# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 #============================================================================ # 2. TITLE AND AUTHOR LIST data_fisrt_block #TrackingRef '- 1_4.cif' _publ_section_title ; Heteroscorpionate Rare-Earth Initiators for the Controlled Ring-Opening Polymerization of Cyclic Esters ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address A.Otero ; Departamento de Quimica Inorganica, Organica y Bioquimica Campus Universitario Universidad de Castilla-La Mancha 13071-Ciudad Real Spain ; A.Lara-Sanchez ; Departamento de Quimica Inorganica, Organica y Bioquimica Campus Universitario Universidad de Castilla-La Mancha 13071-Ciudad Real Spain ; J.Fernandez-Baeza ; Departamento de Quimica Inorganica, Organica y Bioquimica Campus Universitario Universidad de Castilla-La Mancha 13071-Ciudad Real Spain ; C.Alonso-Moreno ; Departamento de Quimica Inorganica, Organica y Bioquimica Campus Universitario Universidad de Castilla-La Mancha 13071-Ciudad Real Spain ; ; I.Marquez-Segovia ; ; Departamento de Quimica Inorganica, Organica y Bioquimica Campus Universitario Universidad de Castilla-La Mancha 13071-Ciudad Real Spain ; L.Sanchez-Barba ; Departamento de Quimica Inorganica, Organica y Bioquimica Campus Universitario Universidad de Castilla-La Mancha 13071-Ciudad Real Spain ; A.Rodriguez ; Departamento de Quimica Inorganica, Organica y Bioquimica Campus Universitario Universidad de Castilla-La Mancha 13071-Ciudad Real Spain ; #============================================================================ data_2 _database_code_depnum_ccdc_archive 'CCDC 713430' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H74 N12 Nd2 O2 Si4, 2(C7 H8)' _chemical_formula_sum 'C62 H90 N12 Nd2 O2 Si4' _chemical_formula_weight 1436.30 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' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.7654(9) _cell_length_b 25.9552(18) _cell_length_c 13.4362(9) _cell_angle_alpha 90.00 _cell_angle_beta 110.8830(10) _cell_angle_gamma 90.00 _cell_volume 3833.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 4992 _cell_measurement_theta_min 2.257 _cell_measurement_theta_max 22.469 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.244 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1476 _exptl_absorpt_coefficient_mu 1.446 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5819 _exptl_absorpt_correction_T_max 0.7322 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28800 _diffrn_reflns_av_R_equivalents 0.0446 _diffrn_reflns_av_sigmaI/netI 0.0887 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 28.27 _reflns_number_total 18049 _reflns_number_gt 14220 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0746P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.010(13) _chemical_absolute_configuration rm _refine_ls_number_reflns 18049 _refine_ls_number_parameters 661 _refine_ls_number_restraints 112 _refine_ls_R_factor_all 0.0743 _refine_ls_R_factor_gt 0.0542 _refine_ls_wR_factor_ref 0.1445 _refine_ls_wR_factor_gt 0.1311 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 0.997 _refine_ls_shift/su_max 0.057 _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 Nd1 Nd 0.38849(3) 0.410792(13) 0.00140(3) 0.02902(9) Uani 1 1 d . . . Nd2 Nd 0.24221(3) 0.545046(13) -0.02340(3) 0.03216(10) Uani 1 1 d . . . Si1 Si 0.3826(2) 0.29642(9) -0.0819(2) 0.0497(6) Uani 1 1 d . . . HI1 H 0.4413 0.3217 -0.0926 0.060 Uiso 1 1 calc R . . Si2 Si 0.1609(2) 0.31682(11) -0.0169(2) 0.0579(7) Uani 1 1 d . . . HI2 H 0.1683 0.2814 0.0142 0.069 Uiso 1 1 calc R . . Si3 Si 0.1703(3) 0.57399(13) 0.2092(2) 0.0640(7) Uani 1 1 d . . . HI3 H 0.1011 0.5952 0.2132 0.077 Uiso 1 1 calc R . . Si4 Si 0.2153(3) 0.65670(11) 0.0668(2) 0.0691(9) Uani 1 1 d . . . HI4 H 0.2394 0.6538 0.0027 0.083 Uiso 1 1 calc R . . N1 N 0.6257(5) 0.4252(2) 0.0483(5) 0.0315(13) Uani 1 1 d . . . N2 N 0.6573(5) 0.4528(2) 0.1443(5) 0.0341(13) Uani 1 1 d . . . N3 N 0.4884(6) 0.3809(2) 0.1986(5) 0.0395(14) Uani 1 1 d . . . N4 N 0.5353(5) 0.4277(2) 0.2439(4) 0.0336(13) Uani 1 1 d . . . N5 N 0.4668(5) 0.5382(2) 0.0562(4) 0.0297(12) Uani 1 1 d . . . N6 N 0.2935(6) 0.3318(2) -0.0346(5) 0.0414(15) Uani 1 1 d . . . N7 N 0.0126(5) 0.5362(3) -0.1366(5) 0.0423(15) Uani 1 1 d . . . N8 N 0.0169(5) 0.5056(2) -0.2196(5) 0.0376(14) Uani 1 1 d . . . N9 N 0.2264(5) 0.5842(2) -0.2149(5) 0.0357(13) Uani 1 1 d . . . N10 N 0.1588(5) 0.5464(2) -0.2836(4) 0.0316(11) Uani 1 1 d . . . N11 N 0.3282(5) 0.4577(2) -0.1709(4) 0.0331(13) Uani 1 1 d . . . N12 N 0.2034(6) 0.5944(3) 0.1043(5) 0.0484(17) Uani 1 1 d . . . O1 O 0.3542(4) 0.48427(19) 0.1103(4) 0.0339(11) Uani 1 1 d . . . O2 O 0.1978(4) 0.45229(18) -0.0857(4) 0.0323(10) Uani 1 1 d . . . C1 C 0.7810(7) 0.4548(3) 0.1934(6) 0.0409(18) Uani 1 1 d . . . C2 C 0.8323(7) 0.4300(3) 0.1310(6) 0.0446(19) Uani 1 1 d . . . H2 H 0.9168 0.4259 0.1446 0.054 Uiso 1 1 calc R . . C3 C 0.7338(6) 0.4114(3) 0.0404(5) 0.0385(15) Uani 1 1 d . . . C4 C 0.8352(7) 0.4773(4) 0.3044(7) 0.054(2) Uani 1 1 d . . . H4A H 0.8612 0.4493 0.3566 0.080 Uiso 1 1 calc R . . H4B H 0.7740 0.4984 0.3192 0.080 Uiso 1 1 calc R . . H4C H 0.9056 0.4987 0.3092 0.080 Uiso 1 1 calc R . . C5 C 0.7399(8) 0.3801(4) -0.0521(7) 0.052(2) Uani 1 1 d . . . H5A H 0.6589 0.3665 -0.0930 0.077 Uiso 1 1 calc R . . H5B H 0.7968 0.3514 -0.0253 0.077 Uiso 1 1 calc R . . H5C H 0.7678 0.4020 -0.0982 0.077 Uiso 1 1 calc R . . C6 C 0.5429(8) 0.4299(3) 0.3458(6) 0.0456(19) Uani 1 1 d . . . C7 C 0.5050(9) 0.3821(4) 0.3698(7) 0.056(2) Uani 1 1 d . . . H7 H 0.5023 0.3711 0.4364 0.067 Uiso 1 1 calc R . . C8 C 0.4725(8) 0.3544(3) 0.2772(7) 0.049(2) Uani 1 1 d . . . C9 C 0.5890(10) 0.4749(4) 0.4152(7) 0.063(3) Uani 1 1 d . . . H9A H 0.6441 0.4946 0.3896 0.094 Uiso 1 1 calc R . . H9B H 0.6329 0.4633 0.4882 0.094 Uiso 1 1 calc R . . H9C H 0.5205 0.4968 0.4138 0.094 Uiso 1 1 calc R . . C10 C 0.4236(11) 0.2987(4) 0.2578(8) 0.071(3) Uani 1 1 d . . . H10A H 0.3584 0.2946 0.2865 0.107 Uiso 1 1 calc R . . H10B H 0.4897 0.2746 0.2934 0.107 Uiso 1 1 calc R . . H10C H 0.3917 0.2917 0.1811 0.107 Uiso 1 1 calc R . . C11 C 0.5609(6) 0.4659(3) 0.1796(6) 0.0324(15) Uani 1 1 d . . . C12 C 0.4673(6) 0.4983(3) 0.1178(5) 0.0325(16) Uani 1 1 d . . . C13 C 0.5810(7) 0.5619(3) 0.0613(6) 0.0366(17) Uani 1 1 d . . . H13 H 0.6344 0.5345 0.0493 0.044 Uiso 1 1 calc R . . C14 C 0.5522(8) 0.6008(3) -0.0304(7) 0.049(2) Uani 1 1 d . . . H14A H 0.5300 0.5822 -0.0982 0.074 Uiso 1 1 calc R . . H14B H 0.6239 0.6222 -0.0207 0.074 Uiso 1 1 calc R . . H14C H 0.4842 0.6227 -0.0308 0.074 Uiso 1 1 calc R . . C15 C 0.6483(7) 0.5874(3) 0.1643(6) 0.0368(16) Uani 1 1 d . . . C16 C 0.5908(8) 0.5993(3) 0.2372(7) 0.0468(19) Uani 1 1 d . . . H16 H 0.5078 0.5907 0.2222 0.056 Uiso 1 1 calc R . . C17 C 0.6593(10) 0.6243(4) 0.3332(8) 0.066(3) Uani 1 1 d . . . H17 H 0.6205 0.6331 0.3819 0.079 Uiso 1 1 calc R . . C18 C 0.7833(10) 0.6369(4) 0.3595(8) 0.063(3) Uani 1 1 d . . . H18 H 0.8277 0.6536 0.4247 0.076 Uiso 1 1 calc R . . C19 C 0.8377(9) 0.6242(4) 0.2880(8) 0.062(3) Uani 1 1 d . . . H19 H 0.9214 0.6318 0.3047 0.074 Uiso 1 1 calc R . . C20 C 0.7729(8) 0.6003(3) 0.1911(7) 0.051(2) Uani 1 1 d . . . H20 H 0.8127 0.5926 0.1426 0.061 Uiso 1 1 calc R . . C21 C 0.3107(13) 0.2657(5) -0.2125(9) 0.092(4) Uani 1 1 d . . . H21A H 0.2512 0.2402 -0.2083 0.137 Uiso 1 1 calc R . . H21B H 0.3730 0.2487 -0.2335 0.137 Uiso 1 1 calc R . . H21C H 0.2693 0.2920 -0.2655 0.137 Uiso 1 1 calc R . . C22 C 0.4803(13) 0.2480(4) 0.0139(10) 0.094(4) Uani 1 1 d . . . H22A H 0.5345 0.2657 0.0775 0.140 Uiso 1 1 calc R . . H22B H 0.5290 0.2292 -0.0200 0.140 Uiso 1 1 calc R . . H22C H 0.4287 0.2237 0.0343 0.140 Uiso 1 1 calc R . . C23 C 0.0278(10) 0.3180(6) -0.1454(10) 0.099(4) Uani 1 1 d . . . H23A H 0.0226 0.3518 -0.1790 0.149 Uiso 1 1 calc R . . H23B H -0.0471 0.3114 -0.1312 0.149 Uiso 1 1 calc R . . H23C H 0.0381 0.2913 -0.1931 0.149 Uiso 1 1 calc R . . C24 C 0.1324(11) 0.3635(6) 0.0778(10) 0.090(4) Uani 1 1 d . . . H24A H 0.2036 0.3647 0.1439 0.136 Uiso 1 1 calc R . . H24B H 0.0611 0.3524 0.0938 0.136 Uiso 1 1 calc R . . H24C H 0.1176 0.3978 0.0454 0.136 Uiso 1 1 calc R . . C25 C -0.1004(7) 0.5268(4) -0.1341(7) 0.059(3) Uani 1 1 d . . . C26 C -0.1613(8) 0.4909(4) -0.2129(8) 0.063(3) Uani 1 1 d . . . H26 H -0.2420 0.4789 -0.2281 0.075 Uiso 1 1 calc R . . C27 C -0.0860(8) 0.4759(4) -0.2637(7) 0.055(2) Uani 1 1 d . . . C28 C -0.1433(10) 0.5531(5) -0.0592(9) 0.081(4) Uani 1 1 d . . . H28A H -0.0736 0.5648 0.0019 0.122 Uiso 1 1 calc R . . H28B H -0.1927 0.5294 -0.0347 0.122 Uiso 1 1 calc R . . H28C H -0.1928 0.5828 -0.0942 0.122 Uiso 1 1 calc R . . C29 C -0.1007(8) 0.4391(4) -0.3489(8) 0.067(3) Uani 1 1 d . . . H29A H -0.1618 0.4133 -0.3491 0.101 Uiso 1 1 calc R . . H29B H -0.0229 0.4219 -0.3375 0.101 Uiso 1 1 calc R . . H29C H -0.1275 0.4571 -0.4174 0.101 Uiso 1 1 calc R . . C30 C 0.1242(7) 0.5636(3) -0.3875(6) 0.0411(18) Uani 1 1 d . . . C31 C 0.1724(8) 0.6121(3) -0.3819(6) 0.0446(19) Uani 1 1 d . . . H31 H 0.1659 0.6336 -0.4408 0.054 Uiso 1 1 calc R . . C32 C 0.2323(7) 0.6243(3) -0.2754(6) 0.0393(17) Uani 1 1 d . . . C33 C 0.3005(8) 0.6719(3) -0.2274(7) 0.056(2) Uani 1 1 d . . . H33A H 0.3110 0.6735 -0.1517 0.084 Uiso 1 1 calc R . . H33B H 0.2549 0.7022 -0.2642 0.084 Uiso 1 1 calc R . . H33C H 0.3805 0.6714 -0.2346 0.084 Uiso 1 1 calc R . . C34 C 0.0477(7) 0.5334(3) -0.4783(5) 0.0433(18) Uani 1 1 d . . . H34A H -0.0380 0.5388 -0.4879 0.065 Uiso 1 1 calc R . . H34B H 0.0679 0.4968 -0.4653 0.065 Uiso 1 1 calc R . . H34C H 0.0619 0.5445 -0.5426 0.065 Uiso 1 1 calc R . . C35 C 0.1289(6) 0.5032(3) -0.2384(6) 0.0335(15) Uani 1 1 d . . . C36 C 0.2201(6) 0.4701(3) -0.1707(6) 0.0328(15) Uani 1 1 d . . . C37 C 0.3672(6) 0.4732(3) -0.2593(5) 0.0373(17) Uani 1 1 d . . . H37 H 0.3564 0.5112 -0.2702 0.045 Uiso 1 1 calc R . . C38 C 0.5041(7) 0.4597(4) -0.2265(7) 0.052(2) Uani 1 1 d . . . H38A H 0.5491 0.4750 -0.1569 0.079 Uiso 1 1 calc R . . H38B H 0.5354 0.4734 -0.2797 0.079 Uiso 1 1 calc R . . H38C H 0.5142 0.4222 -0.2223 0.079 Uiso 1 1 calc R . . C39 C 0.2957(8) 0.4455(3) -0.3635(6) 0.0463(19) Uani 1 1 d . . . C40 C 0.2154(8) 0.4059(4) -0.3719(6) 0.051(2) Uani 1 1 d . . . H40 H 0.2029 0.3941 -0.3096 0.062 Uiso 1 1 calc R . . C41 C 0.1500(10) 0.3821(4) -0.4721(8) 0.071(3) Uani 1 1 d . . . H41 H 0.0920 0.3558 -0.4771 0.086 Uiso 1 1 calc R . . C42 C 0.1723(11) 0.3977(5) -0.5603(8) 0.080(4) Uani 1 1 d . . . H42 H 0.1299 0.3820 -0.6271 0.096 Uiso 1 1 calc R . . C43 C 0.2561(12) 0.4363(6) -0.5533(8) 0.086(4) Uani 1 1 d . . . H43 H 0.2737 0.4459 -0.6144 0.104 Uiso 1 1 calc R . . C44 C 0.3139(9) 0.4606(4) -0.4571(7) 0.062(3) Uani 1 1 d . . . H44 H 0.3676 0.4883 -0.4542 0.075 Uiso 1 1 calc R . . C45 C 0.1205(11) 0.5060(5) 0.1905(9) 0.076(3) Uani 1 1 d . . . H45A H 0.0546 0.5021 0.1214 0.115 Uiso 1 1 calc R . . H45B H 0.0914 0.4958 0.2475 0.115 Uiso 1 1 calc R . . H45C H 0.1891 0.4840 0.1927 0.115 Uiso 1 1 calc R . . C46 C 0.2930(15) 0.5809(7) 0.3306(10) 0.121(6) Uani 1 1 d . . . H46A H 0.3557 0.5553 0.3345 0.182 Uiso 1 1 calc R . . H46B H 0.2643 0.5756 0.3899 0.182 Uiso 1 1 calc R . . H46C H 0.3272 0.6156 0.3349 0.182 Uiso 1 1 calc R . . C47 C 0.3338(14) 0.6959(5) 0.1610(10) 0.098(4) Uani 1 1 d . . . H47A H 0.3344 0.6899 0.2332 0.148 Uiso 1 1 calc R . . H47B H 0.3176 0.7324 0.1427 0.148 Uiso 1 1 calc R . . H47C H 0.4130 0.6865 0.1577 0.148 Uiso 1 1 calc R . . C48 C 0.0817(7) 0.6951(3) 0.0248(12) 0.144(7) Uani 1 1 d . . . H48A H 0.0434 0.6935 -0.0530 0.217 Uiso 1 1 calc R . . H48B H 0.1030 0.7309 0.0468 0.217 Uiso 1 1 calc R . . H48C H 0.0248 0.6821 0.0572 0.217 Uiso 1 1 calc R . . C71 C 0.9319(7) 0.2722(3) 0.4516(7) 0.067(5) Uiso 0.50 1 d PRD . . C72 C 0.9946(7) 0.2569(3) 0.3863(7) 0.049(4) Uiso 0.50 1 d PRD . . H72 H 1.0636 0.2351 0.4135 0.058 Uiso 0.50 1 calc PR . . C73 C 0.9563(8) 0.2735(3) 0.2811(7) 0.114(9) Uiso 0.50 1 d PRD . . H73 H 0.9991 0.2631 0.2365 0.137 Uiso 0.50 1 calc PR . . C74 C 0.8552(8) 0.3055(3) 0.2412(7) 0.092(7) Uiso 0.50 1 d PRD . . H74 H 0.8290 0.3168 0.1693 0.110 Uiso 0.50 1 calc PR . . C75 C 0.7926(7) 0.3208(3) 0.3065(7) 0.060(5) Uiso 0.50 1 d PRD . . H75 H 0.7235 0.3426 0.2792 0.072 Uiso 0.50 1 calc PR . . C76 C 0.8309(7) 0.3041(3) 0.4117(7) 0.070(5) Uiso 0.50 1 d PRD . . H76 H 0.7881 0.3146 0.4563 0.084 Uiso 0.50 1 calc PR . . C77 C 0.9762(5) 0.2520(2) 0.5411(4) 0.088(7) Uiso 0.50 1 d PD . . H77A H 0.9307 0.2633 0.5857 0.132 Uiso 0.50 1 calc PR . . H77B H 1.0616 0.2624 0.5744 0.132 Uiso 0.50 1 calc PR . . H77C H 0.9712 0.2144 0.5338 0.132 Uiso 0.50 1 calc PR . . C81 C 0.4446(5) 0.2707(2) 0.5491(4) 0.084(3) Uiso 1 1 d RD . . C82 C 0.4820(5) 0.3151(2) 0.6099(4) 0.086(3) Uiso 1 1 d RD . . H82 H 0.4234 0.3373 0.6210 0.104 Uiso 1 1 calc R . . C83 C 0.6050(5) 0.3269(2) 0.6546(4) 0.092(4) Uiso 1 1 d RD . . H83 H 0.6306 0.3573 0.6962 0.110 Uiso 1 1 calc R . . C84 C 0.6907(5) 0.2944(2) 0.6385(4) 0.108(4) Uiso 1 1 d RD . . H84 H 0.7748 0.3025 0.6690 0.130 Uiso 1 1 calc R . . C85 C 0.6533(5) 0.2501(2) 0.5776(4) 0.126(6) Uiso 1 1 d RD . . H85 H 0.7119 0.2278 0.5665 0.151 Uiso 1 1 calc R . . C86 C 0.5303(5) 0.2382(2) 0.5329(4) 0.099(4) Uiso 1 1 d RD . . H86 H 0.5047 0.2079 0.4913 0.119 Uiso 1 1 calc R . . C87 C 0.3201(6) 0.2580(3) 0.5001(5) 0.112(5) Uiso 1 1 d D . . H87A H 0.3123 0.2255 0.4611 0.167 Uiso 1 1 calc R . . H87B H 0.2783 0.2855 0.4504 0.167 Uiso 1 1 calc R . . H87C H 0.2835 0.2543 0.5547 0.167 Uiso 1 1 calc R . . C91 C 0.2154(6) 0.1773(3) 0.2261(5) 0.052(4) Uiso 0.50 1 d PRD . . H91 H 0.1919 0.2045 0.1757 0.063 Uiso 0.50 1 calc PR . . C92 C 0.1322(6) 0.1568(3) 0.2673(5) 0.071(6) Uiso 0.50 1 d PRD . . H92 H 0.0517 0.1701 0.2450 0.085 Uiso 0.50 1 calc PR . . C93 C 0.1667(6) 0.1170(3) 0.3411(5) 0.083(7) Uiso 0.50 1 d PRD . . H93 H 0.1098 0.1030 0.3692 0.100 Uiso 0.50 1 calc PR . . C94 C 0.2844(6) 0.0975(3) 0.3737(5) 0.045(4) Uiso 0.50 1 d PRD . . H94 H 0.3079 0.0703 0.4241 0.054 Uiso 0.50 1 calc PR . . C95 C 0.3676(6) 0.1179(3) 0.3325(5) 0.063(5) Uiso 0.50 1 d PRD . . C96 C 0.3331(6) 0.1578(3) 0.2587(5) 0.043(4) Uiso 0.50 1 d PRD . . H96 H 0.3900 0.1718 0.2306 0.052 Uiso 0.50 1 calc PR . . C97 C 0.471(2) 0.0981(11) 0.362(2) 0.101(8) Uiso 0.50 1 d PD . . H97A H 0.5207 0.1157 0.3280 0.152 Uiso 0.50 1 calc PR . . H97B H 0.4638 0.0615 0.3428 0.152 Uiso 0.50 1 calc PR . . H97C H 0.5093 0.1014 0.4399 0.152 Uiso 0.50 1 calc PR . . 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 Nd1 0.02668(17) 0.02685(17) 0.03147(17) 0.00254(15) 0.00785(13) -0.00019(15) Nd2 0.02841(18) 0.03360(19) 0.03420(18) 0.00258(16) 0.01084(14) 0.00597(16) Si1 0.0650(15) 0.0282(11) 0.0562(14) -0.0019(10) 0.0219(12) -0.0016(10) Si2 0.0448(13) 0.0556(15) 0.0674(16) 0.0137(13) 0.0128(12) -0.0161(12) Si3 0.0629(17) 0.084(2) 0.0575(16) -0.0068(14) 0.0362(14) 0.0012(15) Si4 0.104(2) 0.0464(15) 0.0621(17) -0.0009(13) 0.0359(16) 0.0296(15) N1 0.023(3) 0.034(3) 0.037(3) -0.004(2) 0.010(2) 0.005(2) N2 0.030(3) 0.032(3) 0.035(3) 0.002(2) 0.004(2) 0.004(2) N3 0.043(4) 0.033(3) 0.038(3) 0.006(3) 0.009(3) -0.004(3) N4 0.029(3) 0.035(3) 0.033(3) 0.000(2) 0.007(2) 0.003(2) N5 0.025(3) 0.032(3) 0.031(3) 0.002(2) 0.010(2) 0.003(2) N6 0.042(3) 0.031(3) 0.046(4) -0.002(3) 0.010(3) -0.003(3) N7 0.028(3) 0.048(4) 0.051(4) 0.014(3) 0.014(3) 0.010(3) N8 0.025(3) 0.041(4) 0.039(3) 0.007(3) 0.002(3) -0.001(3) N9 0.030(3) 0.034(3) 0.037(3) 0.003(3) 0.006(3) -0.006(2) N10 0.027(2) 0.032(3) 0.032(3) 0.000(3) 0.005(2) 0.003(3) N11 0.025(3) 0.042(3) 0.028(3) 0.008(2) 0.004(2) 0.000(3) N12 0.050(4) 0.056(4) 0.041(4) -0.001(3) 0.018(3) 0.013(3) O1 0.027(2) 0.039(3) 0.036(3) 0.002(2) 0.012(2) -0.001(2) O2 0.024(2) 0.035(3) 0.036(3) 0.004(2) 0.008(2) 0.0019(19) C1 0.032(4) 0.035(4) 0.046(4) -0.006(3) 0.002(3) -0.003(3) C2 0.027(3) 0.052(5) 0.052(5) 0.005(4) 0.010(3) 0.003(3) C3 0.032(3) 0.041(4) 0.043(4) 0.009(4) 0.015(3) 0.003(4) C4 0.031(4) 0.062(6) 0.056(5) -0.007(4) 0.000(4) 0.005(4) C5 0.045(5) 0.064(6) 0.053(5) 0.002(4) 0.025(4) 0.014(4) C6 0.048(5) 0.052(5) 0.036(4) 0.000(3) 0.013(4) 0.004(4) C7 0.069(6) 0.062(6) 0.034(4) 0.001(4) 0.015(4) -0.003(5) C8 0.045(5) 0.049(5) 0.051(5) 0.014(4) 0.013(4) 0.007(4) C9 0.070(6) 0.066(6) 0.051(5) -0.011(4) 0.021(5) 0.003(5) C10 0.105(8) 0.047(5) 0.066(6) 0.022(5) 0.035(6) -0.007(5) C11 0.031(4) 0.029(3) 0.037(4) -0.001(3) 0.011(3) -0.002(3) C12 0.033(4) 0.036(4) 0.025(3) -0.012(3) 0.006(3) 0.000(3) C13 0.038(4) 0.034(4) 0.043(4) 0.014(3) 0.021(3) 0.014(3) C14 0.042(4) 0.055(5) 0.050(5) 0.014(4) 0.015(4) 0.005(4) C15 0.039(4) 0.023(3) 0.049(4) 0.001(3) 0.017(3) 0.002(3) C16 0.054(5) 0.037(4) 0.054(5) -0.006(4) 0.025(4) 0.000(4) C17 0.084(7) 0.069(6) 0.061(6) -0.016(5) 0.044(5) 0.002(6) C18 0.075(7) 0.045(5) 0.059(6) -0.007(4) 0.009(5) -0.016(5) C19 0.054(6) 0.060(6) 0.067(6) -0.005(5) 0.017(5) -0.020(5) C20 0.040(4) 0.050(5) 0.063(5) -0.010(4) 0.019(4) -0.012(4) C21 0.152(12) 0.064(7) 0.064(7) -0.024(6) 0.045(7) -0.039(8) C22 0.126(11) 0.055(7) 0.092(8) 0.021(6) 0.029(8) 0.050(7) C23 0.049(6) 0.140(13) 0.090(9) 0.019(8) 0.003(6) -0.009(7) C24 0.065(7) 0.129(11) 0.095(9) 0.004(8) 0.050(7) 0.001(7) C25 0.033(4) 0.085(7) 0.062(6) 0.035(5) 0.022(4) 0.014(4) C26 0.029(4) 0.077(7) 0.071(6) 0.016(5) 0.004(4) -0.008(4) C27 0.033(4) 0.066(6) 0.060(5) 0.023(5) 0.008(4) -0.007(4) C28 0.065(6) 0.098(9) 0.098(8) 0.037(7) 0.049(6) 0.035(6) C29 0.037(4) 0.063(6) 0.077(6) 0.011(5) -0.010(4) -0.023(4) C30 0.042(4) 0.043(4) 0.031(4) 0.003(3) 0.004(3) 0.001(3) C31 0.059(5) 0.038(4) 0.032(4) 0.005(3) 0.011(4) -0.002(4) C32 0.041(4) 0.034(4) 0.039(4) 0.011(3) 0.010(3) 0.003(3) C33 0.060(5) 0.036(4) 0.060(5) 0.009(4) 0.007(4) -0.014(4) C34 0.044(4) 0.048(5) 0.032(4) 0.004(3) 0.007(3) 0.004(3) C35 0.024(3) 0.033(4) 0.040(4) -0.003(3) 0.008(3) -0.003(3) C36 0.028(3) 0.030(4) 0.038(4) 0.001(3) 0.010(3) -0.005(3) C37 0.031(4) 0.050(4) 0.032(4) 0.003(3) 0.013(3) 0.000(3) C38 0.037(4) 0.078(6) 0.046(5) 0.013(4) 0.019(4) 0.009(4) C39 0.045(4) 0.055(5) 0.036(4) 0.010(4) 0.011(3) 0.008(4) C40 0.059(5) 0.045(5) 0.046(4) -0.004(4) 0.014(4) 0.001(4) C41 0.078(7) 0.065(7) 0.061(6) -0.025(5) 0.013(5) -0.009(5) C42 0.084(8) 0.101(10) 0.037(5) -0.019(5) 0.002(5) 0.017(7) C43 0.088(8) 0.128(11) 0.039(5) 0.003(6) 0.019(6) 0.025(8) C44 0.060(6) 0.087(7) 0.041(5) 0.010(5) 0.019(4) 0.017(5) C45 0.076(8) 0.102(9) 0.061(6) 0.013(6) 0.037(6) -0.005(7) C46 0.151(14) 0.145(14) 0.077(9) -0.023(9) 0.052(9) -0.060(12) C47 0.133(12) 0.070(8) 0.101(10) -0.024(7) 0.053(9) -0.012(8) C48 0.181(18) 0.079(10) 0.151(15) -0.013(10) 0.031(13) 0.064(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 N6 2.303(6) . ? Nd1 O2 2.386(4) . ? Nd1 N11 2.485(5) . ? Nd1 O1 2.523(5) . ? Nd1 N3 2.605(6) . ? Nd1 N1 2.660(5) . ? Nd1 C12 2.726(7) . ? Nd1 C36 2.894(7) . ? Nd1 C11 2.903(7) . ? Nd1 Si1 3.164(2) . ? Nd1 Nd2 3.8479(5) . ? Nd2 N12 2.314(7) . ? Nd2 O1 2.401(5) . ? Nd2 N5 2.479(5) . ? Nd2 O2 2.541(5) . ? Nd2 N7 2.595(6) . ? Nd2 N9 2.710(6) . ? Nd2 C36 2.721(7) . ? Nd2 C12 2.916(7) . ? Nd2 C35 2.925(7) . ? Nd2 Si4 3.200(3) . ? Si1 N6 1.679(7) . ? Si1 C21 1.837(10) . ? Si1 C22 1.871(10) . ? Si2 N6 1.704(7) . ? Si2 C24 1.872(13) . ? Si2 C23 1.872(11) . ? Si3 N12 1.677(8) . ? Si3 C46 1.760(14) . ? Si3 C45 1.848(12) . ? Si4 N12 1.714(8) . ? Si4 C48 1.775(8) . ? Si4 C47 1.822(13) . ? N1 C3 1.361(9) . ? N1 N2 1.405(8) . ? N2 C1 1.368(9) . ? N2 C11 1.417(9) . ? N3 C8 1.329(10) . ? N3 N4 1.381(8) . ? N4 C6 1.342(10) . ? N4 C11 1.416(9) . ? N5 C12 1.324(9) . ? N5 C13 1.458(9) . ? N7 C25 1.363(10) . ? N7 N8 1.385(9) . ? N8 C27 1.378(10) . ? N8 C35 1.429(10) . ? N9 C32 1.337(9) . ? N9 N10 1.387(8) . ? N10 C35 1.377(9) . ? N10 C30 1.381(9) . ? N11 C36 1.313(9) . ? N11 C37 1.473(9) . ? O1 C12 1.349(8) . ? O2 C36 1.342(8) . ? C1 C2 1.357(11) . ? C1 C4 1.515(11) . ? C2 C3 1.433(10) . ? C3 C5 1.508(12) . ? C6 C7 1.395(12) . ? C6 C9 1.471(12) . ? C7 C8 1.368(12) . ? C8 C10 1.542(13) . ? C11 C12 1.399(10) . ? C13 C15 1.483(11) . ? C13 C14 1.533(10) . ? C15 C16 1.409(11) . ? C15 C20 1.419(11) . ? C16 C17 1.412(12) . ? C17 C18 1.411(14) . ? C18 C19 1.370(14) . ? C19 C20 1.398(12) . ? C25 C26 1.402(14) . ? C25 C28 1.446(14) . ? C26 C27 1.354(14) . ? C27 C29 1.454(14) . ? C30 C31 1.372(11) . ? C30 C34 1.459(10) . ? C31 C32 1.388(10) . ? C32 C33 1.490(11) . ? C35 C36 1.422(10) . ? C37 C39 1.532(11) . ? C37 C38 1.550(11) . ? C39 C40 1.373(12) . ? C39 C44 1.405(12) . ? C40 C41 1.432(12) . ? C41 C42 1.363(16) . ? C42 C43 1.384(17) . ? C43 C44 1.379(14) . ? C71 C77 1.244(10) . ? C71 C72 1.3900(15) . ? C71 C76 1.3900 . ? C72 C73 1.3900 . ? C73 C74 1.3900 . ? C74 C75 1.3900 . ? C75 C76 1.3900(19) . ? C81 C82 1.3900 . ? C81 C86 1.3900 . ? C81 C87 1.414(9) . ? C82 C83 1.3900 . ? C83 C84 1.3900 . ? C84 C85 1.3900 . ? C85 C86 1.3900 . ? C91 C92 1.3900 . ? C91 C96 1.3900 . ? C92 C93 1.3900 . ? C93 C94 1.3900 . ? C94 C95 1.3900 . ? C95 C97 1.25(3) . ? C95 C96 1.3900 . ? 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 N6 Nd1 O2 89.89(19) . . ? N6 Nd1 N11 106.5(2) . . ? O2 Nd1 N11 54.24(18) . . ? N6 Nd1 O1 129.0(2) . . ? O2 Nd1 O1 68.05(16) . . ? N11 Nd1 O1 96.82(18) . . ? N6 Nd1 N3 87.6(2) . . ? O2 Nd1 N3 129.63(19) . . ? N11 Nd1 N3 165.74(18) . . ? O1 Nd1 N3 75.06(18) . . ? N6 Nd1 N1 124.4(2) . . ? O2 Nd1 N1 140.95(16) . . ? N11 Nd1 N1 94.52(18) . . ? O1 Nd1 N1 97.34(16) . . ? N3 Nd1 N1 75.28(19) . . ? N6 Nd1 C12 154.5(2) . . ? O2 Nd1 C12 88.48(19) . . ? N11 Nd1 C12 93.0(2) . . ? O1 Nd1 C12 29.47(18) . . ? N3 Nd1 C12 74.1(2) . . ? N1 Nd1 C12 68.47(19) . . ? N6 Nd1 C36 99.4(2) . . ? O2 Nd1 C36 27.34(18) . . ? N11 Nd1 C36 26.9(2) . . ? O1 Nd1 C36 81.72(18) . . ? N3 Nd1 C36 154.6(2) . . ? N1 Nd1 C36 118.43(19) . . ? C12 Nd1 C36 90.7(2) . . ? N6 Nd1 C11 139.1(2) . . ? O2 Nd1 C11 116.14(18) . . ? N11 Nd1 C11 114.25(19) . . ? O1 Nd1 C11 50.10(17) . . ? N3 Nd1 C11 51.56(19) . . ? N1 Nd1 C11 50.92(19) . . ? C12 Nd1 C11 28.6(2) . . ? C36 Nd1 C11 118.4(2) . . ? N6 Nd1 Si1 30.96(17) . . ? O2 Nd1 Si1 110.60(13) . . ? N11 Nd1 Si1 99.62(15) . . ? O1 Nd1 Si1 157.89(12) . . ? N3 Nd1 Si1 91.47(15) . . ? N1 Nd1 Si1 96.01(13) . . ? C12 Nd1 Si1 160.83(15) . . ? C36 Nd1 Si1 107.09(15) . . ? C11 Nd1 Si1 132.41(15) . . ? N6 Nd1 Nd2 128.30(16) . . ? O2 Nd1 Nd2 40.12(11) . . ? N11 Nd1 Nd2 60.36(15) . . ? O1 Nd1 Nd2 37.48(11) . . ? N3 Nd1 Nd2 112.54(15) . . ? N1 Nd1 Nd2 106.99(12) . . ? C12 Nd1 Nd2 49.11(15) . . ? C36 Nd1 Nd2 44.89(14) . . ? C11 Nd1 Nd2 77.58(14) . . ? Si1 Nd1 Nd2 150.01(5) . . ? N12 Nd2 O1 90.5(2) . . ? N12 Nd2 N5 100.5(2) . . ? O1 Nd2 N5 54.11(17) . . ? N12 Nd2 O2 134.2(2) . . ? O1 Nd2 O2 67.51(15) . . ? N5 Nd2 O2 97.83(17) . . ? N12 Nd2 N7 92.5(2) . . ? O1 Nd2 N7 123.99(18) . . ? N5 Nd2 N7 166.8(2) . . ? O2 Nd2 N7 70.99(18) . . ? N12 Nd2 N9 122.1(2) . . ? O1 Nd2 N9 142.24(18) . . ? N5 Nd2 N9 97.97(18) . . ? O2 Nd2 N9 96.09(16) . . ? N7 Nd2 N9 76.83(18) . . ? N12 Nd2 C36 160.5(2) . . ? O1 Nd2 C36 87.7(2) . . ? N5 Nd2 C36 94.2(2) . . ? O2 Nd2 C36 29.30(18) . . ? N7 Nd2 C36 72.6(2) . . ? N9 Nd2 C36 67.7(2) . . ? N12 Nd2 C12 97.0(2) . . ? O1 Nd2 C12 27.26(19) . . ? N5 Nd2 C12 26.9(2) . . ? O2 Nd2 C12 81.51(17) . . ? N7 Nd2 C12 149.2(2) . . ? N9 Nd2 C12 120.8(2) . . ? C36 Nd2 C12 90.3(2) . . ? N12 Nd2 C35 142.8(2) . . ? O1 Nd2 C35 115.51(18) . . ? N5 Nd2 C35 116.09(19) . . ? O2 Nd2 C35 49.87(17) . . ? N7 Nd2 C35 51.4(2) . . ? N9 Nd2 C35 49.34(19) . . ? C36 Nd2 C35 28.9(2) . . ? C12 Nd2 C35 118.46(19) . . ? N12 Nd2 Si4 31.28(19) . . ? O1 Nd2 Si4 114.43(13) . . ? N5 Nd2 Si4 97.81(15) . . ? O2 Nd2 Si4 161.12(13) . . ? N7 Nd2 Si4 94.55(17) . . ? N9 Nd2 Si4 92.14(14) . . ? C36 Nd2 Si4 157.86(16) . . ? C12 Nd2 Si4 108.66(14) . . ? C35 Nd2 Si4 129.66(15) . . ? N12 Nd2 Nd1 129.62(17) . . ? O1 Nd2 Nd1 39.74(12) . . ? N5 Nd2 Nd1 61.46(14) . . ? O2 Nd2 Nd1 37.22(10) . . ? N7 Nd2 Nd1 108.10(15) . . ? N9 Nd2 Nd1 107.40(13) . . ? C36 Nd2 Nd1 48.65(15) . . ? C12 Nd2 Nd1 44.96(13) . . ? C35 Nd2 Nd1 77.40(14) . . ? Si4 Nd2 Nd1 152.73(6) . . ? N6 Si1 C21 117.5(5) . . ? N6 Si1 C22 114.9(5) . . ? C21 Si1 C22 109.1(6) . . ? N6 Si1 Nd1 44.9(2) . . ? C21 Si1 Nd1 133.6(4) . . ? C22 Si1 Nd1 117.2(4) . . ? N6 Si2 C24 110.0(4) . . ? N6 Si2 C23 112.0(5) . . ? C24 Si2 C23 108.8(6) . . ? N12 Si3 C46 112.8(6) . . ? N12 Si3 C45 110.2(5) . . ? C46 Si3 C45 109.8(7) . . ? N12 Si4 C48 117.8(4) . . ? N12 Si4 C47 116.4(5) . . ? C48 Si4 C47 106.2(6) . . ? N12 Si4 Nd2 44.5(2) . . ? C48 Si4 Nd2 125.7(4) . . ? C47 Si4 Nd2 127.9(5) . . ? C3 N1 N2 104.9(5) . . ? C3 N1 Nd1 151.0(5) . . ? N2 N1 Nd1 101.6(4) . . ? C1 N2 N1 110.4(6) . . ? C1 N2 C11 132.1(6) . . ? N1 N2 C11 116.6(5) . . ? C8 N3 N4 104.6(6) . . ? C8 N3 Nd1 145.3(5) . . ? N4 N3 Nd1 98.7(4) . . ? C6 N4 N3 111.0(6) . . ? C6 N4 C11 129.9(6) . . ? N3 N4 C11 119.0(5) . . ? C12 N5 C13 120.2(5) . . ? C12 N5 Nd2 95.3(4) . . ? C13 N5 Nd2 144.4(4) . . ? Si1 N6 Si2 130.9(4) . . ? Si1 N6 Nd1 104.1(3) . . ? Si2 N6 Nd1 125.0(3) . . ? C25 N7 N8 103.5(7) . . ? C25 N7 Nd2 145.3(5) . . ? N8 N7 Nd2 101.1(4) . . ? C27 N8 N7 112.8(7) . . ? C27 N8 C35 128.6(7) . . ? N7 N8 C35 118.0(6) . . ? C32 N9 N10 106.7(6) . . ? C32 N9 Nd2 150.2(5) . . ? N10 N9 Nd2 101.3(4) . . ? C35 N10 C30 132.7(6) . . ? C35 N10 N9 117.2(5) . . ? C30 N10 N9 109.7(6) . . ? C36 N11 C37 121.0(6) . . ? C36 N11 Nd1 94.2(4) . . ? C37 N11 Nd1 144.8(5) . . ? Si3 N12 Si4 127.9(4) . . ? Si3 N12 Nd2 127.9(4) . . ? Si4 N12 Nd2 104.2(3) . . ? C12 O1 Nd2 98.2(4) . . ? C12 O1 Nd1 83.6(4) . . ? Nd2 O1 Nd1 102.78(17) . . ? C36 O2 Nd1 97.9(4) . . ? C36 O2 Nd2 82.8(4) . . ? Nd1 O2 Nd2 102.66(16) . . ? C2 C1 N2 108.4(6) . . ? C2 C1 C4 131.8(7) . . ? N2 C1 C4 119.4(7) . . ? C1 C2 C3 106.3(7) . . ? N1 C3 C2 109.9(7) . . ? N1 C3 C5 121.8(6) . . ? C2 C3 C5 128.3(7) . . ? N4 C6 C7 106.7(7) . . ? N4 C6 C9 123.8(8) . . ? C7 C6 C9 129.5(8) . . ? C8 C7 C6 105.4(8) . . ? N3 C8 C7 112.2(8) . . ? N3 C8 C10 120.0(8) . . ? C7 C8 C10 127.8(8) . . ? C12 C11 N4 119.3(6) . . ? C12 C11 N2 119.9(6) . . ? N4 C11 N2 114.0(6) . . ? C12 C11 Nd1 68.7(4) . . ? N4 C11 Nd1 85.4(4) . . ? N2 C11 Nd1 90.8(4) . . ? N5 C12 O1 112.3(6) . . ? N5 C12 C11 131.9(7) . . ? O1 C12 C11 115.4(6) . . ? N5 C12 Nd1 111.6(4) . . ? O1 C12 Nd1 66.9(3) . . ? C11 C12 Nd1 82.8(4) . . ? N5 C12 Nd2 57.8(3) . . ? O1 C12 Nd2 54.6(3) . . ? C11 C12 Nd2 167.5(5) . . ? Nd1 C12 Nd2 85.93(18) . . ? N5 C13 C15 114.1(6) . . ? N5 C13 C14 107.7(6) . . ? C15 C13 C14 110.4(6) . . ? C16 C15 C20 118.7(8) . . ? C16 C15 C13 121.2(7) . . ? C20 C15 C13 120.1(7) . . ? C15 C16 C17 118.4(8) . . ? C18 C17 C16 122.6(9) . . ? C19 C18 C17 117.9(9) . . ? C18 C19 C20 121.6(9) . . ? C19 C20 C15 120.8(9) . . ? N7 C25 C26 109.9(9) . . ? N7 C25 C28 121.2(10) . . ? C26 C25 C28 128.9(9) . . ? C27 C26 C25 108.8(8) . . ? C26 C27 N8 104.8(9) . . ? C26 C27 C29 132.0(9) . . ? N8 C27 C29 123.2(8) . . ? C31 C30 N10 105.9(6) . . ? C31 C30 C34 131.1(7) . . ? N10 C30 C34 123.0(7) . . ? C30 C31 C32 108.3(7) . . ? N9 C32 C31 109.4(7) . . ? N9 C32 C33 121.3(7) . . ? C31 C32 C33 129.3(7) . . ? N10 C35 C36 121.4(6) . . ? N10 C35 N8 116.0(6) . . ? C36 C35 N8 116.5(6) . . ? N10 C35 Nd2 92.0(4) . . ? C36 C35 Nd2 67.6(4) . . ? N8 C35 Nd2 86.2(4) . . ? N11 C36 O2 113.6(6) . . ? N11 C36 C35 131.1(7) . . ? O2 C36 C35 114.9(6) . . ? N11 C36 Nd2 109.6(5) . . ? O2 C36 Nd2 67.9(4) . . ? C35 C36 Nd2 83.5(4) . . ? N11 C36 Nd1 58.9(4) . . ? O2 C36 Nd1 54.7(3) . . ? C35 C36 Nd1 168.0(5) . . ? Nd2 C36 Nd1 86.5(2) . . ? N11 C37 C39 112.4(6) . . ? N11 C37 C38 107.5(6) . . ? C39 C37 C38 109.3(7) . . ? C40 C39 C44 117.1(8) . . ? C40 C39 C37 124.3(7) . . ? C44 C39 C37 118.6(8) . . ? C39 C40 C41 121.6(9) . . ? C42 C41 C40 118.9(10) . . ? C41 C42 C43 120.6(9) . . ? C44 C43 C42 119.7(11) . . ? C43 C44 C39 122.0(11) . . ? C77 C71 C72 110.9(5) . . ? C77 C71 C76 129.0(5) . . ? C72 C71 C76 120.00(6) . . ? C73 C72 C71 120.00(6) . . ? C72 C73 C74 120.0 . . ? C73 C74 C75 120.0 . . ? C76 C75 C74 120.00(5) . . ? C75 C76 C71 120.0 . . ? C82 C81 C86 120.0 . . ? C82 C81 C87 121.7(4) . . ? C86 C81 C87 118.3(4) . . ? C81 C82 C83 120.0 . . ? C84 C83 C82 120.0 . . ? C83 C84 C85 120.0 . . ? C86 C85 C84 120.0 . . ? C85 C86 C81 120.0 . . ? C92 C91 C96 120.0 . . ? C93 C92 C91 120.0 . . ? C94 C93 C92 120.0 . . ? C93 C94 C95 120.0 . . ? C97 C95 C94 117.3(14) . . ? C97 C95 C96 122.7(14) . . ? C94 C95 C96 120.0 . . ? C95 C96 C91 120.0 . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.427 _refine_diff_density_min -0.561 _refine_diff_density_rms 0.126 #=====end data_4 _database_code_depnum_ccdc_archive 'CCDC 766527' #TrackingRef '- 1_4.cif' # start Validation Reply Form _vrf_CHEMW03_4 ; PROBLEM: The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.90 <> 1.10 From the CIF: _cell_formula_units_Z 4 From the CIF: _chemical_formula_weight 1536.71 RESPONSE: This alert and related are due to the squeeze application has been used. See above. ; _vrf_PLAT605_4 ; PROBLEM: Structure Contains Solvent Accessible VOIDS of . 225.00 A**3 RESPONSE: The compound crystallise with one molecule of toluene solvent. Other toluene molecules were found heavily disordered. An investigation of the void space in the structure show two principal voids of about 224 A3 in the unit cell. The option squeeze in Platon (Spek, A. L. Acta Crystallogr. 1990, A46, C-34) was used to eliminate the contribution of the electron density in the solvent region from the intensity data. The total electron density taken into account was 77 electrons per void, equivalent to 1.5 toluene molecule per void. The derived quantities (Mr, F(000), and Dx in the Crystal data are corrected with the contribution from this disordered solvent. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H74 N12 O2 Si4 Sm2, 4(C7 H8)' _chemical_formula_sum 'C68 H106 N12 O2 Si4 Sm2' _chemical_formula_weight 1536.71 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.639(6) _cell_length_b 26.133(13) _cell_length_c 19.332(9) _cell_angle_alpha 90.00 _cell_angle_beta 94.835(7) _cell_angle_gamma 90.00 _cell_volume 6363(5) _cell_formula_units_Z 4 _cell_measurement_temperature 230(2) _cell_measurement_reflns_used 1193 _cell_measurement_theta_min 2.246 _cell_measurement_theta_max 16.702 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.604 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3176 _exptl_absorpt_coefficient_mu 1.961 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6318 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 230(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCd area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26689 _diffrn_reflns_av_R_equivalents 0.1493 _diffrn_reflns_av_sigmaI/netI 0.2145 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11032 _reflns_number_gt 4899 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT, SADABS, XPREP' _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. ; # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 224 77 ' ' 2 0.183 0.227 0.260 7 2 ' ' 3 0.241 0.159 0.344 8 2 ' ' 4 0.500 0.500 0.500 224 76 ' ' 5 0.258 0.659 0.156 8 2 ' ' 6 0.317 0.727 0.240 7 3 ' ' 7 0.683 0.273 0.760 7 2 ' ' 8 0.741 0.341 0.844 8 2 ' ' 9 0.758 0.841 0.656 8 2 ' ' 10 0.817 0.773 0.740 7 3 ' ' _platon_squeeze_details ? _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^)+(0.1019P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11032 _refine_ls_number_parameters 568 _refine_ls_number_restraints 99 _refine_ls_R_factor_all 0.1630 _refine_ls_R_factor_gt 0.0888 _refine_ls_wR_factor_ref 0.2311 _refine_ls_wR_factor_gt 0.1973 _refine_ls_goodness_of_fit_ref 0.936 _refine_ls_restrained_S_all 0.985 _refine_ls_shift/su_max 0.031 _refine_ls_shift/su_mean 0.004 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 0.29392(6) 0.36784(3) 0.08667(3) 0.0299(2) Uani 1 1 d . D . Sm2 Sm 0.34365(6) 0.22789(3) 0.04404(4) 0.0376(3) Uani 1 1 d . D . Si1 Si 0.1662(4) 0.3625(2) 0.2363(2) 0.0714(16) Uani 1 1 d . . . HI1 H 0.2161 0.3337 0.2402 0.086 Uiso 1 1 calc R A 1 Si2 Si 0.1454(4) 0.45676(18) 0.1414(2) 0.0561(13) Uani 1 1 d . . . HI2 H 0.1749 0.4622 0.0967 0.067 Uiso 1 1 calc R D . Si3 Si 0.4839(5) 0.1258(3) 0.0415(3) 0.095(2) Uiso 1 1 d . . . HI3 H 0.4494 0.1371 -0.0033 0.114 Uiso 1 1 calc R B 1 Si4 Si 0.5184(4) 0.18089(19) 0.1795(2) 0.0602(14) Uani 1 1 d . . . HI4 H 0.5297 0.1472 0.2010 0.072 Uiso 1 1 calc R C 1 N1 N 0.3722(9) 0.4198(4) -0.0115(5) 0.030(3) Uani 1 1 d . . . N2 N 0.4761(9) 0.4068(4) -0.0094(5) 0.034(3) Uani 1 1 d . D . N3 N 0.4575(9) 0.4085(4) 0.1475(5) 0.035(3) Uani 1 1 d . . . N4 N 0.5404(9) 0.3890(4) 0.1098(6) 0.036(3) Uani 1 1 d . D . N5 N 0.4578(9) 0.2871(5) -0.0154(6) 0.041(3) Uani 1 1 d . . . N6 N 0.1944(8) 0.4003(4) 0.1703(5) 0.039(3) Uani 1 1 d . D . N7 N 0.2258(10) 0.2102(4) -0.0710(5) 0.036(3) Uani 1 1 d . . . N8 N 0.1232(10) 0.2193(4) -0.0526(6) 0.039(3) Uani 1 1 d . D . N9 N 0.1989(13) 0.1736(5) 0.0884(7) 0.061(4) Uani 1 1 d . . . N10 N 0.1057(11) 0.2029(6) 0.0673(7) 0.054(4) Uani 1 1 d . D . N11 N 0.1631(8) 0.3296(4) 0.0013(5) 0.030(3) Uani 1 1 d . . . N12 N 0.4597(11) 0.1739(5) 0.0979(6) 0.063(4) Uani 1 1 d . D . O1 O 0.4295(6) 0.3001(3) 0.0957(4) 0.031(2) Uani 1 1 d . . . O2 O 0.2175(7) 0.2858(3) 0.0961(4) 0.032(2) Uani 1 1 d . . . C1 C 0.5304(13) 0.4342(6) -0.0527(7) 0.044(4) Uani 1 1 d . . . C2 C 0.4589(14) 0.4665(6) -0.0848(8) 0.054(4) Uani 1 1 d . D . H2 H 0.4716 0.4909 -0.1181 0.065 Uiso 1 1 calc R . . C3 C 0.3606(13) 0.4557(5) -0.0578(7) 0.041(4) Uani 1 1 d . D . C4 C 0.6455(12) 0.4286(7) -0.0602(8) 0.072(6) Uani 1 1 d . D . H4A H 0.6739 0.4019 -0.0300 0.108 Uiso 1 1 calc R . . H4B H 0.6810 0.4602 -0.0481 0.108 Uiso 1 1 calc R . . H4C H 0.6561 0.4200 -0.1074 0.108 Uiso 1 1 calc R . . C5 C 0.2598(13) 0.4815(7) -0.0794(8) 0.067(5) Uani 1 1 d . . . H5A H 0.2043 0.4677 -0.0540 0.101 Uiso 1 1 calc R D . H5B H 0.2424 0.4763 -0.1282 0.101 Uiso 1 1 calc R . . H5C H 0.2667 0.5175 -0.0701 0.101 Uiso 1 1 calc R . . C6 C 0.6332(14) 0.3904(6) 0.1472(8) 0.046(4) Uani 1 1 d . . . C7 C 0.6158(13) 0.4133(6) 0.2072(7) 0.046(4) Uani 1 1 d . D . H7 H 0.6676 0.4210 0.2427 0.055 Uiso 1 1 calc R . . C8 C 0.5063(12) 0.4240(5) 0.2079(7) 0.038(4) Uani 1 1 d . D . C9 C 0.7313(13) 0.3693(6) 0.1190(9) 0.069(5) Uani 1 1 d . D . H9A H 0.7134 0.3553 0.0736 0.104 Uiso 1 1 calc R . . H9B H 0.7609 0.3429 0.1493 0.104 Uiso 1 1 calc R . . H9C H 0.7824 0.3962 0.1161 0.104 Uiso 1 1 calc R . . C10 C 0.4479(11) 0.4456(8) 0.2642(7) 0.070(6) Uani 1 1 d . . . H10A H 0.3739 0.4482 0.2488 0.105 Uiso 1 1 calc R D . H10B H 0.4754 0.4790 0.2762 0.105 Uiso 1 1 calc R . . H10C H 0.4566 0.4237 0.3041 0.105 Uiso 1 1 calc R . . C12 C 0.5159(11) 0.3679(6) 0.0411(7) 0.042(4) Uani 1 1 d . . . C13 C 0.4715(12) 0.3191(6) 0.0363(7) 0.042(4) Uani 1 1 d . D . C14 C 0.5141(12) 0.2985(7) -0.0781(8) 0.056(5) Uani 1 1 d . E . H14 H 0.5625 0.3270 -0.0659 0.067 Uiso 1 1 calc R . . C15 C 0.4423(15) 0.3156(8) -0.1386(9) 0.089(7) Uani 1 1 d . . . H15A H 0.4032 0.3451 -0.1259 0.134 Uiso 1 1 calc R E . H15B H 0.3937 0.2885 -0.1525 0.134 Uiso 1 1 calc R . . H15C H 0.4836 0.3241 -0.1764 0.134 Uiso 1 1 calc R . . C16 C 0.5823(14) 0.2529(8) -0.0945(10) 0.078(6) Uani 1 1 d D . . H16A H 0.5369 0.2231 -0.1015 0.094 Uiso 1 1 calc R E . H16B H 0.6136 0.2595 -0.1378 0.094 Uiso 1 1 calc R . . C19 C 0.1646(18) 0.3943(9) 0.3216(10) 0.121(9) Uani 1 1 d . D . H19A H 0.1481 0.3697 0.3559 0.181 Uiso 1 1 calc R . . H19B H 0.1118 0.4208 0.3187 0.181 Uiso 1 1 calc R . . H19C H 0.2331 0.4090 0.3344 0.181 Uiso 1 1 calc R . . C20 C 0.0022(13) 0.4633(8) 0.1234(10) 0.087(7) Uani 1 1 d . D . H20A H -0.0247 0.4350 0.0957 0.130 Uiso 1 1 calc R . . H20B H -0.0133 0.4947 0.0987 0.130 Uiso 1 1 calc R . . H20C H -0.0308 0.4638 0.1664 0.130 Uiso 1 1 calc R . . C21 C 0.1818(17) 0.5125(7) 0.1922(10) 0.100(7) Uani 1 1 d . D . H21A H 0.2570 0.5123 0.2045 0.150 Uiso 1 1 calc R . . H21B H 0.1450 0.5124 0.2337 0.150 Uiso 1 1 calc R . . H21C H 0.1629 0.5427 0.1657 0.150 Uiso 1 1 calc R . . C22 C 0.0502(13) 0.2046(5) -0.1024(7) 0.041(4) Uani 1 1 d . . . C23 C 0.1049(15) 0.1858(6) -0.1569(8) 0.063(5) Uani 1 1 d . E . H23 H 0.0759 0.1723 -0.1988 0.075 Uiso 1 1 calc R . . C24 C 0.2180(14) 0.1917(6) -0.1341(8) 0.050(4) Uani 1 1 d . E . C25 C -0.0642(12) 0.2085(7) -0.0974(8) 0.059(6) Uani 1 1 d . E . H25A H -0.0773 0.2232 -0.0534 0.089 Uiso 1 1 calc R . . H25B H -0.0954 0.1750 -0.1012 0.089 Uiso 1 1 calc R . . H25C H -0.0950 0.2298 -0.1341 0.089 Uiso 1 1 calc R . . C26 C 0.3068(12) 0.1807(6) -0.1740(8) 0.066(5) Uani 1 1 d . . . H26A H 0.3719 0.1883 -0.1467 0.099 Uiso 1 1 calc R E . H26B H 0.3019 0.2014 -0.2153 0.099 Uiso 1 1 calc R . . H26C H 0.3057 0.1452 -0.1867 0.099 Uiso 1 1 calc R . . C27 C 0.0327(15) 0.1900(10) 0.1141(11) 0.066(7) Uani 1 1 d . . . C28 C 0.085(4) 0.1576(11) 0.1571(13) 0.071(2) Uiso 1 1 d . E . H28 H 0.0534 0.1429 0.1941 0.085 Uiso 1 1 calc R . . C29 C 0.179(2) 0.1474(13) 0.1459(17) 0.109(12) Uani 1 1 d . E . C30 C -0.0712(19) 0.2172(10) 0.0993(11) 0.076(10) Uani 1 1 d . E . H30A H -0.0688 0.2376 0.0582 0.114 Uiso 1 1 calc R . . H30B H -0.0840 0.2388 0.1378 0.114 Uiso 1 1 calc R . . H30C H -0.1273 0.1925 0.0923 0.114 Uiso 1 1 calc R . . C31 C 0.246(2) 0.1101(8) 0.1822(11) 0.103(12) Uani 1 1 d . . . H31A H 0.3125 0.1087 0.1624 0.155 Uiso 1 1 calc R E . H31B H 0.2119 0.0772 0.1784 0.155 Uiso 1 1 calc R . . H31C H 0.2568 0.1196 0.2303 0.155 Uiso 1 1 calc R . . C32 C 0.1119(12) 0.2391(6) 0.0161(8) 0.046(4) Uani 1 1 d . . . C33 C 0.1618(11) 0.2873(6) 0.0349(7) 0.042(4) Uani 1 1 d . D . C34 C 0.0938(12) 0.3366(6) -0.0641(8) 0.050(4) Uani 1 1 d . D . H34 H 0.0503 0.3058 -0.0722 0.060 Uiso 1 1 calc R . . C35 C 0.1629(15) 0.3425(7) -0.1229(7) 0.074(6) Uani 1 1 d . . . H35A H 0.2044 0.3120 -0.1269 0.112 Uiso 1 1 calc R D . H35B H 0.2093 0.3712 -0.1141 0.112 Uiso 1 1 calc R . . H35C H 0.1192 0.3480 -0.1653 0.112 Uiso 1 1 calc R . . C36 C 0.0245(15) 0.3823(8) -0.0572(11) 0.093(7) Uani 1 1 d D . . H36A H 0.0637 0.4083 -0.0299 0.112 Uiso 1 1 calc R D . H36B H 0.0047 0.3964 -0.1029 0.112 Uiso 1 1 calc R . . C17 C 0.673(2) 0.2403(15) -0.0375(15) 0.138(17) Uiso 1 1 d D E . H17A H 0.7108 0.2105 -0.0510 0.206 Uiso 1 1 calc R . . H17B H 0.6432 0.2338 0.0057 0.206 Uiso 1 1 calc R . . H17C H 0.7211 0.2687 -0.0321 0.206 Uiso 1 1 calc R . . C37 C -0.073(2) 0.3683(11) -0.0230(13) 0.159(11) Uiso 1 1 d D D . H37A H -0.1157 0.3983 -0.0179 0.238 Uiso 1 1 calc R . . H37B H -0.0537 0.3538 0.0218 0.238 Uiso 1 1 calc R . . H37C H -0.1138 0.3437 -0.0512 0.238 Uiso 1 1 calc R . . C18 C 0.033(3) 0.3386(16) 0.225(2) 0.064(11) Uiso 0.50 1 d P D 1 H18A H 0.0229 0.3210 0.1815 0.096 Uiso 0.50 1 calc PR D 1 H18B H -0.0156 0.3666 0.2258 0.096 Uiso 0.50 1 calc PR D 1 H18C H 0.0217 0.3153 0.2621 0.096 Uiso 0.50 1 calc PR D 1 C38 C 0.4199(18) 0.0613(10) 0.0584(12) 0.135(9) Uiso 1 1 d . E 1 H38A H 0.3471 0.0665 0.0675 0.202 Uiso 1 1 calc R E 1 H38B H 0.4574 0.0453 0.0978 0.202 Uiso 1 1 calc R E 1 H38C H 0.4228 0.0398 0.0184 0.202 Uiso 1 1 calc R E 1 C39 C 0.6096(17) 0.1141(10) 0.0257(11) 0.122(8) Uiso 1 1 d . E 1 H39A H 0.6445 0.1458 0.0168 0.183 Uiso 1 1 calc R E 1 H39B H 0.6108 0.0921 -0.0139 0.183 Uiso 1 1 calc R E 1 H39C H 0.6459 0.0978 0.0654 0.183 Uiso 1 1 calc R E 1 C40 C 0.4306(13) 0.2195(6) 0.2311(8) 0.067(5) Uiso 1 1 d . E 1 H40A H 0.3633 0.2026 0.2322 0.101 Uiso 1 1 calc R E 1 H40B H 0.4202 0.2526 0.2103 0.101 Uiso 1 1 calc R E 1 H40C H 0.4629 0.2232 0.2776 0.101 Uiso 1 1 calc R E 1 C41 C 0.6458(15) 0.2158(7) 0.1828(10) 0.089(6) Uiso 1 1 d . E 1 H41A H 0.6949 0.1973 0.1570 0.133 Uiso 1 1 calc R E 1 H41B H 0.6743 0.2191 0.2302 0.133 Uiso 1 1 calc R E 1 H41C H 0.6343 0.2492 0.1629 0.133 Uiso 1 1 calc R E 1 C18A C 0.050(3) 0.3155(16) 0.214(2) 0.079(13) Uiso 0.50 1 d P D 2 H18D H 0.0568 0.3012 0.1686 0.119 Uiso 0.50 1 calc PR D 2 H18E H -0.0158 0.3335 0.2139 0.119 Uiso 0.50 1 calc PR D 2 H18F H 0.0527 0.2886 0.2476 0.119 Uiso 0.50 1 calc PR D 2 C61 C 0.2661(15) 0.4678(8) -0.3114(11) 0.095(6) Uani 1 1 d DU . . C62 C 0.1707(15) 0.4735(7) -0.2827(8) 0.087(5) Uani 1 1 d DU . . H62 H 0.1520 0.4517 -0.2477 0.104 Uiso 1 1 calc R . . C63 C 0.1051(14) 0.5113(8) -0.3066(9) 0.111(6) Uani 1 1 d DU . . H63 H 0.0410 0.5164 -0.2872 0.133 Uiso 1 1 calc R . . C64 C 0.1327(16) 0.5424(7) -0.3595(10) 0.108(6) Uani 1 1 d DU . . H64 H 0.0860 0.5671 -0.3786 0.130 Uiso 1 1 calc R . . C65 C 0.2296(16) 0.5361(8) -0.3832(9) 0.098(6) Uani 1 1 d DU . . H65 H 0.2505 0.5589 -0.4164 0.118 Uiso 1 1 calc R . . C66 C 0.2979(15) 0.4983(9) -0.3608(11) 0.101(6) Uani 1 1 d DU . . H66 H 0.3630 0.4939 -0.3791 0.122 Uiso 1 1 calc R . . C67 C 0.337(2) 0.4250(10) -0.2783(14) 0.155(10) Uani 1 1 d DU . . H67A H 0.3001 0.4076 -0.2438 0.233 Uiso 1 1 calc R . . H67B H 0.4014 0.4396 -0.2569 0.233 Uiso 1 1 calc R . . H67C H 0.3538 0.4012 -0.3135 0.233 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 0.0253(5) 0.0320(4) 0.0318(4) -0.0020(3) -0.0001(3) -0.0022(4) Sm2 0.0424(6) 0.0285(4) 0.0393(5) 0.0019(4) -0.0120(4) 0.0013(4) Si1 0.081(4) 0.090(4) 0.045(3) -0.006(3) 0.020(3) -0.007(3) Si2 0.052(3) 0.054(3) 0.064(3) -0.019(3) 0.015(3) -0.004(3) Si4 0.075(4) 0.051(3) 0.051(3) -0.001(2) -0.021(3) 0.018(3) N1 0.032(8) 0.033(6) 0.025(6) 0.005(5) 0.004(5) 0.008(6) N2 0.032(8) 0.036(7) 0.034(6) 0.005(6) 0.002(6) -0.004(6) N3 0.037(8) 0.040(7) 0.028(6) -0.008(6) 0.001(6) -0.013(6) N4 0.031(8) 0.037(7) 0.039(7) 0.002(6) 0.001(7) -0.002(6) N5 0.042(8) 0.043(7) 0.038(7) -0.008(6) 0.000(6) 0.002(6) N6 0.034(7) 0.038(7) 0.044(7) -0.014(6) 0.002(6) 0.000(6) N7 0.045(9) 0.030(6) 0.031(6) -0.016(6) -0.011(6) -0.007(6) N8 0.030(8) 0.041(7) 0.046(8) 0.004(6) 0.006(7) -0.005(6) N9 0.099(14) 0.035(8) 0.045(8) 0.028(7) -0.009(8) -0.025(8) N10 0.049(10) 0.060(9) 0.054(8) -0.012(8) 0.002(8) -0.030(8) N11 0.037(8) 0.011(5) 0.040(7) 0.011(5) 0.000(6) 0.004(5) N12 0.100(12) 0.036(8) 0.051(8) -0.014(7) -0.007(8) 0.005(8) O1 0.020(5) 0.037(5) 0.033(5) -0.003(5) -0.011(4) 0.002(4) O2 0.027(6) 0.041(6) 0.029(5) -0.001(4) 0.005(5) -0.019(5) C1 0.051(12) 0.054(10) 0.026(8) -0.001(8) 0.002(8) -0.031(9) C2 0.067(13) 0.043(10) 0.049(10) 0.004(9) -0.010(10) -0.011(10) C3 0.054(12) 0.035(9) 0.031(8) -0.002(7) -0.017(8) 0.002(8) C4 0.038(11) 0.107(16) 0.075(12) 0.024(12) 0.028(9) -0.013(11) C5 0.078(14) 0.064(12) 0.059(10) 0.008(10) 0.001(10) -0.012(11) C6 0.058(13) 0.037(9) 0.039(9) 0.023(8) -0.013(9) -0.005(9) C7 0.050(12) 0.054(10) 0.029(8) 0.004(8) -0.017(8) -0.012(9) C8 0.031(10) 0.038(9) 0.041(9) 0.009(7) -0.015(8) -0.026(8) C9 0.067(14) 0.056(11) 0.087(13) 0.008(11) 0.017(11) 0.007(10) C10 0.036(11) 0.132(18) 0.042(9) -0.011(11) 0.004(8) 0.006(11) C12 0.025(9) 0.054(10) 0.046(9) -0.004(9) -0.001(7) -0.005(8) C13 0.037(10) 0.054(10) 0.037(9) 0.017(9) 0.010(8) 0.027(9) C14 0.029(10) 0.070(12) 0.072(12) -0.034(10) 0.028(9) -0.011(9) C15 0.100(17) 0.102(17) 0.065(12) 0.005(12) -0.003(12) -0.024(14) C16 0.063(13) 0.081(14) 0.090(13) -0.028(12) -0.007(11) 0.015(12) C19 0.12(2) 0.15(2) 0.099(16) 0.025(16) 0.040(15) 0.030(18) C20 0.053(13) 0.091(15) 0.111(18) -0.025(14) -0.026(12) 0.035(12) C21 0.130(19) 0.065(13) 0.109(15) -0.007(13) 0.036(14) 0.001(14) C22 0.043(12) 0.035(8) 0.042(9) 0.002(8) -0.018(8) -0.013(8) C23 0.095(16) 0.051(11) 0.045(9) -0.015(9) 0.017(11) -0.001(11) C24 0.057(13) 0.035(9) 0.055(10) -0.007(8) -0.024(9) 0.006(9) C25 0.041(12) 0.079(15) 0.053(10) -0.025(11) -0.024(9) -0.018(11) C26 0.057(12) 0.072(12) 0.070(11) -0.035(10) 0.014(10) 0.024(10) C27 0.072(12) 0.062(2) 0.069(13) -0.024(14) 0.031(11) -0.034(13) C29 0.09(2) 0.11(2) 0.12(2) -0.03(2) -0.042(19) -0.022(19) C30 0.061(2) 0.081(3) 0.091(16) -0.030(17) 0.031(15) -0.038(2) C31 0.114(3) 0.078(16) 0.105(19) 0.055(16) -0.064(2) -0.035(19) C32 0.042(11) 0.035(9) 0.064(11) 0.012(9) 0.012(9) -0.006(8) C33 0.028(10) 0.059(11) 0.040(9) -0.026(9) 0.012(8) 0.004(8) C34 0.040(11) 0.040(9) 0.064(11) 0.007(9) -0.032(9) -0.004(8) C35 0.120(17) 0.067(12) 0.033(9) -0.007(9) -0.009(11) 0.041(12) C36 0.067(15) 0.079(15) 0.123(17) 0.009(14) -0.021(13) 0.012(12) C61 0.116(14) 0.078(11) 0.085(12) -0.042(10) -0.032(11) 0.008(11) C62 0.104(14) 0.068(11) 0.084(11) -0.006(10) -0.014(11) -0.022(11) C63 0.115(14) 0.109(14) 0.105(13) -0.021(12) -0.009(12) 0.001(12) C64 0.117(14) 0.104(14) 0.102(13) -0.020(11) -0.009(12) 0.011(13) C65 0.108(15) 0.114(14) 0.072(11) -0.013(11) 0.003(11) -0.024(12) C66 0.106(14) 0.107(14) 0.090(12) -0.033(11) -0.002(11) -0.001(11) C67 0.16(2) 0.106(19) 0.19(2) -0.052(17) -0.03(2) 0.020(17) _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 N6 2.294(10) . ? Sm1 O2 2.366(8) . ? Sm1 N11 2.449(11) . ? Sm1 O1 2.460(8) . ? Sm1 N3 2.526(11) . ? Sm1 N1 2.596(10) . ? Sm1 C33 2.818(16) . ? Sm1 C13 2.825(13) . ? Sm1 C12 3.012(13) . ? Sm1 Si2 3.221(5) . ? Sm1 Si1 3.432(5) . ? Sm1 Sm2 3.813(2) . ? Sm2 N12 2.230(13) . ? Sm2 O1 2.358(8) . ? Sm2 N5 2.465(11) . ? Sm2 O2 2.472(8) . ? Sm2 N9 2.523(13) . ? Sm2 N7 2.611(10) . ? Sm2 C33 2.767(15) . ? Sm2 C13 2.890(17) . ? Sm2 C32 2.949(15) . ? Sm2 Si3 3.205(7) . ? Si1 N6 1.676(12) . ? Si1 C18 1.79(4) . ? Si1 C19 1.85(2) . ? Si1 C18A 1.93(4) . ? Si2 N6 1.677(12) . ? Si2 C21 1.796(19) . ? Si2 C20 1.822(16) . ? Si3 C39 1.67(2) . ? Si3 N12 1.708(13) . ? Si3 C38 1.91(2) . ? Si4 N12 1.695(13) . ? Si4 C41 1.847(18) . ? Si4 C40 1.852(15) . ? N1 C3 1.296(16) . ? N1 N2 1.353(14) . ? N2 C1 1.336(16) . ? N2 C12 1.467(17) . ? N3 C8 1.335(15) . ? N3 N4 1.420(14) . ? N4 C6 1.326(17) . ? N4 C12 1.447(17) . ? N5 C13 1.302(17) . ? N5 C14 1.487(16) . ? N7 C24 1.309(16) . ? N7 N8 1.394(14) . ? N8 C22 1.334(17) . ? N8 C32 1.443(18) . ? N9 C29 1.35(3) . ? N9 N10 1.435(18) . ? N10 C32 1.377(18) . ? N10 C27 1.387(19) . ? N11 C33 1.283(17) . ? N11 C34 1.487(17) . ? O1 C13 1.397(14) . ? O2 C33 1.327(16) . ? C1 C2 1.35(2) . ? C1 C4 1.481(19) . ? C2 C3 1.416(19) . ? C3 C5 1.47(2) . ? C6 C7 1.340(19) . ? C6 C9 1.50(2) . ? C7 C8 1.413(19) . ? C8 C10 1.479(19) . ? C12 C13 1.40(2) . ? C14 C15 1.49(2) . ? C14 C16 1.52(2) . ? C16 C17 1.558(18) . ? C22 C23 1.396(18) . ? C22 C25 1.460(19) . ? C23 C24 1.47(2) . ? C24 C26 1.444(19) . ? C27 C28 1.32(3) . ? C27 C30 1.50(3) . ? C28 C29 1.25(5) . ? C29 C31 1.43(3) . ? C32 C33 1.44(2) . ? C34 C35 1.50(2) . ? C34 C36 1.49(2) . ? C36 C37 1.498(17) . ? C61 C66 1.33(3) . ? C61 C62 1.377(15) . ? C61 C67 1.54(3) . ? C62 C63 1.347(14) . ? C63 C64 1.375(15) . ? C64 C65 1.353(14) . ? C65 C66 1.359(15) . ? 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 N6 Sm1 O2 91.7(3) . . ? N6 Sm1 N11 104.3(4) . . ? O2 Sm1 N11 54.9(3) . . ? N6 Sm1 O1 129.5(3) . . ? O2 Sm1 O1 68.2(3) . . ? N11 Sm1 O1 100.5(3) . . ? N6 Sm1 N3 89.5(4) . . ? O2 Sm1 N3 132.0(3) . . ? N11 Sm1 N3 164.9(3) . . ? O1 Sm1 N3 74.4(3) . . ? N6 Sm1 N1 125.9(4) . . ? O2 Sm1 N1 135.6(3) . . ? N11 Sm1 N1 89.9(3) . . ? O1 Sm1 N1 97.0(3) . . ? N3 Sm1 N1 76.8(3) . . ? N6 Sm1 C33 100.6(4) . . ? O2 Sm1 C33 28.0(4) . . ? N11 Sm1 C33 27.1(4) . . ? O1 Sm1 C33 82.9(4) . . ? N3 Sm1 C33 156.5(4) . . ? N1 Sm1 C33 112.5(4) . . ? N6 Sm1 C13 155.4(4) . . ? O2 Sm1 C13 87.6(4) . . ? N11 Sm1 C13 95.4(4) . . ? O1 Sm1 C13 29.6(3) . . ? N3 Sm1 C13 73.0(4) . . ? N1 Sm1 C13 67.7(4) . . ? C33 Sm1 C13 90.3(4) . . ? N6 Sm1 C12 141.8(4) . . ? O2 Sm1 C12 114.8(4) . . ? N11 Sm1 C12 113.3(4) . . ? O1 Sm1 C12 50.2(4) . . ? N3 Sm1 C12 52.4(4) . . ? N1 Sm1 C12 50.5(4) . . ? C33 Sm1 C12 115.8(4) . . ? C13 Sm1 C12 27.4(4) . . ? N6 Sm1 Si2 29.8(3) . . ? O2 Sm1 Si2 112.1(2) . . ? N11 Sm1 Si2 97.8(2) . . ? O1 Sm1 Si2 156.6(2) . . ? N3 Sm1 Si2 91.2(3) . . ? N1 Sm1 Si2 97.5(3) . . ? C33 Sm1 Si2 108.1(3) . . ? C13 Sm1 Si2 160.2(4) . . ? C12 Sm1 Si2 132.7(3) . . ? N6 Sm1 Si1 25.3(3) . . ? O2 Sm1 Si1 71.0(2) . . ? N11 Sm1 Si1 102.3(2) . . ? O1 Sm1 Si1 106.6(2) . . ? N3 Sm1 Si1 92.8(2) . . ? N1 Sm1 Si1 150.8(2) . . ? C33 Sm1 Si1 87.8(3) . . ? C13 Sm1 Si1 135.7(3) . . ? C12 Sm1 Si1 139.7(3) . . ? Si2 Sm1 Si1 54.85(13) . . ? N6 Sm1 Sm2 128.2(3) . . ? O2 Sm1 Sm2 39.0(2) . . ? N11 Sm1 Sm2 65.0(2) . . ? O1 Sm1 Sm2 36.74(19) . . ? N3 Sm1 Sm2 111.1(3) . . ? N1 Sm1 Sm2 105.3(2) . . ? C33 Sm1 Sm2 46.4(3) . . ? C13 Sm1 Sm2 48.9(3) . . ? C12 Sm1 Sm2 76.3(3) . . ? Si2 Sm1 Sm2 150.94(9) . . ? Si1 Sm1 Sm2 103.93(10) . . ? N12 Sm2 O1 92.7(4) . . ? N12 Sm2 N5 103.1(4) . . ? O1 Sm2 N5 55.1(3) . . ? N12 Sm2 O2 128.2(4) . . ? O1 Sm2 O2 68.1(3) . . ? N5 Sm2 O2 103.2(3) . . ? N12 Sm2 N9 87.3(5) . . ? O1 Sm2 N9 128.9(4) . . ? N5 Sm2 N9 169.0(5) . . ? O2 Sm2 N9 72.2(4) . . ? N12 Sm2 N7 126.2(4) . . ? O1 Sm2 N7 135.4(3) . . ? N5 Sm2 N7 91.7(4) . . ? O2 Sm2 N7 96.6(3) . . ? N9 Sm2 N7 79.1(4) . . ? N12 Sm2 C33 153.6(4) . . ? O1 Sm2 C33 85.9(4) . . ? N5 Sm2 C33 97.7(4) . . ? O2 Sm2 C33 28.6(3) . . ? N9 Sm2 C33 73.4(5) . . ? N7 Sm2 C33 68.5(4) . . ? N12 Sm2 C13 101.4(4) . . ? O1 Sm2 C13 28.6(3) . . ? N5 Sm2 C13 26.6(3) . . ? O2 Sm2 C13 84.2(3) . . ? N9 Sm2 C13 155.0(4) . . ? N7 Sm2 C13 112.5(4) . . ? C33 Sm2 C13 90.0(4) . . ? N12 Sm2 C32 138.8(4) . . ? O1 Sm2 C32 114.4(4) . . ? N5 Sm2 C32 117.6(4) . . ? O2 Sm2 C32 49.4(4) . . ? N9 Sm2 C32 51.7(4) . . ? N7 Sm2 C32 51.3(4) . . ? C33 Sm2 C32 29.0(4) . . ? C13 Sm2 C32 117.4(4) . . ? N12 Sm2 Si3 30.4(3) . . ? O1 Sm2 Si3 115.9(2) . . ? N5 Sm2 Si3 99.7(3) . . ? O2 Sm2 Si3 153.1(2) . . ? N9 Sm2 Si3 87.4(4) . . ? N7 Sm2 Si3 96.6(3) . . ? C33 Sm2 Si3 157.4(3) . . ? C13 Sm2 Si3 111.9(3) . . ? C32 Sm2 Si3 128.5(3) . . ? N12 Sm2 Sm1 128.3(3) . . ? O1 Sm2 Sm1 38.6(2) . . ? N5 Sm2 Sm1 67.2(3) . . ? O2 Sm2 Sm1 37.02(18) . . ? N9 Sm2 Sm1 109.2(3) . . ? N7 Sm2 Sm1 105.2(2) . . ? C33 Sm2 Sm1 47.5(3) . . ? C13 Sm2 Sm1 47.4(3) . . ? C32 Sm2 Sm1 76.4(3) . . ? Si3 Sm2 Sm1 154.56(13) . . ? N6 Si1 C18 111.8(14) . . ? N6 Si1 C19 115.6(9) . . ? C18 Si1 C19 100.6(14) . . ? N6 Si1 C18A 114.2(13) . . ? C18 Si1 C18A 20.7(16) . . ? C19 Si1 C18A 115.0(14) . . ? N6 Si1 Sm1 35.8(4) . . ? C18 Si1 Sm1 114.6(12) . . ? C19 Si1 Sm1 140.8(8) . . ? C18A Si1 Sm1 103.7(12) . . ? N6 Si2 C21 117.4(8) . . ? N6 Si2 C20 118.7(8) . . ? C21 Si2 C20 103.4(9) . . ? N6 Si2 Sm1 42.8(4) . . ? C21 Si2 Sm1 129.4(7) . . ? C20 Si2 Sm1 127.0(6) . . ? C39 Si3 N12 118.3(11) . . ? C39 Si3 C38 107.0(12) . . ? N12 Si3 C38 116.0(9) . . ? C39 Si3 Sm2 133.7(9) . . ? N12 Si3 Sm2 41.4(5) . . ? C38 Si3 Sm2 119.3(8) . . ? N12 Si4 C41 113.4(8) . . ? N12 Si4 C40 109.0(7) . . ? C41 Si4 C40 105.8(8) . . ? C3 N1 N2 104.8(11) . . ? C3 N1 Sm1 148.8(10) . . ? N2 N1 Sm1 106.0(7) . . ? C1 N2 N1 113.2(12) . . ? C1 N2 C12 128.5(13) . . ? N1 N2 C12 118.1(10) . . ? C8 N3 N4 104.5(11) . . ? C8 N3 Sm1 146.5(9) . . ? N4 N3 Sm1 102.7(7) . . ? C6 N4 N3 111.6(11) . . ? C6 N4 C12 128.4(12) . . ? N3 N4 C12 119.9(11) . . ? C13 N5 C14 117.0(12) . . ? C13 N5 Sm2 95.2(9) . . ? C14 N5 Sm2 147.7(9) . . ? Si2 N6 Si1 132.6(7) . . ? Si2 N6 Sm1 107.4(5) . . ? Si1 N6 Sm1 118.8(6) . . ? C24 N7 N8 107.5(12) . . ? C24 N7 Sm2 148.5(11) . . ? N8 N7 Sm2 103.3(7) . . ? C22 N8 N7 111.7(11) . . ? C22 N8 C32 130.6(13) . . ? N7 N8 C32 117.5(12) . . ? C29 N9 N10 107.3(17) . . ? C29 N9 Sm2 139.3(15) . . ? N10 N9 Sm2 101.8(8) . . ? C32 N10 C27 135.8(19) . . ? C32 N10 N9 118.5(12) . . ? C27 N10 N9 105.1(16) . . ? C33 N11 C34 120.3(12) . . ? C33 N11 Sm1 92.7(9) . . ? C34 N11 Sm1 147.0(8) . . ? Si3 N12 Si4 125.9(9) . . ? Si3 N12 Sm2 108.2(6) . . ? Si4 N12 Sm2 125.8(7) . . ? C13 O1 Sm2 97.4(8) . . ? C13 O1 Sm1 89.8(7) . . ? Sm2 O1 Sm1 104.6(3) . . ? C33 O2 Sm1 95.3(9) . . ? C33 O2 Sm2 88.1(7) . . ? Sm1 O2 Sm2 104.0(3) . . ? N2 C1 C2 105.3(14) . . ? N2 C1 C4 124.7(15) . . ? C2 C1 C4 130.0(14) . . ? C1 C2 C3 106.2(14) . . ? N1 C3 C2 110.3(14) . . ? N1 C3 C5 125.0(15) . . ? C2 C3 C5 124.7(14) . . ? N4 C6 C7 106.4(15) . . ? N4 C6 C9 120.8(14) . . ? C7 C6 C9 132.8(16) . . ? C6 C7 C8 109.2(14) . . ? N3 C8 C7 108.2(13) . . ? N3 C8 C10 122.5(13) . . ? C7 C8 C10 129.2(13) . . ? C13 C12 N4 117.6(13) . . ? C13 C12 N2 118.4(12) . . ? N4 C12 N2 112.5(12) . . ? C13 C12 Sm1 68.8(8) . . ? N4 C12 Sm1 82.2(7) . . ? N2 C12 Sm1 85.4(7) . . ? N5 C13 C12 131.7(13) . . ? N5 C13 O1 111.6(14) . . ? C12 C13 O1 116.6(13) . . ? N5 C13 Sm1 119.7(10) . . ? C12 C13 Sm1 83.8(8) . . ? O1 C13 Sm1 60.5(6) . . ? N5 C13 Sm2 58.1(8) . . ? C12 C13 Sm2 167.2(10) . . ? O1 C13 Sm2 54.0(7) . . ? Sm1 C13 Sm2 83.7(4) . . ? C15 C14 N5 113.6(12) . . ? C15 C14 C16 112.9(14) . . ? N5 C14 C16 109.5(15) . . ? C17 C16 C14 114.6(19) . . ? N8 C22 C23 106.8(15) . . ? N8 C22 C25 124.1(13) . . ? C23 C22 C25 129.2(15) . . ? C22 C23 C24 105.6(15) . . ? N7 C24 C26 124.8(15) . . ? N7 C24 C23 108.3(14) . . ? C26 C24 C23 126.9(14) . . ? C28 C27 N10 104(2) . . ? C28 C27 C30 144(3) . . ? N10 C27 C30 112(2) . . ? C29 C28 C27 117(3) . . ? C28 C29 N9 106(3) . . ? C28 C29 C31 126(3) . . ? N9 C29 C31 127(3) . . ? N10 C32 C33 118.0(14) . . ? N10 C32 N8 115.5(12) . . ? C33 C32 N8 118.1(12) . . ? N10 C32 Sm2 85.1(9) . . ? C33 C32 Sm2 68.5(8) . . ? N8 C32 Sm2 87.6(8) . . ? N11 C33 O2 116.7(14) . . ? N11 C33 C32 130.5(14) . . ? O2 C33 C32 112.8(15) . . ? N11 C33 Sm2 118.1(9) . . ? O2 C33 Sm2 63.3(7) . . ? C32 C33 Sm2 82.5(9) . . ? N11 C33 Sm1 60.2(8) . . ? O2 C33 Sm1 56.7(7) . . ? C32 C33 Sm1 167.4(12) . . ? Sm2 C33 Sm1 86.1(4) . . ? N11 C34 C35 108.6(12) . . ? N11 C34 C36 109.4(14) . . ? C35 C34 C36 111.2(14) . . ? C37 C36 C34 110.5(19) . . ? C66 C61 C62 123.4(16) . . ? C66 C61 C67 122(2) . . ? C62 C61 C67 114(2) . . ? C63 C62 C61 118.5(14) . . ? C62 C63 C64 120.1(13) . . ? C65 C64 C63 118.3(13) . . ? C64 C65 C66 123.3(15) . . ? C61 C66 C65 116.2(14) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 2.710 _refine_diff_density_min -2.217 _refine_diff_density_rms 0.208