5678 0.115 Uiso 1 1 calc R . . H50C H 0.6916 0.7884 0.5619 0.115 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.0369(3) 0.0390(3) 0.0326(3) -0.0036(2) -0.0031(3) 0.0042(2) Si1 0.070(2) 0.0537(19) 0.0456(18) -0.0151(15) -0.0144(18) 0.0228(18) Si2 0.0467(17) 0.0437(16) 0.0397(17) -0.0038(14) 0.0012(14) 0.0108(14) Na1 0.050(2) 0.054(3) 0.059(3) 0.004(2) 0.001(2) -0.012(2) O1 0.060(5) 0.077(6) 0.061(6) 0.010(5) -0.006(4) -0.002(5) O2 0.069(6) 0.062(5) 0.071(6) 0.004(5) 0.016(5) -0.006(5) O3 0.066(6) 0.088(7) 0.108(8) 0.033(6) -0.026(6) -0.004(5) O4 0.083(6) 0.064(6) 0.090(7) -0.013(5) -0.005(6) -0.017(5) N1 0.039(5) 0.046(5) 0.045(5) -0.006(5) -0.010(4) 0.004(4) N2 0.036(4) 0.033(4) 0.039(5) -0.007(4) -0.002(4) -0.010(4) N3 0.035(4) 0.031(4) 0.033(5) -0.004(4) 0.002(4) -0.003(4) N4 0.048(5) 0.041(5) 0.031(5) -0.003(4) 0.004(4) -0.010(4) N5 0.040(5) 0.052(5) 0.032(5) -0.016(4) -0.005(4) 0.010(4) C1 0.051(7) 0.082(9) 0.076(9) -0.039(7) -0.025(7) 0.039(7) C2 0.033(5) 0.042(6) 0.044(6) -0.011(5) 0.000(5) 0.005(5) C3 0.040(6) 0.033(5) 0.040(6) -0.005(5) -0.008(5) 0.013(5) C4 0.029(5) 0.044(6) 0.045(6) -0.013(5) -0.005(5) -0.008(5) C5 0.047(6) 0.062(7) 0.041(6) 0.003(6) 0.019(5) 0.004(6) C6 0.067(3) 0.065(4) 0.081(4) -0.022(3) -0.037(3) 0.018(3) C7 0.067(3) 0.065(4) 0.081(4) -0.022(3) -0.037(3) 0.018(3) C8 0.067(3) 0.065(4) 0.081(4) -0.022(3) -0.037(3) 0.018(3) C9 0.067(3) 0.065(4) 0.081(4) -0.022(3) -0.037(3) 0.018(3) C10 0.067(3) 0.065(4) 0.081(4) -0.022(3) -0.037(3) 0.018(3) C11 0.067(3) 0.065(4) 0.081(4) -0.022(3) -0.037(3) 0.018(3) C12 0.119(8) 0.088(6) 0.083(6) 0.019(6) -0.034(6) 0.007(6) C13 0.119(8) 0.088(6) 0.083(6) 0.019(6) -0.034(6) 0.007(6) C14 0.119(8) 0.088(6) 0.083(6) 0.019(6) -0.034(6) 0.007(6) C15 0.077(6) 0.123(8) 0.094(7) -0.016(6) -0.019(5) -0.012(5) C16 0.077(6) 0.123(8) 0.094(7) -0.016(6) -0.019(5) -0.012(5) C17 0.077(6) 0.123(8) 0.094(7) -0.016(6) -0.019(5) -0.012(5) C18 0.079(4) 0.048(3) 0.048(3) 0.002(2) 0.007(3) -0.005(3) C19 0.079(4) 0.048(3) 0.048(3) 0.002(2) 0.007(3) -0.005(3) C20 0.079(4) 0.048(3) 0.048(3) 0.002(2) 0.007(3) -0.005(3) C21 0.079(4) 0.048(3) 0.048(3) 0.002(2) 0.007(3) -0.005(3) C22 0.079(4) 0.048(3) 0.048(3) 0.002(2) 0.007(3) -0.005(3) C23 0.079(4) 0.048(3) 0.048(3) 0.002(2) 0.007(3) -0.005(3) C24 0.079(6) 0.105(7) 0.089(7) -0.008(5) 0.009(5) -0.029(5) C25 0.079(6) 0.105(7) 0.089(7) -0.008(5) 0.009(5) -0.029(5) C26 0.079(6) 0.105(7) 0.089(7) -0.008(5) 0.009(5) -0.029(5) C27 0.063(4) 0.067(5) 0.055(4) -0.010(4) -0.016(4) 0.006(4) C28 0.063(4) 0.067(5) 0.055(4) -0.010(4) -0.016(4) 0.006(4) C29 0.063(4) 0.067(5) 0.055(4) -0.010(4) -0.016(4) 0.006(4) C30 0.031(5) 0.033(5) 0.037(6) 0.012(5) 0.009(5) 0.004(4) C31 0.055(7) 0.036(6) 0.051(7) 0.007(5) 0.012(6) 0.003(5) C32 0.053(7) 0.053(7) 0.086(10) -0.002(7) 0.016(7) 0.005(6) C33 0.067(8) 0.055(7) 0.070(9) -0.012(7) 0.022(7) -0.017(6) C34 0.066(5) 0.063(4) 0.057(4) -0.014(4) 0.003(4) -0.014(4) C35 0.066(5) 0.063(4) 0.057(4) -0.014(4) 0.003(4) -0.014(4) C36 0.066(5) 0.063(4) 0.057(4) -0.014(4) 0.003(4) -0.014(4) C37 0.082(10) 0.073(9) 0.076(10) 0.025(8) -0.008(8) -0.003(8) C38 0.096(10) 0.058(8) 0.062(9) 0.008(7) 0.008(8) -0.027(8) C39 0.071(9) 0.083(10) 0.095(12) 0.003(9) -0.005(8) 0.005(8) C40 0.099(12) 0.069(10) 0.142(15) -0.011(10) 0.054(11) -0.016(9) C41 0.092(12) 0.120(16) 0.144(17) 0.030(16) -0.048(12) -0.054(10) C41' 0.092(12) 0.120(16) 0.144(17) 0.030(16) -0.048(12) -0.054(10) C42 0.092(12) 0.120(16) 0.144(17) 0.030(16) -0.048(12) -0.054(10) C42' 0.092(12) 0.120(16) 0.144(17) 0.030(16) -0.048(12) -0.054(10) C43 0.094(11) 0.090(11) 0.098(12) 0.000(10) -0.009(10) 0.006(10) C44 0.130(15) 0.084(12) 0.174(19) -0.037(13) 0.065(14) -0.032(11) C48 0.076(9) 0.053(8) 0.135(13) 0.008(9) -0.013(9) 0.006(7) C49 0.069(8) 0.087(9) 0.040(7) -0.006(6) -0.018(6) 0.018(7) C50 0.061(8) 0.109(11) 0.060(8) -0.001(8) 0.027(7) 0.030(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 N2 2.270(8) . ? Sm1 N1 2.299(8) . ? Sm1 N3 2.316(7) . ? Sm1 N5 2.317(7) . ? Sm1 C4 3.019(10) . ? Sm1 C3 3.024(10) . ? Sm1 C2 3.062(9) . ? Sm1 Si1 3.461(3) . ? Si1 N5 1.702(8) . ? Si1 C46' 1.845(16) . ? Si1 C47 1.850(16) . ? Si1 C45 1.866(16) . ? Si1 C45' 1.877(16) . ? Si1 C46 1.884(16) . ? Si1 C47' 1.907(16) . ? Si2 N5 1.714(8) . ? Si2 C48 1.855(12) . ? Si2 C49 1.860(10) . ? Si2 C50 1.876(11) . ? Na1 O1 2.394(9) . ? Na1 O3 2.402(9) . ? Na1 O4 2.417(9) . ? Na1 O2 2.450(9) . ? Na1 N4 2.453(9) . ? O1 C37 1.413(13) . ? O1 C39 1.425(13) . ? O2 C38 1.421(14) . ? O2 C40 1.421(14) . ? O3 C43 1.398(14) . ? O3 C41 1.448(18) . ? O3 C41' 1.450(18) . ? O4 C44 1.392(15) . ? O4 C42' 1.434(18) . ? O4 C42 1.451(18) . ? N1 C2 1.375(11) . ? N1 C6 1.437(13) . ? N2 C4 1.379(11) . ? N2 C18 1.421(12) . ? N3 C30 1.359(11) . ? N3 C31 1.471(12) . ? N4 C30 1.313(12) . ? N4 C34 1.458(13) . ? C1 C2 1.343(13) . ? C1 H1A 0.9400 . ? C1 H1B 0.9400 . ? C2 C3 1.570(13) . ? C3 C4 1.543(13) . ? C3 C30 1.570(13) . ? C3 H3 0.94(9) . ? C4 C5 1.358(13) . ? C5 H5A 0.9400 . ? C5 H5B 0.9400 . ? C6 C11 1.387(17) . ? C6 C7 1.435(18) . ? C7 C8 1.399(15) . ? C7 C12 1.503(19) . ? C8 C9 1.372(16) . ? C8 H8 0.9400 . ? C9 C10 1.401(17) . ? C9 H9 0.9400 . ? C10 C11 1.382(15) . ? C10 H10 0.9400 . ? C11 C15 1.488(19) . ? C12 C14 1.516(18) . ? C12 C13 1.518(19) . ? C12 H12 0.9900 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 H13C 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 C16 1.512(18) . ? C15 C17 1.517(18) . ? C15 H15 0.9900 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 C19 1.402(15) . ? C18 C23 1.420(16) . ? C19 C20 1.373(14) . ? C19 C24 1.520(17) . ? C20 C21 1.366(15) . ? C20 H20 0.9400 . ? C21 C22 1.378(14) . ? C21 H21 0.9400 . ? C22 C23 1.372(14) . ? C22 H22 0.9400 . ? C23 C27 1.525(15) . ? C24 C26 1.515(17) . ? C24 C25 1.521(17) . ? C24 H24 0.9900 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C25 H25C 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C26 H26C 0.9700 . ? C27 C29 1.536(14) . ? C27 C28 1.550(14) . ? C27 H27 0.9900 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 H28C 0.9700 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C29 H29C 0.9700 . ? C31 C32 1.503(14) . ? C31 C33 1.515(14) . ? C31 H31 0.9900 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C32 H32C 0.9700 . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C33 H33C 0.9700 . ? C34 C36 1.501(15) . ? C34 C35 1.529(15) . ? C34 H34 1.01(8) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C35 H35C 0.9700 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C36 H36C 0.9700 . ? C37 C38 1.507(16) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C39 H39C 0.9700 . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C40 H40C 0.9700 . ? C41 C42 1.50(2) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41' C42' 1.483(19) . ? C41' H41C 0.9800 . ? C41' H41D 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42' H42C 0.9800 . ? C42' H42D 0.9800 . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C43 H43C 0.9700 . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C44 H44C 0.9700 . ? C45 H45D 0.9700 . ? C45 H45E 0.9700 . ? C45 H45F 0.9700 . ? C45' H45A 0.9700 . ? C45' H45B 0.9700 . ? C45' H45C 0.9700 . ? C46 H46D 0.9700 . ? C46 H46E 0.9700 . ? C46 H46F 0.9700 . ? C46' H46A 0.9700 . ? C46' H46B 0.9700 . ? C46' H46C 0.9700 . ? C47 H47D 0.9700 . ? C47 H47E 0.9700 . ? C47 H47F 0.9700 . ? C47' H47A 0.9700 . ? C47' H47B 0.9700 . ? C47' H47C 0.9700 . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C48 H48C 0.9700 . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C49 H49C 0.9700 . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C50 H50C 0.9700 . ? 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 Sm1 N1 93.0(3) . . ? N2 Sm1 N3 88.5(3) . . ? N1 Sm1 N3 84.8(3) . . ? N2 Sm1 N5 123.7(3) . . ? N1 Sm1 N5 133.9(3) . . ? N3 Sm1 N5 119.5(3) . . ? N2 Sm1 C4 25.6(3) . . ? N1 Sm1 C4 70.6(3) . . ? N3 Sm1 C4 74.8(3) . . ? N5 Sm1 C4 149.2(3) . . ? N2 Sm1 C3 54.1(3) . . ? N1 Sm1 C3 54.6(3) . . ? N3 Sm1 C3 53.0(3) . . ? N5 Sm1 C3 170.4(3) . . ? C4 Sm1 C3 29.6(3) . . ? N2 Sm1 C2 76.1(3) . . ? N1 Sm1 C2 24.9(3) . . ? N3 Sm1 C2 66.6(3) . . ? N5 Sm1 C2 157.7(3) . . ? C4 Sm1 C2 51.0(3) . . ? C3 Sm1 C2 29.9(2) . . ? N2 Sm1 Si1 141.77(19) . . ? N1 Sm1 Si1 108.3(2) . . ? N3 Sm1 Si1 123.9(2) . . ? N5 Sm1 Si1 25.72(19) . . ? C4 Sm1 Si1 161.28(19) . . ? C3 Sm1 Si1 161.23(19) . . ? C2 Sm1 Si1 132.13(19) . . ? N5 Si1 C46' 115.7(9) . . ? N5 Si1 C47 117.8(10) . . ? C46' Si1 C47 84.2(12) . . ? N5 Si1 C45 109.4(10) . . ? C46' Si1 C45 123.2(13) . . ? C47 Si1 C45 103.9(12) . . ? N5 Si1 C45' 105.3(10) . . ? C46' Si1 C45' 111.7(12) . . ? C47 Si1 C45' 121.2(12) . . ? C45 Si1 C45' 20.0(11) . . ? N5 Si1 C46 113.0(9) . . ? C46' Si1 C46 23.7(10) . . ? C47 Si1 C46 105.2(12) . . ? C45 Si1 C46 106.6(12) . . ? C45' Si1 C46 91.2(12) . . ? N5 Si1 C47' 109.0(10) . . ? C46' Si1 C47' 105.9(11) . . ? C47 Si1 C47' 21.9(11) . . ? C45 Si1 C47' 89.5(12) . . ? C45' Si1 C47' 109.1(12) . . ? C46 Si1 C47' 125.9(12) . . ? N5 Si1 Sm1 36.2(3) . . ? C46' Si1 Sm1 141.5(9) . . ? C47 Si1 Sm1 128.6(9) . . ? C45 Si1 Sm1 73.2(10) . . ? C45' Si1 Sm1 71.3(10) . . ? C46 Si1 Sm1 125.1(8) . . ? C47' Si1 Sm1 109.0(8) . . ? N5 Si2 C48 114.2(5) . . ? N5 Si2 C49 109.3(5) . . ? C48 Si2 C49 105.9(6) . . ? N5 Si2 C50 113.1(5) . . ? C48 Si2 C50 108.0(6) . . ? C49 Si2 C50 105.8(6) . . ? O1 Na1 O3 146.5(4) . . ? O1 Na1 O4 84.7(3) . . ? O3 Na1 O4 71.0(3) . . ? O1 Na1 O2 71.2(3) . . ? O3 Na1 O2 86.5(3) . . ? O4 Na1 O2 91.9(3) . . ? O1 Na1 N4 92.7(3) . . ? O3 Na1 N4 120.4(3) . . ? O4 Na1 N4 128.6(3) . . ? O2 Na1 N4 135.6(3) . . ? C37 O1 C39 112.8(10) . . ? C37 O1 Na1 107.8(7) . . ? C39 O1 Na1 123.3(8) . . ? C38 O2 C40 112.8(11) . . ? C38 O2 Na1 111.6(7) . . ? C40 O2 Na1 127.9(8) . . ? C43 O3 C41 126.3(18) . . ? C43 O3 C41' 103.2(17) . . ? C41 O3 C41' 28(2) . . ? C43 O3 Na1 130.3(9) . . ? C41 O3 Na1 100.6(16) . . ? C41' O3 Na1 114.9(15) . . ? C44 O4 C42' 109.7(19) . . ? C44 O4 C42 118(2) . . ? C42' O4 C42 16(3) . . ? C44 O4 Na1 130.4(9) . . ? C42' O4 Na1 118.0(15) . . ? C42 O4 Na1 105.6(15) . . ? C2 N1 C6 116.8(8) . . ? C2 N1 Sm1 110.4(6) . . ? C6 N1 Sm1 132.1(7) . . ? C4 N2 C18 115.8(8) . . ? C4 N2 Sm1 109.2(6) . . ? C18 N2 Sm1 134.4(6) . . ? C30 N3 C31 117.5(8) . . ? C30 N3 Sm1 111.1(6) . . ? C31 N3 Sm1 127.0(6) . . ? C30 N4 C34 120.1(9) . . ? C30 N4 Na1 132.4(6) . . ? C34 N4 Na1 106.3(7) . . ? Si1 N5 Si2 123.8(5) . . ? Si1 N5 Sm1 118.1(4) . . ? Si2 N5 Sm1 118.1(4) . . ? C2 C1 H1A 120.0 . . ? C2 C1 H1B 120.0 . . ? H1A C1 H1B 120.0 . . ? C1 C2 N1 126.6(10) . . ? C1 C2 C3 115.5(9) . . ? N1 C2 C3 117.7(8) . . ? C1 C2 Sm1 170.2(8) . . ? N1 C2 Sm1 44.7(4) . . ? C3 C2 Sm1 73.7(5) . . ? C4 C3 C30 114.2(7) . . ? C4 C3 C2 114.5(8) . . ? C30 C3 C2 114.6(8) . . ? C4 C3 Sm1 75.0(5) . . ? C30 C3 Sm1 77.0(5) . . ? C2 C3 Sm1 76.4(5) . . ? C4 C3 H3 116(6) . . ? C30 C3 H3 99(6) . . ? C2 C3 H3 96(6) . . ? Sm1 C3 H3 168(6) . . ? C5 C4 N2 126.0(10) . . ? C5 C4 C3 116.5(9) . . ? N2 C4 C3 117.5(8) . . ? C5 C4 Sm1 160.9(7) . . ? N2 C4 Sm1 45.3(5) . . ? C3 C4 Sm1 75.4(5) . . ? C4 C5 H5A 120.0 . . ? C4 C5 H5B 120.0 . . ? H5A C5 H5B 120.0 . . ? C11 C6 C7 120.0(11) . . ? C11 C6 N1 121.4(12) . . ? C7 C6 N1 118.3(11) . . ? C8 C7 C6 118.6(13) . . ? C8 C7 C12 117.5(14) . . ? C6 C7 C12 123.9(11) . . ? C9 C8 C7 120.5(14) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C8 C9 C10 120.5(12) . . ? C8 C9 H9 119.7 . . ? C10 C9 H9 119.7 . . ? C11 C10 C9 120.4(13) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C10 C11 C6 120.0(14) . . ? C10 C11 C15 120.1(13) . . ? C6 C11 C15 119.9(12) . . ? C7 C12 C14 111.9(13) . . ? C7 C12 C13 111.5(13) . . ? C14 C12 C13 109.4(13) . . ? C7 C12 H12 108.0 . . ? C14 C12 H12 108.0 . . ? C13 C12 H12 108.0 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 C16 114.8(13) . . ? C11 C15 C17 112.6(14) . . ? C16 C15 C17 107.7(13) . . ? C11 C15 H15 107.1 . . ? C16 C15 H15 107.1 . . ? C17 C15 H15 107.1 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C23 116.7(10) . . ? C19 C18 N2 122.3(11) . . ? C23 C18 N2 120.6(10) . . ? C20 C19 C18 122.3(12) . . ? C20 C19 C24 119.1(12) . . ? C18 C19 C24 118.6(11) . . ? C21 C20 C19 119.3(11) . . ? C21 C20 H20 120.3 . . ? C19 C20 H20 120.3 . . ? C20 C21 C22 120.6(11) . . ? C20 C21 H21 119.7 . . ? C22 C21 H21 119.7 . . ? C23 C22 C21 120.8(12) . . ? C23 C22 H22 119.6 . . ? C21 C22 H22 119.6 . . ? C22 C23 C18 120.2(11) . . ? C22 C23 C27 118.7(11) . . ? C18 C23 C27 121.1(10) . . ? C26 C24 C19 112.4(12) . . ? C26 C24 C25 110.4(12) . . ? C19 C24 C25 112.2(12) . . ? C26 C24 H24 107.2 . . ? C19 C24 H24 107.2 . . ? C25 C24 H24 107.2 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 C29 111.2(10) . . ? C23 C27 C28 112.3(10) . . ? C29 C27 C28 110.6(9) . . ? C23 C27 H27 107.5 . . ? C29 C27 H27 107.5 . . ? C28 C27 H27 107.5 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N4 C30 N3 123.6(8) . . ? N4 C30 C3 121.9(8) . . ? N3 C30 C3 114.4(8) . . ? N3 C31 C32 113.9(8) . . ? N3 C31 C33 108.2(9) . . ? C32 C31 C33 112.0(9) . . ? N3 C31 H31 107.5 . . ? C32 C31 H31 107.5 . . ? C33 C31 H31 107.5 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N4 C34 C36 112.5(10) . . ? N4 C34 C35 108.9(10) . . ? C36 C34 C35 109.1(10) . . ? N4 C34 H34 114(5) . . ? C36 C34 H34 106(5) . . ? C35 C34 H34 105(5) . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O1 C37 C38 111.0(10) . . ? O1 C37 H37A 109.4 . . ? C38 C37 H37A 109.4 . . ? O1 C37 H37B 109.4 . . ? C38 C37 H37B 109.4 . . ? H37A C37 H37B 108.0 . . ? O2 C38 C37 108.5(10) . . ? O2 C38 H38A 110.0 . . ? C37 C38 H38A 110.0 . . ? O2 C38 H38B 110.0 . . ? C37 C38 H38B 110.0 . . ? H38A C38 H38B 108.4 . . ? O1 C39 H39A 109.5 . . ? O1 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? O1 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? O2 C40 H40A 109.5 . . ? O2 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? O2 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? O3 C41 C42 97(2) . . ? O3 C41 H41A 112.4 . . ? C42 C41 H41A 112.4 . . ? O3 C41 H41B 112.4 . . ? C42 C41 H41B 112.4 . . ? H41A C41 H41B 109.9 . . ? O3 C41' C42' 119(3) . . ? O3 C41' H41C 107.5 . . ? C42' C41' H41C 107.5 . . ? O3 C41' H41D 107.5 . . ? C42' C41' H41D 107.5 . . ? H41C C41' H41D 107.0 . . ? O4 C42 C41 108(3) . . ? O4 C42 H42A 110.1 . . ? C41 C42 H42A 110.1 . . ? O4 C42 H42B 110.1 . . ? C41 C42 H42B 110.1 . . ? H42A C42 H42B 108.5 . . ? O4 C42' C41' 115(3) . . ? O4 C42' H42C 108.6 . . ? C41' C42' H42C 108.6 . . ? O4 C42' H42D 108.6 . . ? C41' C42' H42D 108.6 . . ? H42C C42' H42D 107.6 . . ? O3 C43 H43A 109.5 . . ? O3 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? O3 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? O4 C44 H44A 109.5 . . ? O4 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? O4 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? Si1 C45 H45D 109.5 . . ? Si1 C45 H45E 109.5 . . ? H45D C45 H45E 109.5 . . ? Si1 C45 H45F 109.5 . . ? H45D C45 H45F 109.5 . . ? H45E C45 H45F 109.5 . . ? Si1 C45' H45A 109.5 . . ? Si1 C45' H45B 109.5 . . ? H45A C45' H45B 109.5 . . ? Si1 C45' H45C 109.5 . . ? H45A C45' H45C 109.5 . . ? H45B C45' H45C 109.5 . . ? Si1 C46 H46D 109.5 . . ? Si1 C46 H46E 109.5 . . ? H46D C46 H46E 109.5 . . ? Si1 C46 H46F 109.5 . . ? H46D C46 H46F 109.5 . . ? H46E C46 H46F 109.5 . . ? Si1 C46' H46A 109.5 . . ? Si1 C46' H46B 109.5 . . ? H46A C46' H46B 109.5 . . ? Si1 C46' H46C 109.5 . . ? H46A C46' H46C 109.5 . . ? H46B C46' H46C 109.5 . . ? Si1 C47 H47D 109.5 . . ? Si1 C47 H47E 109.5 . . ? H47D C47 H47E 109.5 . . ? Si1 C47 H47F 109.5 . . ? H47D C47 H47F 109.5 . . ? H47E C47 H47F 109.5 . . ? Si1 C47' H47A 109.5 . . ? Si1 C47' H47B 109.5 . . ? H47A C47' H47B 109.5 . . ? Si1 C47' H47C 109.5 . . ? H47A C47' H47C 109.5 . . ? H47B C47' H47C 109.5 . . ? Si2 C48 H48A 109.5 . . ? Si2 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? Si2 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? Si2 C49 H49A 109.5 . . ? Si2 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? Si2 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? Si2 C50 H50A 109.5 . . ? Si2 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? Si2 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Sm1 Si1 N5 -55.2(6) . . . . ? N1 Sm1 Si1 N5 -175.7(5) . . . . ? N3 Sm1 Si1 N5 88.2(5) . . . . ? C4 Sm1 Si1 N5 -92.5(8) . . . . ? C3 Sm1 Si1 N5 162.3(8) . . . . ? C2 Sm1 Si1 N5 176.0(6) . . . . ? N2 Sm1 Si1 C46' 2.3(14) . . . . ? N1 Sm1 Si1 C46' -118.1(14) . . . . ? N3 Sm1 Si1 C46' 145.7(14) . . . . ? N5 Sm1 Si1 C46' 57.5(15) . . . . ? C4 Sm1 Si1 C46' -34.9(15) . . . . ? C3 Sm1 Si1 C46' -140.2(15) . . . . ? C2 Sm1 Si1 C46' -126.4(14) . . . . ? N2 Sm1 Si1 C47 -140.6(12) . . . . ? N1 Sm1 Si1 C47 99.0(12) . . . . ? N3 Sm1 Si1 C47 2.8(12) . . . . ? N5 Sm1 Si1 C47 -85.4(13) . . . . ? C4 Sm1 Si1 C47 -177.8(13) . . . . ? C3 Sm1 Si1 C47 76.9(13) . . . . ? C2 Sm1 Si1 C47 90.7(12) . . . . ? N2 Sm1 Si1 C45 124.9(9) . . . . ? N1 Sm1 Si1 C45 4.4(9) . . . . ? N3 Sm1 Si1 C45 -91.7(9) . . . . ? N5 Sm1 Si1 C45 -179.9(10) . . . . ? C4 Sm1 Si1 C45 87.6(10) . . . . ? C3 Sm1 Si1 C45 -17.7(11) . . . . ? C2 Sm1 Si1 C45 -3.9(9) . . . . ? N2 Sm1 Si1 C45' 103.9(9) . . . . ? N1 Sm1 Si1 C45' -16.5(9) . . . . ? N3 Sm1 Si1 C45' -112.6(9) . . . . ? N5 Sm1 Si1 C45' 159.1(10) . . . . ? C4 Sm1 Si1 C45' 66.7(10) . . . . ? C3 Sm1 Si1 C45' -38.6(11) . . . . ? C2 Sm1 Si1 C45' -24.8(9) . . . . ? N2 Sm1 Si1 C46 26.1(11) . . . . ? N1 Sm1 Si1 C46 -94.3(11) . . . . ? N3 Sm1 Si1 C46 169.5(11) . . . . ? N5 Sm1 Si1 C46 81.3(11) . . . . ? C4 Sm1 Si1 C46 -11.1(12) . . . . ? C3 Sm1 Si1 C46 -116.4(12) . . . . ? C2 Sm1 Si1 C46 -102.6(11) . . . . ? N2 Sm1 Si1 C47' -151.7(10) . . . . ? N1 Sm1 Si1 C47' 87.9(10) . . . . ? N3 Sm1 Si1 C47' -8.2(10) . . . . ? N5 Sm1 Si1 C47' -96.4(11) . . . . ? C4 Sm1 Si1 C47' 171.1(11) . . . . ? C3 Sm1 Si1 C47' 65.8(11) . . . . ? C2 Sm1 Si1 C47' 79.6(10) . . . . ? O3 Na1 O1 C37 26.7(11) . . . . ? O4 Na1 O1 C37 69.6(8) . . . . ? O2 Na1 O1 C37 -24.2(8) . . . . ? N4 Na1 O1 C37 -161.9(8) . . . . ? O3 Na1 O1 C39 161.0(9) . . . . ? O4 Na1 O1 C39 -156.2(9) . . . . ? O2 Na1 O1 C39 110.1(9) . . . . ? N4 Na1 O1 C39 -27.7(9) . . . . ? O1 Na1 O2 C38 -7.3(7) . . . . ? O3 Na1 O2 C38 -161.9(8) . . . . ? O4 Na1 O2 C38 -91.1(8) . . . . ? N4 Na1 O2 C38 66.6(9) . . . . ? O1 Na1 O2 C40 -154.1(11) . . . . ? O3 Na1 O2 C40 51.3(11) . . . . ? O4 Na1 O2 C40 122.1(10) . . . . ? N4 Na1 O2 C40 -80.2(11) . . . . ? O1 Na1 O3 C43 169.4(10) . . . . ? O4 Na1 O3 C43 123.6(12) . . . . ? O2 Na1 O3 C43 -143.2(12) . . . . ? N4 Na1 O3 C43 -0.6(13) . . . . ? O1 Na1 O3 C41 7.6(19) . . . . ? O4 Na1 O3 C41 -38.2(17) . . . . ? O2 Na1 O3 C41 55.0(17) . . . . ? N4 Na1 O3 C41 -162.4(17) . . . . ? O1 Na1 O3 C41' 33(2) . . . . ? O4 Na1 O3 C41' -13(2) . . . . ? O2 Na1 O3 C41' 80(2) . . . . ? N4 Na1 O3 C41' -137(2) . . . . ? O1 Na1 O4 C44 49.9(13) . . . . ? O3 Na1 O4 C44 -153.5(13) . . . . ? O2 Na1 O4 C44 120.8(13) . . . . ? N4 Na1 O4 C44 -39.3(14) . . . . ? O1 Na1 O4 C42' -148(3) . . . . ? O3 Na1 O4 C42' 9(3) . . . . ? O2 Na1 O4 C42' -77(3) . . . . ? N4 Na1 O4 C42' 123(3) . . . . ? O1 Na1 O4 C42 -159(2) . . . . ? O3 Na1 O4 C42 -2(2) . . . . ? O2 Na1 O4 C42 -88(2) . . . . ? N4 Na1 O4 C42 112(2) . . . . ? N2 Sm1 N1 C2 47.0(7) . . . . ? N3 Sm1 N1 C2 -41.2(7) . . . . ? N5 Sm1 N1 C2 -167.9(6) . . . . ? C4 Sm1 N1 C2 34.5(6) . . . . ? C3 Sm1 N1 C2 6.2(6) . . . . ? Si1 Sm1 N1 C2 -165.3(6) . . . . ? N2 Sm1 N1 C6 -143.4(11) . . . . ? N3 Sm1 N1 C6 128.4(11) . . . . ? N5 Sm1 N1 C6 1.7(12) . . . . ? C4 Sm1 N1 C6 -155.9(11) . . . . ? C3 Sm1 N1 C6 175.8(12) . . . . ? C2 Sm1 N1 C6 169.6(15) . . . . ? Si1 Sm1 N1 C6 4.4(11) . . . . ? N1 Sm1 N2 C4 -28.3(6) . . . . ? N3 Sm1 N2 C4 56.4(6) . . . . ? N5 Sm1 N2 C4 -178.6(5) . . . . ? C3 Sm1 N2 C4 12.8(5) . . . . ? C2 Sm1 N2 C4 -9.8(6) . . . . ? Si1 Sm1 N2 C4 -153.2(4) . . . . ? N1 Sm1 N2 C18 141.5(10) . . . . ? N3 Sm1 N2 C18 -133.8(10) . . . . ? N5 Sm1 N2 C18 -8.8(11) . . . . ? C4 Sm1 N2 C18 169.9(13) . . . . ? C3 Sm1 N2 C18 -177.4(11) . . . . ? C2 Sm1 N2 C18 160.0(10) . . . . ? Si1 Sm1 N2 C18 16.6(11) . . . . ? N2 Sm1 N3 C30 -30.4(6) . . . . ? N1 Sm1 N3 C30 62.7(6) . . . . ? N5 Sm1 N3 C30 -158.9(6) . . . . ? C4 Sm1 N3 C30 -8.6(6) . . . . ? C3 Sm1 N3 C30 14.0(5) . . . . ? C2 Sm1 N3 C30 45.1(6) . . . . ? Si1 Sm1 N3 C30 171.2(5) . . . . ? N2 Sm1 N3 C31 125.2(8) . . . . ? N1 Sm1 N3 C31 -141.7(8) . . . . ? N5 Sm1 N3 C31 -3.3(8) . . . . ? C4 Sm1 N3 C31 147.1(8) . . . . ? C3 Sm1 N3 C31 169.6(9) . . . . ? C2 Sm1 N3 C31 -159.3(8) . . . . ? Si1 Sm1 N3 C31 -33.2(8) . . . . ? O1 Na1 N4 C30 70.2(9) . . . . ? O3 Na1 N4 C30 -115.3(9) . . . . ? O4 Na1 N4 C30 155.6(8) . . . . ? O2 Na1 N4 C30 4.6(11) . . . . ? O1 Na1 N4 C34 -97.1(7) . . . . ? O3 Na1 N4 C34 77.4(8) . . . . ? O4 Na1 N4 C34 -11.7(9) . . . . ? O2 Na1 N4 C34 -162.7(7) . . . . ? C46' Si1 N5 Si2 36.9(11) . . . . ? C47 Si1 N5 Si2 -60.4(11) . . . . ? C45 Si1 N5 Si2 -178.7(10) . . . . ? C45' Si1 N5 Si2 160.8(9) . . . . ? C46 Si1 N5 Si2 62.8(11) . . . . ? C47' Si1 N5 Si2 -82.3(10) . . . . ? Sm1 Si1 N5 Si2 -178.7(9) . . . . ? C46' Si1 N5 Sm1 -144.3(10) . . . . ? C47 Si1 N5 Sm1 118.3(10) . . . . ? C45 Si1 N5 Sm1 0.1(10) . . . . ? C45' Si1 N5 Sm1 -20.5(10) . . . . ? C46 Si1 N5 Sm1 -118.5(9) . . . . ? C47' Si1 N5 Sm1 96.5(10) . . . . ? C48 Si2 N5 Si1 -55.9(8) . . . . ? C49 Si2 N5 Si1 -174.3(6) . . . . ? C50 Si2 N5 Si1 68.2(8) . . . . ? C48 Si2 N5 Sm1 125.3(6) . . . . ? C49 Si2 N5 Sm1 7.0(7) . . . . ? C50 Si2 N5 Sm1 -110.6(6) . . . . ? N2 Sm1 N5 Si1 142.4(4) . . . . ? N1 Sm1 N5 Si1 5.7(7) . . . . ? N3 Sm1 N5 Si1 -107.8(5) . . . . ? C4 Sm1 N5 Si1 141.2(4) . . . . ? C3 Sm1 N5 Si1 -144.0(15) . . . . ? C2 Sm1 N5 Si1 -7.8(11) . . . . ? N2 Sm1 N5 Si2 -38.8(6) . . . . ? N1 Sm1 N5 Si2 -175.5(4) . . . . ? N3 Sm1 N5 Si2 71.1(5) . . . . ? C4 Sm1 N5 Si2 -40.0(8) . . . . ? C3 Sm1 N5 Si2 35(2) . . . . ? C2 Sm1 N5 Si2 171.0(5) . . . . ? Si1 Sm1 N5 Si2 178.8(9) . . . . ? C6 N1 C2 C1 2.5(17) . . . . ? Sm1 N1 C2 C1 173.8(10) . . . . ? C6 N1 C2 C3 177.6(10) . . . . ? Sm1 N1 C2 C3 -11.0(11) . . . . ? C6 N1 C2 Sm1 -171.4(12) . . . . ? N2 Sm1 C2 C1 -162(5) . . . . ? N1 Sm1 C2 C1 -30(5) . . . . ? N3 Sm1 C2 C1 104(5) . . . . ? N5 Sm1 C2 C1 -7(5) . . . . ? C4 Sm1 C2 C1 -167(5) . . . . ? C3 Sm1 C2 C1 160(5) . . . . ? Si1 Sm1 C2 C1 -11(5) . . . . ? N2 Sm1 C2 N1 -131.2(7) . . . . ? N3 Sm1 C2 N1 134.4(7) . . . . ? N5 Sm1 C2 N1 23.6(11) . . . . ? C4 Sm1 C2 N1 -136.6(8) . . . . ? C3 Sm1 C2 N1 -169.8(10) . . . . ? Si1 Sm1 C2 N1 19.0(8) . . . . ? N2 Sm1 C2 C3 38.6(5) . . . . ? N1 Sm1 C2 C3 169.8(10) . . . . ? N3 Sm1 C2 C3 -55.8(5) . . . . ? N5 Sm1 C2 C3 -166.6(7) . . . . ? C4 Sm1 C2 C3 33.2(5) . . . . ? Si1 Sm1 C2 C3 -171.2(4) . . . . ? C1 C2 C3 C4 117.4(11) . . . . ? N1 C2 C3 C4 -58.2(12) . . . . ? Sm1 C2 C3 C4 -66.3(7) . . . . ? C1 C2 C3 C30 -107.7(11) . . . . ? N1 C2 C3 C30 76.6(11) . . . . ? Sm1 C2 C3 C30 68.6(7) . . . . ? C1 C2 C3 Sm1 -176.3(10) . . . . ? N1 C2 C3 Sm1 8.1(8) . . . . ? N2 Sm1 C3 C4 -11.1(5) . . . . ? N1 Sm1 C3 C4 115.2(6) . . . . ? N3 Sm1 C3 C4 -131.4(6) . . . . ? N5 Sm1 C3 C4 -91.3(18) . . . . ? C2 Sm1 C3 C4 120.4(8) . . . . ? Si1 Sm1 C3 C4 141.2(5) . . . . ? N2 Sm1 C3 C30 108.7(5) . . . . ? N1 Sm1 C3 C30 -125.0(6) . . . . ? N3 Sm1 C3 C30 -11.6(4) . . . . ? N5 Sm1 C3 C30 28.6(19) . . . . ? C4 Sm1 C3 C30 119.8(7) . . . . ? C2 Sm1 C3 C30 -119.7(8) . . . . ? Si1 Sm1 C3 C30 -99.0(7) . . . . ? N2 Sm1 C3 C2 -131.6(6) . . . . ? N1 Sm1 C3 C2 -5.2(5) . . . . ? N3 Sm1 C3 C2 108.1(6) . . . . ? N5 Sm1 C3 C2 148.3(16) . . . . ? C4 Sm1 C3 C2 -120.4(8) . . . . ? Si1 Sm1 C3 C2 20.7(10) . . . . ? C18 N2 C4 C5 -14.4(14) . . . . ? Sm1 N2 C4 C5 157.6(8) . . . . ? C18 N2 C4 C3 164.7(9) . . . . ? Sm1 N2 C4 C3 -23.3(9) . . . . ? C18 N2 C4 Sm1 -172.0(10) . . . . ? C30 C3 C4 C5 128.2(9) . . . . ? C2 C3 C4 C5 -96.8(10) . . . . ? Sm1 C3 C4 C5 -163.9(8) . . . . ? C30 C3 C4 N2 -51.0(11) . . . . ? C2 C3 C4 N2 84.0(10) . . . . ? Sm1 C3 C4 N2 16.9(7) . . . . ? C30 C3 C4 Sm1 -67.9(7) . . . . ? C2 C3 C4 Sm1 67.1(7) . . . . ? N2 Sm1 C4 C5 -70(2) . . . . ? N1 Sm1 C4 C5 79(2) . . . . ? N3 Sm1 C4 C5 169(2) . . . . ? N5 Sm1 C4 C5 -68(2) . . . . ? C3 Sm1 C4 C5 131(3) . . . . ? C2 Sm1 C4 C5 97(2) . . . . ? Si1 Sm1 C4 C5 -10(3) . . . . ? N1 Sm1 C4 N2 149.9(6) . . . . ? N3 Sm1 C4 N2 -120.4(6) . . . . ? N5 Sm1 C4 N2 2.3(9) . . . . ? C3 Sm1 C4 N2 -158.7(9) . . . . ? C2 Sm1 C4 N2 167.7(7) . . . . ? Si1 Sm1 C4 N2 60.2(9) . . . . ? N2 Sm1 C4 C3 158.7(9) . . . . ? N1 Sm1 C4 C3 -51.4(5) . . . . ? N3 Sm1 C4 C3 38.4(5) . . . . ? N5 Sm1 C4 C3 161.0(5) . . . . ? C2 Sm1 C4 C3 -33.6(5) . . . . ? Si1 Sm1 C4 C3 -141.1(6) . . . . ? C2 N1 C6 C11 -108.2(13) . . . . ? Sm1 N1 C6 C11 82.7(15) . . . . ? C2 N1 C6 C7 78.9(14) . . . . ? Sm1 N1 C6 C7 -90.2(13) . . . . ? C11 C6 C7 C8 -1.6(18) . . . . ? N1 C6 C7 C8 171.4(10) . . . . ? C11 C6 C7 C12 -179.5(13) . . . . ? N1 C6 C7 C12 -6.5(19) . . . . ? C6 C7 C8 C9 1.0(18) . . . . ? C12 C7 C8 C9 179.0(12) . . . . ? C7 C8 C9 C10 0.4(19) . . . . ? C8 C9 C10 C11 -1.1(19) . . . . ? C9 C10 C11 C6 0.4(19) . . . . ? C9 C10 C11 C15 -177.1(12) . . . . ? C7 C6 C11 C10 0.9(19) . . . . ? N1 C6 C11 C10 -171.8(11) . . . . ? C7 C6 C11 C15 178.5(12) . . . . ? N1 C6 C11 C15 5.7(19) . . . . ? C8 C7 C12 C14 62.7(17) . . . . ? C6 C7 C12 C14 -119.4(14) . . . . ? C8 C7 C12 C13 -60.2(16) . . . . ? C6 C7 C12 C13 117.7(14) . . . . ? C10 C11 C15 C16 19(2) . . . . ? C6 C11 C15 C16 -158.3(12) . . . . ? C10 C11 C15 C17 -104.4(14) . . . . ? C6 C11 C15 C17 78.0(16) . . . . ? C4 N2 C18 C19 110.8(11) . . . . ? Sm1 N2 C18 C19 -58.6(16) . . . . ? C4 N2 C18 C23 -76.6(13) . . . . ? Sm1 N2 C18 C23 114.0(11) . . . . ? C23 C18 C19 C20 -2.4(18) . . . . ? N2 C18 C19 C20 170.5(10) . . . . ? C23 C18 C19 C24 176.3(11) . . . . ? N2 C18 C19 C24 -10.9(17) . . . . ? C18 C19 C20 C21 1.9(18) . . . . ? C24 C19 C20 C21 -176.8(11) . . . . ? C19 C20 C21 C22 0.7(17) . . . . ? C20 C21 C22 C23 -2.7(18) . . . . ? C21 C22 C23 C18 2.1(18) . . . . ? C21 C22 C23 C27 179.4(10) . . . . ? C19 C18 C23 C22 0.4(17) . . . . ? N2 C18 C23 C22 -172.6(10) . . . . ? C19 C18 C23 C27 -176.8(10) . . . . ? N2 C18 C23 C27 10.2(17) . . . . ? C20 C19 C24 C26 53.9(17) . . . . ? C18 C19 C24 C26 -124.7(13) . . . . ? C20 C19 C24 C25 -71.2(15) . . . . ? C18 C19 C24 C25 110.2(14) . . . . ? C22 C23 C27 C29 -66.8(14) . . . . ? C18 C23 C27 C29 110.5(12) . . . . ? C22 C23 C27 C28 57.9(14) . . . . ? C18 C23 C27 C28 -124.9(12) . . . . ? C34 N4 C30 N3 -175.5(9) . . . . ? Na1 N4 C30 N3 18.6(14) . . . . ? C34 N4 C30 C3 7.0(14) . . . . ? Na1 N4 C30 C3 -158.9(7) . . . . ? C31 N3 C30 N4 0.1(13) . . . . ? Sm1 N3 C30 N4 158.3(7) . . . . ? C31 N3 C30 C3 177.7(8) . . . . ? Sm1 N3 C30 C3 -24.1(9) . . . . ? C4 C3 C30 N4 -98.1(10) . . . . ? C2 C3 C30 N4 126.9(9) . . . . ? Sm1 C3 C30 N4 -164.9(8) . . . . ? C4 C3 C30 N3 84.2(10) . . . . ? C2 C3 C30 N3 -50.8(11) . . . . ? Sm1 C3 C30 N3 17.5(6) . . . . ? C30 N3 C31 C32 72.2(11) . . . . ? Sm1 N3 C31 C32 -82.1(11) . . . . ? C30 N3 C31 C33 -162.6(8) . . . . ? Sm1 N3 C31 C33 43.1(11) . . . . ? C30 N4 C34 C36 -93.4(12) . . . . ? Na1 N4 C34 C36 75.8(10) . . . . ? C30 N4 C34 C35 145.5(10) . . . . ? Na1 N4 C34 C35 -45.3(10) . . . . ? C39 O1 C37 C38 -85.8(13) . . . . ? Na1 O1 C37 C38 53.6(12) . . . . ? C40 O2 C38 C37 -172.2(10) . . . . ? Na1 O2 C38 C37 35.8(11) . . . . ? O1 C37 C38 O2 -61.9(13) . . . . ? C43 O3 C41 C42 -92(3) . . . . ? C41' O3 C41 C42 -53(4) . . . . ? Na1 O3 C41 C42 71(2) . . . . ? C43 O3 C41' C42' -131(4) . . . . ? C41 O3 C41' C42' 80(7) . . . . ? Na1 O3 C41' C42' 16(5) . . . . ? C44 O4 C42 C41 -161.6(19) . . . . ? C42' O4 C42 C41 -98(14) . . . . ? Na1 O4 C42 C41 43(3) . . . . ? O3 C41 C42 O4 -81(3) . . . . ? C44 O4 C42' C41' 162(4) . . . . ? C42 O4 C42' C41' 39(10) . . . . ? Na1 O4 C42' C41' -4(5) . . . . ? O3 C41' C42' O4 -8(7) . . . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.781 _refine_diff_density_min -0.508 _refine_diff_density_rms 0.095 _database_code_depnum_ccdc_archive 'CCDC 976990'