# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Stephen Liddle' 'Alexander J. Blake' 'William Lewis' 'David P. Mills' 'Ashley J. Wooles' _publ_contact_author_name 'Stephen Liddle' _publ_contact_author_email STEPHEN.LIDDLE@NOTTINGHAM.AC.UK _publ_section_title ; Lanthanide Tri-Benzyl Complexes: Structural Variations and Useful Precursors to Phosphorus-Stabilised Lanthanide Carbenes ; # Attachment '12.cif' data_12 _database_code_depnum_ccdc_archive 'CCDC 736110' _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62 H77 La N4 P4 Si4' _chemical_formula_sum 'C62 H77 La N4 P4 Si4' _chemical_formula_weight 1253.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 31.4117(10) _cell_length_b 25.7418(8) _cell_length_c 21.0396(7) _cell_angle_alpha 90.00 _cell_angle_beta 131.118(2) _cell_angle_gamma 90.00 _cell_volume 12816.5(7) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 20250 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 27.47 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.299 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5200 _exptl_absorpt_coefficient_mu 0.881 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.66 _exptl_absorpt_correction_T_max 0.78 _exptl_absorpt_process_details '(SADABS; Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 55829 _diffrn_reflns_av_R_equivalents 0.0292 _diffrn_reflns_av_sigmaI/netI 0.0281 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 27.52 _reflns_number_total 14735 _reflns_number_gt 12845 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'enCIFer(Allen et al.,2004);PLATON(Spek,2003)' _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^)+(0.0390P)^2^+7.8983P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom, Me from difmap' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14735 _refine_ls_number_parameters 688 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0354 _refine_ls_R_factor_gt 0.0284 _refine_ls_wR_factor_ref 0.0711 _refine_ls_wR_factor_gt 0.0680 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 La1 La 0.265451(4) 0.619051(4) 0.755393(6) 0.01597(4) Uani 1 1 d . . . C1 C 0.16524(8) 0.59212(7) 0.67854(12) 0.0227(4) Uani 1 1 d . . . P1 P 0.17479(2) 0.529731(18) 0.67520(3) 0.01984(10) Uani 1 1 d . . . P2 P 0.139670(19) 0.651410(18) 0.65360(3) 0.01828(10) Uani 1 1 d . . . C2 C 0.11149(8) 0.66714(8) 0.70446(13) 0.0249(4) Uani 1 1 d . . . C3 C 0.14191(9) 0.69865(9) 0.77538(14) 0.0327(5) Uani 1 1 d . . . H3A H 0.1756 0.7149 0.7943 0.039 Uiso 1 1 calc R . . C4 C 0.12320(12) 0.70653(11) 0.81909(16) 0.0456(6) Uani 1 1 d . . . H4A H 0.1440 0.7284 0.8674 0.055 Uiso 1 1 calc R . . C5 C 0.07468(13) 0.68275(12) 0.79241(19) 0.0530(7) Uani 1 1 d . . . H5A H 0.0619 0.6883 0.8221 0.064 Uiso 1 1 calc R . . C6 C 0.04451(12) 0.65083(11) 0.72267(19) 0.0502(7) Uani 1 1 d . . . H6A H 0.0113 0.6340 0.7048 0.060 Uiso 1 1 calc R . . C7 C 0.06269(10) 0.64321(9) 0.67866(16) 0.0359(5) Uani 1 1 d . . . H7A H 0.0416 0.6214 0.6303 0.043 Uiso 1 1 calc R . . C8 C 0.07958(8) 0.66098(7) 0.54162(12) 0.0220(4) Uani 1 1 d . . . C9 C 0.03435(8) 0.69426(8) 0.51001(14) 0.0291(4) Uani 1 1 d . . . H9A H 0.0330 0.7125 0.5479 0.035 Uiso 1 1 calc R . . C10 C -0.00870(9) 0.70085(9) 0.42345(14) 0.0366(5) Uani 1 1 d . . . H10A H -0.0390 0.7239 0.4026 0.044 Uiso 1 1 calc R . . C11 C -0.00757(9) 0.67420(9) 0.36799(14) 0.0380(6) Uani 1 1 d . . . H11A H -0.0369 0.6792 0.3090 0.046 Uiso 1 1 calc R . . C12 C 0.03615(9) 0.64010(10) 0.39795(14) 0.0353(5) Uani 1 1 d . . . H12A H 0.0365 0.6212 0.3596 0.042 Uiso 1 1 calc R . . C13 C 0.07928(9) 0.63367(8) 0.48387(13) 0.0286(4) Uani 1 1 d . . . H13A H 0.1092 0.6103 0.5040 0.034 Uiso 1 1 calc R . . C14 C 0.14902(8) 0.48735(8) 0.71327(12) 0.0246(4) Uani 1 1 d . . . C15 C 0.13199(9) 0.50764(9) 0.75402(14) 0.0336(5) Uani 1 1 d . . . H15A H 0.1328 0.5441 0.7615 0.040 Uiso 1 1 calc R . . C16 C 0.11364(12) 0.47465(11) 0.78418(16) 0.0476(7) Uani 1 1 d . . . H16A H 0.1018 0.4887 0.8122 0.057 Uiso 1 1 calc R . . C17 C 0.11246(12) 0.42164(11) 0.77370(16) 0.0496(7) Uani 1 1 d . . . H17A H 0.1004 0.3993 0.7952 0.060 Uiso 1 1 calc R . . C18 C 0.12868(11) 0.40109(10) 0.73214(17) 0.0446(6) Uani 1 1 d . . . H18A H 0.1278 0.3646 0.7248 0.054 Uiso 1 1 calc R . . C19 C 0.14626(9) 0.43366(8) 0.70106(14) 0.0329(5) Uani 1 1 d . . . H19A H 0.1566 0.4194 0.6711 0.039 Uiso 1 1 calc R . . C20 C 0.13264(9) 0.50433(8) 0.56770(13) 0.0276(4) Uani 1 1 d . . . C21 C 0.07387(10) 0.50587(11) 0.51507(15) 0.0433(6) Uani 1 1 d . . . H21A H 0.0568 0.5188 0.5359 0.052 Uiso 1 1 calc R . . C22 C 0.04029(12) 0.48860(12) 0.43217(16) 0.0573(8) Uani 1 1 d . . . H22A H 0.0003 0.4899 0.3964 0.069 Uiso 1 1 calc R . . C23 C 0.06505(14) 0.46961(11) 0.40187(17) 0.0576(8) Uani 1 1 d . . . H23A H 0.0420 0.4579 0.3452 0.069 Uiso 1 1 calc R . . C24 C 0.12294(13) 0.46764(10) 0.45345(16) 0.0490(7) Uani 1 1 d . . . H24A H 0.1399 0.4543 0.4326 0.059 Uiso 1 1 calc R . . C25 C 0.15658(11) 0.48519(8) 0.53620(14) 0.0348(5) Uani 1 1 d . . . H25A H 0.1966 0.4840 0.5715 0.042 Uiso 1 1 calc R . . N1 N 0.24172(7) 0.52133(6) 0.72880(10) 0.0209(3) Uani 1 1 d . . . Si1 Si 0.28920(2) 0.47207(2) 0.78552(4) 0.02483(12) Uani 1 1 d . . . C26 C 0.36091(9) 0.50176(9) 0.84648(15) 0.0360(5) Uani 1 1 d . . . H26A H 0.3667 0.5116 0.8076 0.054 Uiso 1 1 calc R . . H26B H 0.3898 0.4765 0.8874 0.054 Uiso 1 1 calc R . . H26C H 0.3638 0.5327 0.8763 0.054 Uiso 1 1 calc R . . C27 C 0.28199(11) 0.41851(8) 0.71873(16) 0.0394(6) Uani 1 1 d . . . H27A H 0.2452 0.4016 0.6877 0.059 Uiso 1 1 calc R . . H27B H 0.3121 0.3930 0.7549 0.059 Uiso 1 1 calc R . . H27C H 0.2849 0.4329 0.6786 0.059 Uiso 1 1 calc R . . C28 C 0.28868(10) 0.44054(9) 0.86534(14) 0.0349(5) Uani 1 1 d . . . H28A H 0.2532 0.4215 0.8362 0.052 Uiso 1 1 calc R . . H28B H 0.2920 0.4673 0.9016 0.052 Uiso 1 1 calc R . . H28C H 0.3206 0.4164 0.8999 0.052 Uiso 1 1 calc R . . N2 N 0.19093(6) 0.69115(6) 0.68687(10) 0.0189(3) Uani 1 1 d . . . Si2 Si 0.18557(2) 0.75521(2) 0.65903(3) 0.02029(11) Uani 1 1 d . . . C29 C 0.13174(9) 0.79397(8) 0.65134(16) 0.0360(5) Uani 1 1 d . . . H29A H 0.1413 0.7938 0.7061 0.054 Uiso 1 1 calc R . . H29B H 0.0943 0.7785 0.6085 0.054 Uiso 1 1 calc R . . H29C H 0.1315 0.8298 0.6355 0.054 Uiso 1 1 calc R . . C30 C 0.25383(8) 0.78998(8) 0.73855(13) 0.0267(4) Uani 1 1 d . . . H30A H 0.2853 0.7669 0.7584 0.040 Uiso 1 1 calc R . . H30B H 0.2570 0.8004 0.7864 0.040 Uiso 1 1 calc R . . H30C H 0.2550 0.8209 0.7126 0.040 Uiso 1 1 calc R . . C31 C 0.16717(11) 0.76069(9) 0.55504(14) 0.0369(5) Uani 1 1 d . . . H31A H 0.1947 0.7411 0.5567 0.055 Uiso 1 1 calc R . . H31B H 0.1679 0.7973 0.5431 0.055 Uiso 1 1 calc R . . H31C H 0.1293 0.7465 0.5107 0.055 Uiso 1 1 calc R . . C32 C 0.36922(8) 0.68840(7) 0.84540(11) 0.0200(4) Uani 1 1 d . . . H32A H 0.3576 0.7253 0.8272 0.024 Uiso 1 1 calc R . . P3 P 0.377730(19) 0.657149(18) 0.78115(3) 0.01709(9) Uani 1 1 d . . . P4 P 0.37573(2) 0.675455(18) 0.93231(3) 0.01814(10) Uani 1 1 d . . . C33 C 0.44548(8) 0.62503(7) 0.83841(12) 0.0209(4) Uani 1 1 d . . . C34 C 0.44878(9) 0.57641(8) 0.81347(14) 0.0294(4) Uani 1 1 d . . . H34A H 0.4151 0.5587 0.7688 0.035 Uiso 1 1 calc R . . C35 C 0.50092(10) 0.55336(9) 0.85331(17) 0.0418(6) Uani 1 1 d . . . H35A H 0.5029 0.5198 0.8365 0.050 Uiso 1 1 calc R . . C36 C 0.54990(9) 0.57939(10) 0.91738(16) 0.0407(6) Uani 1 1 d . . . H36A H 0.5856 0.5640 0.9440 0.049 Uiso 1 1 calc R . . C37 C 0.54717(9) 0.62769(9) 0.94286(15) 0.0379(5) Uani 1 1 d . . . H37A H 0.5810 0.6455 0.9870 0.045 Uiso 1 1 calc R . . C38 C 0.49533(9) 0.65032(8) 0.90433(13) 0.0296(4) Uani 1 1 d . . . H38A H 0.4937 0.6833 0.9229 0.036 Uiso 1 1 calc R . . C39 C 0.38052(8) 0.70993(7) 0.72649(11) 0.0197(4) Uani 1 1 d . . . C40 C 0.42302(8) 0.71486(8) 0.72283(12) 0.0246(4) Uani 1 1 d . . . H40A H 0.4541 0.6915 0.7536 0.030 Uiso 1 1 calc R . . C41 C 0.42004(9) 0.75383(8) 0.67419(13) 0.0288(4) Uani 1 1 d . . . H41A H 0.4489 0.7567 0.6714 0.035 Uiso 1 1 calc R . . C42 C 0.37560(10) 0.78819(8) 0.63024(13) 0.0304(5) Uani 1 1 d . . . H42A H 0.3742 0.8151 0.5980 0.037 Uiso 1 1 calc R . . C43 C 0.33292(10) 0.78370(9) 0.63274(15) 0.0356(5) Uani 1 1 d . . . H43A H 0.3022 0.8075 0.6024 0.043 Uiso 1 1 calc R . . C44 C 0.33514(9) 0.74436(8) 0.67978(14) 0.0307(5) Uani 1 1 d . . . H44A H 0.3052 0.7408 0.6802 0.037 Uiso 1 1 calc R . . C45 C 0.44603(8) 0.65766(8) 1.02851(12) 0.0254(4) Uani 1 1 d . . . C46 C 0.47500(10) 0.68426(11) 1.10446(14) 0.0411(6) Uani 1 1 d . . . H46A H 0.4595 0.7152 1.1067 0.049 Uiso 1 1 calc R . . C47 C 0.52657(11) 0.66563(14) 1.17710(16) 0.0572(8) Uani 1 1 d . . . H47A H 0.5462 0.6840 1.2287 0.069 Uiso 1 1 calc R . . C48 C 0.54926(11) 0.62122(13) 1.17491(18) 0.0582(9) Uani 1 1 d . . . H48A H 0.5845 0.6088 1.2249 0.070 Uiso 1 1 calc R . . C49 C 0.52122(10) 0.59429(12) 1.10040(17) 0.0479(7) Uani 1 1 d . . . H49A H 0.5370 0.5632 1.0992 0.057 Uiso 1 1 calc R . . C50 C 0.46997(10) 0.61250(9) 1.02723(15) 0.0346(5) Uani 1 1 d . . . H50A H 0.4510 0.5941 0.9758 0.042 Uiso 1 1 calc R . . C51 C 0.36047(9) 0.73845(8) 0.95258(12) 0.0250(4) Uani 1 1 d . . . C52 C 0.39484(11) 0.78173(9) 0.97659(14) 0.0370(5) Uani 1 1 d . . . H52A H 0.4289 0.7784 0.9865 0.044 Uiso 1 1 calc R . . C53 C 0.37937(14) 0.82987(9) 0.98610(17) 0.0509(7) Uani 1 1 d . . . H53A H 0.4028 0.8593 1.0021 0.061 Uiso 1 1 calc R . . C54 C 0.33043(14) 0.83487(10) 0.97247(17) 0.0530(8) Uani 1 1 d . . . H54A H 0.3203 0.8677 0.9798 0.064 Uiso 1 1 calc R . . C55 C 0.29612(12) 0.79287(10) 0.94845(16) 0.0458(6) Uani 1 1 d . . . H55A H 0.2622 0.7966 0.9389 0.055 Uiso 1 1 calc R . . C56 C 0.31075(10) 0.74461(9) 0.93798(13) 0.0311(5) Uani 1 1 d . . . H56A H 0.2865 0.7157 0.9207 0.037 Uiso 1 1 calc R . . N3 N 0.32645(7) 0.61867(6) 0.71514(10) 0.0194(3) Uani 1 1 d . . . Si3 Si 0.29692(2) 0.59749(2) 0.61588(3) 0.02311(11) Uani 1 1 d . . . C57 C 0.21930(9) 0.60917(9) 0.54728(14) 0.0341(5) Uani 1 1 d . . . H57A H 0.2048 0.5906 0.5704 0.051 Uiso 1 1 calc R . . H57B H 0.2000 0.5965 0.4901 0.051 Uiso 1 1 calc R . . H57C H 0.2123 0.6465 0.5453 0.051 Uiso 1 1 calc R . . C58 C 0.30727(11) 0.52633(9) 0.61529(16) 0.0399(6) Uani 1 1 d . . . H58A H 0.2979 0.5083 0.6458 0.060 Uiso 1 1 calc R . . H58B H 0.3468 0.5194 0.6428 0.060 Uiso 1 1 calc R . . H58C H 0.2825 0.5138 0.5569 0.060 Uiso 1 1 calc R . . C59 C 0.32249(13) 0.63010(11) 0.56741(17) 0.0491(7) Uani 1 1 d . . . H59A H 0.3143 0.6674 0.5617 0.074 Uiso 1 1 calc R . . H59B H 0.3033 0.6152 0.5116 0.074 Uiso 1 1 calc R . . H59C H 0.3634 0.6249 0.6034 0.074 Uiso 1 1 calc R . . N4 N 0.33175(7) 0.63218(6) 0.91306(10) 0.0197(3) Uani 1 1 d . . . Si4 Si 0.32861(2) 0.60268(2) 0.98423(3) 0.02465(12) Uani 1 1 d . . . C60 C 0.25542(9) 0.57708(10) 0.92022(15) 0.0395(6) Uani 1 1 d . . . H60A H 0.2482 0.5519 0.8791 0.059 Uiso 1 1 calc R . . H60B H 0.2284 0.6058 0.8904 0.059 Uiso 1 1 calc R . . H60C H 0.2511 0.5601 0.9574 0.059 Uiso 1 1 calc R . . C61 C 0.38134(11) 0.54927(10) 1.04430(16) 0.0442(6) Uani 1 1 d . . . H61A H 0.3807 0.5275 1.0054 0.066 Uiso 1 1 calc R . . H61B H 0.3719 0.5280 1.0722 0.066 Uiso 1 1 calc R . . H61C H 0.4191 0.5642 1.0868 0.066 Uiso 1 1 calc R . . C62 C 0.34146(12) 0.64682(11) 1.06600(15) 0.0467(6) Uani 1 1 d . . . H62A H 0.3781 0.6641 1.0968 0.070 Uiso 1 1 calc R . . H62B H 0.3416 0.6265 1.1055 0.070 Uiso 1 1 calc R . . H62C H 0.3114 0.6730 1.0385 0.070 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 La1 0.01560(6) 0.01525(6) 0.01714(6) 0.00009(4) 0.01080(5) -0.00041(4) C1 0.0187(9) 0.0198(9) 0.0249(10) 0.0008(7) 0.0123(8) -0.0001(7) P1 0.0190(2) 0.0165(2) 0.0212(2) -0.00001(18) 0.0120(2) -0.00234(18) P2 0.0155(2) 0.0188(2) 0.0194(2) 0.00113(18) 0.01101(19) 0.00112(17) C2 0.0260(10) 0.0262(10) 0.0269(10) 0.0042(8) 0.0193(9) 0.0052(8) C3 0.0316(11) 0.0389(12) 0.0302(11) -0.0005(9) 0.0215(10) -0.0013(9) C4 0.0544(16) 0.0568(16) 0.0375(13) -0.0077(12) 0.0353(13) -0.0047(13) C5 0.0624(18) 0.0655(18) 0.0629(18) -0.0084(15) 0.0550(17) -0.0049(15) C6 0.0498(16) 0.0579(17) 0.0707(19) -0.0119(14) 0.0517(16) -0.0118(13) C7 0.0343(12) 0.0383(13) 0.0463(14) -0.0060(10) 0.0313(11) -0.0037(10) C8 0.0170(9) 0.0218(9) 0.0235(9) 0.0021(7) 0.0118(8) -0.0017(7) C9 0.0214(10) 0.0261(10) 0.0316(11) 0.0006(8) 0.0139(9) 0.0019(8) C10 0.0217(10) 0.0310(12) 0.0355(12) 0.0090(9) 0.0095(10) 0.0038(9) C11 0.0257(11) 0.0414(13) 0.0259(11) 0.0095(10) 0.0078(9) -0.0087(10) C12 0.0354(12) 0.0436(13) 0.0241(11) 0.0000(9) 0.0183(10) -0.0086(10) C13 0.0262(10) 0.0329(11) 0.0282(11) 0.0037(9) 0.0185(9) 0.0004(9) C14 0.0200(9) 0.0251(10) 0.0240(10) 0.0012(8) 0.0125(8) -0.0051(8) C15 0.0320(11) 0.0348(12) 0.0353(12) -0.0087(9) 0.0227(10) -0.0122(9) C16 0.0542(16) 0.0621(17) 0.0430(14) -0.0143(12) 0.0391(14) -0.0229(13) C17 0.0554(16) 0.0538(16) 0.0439(15) -0.0008(12) 0.0345(14) -0.0238(13) C18 0.0466(15) 0.0329(13) 0.0508(15) 0.0036(11) 0.0304(13) -0.0126(11) C19 0.0344(12) 0.0252(11) 0.0399(13) -0.0004(9) 0.0248(11) -0.0073(9) C20 0.0322(11) 0.0202(10) 0.0238(10) -0.0002(8) 0.0155(9) -0.0076(8) C21 0.0323(12) 0.0568(16) 0.0291(12) -0.0050(11) 0.0151(11) -0.0155(11) C22 0.0428(15) 0.069(2) 0.0306(13) -0.0044(13) 0.0113(12) -0.0286(14) C23 0.080(2) 0.0480(16) 0.0293(13) -0.0101(11) 0.0295(15) -0.0284(15) C24 0.080(2) 0.0336(13) 0.0366(14) -0.0014(10) 0.0395(15) -0.0022(13) C25 0.0478(14) 0.0261(11) 0.0303(11) 0.0023(9) 0.0256(11) 0.0014(10) N1 0.0209(8) 0.0155(8) 0.0253(8) 0.0011(6) 0.0147(7) -0.0004(6) Si1 0.0264(3) 0.0174(3) 0.0293(3) 0.0048(2) 0.0177(3) 0.0042(2) C26 0.0266(11) 0.0381(13) 0.0388(13) 0.0084(10) 0.0196(10) 0.0057(9) C27 0.0547(15) 0.0207(11) 0.0473(14) 0.0055(10) 0.0355(13) 0.0099(10) C28 0.0360(12) 0.0286(11) 0.0327(12) 0.0095(9) 0.0194(10) 0.0024(9) N2 0.0167(7) 0.0172(7) 0.0207(8) 0.0013(6) 0.0115(7) 0.0001(6) Si2 0.0227(3) 0.0164(2) 0.0206(3) 0.00170(19) 0.0137(2) 0.00147(19) C29 0.0319(12) 0.0221(11) 0.0538(15) 0.0008(10) 0.0281(12) 0.0048(9) C30 0.0269(10) 0.0199(10) 0.0310(11) -0.0006(8) 0.0181(9) -0.0007(8) C31 0.0506(14) 0.0321(12) 0.0274(11) 0.0027(9) 0.0254(11) -0.0019(10) C32 0.0219(9) 0.0209(9) 0.0188(9) 0.0006(7) 0.0140(8) 0.0011(7) P3 0.0163(2) 0.0174(2) 0.0185(2) 0.00028(17) 0.01182(19) 0.00010(17) P4 0.0175(2) 0.0195(2) 0.0160(2) -0.00054(17) 0.01045(19) -0.00015(18) C33 0.0207(9) 0.0202(9) 0.0247(10) 0.0042(7) 0.0161(8) 0.0024(7) C34 0.0228(10) 0.0229(10) 0.0374(12) -0.0029(9) 0.0176(9) -0.0010(8) C35 0.0338(12) 0.0291(12) 0.0566(16) -0.0008(11) 0.0272(12) 0.0083(10) C36 0.0226(11) 0.0393(13) 0.0494(14) 0.0071(11) 0.0191(11) 0.0102(9) C37 0.0196(10) 0.0394(13) 0.0375(13) -0.0007(10) 0.0114(10) -0.0008(9) C38 0.0246(10) 0.0282(11) 0.0303(11) -0.0009(9) 0.0156(9) 0.0009(8) C39 0.0213(9) 0.0200(9) 0.0192(9) -0.0010(7) 0.0139(8) -0.0022(7) C40 0.0196(9) 0.0290(10) 0.0236(10) 0.0010(8) 0.0135(8) -0.0027(8) C41 0.0271(10) 0.0360(12) 0.0239(10) -0.0018(8) 0.0171(9) -0.0091(9) C42 0.0440(13) 0.0249(10) 0.0244(10) 0.0002(8) 0.0233(10) -0.0053(9) C43 0.0448(13) 0.0327(12) 0.0358(12) 0.0128(9) 0.0293(11) 0.0148(10) C44 0.0355(12) 0.0314(11) 0.0371(12) 0.0093(9) 0.0290(11) 0.0102(9) C45 0.0177(9) 0.0353(11) 0.0191(9) 0.0051(8) 0.0104(8) -0.0011(8) C46 0.0294(12) 0.0545(15) 0.0250(11) -0.0021(10) 0.0116(10) -0.0045(11) C47 0.0318(14) 0.087(2) 0.0254(13) 0.0019(13) 0.0069(11) -0.0050(14) C48 0.0212(12) 0.096(3) 0.0358(15) 0.0245(15) 0.0094(11) 0.0077(13) C49 0.0328(13) 0.0624(18) 0.0492(16) 0.0251(13) 0.0273(13) 0.0200(12) C50 0.0287(11) 0.0444(13) 0.0296(11) 0.0109(10) 0.0186(10) 0.0085(10) C51 0.0330(11) 0.0229(10) 0.0199(9) -0.0019(7) 0.0178(9) 0.0013(8) C52 0.0487(14) 0.0300(12) 0.0342(12) -0.0085(9) 0.0281(12) -0.0095(10) C53 0.081(2) 0.0248(12) 0.0450(15) -0.0097(10) 0.0405(16) -0.0093(13) C54 0.083(2) 0.0309(13) 0.0443(15) 0.0015(11) 0.0419(16) 0.0179(14) C55 0.0582(17) 0.0469(15) 0.0403(14) 0.0070(11) 0.0359(13) 0.0220(13) C56 0.0364(12) 0.0317(11) 0.0271(11) 0.0023(9) 0.0217(10) 0.0072(9) N3 0.0204(8) 0.0203(8) 0.0202(8) -0.0019(6) 0.0145(7) -0.0015(6) Si3 0.0254(3) 0.0257(3) 0.0229(3) -0.0059(2) 0.0179(2) -0.0052(2) C57 0.0274(11) 0.0359(12) 0.0247(11) -0.0024(9) 0.0111(9) -0.0004(9) C58 0.0417(13) 0.0345(13) 0.0423(14) -0.0151(10) 0.0271(12) -0.0019(10) C59 0.0672(18) 0.0603(17) 0.0422(14) -0.0249(12) 0.0457(15) -0.0333(14) N4 0.0206(8) 0.0201(8) 0.0183(8) 0.0009(6) 0.0126(7) -0.0011(6) Si4 0.0235(3) 0.0289(3) 0.0207(3) 0.0050(2) 0.0142(2) -0.0002(2) C60 0.0301(12) 0.0486(14) 0.0350(12) 0.0090(11) 0.0193(11) -0.0073(10) C61 0.0420(14) 0.0497(15) 0.0442(14) 0.0271(12) 0.0299(12) 0.0154(12) C62 0.0639(17) 0.0542(16) 0.0343(13) -0.0042(11) 0.0375(14) -0.0078(13) _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 La1 C1 2.5119(19) . ? La1 N4 2.5238(15) . ? La1 N3 2.5541(15) . ? La1 N2 2.5621(15) . ? La1 N1 2.5783(15) . ? La1 C32 3.0463(19) . ? C1 P2 1.6418(19) . ? C1 P1 1.6438(19) . ? P1 N1 1.6186(16) . ? P1 C14 1.827(2) . ? P1 C20 1.832(2) . ? P2 N2 1.6268(16) . ? P2 C8 1.8235(19) . ? P2 C2 1.827(2) . ? C2 C3 1.386(3) . ? C2 C7 1.389(3) . ? C3 C4 1.394(3) . ? C4 C5 1.374(4) . ? C5 C6 1.377(4) . ? C6 C7 1.385(3) . ? C8 C9 1.397(3) . ? C8 C13 1.398(3) . ? C9 C10 1.391(3) . ? C10 C11 1.374(4) . ? C11 C12 1.384(3) . ? C12 C13 1.382(3) . ? C14 C15 1.377(3) . ? C14 C19 1.398(3) . ? C15 C16 1.392(3) . ? C16 C17 1.379(4) . ? C17 C18 1.375(4) . ? C18 C19 1.382(3) . ? C20 C25 1.380(3) . ? C20 C21 1.395(3) . ? C21 C22 1.390(3) . ? C22 C23 1.379(4) . ? C23 C24 1.375(4) . ? C24 C25 1.390(3) . ? N1 Si1 1.7076(16) . ? Si1 C26 1.872(2) . ? Si1 C27 1.873(2) . ? Si1 C28 1.875(2) . ? N2 Si2 1.7208(16) . ? Si2 C31 1.865(2) . ? Si2 C30 1.865(2) . ? Si2 C29 1.876(2) . ? C32 P4 1.7333(18) . ? C32 P3 1.7383(18) . ? P3 N3 1.6006(16) . ? P3 C33 1.8142(19) . ? P3 C39 1.8189(19) . ? P4 N4 1.6055(16) . ? P4 C45 1.818(2) . ? P4 C51 1.820(2) . ? C33 C34 1.387(3) . ? C33 C38 1.394(3) . ? C34 C35 1.390(3) . ? C35 C36 1.380(3) . ? C36 C37 1.379(3) . ? C37 C38 1.383(3) . ? C39 C40 1.393(3) . ? C39 C44 1.393(3) . ? C40 C41 1.391(3) . ? C41 C42 1.374(3) . ? C42 C43 1.380(3) . ? C43 C44 1.385(3) . ? C45 C46 1.392(3) . ? C45 C50 1.394(3) . ? C46 C47 1.391(3) . ? C47 C48 1.364(4) . ? C48 C49 1.378(4) . ? C49 C50 1.386(3) . ? C51 C56 1.388(3) . ? C51 C52 1.395(3) . ? C52 C53 1.393(3) . ? C53 C54 1.372(4) . ? C54 C55 1.367(4) . ? C55 C56 1.392(3) . ? N3 Si3 1.7237(16) . ? Si3 C59 1.862(2) . ? Si3 C58 1.862(2) . ? Si3 C57 1.868(2) . ? N4 Si4 1.7386(16) . ? Si4 C60 1.860(2) . ? Si4 C61 1.865(2) . ? Si4 C62 1.871(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 La1 N4 118.99(6) . . ? C1 La1 N3 132.95(6) . . ? N4 La1 N3 106.61(5) . . ? C1 La1 N2 62.82(5) . . ? N4 La1 N2 107.54(5) . . ? N3 La1 N2 115.04(5) . . ? C1 La1 N1 61.96(6) . . ? N4 La1 N1 106.67(5) . . ? N3 La1 N1 95.58(5) . . ? N2 La1 N1 123.91(5) . . ? C1 La1 C32 159.65(6) . . ? N4 La1 C32 58.91(5) . . ? N3 La1 C32 58.60(5) . . ? N2 La1 C32 97.67(5) . . ? N1 La1 C32 138.17(5) . . ? P2 C1 P1 163.60(14) . . ? P2 C1 La1 95.26(8) . . ? P1 C1 La1 96.34(8) . . ? N1 P1 C1 106.90(9) . . ? N1 P1 C14 111.20(9) . . ? C1 P1 C14 114.75(10) . . ? N1 P1 C20 111.44(9) . . ? C1 P1 C20 113.41(10) . . ? C14 P1 C20 99.15(9) . . ? N2 P2 C1 108.02(9) . . ? N2 P2 C8 111.20(8) . . ? C1 P2 C8 114.31(9) . . ? N2 P2 C2 109.40(9) . . ? C1 P2 C2 110.03(10) . . ? C8 P2 C2 103.78(9) . . ? C3 C2 C7 118.8(2) . . ? C3 C2 P2 120.23(16) . . ? C7 C2 P2 120.53(16) . . ? C2 C3 C4 120.3(2) . . ? C5 C4 C3 120.1(2) . . ? C4 C5 C6 120.1(2) . . ? C5 C6 C7 120.0(2) . . ? C6 C7 C2 120.7(2) . . ? C9 C8 C13 118.09(19) . . ? C9 C8 P2 124.23(16) . . ? C13 C8 P2 117.68(15) . . ? C10 C9 C8 120.5(2) . . ? C11 C10 C9 120.3(2) . . ? C10 C11 C12 120.1(2) . . ? C13 C12 C11 119.8(2) . . ? C12 C13 C8 121.1(2) . . ? C15 C14 C19 119.12(19) . . ? C15 C14 P1 120.78(16) . . ? C19 C14 P1 120.09(16) . . ? C14 C15 C16 120.0(2) . . ? C17 C16 C15 120.4(2) . . ? C18 C17 C16 120.0(2) . . ? C17 C18 C19 119.9(2) . . ? C18 C19 C14 120.6(2) . . ? C25 C20 C21 118.9(2) . . ? C25 C20 P1 122.73(17) . . ? C21 C20 P1 118.33(18) . . ? C22 C21 C20 120.2(3) . . ? C23 C22 C21 120.0(3) . . ? C24 C23 C22 120.2(2) . . ? C23 C24 C25 119.9(3) . . ? C20 C25 C24 120.8(2) . . ? P1 N1 Si1 136.34(10) . . ? P1 N1 La1 94.51(7) . . ? Si1 N1 La1 125.30(8) . . ? N1 Si1 C26 106.26(9) . . ? N1 Si1 C27 113.77(10) . . ? C26 Si1 C27 108.17(12) . . ? N1 Si1 C28 115.44(10) . . ? C26 Si1 C28 106.17(11) . . ? C27 Si1 C28 106.58(11) . . ? P2 N2 Si2 127.49(9) . . ? P2 N2 La1 93.79(7) . . ? Si2 N2 La1 137.25(8) . . ? N2 Si2 C31 110.94(9) . . ? N2 Si2 C30 110.93(8) . . ? C31 Si2 C30 107.61(10) . . ? N2 Si2 C29 114.82(9) . . ? C31 Si2 C29 106.99(11) . . ? C30 Si2 C29 105.15(10) . . ? P4 C32 P3 139.43(12) . . ? P4 C32 La1 83.04(7) . . ? P3 C32 La1 83.93(7) . . ? N3 P3 C32 112.30(9) . . ? N3 P3 C33 111.46(9) . . ? C32 P3 C33 114.05(9) . . ? N3 P3 C39 110.67(8) . . ? C32 P3 C39 104.00(9) . . ? C33 P3 C39 103.72(9) . . ? N4 P4 C32 112.48(9) . . ? N4 P4 C45 108.64(9) . . ? C32 P4 C45 115.93(9) . . ? N4 P4 C51 111.21(9) . . ? C32 P4 C51 102.09(9) . . ? C45 P4 C51 106.14(10) . . ? C34 C33 C38 118.89(18) . . ? C34 C33 P3 120.45(15) . . ? C38 C33 P3 120.51(15) . . ? C33 C34 C35 120.6(2) . . ? C36 C35 C34 119.8(2) . . ? C37 C36 C35 120.2(2) . . ? C36 C37 C38 120.2(2) . . ? C37 C38 C33 120.4(2) . . ? C40 C39 C44 118.45(18) . . ? C40 C39 P3 123.32(15) . . ? C44 C39 P3 117.97(15) . . ? C41 C40 C39 120.19(19) . . ? C42 C41 C40 120.42(19) . . ? C41 C42 C43 120.17(19) . . ? C42 C43 C44 119.6(2) . . ? C43 C44 C39 121.1(2) . . ? C46 C45 C50 118.6(2) . . ? C46 C45 P4 123.54(18) . . ? C50 C45 P4 117.66(16) . . ? C47 C46 C45 120.1(3) . . ? C48 C47 C46 120.6(3) . . ? C47 C48 C49 120.2(2) . . ? C48 C49 C50 120.0(3) . . ? C49 C50 C45 120.5(2) . . ? C56 C51 C52 118.6(2) . . ? C56 C51 P4 118.77(16) . . ? C52 C51 P4 122.43(17) . . ? C53 C52 C51 120.2(2) . . ? C54 C53 C52 120.2(3) . . ? C55 C54 C53 120.4(2) . . ? C54 C55 C56 120.2(3) . . ? C51 C56 C55 120.5(2) . . ? P3 N3 Si3 132.82(10) . . ? P3 N3 La1 104.85(7) . . ? Si3 N3 La1 118.66(8) . . ? N3 Si3 C59 116.02(10) . . ? N3 Si3 C58 111.23(10) . . ? C59 Si3 C58 107.44(12) . . ? N3 Si3 C57 105.92(9) . . ? C59 Si3 C57 108.55(13) . . ? C58 Si3 C57 107.34(11) . . ? P4 N4 Si4 127.78(10) . . ? P4 N4 La1 104.70(7) . . ? Si4 N4 La1 127.48(8) . . ? N4 Si4 C60 105.91(9) . . ? N4 Si4 C61 112.19(10) . . ? C60 Si4 C61 110.70(12) . . ? N4 Si4 C62 115.24(10) . . ? C60 Si4 C62 107.30(13) . . ? C61 Si4 C62 105.44(13) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.845 _refine_diff_density_min -0.368 _refine_diff_density_rms 0.073 # Attachment '13.cif' data_13 _database_code_depnum_ccdc_archive 'CCDC 736111' _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62 H77 Ce N4 P4 Si4' _chemical_formula_sum 'C62 H77 Ce N4 P4 Si4' _chemical_formula_weight 1254.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 31.3680(17) _cell_length_b 25.7369(17) _cell_length_c 21.0352(17) _cell_angle_alpha 90.00 _cell_angle_beta 131.128(2) _cell_angle_gamma 90.00 _cell_volume 12791.6(15) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 13403 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.303 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5208 _exptl_absorpt_coefficient_mu 0.927 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.83 _exptl_absorpt_correction_T_max 0.86 _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 23035 _diffrn_reflns_av_R_equivalents 0.060 _diffrn_reflns_av_sigmaI/netI 0.120 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9781 _reflns_number_gt 6971 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36A (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; SHELXTL (Sheldrick, 2008)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'enCIFer(Allen et al.,2004);PLATON(Spek,2003)' _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^)+(0.0085P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom, Me from difmap' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9781 _refine_ls_number_parameters 688 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0644 _refine_ls_R_factor_gt 0.0430 _refine_ls_wR_factor_ref 0.0791 _refine_ls_wR_factor_gt 0.0743 _refine_ls_goodness_of_fit_ref 0.81 _refine_ls_restrained_S_all 0.81 _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 Ce1 Ce 0.265292(10) 0.880599(10) 0.755225(15) 0.01740(7) Uani 1 1 d . . . C1 C 0.36851(17) 0.81120(18) 0.8448(2) 0.0224(10) Uani 1 1 d . . . H1A H 0.3569 0.7743 0.8266 0.027 Uiso 1 1 calc R . . P1 P 0.37720(5) 0.84270(5) 0.78083(7) 0.0195(3) Uani 1 1 d . . . P2 P 0.37487(5) 0.82451(5) 0.93159(7) 0.0204(3) Uani 1 1 d . . . C2 C 0.37944(17) 0.79029(18) 0.7255(2) 0.0186(10) Uani 1 1 d . . . C3 C 0.3347(2) 0.7560(2) 0.6789(3) 0.0317(12) Uani 1 1 d . . . H3A H 0.3045 0.7596 0.6787 0.038 Uiso 1 1 calc R . . C4 C 0.3326(2) 0.7164(2) 0.6325(3) 0.0371(13) Uani 1 1 d . . . H4A H 0.3021 0.6924 0.6026 0.045 Uiso 1 1 calc R . . C5 C 0.3754(2) 0.7122(2) 0.6302(3) 0.0296(12) Uani 1 1 d . . . H5A H 0.3741 0.6855 0.5977 0.036 Uiso 1 1 calc R . . C6 C 0.41977(19) 0.7464(2) 0.6748(3) 0.0302(12) Uani 1 1 d . . . H6A H 0.4492 0.7434 0.6730 0.036 Uiso 1 1 calc R . . C7 C 0.42213(18) 0.78518(19) 0.7220(3) 0.0253(11) Uani 1 1 d . . . H7A H 0.4531 0.8087 0.7526 0.030 Uiso 1 1 calc R . . C8 C 0.44503(17) 0.87536(19) 0.8382(3) 0.0224(10) Uani 1 1 d . . . C9 C 0.44869(19) 0.9233(2) 0.8134(3) 0.0313(12) Uani 1 1 d . . . H9A H 0.4150 0.9410 0.7685 0.038 Uiso 1 1 calc R . . C10 C 0.5008(2) 0.9464(2) 0.8529(3) 0.0427(14) Uani 1 1 d . . . H10A H 0.5030 0.9799 0.8362 0.051 Uiso 1 1 calc R . . C11 C 0.5494(2) 0.9200(2) 0.9168(3) 0.0417(14) Uani 1 1 d . . . H11A H 0.5852 0.9350 0.9430 0.050 Uiso 1 1 calc R . . C12 C 0.5468(2) 0.8723(2) 0.9430(3) 0.0388(13) Uani 1 1 d . . . H12A H 0.5806 0.8548 0.9880 0.047 Uiso 1 1 calc R . . C13 C 0.49478(19) 0.8497(2) 0.9038(3) 0.0292(12) Uani 1 1 d . . . H13A H 0.4929 0.8165 0.9216 0.035 Uiso 1 1 calc R . . C14 C 0.44564(19) 0.8419(2) 1.0284(3) 0.0256(11) Uani 1 1 d . . . C15 C 0.4741(2) 0.8151(2) 1.1039(3) 0.0417(14) Uani 1 1 d . . . H15A H 0.4585 0.7842 1.1060 0.050 Uiso 1 1 calc R . . C16 C 0.5261(2) 0.8342(3) 1.1772(3) 0.0575(18) Uani 1 1 d . . . H16A H 0.5453 0.8163 1.2290 0.069 Uiso 1 1 calc R . . C17 C 0.5492(2) 0.8772(3) 1.1754(3) 0.0581(19) Uani 1 1 d . . . H17A H 0.5848 0.8890 1.2255 0.070 Uiso 1 1 calc R . . C18 C 0.5213(2) 0.9046(3) 1.1007(4) 0.0513(17) Uani 1 1 d . . . H18A H 0.5375 0.9355 1.0997 0.062 Uiso 1 1 calc R . . C19 C 0.4697(2) 0.8868(2) 1.0275(3) 0.0373(13) Uani 1 1 d . . . H19A H 0.4506 0.9056 0.9763 0.045 Uiso 1 1 calc R . . C20 C 0.35883(19) 0.76198(19) 0.9511(3) 0.0246(11) Uani 1 1 d . . . C21 C 0.3933(2) 0.7185(2) 0.9758(3) 0.0374(13) Uani 1 1 d . . . H21A H 0.4277 0.7217 0.9865 0.045 Uiso 1 1 calc R . . C22 C 0.3774(3) 0.6708(2) 0.9848(3) 0.0534(17) Uani 1 1 d . . . H22A H 0.4008 0.6413 1.0008 0.064 Uiso 1 1 calc R . . C23 C 0.3282(3) 0.6656(2) 0.9709(3) 0.0525(17) Uani 1 1 d . . . H23A H 0.3176 0.6328 0.9775 0.063 Uiso 1 1 calc R . . C24 C 0.2946(2) 0.7084(2) 0.9474(3) 0.0469(15) Uani 1 1 d . . . H24A H 0.2608 0.7053 0.9385 0.056 Uiso 1 1 calc R . . C25 C 0.3095(2) 0.7554(2) 0.9368(3) 0.0331(13) Uani 1 1 d . . . H25A H 0.2852 0.7844 0.9190 0.040 Uiso 1 1 calc R . . N1 N 0.32539(13) 0.88173(15) 0.71507(19) 0.0193(8) Uani 1 1 d . . . Si1 Si 0.29670(5) 0.90295(6) 0.61620(8) 0.0253(3) Uani 1 1 d . . . C26 C 0.3071(2) 0.9739(2) 0.6160(3) 0.0389(13) Uani 1 1 d . . . H26A H 0.3463 0.9807 0.6420 0.058 Uiso 1 1 calc R . . H26B H 0.2990 0.9917 0.6483 0.058 Uiso 1 1 calc R . . H26C H 0.2814 0.9867 0.5578 0.058 Uiso 1 1 calc R . . C27 C 0.21909(19) 0.8908(2) 0.5460(3) 0.0378(14) Uani 1 1 d . . . H27A H 0.2038 0.9096 0.5677 0.057 Uiso 1 1 calc R . . H27B H 0.2123 0.8535 0.5447 0.057 Uiso 1 1 calc R . . H27C H 0.2004 0.9029 0.4889 0.057 Uiso 1 1 calc R . . C28 C 0.3231(2) 0.8710(2) 0.5686(3) 0.0476(16) Uani 1 1 d . . . H28A H 0.3637 0.8775 0.6040 0.071 Uiso 1 1 calc R . . H28B H 0.3031 0.8851 0.5120 0.071 Uiso 1 1 calc R . . H28C H 0.3163 0.8335 0.5647 0.071 Uiso 1 1 calc R . . N2 N 0.33088(14) 0.86856(14) 0.9116(2) 0.0216(9) Uani 1 1 d . . . Si2 Si 0.32787(5) 0.89760(6) 0.98315(8) 0.0259(3) Uani 1 1 d . . . C29 C 0.3412(2) 0.8533(2) 1.0655(3) 0.0450(15) Uani 1 1 d . . . H29A H 0.3083 0.8306 1.0396 0.068 Uiso 1 1 calc R . . H29B H 0.3473 0.8742 1.1100 0.068 Uiso 1 1 calc R . . H29C H 0.3748 0.8321 1.0901 0.068 Uiso 1 1 calc R . . C30 C 0.3805(2) 0.9513(2) 1.0424(3) 0.0426(14) Uani 1 1 d . . . H30A H 0.3789 0.9733 1.0029 0.064 Uiso 1 1 calc R . . H30B H 0.4186 0.9365 1.0840 0.064 Uiso 1 1 calc R . . H30C H 0.3717 0.9721 1.0715 0.064 Uiso 1 1 calc R . . C31 C 0.2550(2) 0.9239(2) 0.9203(3) 0.0415(14) Uani 1 1 d . . . H31A H 0.2473 0.9483 0.8781 0.062 Uiso 1 1 calc R . . H31B H 0.2516 0.9419 0.9579 0.062 Uiso 1 1 calc R . . H31C H 0.2277 0.8953 0.8918 0.062 Uiso 1 1 calc R . . C32 C 0.16676(17) 0.90774(19) 0.6799(3) 0.0229(11) Uani 1 1 d . . . P3 P 0.14028(5) 0.84818(5) 0.65431(7) 0.0202(3) Uani 1 1 d . . . P4 P 0.17560(5) 0.96975(5) 0.67614(7) 0.0220(3) Uani 1 1 d . . . C33 C 0.07938(17) 0.83909(18) 0.5411(3) 0.0225(10) Uani 1 1 d . . . C34 C 0.03477(19) 0.8051(2) 0.5104(3) 0.0336(12) Uani 1 1 d . . . H34A H 0.0342 0.7861 0.5486 0.040 Uiso 1 1 calc R . . C35 C -0.0087(2) 0.7992(2) 0.4241(3) 0.0395(13) Uani 1 1 d . . . H35A H -0.0394 0.7766 0.4034 0.047 Uiso 1 1 calc R . . C36 C -0.0078(2) 0.8258(2) 0.3684(3) 0.0375(14) Uani 1 1 d . . . H36A H -0.0374 0.8210 0.3094 0.045 Uiso 1 1 calc R . . C37 C 0.0361(2) 0.8593(2) 0.3984(3) 0.0352(13) Uani 1 1 d . . . H37A H 0.0368 0.8781 0.3601 0.042 Uiso 1 1 calc R . . C38 C 0.07928(19) 0.86548(19) 0.4845(3) 0.0287(12) Uani 1 1 d . . . H38A H 0.1095 0.8886 0.5048 0.034 Uiso 1 1 calc R . . C39 C 0.11222(19) 0.83257(19) 0.7053(3) 0.0254(11) Uani 1 1 d . . . C40 C 0.06327(19) 0.8566(2) 0.6794(3) 0.0359(13) Uani 1 1 d . . . H40A H 0.0423 0.8785 0.6311 0.043 Uiso 1 1 calc R . . C41 C 0.0446(2) 0.8491(2) 0.7226(3) 0.0513(17) Uani 1 1 d . . . H41A H 0.0114 0.8661 0.7045 0.062 Uiso 1 1 calc R . . C42 C 0.0743(2) 0.8168(3) 0.7922(3) 0.0519(17) Uani 1 1 d . . . H42A H 0.0612 0.8112 0.8214 0.062 Uiso 1 1 calc R . . C43 C 0.1234(2) 0.7927(2) 0.8195(3) 0.0441(15) Uani 1 1 d . . . H43A H 0.1442 0.7709 0.8679 0.053 Uiso 1 1 calc R . . C44 C 0.1421(2) 0.8006(2) 0.7756(3) 0.0321(12) Uani 1 1 d . . . H44A H 0.1756 0.7839 0.7941 0.038 Uiso 1 1 calc R . . C45 C 0.14956(18) 1.0122(2) 0.7139(3) 0.0264(11) Uani 1 1 d . . . C46 C 0.1319(2) 0.9914(2) 0.7543(3) 0.0346(13) Uani 1 1 d . . . H46A H 0.1323 0.9549 0.7613 0.042 Uiso 1 1 calc R . . C47 C 0.1135(2) 1.0248(3) 0.7844(3) 0.0493(17) Uani 1 1 d . . . H47A H 0.1020 1.0108 0.8128 0.059 Uiso 1 1 calc R . . C48 C 0.1119(2) 1.0768(3) 0.7735(3) 0.0520(17) Uani 1 1 d . . . H48A H 0.0992 1.0990 0.7942 0.062 Uiso 1 1 calc R . . C49 C 0.1286(2) 1.0976(2) 0.7324(3) 0.0465(15) Uani 1 1 d . . . H49A H 0.1278 1.1341 0.7253 0.056 Uiso 1 1 calc R . . C50 C 0.1463(2) 1.0654(2) 0.7020(3) 0.0340(12) Uani 1 1 d . . . H50A H 0.1565 1.0799 0.6722 0.041 Uiso 1 1 calc R . . C51 C 0.1331(2) 0.99595(19) 0.5683(3) 0.0283(12) Uani 1 1 d . . . C52 C 0.0747(2) 0.9938(2) 0.5158(3) 0.0450(15) Uani 1 1 d . . . H52A H 0.0577 0.9801 0.5365 0.054 Uiso 1 1 calc R . . C53 C 0.0406(3) 1.0116(3) 0.4333(3) 0.0584(19) Uani 1 1 d . . . H53A H 0.0005 1.0108 0.3980 0.070 Uiso 1 1 calc R . . C54 C 0.0655(3) 1.0303(3) 0.4032(3) 0.0589(19) Uani 1 1 d . . . H54A H 0.0424 1.0416 0.3463 0.071 Uiso 1 1 calc R . . C55 C 0.1229(3) 1.0329(2) 0.4540(3) 0.0496(16) Uani 1 1 d . . . H55A H 0.1397 1.0466 0.4330 0.060 Uiso 1 1 calc R . . C56 C 0.1570(2) 1.0151(2) 0.5373(3) 0.0351(13) Uani 1 1 d . . . H56A H 0.1971 1.0162 0.5725 0.042 Uiso 1 1 calc R . . N3 N 0.19198(13) 0.80869(14) 0.68843(19) 0.0193(8) Uani 1 1 d . . . Si3 Si 0.18610(5) 0.74445(5) 0.65951(8) 0.0222(3) Uani 1 1 d . . . C57 C 0.1322(2) 0.7057(2) 0.6518(3) 0.0388(13) Uani 1 1 d . . . H57A H 0.1414 0.7064 0.7063 0.058 Uiso 1 1 calc R . . H57B H 0.1325 0.6697 0.6369 0.058 Uiso 1 1 calc R . . H57C H 0.0946 0.7208 0.6082 0.058 Uiso 1 1 calc R . . C58 C 0.1671(2) 0.7389(2) 0.5551(3) 0.0394(14) Uani 1 1 d . . . H58A H 0.1949 0.7579 0.5567 0.059 Uiso 1 1 calc R . . H58B H 0.1294 0.7538 0.5112 0.059 Uiso 1 1 calc R . . H58C H 0.1669 0.7023 0.5425 0.059 Uiso 1 1 calc R . . C59 C 0.25431(17) 0.70905(18) 0.7380(3) 0.0268(11) Uani 1 1 d . . . H59A H 0.2577 0.6983 0.7859 0.040 Uiso 1 1 calc R . . H59B H 0.2859 0.7320 0.7580 0.040 Uiso 1 1 calc R . . H59C H 0.2551 0.6783 0.7113 0.040 Uiso 1 1 calc R . . N4 N 0.24233(14) 0.97762(15) 0.7298(2) 0.0230(9) Uani 1 1 d . . . Si4 Si 0.29013(6) 1.02754(5) 0.78657(8) 0.0269(3) Uani 1 1 d . . . C60 C 0.36103(19) 0.9982(2) 0.8465(3) 0.0370(13) Uani 1 1 d . . . H60A H 0.3656 0.9861 0.8071 0.055 Uiso 1 1 calc R . . H60B H 0.3650 0.9688 0.8796 0.055 Uiso 1 1 calc R . . H60C H 0.3901 1.0242 0.8845 0.055 Uiso 1 1 calc R . . C61 C 0.2892(2) 1.0591(2) 0.8661(3) 0.0350(13) Uani 1 1 d . . . H61A H 0.2915 1.0323 0.9013 0.053 Uiso 1 1 calc R . . H61B H 0.2541 1.0789 0.8368 0.053 Uiso 1 1 calc R . . H61C H 0.3217 1.0826 0.9018 0.053 Uiso 1 1 calc R . . C62 C 0.2828(2) 1.0808(2) 0.7200(3) 0.0393(13) Uani 1 1 d . . . H62A H 0.2873 1.0666 0.6815 0.059 Uiso 1 1 calc R . . H62B H 0.3120 1.1072 0.7562 0.059 Uiso 1 1 calc R . . H62C H 0.2453 1.0967 0.6872 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 Ce1 0.01344(13) 0.01836(14) 0.01672(13) 0.00016(12) 0.00834(12) 0.00038(11) C1 0.020(3) 0.021(3) 0.017(2) -0.004(2) 0.009(2) -0.003(2) P1 0.0167(7) 0.0206(7) 0.0192(6) -0.0006(5) 0.0110(6) -0.0001(5) P2 0.0173(7) 0.0231(7) 0.0169(6) -0.0002(5) 0.0095(6) -0.0007(5) C2 0.015(2) 0.018(3) 0.016(2) 0.0018(19) 0.007(2) 0.0010(19) C3 0.036(3) 0.032(3) 0.038(3) -0.006(2) 0.029(3) -0.004(2) C4 0.039(3) 0.038(4) 0.036(3) -0.012(3) 0.025(3) -0.016(3) C5 0.040(3) 0.022(3) 0.024(3) 0.001(2) 0.019(3) 0.006(2) C6 0.023(3) 0.044(4) 0.022(3) 0.002(2) 0.014(3) 0.008(2) C7 0.018(3) 0.030(3) 0.016(2) -0.001(2) 0.006(2) 0.002(2) C8 0.015(2) 0.027(3) 0.022(2) -0.002(2) 0.011(2) 0.000(2) C9 0.017(3) 0.032(3) 0.034(3) 0.004(2) 0.012(3) 0.005(2) C10 0.029(3) 0.033(4) 0.056(4) 0.005(3) 0.023(3) -0.008(3) C11 0.023(3) 0.038(4) 0.050(4) -0.007(3) 0.018(3) -0.010(2) C12 0.021(3) 0.046(4) 0.030(3) 0.001(3) 0.008(3) -0.001(2) C13 0.019(3) 0.028(3) 0.029(3) 0.001(2) 0.011(3) -0.004(2) C14 0.018(3) 0.034(3) 0.019(3) -0.003(2) 0.009(2) 0.000(2) C15 0.031(3) 0.053(4) 0.025(3) 0.002(3) 0.011(3) 0.002(3) C16 0.033(4) 0.080(6) 0.023(3) -0.002(3) 0.003(3) 0.008(3) C17 0.019(3) 0.098(6) 0.030(3) -0.031(4) 0.004(3) -0.018(4) C18 0.030(3) 0.069(5) 0.050(4) -0.032(3) 0.024(3) -0.024(3) C19 0.027(3) 0.051(4) 0.032(3) -0.009(3) 0.019(3) -0.007(3) C20 0.026(3) 0.026(3) 0.012(2) 0.002(2) 0.008(2) 0.001(2) C21 0.044(4) 0.032(3) 0.034(3) 0.005(2) 0.025(3) 0.007(3) C22 0.088(5) 0.028(4) 0.045(4) 0.010(3) 0.045(4) 0.012(3) C23 0.079(5) 0.036(4) 0.037(4) -0.004(3) 0.036(4) -0.017(3) C24 0.058(4) 0.050(4) 0.041(3) -0.004(3) 0.036(4) -0.016(3) C25 0.033(3) 0.040(4) 0.024(3) 0.000(2) 0.018(3) -0.007(2) N1 0.014(2) 0.021(2) 0.0129(18) 0.0029(17) 0.0045(17) 0.0007(17) Si1 0.0241(8) 0.0292(8) 0.0238(7) 0.0062(6) 0.0164(7) 0.0048(6) C26 0.035(3) 0.036(4) 0.036(3) 0.017(3) 0.019(3) 0.003(2) C27 0.033(3) 0.045(4) 0.026(3) 0.006(2) 0.016(3) 0.004(3) C28 0.059(4) 0.060(5) 0.035(3) 0.020(3) 0.036(3) 0.027(3) N2 0.021(2) 0.020(2) 0.020(2) 0.0003(16) 0.0120(19) 0.0026(16) Si2 0.0216(8) 0.0309(9) 0.0212(7) -0.0040(6) 0.0123(7) 0.0001(6) C29 0.051(4) 0.060(4) 0.033(3) 0.005(3) 0.032(3) 0.011(3) C30 0.037(3) 0.045(4) 0.042(3) -0.022(3) 0.025(3) -0.005(3) C31 0.033(3) 0.047(4) 0.032(3) -0.012(3) 0.016(3) 0.004(3) C32 0.014(2) 0.028(3) 0.021(2) 0.006(2) 0.009(2) 0.006(2) P3 0.0136(6) 0.0221(7) 0.0196(6) -0.0015(5) 0.0086(6) -0.0016(5) P4 0.0199(7) 0.0190(7) 0.0223(7) 0.0002(5) 0.0118(6) 0.0030(5) C33 0.010(2) 0.025(3) 0.022(3) -0.002(2) 0.006(2) 0.0016(19) C34 0.020(3) 0.032(3) 0.028(3) -0.003(2) 0.007(3) -0.003(2) C35 0.019(3) 0.033(3) 0.038(3) -0.008(3) 0.006(3) -0.002(2) C36 0.026(3) 0.041(4) 0.023(3) -0.011(3) 0.006(3) 0.007(3) C37 0.025(3) 0.054(4) 0.022(3) -0.003(2) 0.013(3) 0.007(3) C38 0.023(3) 0.035(3) 0.026(3) -0.004(2) 0.015(3) -0.003(2) C39 0.027(3) 0.025(3) 0.026(3) -0.005(2) 0.018(3) -0.006(2) C40 0.029(3) 0.041(4) 0.044(3) 0.008(3) 0.027(3) 0.004(2) C41 0.042(4) 0.065(5) 0.065(4) 0.013(3) 0.043(4) 0.012(3) C42 0.059(4) 0.066(5) 0.058(4) 0.003(3) 0.050(4) -0.001(3) C43 0.040(4) 0.059(4) 0.036(3) 0.008(3) 0.026(3) 0.008(3) C44 0.029(3) 0.036(3) 0.030(3) -0.002(2) 0.019(3) -0.002(2) C45 0.010(2) 0.031(3) 0.021(3) -0.001(2) 0.003(2) 0.004(2) C46 0.031(3) 0.038(3) 0.029(3) 0.005(2) 0.017(3) 0.011(2) C47 0.048(4) 0.067(5) 0.037(3) 0.016(3) 0.030(3) 0.025(3) C48 0.053(4) 0.056(5) 0.039(3) 0.000(3) 0.027(3) 0.025(3) C49 0.041(4) 0.038(4) 0.053(4) -0.006(3) 0.028(3) 0.010(3) C50 0.029(3) 0.029(3) 0.041(3) 0.000(2) 0.021(3) 0.005(2) C51 0.029(3) 0.021(3) 0.023(3) -0.001(2) 0.012(3) 0.009(2) C52 0.034(4) 0.055(4) 0.032(3) 0.003(3) 0.015(3) 0.015(3) C53 0.041(4) 0.071(5) 0.030(3) 0.009(3) 0.009(3) 0.030(3) C54 0.077(5) 0.055(5) 0.026(3) 0.009(3) 0.026(4) 0.032(4) C55 0.074(5) 0.041(4) 0.033(4) 0.003(3) 0.035(4) 0.006(3) C56 0.040(3) 0.034(3) 0.026(3) -0.006(2) 0.020(3) -0.004(2) N3 0.012(2) 0.025(2) 0.0143(19) 0.0001(16) 0.0057(18) -0.0029(16) Si3 0.0206(8) 0.0206(8) 0.0215(7) -0.0019(6) 0.0121(7) -0.0019(5) C57 0.033(3) 0.025(3) 0.050(3) 0.002(3) 0.024(3) -0.004(2) C58 0.048(4) 0.035(4) 0.028(3) -0.004(2) 0.022(3) 0.002(3) C59 0.027(3) 0.018(3) 0.032(3) -0.006(2) 0.017(3) -0.003(2) N4 0.016(2) 0.025(2) 0.020(2) -0.0036(17) 0.0085(19) -0.0010(16) Si4 0.0263(8) 0.0201(8) 0.0294(8) -0.0055(6) 0.0162(7) -0.0046(6) C60 0.031(3) 0.035(4) 0.039(3) -0.011(3) 0.020(3) -0.007(2) C61 0.037(3) 0.031(3) 0.028(3) -0.002(2) 0.018(3) 0.000(2) C62 0.044(3) 0.026(3) 0.048(3) -0.009(3) 0.030(3) -0.012(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 Ce1 C32 2.472(4) . ? Ce1 N2 2.500(3) . ? Ce1 N1 2.522(3) . ? Ce1 N3 2.537(3) . ? Ce1 N4 2.556(4) . ? Ce1 C1 3.033(4) . ? C1 P2 1.736(4) . ? C1 P1 1.738(4) . ? P1 N1 1.614(3) . ? P1 C2 1.813(4) . ? P1 C8 1.820(4) . ? P2 N2 1.614(4) . ? P2 C20 1.811(5) . ? P2 C14 1.824(5) . ? C2 C3 1.378(6) . ? C2 C7 1.395(5) . ? C3 C4 1.382(6) . ? C4 C5 1.378(6) . ? C5 C6 1.370(7) . ? C6 C7 1.376(6) . ? C8 C9 1.374(7) . ? C8 C13 1.395(6) . ? C9 C10 1.388(6) . ? C10 C11 1.376(7) . ? C11 C12 1.370(7) . ? C12 C13 1.382(6) . ? C14 C19 1.387(7) . ? C14 C15 1.389(6) . ? C15 C16 1.404(7) . ? C16 C17 1.334(9) . ? C17 C18 1.388(8) . ? C18 C19 1.387(6) . ? C20 C25 1.378(6) . ? C20 C21 1.398(7) . ? C21 C22 1.384(7) . ? C22 C23 1.377(8) . ? C23 C24 1.372(8) . ? C24 C25 1.369(7) . ? N1 Si1 1.724(3) . ? Si1 C26 1.854(5) . ? Si1 C28 1.858(4) . ? Si1 C27 1.864(5) . ? N2 Si2 1.737(3) . ? Si2 C31 1.859(5) . ? Si2 C30 1.865(5) . ? Si2 C29 1.877(5) . ? C32 P4 1.631(5) . ? C32 P3 1.656(5) . ? P3 N3 1.627(4) . ? P3 C39 1.824(4) . ? P3 C33 1.842(4) . ? P4 N4 1.609(4) . ? P4 C45 1.829(5) . ? P4 C51 1.843(5) . ? C33 C38 1.369(6) . ? C33 C34 1.397(6) . ? C34 C35 1.386(6) . ? C35 C36 1.372(7) . ? C36 C37 1.379(7) . ? C37 C38 1.383(6) . ? C39 C44 1.385(6) . ? C39 C40 1.391(6) . ? C40 C41 1.380(6) . ? C41 C42 1.380(7) . ? C42 C43 1.387(7) . ? C43 C44 1.398(6) . ? C45 C50 1.383(7) . ? C45 C46 1.392(6) . ? C46 C47 1.396(7) . ? C47 C48 1.353(8) . ? C48 C49 1.379(7) . ? C49 C50 1.367(6) . ? C51 C56 1.371(6) . ? C51 C52 1.384(7) . ? C52 C53 1.386(7) . ? C53 C54 1.377(8) . ? C54 C55 1.363(8) . ? C55 C56 1.399(6) . ? N3 Si3 1.729(4) . ? Si3 C58 1.864(4) . ? Si3 C59 1.867(4) . ? Si3 C57 1.876(5) . ? N4 Si4 1.723(4) . ? Si4 C60 1.849(5) . ? Si4 C62 1.864(5) . ? Si4 C61 1.877(4) . ? 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 C32 Ce1 N2 118.57(12) . . ? C32 Ce1 N1 132.62(12) . . ? N2 Ce1 N1 107.02(10) . . ? C32 Ce1 N3 63.60(14) . . ? N2 Ce1 N3 107.46(11) . . ? N1 Ce1 N3 115.33(11) . . ? C32 Ce1 N4 61.86(13) . . ? N2 Ce1 N4 105.74(11) . . ? N1 Ce1 N4 95.07(11) . . ? N3 Ce1 N4 124.66(11) . . ? C32 Ce1 C1 159.81(14) . . ? N2 Ce1 C1 59.43(11) . . ? N1 Ce1 C1 59.14(11) . . ? N3 Ce1 C1 97.06(12) . . ? N4 Ce1 C1 138.07(12) . . ? P2 C1 P1 138.9(3) . . ? P2 C1 Ce1 82.77(16) . . ? P1 C1 Ce1 83.77(16) . . ? N1 P1 C1 111.79(19) . . ? N1 P1 C2 110.79(19) . . ? C1 P1 C2 104.0(2) . . ? N1 P1 C8 111.1(2) . . ? C1 P1 C8 114.36(19) . . ? C2 P1 C8 104.30(19) . . ? N2 P2 C1 112.2(2) . . ? N2 P2 C20 111.5(2) . . ? C1 P2 C20 101.9(2) . . ? N2 P2 C14 108.8(2) . . ? C1 P2 C14 115.9(2) . . ? C20 P2 C14 106.3(2) . . ? C3 C2 C7 117.8(4) . . ? C3 C2 P1 118.8(3) . . ? C7 C2 P1 123.2(3) . . ? C2 C3 C4 121.8(4) . . ? C5 C4 C3 119.2(5) . . ? C6 C5 C4 119.9(4) . . ? C5 C6 C7 120.6(4) . . ? C6 C7 C2 120.6(4) . . ? C9 C8 C13 118.9(4) . . ? C9 C8 P1 121.1(3) . . ? C13 C8 P1 119.7(4) . . ? C8 C9 C10 121.0(5) . . ? C11 C10 C9 119.0(5) . . ? C12 C11 C10 121.0(5) . . ? C11 C12 C13 119.8(5) . . ? C12 C13 C8 120.3(5) . . ? C19 C14 C15 118.9(5) . . ? C19 C14 P2 117.5(3) . . ? C15 C14 P2 123.3(4) . . ? C14 C15 C16 119.3(6) . . ? C17 C16 C15 121.3(6) . . ? C16 C17 C18 120.3(5) . . ? C19 C18 C17 119.6(6) . . ? C18 C19 C14 120.6(5) . . ? C25 C20 C21 117.8(5) . . ? C25 C20 P2 119.9(4) . . ? C21 C20 P2 122.3(4) . . ? C22 C21 C20 120.1(5) . . ? C23 C22 C21 120.8(6) . . ? C24 C23 C22 119.1(6) . . ? C25 C24 C23 120.4(5) . . ? C24 C25 C20 121.8(5) . . ? P1 N1 Si1 131.6(2) . . ? P1 N1 Ce1 105.00(15) . . ? Si1 N1 Ce1 119.71(16) . . ? N1 Si1 C26 111.2(2) . . ? N1 Si1 C28 116.4(2) . . ? C26 Si1 C28 107.1(2) . . ? N1 Si1 C27 105.99(18) . . ? C26 Si1 C27 107.6(2) . . ? C28 Si1 C27 108.1(2) . . ? P2 N2 Si2 127.0(2) . . ? P2 N2 Ce1 104.62(15) . . ? Si2 N2 Ce1 128.32(18) . . ? N2 Si2 C31 106.41(19) . . ? N2 Si2 C30 111.7(2) . . ? C31 Si2 C30 109.8(3) . . ? N2 Si2 C29 115.6(2) . . ? C31 Si2 C29 107.5(2) . . ? C30 Si2 C29 105.7(2) . . ? P4 C32 P3 162.8(3) . . ? P4 C32 Ce1 97.28(19) . . ? P3 C32 Ce1 95.46(19) . . ? N3 P3 C32 107.1(2) . . ? N3 P3 C39 109.2(2) . . ? C32 P3 C39 110.2(2) . . ? N3 P3 C33 112.11(19) . . ? C32 P3 C33 114.2(2) . . ? C39 P3 C33 103.9(2) . . ? N4 P4 C32 105.9(2) . . ? N4 P4 C45 111.5(2) . . ? C32 P4 C45 115.1(2) . . ? N4 P4 C51 111.8(2) . . ? C32 P4 C51 114.2(2) . . ? C45 P4 C51 98.5(2) . . ? C38 C33 C34 118.7(4) . . ? C38 C33 P3 118.0(3) . . ? C34 C33 P3 123.3(4) . . ? C35 C34 C33 119.8(5) . . ? C36 C35 C34 120.6(5) . . ? C35 C36 C37 119.8(5) . . ? C36 C37 C38 119.5(5) . . ? C33 C38 C37 121.5(5) . . ? C44 C39 C40 118.7(4) . . ? C44 C39 P3 120.5(3) . . ? C40 C39 P3 120.4(4) . . ? C41 C40 C39 121.1(5) . . ? C42 C41 C40 120.0(5) . . ? C41 C42 C43 120.0(5) . . ? C42 C43 C44 119.7(5) . . ? C39 C44 C43 120.5(5) . . ? C50 C45 C46 118.6(4) . . ? C50 C45 P4 120.9(4) . . ? C46 C45 P4 120.4(4) . . ? C45 C46 C47 119.2(5) . . ? C48 C47 C46 120.9(5) . . ? C47 C48 C49 120.2(5) . . ? C50 C49 C48 119.7(6) . . ? C49 C50 C45 121.3(5) . . ? C56 C51 C52 119.0(5) . . ? C56 C51 P4 122.5(4) . . ? C52 C51 P4 118.4(4) . . ? C51 C52 C53 120.9(5) . . ? C54 C53 C52 119.1(6) . . ? C55 C54 C53 120.9(5) . . ? C54 C55 C56 119.5(5) . . ? C51 C56 C55 120.5(5) . . ? P3 N3 Si3 126.7(2) . . ? P3 N3 Ce1 93.79(17) . . ? Si3 N3 Ce1 137.75(17) . . ? N3 Si3 C58 111.4(2) . . ? N3 Si3 C59 111.13(18) . . ? C58 Si3 C59 107.3(2) . . ? N3 Si3 C57 114.8(2) . . ? C58 Si3 C57 106.6(2) . . ? C59 Si3 C57 105.1(2) . . ? P4 N4 Si4 135.8(2) . . ? P4 N4 Ce1 94.66(17) . . ? Si4 N4 Ce1 125.90(18) . . ? N4 Si4 C60 106.0(2) . . ? N4 Si4 C62 114.0(2) . . ? C60 Si4 C62 108.1(2) . . ? N4 Si4 C61 115.1(2) . . ? C60 Si4 C61 106.6(2) . . ? C62 Si4 C61 106.6(2) . . ? _diffrn_measured_fraction_theta_max 0.868 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.868 _refine_diff_density_max 1.05 _refine_diff_density_min -0.62 _refine_diff_density_rms 0.08 #=== END of CIF # Attachment '14.cif' data_14 _database_code_depnum_ccdc_archive 'CCDC 736112' _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62 H77 N4 P4 Pr Si4' _chemical_formula_sum 'C62 H77 N4 P4 Pr Si4' _chemical_formula_weight 1255.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 31.291(4) _cell_length_b 25.714(4) _cell_length_c 21.013(3) _cell_angle_alpha 90.00 _cell_angle_beta 131.112(2) _cell_angle_gamma 90.00 _cell_volume 12738(3) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5117 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 27.38 _exptl_crystal_description column _exptl_crystal_colour yellow _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.309 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5216 _exptl_absorpt_coefficient_mu 0.981 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.85 _exptl_absorpt_correction_T_max 0.93 _exptl_absorpt_process_details '(SADABS; Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 31442 _diffrn_reflns_av_R_equivalents 0.0777 _diffrn_reflns_av_sigmaI/netI 0.0937 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 24.50 _reflns_number_total 10571 _reflns_number_gt 7928 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'enCIFer(Allen et al.,2004);PLATON(Spek,2003)' _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^)+(0.0511P)^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, Me from difmap' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10571 _refine_ls_number_parameters 688 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0837 _refine_ls_R_factor_gt 0.0573 _refine_ls_wR_factor_ref 0.1220 _refine_ls_wR_factor_gt 0.1139 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _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 Pr1 Pr 0.265175(13) 0.619635(11) 0.75479(2) 0.01470(10) Uani 1 1 d . . . C1 C 0.1668(2) 0.5932(2) 0.6798(4) 0.0223(14) Uani 1 1 d . . . P1 P 0.17601(6) 0.53069(5) 0.67690(10) 0.0185(3) Uani 1 1 d . . . C2 C 0.1496(2) 0.4885(2) 0.7140(4) 0.0225(14) Uani 1 1 d . . . C3 C 0.1319(3) 0.5091(2) 0.7540(4) 0.0294(16) Uani 1 1 d . . . H3A H 0.1326 0.5456 0.7615 0.035 Uiso 1 1 calc R . . C4 C 0.1128(3) 0.4756(3) 0.7836(5) 0.0441(19) Uani 1 1 d . . . H4A H 0.1002 0.4895 0.8107 0.053 Uiso 1 1 calc R . . C5 C 0.1122(3) 0.4228(3) 0.7735(5) 0.047(2) Uani 1 1 d . . . H5A H 0.1003 0.4004 0.7952 0.057 Uiso 1 1 calc R . . C6 C 0.1287(3) 0.4023(3) 0.7325(5) 0.0414(19) Uani 1 1 d . . . H6A H 0.1274 0.3658 0.7243 0.050 Uiso 1 1 calc R . . C7 C 0.1472(3) 0.4350(2) 0.7030(4) 0.0316(16) Uani 1 1 d . . . H7A H 0.1586 0.4207 0.6745 0.038 Uiso 1 1 calc R . . C8 C 0.1338(3) 0.5054(2) 0.5693(4) 0.0269(15) Uani 1 1 d . . . C9 C 0.0750(3) 0.5073(3) 0.5167(4) 0.0398(18) Uani 1 1 d . . . H9A H 0.0579 0.5211 0.5373 0.048 Uiso 1 1 calc R . . C10 C 0.0413(3) 0.4893(3) 0.4347(5) 0.056(2) Uani 1 1 d . . . H10A H 0.0012 0.4906 0.3996 0.068 Uiso 1 1 calc R . . C11 C 0.0648(4) 0.4697(3) 0.4037(5) 0.053(2) Uani 1 1 d . . . H11A H 0.0412 0.4576 0.3471 0.064 Uiso 1 1 calc R . . C12 C 0.1228(4) 0.4675(3) 0.4546(5) 0.048(2) Uani 1 1 d . . . H12A H 0.1396 0.4537 0.4335 0.057 Uiso 1 1 calc R . . C13 C 0.1566(3) 0.4856(2) 0.5366(4) 0.0323(16) Uani 1 1 d . . . H13A H 0.1967 0.4842 0.5714 0.039 Uiso 1 1 calc R . . N1 N 0.24326(19) 0.52247(17) 0.7305(3) 0.0216(11) Uani 1 1 d . . . Si1 Si 0.29058(7) 0.47289(6) 0.78725(12) 0.0238(4) Uani 1 1 d . . . C26 C 0.2823(3) 0.4192(2) 0.7197(4) 0.0349(17) Uani 1 1 d . . . H26A H 0.2886 0.4329 0.6830 0.052 Uiso 1 1 calc R . . H26B H 0.2440 0.4048 0.6851 0.052 Uiso 1 1 calc R . . H26C H 0.3101 0.3918 0.7559 0.052 Uiso 1 1 calc R . . C27 C 0.2895(3) 0.4411(2) 0.8672(4) 0.0325(16) Uani 1 1 d . . . H27A H 0.2909 0.4680 0.9016 0.049 Uiso 1 1 calc R . . H27B H 0.3224 0.4181 0.9037 0.049 Uiso 1 1 calc R . . H27C H 0.2546 0.4208 0.8377 0.049 Uiso 1 1 calc R . . C28 C 0.3631(3) 0.5016(2) 0.8483(4) 0.0334(17) Uani 1 1 d . . . H28A H 0.3686 0.5118 0.8092 0.050 Uiso 1 1 calc R . . H28B H 0.3917 0.4757 0.8881 0.050 Uiso 1 1 calc R . . H28C H 0.3669 0.5322 0.8794 0.050 Uiso 1 1 calc R . . P2 P 0.14092(6) 0.65253(5) 0.65516(10) 0.0175(3) Uani 1 1 d . . . C14 C 0.0795(2) 0.6613(2) 0.5423(4) 0.0201(14) Uani 1 1 d . . . C15 C 0.0795(3) 0.6345(2) 0.4850(4) 0.0272(15) Uani 1 1 d . . . H15A H 0.1097 0.6114 0.5049 0.033 Uiso 1 1 calc R . . C16 C 0.0359(3) 0.6413(3) 0.3991(4) 0.0343(16) Uani 1 1 d . . . H16A H 0.0365 0.6226 0.3606 0.041 Uiso 1 1 calc R . . C17 C -0.0079(3) 0.6744(3) 0.3688(4) 0.0365(18) Uani 1 1 d . . . H17A H -0.0376 0.6791 0.3098 0.044 Uiso 1 1 calc R . . C18 C -0.0081(3) 0.7010(2) 0.4262(4) 0.0356(17) Uani 1 1 d . . . H18A H -0.0386 0.7239 0.4058 0.043 Uiso 1 1 calc R . . C19 C 0.0346(3) 0.6949(2) 0.5113(4) 0.0288(15) Uani 1 1 d . . . H19A H 0.0336 0.7135 0.5494 0.035 Uiso 1 1 calc R . . C20 C 0.1129(2) 0.6687(2) 0.7066(4) 0.0219(14) Uani 1 1 d . . . C21 C 0.0635(3) 0.6435(2) 0.6801(4) 0.0335(16) Uani 1 1 d . . . H21A H 0.0426 0.6212 0.6323 0.040 Uiso 1 1 calc R . . C22 C 0.0456(3) 0.6518(3) 0.7246(5) 0.047(2) Uani 1 1 d . . . H22A H 0.0120 0.6353 0.7063 0.057 Uiso 1 1 calc R . . C23 C 0.0752(3) 0.6830(3) 0.7940(5) 0.049(2) Uani 1 1 d . . . H23A H 0.0623 0.6880 0.8238 0.058 Uiso 1 1 calc R . . C24 C 0.1243(3) 0.7076(3) 0.8210(5) 0.0431(19) Uani 1 1 d . . . H24A H 0.1453 0.7296 0.8692 0.052 Uiso 1 1 calc R . . C25 C 0.1423(3) 0.6993(2) 0.7766(4) 0.0300(16) Uani 1 1 d . . . H25A H 0.1762 0.7155 0.7956 0.036 Uiso 1 1 calc R . . N2 N 0.19290(19) 0.69179(17) 0.6889(3) 0.0199(11) Uani 1 1 d . . . Si2 Si 0.18649(7) 0.75602(6) 0.65961(11) 0.0191(4) Uani 1 1 d . . . C29 C 0.1679(3) 0.7615(2) 0.5558(4) 0.0351(17) Uani 1 1 d . . . H29A H 0.1951 0.7415 0.5570 0.053 Uiso 1 1 calc R . . H29B H 0.1692 0.7981 0.5442 0.053 Uiso 1 1 calc R . . H29C H 0.1296 0.7478 0.5114 0.053 Uiso 1 1 calc R . . C30 C 0.2545(2) 0.7919(2) 0.7379(4) 0.0251(15) Uani 1 1 d . . . H30A H 0.2863 0.7698 0.7557 0.038 Uiso 1 1 calc R . . H30B H 0.2588 0.8009 0.7872 0.038 Uiso 1 1 calc R . . H30C H 0.2542 0.8237 0.7120 0.038 Uiso 1 1 calc R . . C31 C 0.1325(3) 0.7945(2) 0.6522(5) 0.0345(17) Uani 1 1 d . . . H31A H 0.0946 0.7806 0.6065 0.052 Uiso 1 1 calc R . . H31B H 0.1342 0.8310 0.6405 0.052 Uiso 1 1 calc R . . H31C H 0.1406 0.7921 0.7057 0.052 Uiso 1 1 calc R . . C32 C 0.3678(2) 0.6881(2) 0.8450(4) 0.0173(13) Uani 1 1 d . . . H32A H 0.3559 0.7250 0.8267 0.021 Uiso 1 1 calc R . . P3 P 0.37382(6) 0.67538(5) 0.93075(10) 0.0175(3) Uani 1 1 d . . . C33 C 0.3577(2) 0.7381(2) 0.9507(4) 0.0197(13) Uani 1 1 d . . . C34 C 0.3921(3) 0.7815(2) 0.9752(4) 0.0333(16) Uani 1 1 d . . . H34A H 0.4265 0.7783 0.9857 0.040 Uiso 1 1 calc R . . C35 C 0.3762(4) 0.8293(2) 0.9842(5) 0.045(2) Uani 1 1 d . . . H35A H 0.3995 0.8589 1.0002 0.054 Uiso 1 1 calc R . . C36 C 0.3263(4) 0.8340(3) 0.9699(5) 0.049(2) Uani 1 1 d . . . H36A H 0.3156 0.8667 0.9768 0.058 Uiso 1 1 calc R . . C37 C 0.2924(3) 0.7913(3) 0.9457(4) 0.0412(18) Uani 1 1 d . . . H37A H 0.2583 0.7945 0.9359 0.049 Uiso 1 1 calc R . . C38 C 0.3077(3) 0.7437(2) 0.9355(4) 0.0277(15) Uani 1 1 d . . . H38A H 0.2836 0.7145 0.9179 0.033 Uiso 1 1 calc R . . C39 C 0.4448(2) 0.6583(2) 1.0279(4) 0.0239(14) Uani 1 1 d . . . C40 C 0.4735(3) 0.6850(3) 1.1032(4) 0.0395(18) Uani 1 1 d . . . H40A H 0.4575 0.7158 1.1049 0.047 Uiso 1 1 calc R . . C41 C 0.5252(3) 0.6672(3) 1.1762(5) 0.053(2) Uani 1 1 d . . . H41A H 0.5447 0.6861 1.2274 0.064 Uiso 1 1 calc R . . C42 C 0.5485(3) 0.6222(4) 1.1748(5) 0.055(2) Uani 1 1 d . . . H42A H 0.5836 0.6098 1.2253 0.066 Uiso 1 1 calc R . . C43 C 0.5213(3) 0.5953(3) 1.1009(5) 0.046(2) Uani 1 1 d . . . H43A H 0.5379 0.5647 1.0999 0.055 Uiso 1 1 calc R . . C44 C 0.4690(3) 0.6130(2) 1.0269(4) 0.0321(16) Uani 1 1 d . . . H44A H 0.4499 0.5941 0.9757 0.039 Uiso 1 1 calc R . . N3 N 0.3301(2) 0.63146(16) 0.9108(3) 0.0199(11) Uani 1 1 d . . . Si3 Si 0.32736(7) 0.60197(6) 0.98272(11) 0.0223(4) Uani 1 1 d . . . C57 C 0.2540(3) 0.5762(3) 0.9201(4) 0.0361(17) Uani 1 1 d . . . H57A H 0.2461 0.5512 0.8783 0.054 Uiso 1 1 calc R . . H57B H 0.2268 0.6050 0.8911 0.054 Uiso 1 1 calc R . . H57C H 0.2505 0.5589 0.9580 0.054 Uiso 1 1 calc R . . C58 C 0.3403(3) 0.6459(3) 1.0649(4) 0.0415(18) Uani 1 1 d . . . H58A H 0.3097 0.6716 1.0378 0.062 Uiso 1 1 calc R . . H58B H 0.3766 0.6639 1.0949 0.062 Uiso 1 1 calc R . . H58C H 0.3414 0.6253 1.1052 0.062 Uiso 1 1 calc R . . C59 C 0.3806(3) 0.5486(3) 1.0429(5) 0.0412(19) Uani 1 1 d . . . H59A H 0.3818 0.5283 1.0046 0.062 Uiso 1 1 calc R . . H59B H 0.3699 0.5259 1.0679 0.062 Uiso 1 1 calc R . . H59C H 0.4181 0.5636 1.0878 0.062 Uiso 1 1 calc R . . P4 P 0.37676(6) 0.65711(5) 0.78048(10) 0.0166(3) Uani 1 1 d . . . C45 C 0.4447(2) 0.6251(2) 0.8376(4) 0.0180(13) Uani 1 1 d . . . C46 C 0.4479(3) 0.5770(2) 0.8123(4) 0.0289(15) Uani 1 1 d . . . H46A H 0.4142 0.5593 0.7674 0.035 Uiso 1 1 calc R . . C47 C 0.5012(3) 0.5541(2) 0.8531(5) 0.0399(19) Uani 1 1 d . . . H47A H 0.5035 0.5208 0.8358 0.048 Uiso 1 1 calc R . . C48 C 0.5497(3) 0.5798(2) 0.9173(5) 0.0363(18) Uani 1 1 d . . . H48A H 0.5857 0.5643 0.9448 0.044 Uiso 1 1 calc R . . C49 C 0.5464(3) 0.6281(2) 0.9423(4) 0.0349(17) Uani 1 1 d . . . H49A H 0.5802 0.6461 0.9863 0.042 Uiso 1 1 calc R . . C50 C 0.4943(3) 0.6505(2) 0.9036(4) 0.0299(16) Uani 1 1 d . . . H50A H 0.4924 0.6833 0.9223 0.036 Uiso 1 1 calc R . . C51 C 0.3790(2) 0.7100(2) 0.7247(4) 0.0173(13) Uani 1 1 d . . . C52 C 0.3333(3) 0.7435(2) 0.6772(4) 0.0278(15) Uani 1 1 d . . . H52A H 0.3026 0.7393 0.6759 0.033 Uiso 1 1 calc R . . C53 C 0.3321(3) 0.7831(2) 0.6313(4) 0.0345(17) Uani 1 1 d . . . H53A H 0.3013 0.8069 0.6006 0.041 Uiso 1 1 calc R . . C54 C 0.3750(3) 0.7882(2) 0.6299(4) 0.0270(15) Uani 1 1 d . . . H54A H 0.3736 0.8154 0.5980 0.032 Uiso 1 1 calc R . . C55 C 0.4198(3) 0.7544(2) 0.6741(4) 0.0284(15) Uani 1 1 d . . . H55A H 0.4489 0.7575 0.6717 0.034 Uiso 1 1 calc R . . C56 C 0.4225(2) 0.7156(2) 0.7225(4) 0.0230(14) Uani 1 1 d . . . H56A H 0.4541 0.6927 0.7543 0.028 Uiso 1 1 calc R . . N4 N 0.32490(18) 0.61855(16) 0.7148(3) 0.0178(10) Uani 1 1 d . . . Si4 Si 0.29659(7) 0.59688(6) 0.61616(11) 0.0220(4) Uani 1 1 d . . . C60 C 0.3229(3) 0.6294(3) 0.5684(5) 0.0433(19) Uani 1 1 d . . . H60A H 0.3133 0.6664 0.5605 0.065 Uiso 1 1 calc R . . H60B H 0.3051 0.6134 0.5136 0.065 Uiso 1 1 calc R . . H60C H 0.3642 0.6254 0.6060 0.065 Uiso 1 1 calc R . . C61 C 0.3069(3) 0.5255(2) 0.6163(4) 0.0342(17) Uani 1 1 d . . . H61A H 0.2982 0.5078 0.6479 0.051 Uiso 1 1 calc R . . H61B H 0.3464 0.5186 0.6430 0.051 Uiso 1 1 calc R . . H61C H 0.2816 0.5127 0.5580 0.051 Uiso 1 1 calc R . . C62 C 0.2198(3) 0.6093(2) 0.5472(4) 0.0333(16) Uani 1 1 d . . . H62A H 0.2042 0.5895 0.5677 0.050 Uiso 1 1 calc R . . H62B H 0.2011 0.5984 0.4894 0.050 Uiso 1 1 calc R . . H62C H 0.2133 0.6465 0.5477 0.050 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 Pr1 0.01457(16) 0.01351(15) 0.01782(18) -0.00018(15) 0.01143(14) -0.00052(14) C1 0.014(3) 0.023(3) 0.025(4) 0.001(3) 0.011(3) -0.006(3) P1 0.0197(8) 0.0142(7) 0.0224(9) 0.0001(7) 0.0142(8) -0.0029(6) C2 0.014(3) 0.024(3) 0.023(4) 0.001(3) 0.009(3) -0.005(3) C3 0.029(4) 0.026(3) 0.035(4) -0.008(3) 0.022(4) -0.012(3) C4 0.049(5) 0.056(5) 0.050(5) -0.013(4) 0.042(5) -0.020(4) C5 0.054(5) 0.053(5) 0.035(5) 0.000(4) 0.029(4) -0.028(4) C6 0.044(5) 0.027(3) 0.056(5) 0.000(4) 0.035(4) -0.012(3) C7 0.030(4) 0.027(3) 0.039(4) 0.003(3) 0.023(4) -0.004(3) C8 0.035(4) 0.019(3) 0.024(4) -0.001(3) 0.018(3) -0.007(3) C9 0.031(4) 0.051(4) 0.027(4) -0.004(4) 0.015(4) -0.013(3) C10 0.037(5) 0.069(5) 0.040(5) -0.005(5) 0.015(4) -0.029(4) C11 0.078(7) 0.041(4) 0.025(4) -0.008(4) 0.027(5) -0.030(4) C12 0.079(6) 0.033(4) 0.042(5) -0.004(4) 0.045(5) -0.007(4) C13 0.042(4) 0.029(3) 0.029(4) 0.007(3) 0.025(4) 0.003(3) N1 0.018(3) 0.023(2) 0.027(3) 0.004(2) 0.016(2) 0.005(2) Si1 0.0268(10) 0.0150(8) 0.0307(11) 0.0051(8) 0.0193(9) 0.0041(7) C26 0.048(4) 0.019(3) 0.043(5) 0.008(3) 0.032(4) 0.011(3) C27 0.038(4) 0.026(3) 0.034(4) 0.009(3) 0.023(4) 0.004(3) C28 0.033(4) 0.028(3) 0.043(5) 0.014(3) 0.027(4) 0.011(3) P2 0.0142(8) 0.0177(7) 0.0213(9) 0.0012(7) 0.0120(7) 0.0020(6) C14 0.009(3) 0.017(3) 0.023(4) 0.004(3) 0.006(3) -0.006(2) C15 0.026(4) 0.027(3) 0.030(4) 0.003(3) 0.020(3) -0.001(3) C16 0.038(4) 0.042(4) 0.025(4) 0.001(3) 0.022(4) -0.006(3) C17 0.029(4) 0.042(4) 0.023(4) 0.007(3) 0.011(3) -0.012(3) C18 0.022(4) 0.029(3) 0.036(5) 0.006(3) 0.011(4) -0.001(3) C19 0.025(4) 0.027(3) 0.037(4) -0.005(3) 0.021(4) -0.002(3) C20 0.024(3) 0.023(3) 0.032(4) 0.008(3) 0.024(3) 0.006(3) C21 0.030(4) 0.036(4) 0.038(4) -0.011(3) 0.024(4) -0.004(3) C22 0.047(5) 0.058(5) 0.066(6) -0.007(5) 0.050(5) -0.006(4) C23 0.060(5) 0.059(5) 0.059(6) -0.001(4) 0.053(5) 0.006(4) C24 0.044(5) 0.054(4) 0.036(5) -0.007(4) 0.028(4) -0.010(4) C25 0.035(4) 0.032(3) 0.032(4) 0.000(3) 0.026(4) 0.001(3) N2 0.018(3) 0.022(2) 0.018(3) 0.000(2) 0.011(2) 0.003(2) Si2 0.0211(9) 0.0154(7) 0.0211(10) 0.0023(7) 0.0140(8) 0.0025(7) C29 0.043(4) 0.020(3) 0.035(4) 0.008(3) 0.023(4) 0.005(3) C30 0.028(4) 0.015(3) 0.030(4) -0.001(3) 0.018(3) 0.000(3) C31 0.028(4) 0.026(3) 0.046(5) -0.002(3) 0.022(4) -0.001(3) C32 0.013(3) 0.017(3) 0.018(3) 0.002(3) 0.008(3) 0.004(2) P3 0.0180(8) 0.0183(7) 0.0171(9) 0.0002(7) 0.0120(7) 0.0007(6) C33 0.025(3) 0.020(3) 0.016(3) -0.001(3) 0.014(3) 0.001(3) C34 0.043(4) 0.030(4) 0.033(4) -0.007(3) 0.028(4) -0.007(3) C35 0.074(6) 0.021(3) 0.042(5) -0.013(3) 0.039(5) -0.010(4) C36 0.080(6) 0.025(4) 0.044(5) -0.001(4) 0.043(5) 0.015(4) C37 0.049(5) 0.048(4) 0.034(5) 0.004(4) 0.030(4) 0.017(4) C38 0.040(4) 0.024(3) 0.027(4) 0.002(3) 0.026(4) 0.005(3) C39 0.021(3) 0.029(3) 0.022(4) 0.007(3) 0.015(3) -0.001(3) C40 0.033(4) 0.048(4) 0.027(4) -0.001(4) 0.015(4) -0.006(3) C41 0.035(5) 0.082(6) 0.022(4) -0.006(4) 0.010(4) -0.013(4) C42 0.028(4) 0.095(7) 0.035(5) 0.021(5) 0.018(4) 0.008(5) C43 0.034(4) 0.056(5) 0.056(6) 0.027(4) 0.034(4) 0.020(4) C44 0.027(4) 0.036(4) 0.031(4) 0.005(3) 0.018(3) 0.002(3) N3 0.025(3) 0.017(2) 0.023(3) 0.004(2) 0.018(3) 0.003(2) Si3 0.0236(9) 0.0257(8) 0.0213(10) 0.0049(8) 0.0164(8) 0.0003(7) C57 0.031(4) 0.038(4) 0.032(4) 0.013(3) 0.018(4) -0.002(3) C58 0.047(5) 0.055(4) 0.034(4) -0.003(4) 0.032(4) -0.008(4) C59 0.037(4) 0.046(4) 0.044(5) 0.029(4) 0.027(4) 0.017(3) P4 0.0167(8) 0.0159(7) 0.0199(9) 0.0010(7) 0.0132(7) 0.0013(6) C45 0.022(3) 0.015(3) 0.022(3) -0.002(3) 0.017(3) -0.003(3) C46 0.018(3) 0.028(3) 0.036(4) -0.007(3) 0.016(3) -0.005(3) C47 0.038(4) 0.021(3) 0.060(5) 0.002(3) 0.032(4) 0.010(3) C48 0.019(4) 0.034(4) 0.048(5) 0.002(4) 0.018(4) 0.002(3) C49 0.020(3) 0.037(4) 0.030(4) 0.001(3) 0.008(3) 0.001(3) C50 0.030(4) 0.026(3) 0.034(4) 0.001(3) 0.021(4) 0.004(3) C51 0.022(3) 0.016(3) 0.019(3) -0.001(3) 0.015(3) -0.002(2) C52 0.031(4) 0.029(3) 0.034(4) 0.011(3) 0.026(4) 0.008(3) C53 0.044(4) 0.032(4) 0.033(4) 0.014(3) 0.028(4) 0.021(3) C54 0.040(4) 0.025(3) 0.021(4) -0.001(3) 0.022(3) -0.008(3) C55 0.024(3) 0.037(4) 0.026(4) 0.000(3) 0.018(3) -0.008(3) C56 0.019(3) 0.029(3) 0.020(4) 0.004(3) 0.012(3) -0.004(3) N4 0.019(2) 0.018(2) 0.025(3) 0.001(2) 0.018(2) 0.001(2) Si4 0.0244(9) 0.0243(8) 0.0245(10) -0.0055(8) 0.0192(9) -0.0046(7) C60 0.055(5) 0.050(4) 0.043(5) -0.020(4) 0.040(4) -0.025(4) C61 0.032(4) 0.032(3) 0.031(4) -0.010(3) 0.018(4) 0.005(3) C62 0.028(4) 0.032(4) 0.025(4) -0.001(3) 0.011(3) 0.002(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 Pr1 C1 2.458(5) . ? Pr1 N3 2.492(5) . ? Pr1 N4 2.504(4) . ? Pr1 N2 2.521(4) . ? Pr1 N1 2.552(4) . ? Pr1 C32 2.999(5) . ? C1 P1 1.642(6) . ? C1 P2 1.642(6) . ? P1 N1 1.620(5) . ? P1 C2 1.819(6) . ? P1 C8 1.830(6) . ? C2 C3 1.381(8) . ? C2 C7 1.389(8) . ? C3 C4 1.404(8) . ? C3 H3A 0.9500 . ? C4 C5 1.371(10) . ? C4 H4A 0.9500 . ? C5 C6 1.369(10) . ? C5 H5A 0.9500 . ? C6 C7 1.379(9) . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? C8 C13 1.373(9) . ? C8 C9 1.393(9) . ? C9 C10 1.380(10) . ? C9 H9A 0.9500 . ? C10 C11 1.360(11) . ? C10 H10A 0.9500 . ? C11 C12 1.376(11) . ? C11 H11A 0.9500 . ? C12 C13 1.381(9) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? N1 Si1 1.708(5) . ? Si1 C26 1.872(6) . ? Si1 C28 1.873(6) . ? Si1 C27 1.889(6) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? P2 N2 1.628(5) . ? P2 C20 1.831(6) . ? P2 C14 1.836(6) . ? C14 C15 1.388(8) . ? C14 C19 1.393(8) . ? C15 C16 1.382(9) . ? C15 H15A 0.9500 . ? C16 C17 1.365(9) . ? C16 H16A 0.9500 . ? C17 C18 1.390(9) . ? C17 H17A 0.9500 . ? C18 C19 1.366(9) . ? C18 H18A 0.9500 . ? C19 H19A 0.9500 . ? C20 C25 1.359(8) . ? C20 C21 1.411(8) . ? C21 C22 1.386(9) . ? C21 H21A 0.9500 . ? C22 C23 1.361(10) . ? C22 H22A 0.9500 . ? C23 C24 1.392(10) . ? C23 H23A 0.9500 . ? C24 C25 1.388(9) . ? C24 H24A 0.9500 . ? C25 H25A 0.9500 . ? N2 Si2 1.727(5) . ? Si2 C29 1.857(7) . ? Si2 C30 1.866(6) . ? Si2 C31 1.874(6) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 P3 1.715(6) . ? C32 P4 1.748(6) . ? C32 H32A 1.0000 . ? P3 N3 1.603(5) . ? P3 C33 1.819(6) . ? P3 C39 1.826(6) . ? C33 C38 1.383(8) . ? C33 C34 1.392(8) . ? C34 C35 1.385(9) . ? C34 H34A 0.9500 . ? C35 C36 1.388(10) . ? C35 H35A 0.9500 . ? C36 C37 1.370(10) . ? C36 H36A 0.9500 . ? C37 C38 1.382(8) . ? C37 H37A 0.9500 . ? C38 H38A 0.9500 . ? C39 C40 1.383(9) . ? C39 C44 1.397(8) . ? C40 C41 1.384(10) . ? C40 H40A 0.9500 . ? C41 C42 1.377(11) . ? C41 H41A 0.9500 . ? C42 C43 1.370(11) . ? C42 H42A 0.9500 . ? C43 C44 1.399(9) . ? C43 H43A 0.9500 . ? C44 H44A 0.9500 . ? N3 Si3 1.742(5) . ? Si3 C57 1.863(6) . ? Si3 C59 1.868(6) . ? Si3 C58 1.873(7) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? P4 N4 1.605(5) . ? P4 C45 1.811(6) . ? P4 C51 1.826(6) . ? C45 C46 1.375(7) . ? C45 C50 1.388(8) . ? C46 C47 1.409(8) . ? C46 H46A 0.9500 . ? C47 C48 1.366(9) . ? C47 H47A 0.9500 . ? C48 C49 1.379(9) . ? C48 H48A 0.9500 . ? C49 C50 1.381(8) . ? C49 H49A 0.9500 . ? C50 H50A 0.9500 . ? C51 C52 1.379(8) . ? C51 C56 1.400(8) . ? C52 C53 1.387(8) . ? C52 H52A 0.9500 . ? C53 C54 1.367(9) . ? C53 H53A 0.9500 . ? C54 C55 1.368(9) . ? C54 H54A 0.9500 . ? C55 C56 1.386(8) . ? C55 H55A 0.9500 . ? C56 H56A 0.9500 . ? N4 Si4 1.725(5) . ? Si4 C62 1.842(6) . ? Si4 C61 1.863(6) . ? Si4 C60 1.863(6) . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 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 C1 Pr1 N3 118.13(18) . . ? C1 Pr1 N4 132.70(18) . . ? N3 Pr1 N4 107.48(15) . . ? C1 Pr1 N2 63.78(16) . . ? N3 Pr1 N2 107.09(15) . . ? N4 Pr1 N2 114.94(15) . . ? C1 Pr1 N1 62.79(16) . . ? N3 Pr1 N1 105.18(15) . . ? N4 Pr1 N1 94.81(14) . . ? N2 Pr1 N1 125.77(14) . . ? C1 Pr1 C32 159.43(17) . . ? N3 Pr1 C32 59.27(15) . . ? N4 Pr1 C32 59.58(15) . . ? N2 Pr1 C32 96.66(15) . . ? N1 Pr1 C32 137.42(14) . . ? P1 C1 P2 163.7(4) . . ? P1 C1 Pr1 96.8(3) . . ? P2 C1 Pr1 95.5(2) . . ? N1 P1 C1 106.3(3) . . ? N1 P1 C2 111.8(3) . . ? C1 P1 C2 115.3(3) . . ? N1 P1 C8 111.4(3) . . ? C1 P1 C8 113.0(3) . . ? C2 P1 C8 99.0(3) . . ? C3 C2 C7 118.7(6) . . ? C3 C2 P1 120.7(4) . . ? C7 C2 P1 120.6(5) . . ? C2 C3 C4 119.5(6) . . ? C2 C3 H3A 120.2 . . ? C4 C3 H3A 120.2 . . ? C5 C4 C3 120.3(7) . . ? C5 C4 H4A 119.8 . . ? C3 C4 H4A 119.8 . . ? C6 C5 C4 120.5(6) . . ? C6 C5 H5A 119.8 . . ? C4 C5 H5A 119.8 . . ? C5 C6 C7 119.4(6) . . ? C5 C6 H6A 120.3 . . ? C7 C6 H6A 120.3 . . ? C6 C7 C2 121.5(7) . . ? C6 C7 H7A 119.2 . . ? C2 C7 H7A 119.2 . . ? C13 C8 C9 117.8(6) . . ? C13 C8 P1 124.0(5) . . ? C9 C8 P1 118.2(5) . . ? C10 C9 C8 120.4(7) . . ? C10 C9 H9A 119.8 . . ? C8 C9 H9A 119.8 . . ? C11 C10 C9 120.8(8) . . ? C11 C10 H10A 119.6 . . ? C9 C10 H10A 119.6 . . ? C10 C11 C12 119.7(7) . . ? C10 C11 H11A 120.1 . . ? C12 C11 H11A 120.1 . . ? C11 C12 C13 119.5(7) . . ? C11 C12 H12A 120.2 . . ? C13 C12 H12A 120.2 . . ? C8 C13 C12 121.7(7) . . ? C8 C13 H13A 119.1 . . ? C12 C13 H13A 119.1 . . ? P1 N1 Si1 135.8(3) . . ? P1 N1 Pr1 93.8(2) . . ? Si1 N1 Pr1 126.6(2) . . ? N1 Si1 C26 113.4(3) . . ? N1 Si1 C28 106.7(3) . . ? C26 Si1 C28 108.1(3) . . ? N1 Si1 C27 115.4(3) . . ? C26 Si1 C27 106.3(3) . . ? C28 Si1 C27 106.5(3) . . ? Si1 C26 H26A 109.5 . . ? Si1 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si1 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si1 C27 H27A 109.5 . . ? Si1 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si1 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si1 C28 H28A 109.5 . . ? Si1 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si1 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N2 P2 C1 107.1(3) . . ? N2 P2 C20 109.3(3) . . ? C1 P2 C20 110.7(3) . . ? N2 P2 C14 112.5(2) . . ? C1 P2 C14 113.7(3) . . ? C20 P2 C14 103.5(3) . . ? C15 C14 C19 118.5(6) . . ? C15 C14 P2 117.6(4) . . ? C19 C14 P2 123.9(5) . . ? C16 C15 C14 120.6(6) . . ? C16 C15 H15A 119.7 . . ? C14 C15 H15A 119.7 . . ? C17 C16 C15 120.8(7) . . ? C17 C16 H16A 119.6 . . ? C15 C16 H16A 119.6 . . ? C16 C17 C18 118.7(6) . . ? C16 C17 H17A 120.6 . . ? C18 C17 H17A 120.6 . . ? C19 C18 C17 121.3(6) . . ? C19 C18 H18A 119.4 . . ? C17 C18 H18A 119.4 . . ? C18 C19 C14 120.1(6) . . ? C18 C19 H19A 119.9 . . ? C14 C19 H19A 119.9 . . ? C25 C20 C21 118.6(6) . . ? C25 C20 P2 121.6(5) . . ? C21 C20 P2 119.3(5) . . ? C22 C21 C20 119.2(6) . . ? C22 C21 H21A 120.4 . . ? C20 C21 H21A 120.4 . . ? C23 C22 C21 121.4(7) . . ? C23 C22 H22A 119.3 . . ? C21 C22 H22A 119.3 . . ? C22 C23 C24 119.7(7) . . ? C22 C23 H23A 120.1 . . ? C24 C23 H23A 120.1 . . ? C25 C24 C23 118.9(7) . . ? C25 C24 H24A 120.5 . . ? C23 C24 H24A 120.5 . . ? C20 C25 C24 122.1(6) . . ? C20 C25 H25A 118.9 . . ? C24 C25 H25A 118.9 . . ? P2 N2 Si2 126.1(3) . . ? P2 N2 Pr1 93.52(19) . . ? Si2 N2 Pr1 138.7(2) . . ? N2 Si2 C29 111.4(3) . . ? N2 Si2 C30 111.1(2) . . ? C29 Si2 C30 107.0(3) . . ? N2 Si2 C31 115.0(3) . . ? C29 Si2 C31 107.0(3) . . ? C30 Si2 C31 104.8(3) . . ? Si2 C29 H29A 109.5 . . ? Si2 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? Si2 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 . . ? P3 C32 P4 139.9(3) . . ? P3 C32 Pr1 83.4(2) . . ? P4 C32 Pr1 83.9(2) . . ? P3 C32 H32A 110.0 . . ? P4 C32 H32A 110.0 . . ? Pr1 C32 H32A 110.0 . . ? N3 P3 C32 112.0(3) . . ? N3 P3 C33 111.5(2) . . ? C32 P3 C33 102.5(3) . . ? N3 P3 C39 109.0(3) . . ? C32 P3 C39 115.7(3) . . ? C33 P3 C39 105.9(3) . . ? C38 C33 C34 118.9(5) . . ? C38 C33 P3 118.8(4) . . ? C34 C33 P3 122.2(5) . . ? C35 C34 C33 120.2(6) . . ? C35 C34 H34A 119.9 . . ? C33 C34 H34A 119.9 . . ? C34 C35 C36 120.1(6) . . ? C34 C35 H35A 120.0 . . ? C36 C35 H35A 120.0 . . ? C37 C36 C35 119.7(6) . . ? C37 C36 H36A 120.1 . . ? C35 C36 H36A 120.1 . . ? C36 C37 C38 120.3(7) . . ? C36 C37 H37A 119.8 . . ? C38 C37 H37A 119.8 . . ? C37 C38 C33 120.7(6) . . ? C37 C38 H38A 119.6 . . ? C33 C38 H38A 119.6 . . ? C40 C39 C44 118.8(6) . . ? C40 C39 P3 123.9(5) . . ? C44 C39 P3 117.2(5) . . ? C39 C40 C41 120.7(7) . . ? C39 C40 H40A 119.7 . . ? C41 C40 H40A 119.7 . . ? C42 C41 C40 120.2(8) . . ? C42 C41 H41A 119.9 . . ? C40 C41 H41A 119.9 . . ? C43 C42 C41 120.4(7) . . ? C43 C42 H42A 119.8 . . ? C41 C42 H42A 119.8 . . ? C42 C43 C44 119.7(7) . . ? C42 C43 H43A 120.1 . . ? C44 C43 H43A 120.1 . . ? C39 C44 C43 120.2(7) . . ? C39 C44 H44A 119.9 . . ? C43 C44 H44A 119.9 . . ? P3 N3 Si3 126.9(3) . . ? P3 N3 Pr1 104.3(2) . . ? Si3 N3 Pr1 128.7(2) . . ? N3 Si3 C57 106.5(3) . . ? N3 Si3 C59 112.1(3) . . ? C57 Si3 C59 110.7(3) . . ? N3 Si3 C58 115.7(3) . . ? C57 Si3 C58 106.5(3) . . ? C59 Si3 C58 105.3(3) . . ? Si3 C57 H57A 109.5 . . ? Si3 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? Si3 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? Si3 C58 H58A 109.5 . . ? Si3 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? Si3 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? Si3 C59 H59A 109.5 . . ? Si3 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? Si3 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? N4 P4 C32 111.2(2) . . ? N4 P4 C45 111.8(2) . . ? C32 P4 C45 114.3(3) . . ? N4 P4 C51 110.6(3) . . ? C32 P4 C51 104.6(3) . . ? C45 P4 C51 103.9(2) . . ? C46 C45 C50 119.4(5) . . ? C46 C45 P4 120.3(4) . . ? C50 C45 P4 120.2(4) . . ? C45 C46 C47 119.9(6) . . ? C45 C46 H46A 120.0 . . ? C47 C46 H46A 120.0 . . ? C48 C47 C46 120.0(6) . . ? C48 C47 H47A 120.0 . . ? C46 C47 H47A 120.0 . . ? C47 C48 C49 119.9(6) . . ? C47 C48 H48A 120.0 . . ? C49 C48 H48A 120.0 . . ? C48 C49 C50 120.4(6) . . ? C48 C49 H49A 119.8 . . ? C50 C49 H49A 119.8 . . ? C49 C50 C45 120.3(6) . . ? C49 C50 H50A 119.9 . . ? C45 C50 H50A 119.9 . . ? C52 C51 C56 118.6(5) . . ? C52 C51 P4 118.1(4) . . ? C56 C51 P4 123.1(4) . . ? C51 C52 C53 120.3(6) . . ? C51 C52 H52A 119.9 . . ? C53 C52 H52A 119.9 . . ? C54 C53 C52 120.4(6) . . ? C54 C53 H53A 119.8 . . ? C52 C53 H53A 119.8 . . ? C53 C54 C55 120.4(6) . . ? C53 C54 H54A 119.8 . . ? C55 C54 H54A 119.8 . . ? C54 C55 C56 119.8(6) . . ? C54 C55 H55A 120.1 . . ? C56 C55 H55A 120.1 . . ? C55 C56 C51 120.5(6) . . ? C55 C56 H56A 119.8 . . ? C51 C56 H56A 119.8 . . ? P4 N4 Si4 131.5(3) . . ? P4 N4 Pr1 105.1(2) . . ? Si4 N4 Pr1 120.0(2) . . ? N4 Si4 C62 105.3(3) . . ? N4 Si4 C61 111.4(3) . . ? C62 Si4 C61 107.9(3) . . ? N4 Si4 C60 116.2(3) . . ? C62 Si4 C60 108.0(3) . . ? C61 Si4 C60 107.7(3) . . ? Si4 C60 H60A 109.5 . . ? Si4 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? Si4 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? Si4 C61 H61A 109.5 . . ? Si4 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? Si4 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? Si4 C62 H62A 109.5 . . ? Si4 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? Si4 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 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 N3 Pr1 C1 P1 -96.6(3) . . . . ? N4 Pr1 C1 P1 66.5(3) . . . . ? N2 Pr1 C1 P1 167.2(3) . . . . ? N1 Pr1 C1 P1 -3.3(2) . . . . ? C32 Pr1 C1 P1 -173.7(3) . . . . ? N3 Pr1 C1 P2 94.1(3) . . . . ? N4 Pr1 C1 P2 -102.8(3) . . . . ? N2 Pr1 C1 P2 -2.1(2) . . . . ? N1 Pr1 C1 P2 -172.5(3) . . . . ? C32 Pr1 C1 P2 17.1(7) . . . . ? P2 C1 P1 N1 143.4(14) . . . . ? Pr1 C1 P1 N1 4.8(3) . . . . ? P2 C1 P1 C2 -92.0(15) . . . . ? Pr1 C1 P1 C2 129.3(3) . . . . ? P2 C1 P1 C8 20.9(15) . . . . ? Pr1 C1 P1 C8 -117.8(3) . . . . ? N1 P1 C2 C3 111.7(5) . . . . ? C1 P1 C2 C3 -10.0(6) . . . . ? C8 P1 C2 C3 -130.9(5) . . . . ? N1 P1 C2 C7 -68.0(6) . . . . ? C1 P1 C2 C7 170.3(5) . . . . ? C8 P1 C2 C7 49.5(6) . . . . ? C7 C2 C3 C4 0.9(9) . . . . ? P1 C2 C3 C4 -178.7(5) . . . . ? C2 C3 C4 C5 0.6(11) . . . . ? C3 C4 C5 C6 -1.9(12) . . . . ? C4 C5 C6 C7 1.6(11) . . . . ? C5 C6 C7 C2 0.0(11) . . . . ? C3 C2 C7 C6 -1.3(10) . . . . ? P1 C2 C7 C6 178.4(5) . . . . ? N1 P1 C8 C13 -4.4(6) . . . . ? C1 P1 C8 C13 115.2(5) . . . . ? C2 P1 C8 C13 -122.3(5) . . . . ? N1 P1 C8 C9 176.8(5) . . . . ? C1 P1 C8 C9 -63.5(6) . . . . ? C2 P1 C8 C9 59.0(5) . . . . ? C13 C8 C9 C10 0.5(10) . . . . ? P1 C8 C9 C10 179.3(5) . . . . ? C8 C9 C10 C11 -0.4(11) . . . . ? C9 C10 C11 C12 0.4(12) . . . . ? C10 C11 C12 C13 -0.4(11) . . . . ? C9 C8 C13 C12 -0.5(9) . . . . ? P1 C8 C13 C12 -179.3(5) . . . . ? C11 C12 C13 C8 0.5(10) . . . . ? C1 P1 N1 Si1 153.0(4) . . . . ? C2 P1 N1 Si1 26.3(5) . . . . ? C8 P1 N1 Si1 -83.5(5) . . . . ? C1 P1 N1 Pr1 -4.6(3) . . . . ? C2 P1 N1 Pr1 -131.3(2) . . . . ? C8 P1 N1 Pr1 119.0(2) . . . . ? C1 Pr1 N1 P1 3.3(2) . . . . ? N3 Pr1 N1 P1 117.5(2) . . . . ? N4 Pr1 N1 P1 -132.9(2) . . . . ? N2 Pr1 N1 P1 -7.3(3) . . . . ? C32 Pr1 N1 P1 178.31(18) . . . . ? C1 Pr1 N1 Si1 -157.3(4) . . . . ? N3 Pr1 N1 Si1 -43.1(3) . . . . ? N4 Pr1 N1 Si1 66.4(3) . . . . ? N2 Pr1 N1 Si1 -168.0(3) . . . . ? C32 Pr1 N1 Si1 17.7(4) . . . . ? P1 N1 Si1 C26 73.3(5) . . . . ? Pr1 N1 Si1 C26 -135.1(3) . . . . ? P1 N1 Si1 C28 -167.8(4) . . . . ? Pr1 N1 Si1 C28 -16.1(4) . . . . ? P1 N1 Si1 C27 -49.7(6) . . . . ? Pr1 N1 Si1 C27 101.9(3) . . . . ? P1 C1 P2 N2 -135.7(14) . . . . ? Pr1 C1 P2 N2 3.1(3) . . . . ? P1 C1 P2 C20 105.2(15) . . . . ? Pr1 C1 P2 C20 -116.0(3) . . . . ? P1 C1 P2 C14 -10.7(16) . . . . ? Pr1 C1 P2 C14 128.0(2) . . . . ? N2 P2 C14 C15 85.6(5) . . . . ? C1 P2 C14 C15 -36.3(5) . . . . ? C20 P2 C14 C15 -156.4(4) . . . . ? N2 P2 C14 C19 -91.3(5) . . . . ? C1 P2 C14 C19 146.7(5) . . . . ? C20 P2 C14 C19 26.6(5) . . . . ? C19 C14 C15 C16 0.2(8) . . . . ? P2 C14 C15 C16 -176.9(5) . . . . ? C14 C15 C16 C17 0.1(9) . . . . ? C15 C16 C17 C18 -0.5(9) . . . . ? C16 C17 C18 C19 0.6(9) . . . . ? C17 C18 C19 C14 -0.2(9) . . . . ? C15 C14 C19 C18 -0.2(8) . . . . ? P2 C14 C19 C18 176.8(5) . . . . ? N2 P2 C20 C25 -15.5(6) . . . . ? C1 P2 C20 C25 102.3(5) . . . . ? C14 P2 C20 C25 -135.6(5) . . . . ? N2 P2 C20 C21 173.0(5) . . . . ? C1 P2 C20 C21 -69.3(6) . . . . ? C14 P2 C20 C21 52.8(5) . . . . ? C25 C20 C21 C22 1.7(9) . . . . ? P2 C20 C21 C22 173.5(5) . . . . ? C20 C21 C22 C23 -1.0(11) . . . . ? C21 C22 C23 C24 0.4(12) . . . . ? C22 C23 C24 C25 -0.4(11) . . . . ? C21 C20 C25 C24 -1.8(10) . . . . ? P2 C20 C25 C24 -173.4(5) . . . . ? C23 C24 C25 C20 1.1(11) . . . . ? C1 P2 N2 Si2 164.5(4) . . . . ? C20 P2 N2 Si2 -75.5(4) . . . . ? C14 P2 N2 Si2 38.9(4) . . . . ? C1 P2 N2 Pr1 -3.0(3) . . . . ? C20 P2 N2 Pr1 116.9(2) . . . . ? C14 P2 N2 Pr1 -128.6(2) . . . . ? C1 Pr1 N2 P2 2.1(2) . . . . ? N3 Pr1 N2 P2 -111.3(2) . . . . ? N4 Pr1 N2 P2 129.34(19) . . . . ? N1 Pr1 N2 P2 12.7(3) . . . . ? C32 Pr1 N2 P2 -171.2(2) . . . . ? C1 Pr1 N2 Si2 -162.5(5) . . . . ? N3 Pr1 N2 Si2 84.0(4) . . . . ? N4 Pr1 N2 Si2 -35.3(4) . . . . ? N1 Pr1 N2 Si2 -152.0(3) . . . . ? C32 Pr1 N2 Si2 24.2(4) . . . . ? P2 N2 Si2 C29 -80.0(4) . . . . ? Pr1 N2 Si2 C29 80.9(4) . . . . ? P2 N2 Si2 C30 160.7(3) . . . . ? Pr1 N2 Si2 C30 -38.3(5) . . . . ? P2 N2 Si2 C31 41.9(5) . . . . ? Pr1 N2 Si2 C31 -157.1(4) . . . . ? C1 Pr1 C32 P3 82.7(5) . . . . ? N3 Pr1 C32 P3 -6.00(16) . . . . ? N4 Pr1 C32 P3 -145.0(2) . . . . ? N2 Pr1 C32 P3 100.0(2) . . . . ? N1 Pr1 C32 P3 -84.7(3) . . . . ? C1 Pr1 C32 P4 -135.4(5) . . . . ? N3 Pr1 C32 P4 135.9(2) . . . . ? N4 Pr1 C32 P4 -3.05(17) . . . . ? N2 Pr1 C32 P4 -118.1(2) . . . . ? N1 Pr1 C32 P4 57.3(3) . . . . ? P4 C32 P3 N3 -63.7(6) . . . . ? Pr1 C32 P3 N3 8.7(2) . . . . ? P4 C32 P3 C33 176.7(5) . . . . ? Pr1 C32 P3 C33 -111.0(2) . . . . ? P4 C32 P3 C39 62.0(6) . . . . ? Pr1 C32 P3 C39 134.3(2) . . . . ? N3 P3 C33 C38 -9.0(6) . . . . ? C32 P3 C33 C38 111.0(5) . . . . ? C39 P3 C33 C38 -127.4(5) . . . . ? N3 P3 C33 C34 175.5(5) . . . . ? C32 P3 C33 C34 -64.6(6) . . . . ? C39 P3 C33 C34 57.1(6) . . . . ? C38 C33 C34 C35 0.1(10) . . . . ? P3 C33 C34 C35 175.7(5) . . . . ? C33 C34 C35 C36 0.8(11) . . . . ? C34 C35 C36 C37 -0.8(11) . . . . ? C35 C36 C37 C38 -0.1(11) . . . . ? C36 C37 C38 C33 1.0(10) . . . . ? C34 C33 C38 C37 -1.0(9) . . . . ? P3 C33 C38 C37 -176.7(5) . . . . ? N3 P3 C39 C40 -109.9(5) . . . . ? C32 P3 C39 C40 122.9(5) . . . . ? C33 P3 C39 C40 10.1(6) . . . . ? N3 P3 C39 C44 64.5(5) . . . . ? C32 P3 C39 C44 -62.6(5) . . . . ? C33 P3 C39 C44 -175.4(4) . . . . ? C44 C39 C40 C41 0.1(10) . . . . ? P3 C39 C40 C41 174.5(5) . . . . ? C39 C40 C41 C42 -0.7(11) . . . . ? C40 C41 C42 C43 1.3(12) . . . . ? C41 C42 C43 C44 -1.3(11) . . . . ? C40 C39 C44 C43 -0.1(9) . . . . ? P3 C39 C44 C43 -174.8(5) . . . . ? C42 C43 C44 C39 0.7(10) . . . . ? C32 P3 N3 Si3 172.4(3) . . . . ? C33 P3 N3 Si3 -73.3(4) . . . . ? C39 P3 N3 Si3 43.2(4) . . . . ? C32 P3 N3 Pr1 -10.7(3) . . . . ? C33 P3 N3 Pr1 103.5(3) . . . . ? C39 P3 N3 Pr1 -140.0(2) . . . . ? C1 Pr1 N3 P3 -149.9(2) . . . . ? N4 Pr1 N3 P3 43.0(2) . . . . ? N2 Pr1 N3 P3 -81.0(2) . . . . ? N1 Pr1 N3 P3 143.2(2) . . . . ? C32 Pr1 N3 P3 6.58(18) . . . . ? C1 Pr1 N3 Si3 26.9(3) . . . . ? N4 Pr1 N3 Si3 -140.2(3) . . . . ? N2 Pr1 N3 Si3 95.8(3) . . . . ? N1 Pr1 N3 Si3 -40.0(3) . . . . ? C32 Pr1 N3 Si3 -176.6(3) . . . . ? P3 N3 Si3 C57 157.6(3) . . . . ? Pr1 N3 Si3 C57 -18.5(4) . . . . ? P3 N3 Si3 C59 -81.2(4) . . . . ? Pr1 N3 Si3 C59 102.7(4) . . . . ? P3 N3 Si3 C58 39.5(5) . . . . ? Pr1 N3 Si3 C58 -136.6(3) . . . . ? P3 C32 P4 N4 76.6(5) . . . . ? Pr1 C32 P4 N4 4.4(2) . . . . ? P3 C32 P4 C45 -51.2(6) . . . . ? Pr1 C32 P4 C45 -123.3(2) . . . . ? P3 C32 P4 C51 -164.1(5) . . . . ? Pr1 C32 P4 C51 123.8(2) . . . . ? N4 P4 C45 C46 11.4(6) . . . . ? C32 P4 C45 C46 138.8(5) . . . . ? C51 P4 C45 C46 -107.9(5) . . . . ? N4 P4 C45 C50 -173.0(5) . . . . ? C32 P4 C45 C50 -45.6(6) . . . . ? C51 P4 C45 C50 67.7(5) . . . . ? C50 C45 C46 C47 -0.4(9) . . . . ? P4 C45 C46 C47 175.3(5) . . . . ? C45 C46 C47 C48 -0.3(10) . . . . ? C46 C47 C48 C49 0.0(11) . . . . ? C47 C48 C49 C50 1.1(11) . . . . ? C48 C49 C50 C45 -1.9(10) . . . . ? C46 C45 C50 C49 1.5(9) . . . . ? P4 C45 C50 C49 -174.2(5) . . . . ? N4 P4 C51 C52 62.4(5) . . . . ? C32 P4 C51 C52 -57.4(5) . . . . ? C45 P4 C51 C52 -177.5(5) . . . . ? N4 P4 C51 C56 -112.3(5) . . . . ? C32 P4 C51 C56 127.9(5) . . . . ? C45 P4 C51 C56 7.8(6) . . . . ? C56 C51 C52 C53 -2.8(9) . . . . ? P4 C51 C52 C53 -177.7(5) . . . . ? C51 C52 C53 C54 2.6(10) . . . . ? C52 C53 C54 C55 -0.3(10) . . . . ? C53 C54 C55 C56 -1.8(10) . . . . ? C54 C55 C56 C51 1.6(9) . . . . ? C52 C51 C56 C55 0.7(9) . . . . ? P4 C51 C56 C55 175.3(5) . . . . ? C32 P4 N4 Si4 153.0(3) . . . . ? C45 P4 N4 Si4 -77.9(4) . . . . ? C51 P4 N4 Si4 37.3(4) . . . . ? C32 P4 N4 Pr1 -5.4(3) . . . . ? C45 P4 N4 Pr1 123.6(2) . . . . ? C51 P4 N4 Pr1 -121.1(2) . . . . ? C1 Pr1 N4 P4 162.7(2) . . . . ? N3 Pr1 N4 P4 -32.9(2) . . . . ? N2 Pr1 N4 P4 86.2(2) . . . . ? N1 Pr1 N4 P4 -140.4(2) . . . . ? C32 Pr1 N4 P4 3.42(19) . . . . ? C1 Pr1 N4 Si4 1.2(4) . . . . ? N3 Pr1 N4 Si4 165.6(2) . . . . ? N2 Pr1 N4 Si4 -75.3(3) . . . . ? N1 Pr1 N4 Si4 58.1(3) . . . . ? C32 Pr1 N4 Si4 -158.1(3) . . . . ? P4 N4 Si4 C62 -128.9(4) . . . . ? Pr1 N4 Si4 C62 27.0(3) . . . . ? P4 N4 Si4 C61 114.5(4) . . . . ? Pr1 N4 Si4 C61 -89.7(3) . . . . ? P4 N4 Si4 C60 -9.5(5) . . . . ? Pr1 N4 Si4 C60 146.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.587 _refine_diff_density_min -0.945 _refine_diff_density_rms 0.113 # Attachment '16.cif' data_16 _database_code_depnum_ccdc_archive 'CCDC 736113' _refine_special_details ; Poor data resulted in a high Rint which is largely responsible for the level A alerts. Nevertheless, the structure is clear-cut and chemically unambiguous. ; _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62 H77 N4 P4 Si4 Sm' _chemical_formula_sum 'C62 H77 N4 P4 Si4 Sm' _chemical_formula_weight 1264.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 31.20(2) _cell_length_b 25.748(16) _cell_length_c 21.026(14) _cell_angle_alpha 90.00 _cell_angle_beta 131.129(11) _cell_angle_gamma 90.00 _cell_volume 12724(14) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 473 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 24.85 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.321 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5240 _exptl_absorpt_coefficient_mu 1.139 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.90 _exptl_absorpt_correction_T_max 0.96 _exptl_absorpt_process_details '(SADABS; Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 21961 _diffrn_reflns_av_R_equivalents 0.2773 _diffrn_reflns_av_sigmaI/netI 0.2987 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 21.03 _reflns_number_total 6738 _reflns_number_gt 3006 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'enCIFer(Allen et al.,2004);PLATON(Spek,2003)' _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^)+(0.0434P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0047(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6738 _refine_ls_number_parameters 689 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1956 _refine_ls_R_factor_gt 0.0720 _refine_ls_wR_factor_ref 0.2007 _refine_ls_wR_factor_gt 0.1410 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_restrained_S_all 0.988 _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 Sm1 Sm 0.26512(5) 0.61992(4) 0.75529(6) 0.0364(5) Uani 1 1 d . . . C1 C 0.1683(7) 0.5942(6) 0.6795(10) 0.030(5) Uani 1 1 d . . . P1 P 0.1424(2) 0.65316(18) 0.6572(3) 0.0401(15) Uani 1 1 d . . . P2 P 0.1775(2) 0.53124(18) 0.6779(3) 0.0393(15) Uani 1 1 d . . . C2 C 0.1110(9) 0.6676(7) 0.7046(11) 0.039(6) Uani 1 1 d . . . C3 C 0.0638(9) 0.6437(7) 0.6819(13) 0.046(6) Uani 1 1 d . . . H3A H 0.0426 0.6212 0.6343 0.056 Uiso 1 1 calc R . . C4 C 0.0465(10) 0.6511(8) 0.7253(16) 0.062(7) Uani 1 1 d . . . H4A H 0.0129 0.6346 0.7072 0.075 Uiso 1 1 calc R . . C5 C 0.0773(11) 0.6826(8) 0.7959(14) 0.062(7) Uani 1 1 d . . . H5A H 0.0648 0.6871 0.8263 0.075 Uiso 1 1 calc R . . C6 C 0.1247(10) 0.7070(7) 0.8223(13) 0.051(6) Uani 1 1 d . . . H6A H 0.1457 0.7284 0.8712 0.062 Uiso 1 1 calc R . . C7 C 0.1425(9) 0.7006(8) 0.7770(13) 0.050(6) Uani 1 1 d . . . H7A H 0.1755 0.7182 0.7942 0.059 Uiso 1 1 calc R . . C8 C 0.0804(9) 0.6646(7) 0.5429(12) 0.044(6) Uani 1 1 d . . . C9 C 0.0799(10) 0.6364(7) 0.4857(14) 0.051(6) Uani 1 1 d . . . H9A H 0.1102 0.6131 0.5058 0.061 Uiso 1 1 calc R . . C10 C 0.0353(10) 0.6422(8) 0.3994(13) 0.047(6) Uani 1 1 d . . . H10A H 0.0347 0.6233 0.3600 0.056 Uiso 1 1 calc R . . C11 C -0.0075(9) 0.6754(8) 0.3728(14) 0.063(8) Uani 1 1 d . . . H11A H -0.0375 0.6805 0.3138 0.075 Uiso 1 1 calc R . . C12 C -0.0089(11) 0.7023(9) 0.4285(17) 0.067(7) Uani 1 1 d . . . H12A H -0.0395 0.7250 0.4086 0.081 Uiso 1 1 calc R . . C13 C 0.0358(9) 0.6950(7) 0.5144(13) 0.039(5) Uani 1 1 d . . . H13A H 0.0349 0.7118 0.5537 0.046 Uiso 1 1 calc R . . C14 C 0.1491(7) 0.4892(6) 0.7137(11) 0.026(5) Uani 1 1 d . . . C15 C 0.1331(8) 0.5092(8) 0.7548(12) 0.050(6) Uani 1 1 d . . . H15A H 0.1365 0.5455 0.7654 0.060 Uiso 1 1 calc R . . C16 C 0.1116(10) 0.4771(10) 0.7818(13) 0.074(8) Uani 1 1 d . . . H16A H 0.0972 0.4916 0.8060 0.089 Uiso 1 1 calc R . . C17 C 0.1116(10) 0.4257(10) 0.7729(14) 0.070(7) Uani 1 1 d . . . H17A H 0.0991 0.4038 0.7943 0.085 Uiso 1 1 calc R . . C18 C 0.1292(9) 0.4032(8) 0.7339(14) 0.062(7) Uani 1 1 d . . . H18A H 0.1288 0.3665 0.7284 0.075 Uiso 1 1 calc R . . C19 C 0.1474(8) 0.4351(7) 0.7033(11) 0.047(6) Uani 1 1 d . . . H19A H 0.1588 0.4205 0.6750 0.056 Uiso 1 1 calc R . . C20 C 0.1333(10) 0.5053(7) 0.5701(12) 0.043(6) Uani 1 1 d . . . C21 C 0.1607(9) 0.4847(7) 0.5399(14) 0.049(6) Uani 1 1 d . . . H21A H 0.2009 0.4834 0.5746 0.059 Uiso 1 1 calc R . . C22 C 0.1235(12) 0.4669(7) 0.4555(16) 0.056(7) Uani 1 1 d . . . H22A H 0.1397 0.4524 0.4339 0.067 Uiso 1 1 calc R . . C23 C 0.0664(13) 0.4691(9) 0.4039(16) 0.072(8) Uani 1 1 d . . . H23A H 0.0431 0.4572 0.3473 0.087 Uiso 1 1 calc R . . C24 C 0.0424(11) 0.4892(9) 0.4353(15) 0.074(9) Uani 1 1 d . . . H24A H 0.0022 0.4902 0.3997 0.089 Uiso 1 1 calc R . . C25 C 0.0747(10) 0.5077(8) 0.5157(16) 0.061(7) Uani 1 1 d . . . H25A H 0.0567 0.5223 0.5344 0.073 Uiso 1 1 calc R . . N1 N 0.1939(6) 0.6918(4) 0.6901(8) 0.027(4) Uani 1 1 d . . . Si1 Si 0.1875(2) 0.75645(18) 0.6605(3) 0.0396(16) Uani 1 1 d . . . C26 C 0.1341(8) 0.7939(7) 0.6543(13) 0.061(7) Uani 1 1 d . . . H26A H 0.0958 0.7810 0.6071 0.092 Uiso 1 1 calc R . . H26B H 0.1366 0.8307 0.6454 0.092 Uiso 1 1 calc R . . H26C H 0.1415 0.7898 0.7071 0.092 Uiso 1 1 calc R . . C27 C 0.2561(7) 0.7929(6) 0.7392(10) 0.042(5) Uani 1 1 d . . . H27A H 0.2627 0.7982 0.7912 0.063 Uiso 1 1 calc R . . H27B H 0.2537 0.8267 0.7155 0.063 Uiso 1 1 calc R . . H27C H 0.2876 0.7729 0.7518 0.063 Uiso 1 1 calc R . . C28 C 0.1674(10) 0.7610(7) 0.5547(11) 0.061(7) Uani 1 1 d . . . H28A H 0.1316 0.7424 0.5126 0.091 Uiso 1 1 calc R . . H28B H 0.1975 0.7455 0.5579 0.091 Uiso 1 1 calc R . . H28C H 0.1627 0.7976 0.5382 0.091 Uiso 1 1 calc R . . N2 N 0.2460(6) 0.5242(5) 0.7343(8) 0.041(5) Uani 1 1 d . . . Si2 Si 0.2919(2) 0.47364(19) 0.7885(3) 0.0441(17) Uani 1 1 d . . . C29 C 0.3652(9) 0.5025(8) 0.8509(13) 0.070(7) Uani 1 1 d . . . H29A H 0.3734 0.5077 0.8136 0.105 Uiso 1 1 calc R . . H29B H 0.3934 0.4788 0.8968 0.105 Uiso 1 1 calc R . . H29C H 0.3668 0.5360 0.8746 0.105 Uiso 1 1 calc R . . C30 C 0.2909(9) 0.4414(7) 0.8693(12) 0.059(7) Uani 1 1 d . . . H30A H 0.2601 0.4158 0.8409 0.089 Uiso 1 1 calc R . . H30B H 0.2846 0.4679 0.8960 0.089 Uiso 1 1 calc R . . H30C H 0.3274 0.4241 0.9125 0.089 Uiso 1 1 calc R . . C31 C 0.2844(8) 0.4185(7) 0.7226(11) 0.052(6) Uani 1 1 d . . . H31A H 0.2928 0.4311 0.6879 0.078 Uiso 1 1 calc R . . H31B H 0.2454 0.4051 0.6859 0.078 Uiso 1 1 calc R . . H31C H 0.3110 0.3907 0.7598 0.078 Uiso 1 1 calc R . . C32 C 0.3649(7) 0.6885(7) 0.8422(11) 0.039(5) Uani 1 1 d . . . H32A H 0.3530 0.7254 0.8238 0.046 Uiso 1 1 calc R . . P3 P 0.3751(2) 0.65653(18) 0.7791(3) 0.0392(15) Uani 1 1 d . . . P4 P 0.3721(2) 0.67493(18) 0.9291(3) 0.0369(15) Uani 1 1 d . . . C33 C 0.3782(10) 0.7100(7) 0.7247(12) 0.039(5) Uani 1 1 d . . . C34 C 0.3298(9) 0.7421(8) 0.6752(13) 0.060(7) Uani 1 1 d . . . H34A H 0.2989 0.7376 0.6735 0.073 Uiso 1 1 calc R . . C35 C 0.3297(10) 0.7807(7) 0.6285(12) 0.054(6) Uani 1 1 d . . . H35A H 0.2979 0.8033 0.5945 0.065 Uiso 1 1 calc R . . C36 C 0.3743(11) 0.7871(7) 0.6303(13) 0.049(6) Uani 1 1 d . . . H36A H 0.3728 0.8145 0.5986 0.059 Uiso 1 1 calc R . . C37 C 0.4205(9) 0.7553(8) 0.6758(11) 0.056(7) Uani 1 1 d . . . H37A H 0.4509 0.7596 0.6762 0.068 Uiso 1 1 calc R . . C38 C 0.4208(9) 0.7155(8) 0.7229(11) 0.044(6) Uani 1 1 d . . . H38A H 0.4518 0.6918 0.7541 0.052 Uiso 1 1 calc R . . C39 C 0.4429(8) 0.6258(7) 0.8375(10) 0.034(5) Uani 1 1 d . . . C40 C 0.4477(10) 0.5753(7) 0.8115(12) 0.049(6) Uani 1 1 d . . . H40A H 0.4147 0.5570 0.7660 0.059 Uiso 1 1 calc R . . C41 C 0.4999(11) 0.5551(7) 0.8530(14) 0.056(7) Uani 1 1 d . . . H41A H 0.5026 0.5220 0.8359 0.067 Uiso 1 1 calc R . . C42 C 0.5489(10) 0.5794(8) 0.9182(14) 0.059(7) Uani 1 1 d . . . H42A H 0.5846 0.5630 0.9461 0.071 Uiso 1 1 calc R . . C43 C 0.5468(9) 0.6268(9) 0.9432(13) 0.058(6) Uani 1 1 d . . . H43A H 0.5810 0.6444 0.9877 0.070 Uiso 1 1 calc R . . C44 C 0.4941(9) 0.6500(7) 0.9030(13) 0.049(6) Uani 1 1 d . . . H44A H 0.4930 0.6835 0.9209 0.059 Uiso 1 1 calc R . . C45 C 0.4416(8) 0.6577(7) 1.0258(11) 0.035(5) Uani 1 1 d . . . C46 C 0.4687(9) 0.6139(7) 1.0276(14) 0.051(6) Uani 1 1 d . . . H46A H 0.4504 0.5949 0.9769 0.061 Uiso 1 1 calc R . . C47 C 0.5202(11) 0.5973(9) 1.0992(16) 0.066(7) Uani 1 1 d . . . H47A H 0.5372 0.5674 1.0973 0.079 Uiso 1 1 calc R . . C48 C 0.5481(9) 0.6233(9) 1.1746(16) 0.063(7) Uani 1 1 d . . . H48A H 0.5827 0.6103 1.2255 0.076 Uiso 1 1 calc R . . C49 C 0.5253(12) 0.6670(10) 1.1740(15) 0.080(8) Uani 1 1 d . . . H49A H 0.5459 0.6868 1.2244 0.096 Uiso 1 1 calc R . . C50 C 0.4714(9) 0.6852(8) 1.1009(14) 0.055(6) Uani 1 1 d . . . H50A H 0.4558 0.7160 1.1033 0.066 Uiso 1 1 calc R . . C51 C 0.3556(10) 0.7384(7) 0.9467(12) 0.047(6) Uani 1 1 d . . . C52 C 0.3058(10) 0.7434(7) 0.9352(11) 0.053(7) Uani 1 1 d . . . H52A H 0.2831 0.7136 0.9209 0.063 Uiso 1 1 calc R . . C53 C 0.2894(11) 0.7915(9) 0.9444(12) 0.060(7) Uani 1 1 d . . . H53A H 0.2549 0.7944 0.9342 0.072 Uiso 1 1 calc R . . C54 C 0.3229(12) 0.8341(9) 0.9681(13) 0.064(7) Uani 1 1 d . . . H54A H 0.3118 0.8668 0.9742 0.077 Uiso 1 1 calc R . . C55 C 0.3731(11) 0.8296(8) 0.9833(14) 0.066(7) Uani 1 1 d . . . H55A H 0.3968 0.8593 1.0017 0.080 Uiso 1 1 calc R . . C56 C 0.3901(9) 0.7816(8) 0.9721(11) 0.051(6) Uani 1 1 d . . . H56A H 0.4244 0.7792 0.9819 0.061 Uiso 1 1 calc R . . N3 N 0.3242(5) 0.6182(4) 0.7151(7) 0.024(3) Uani 1 1 d U . . Si3 Si 0.2960(3) 0.5955(2) 0.6163(3) 0.0413(16) Uani 1 1 d U . . C57 C 0.3060(9) 0.5243(6) 0.6165(12) 0.064(7) Uani 1 1 d . . . H57A H 0.3456 0.5171 0.6436 0.096 Uiso 1 1 calc R . . H57B H 0.2808 0.5115 0.5582 0.096 Uiso 1 1 calc R . . H57C H 0.2969 0.5068 0.6476 0.096 Uiso 1 1 calc R . . C58 C 0.3245(9) 0.6265(8) 0.5718(11) 0.063(7) Uani 1 1 d . . . H58A H 0.3653 0.6190 0.6080 0.095 Uiso 1 1 calc R . . H58B H 0.3188 0.6641 0.5688 0.095 Uiso 1 1 calc R . . H58C H 0.3047 0.6128 0.5150 0.095 Uiso 1 1 calc R . . C59 C 0.2173(8) 0.6081(7) 0.5407(11) 0.051(6) Uani 1 1 d . . . H59A H 0.2103 0.6454 0.5290 0.076 Uiso 1 1 calc R . . H59B H 0.2014 0.5962 0.5657 0.076 Uiso 1 1 calc R . . H59C H 0.1991 0.5893 0.4879 0.076 Uiso 1 1 calc R . . N4 N 0.3279(6) 0.6307(5) 0.9080(9) 0.043(5) Uani 1 1 d . . . Si4 Si 0.3259(2) 0.60157(19) 0.9813(3) 0.0433(17) Uani 1 1 d . . . C60 C 0.3792(9) 0.5489(8) 1.0412(13) 0.069(7) Uani 1 1 d . . . H60A H 0.3815 0.5296 1.0034 0.103 Uiso 1 1 calc R . . H60B H 0.3677 0.5254 1.0643 0.103 Uiso 1 1 calc R . . H60C H 0.4164 0.5640 1.0874 0.103 Uiso 1 1 calc R . . C61 C 0.3410(9) 0.6455(7) 1.0634(11) 0.055(7) Uani 1 1 d . . . H61A H 0.3130 0.6736 1.0367 0.083 Uiso 1 1 calc R . . H61B H 0.3793 0.6602 1.0959 0.083 Uiso 1 1 calc R . . H61C H 0.3390 0.6259 1.1013 0.083 Uiso 1 1 calc R . . C62 C 0.2531(8) 0.5767(8) 0.9203(11) 0.055(6) Uani 1 1 d . . . H62A H 0.2266 0.6059 0.8988 0.082 Uiso 1 1 calc R . . H62B H 0.2513 0.5549 0.9567 0.082 Uiso 1 1 calc R . . H62C H 0.2426 0.5559 0.8728 0.082 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 0.0423(8) 0.0284(7) 0.0384(7) 0.0001(6) 0.0264(6) -0.0010(6) C1 0.015(11) 0.010(9) 0.032(11) 0.005(8) 0.001(10) 0.004(8) P1 0.041(4) 0.034(3) 0.040(3) 0.000(3) 0.024(3) 0.001(3) P2 0.044(4) 0.032(3) 0.037(3) 0.001(3) 0.025(3) 0.000(3) C2 0.034(14) 0.036(12) 0.020(12) -0.010(10) 0.006(11) 0.003(10) C3 0.050(17) 0.049(14) 0.046(14) 0.002(11) 0.034(14) -0.013(12) C4 0.075(19) 0.062(15) 0.10(2) -0.018(15) 0.082(19) -0.027(13) C5 0.10(2) 0.058(15) 0.070(18) -0.027(13) 0.070(17) -0.030(14) C6 0.08(2) 0.038(13) 0.047(15) -0.016(11) 0.049(15) -0.017(12) C7 0.039(15) 0.068(16) 0.052(15) 0.008(13) 0.034(14) 0.001(11) C8 0.058(17) 0.041(13) 0.033(13) 0.020(11) 0.030(13) 0.025(11) C9 0.09(2) 0.039(14) 0.063(17) 0.010(12) 0.067(17) -0.009(11) C10 0.067(18) 0.057(15) 0.029(14) 0.005(11) 0.037(14) -0.011(13) C11 0.042(17) 0.024(13) 0.048(16) 0.016(12) -0.003(14) -0.001(11) C12 0.08(2) 0.055(16) 0.09(2) 0.002(15) 0.06(2) 0.007(13) C13 0.046(15) 0.042(13) 0.029(14) -0.003(10) 0.025(13) 0.006(11) C14 0.034(13) 0.013(11) 0.043(13) -0.014(9) 0.031(12) -0.008(8) C15 0.032(14) 0.051(14) 0.049(15) -0.006(12) 0.018(13) -0.010(11) C16 0.09(2) 0.063(18) 0.077(18) -0.022(14) 0.057(17) -0.035(15) C17 0.067(19) 0.07(2) 0.066(18) -0.007(14) 0.041(16) -0.020(14) C18 0.065(18) 0.031(13) 0.075(18) 0.009(12) 0.039(16) -0.012(11) C19 0.033(14) 0.050(15) 0.042(13) 0.000(11) 0.019(12) -0.012(10) C20 0.050(17) 0.030(12) 0.032(13) 0.004(10) 0.020(14) -0.012(10) C21 0.047(16) 0.024(12) 0.066(18) -0.011(11) 0.033(15) -0.013(10) C22 0.07(2) 0.045(14) 0.052(17) 0.008(13) 0.044(16) 0.013(13) C23 0.09(3) 0.053(16) 0.048(18) -0.002(13) 0.04(2) -0.019(15) C24 0.06(2) 0.075(18) 0.036(17) -0.024(14) 0.013(16) -0.046(15) C25 0.028(17) 0.094(18) 0.070(19) 0.010(15) 0.036(15) 0.003(13) N1 0.041(11) 0.012(8) 0.034(9) 0.002(7) 0.028(8) -0.004(7) Si1 0.050(4) 0.022(3) 0.044(4) 0.009(3) 0.030(4) 0.005(3) C26 0.038(15) 0.042(13) 0.070(16) 0.006(11) 0.020(13) 0.016(10) C27 0.040(14) 0.037(11) 0.041(13) 0.016(10) 0.023(12) 0.012(10) C28 0.09(2) 0.038(13) 0.052(14) 0.005(11) 0.046(15) 0.006(11) N2 0.033(12) 0.034(9) 0.028(10) -0.019(7) 0.008(9) -0.008(7) Si2 0.048(4) 0.027(3) 0.049(4) 0.003(3) 0.028(3) 0.004(3) C29 0.055(17) 0.072(16) 0.073(17) 0.010(13) 0.038(15) 0.004(12) C30 0.066(17) 0.034(12) 0.081(16) 0.018(11) 0.050(14) 0.012(10) C31 0.060(16) 0.049(13) 0.036(12) 0.012(10) 0.026(12) 0.010(11) C32 0.038(14) 0.035(12) 0.041(13) 0.005(10) 0.025(11) 0.010(9) P3 0.045(4) 0.029(3) 0.037(3) -0.001(3) 0.024(3) 0.000(3) P4 0.039(4) 0.027(3) 0.039(3) -0.003(2) 0.023(3) -0.001(2) C33 0.061(17) 0.041(13) 0.041(13) 0.001(10) 0.044(14) 0.003(12) C34 0.062(18) 0.055(15) 0.065(16) 0.022(13) 0.042(15) 0.032(13) C35 0.073(19) 0.040(14) 0.043(14) 0.006(11) 0.036(14) 0.007(12) C36 0.075(19) 0.041(13) 0.048(15) 0.009(11) 0.049(16) 0.002(13) C37 0.049(17) 0.065(15) 0.010(11) 0.005(11) 0.000(12) -0.008(13) C38 0.034(15) 0.059(15) 0.022(12) 0.000(11) 0.012(12) 0.002(11) C39 0.039(14) 0.048(13) 0.016(10) 0.013(10) 0.017(11) 0.001(11) C40 0.068(18) 0.027(12) 0.050(14) -0.009(11) 0.037(14) 0.011(11) C41 0.09(2) 0.026(13) 0.069(18) 0.007(13) 0.060(17) 0.017(14) C42 0.064(19) 0.049(15) 0.058(16) -0.027(13) 0.037(15) -0.001(13) C43 0.029(16) 0.10(2) 0.055(15) 0.017(15) 0.031(13) -0.001(14) C44 0.042(16) 0.026(11) 0.057(15) -0.014(11) 0.023(14) -0.014(11) C45 0.042(14) 0.037(13) 0.025(13) 0.006(10) 0.021(12) 0.000(11) C46 0.055(17) 0.037(14) 0.059(16) -0.002(12) 0.037(15) 0.000(12) C47 0.06(2) 0.063(16) 0.059(17) 0.007(15) 0.031(16) 0.002(14) C48 0.051(17) 0.057(16) 0.071(19) 0.030(15) 0.035(16) 0.029(14) C49 0.10(2) 0.071(19) 0.048(17) -0.003(14) 0.038(19) -0.018(16) C50 0.030(15) 0.072(16) 0.056(16) -0.001(14) 0.025(14) 0.012(12) C51 0.044(16) 0.047(14) 0.034(13) -0.008(10) 0.019(13) -0.001(12) C52 0.09(2) 0.037(14) 0.038(14) 0.012(10) 0.043(15) 0.011(12) C53 0.11(2) 0.046(15) 0.053(15) 0.010(12) 0.065(16) 0.028(15) C54 0.09(2) 0.046(17) 0.055(16) 0.014(12) 0.046(17) 0.031(15) C55 0.08(2) 0.045(16) 0.080(18) -0.021(12) 0.058(17) -0.018(13) C56 0.059(16) 0.044(14) 0.033(13) -0.010(11) 0.023(13) -0.023(13) N3 0.026(9) 0.011(7) 0.030(7) -0.015(7) 0.016(7) -0.013(7) Si3 0.056(4) 0.037(3) 0.040(3) 0.000(3) 0.035(4) -0.002(3) C57 0.10(2) 0.035(13) 0.073(16) -0.034(11) 0.063(16) -0.017(12) C58 0.100(19) 0.076(16) 0.054(14) -0.030(12) 0.069(15) -0.020(13) C59 0.068(17) 0.060(15) 0.040(12) 0.003(10) 0.042(13) 0.007(11) N4 0.045(11) 0.027(9) 0.042(10) -0.002(7) 0.023(9) -0.004(7) Si4 0.051(4) 0.034(3) 0.042(4) 0.005(3) 0.029(3) 0.002(3) C60 0.052(17) 0.090(18) 0.070(16) 0.014(13) 0.043(14) -0.007(12) C61 0.074(18) 0.040(12) 0.043(13) 0.021(10) 0.035(13) 0.012(11) C62 0.046(15) 0.075(16) 0.046(13) -0.006(12) 0.032(12) -0.028(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 Sm1 C1 2.404(17) . ? Sm1 N4 2.439(14) . ? Sm1 N3 2.481(13) . ? Sm1 N1 2.497(13) . ? Sm1 N2 2.506(13) . ? Sm1 C32 2.943(18) . ? C1 P1 1.637(15) . ? C1 P2 1.650(15) . ? P1 N1 1.610(14) . ? P1 C2 1.84(2) . ? P1 C8 1.869(19) . ? P2 N2 1.636(15) . ? P2 C20 1.836(19) . ? P2 C14 1.845(18) . ? C2 C3 1.36(3) . ? C2 C7 1.43(2) . ? C3 C4 1.34(3) . ? C4 C5 1.38(3) . ? C5 C6 1.35(3) . ? C6 C7 1.39(3) . ? C8 C13 1.35(2) . ? C8 C9 1.40(3) . ? C9 C10 1.39(2) . ? C10 C11 1.36(3) . ? C11 C12 1.39(3) . ? C12 C13 1.39(3) . ? C14 C15 1.35(3) . ? C14 C19 1.41(2) . ? C15 C16 1.40(3) . ? C16 C17 1.34(3) . ? C17 C18 1.38(3) . ? C18 C19 1.37(3) . ? C20 C25 1.38(3) . ? C20 C21 1.46(3) . ? C21 C22 1.41(3) . ? C22 C23 1.34(3) . ? C23 C24 1.38(3) . ? C24 C25 1.36(3) . ? N1 Si1 1.742(12) . ? Si1 C26 1.86(2) . ? Si1 C28 1.876(19) . ? Si1 C27 1.881(17) . ? N2 Si2 1.701(15) . ? Si2 C29 1.89(2) . ? Si2 C31 1.887(18) . ? Si2 C30 1.91(2) . ? C32 P4 1.723(19) . ? C32 P3 1.757(19) . ? P3 N3 1.579(12) . ? P3 C39 1.788(19) . ? P3 C33 1.835(19) . ? P4 N4 1.608(15) . ? P4 C45 1.798(19) . ? P4 C51 1.82(2) . ? C33 C38 1.36(3) . ? C33 C34 1.41(3) . ? C34 C35 1.40(3) . ? C35 C36 1.38(3) . ? C36 C37 1.36(3) . ? C37 C38 1.42(3) . ? C39 C44 1.39(2) . ? C39 C40 1.46(2) . ? C40 C41 1.35(3) . ? C41 C42 1.36(3) . ? C42 C43 1.35(3) . ? C43 C44 1.40(3) . ? C45 C50 1.39(2) . ? C45 C46 1.39(2) . ? C46 C47 1.36(3) . ? C47 C48 1.38(3) . ? C48 C49 1.33(3) . ? C49 C50 1.42(3) . ? C51 C56 1.39(3) . ? C51 C52 1.41(3) . ? C52 C53 1.40(3) . ? C53 C54 1.36(3) . ? C54 C55 1.38(3) . ? C55 C56 1.43(3) . ? N3 Si3 1.742(13) . ? Si3 C58 1.84(2) . ? Si3 C57 1.858(17) . ? Si3 C59 1.878(19) . ? N4 Si4 1.754(16) . ? Si4 C62 1.839(18) . ? Si4 C61 1.845(19) . ? Si4 C60 1.85(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Sm1 N4 118.4(6) . . ? C1 Sm1 N3 131.4(5) . . ? N4 Sm1 N3 108.4(5) . . ? C1 Sm1 N1 64.2(4) . . ? N4 Sm1 N1 107.0(4) . . ? N3 Sm1 N1 114.7(4) . . ? C1 Sm1 N2 64.1(5) . . ? N4 Sm1 N2 103.7(4) . . ? N3 Sm1 N2 93.8(4) . . ? N1 Sm1 N2 127.6(4) . . ? C1 Sm1 C32 158.8(5) . . ? N4 Sm1 C32 60.6(5) . . ? N3 Sm1 C32 60.2(4) . . ? N1 Sm1 C32 95.3(5) . . ? N2 Sm1 C32 137.0(5) . . ? P1 C1 P2 164.8(11) . . ? P1 C1 Sm1 95.8(7) . . ? P2 C1 Sm1 97.1(7) . . ? N1 P1 C1 106.6(8) . . ? N1 P1 C2 112.3(9) . . ? C1 P1 C2 111.8(9) . . ? N1 P1 C8 110.6(8) . . ? C1 P1 C8 114.4(9) . . ? C2 P1 C8 101.3(9) . . ? N2 P2 C1 104.9(8) . . ? N2 P2 C20 114.7(10) . . ? C1 P2 C20 112.5(8) . . ? N2 P2 C14 113.0(8) . . ? C1 P2 C14 115.5(9) . . ? C20 P2 C14 96.7(9) . . ? C3 C2 C7 118(2) . . ? C3 C2 P1 123.9(16) . . ? C7 C2 P1 117.4(17) . . ? C4 C3 C2 121(2) . . ? C3 C4 C5 121(2) . . ? C6 C5 C4 121(2) . . ? C5 C6 C7 119(2) . . ? C6 C7 C2 120(2) . . ? C13 C8 C9 119.8(18) . . ? C13 C8 P1 123.8(17) . . ? C9 C8 P1 116.2(16) . . ? C10 C9 C8 120(2) . . ? C11 C10 C9 118(2) . . ? C10 C11 C12 122(2) . . ? C11 C12 C13 118(2) . . ? C8 C13 C12 121.1(19) . . ? C15 C14 C19 119.0(18) . . ? C15 C14 P2 121.0(14) . . ? C19 C14 P2 119.9(15) . . ? C14 C15 C16 121(2) . . ? C17 C16 C15 119(3) . . ? C16 C17 C18 122(2) . . ? C19 C18 C17 118(2) . . ? C18 C19 C14 120(2) . . ? C25 C20 C21 119.4(19) . . ? C25 C20 P2 121(2) . . ? C21 C20 P2 119.3(17) . . ? C22 C21 C20 116(2) . . ? C23 C22 C21 124(2) . . ? C22 C23 C24 118(2) . . ? C25 C24 C23 122(3) . . ? C24 C25 C20 121(2) . . ? P1 N1 Si1 126.2(8) . . ? P1 N1 Sm1 93.1(5) . . ? Si1 N1 Sm1 139.1(7) . . ? N1 Si1 C26 114.0(9) . . ? N1 Si1 C28 110.8(8) . . ? C26 Si1 C28 107.5(10) . . ? N1 Si1 C27 111.5(7) . . ? C26 Si1 C27 104.6(9) . . ? C28 Si1 C27 108.2(9) . . ? P2 N2 Si2 133.8(9) . . ? P2 N2 Sm1 93.7(6) . . ? Si2 N2 Sm1 129.6(7) . . ? N2 Si2 C29 105.4(8) . . ? N2 Si2 C31 116.1(7) . . ? C29 Si2 C31 108.3(10) . . ? N2 Si2 C30 115.5(9) . . ? C29 Si2 C30 106.0(9) . . ? C31 Si2 C30 105.1(8) . . ? P4 C32 P3 137.9(11) . . ? P4 C32 Sm1 83.3(7) . . ? P3 C32 Sm1 83.8(6) . . ? N3 P3 C32 110.9(8) . . ? N3 P3 C39 112.4(8) . . ? C32 P3 C39 114.2(8) . . ? N3 P3 C33 111.9(8) . . ? C32 P3 C33 103.3(9) . . ? C39 P3 C33 103.6(10) . . ? N4 P4 C32 111.1(8) . . ? N4 P4 C45 108.3(8) . . ? C32 P4 C45 117.9(9) . . ? N4 P4 C51 112.6(10) . . ? C32 P4 C51 100.2(9) . . ? C45 P4 C51 106.5(9) . . ? C38 C33 C34 120.8(19) . . ? C38 C33 P3 123.3(17) . . ? C34 C33 P3 115.5(18) . . ? C35 C34 C33 116(2) . . ? C36 C35 C34 122(2) . . ? C37 C36 C35 122(2) . . ? C36 C37 C38 116(2) . . ? C33 C38 C37 122(2) . . ? C44 C39 C40 115.9(18) . . ? C44 C39 P3 123.4(16) . . ? C40 C39 P3 120.3(15) . . ? C41 C40 C39 118.7(19) . . ? C40 C41 C42 124(2) . . ? C43 C42 C41 120(2) . . ? C42 C43 C44 119(2) . . ? C39 C44 C43 122.4(19) . . ? C50 C45 C46 116.1(18) . . ? C50 C45 P4 124.6(16) . . ? C46 C45 P4 119.3(16) . . ? C47 C46 C45 123(2) . . ? C46 C47 C48 121(2) . . ? C49 C48 C47 118(2) . . ? C48 C49 C50 123(2) . . ? C45 C50 C49 120(2) . . ? C56 C51 C52 119(2) . . ? C56 C51 P4 123(2) . . ? C52 C51 P4 118.3(16) . . ? C53 C52 C51 121(2) . . ? C54 C53 C52 120(2) . . ? C53 C54 C55 120(2) . . ? C54 C55 C56 122(2) . . ? C51 C56 C55 119(2) . . ? P3 N3 Si3 131.5(9) . . ? P3 N3 Sm1 104.7(6) . . ? Si3 N3 Sm1 120.5(6) . . ? N3 Si3 C58 115.3(7) . . ? N3 Si3 C57 112.1(8) . . ? C58 Si3 C57 106.9(10) . . ? N3 Si3 C59 107.7(7) . . ? C58 Si3 C59 107.2(9) . . ? C57 Si3 C59 107.2(9) . . ? P4 N4 Si4 125.5(9) . . ? P4 N4 Sm1 104.2(7) . . ? Si4 N4 Sm1 130.3(7) . . ? N4 Si4 C62 106.1(8) . . ? N4 Si4 C61 115.2(8) . . ? C62 Si4 C61 107.8(10) . . ? N4 Si4 C60 112.0(9) . . ? C62 Si4 C60 111.3(9) . . ? C61 Si4 C60 104.5(9) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 21.03 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.113 _refine_diff_density_min -0.755 _refine_diff_density_rms 0.151 # Attachment '17.cif' data_17 _database_code_depnum_ccdc_archive 'CCDC 736114' _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62 H77 Gd N4 P4 Si4' _chemical_formula_sum 'C62 H77 Gd N4 P4 Si4' _chemical_formula_weight 1271.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 31.0859(8) _cell_length_b 25.7873(7) _cell_length_c 21.0064(5) _cell_angle_alpha 90.00 _cell_angle_beta 131.182(2) _cell_angle_gamma 90.00 _cell_volume 12673.5(6) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 16770 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 27.52 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.333 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5256 _exptl_absorpt_coefficient_mu 1.264 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.74 _exptl_absorpt_correction_T_max 0.80 _exptl_absorpt_process_details '(SADABS; Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 40500 _diffrn_reflns_av_R_equivalents 0.0273 _diffrn_reflns_av_sigmaI/netI 0.0342 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 27.53 _reflns_number_total 14507 _reflns_number_gt 11824 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'enCIFer(Allen et al.,2004);PLATON(Spek,2003)' _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^)+(0.0229P)^2^+14.8989P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom, Me from difmap' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14507 _refine_ls_number_parameters 688 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0404 _refine_ls_R_factor_gt 0.0255 _refine_ls_wR_factor_ref 0.0611 _refine_ls_wR_factor_gt 0.0543 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.004 _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 0.265318(4) 0.620178(4) 0.756071(6) 0.01505(3) Uani 1 1 d . . . C1 C 0.16814(9) 0.59455(8) 0.68185(14) 0.0216(5) Uani 1 1 d . . . P1 P 0.14262(2) 0.65390(2) 0.65704(4) 0.01815(12) Uani 1 1 d . . . P2 P 0.17783(2) 0.53224(2) 0.67913(4) 0.01926(12) Uani 1 1 d . . . C2 C 0.08116(9) 0.66346(8) 0.54423(14) 0.0215(5) Uani 1 1 d . . . C3 C 0.08070(10) 0.63622(10) 0.48666(15) 0.0282(5) Uani 1 1 d . . . H3A H 0.1113 0.6133 0.5068 0.034 Uiso 1 1 calc R . . C4 C 0.03633(11) 0.64205(11) 0.40030(16) 0.0348(6) Uani 1 1 d . . . H4A H 0.0365 0.6231 0.3617 0.042 Uiso 1 1 calc R . . C5 C -0.00820(11) 0.67543(11) 0.37056(16) 0.0375(7) Uani 1 1 d . . . H5A H -0.0383 0.6800 0.3114 0.045 Uiso 1 1 calc R . . C6 C -0.00889(11) 0.70207(10) 0.42653(17) 0.0376(7) Uani 1 1 d . . . H6A H -0.0398 0.7247 0.4058 0.045 Uiso 1 1 calc R . . C7 C 0.03512(10) 0.69621(9) 0.51288(16) 0.0303(6) Uani 1 1 d . . . H7A H 0.0340 0.7145 0.5510 0.036 Uiso 1 1 calc R . . C8 C 0.11397(10) 0.66956(9) 0.70762(15) 0.0242(5) Uani 1 1 d . . . C9 C 0.06501(11) 0.64476(11) 0.68204(18) 0.0350(6) Uani 1 1 d . . . H9A H 0.0442 0.6225 0.6341 0.042 Uiso 1 1 calc R . . C10 C 0.04636(14) 0.65212(13) 0.7257(2) 0.0498(8) Uani 1 1 d . . . H10A H 0.0128 0.6350 0.7075 0.060 Uiso 1 1 calc R . . C11 C 0.07627(14) 0.68419(13) 0.7954(2) 0.0499(8) Uani 1 1 d . . . H11A H 0.0633 0.6893 0.8252 0.060 Uiso 1 1 calc R . . C12 C 0.12481(13) 0.70873(12) 0.82183(18) 0.0416(7) Uani 1 1 d . . . H12A H 0.1455 0.7307 0.8700 0.050 Uiso 1 1 calc R . . C13 C 0.14383(11) 0.70146(10) 0.77821(15) 0.0290(5) Uani 1 1 d . . . H13A H 0.1775 0.7185 0.7969 0.035 Uiso 1 1 calc R . . C14 C 0.13532(10) 0.50647(9) 0.57147(14) 0.0256(5) Uani 1 1 d . . . C15 C 0.15898(12) 0.48545(9) 0.54008(16) 0.0325(6) Uani 1 1 d . . . H15A H 0.1994 0.4834 0.5754 0.039 Uiso 1 1 calc R . . C16 C 0.12441(15) 0.46723(11) 0.45733(18) 0.0456(8) Uani 1 1 d . . . H16A H 0.1412 0.4529 0.4365 0.055 Uiso 1 1 calc R . . C17 C 0.06597(16) 0.46994(12) 0.40587(18) 0.0524(9) Uani 1 1 d . . . H17A H 0.0424 0.4575 0.3494 0.063 Uiso 1 1 calc R . . C18 C 0.04139(14) 0.49073(13) 0.43601(18) 0.0537(9) Uani 1 1 d . . . H18A H 0.0010 0.4926 0.4003 0.064 Uiso 1 1 calc R . . C19 C 0.07589(12) 0.50888(12) 0.51850(17) 0.0419(7) Uani 1 1 d . . . H19A H 0.0589 0.5231 0.5391 0.050 Uiso 1 1 calc R . . C20 C 0.15054(10) 0.48996(9) 0.71562(14) 0.0241(5) Uani 1 1 d . . . C21 C 0.14825(11) 0.43623(10) 0.70422(17) 0.0344(6) Uani 1 1 d . . . H21A H 0.1601 0.4219 0.6762 0.041 Uiso 1 1 calc R . . C22 C 0.12901(13) 0.40392(11) 0.73328(19) 0.0444(7) Uani 1 1 d . . . H22A H 0.1285 0.3674 0.7265 0.053 Uiso 1 1 calc R . . C23 C 0.11076(13) 0.42460(12) 0.77190(18) 0.0494(8) Uani 1 1 d . . . H23A H 0.0977 0.4023 0.7922 0.059 Uiso 1 1 calc R . . C24 C 0.11109(13) 0.47769(13) 0.78168(18) 0.0456(8) Uani 1 1 d . . . H24A H 0.0977 0.4918 0.8077 0.055 Uiso 1 1 calc R . . C25 C 0.13109(11) 0.51044(10) 0.75333(16) 0.0322(6) Uani 1 1 d . . . H25A H 0.1313 0.5469 0.7600 0.039 Uiso 1 1 calc R . . N1 N 0.19542(8) 0.69253(7) 0.69106(11) 0.0184(4) Uani 1 1 d . . . Si1 Si 0.18889(3) 0.75657(2) 0.66150(4) 0.01993(13) Uani 1 1 d . . . C26 C 0.25661(10) 0.79389(9) 0.73801(15) 0.0264(5) Uani 1 1 d . . . H26A H 0.2887 0.7736 0.7527 0.040 Uiso 1 1 calc R . . H26B H 0.2627 0.8009 0.7893 0.040 Uiso 1 1 calc R . . H26C H 0.2540 0.8268 0.7122 0.040 Uiso 1 1 calc R . . C27 C 0.16817(12) 0.76151(10) 0.55564(15) 0.0336(6) Uani 1 1 d . . . H27A H 0.1955 0.7420 0.5562 0.050 Uiso 1 1 calc R . . H27B H 0.1684 0.7980 0.5428 0.050 Uiso 1 1 calc R . . H27C H 0.1298 0.7471 0.5123 0.050 Uiso 1 1 calc R . . C28 C 0.13447(11) 0.79462(9) 0.65493(18) 0.0353(6) Uani 1 1 d . . . H28A H 0.1458 0.7959 0.7109 0.053 Uiso 1 1 calc R . . H28B H 0.0971 0.7778 0.6148 0.053 Uiso 1 1 calc R . . H28C H 0.1322 0.8300 0.6357 0.053 Uiso 1 1 calc R . . N2 N 0.24602(8) 0.52481(7) 0.73445(11) 0.0197(4) Uani 1 1 d . . . Si2 Si 0.29254(3) 0.47430(2) 0.79040(4) 0.02448(14) Uani 1 1 d . . . C29 C 0.36606(11) 0.50147(11) 0.85183(17) 0.0356(6) Uani 1 1 d . . . H29A H 0.3731 0.5083 0.8135 0.053 Uiso 1 1 calc R . . H29B H 0.3942 0.4765 0.8950 0.053 Uiso 1 1 calc R . . H29C H 0.3694 0.5339 0.8792 0.053 Uiso 1 1 calc R . . C30 C 0.28349(13) 0.42004(9) 0.72309(18) 0.0385(7) Uani 1 1 d . . . H30A H 0.2875 0.4336 0.6836 0.058 Uiso 1 1 calc R . . H30B H 0.2455 0.4046 0.6912 0.058 Uiso 1 1 calc R . . H30C H 0.3128 0.3936 0.7593 0.058 Uiso 1 1 calc R . . C31 C 0.29063(11) 0.44312(10) 0.86929(16) 0.0333(6) Uani 1 1 d . . . H31A H 0.2954 0.4698 0.9068 0.050 Uiso 1 1 calc R . . H31B H 0.3216 0.4177 0.9029 0.050 Uiso 1 1 calc R . . H31C H 0.2538 0.4256 0.8394 0.050 Uiso 1 1 calc R . . C32 C 0.36473(9) 0.68822(8) 0.84174(13) 0.0194(4) Uani 1 1 d . . . H32A H 0.3526 0.7250 0.8229 0.023 Uiso 1 1 calc R . . P3 P 0.37121(2) 0.67500(2) 0.92855(3) 0.01752(11) Uani 1 1 d . . . P4 P 0.37412(2) 0.65657(2) 0.77865(3) 0.01681(11) Uani 1 1 d . . . C33 C 0.44262(9) 0.65849(9) 1.02625(14) 0.0234(5) Uani 1 1 d . . . C34 C 0.46811(11) 0.61377(10) 1.02685(16) 0.0318(6) Uani 1 1 d . . . H34A H 0.4494 0.5947 0.9761 0.038 Uiso 1 1 calc R . . C35 C 0.52035(12) 0.59695(13) 1.10072(19) 0.0446(7) Uani 1 1 d . . . H35A H 0.5372 0.5663 1.1004 0.054 Uiso 1 1 calc R . . C36 C 0.54810(12) 0.62444(14) 1.17472(19) 0.0506(8) Uani 1 1 d . . . H36A H 0.5839 0.6128 1.2254 0.061 Uiso 1 1 calc R . . C37 C 0.52378(13) 0.66875(14) 1.17501(18) 0.0524(9) Uani 1 1 d . . . H37A H 0.5431 0.6879 1.2259 0.063 Uiso 1 1 calc R . . C38 C 0.47127(11) 0.68582(11) 1.10165(16) 0.0376(6) Uani 1 1 d . . . H38A H 0.4547 0.7164 1.1028 0.045 Uiso 1 1 calc R . . C39 C 0.35436(10) 0.73744(9) 0.94808(14) 0.0234(5) Uani 1 1 d . . . C40 C 0.38885(12) 0.78109(9) 0.97254(16) 0.0330(6) Uani 1 1 d . . . H40A H 0.4235 0.7782 0.9829 0.040 Uiso 1 1 calc R . . C41 C 0.37249(15) 0.82871(10) 0.98169(18) 0.0456(8) Uani 1 1 d . . . H41A H 0.3959 0.8584 0.9982 0.055 Uiso 1 1 calc R . . C42 C 0.32249(15) 0.83304(11) 0.96699(18) 0.0478(8) Uani 1 1 d . . . H42A H 0.3118 0.8656 0.9742 0.057 Uiso 1 1 calc R . . C43 C 0.28787(13) 0.79050(11) 0.94195(17) 0.0408(7) Uani 1 1 d . . . H43A H 0.2532 0.7938 0.9312 0.049 Uiso 1 1 calc R . . C44 C 0.30375(11) 0.74278(10) 0.93233(15) 0.0289(5) Uani 1 1 d . . . H44A H 0.2797 0.7135 0.9148 0.035 Uiso 1 1 calc R . . C45 C 0.44277(9) 0.62478(8) 0.83671(14) 0.0202(5) Uani 1 1 d . . . C46 C 0.44669(10) 0.57652(9) 0.81132(16) 0.0284(5) Uani 1 1 d . . . H46A H 0.4128 0.5588 0.7660 0.034 Uiso 1 1 calc R . . C47 C 0.49951(12) 0.55401(10) 0.85146(18) 0.0392(7) Uani 1 1 d . . . H47A H 0.5017 0.5209 0.8340 0.047 Uiso 1 1 calc R . . C48 C 0.54877(11) 0.57963(11) 0.91649(17) 0.0378(6) Uani 1 1 d . . . H48A H 0.5850 0.5643 0.9435 0.045 Uiso 1 1 calc R . . C49 C 0.54564(11) 0.62743(10) 0.94247(17) 0.0358(6) Uani 1 1 d . . . H49A H 0.5797 0.6451 0.9874 0.043 Uiso 1 1 calc R . . C50 C 0.49291(10) 0.64994(10) 0.90334(15) 0.0288(5) Uani 1 1 d . . . H50A H 0.4910 0.6827 0.9221 0.035 Uiso 1 1 calc R . . C51 C 0.37713(10) 0.70878(8) 0.72345(13) 0.0201(5) Uani 1 1 d . . . C52 C 0.33018(11) 0.74159(10) 0.67344(16) 0.0326(6) Uani 1 1 d . . . H52A H 0.2987 0.7368 0.6708 0.039 Uiso 1 1 calc R . . C53 C 0.32849(12) 0.78131(10) 0.62722(17) 0.0367(6) Uani 1 1 d . . . H53A H 0.2966 0.8041 0.5945 0.044 Uiso 1 1 calc R . . C54 C 0.37331(11) 0.78765(10) 0.62892(15) 0.0303(6) Uani 1 1 d . . . H54A H 0.3724 0.8149 0.5976 0.036 Uiso 1 1 calc R . . C55 C 0.41938(10) 0.75449(10) 0.67604(15) 0.0289(5) Uani 1 1 d . . . H55A H 0.4497 0.7583 0.6759 0.035 Uiso 1 1 calc R . . C56 C 0.42161(10) 0.71549(9) 0.72369(14) 0.0251(5) Uani 1 1 d . . . H56A H 0.4539 0.6932 0.7568 0.030 Uiso 1 1 calc R . . N3 N 0.32723(8) 0.63047(7) 0.90764(11) 0.0188(4) Uani 1 1 d . . . Si3 Si 0.32540(3) 0.60131(3) 0.98091(4) 0.02271(14) Uani 1 1 d . . . C57 C 0.25180(11) 0.57599(11) 0.92019(16) 0.0372(6) Uani 1 1 d . . . H57A H 0.2434 0.5506 0.8786 0.056 Uiso 1 1 calc R . . H57B H 0.2244 0.6047 0.8909 0.056 Uiso 1 1 calc R . . H57C H 0.2487 0.5593 0.9590 0.056 Uiso 1 1 calc R . . C58 C 0.37942(12) 0.54839(11) 1.04128(17) 0.0391(7) Uani 1 1 d . . . H58A H 0.3793 0.5272 1.0024 0.059 Uiso 1 1 calc R . . H58B H 0.3699 0.5266 1.0688 0.059 Uiso 1 1 calc R . . H58C H 0.4174 0.5636 1.0843 0.059 Uiso 1 1 calc R . . C59 C 0.33998(13) 0.64613(12) 1.06360(17) 0.0416(7) Uani 1 1 d . . . H59A H 0.3094 0.6720 1.0366 0.062 Uiso 1 1 calc R . . H59B H 0.3767 0.6636 1.0927 0.062 Uiso 1 1 calc R . . H59C H 0.3415 0.6261 1.1047 0.062 Uiso 1 1 calc R . . N4 N 0.32173(8) 0.61808(7) 0.71341(11) 0.0184(4) Uani 1 1 d . . . Si4 Si 0.29541(3) 0.59539(3) 0.61568(4) 0.02249(13) Uani 1 1 d . . . C60 C 0.30640(12) 0.52418(10) 0.61791(17) 0.0363(6) Uani 1 1 d . . . H60A H 0.2979 0.5070 0.6501 0.054 Uiso 1 1 calc R . . H60B H 0.3462 0.5173 0.6448 0.054 Uiso 1 1 calc R . . H60C H 0.2809 0.5107 0.5600 0.054 Uiso 1 1 calc R . . C61 C 0.32594(14) 0.62629(12) 0.57262(18) 0.0453(8) Uani 1 1 d . . . H61A H 0.3168 0.6634 0.5638 0.068 Uiso 1 1 calc R . . H61B H 0.3095 0.6100 0.5186 0.068 Uiso 1 1 calc R . . H61C H 0.3675 0.6217 0.6129 0.068 Uiso 1 1 calc R . . C62 C 0.21714(11) 0.60768(10) 0.54104(16) 0.0342(6) Uani 1 1 d . . . H62A H 0.2003 0.5902 0.5615 0.051 Uiso 1 1 calc R . . H62B H 0.1997 0.5942 0.4850 0.051 Uiso 1 1 calc R . . H62C H 0.2101 0.6451 0.5373 0.051 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 0.01418(5) 0.01553(5) 0.01567(5) 0.00014(4) 0.00993(4) 0.00015(4) C1 0.0171(11) 0.0202(11) 0.0251(12) 0.0000(9) 0.0129(10) -0.0011(9) P1 0.0147(3) 0.0190(3) 0.0196(3) 0.0010(2) 0.0108(2) 0.0012(2) P2 0.0184(3) 0.0176(3) 0.0201(3) -0.0001(2) 0.0119(2) -0.0023(2) C2 0.0150(11) 0.0215(11) 0.0219(11) 0.0032(9) 0.0095(10) -0.0002(9) C3 0.0244(13) 0.0343(13) 0.0264(13) 0.0033(10) 0.0170(11) 0.0004(10) C4 0.0329(15) 0.0459(16) 0.0240(13) 0.0001(12) 0.0180(12) -0.0077(12) C5 0.0246(14) 0.0433(16) 0.0245(13) 0.0097(12) 0.0075(11) -0.0068(12) C6 0.0197(13) 0.0337(14) 0.0365(15) 0.0086(12) 0.0087(12) 0.0032(11) C7 0.0208(12) 0.0283(13) 0.0315(13) 0.0005(11) 0.0128(11) 0.0020(10) C8 0.0222(12) 0.0266(12) 0.0268(12) 0.0040(10) 0.0175(11) 0.0055(9) C9 0.0325(15) 0.0384(15) 0.0453(16) -0.0092(13) 0.0304(13) -0.0060(12) C10 0.0500(19) 0.0572(19) 0.072(2) -0.0153(17) 0.0530(19) -0.0134(15) C11 0.062(2) 0.062(2) 0.060(2) -0.0087(16) 0.0550(19) -0.0052(17) C12 0.0469(18) 0.0521(18) 0.0355(15) -0.0074(13) 0.0313(15) -0.0033(14) C13 0.0252(13) 0.0355(14) 0.0265(13) 0.0008(11) 0.0171(11) 0.0015(11) C14 0.0286(13) 0.0213(11) 0.0231(12) -0.0014(9) 0.0154(11) -0.0064(10) C15 0.0407(16) 0.0267(13) 0.0277(13) 0.0019(10) 0.0215(12) 0.0004(11) C16 0.071(2) 0.0354(15) 0.0320(15) 0.0004(12) 0.0347(17) 0.0003(15) C17 0.070(2) 0.0474(18) 0.0256(15) -0.0083(13) 0.0250(16) -0.0248(16) C18 0.0356(17) 0.074(2) 0.0287(15) -0.0081(15) 0.0112(14) -0.0265(16) C19 0.0319(15) 0.0576(19) 0.0288(14) -0.0081(13) 0.0168(13) -0.0149(13) C20 0.0194(12) 0.0259(12) 0.0224(12) 0.0017(9) 0.0118(10) -0.0043(9) C21 0.0325(15) 0.0296(13) 0.0417(15) 0.0011(12) 0.0247(13) -0.0051(11) C22 0.0438(18) 0.0342(15) 0.0527(18) 0.0033(14) 0.0307(16) -0.0114(13) C23 0.0490(19) 0.056(2) 0.0404(17) 0.0011(15) 0.0283(16) -0.0252(15) C24 0.0444(18) 0.068(2) 0.0356(16) -0.0151(14) 0.0311(15) -0.0237(15) C25 0.0282(14) 0.0374(14) 0.0306(14) -0.0060(11) 0.0192(12) -0.0103(11) N1 0.0176(9) 0.0173(9) 0.0202(9) 0.0004(7) 0.0124(8) -0.0005(7) Si1 0.0204(3) 0.0174(3) 0.0211(3) 0.0019(2) 0.0133(3) 0.0021(2) C26 0.0275(13) 0.0201(11) 0.0301(13) 0.0004(9) 0.0184(11) 0.0011(10) C27 0.0379(15) 0.0313(13) 0.0263(13) 0.0037(11) 0.0189(12) 0.0001(11) C28 0.0307(14) 0.0213(12) 0.0537(17) 0.0016(12) 0.0278(14) 0.0061(10) N2 0.0185(9) 0.0166(9) 0.0230(10) 0.0009(7) 0.0132(8) -0.0008(7) Si2 0.0258(3) 0.0183(3) 0.0281(3) 0.0044(3) 0.0171(3) 0.0042(3) C29 0.0247(13) 0.0412(15) 0.0380(15) 0.0077(12) 0.0193(12) 0.0067(11) C30 0.0513(18) 0.0213(12) 0.0461(16) 0.0063(12) 0.0334(15) 0.0097(12) C31 0.0352(15) 0.0271(13) 0.0315(14) 0.0069(11) 0.0193(12) 0.0016(11) C32 0.0215(11) 0.0193(11) 0.0196(11) 0.0021(9) 0.0145(10) 0.0023(9) P3 0.0162(3) 0.0190(3) 0.0157(3) -0.0009(2) 0.0097(2) 0.0001(2) P4 0.0154(3) 0.0180(3) 0.0178(3) 0.0005(2) 0.0112(2) 0.0006(2) C33 0.0173(11) 0.0310(12) 0.0201(11) 0.0031(10) 0.0114(10) -0.0020(9) C34 0.0269(13) 0.0404(15) 0.0268(13) 0.0064(11) 0.0172(11) 0.0057(11) C35 0.0319(15) 0.0573(19) 0.0463(18) 0.0215(15) 0.0265(14) 0.0197(14) C36 0.0210(14) 0.083(2) 0.0312(16) 0.0201(16) 0.0099(12) 0.0068(15) C37 0.0291(16) 0.077(2) 0.0236(14) -0.0031(14) 0.0053(13) -0.0051(15) C38 0.0291(14) 0.0477(16) 0.0233(13) -0.0034(12) 0.0118(12) -0.0026(12) C39 0.0292(13) 0.0230(11) 0.0174(11) -0.0009(9) 0.0150(10) 0.0020(10) C40 0.0414(16) 0.0266(13) 0.0338(14) -0.0062(11) 0.0259(13) -0.0051(11) C41 0.069(2) 0.0226(13) 0.0407(16) -0.0074(12) 0.0342(17) -0.0055(13) C42 0.075(2) 0.0276(15) 0.0387(16) 0.0004(12) 0.0362(17) 0.0167(15) C43 0.0467(17) 0.0437(16) 0.0354(15) 0.0040(13) 0.0285(14) 0.0194(14) C44 0.0324(14) 0.0290(13) 0.0249(12) 0.0003(10) 0.0186(11) 0.0044(11) C45 0.0187(11) 0.0219(11) 0.0207(11) 0.0036(9) 0.0133(9) 0.0018(9) C46 0.0200(12) 0.0257(12) 0.0329(13) -0.0023(10) 0.0146(11) 0.0002(10) C47 0.0305(15) 0.0288(13) 0.0532(17) 0.0004(13) 0.0254(14) 0.0077(11) C48 0.0213(13) 0.0400(15) 0.0428(16) 0.0075(13) 0.0171(12) 0.0096(11) C49 0.0174(12) 0.0415(16) 0.0327(14) -0.0001(12) 0.0097(11) -0.0011(11) C50 0.0222(12) 0.0294(13) 0.0266(13) -0.0003(10) 0.0126(11) 0.0024(10) C51 0.0229(12) 0.0197(11) 0.0184(11) -0.0012(9) 0.0139(10) -0.0017(9) C52 0.0349(15) 0.0376(14) 0.0362(14) 0.0135(12) 0.0281(13) 0.0132(12) C53 0.0442(17) 0.0361(15) 0.0381(15) 0.0163(12) 0.0307(14) 0.0173(12) C54 0.0402(15) 0.0289(13) 0.0235(12) 0.0024(10) 0.0217(12) -0.0040(11) C55 0.0237(13) 0.0376(14) 0.0248(12) -0.0003(11) 0.0157(11) -0.0089(11) C56 0.0195(12) 0.0309(13) 0.0224(12) 0.0026(10) 0.0127(10) -0.0026(10) N3 0.0190(9) 0.0198(9) 0.0163(9) 0.0008(7) 0.0111(8) -0.0012(7) Si3 0.0216(3) 0.0275(3) 0.0192(3) 0.0038(3) 0.0135(3) 0.0003(3) C57 0.0282(14) 0.0479(17) 0.0319(14) 0.0082(12) 0.0182(12) -0.0058(12) C58 0.0380(16) 0.0438(16) 0.0385(15) 0.0199(13) 0.0265(14) 0.0125(13) C59 0.0562(19) 0.0491(17) 0.0323(15) -0.0013(13) 0.0347(15) -0.0028(14) N4 0.0180(9) 0.0202(9) 0.0196(9) -0.0011(7) 0.0135(8) -0.0004(7) Si4 0.0236(3) 0.0266(3) 0.0216(3) -0.0052(3) 0.0168(3) -0.0046(3) C60 0.0354(15) 0.0348(14) 0.0384(15) -0.0122(12) 0.0241(13) -0.0016(12) C61 0.0575(19) 0.0597(19) 0.0385(16) -0.0234(14) 0.0402(16) -0.0290(16) C62 0.0274(14) 0.0346(14) 0.0255(13) -0.0006(11) 0.0110(11) -0.0001(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 Gd1 C1 2.406(2) . ? Gd1 N3 2.4170(18) . ? Gd1 N4 2.4395(18) . ? Gd1 N1 2.4819(18) . ? Gd1 N2 2.5011(17) . ? Gd1 C32 2.923(2) . ? C1 P2 1.643(2) . ? C1 P1 1.643(2) . ? P1 N1 1.6285(18) . ? P1 C8 1.825(2) . ? P1 C2 1.834(2) . ? P2 N2 1.6236(19) . ? P2 C20 1.831(2) . ? P2 C14 1.835(2) . ? C2 C3 1.390(3) . ? C2 C7 1.398(3) . ? C3 C4 1.386(3) . ? C4 C5 1.381(4) . ? C5 C6 1.374(4) . ? C6 C7 1.385(3) . ? C8 C13 1.387(3) . ? C8 C9 1.392(3) . ? C9 C10 1.383(4) . ? C10 C11 1.379(4) . ? C11 C12 1.372(4) . ? C12 C13 1.392(4) . ? C14 C15 1.381(4) . ? C14 C19 1.396(4) . ? C15 C16 1.392(4) . ? C16 C17 1.374(5) . ? C17 C18 1.382(5) . ? C18 C19 1.387(4) . ? C20 C25 1.379(4) . ? C20 C21 1.400(3) . ? C21 C22 1.380(4) . ? C22 C23 1.368(4) . ? C23 C24 1.383(4) . ? C24 C25 1.393(4) . ? N1 Si1 1.7285(18) . ? Si1 C26 1.867(2) . ? Si1 C27 1.868(3) . ? Si1 C28 1.880(3) . ? N2 Si2 1.7122(19) . ? Si2 C29 1.870(3) . ? Si2 C30 1.874(3) . ? Si2 C31 1.878(3) . ? C32 P3 1.732(2) . ? C32 P4 1.737(2) . ? P3 N3 1.6093(18) . ? P3 C39 1.822(2) . ? P3 C33 1.822(2) . ? P4 N4 1.6053(18) . ? P4 C45 1.813(2) . ? P4 C51 1.819(2) . ? C33 C38 1.393(3) . ? C33 C34 1.394(3) . ? C34 C35 1.384(4) . ? C35 C36 1.378(4) . ? C36 C37 1.372(5) . ? C37 C38 1.386(4) . ? C39 C44 1.385(3) . ? C39 C40 1.398(3) . ? C40 C41 1.390(4) . ? C41 C42 1.375(5) . ? C42 C43 1.376(4) . ? C43 C44 1.389(3) . ? C45 C46 1.390(3) . ? C45 C50 1.392(3) . ? C46 C47 1.386(3) . ? C47 C48 1.376(4) . ? C48 C49 1.377(4) . ? C49 C50 1.388(3) . ? C51 C52 1.390(3) . ? C51 C56 1.390(3) . ? C52 C53 1.388(3) . ? C53 C54 1.380(4) . ? C54 C55 1.377(4) . ? C55 C56 1.388(3) . ? N3 Si3 1.7474(19) . ? Si3 C57 1.856(3) . ? Si3 C58 1.867(3) . ? Si3 C59 1.877(3) . ? N4 Si4 1.7360(19) . ? Si4 C62 1.859(3) . ? Si4 C60 1.863(3) . ? Si4 C61 1.867(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Gd1 N3 117.05(7) . . ? C1 Gd1 N4 130.94(7) . . ? N3 Gd1 N4 110.17(6) . . ? C1 Gd1 N1 65.12(7) . . ? N3 Gd1 N1 106.96(6) . . ? N4 Gd1 N1 113.28(6) . . ? C1 Gd1 N2 64.13(7) . . ? N3 Gd1 N2 103.58(6) . . ? N4 Gd1 N2 93.21(6) . . ? N1 Gd1 N2 128.38(6) . . ? C1 Gd1 C32 158.59(7) . . ? N3 Gd1 C32 61.38(6) . . ? N4 Gd1 C32 61.00(6) . . ? N1 Gd1 C32 94.30(6) . . ? N2 Gd1 C32 137.06(6) . . ? P2 C1 P1 164.06(16) . . ? P2 C1 Gd1 96.34(10) . . ? P1 C1 Gd1 95.03(10) . . ? N1 P1 C1 107.10(10) . . ? N1 P1 C8 110.26(10) . . ? C1 P1 C8 109.88(11) . . ? N1 P1 C2 112.10(10) . . ? C1 P1 C2 114.19(11) . . ? C8 P1 C2 103.29(11) . . ? N2 P2 C1 105.87(10) . . ? N2 P2 C20 112.12(10) . . ? C1 P2 C20 114.95(12) . . ? N2 P2 C14 112.37(11) . . ? C1 P2 C14 113.42(11) . . ? C20 P2 C14 98.28(11) . . ? C3 C2 C7 118.3(2) . . ? C3 C2 P1 117.47(17) . . ? C7 C2 P1 124.20(19) . . ? C4 C3 C2 121.0(2) . . ? C5 C4 C3 119.8(3) . . ? C6 C5 C4 120.0(2) . . ? C5 C6 C7 120.5(3) . . ? C6 C7 C2 120.3(3) . . ? C13 C8 C9 118.5(2) . . ? C13 C8 P1 120.91(19) . . ? C9 C8 P1 120.15(19) . . ? C10 C9 C8 120.7(3) . . ? C11 C10 C9 120.2(3) . . ? C12 C11 C10 119.9(3) . . ? C11 C12 C13 120.2(3) . . ? C8 C13 C12 120.5(3) . . ? C15 C14 C19 118.6(2) . . ? C15 C14 P2 123.6(2) . . ? C19 C14 P2 117.9(2) . . ? C14 C15 C16 120.8(3) . . ? C17 C16 C15 119.9(3) . . ? C16 C17 C18 120.2(3) . . ? C17 C18 C19 119.8(3) . . ? C18 C19 C14 120.6(3) . . ? C25 C20 C21 119.0(2) . . ? C25 C20 P2 120.77(19) . . ? C21 C20 P2 120.21(19) . . ? C22 C21 C20 120.7(3) . . ? C23 C22 C21 119.8(3) . . ? C22 C23 C24 120.6(3) . . ? C23 C24 C25 119.9(3) . . ? C20 C25 C24 120.1(3) . . ? P1 N1 Si1 125.50(11) . . ? P1 N1 Gd1 92.62(8) . . ? Si1 N1 Gd1 140.28(10) . . ? N1 Si1 C26 112.58(10) . . ? N1 Si1 C27 111.07(10) . . ? C26 Si1 C27 107.40(12) . . ? N1 Si1 C28 114.34(11) . . ? C26 Si1 C28 104.13(11) . . ? C27 Si1 C28 106.78(13) . . ? P2 N2 Si2 134.09(12) . . ? P2 N2 Gd1 93.32(8) . . ? Si2 N2 Gd1 129.07(9) . . ? N2 Si2 C29 106.54(11) . . ? N2 Si2 C30 114.25(11) . . ? C29 Si2 C30 107.97(13) . . ? N2 Si2 C31 115.35(11) . . ? C29 Si2 C31 106.62(12) . . ? C30 Si2 C31 105.67(12) . . ? P3 C32 P4 138.55(14) . . ? P3 C32 Gd1 82.70(8) . . ? P4 C32 Gd1 83.62(8) . . ? N3 P3 C32 111.36(10) . . ? N3 P3 C39 111.95(11) . . ? C32 P3 C39 102.23(10) . . ? N3 P3 C33 109.06(10) . . ? C32 P3 C33 116.28(11) . . ? C39 P3 C33 105.70(11) . . ? N4 P4 C32 110.86(10) . . ? N4 P4 C45 112.20(10) . . ? C32 P4 C45 114.45(10) . . ? N4 P4 C51 111.27(10) . . ? C32 P4 C51 104.10(10) . . ? C45 P4 C51 103.41(10) . . ? C38 C33 C34 118.3(2) . . ? C38 C33 P3 123.70(19) . . ? C34 C33 P3 117.84(18) . . ? C35 C34 C33 120.7(3) . . ? C36 C35 C34 120.3(3) . . ? C37 C36 C35 119.7(3) . . ? C36 C37 C38 120.6(3) . . ? C37 C38 C33 120.4(3) . . ? C44 C39 C40 118.9(2) . . ? C44 C39 P3 118.94(18) . . ? C40 C39 P3 122.0(2) . . ? C41 C40 C39 120.0(3) . . ? C42 C41 C40 120.2(3) . . ? C41 C42 C43 120.3(3) . . ? C42 C43 C44 119.9(3) . . ? C39 C44 C43 120.6(3) . . ? C46 C45 C50 118.7(2) . . ? C46 C45 P4 120.56(17) . . ? C50 C45 P4 120.56(17) . . ? C47 C46 C45 120.6(2) . . ? C48 C47 C46 120.1(2) . . ? C47 C48 C49 120.0(2) . . ? C48 C49 C50 120.2(2) . . ? C49 C50 C45 120.3(2) . . ? C52 C51 C56 118.3(2) . . ? C52 C51 P4 117.60(18) . . ? C56 C51 P4 123.94(18) . . ? C53 C52 C51 121.0(2) . . ? C54 C53 C52 119.8(2) . . ? C55 C54 C53 120.0(2) . . ? C54 C55 C56 120.2(2) . . ? C55 C56 C51 120.7(2) . . ? P3 N3 Si3 125.53(11) . . ? P3 N3 Gd1 103.56(9) . . ? Si3 N3 Gd1 130.81(9) . . ? N3 Si3 C57 106.65(10) . . ? N3 Si3 C58 112.11(11) . . ? C57 Si3 C58 111.11(13) . . ? N3 Si3 C59 114.97(11) . . ? C57 Si3 C59 106.85(14) . . ? C58 Si3 C59 105.09(13) . . ? P4 N4 Si4 129.88(11) . . ? P4 N4 Gd1 104.08(8) . . ? Si4 N4 Gd1 123.29(9) . . ? N4 Si4 C62 106.02(11) . . ? N4 Si4 C60 111.51(11) . . ? C62 Si4 C60 107.80(12) . . ? N4 Si4 C61 115.79(11) . . ? C62 Si4 C61 108.62(14) . . ? C60 Si4 C61 106.84(14) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.808 _refine_diff_density_min -0.420 _refine_diff_density_rms 0.074 # Attachment '19.cif' data_19 _database_code_depnum_ccdc_archive 'CCDC 736115' _refine_special_details ; THF molecule is disordered over the crystallographic mirror plane. Modelled in two parts with distance, simialrity and ADP restraints. ; _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H53 Er N2 O P2 Si2' _chemical_formula_sum 'C42 H53 Er N2 O P2 Si2' _chemical_formula_weight 887.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 10.4181(4) _cell_length_b 19.2561(8) _cell_length_c 10.6622(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.416(2) _cell_angle_gamma 90.00 _cell_volume 2135.16(14) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3496 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 25.65 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.380 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 906 _exptl_absorpt_coefficient_mu 2.129 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.54 _exptl_absorpt_correction_T_max 0.72 _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 5626 _diffrn_reflns_av_R_equivalents 0.0216 _diffrn_reflns_av_sigmaI/netI 0.0451 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2117 _reflns_number_gt 2074 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36A (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; SHELXTL (Sheldrick, 2008)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'enCIFer (Allen et al., 2004); PLATON (Spek, 2003)' _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^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom, Me from difmap' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2117 _refine_ls_number_parameters 268 _refine_ls_number_restraints 180 _refine_ls_R_factor_all 0.0186 _refine_ls_R_factor_gt 0.0183 _refine_ls_wR_factor_ref 0.0469 _refine_ls_wR_factor_gt 0.0468 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Er1 Er 0.727141(18) 0.7500 0.601443(18) 0.02033(8) Uani 1 2 d S . . C1 C 0.8141(4) 0.7500 0.8088(4) 0.0212(9) Uani 1 2 d S . . P1 P 0.85723(7) 0.83254(3) 0.79801(8) 0.01948(17) Uani 1 1 d . . . C2 C 0.7895(3) 0.88322(13) 0.9225(3) 0.0216(6) Uani 1 1 d . A . C3 C 0.8491(3) 0.93863(14) 0.9821(3) 0.0319(8) Uani 1 1 d . . . H3 H 0.9325 0.9519 0.9598 0.038 Uiso 1 1 calc R A . C4 C 0.7897(4) 0.97607(17) 1.0750(4) 0.0380(9) Uani 1 1 d . A . H4 H 0.8339 1.0129 1.1182 0.046 Uiso 1 1 calc R . . C5 C 0.6658(3) 0.95880(17) 1.1033(4) 0.0358(8) Uani 1 1 d . . . H5 H 0.6230 0.9852 1.1635 0.043 Uiso 1 1 calc R A . C6 C 0.6040(3) 0.90319(17) 1.0440(3) 0.0360(8) Uani 1 1 d . A . H6 H 0.5194 0.8911 1.0644 0.043 Uiso 1 1 calc R . . C7 C 0.6650(3) 0.86530(15) 0.9553(4) 0.0313(8) Uani 1 1 d . . . H7 H 0.6225 0.8267 0.9161 0.038 Uiso 1 1 calc R A . C8 C 1.0307(3) 0.84744(13) 0.8164(3) 0.0243(7) Uani 1 1 d . A . C9 C 1.0980(3) 0.86041(16) 0.7106(4) 0.0326(8) Uani 1 1 d . . . H9 H 1.0528 0.8664 0.6314 0.039 Uiso 1 1 calc R A . C10 C 1.2321(3) 0.86467(18) 0.7201(4) 0.0411(10) Uani 1 1 d . A . H10 H 1.2780 0.8734 0.6474 0.049 Uiso 1 1 calc R . . C11 C 1.2972(3) 0.85618(17) 0.8350(4) 0.0421(10) Uani 1 1 d . . . H11 H 1.3884 0.8587 0.8415 0.050 Uiso 1 1 calc R A . C12 C 1.2310(4) 0.84409(17) 0.9406(5) 0.0428(10) Uani 1 1 d . A . H12 H 1.2761 0.8394 1.0202 0.051 Uiso 1 1 calc R . . C13 C 1.0960(3) 0.83878(15) 0.9301(4) 0.0341(9) Uani 1 1 d . . . H13 H 1.0502 0.8291 1.0025 0.041 Uiso 1 1 calc R A . N1 N 0.8010(2) 0.85994(11) 0.6617(2) 0.0205(5) Uani 1 1 d . A . Si1 Si 0.76089(9) 0.94218(4) 0.60972(9) 0.0253(2) Uani 1 1 d . . . C14 C 0.6059(3) 0.97245(16) 0.6702(4) 0.0404(9) Uani 1 1 d . A . H14A H 0.5389 0.9377 0.6508 0.061 Uiso 1 1 calc R . . H14B H 0.5810 1.0167 0.6303 0.061 Uiso 1 1 calc R . . H14C H 0.6166 0.9789 0.7615 0.061 Uiso 1 1 calc R . . C15 C 0.8859(4) 1.00963(15) 0.6551(4) 0.0441(10) Uani 1 1 d . A . H15A H 0.8853 1.0189 0.7455 0.066 Uiso 1 1 calc R . . H15B H 0.8667 1.0526 0.6083 0.066 Uiso 1 1 calc R . . H15C H 0.9710 0.9925 0.6352 0.066 Uiso 1 1 calc R . . C16 C 0.7415(4) 0.93790(18) 0.4345(4) 0.0420(9) Uani 1 1 d . A . H16A H 0.8199 0.9187 0.4015 0.063 Uiso 1 1 calc R . . H16B H 0.7264 0.9847 0.4007 0.063 Uiso 1 1 calc R . . H16C H 0.6682 0.9080 0.4096 0.063 Uiso 1 1 calc R . . C17 C 0.5013(4) 0.7500 0.6237(5) 0.0388(12) Uani 1 2 d S A . H17A H 0.4735 0.7080 0.6684 0.047 Uiso 0.50 1 calc PR . . H17B H 0.4735 0.7920 0.6684 0.047 Uiso 0.50 1 calc PR . . C18 C 0.4535(5) 0.7500 0.4939(5) 0.0359(11) Uani 1 2 d S . . C19 C 0.4337(4) 0.81177(17) 0.4242(4) 0.0444(9) Uani 1 1 d . A . H19 H 0.4459 0.8551 0.4658 0.053 Uiso 1 1 calc R . . C20 C 0.3975(6) 0.81137(19) 0.2986(4) 0.0682(15) Uani 1 1 d . . . H20 H 0.3827 0.8541 0.2557 0.082 Uiso 1 1 calc R A . C21 C 0.3822(9) 0.7500 0.2338(6) 0.085(3) Uani 1 2 d S . . H21 H 0.3615 0.7500 0.1458 0.102 Uiso 1 2 calc SR . . O1 O 0.8139(3) 0.7500 0.4039(3) 0.0386(8) Uani 0.50 2 d SPDU A 1 C22 C 0.7521(5) 0.7500 0.2798(4) 0.0448(11) Uani 0.50 2 d SPDU A 1 H22C H 0.6828 0.7852 0.2727 0.054 Uiso 0.25 1 calc PR A 1 H22D H 0.7149 0.7038 0.2589 0.054 Uiso 0.25 1 calc PR A 1 C23 C 0.8576(19) 0.768(2) 0.195(2) 0.049(2) Uani 0.25 1 d PDU A 1 H23C H 0.8654 0.8185 0.1847 0.058 Uiso 0.25 1 calc PR A 1 H23D H 0.8404 0.7464 0.1107 0.058 Uiso 0.25 1 calc PR A 1 C24 C 0.979(2) 0.7374(18) 0.2595(10) 0.055(3) Uani 0.25 1 d PDU A 1 H24C H 1.0573 0.7627 0.2361 0.067 Uiso 0.25 1 calc PR A 1 H24D H 0.9890 0.6874 0.2410 0.067 Uiso 0.25 1 calc PR A 1 C25 C 0.9511(4) 0.7500 0.3963(5) 0.0590(13) Uani 0.50 2 d SPDU A 1 H25C H 0.9903 0.7129 0.4503 0.071 Uiso 0.25 1 calc PR A 1 H25D H 0.9873 0.7952 0.4251 0.071 Uiso 0.25 1 calc PR A 1 O1A O 0.8139(3) 0.7500 0.4039(3) 0.0386(8) Uani 0.50 2 d SPDU A 2 C22A C 0.7521(5) 0.7500 0.2798(4) 0.0448(11) Uani 0.50 2 d SPDU A 2 H22A H 0.7074 0.7948 0.2634 0.054 Uiso 0.25 1 calc PR A 2 H22B H 0.6877 0.7122 0.2719 0.054 Uiso 0.25 1 calc PR A 2 C23A C 0.8536(19) 0.739(3) 0.187(2) 0.050(3) Uani 0.25 1 d PDU A 2 H23A H 0.8314 0.7623 0.1053 0.060 Uiso 0.25 1 calc PR A 2 H23B H 0.8727 0.6897 0.1735 0.060 Uiso 0.25 1 calc PR A 2 C24A C 0.962(3) 0.7765(15) 0.2623(12) 0.055(3) Uani 0.25 1 d PDU A 2 H24A H 0.9503 0.8275 0.2582 0.066 Uiso 0.25 1 calc PR A 2 H24B H 1.0465 0.7645 0.2307 0.066 Uiso 0.25 1 calc PR A 2 C25A C 0.9511(4) 0.7500 0.3963(5) 0.0590(13) Uani 0.50 2 d SPDU A 2 H25A H 0.9876 0.7028 0.4073 0.071 Uiso 0.25 1 calc PR A 2 H25B H 0.9937 0.7817 0.4589 0.071 Uiso 0.25 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Er1 0.01971(11) 0.02301(10) 0.01807(13) 0.000 -0.00044(9) 0.000 C1 0.018(2) 0.0224(17) 0.023(2) 0.000 0.002(2) 0.000 P1 0.0187(4) 0.0192(3) 0.0203(4) -0.0008(3) -0.0006(4) 0.0003(3) C2 0.0220(15) 0.0219(12) 0.0212(16) 0.0013(12) 0.0033(15) 0.0013(11) C3 0.0328(18) 0.0282(14) 0.036(2) -0.0076(14) 0.0099(18) -0.0046(13) C4 0.041(2) 0.0335(15) 0.040(2) -0.0136(16) 0.0090(19) -0.0043(15) C5 0.038(2) 0.0406(17) 0.029(2) -0.0061(16) 0.0104(18) 0.0066(16) C6 0.0245(16) 0.0500(18) 0.034(2) -0.0044(17) 0.0084(17) 0.0014(15) C7 0.0282(17) 0.0352(15) 0.030(2) -0.0099(15) 0.0025(17) -0.0043(13) C8 0.0200(16) 0.0191(12) 0.033(2) -0.0040(12) -0.0029(17) 0.0005(11) C9 0.0244(17) 0.0429(16) 0.031(2) -0.0094(16) 0.0051(17) -0.0011(14) C10 0.0231(18) 0.0510(19) 0.050(3) -0.0132(19) 0.008(2) -0.0002(15) C11 0.0186(16) 0.0402(17) 0.067(3) -0.0110(19) -0.002(2) 0.0039(13) C12 0.028(2) 0.0436(19) 0.054(3) 0.0040(19) -0.016(2) 0.0000(14) C13 0.0287(18) 0.0330(16) 0.040(2) 0.0051(15) -0.0040(19) -0.0050(13) N1 0.0186(12) 0.0218(11) 0.0213(14) 0.0035(10) 0.0016(13) 0.0002(9) Si1 0.0257(4) 0.0226(4) 0.0275(5) 0.0061(3) 0.0008(4) 0.0004(3) C14 0.039(2) 0.0340(15) 0.048(2) 0.0029(16) 0.004(2) 0.0133(15) C15 0.049(2) 0.0265(14) 0.056(3) 0.0075(16) -0.007(2) -0.0063(15) C16 0.052(2) 0.0407(17) 0.033(2) 0.0127(16) -0.002(2) 0.0013(16) C17 0.022(2) 0.054(3) 0.040(3) 0.000 0.001(2) 0.000 C18 0.026(2) 0.042(2) 0.041(3) 0.000 0.008(2) 0.000 C19 0.059(2) 0.0327(17) 0.042(2) -0.0022(17) 0.005(2) 0.0005(17) C20 0.121(4) 0.036(2) 0.046(3) 0.0066(19) -0.004(3) 0.005(2) C21 0.171(9) 0.053(3) 0.028(3) 0.000 -0.015(5) 0.000 O1 0.0314(16) 0.0652(18) 0.0199(16) 0.000 0.0059(16) 0.000 C22 0.043(2) 0.065(3) 0.027(2) 0.000 0.003(2) 0.000 C23 0.054(4) 0.070(5) 0.023(4) 0.003(5) 0.009(4) 0.003(5) C24 0.044(4) 0.090(6) 0.034(4) 0.003(5) 0.016(4) 0.003(5) C25 0.041(2) 0.104(3) 0.033(2) 0.000 0.008(2) 0.000 O1A 0.0314(16) 0.0652(18) 0.0199(16) 0.000 0.0059(16) 0.000 C22A 0.043(2) 0.065(3) 0.027(2) 0.000 0.003(2) 0.000 C23A 0.053(4) 0.072(5) 0.026(4) 0.000(5) 0.006(4) 0.000(5) C24A 0.046(4) 0.087(5) 0.035(4) 0.001(5) 0.015(4) -0.002(5) C25A 0.041(2) 0.104(3) 0.033(2) 0.000 0.008(2) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Er1 N1 2.330(2) . ? Er1 N1 2.330(2) 4_575 ? Er1 C1 2.339(4) . ? Er1 O1 2.341(3) . ? Er1 C17 2.379(5) . ? C1 P1 1.6575(14) . ? C1 P1 1.6575(14) 4_575 ? P1 N1 1.623(3) . ? P1 C2 1.823(3) . ? P1 C8 1.829(3) . ? C2 C3 1.371(4) . ? C2 C7 1.406(5) . ? C3 C4 1.399(5) . ? C4 C5 1.383(5) . ? C5 C6 1.382(5) . ? C6 C7 1.379(5) . ? C8 C13 1.365(5) . ? C8 C9 1.385(5) . ? C9 C10 1.396(5) . ? C10 C11 1.374(6) . ? C11 C12 1.375(7) . ? C12 C13 1.408(5) . ? N1 Si1 1.721(2) . ? Si1 C14 1.867(4) . ? Si1 C16 1.869(4) . ? Si1 C15 1.882(3) . ? C17 C18 1.443(7) . ? C18 C19 1.411(5) 4_575 ? C18 C19 1.411(5) . ? C19 C20 1.370(6) . ? C20 C21 1.373(5) . ? C21 C20 1.373(5) 4_575 ? O1 C22 1.436(3) . ? O1 C25 1.437(3) . ? C22 C23 1.505(5) . ? C23 C24 1.524(5) . ? C24 C25 1.525(5) . ? C23A C24A 1.524(5) . ? 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 Er1 N1 130.66(12) . 4_575 ? N1 Er1 C1 68.68(7) . . ? N1 Er1 C1 68.68(7) 4_575 . ? N1 Er1 O1 96.27(7) . . ? N1 Er1 O1 96.27(7) 4_575 . ? C1 Er1 O1 134.60(12) . . ? N1 Er1 C17 106.55(8) . . ? N1 Er1 C17 106.55(8) 4_575 . ? C1 Er1 C17 103.61(17) . . ? O1 Er1 C17 121.80(15) . . ? P1 C1 P1 147.0(3) . 4_575 ? P1 C1 Er1 91.45(16) . . ? P1 C1 Er1 91.45(16) 4_575 . ? N1 P1 C1 106.83(17) . . ? N1 P1 C2 110.08(13) . . ? C1 P1 C2 110.14(18) . . ? N1 P1 C8 110.27(15) . . ? C1 P1 C8 114.41(16) . . ? C2 P1 C8 105.13(14) . . ? C3 C2 C7 118.3(3) . . ? C3 C2 P1 124.8(2) . . ? C7 C2 P1 116.9(2) . . ? C2 C3 C4 121.5(3) . . ? C5 C4 C3 119.2(3) . . ? C6 C5 C4 120.1(3) . . ? C7 C6 C5 120.2(3) . . ? C6 C7 C2 120.7(3) . . ? C13 C8 C9 119.7(3) . . ? C13 C8 P1 120.9(3) . . ? C9 C8 P1 119.1(3) . . ? C8 C9 C10 120.3(4) . . ? C11 C10 C9 119.7(4) . . ? C10 C11 C12 120.3(3) . . ? C11 C12 C13 119.6(4) . . ? C8 C13 C12 120.3(4) . . ? P1 N1 Si1 130.95(15) . . ? P1 N1 Er1 92.69(9) . . ? Si1 N1 Er1 132.65(13) . . ? N1 Si1 C14 111.99(14) . . ? N1 Si1 C16 106.91(14) . . ? C14 Si1 C16 108.38(19) . . ? N1 Si1 C15 113.64(14) . . ? C14 Si1 C15 107.16(17) . . ? C16 Si1 C15 108.63(19) . . ? C18 C17 Er1 101.0(3) . . ? C19 C18 C19 114.9(5) 4_575 . ? C19 C18 C17 122.4(3) 4_575 . ? C19 C18 C17 122.4(3) . . ? C20 C19 C18 122.2(4) . . ? C19 C20 C21 120.9(4) . . ? C20 C21 C20 118.7(6) 4_575 . ? C22 O1 C25 109.9(4) . . ? C22 O1 Er1 130.8(3) . . ? C25 O1 Er1 119.3(3) . . ? O1 C22 C23 104.6(12) . . ? C22 C23 C24 105.0(14) . . ? C23 C24 C25 99.8(16) . . ? O1 C25 C24 107.7(9) . . ? _diffrn_measured_fraction_theta_max 0.544 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.544 _refine_diff_density_max 0.429 _refine_diff_density_min -0.320 _refine_diff_density_rms 0.050 # Attachment '2.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 736116' _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H45 Ce O3' _chemical_formula_sum 'C33 H45 Ce O3' _chemical_formula_weight 629.81 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.1283(4) _cell_length_b 10.4797(3) _cell_length_c 20.7200(6) _cell_angle_alpha 90.00 _cell_angle_beta 101.182(2) _cell_angle_gamma 90.00 _cell_volume 3009.57(15) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 11467 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 27.53 _exptl_crystal_description column _exptl_crystal_colour orange _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.390 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1300 _exptl_absorpt_coefficient_mu 1.542 _exptl_absorpt_correction_type multi-scaN _exptl_absorpt_correction_T_min 0.56 _exptl_absorpt_correction_T_max 0.73 _exptl_absorpt_process_details '(SADABS; Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 18876 _diffrn_reflns_av_R_equivalents 0.0174 _diffrn_reflns_av_sigmaI/netI 0.0210 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 27.53 _reflns_number_total 6883 _reflns_number_gt 5972 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'enCIFer(Allen et al.,2004);PLATON(Spek,2003)' _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^)+(0.0264P)^2^+2.3150P] 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 6883 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0286 _refine_ls_R_factor_gt 0.0219 _refine_ls_wR_factor_ref 0.0566 _refine_ls_wR_factor_gt 0.0525 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 Ce1 Ce 0.230275(8) 0.096462(10) 0.152116(5) 0.01903(4) Uani 1 1 d . . . O1 O 0.27243(11) 0.25603(14) 0.06309(7) 0.0272(3) Uani 1 1 d . . . O2 O 0.28025(10) 0.30935(14) 0.21620(7) 0.0256(3) Uani 1 1 d . . . O3 O 0.07849(10) 0.24835(13) 0.11891(7) 0.0254(3) Uani 1 1 d . . . C1 C 0.13534(15) -0.0162(2) 0.04757(11) 0.0280(4) Uani 1 1 d . . . H1A H 0.0835 -0.0730 0.0566 0.034 Uiso 1 1 calc R . . H1B H 0.1102 0.0436 0.0113 0.034 Uiso 1 1 calc R . . C2 C 0.22063(16) -0.08364(19) 0.03850(10) 0.0259(4) Uani 1 1 d . . . C3 C 0.28052(17) -0.0394(2) -0.00440(11) 0.0306(5) Uani 1 1 d . . . H3A H 0.2607 0.0330 -0.0312 0.037 Uiso 1 1 calc R . . C4 C 0.36675(19) -0.0981(3) -0.00859(12) 0.0405(6) Uani 1 1 d . . . H4A H 0.4046 -0.0661 -0.0382 0.049 Uiso 1 1 calc R . . C5 C 0.39848(19) -0.2039(3) 0.03036(13) 0.0440(6) Uani 1 1 d . . . H5A H 0.4578 -0.2441 0.0277 0.053 Uiso 1 1 calc R . . C6 C 0.34215(19) -0.2494(2) 0.07300(12) 0.0386(6) Uani 1 1 d . . . H6A H 0.3632 -0.3215 0.0997 0.046 Uiso 1 1 calc R . . C7 C 0.25511(17) -0.1911(2) 0.07729(11) 0.0308(5) Uani 1 1 d . . . H7A H 0.2179 -0.2244 0.1070 0.037 Uiso 1 1 calc R . . C8 C 0.16293(16) 0.0582(2) 0.25930(11) 0.0266(4) Uani 1 1 d . . . H8A H 0.2113 0.0235 0.2962 0.032 Uiso 1 1 calc R . . H8B H 0.1299 0.1335 0.2735 0.032 Uiso 1 1 calc R . . C9 C 0.09788(15) -0.0365(2) 0.22552(10) 0.0254(4) Uani 1 1 d . . . C10 C 0.12559(16) -0.1650(2) 0.21924(11) 0.0297(5) Uani 1 1 d . . . H10A H 0.1874 -0.1922 0.2417 0.036 Uiso 1 1 calc R . . C11 C 0.06519(18) -0.2523(2) 0.18127(12) 0.0356(5) Uani 1 1 d . . . H11A H 0.0857 -0.3383 0.1793 0.043 Uiso 1 1 calc R . . C12 C -0.02428(18) -0.2165(2) 0.14625(12) 0.0369(5) Uani 1 1 d . . . H12A H -0.0645 -0.2760 0.1192 0.044 Uiso 1 1 calc R . . C13 C -0.05390(17) -0.0911(2) 0.15155(12) 0.0356(5) Uani 1 1 d . . . H13A H -0.1155 -0.0650 0.1282 0.043 Uiso 1 1 calc R . . C14 C 0.00482(16) -0.0038(2) 0.19024(11) 0.0306(5) Uani 1 1 d . . . H14A H -0.0179 0.0809 0.1933 0.037 Uiso 1 1 calc R . . C15 C 0.41629(15) 0.0610(2) 0.16591(11) 0.0278(4) Uani 1 1 d . . . H15A H 0.4342 -0.0039 0.1357 0.033 Uiso 1 1 calc R . . H15B H 0.4533 0.1408 0.1644 0.033 Uiso 1 1 calc R . . C16 C 0.41827(14) 0.0146(2) 0.23133(10) 0.0239(4) Uani 1 1 d . . . C17 C 0.44208(15) 0.0959(2) 0.28684(11) 0.0273(4) Uani 1 1 d . . . H17A H 0.4624 0.1807 0.2807 0.033 Uiso 1 1 calc R . . C18 C 0.43671(17) 0.0559(2) 0.34920(11) 0.0316(5) Uani 1 1 d . . . H18A H 0.4539 0.1134 0.3850 0.038 Uiso 1 1 calc R . . C19 C 0.40664(16) -0.0673(2) 0.36116(11) 0.0298(5) Uani 1 1 d . . . H19A H 0.4025 -0.0940 0.4043 0.036 Uiso 1 1 calc R . . C20 C 0.38306(16) -0.1493(2) 0.30801(11) 0.0287(5) Uani 1 1 d . . . H20A H 0.3631 -0.2339 0.3150 0.034 Uiso 1 1 calc R . . C21 C 0.38812(15) -0.1101(2) 0.24471(11) 0.0260(4) Uani 1 1 d . . . H21A H 0.3709 -0.1686 0.2093 0.031 Uiso 1 1 calc R . . C22 C 0.36869(16) 0.2786(2) 0.05020(12) 0.0343(5) Uani 1 1 d . . . H22A H 0.3912 0.2041 0.0279 0.041 Uiso 1 1 calc R . . H22B H 0.4151 0.2948 0.0917 0.041 Uiso 1 1 calc R . . C23 C 0.3593(2) 0.3940(3) 0.00647(18) 0.0664(10) Uani 1 1 d . . . H23A H 0.3700 0.4733 0.0329 0.080 Uiso 1 1 calc R . . H23B H 0.4062 0.3907 -0.0233 0.080 Uiso 1 1 calc R . . C24 C 0.2611(2) 0.3879(4) -0.03047(18) 0.0721(11) Uani 1 1 d . . . H24A H 0.2582 0.3378 -0.0713 0.086 Uiso 1 1 calc R . . H24B H 0.2359 0.4746 -0.0424 0.086 Uiso 1 1 calc R . . C25 C 0.20334(18) 0.3238(3) 0.01421(12) 0.0396(6) Uani 1 1 d . . . H25A H 0.1681 0.3880 0.0355 0.048 Uiso 1 1 calc R . . H25B H 0.1561 0.2637 -0.0110 0.048 Uiso 1 1 calc R . . C26 C 0.32843(18) 0.4190(2) 0.19391(12) 0.0311(5) Uani 1 1 d . . . H26A H 0.2965 0.4438 0.1488 0.037 Uiso 1 1 calc R . . H26B H 0.3969 0.3991 0.1939 0.037 Uiso 1 1 calc R . . C27 C 0.32063(18) 0.5249(2) 0.24197(13) 0.0371(6) Uani 1 1 d . . . H27A H 0.2582 0.5704 0.2302 0.045 Uiso 1 1 calc R . . H27B H 0.3741 0.5870 0.2446 0.045 Uiso 1 1 calc R . . C28 C 0.32784(19) 0.4505(3) 0.30601(13) 0.0420(6) Uani 1 1 d . . . H28A H 0.3957 0.4291 0.3253 0.050 Uiso 1 1 calc R . . H28B H 0.2996 0.4991 0.3386 0.050 Uiso 1 1 calc R . . C29 C 0.26978(16) 0.3322(2) 0.28391(11) 0.0307(5) Uani 1 1 d . . . H29A H 0.2946 0.2586 0.3122 0.037 Uiso 1 1 calc R . . H29B H 0.2011 0.3454 0.2861 0.037 Uiso 1 1 calc R . . C30 C 0.05972(17) 0.3622(2) 0.15441(12) 0.0330(5) Uani 1 1 d . . . H30A H 0.1143 0.4228 0.1582 0.040 Uiso 1 1 calc R . . H30B H 0.0504 0.3399 0.1992 0.040 Uiso 1 1 calc R . . C31 C -0.03128(17) 0.4207(2) 0.11483(12) 0.0341(5) Uani 1 1 d . . . H31A H -0.0170 0.4762 0.0792 0.041 Uiso 1 1 calc R . . H31B H -0.0668 0.4704 0.1431 0.041 Uiso 1 1 calc R . . C32 C -0.08699(16) 0.3020(2) 0.08739(12) 0.0354(5) Uani 1 1 d . . . H32A H -0.1181 0.2605 0.1209 0.042 Uiso 1 1 calc R . . H32B H -0.1368 0.3223 0.0481 0.042 Uiso 1 1 calc R . . C33 C -0.00796(15) 0.2189(2) 0.06971(11) 0.0276(4) Uani 1 1 d . . . H33A H -0.0248 0.1274 0.0715 0.033 Uiso 1 1 calc R . . H33B H 0.0024 0.2390 0.0249 0.033 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 Ce1 0.01836(6) 0.01877(6) 0.01947(6) -0.00245(4) 0.00247(4) -0.00024(4) O1 0.0260(8) 0.0312(8) 0.0243(7) 0.0049(6) 0.0046(6) 0.0001(6) O2 0.0267(7) 0.0243(7) 0.0265(7) -0.0069(6) 0.0065(6) -0.0049(6) O3 0.0218(7) 0.0247(7) 0.0282(8) -0.0084(6) 0.0009(6) 0.0033(6) C1 0.0256(11) 0.0277(10) 0.0291(11) -0.0094(9) 0.0013(8) -0.0006(9) C2 0.0288(11) 0.0254(10) 0.0216(10) -0.0091(8) 0.0001(8) -0.0001(8) C3 0.0339(12) 0.0334(11) 0.0224(10) -0.0009(9) 0.0007(9) 0.0071(10) C4 0.0409(14) 0.0549(16) 0.0280(12) 0.0029(11) 0.0124(10) 0.0121(12) C5 0.0430(14) 0.0532(16) 0.0373(13) 0.0003(12) 0.0116(11) 0.0235(13) C6 0.0484(15) 0.0334(12) 0.0330(13) 0.0012(10) 0.0055(11) 0.0142(11) C7 0.0363(12) 0.0296(11) 0.0261(11) -0.0036(9) 0.0054(9) 0.0012(9) C8 0.0277(11) 0.0265(10) 0.0270(11) -0.0009(9) 0.0083(9) -0.0016(9) C9 0.0238(10) 0.0273(10) 0.0270(11) 0.0028(9) 0.0095(8) -0.0022(8) C10 0.0258(11) 0.0299(11) 0.0326(12) -0.0004(9) 0.0043(9) -0.0008(9) C11 0.0376(13) 0.0289(11) 0.0400(13) -0.0021(10) 0.0073(10) -0.0064(10) C12 0.0360(13) 0.0408(13) 0.0328(12) 0.0001(11) 0.0035(10) -0.0159(11) C13 0.0223(11) 0.0485(14) 0.0350(12) 0.0114(11) 0.0028(9) -0.0051(10) C14 0.0268(11) 0.0315(11) 0.0352(12) 0.0068(10) 0.0099(9) -0.0003(9) C15 0.0214(10) 0.0330(11) 0.0288(11) 0.0026(9) 0.0042(8) 0.0034(9) C16 0.0167(9) 0.0265(10) 0.0272(10) -0.0009(8) 0.0013(8) 0.0044(8) C17 0.0234(10) 0.0256(10) 0.0319(11) -0.0022(9) 0.0033(9) -0.0016(8) C18 0.0310(12) 0.0323(11) 0.0297(11) -0.0090(9) 0.0013(9) -0.0007(9) C19 0.0304(12) 0.0353(12) 0.0230(10) 0.0018(9) 0.0032(9) 0.0040(9) C20 0.0281(11) 0.0247(10) 0.0319(12) 0.0014(9) 0.0020(9) 0.0022(9) C21 0.0254(10) 0.0251(10) 0.0262(10) -0.0066(8) 0.0016(8) 0.0030(8) C22 0.0288(12) 0.0396(13) 0.0369(12) 0.0089(11) 0.0126(10) 0.0035(10) C23 0.0485(18) 0.083(2) 0.074(2) 0.0463(19) 0.0268(16) 0.0154(16) C24 0.0434(17) 0.104(3) 0.066(2) 0.056(2) 0.0032(15) -0.0039(17) C25 0.0324(13) 0.0497(15) 0.0352(13) 0.0152(11) 0.0025(10) 0.0029(11) C26 0.0346(12) 0.0249(10) 0.0355(12) -0.0058(9) 0.0110(10) -0.0070(9) C27 0.0335(12) 0.0278(11) 0.0516(15) -0.0145(11) 0.0123(11) -0.0061(10) C28 0.0397(14) 0.0491(15) 0.0387(14) -0.0204(12) 0.0111(11) -0.0155(12) C29 0.0289(11) 0.0368(12) 0.0270(11) -0.0091(9) 0.0071(9) -0.0040(9) C30 0.0298(12) 0.0301(11) 0.0365(12) -0.0142(10) 0.0001(10) 0.0064(9) C31 0.0343(12) 0.0298(11) 0.0363(13) -0.0064(10) 0.0017(10) 0.0108(10) C32 0.0242(11) 0.0395(13) 0.0399(13) -0.0071(11) 0.0001(9) 0.0052(10) C33 0.0231(10) 0.0282(10) 0.0287(11) -0.0071(9) -0.0015(8) -0.0010(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ce1 C1 2.600(2) . ? Ce1 C8 2.611(2) . ? Ce1 C15 2.614(2) . ? Ce1 O2 2.6222(14) . ? Ce1 O1 2.6419(14) . ? Ce1 O3 2.6521(14) . ? Ce1 C16 2.9654(19) . ? Ce1 C9 2.976(2) . ? Ce1 C2 3.000(2) . ? O1 C25 1.449(3) . ? O1 C22 1.455(3) . ? O2 C26 1.455(3) . ? O2 C29 1.459(2) . ? O3 C30 1.453(2) . ? O3 C33 1.464(2) . ? C1 C2 1.441(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C7 1.414(3) . ? C2 C3 1.419(3) . ? C3 C4 1.382(3) . ? C3 H3A 0.9500 . ? C4 C5 1.393(4) . ? C4 H4A 0.9500 . ? C5 C6 1.383(4) . ? C5 H5A 0.9500 . ? C6 C7 1.391(3) . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? C8 C9 1.439(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.415(3) . ? C9 C14 1.417(3) . ? C10 C11 1.388(3) . ? C10 H10A 0.9500 . ? C11 C12 1.382(3) . ? C11 H11A 0.9500 . ? C12 C13 1.390(4) . ? C12 H12A 0.9500 . ? C13 C14 1.382(3) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? C15 C16 1.435(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.418(3) . ? C16 C21 1.418(3) . ? C17 C18 1.374(3) . ? C17 H17A 0.9500 . ? C18 C19 1.396(3) . ? C18 H18A 0.9500 . ? C19 C20 1.385(3) . ? C19 H19A 0.9500 . ? C20 C21 1.389(3) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? C22 C23 1.501(4) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.450(5) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.506(4) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.510(3) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.525(4) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.508(3) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.514(3) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.522(3) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.516(3) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ce1 C8 115.14(7) . . ? C1 Ce1 C15 111.84(7) . . ? C8 Ce1 C15 114.18(7) . . ? C1 Ce1 O2 148.54(6) . . ? C8 Ce1 O2 78.85(6) . . ? C15 Ce1 O2 84.21(6) . . ? C1 Ce1 O1 81.68(6) . . ? C8 Ce1 O1 149.28(6) . . ? C15 Ce1 O1 78.95(6) . . ? O2 Ce1 O1 74.93(5) . . ? C1 Ce1 O3 78.21(6) . . ? C8 Ce1 O3 84.44(6) . . ? C15 Ce1 O3 149.17(6) . . ? O2 Ce1 O3 75.26(4) . . ? O1 Ce1 O3 73.70(5) . . ? C1 Ce1 C16 126.29(6) . . ? C8 Ce1 C16 85.40(6) . . ? C15 Ce1 C16 28.95(6) . . ? O2 Ce1 C16 80.88(5) . . ? O1 Ce1 C16 105.70(5) . . ? O3 Ce1 C16 155.45(5) . . ? C1 Ce1 C9 86.52(7) . . ? C8 Ce1 C9 28.92(6) . . ? C15 Ce1 C9 126.56(6) . . ? O2 Ce1 C9 105.89(5) . . ? O1 Ce1 C9 154.46(5) . . ? O3 Ce1 C9 81.77(5) . . ? C16 Ce1 C9 99.55(6) . . ? C1 Ce1 C2 28.69(6) . . ? C8 Ce1 C2 127.04(6) . . ? C15 Ce1 C2 83.58(7) . . ? O2 Ce1 C2 154.10(5) . . ? O1 Ce1 C2 80.35(5) . . ? O3 Ce1 C2 105.23(5) . . ? C16 Ce1 C2 98.74(6) . . ? C9 Ce1 C2 99.73(6) . . ? C25 O1 C22 108.59(16) . . ? C25 O1 Ce1 125.86(13) . . ? C22 O1 Ce1 125.19(12) . . ? C26 O2 C29 108.47(15) . . ? C26 O2 Ce1 127.40(12) . . ? C29 O2 Ce1 123.98(12) . . ? C30 O3 C33 108.45(15) . . ? C30 O3 Ce1 125.41(12) . . ? C33 O3 Ce1 125.26(11) . . ? C2 C1 Ce1 91.27(12) . . ? C2 C1 H1A 113.4 . . ? Ce1 C1 H1A 113.4 . . ? C2 C1 H1B 113.4 . . ? Ce1 C1 H1B 113.4 . . ? H1A C1 H1B 110.7 . . ? C7 C2 C3 115.8(2) . . ? C7 C2 C1 121.4(2) . . ? C3 C2 C1 122.5(2) . . ? C7 C2 Ce1 95.56(13) . . ? C3 C2 Ce1 110.14(14) . . ? C1 C2 Ce1 60.04(11) . . ? C4 C3 C2 122.3(2) . . ? C4 C3 H3A 118.9 . . ? C2 C3 H3A 118.9 . . ? C3 C4 C5 120.4(2) . . ? C3 C4 H4A 119.8 . . ? C5 C4 H4A 119.8 . . ? C6 C5 C4 118.9(2) . . ? C6 C5 H5A 120.5 . . ? C4 C5 H5A 120.5 . . ? C5 C6 C7 121.0(2) . . ? C5 C6 H6A 119.5 . . ? C7 C6 H6A 119.5 . . ? C6 C7 C2 121.6(2) . . ? C6 C7 H7A 119.2 . . ? C2 C7 H7A 119.2 . . ? C9 C8 Ce1 89.77(13) . . ? C9 C8 H8A 113.7 . . ? Ce1 C8 H8A 113.7 . . ? C9 C8 H8B 113.7 . . ? Ce1 C8 H8B 113.7 . . ? H8A C8 H8B 110.9 . . ? C10 C9 C14 115.4(2) . . ? C10 C9 C8 122.6(2) . . ? C14 C9 C8 121.7(2) . . ? C10 C9 Ce1 100.72(13) . . ? C14 C9 Ce1 103.60(13) . . ? C8 C9 Ce1 61.32(11) . . ? C11 C10 C9 122.0(2) . . ? C11 C10 H10A 119.0 . . ? C9 C10 H10A 119.0 . . ? C12 C11 C10 121.2(2) . . ? C12 C11 H11A 119.4 . . ? C10 C11 H11A 119.4 . . ? C11 C12 C13 118.3(2) . . ? C11 C12 H12A 120.8 . . ? C13 C12 H12A 120.8 . . ? C14 C13 C12 121.0(2) . . ? C14 C13 H13A 119.5 . . ? C12 C13 H13A 119.5 . . ? C13 C14 C9 122.1(2) . . ? C13 C14 H14A 119.0 . . ? C9 C14 H14A 119.0 . . ? C16 C15 Ce1 89.23(12) . . ? C16 C15 H15A 113.8 . . ? Ce1 C15 H15A 113.8 . . ? C16 C15 H15B 113.8 . . ? Ce1 C15 H15B 113.8 . . ? H15A C15 H15B 111.0 . . ? C17 C16 C21 115.33(19) . . ? C17 C16 C15 121.4(2) . . ? C21 C16 C15 123.05(19) . . ? C17 C16 Ce1 108.74(13) . . ? C21 C16 Ce1 95.97(13) . . ? C15 C16 Ce1 61.83(11) . . ? C18 C17 C16 122.1(2) . . ? C18 C17 H17A 118.9 . . ? C16 C17 H17A 118.9 . . ? C17 C18 C19 121.5(2) . . ? C17 C18 H18A 119.2 . . ? C19 C18 H18A 119.2 . . ? C20 C19 C18 117.8(2) . . ? C20 C19 H19A 121.1 . . ? C18 C19 H19A 121.1 . . ? C19 C20 C21 121.2(2) . . ? C19 C20 H20A 119.4 . . ? C21 C20 H20A 119.4 . . ? C20 C21 C16 121.95(19) . . ? C20 C21 H21A 119.0 . . ? C16 C21 H21A 119.0 . . ? O1 C22 C23 105.38(19) . . ? O1 C22 H22A 110.7 . . ? C23 C22 H22A 110.7 . . ? O1 C22 H22B 110.7 . . ? C23 C22 H22B 110.7 . . ? H22A C22 H22B 108.8 . . ? C24 C23 C22 104.3(3) . . ? C24 C23 H23A 110.9 . . ? C22 C23 H23A 110.9 . . ? C24 C23 H23B 110.9 . . ? C22 C23 H23B 110.9 . . ? H23A C23 H23B 108.9 . . ? C23 C24 C25 105.8(2) . . ? C23 C24 H24A 110.6 . . ? C25 C24 H24A 110.6 . . ? C23 C24 H24B 110.6 . . ? C25 C24 H24B 110.6 . . ? H24A C24 H24B 108.7 . . ? O1 C25 C24 106.0(2) . . ? O1 C25 H25A 110.5 . . ? C24 C25 H25A 110.5 . . ? O1 C25 H25B 110.5 . . ? C24 C25 H25B 110.5 . . ? H25A C25 H25B 108.7 . . ? O2 C26 C27 105.83(18) . . ? O2 C26 H26A 110.6 . . ? C27 C26 H26A 110.6 . . ? O2 C26 H26B 110.6 . . ? C27 C26 H26B 110.6 . . ? H26A C26 H26B 108.7 . . ? C26 C27 C28 101.33(19) . . ? C26 C27 H27A 111.5 . . ? C28 C27 H27A 111.5 . . ? C26 C27 H27B 111.5 . . ? C28 C27 H27B 111.5 . . ? H27A C27 H27B 109.3 . . ? C29 C28 C27 102.46(19) . . ? C29 C28 H28A 111.3 . . ? C27 C28 H28A 111.3 . . ? C29 C28 H28B 111.3 . . ? C27 C28 H28B 111.3 . . ? H28A C28 H28B 109.2 . . ? O2 C29 C28 106.03(18) . . ? O2 C29 H29A 110.5 . . ? C28 C29 H29A 110.5 . . ? O2 C29 H29B 110.5 . . ? C28 C29 H29B 110.5 . . ? H29A C29 H29B 108.7 . . ? O3 C30 C31 106.10(17) . . ? O3 C30 H30A 110.5 . . ? C31 C30 H30A 110.5 . . ? O3 C30 H30B 110.5 . . ? C31 C30 H30B 110.5 . . ? H30A C30 H30B 108.7 . . ? C30 C31 C32 101.25(18) . . ? C30 C31 H31A 111.5 . . ? C32 C31 H31A 111.5 . . ? C30 C31 H31B 111.5 . . ? C32 C31 H31B 111.5 . . ? H31A C31 H31B 109.3 . . ? C33 C32 C31 102.01(18) . . ? C33 C32 H32A 111.4 . . ? C31 C32 H32A 111.4 . . ? C33 C32 H32B 111.4 . . ? C31 C32 H32B 111.4 . . ? H32A C32 H32B 109.2 . . ? O3 C33 C32 105.34(16) . . ? O3 C33 H33A 110.7 . . ? C32 C33 H33A 110.7 . . ? O3 C33 H33B 110.7 . . ? C32 C33 H33B 110.7 . . ? H33A C33 H33B 108.8 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.260 _refine_diff_density_min -0.779 _refine_diff_density_rms 0.068 # Attachment '3.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 736117' _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H45 O3 Pr' _chemical_formula_sum 'C33 H45 O3 Pr' _chemical_formula_weight 630.60 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.1610(17) _cell_length_b 10.5360(13) _cell_length_c 20.775(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.262(2) _cell_angle_gamma 90.00 _cell_volume 3040.0(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 10761 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 27.50 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.378 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1304 _exptl_absorpt_coefficient_mu 1.632 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.59 _exptl_absorpt_correction_T_max 0.73 _exptl_absorpt_process_details '(SADABS; Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 19960 _diffrn_reflns_av_R_equivalents 0.0580 _diffrn_reflns_av_sigmaI/netI 0.0452 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 24.00 _reflns_number_total 4759 _reflns_number_gt 4051 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'enCIFer(Allen et al.,2004);PLATON(Spek,2003)' _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^)+(0.0476P)^2^+27.2265P] 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 4759 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0574 _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_ref 0.1401 _refine_ls_wR_factor_gt 0.1347 _refine_ls_goodness_of_fit_ref 1.137 _refine_ls_restrained_S_all 1.137 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pr1 Pr 0.27033(3) 0.40184(4) 0.348118(18) 0.02191(16) Uani 1 1 d . . . O1 O 0.4219(3) 0.2521(5) 0.3812(2) 0.0276(11) Uani 1 1 d . . . O2 O 0.2286(4) 0.2444(5) 0.4366(2) 0.0307(12) Uani 1 1 d . . . O3 O 0.2203(4) 0.1911(5) 0.2843(2) 0.0282(11) Uani 1 1 d . . . C1 C 0.0866(5) 0.4395(8) 0.3337(4) 0.0312(17) Uani 1 1 d . . . H1A H 0.0493 0.3605 0.3354 0.037 Uiso 1 1 calc R . . H1B H 0.0694 0.5039 0.3642 0.037 Uiso 1 1 calc R . . C2 C 0.0820(5) 0.4866(7) 0.2684(3) 0.0254(16) Uani 1 1 d . . . C3 C 0.1115(5) 0.6113(7) 0.2548(4) 0.0299(17) Uani 1 1 d . . . H3A H 0.1285 0.6698 0.2900 0.036 Uiso 1 1 calc R . . C4 C 0.1161(6) 0.6499(8) 0.1915(4) 0.0329(18) Uani 1 1 d . . . H4A H 0.1357 0.7341 0.1844 0.039 Uiso 1 1 calc R . . C5 C 0.0925(6) 0.5677(8) 0.1385(4) 0.0350(19) Uani 1 1 d . . . H5A H 0.0965 0.5940 0.0954 0.042 Uiso 1 1 calc R . . C6 C 0.0630(6) 0.4457(8) 0.1506(4) 0.0363(19) Uani 1 1 d . . . H6A H 0.0458 0.3884 0.1150 0.044 Uiso 1 1 calc R . . C7 C 0.0581(5) 0.4056(7) 0.2132(4) 0.0305(17) Uani 1 1 d . . . H7A H 0.0382 0.3211 0.2193 0.037 Uiso 1 1 calc R . . C8 C 0.3639(5) 0.5162(7) 0.4515(3) 0.0300(17) Uani 1 1 d . . . H8A H 0.3896 0.4575 0.4879 0.036 Uiso 1 1 calc R . . H8B H 0.4154 0.5728 0.4422 0.036 Uiso 1 1 calc R . . C9 C 0.2794(6) 0.5836(7) 0.4611(4) 0.0325(18) Uani 1 1 d . . . C10 C 0.2448(6) 0.6922(8) 0.4231(4) 0.039(2) Uani 1 1 d . . . H10A H 0.2819 0.7257 0.3935 0.047 Uiso 1 1 calc R . . C11 C 0.1597(7) 0.7501(8) 0.4277(4) 0.043(2) Uani 1 1 d . . . H11A H 0.1395 0.8225 0.4013 0.051 Uiso 1 1 calc R . . C12 C 0.1022(7) 0.7057(10) 0.4700(4) 0.051(2) Uani 1 1 d . . . H12A H 0.0432 0.7462 0.4727 0.061 Uiso 1 1 calc R . . C13 C 0.1342(7) 0.5994(9) 0.5084(4) 0.045(2) Uani 1 1 d . . . H13A H 0.0962 0.5668 0.5376 0.053 Uiso 1 1 calc R . . C14 C 0.2203(6) 0.5409(8) 0.5043(4) 0.0347(18) Uani 1 1 d . . . H14A H 0.2404 0.4695 0.5315 0.042 Uiso 1 1 calc R . . C15 C 0.3360(6) 0.4431(7) 0.2417(4) 0.0318(17) Uani 1 1 d . . . H15A H 0.3684 0.3685 0.2268 0.038 Uiso 1 1 calc R . . H15B H 0.2872 0.4782 0.2054 0.038 Uiso 1 1 calc R . . C16 C 0.4023(5) 0.5375(7) 0.2751(3) 0.0289(17) Uani 1 1 d . . . C17 C 0.4951(6) 0.5045(8) 0.3105(4) 0.0339(18) Uani 1 1 d . . . H17A H 0.5173 0.4198 0.3083 0.041 Uiso 1 1 calc R . . C18 C 0.5545(6) 0.5926(8) 0.3483(4) 0.037(2) Uani 1 1 d . . . H18A H 0.6164 0.5671 0.3712 0.045 Uiso 1 1 calc R . . C19 C 0.5250(6) 0.7176(8) 0.3533(4) 0.039(2) Uani 1 1 d . . . H19A H 0.5653 0.7773 0.3799 0.046 Uiso 1 1 calc R . . C20 C 0.4346(6) 0.7526(8) 0.3182(4) 0.0389(19) Uani 1 1 d . . . H20A H 0.4137 0.8379 0.3202 0.047 Uiso 1 1 calc R . . C21 C 0.3747(6) 0.6659(8) 0.2807(4) 0.0330(18) Uani 1 1 d . . . H21A H 0.3132 0.6929 0.2580 0.040 Uiso 1 1 calc R . . C22 C 0.4408(6) 0.1380(8) 0.3457(4) 0.038(2) Uani 1 1 d . . . H22A H 0.4490 0.1599 0.3007 0.046 Uiso 1 1 calc R . . H22B H 0.3869 0.0771 0.3425 0.046 Uiso 1 1 calc R . . C23 C 0.5324(6) 0.0814(8) 0.3845(4) 0.0374(19) Uani 1 1 d . . . H23A H 0.5677 0.0330 0.3559 0.045 Uiso 1 1 calc R . . H23B H 0.5190 0.0251 0.4198 0.045 Uiso 1 1 calc R . . C24 C 0.5881(6) 0.1995(8) 0.4126(4) 0.0384(19) Uani 1 1 d . . . H24A H 0.6374 0.1790 0.4520 0.046 Uiso 1 1 calc R . . H24B H 0.6196 0.2412 0.3796 0.046 Uiso 1 1 calc R . . C25 C 0.5089(5) 0.2811(8) 0.4296(4) 0.0318(17) Uani 1 1 d . . . H25A H 0.4991 0.2614 0.4745 0.038 Uiso 1 1 calc R . . H25B H 0.5255 0.3721 0.4277 0.038 Uiso 1 1 calc R . . C26 C 0.1317(6) 0.2230(8) 0.4501(4) 0.0373(19) Uani 1 1 d . . . H26A H 0.0847 0.2066 0.4091 0.045 Uiso 1 1 calc R . . H26B H 0.1099 0.2972 0.4726 0.045 Uiso 1 1 calc R . . C27 C 0.1434(8) 0.1084(12) 0.4939(6) 0.075(4) Uani 1 1 d . . . H27A H 0.0971 0.1114 0.5239 0.090 Uiso 1 1 calc R . . H27B H 0.1318 0.0299 0.4674 0.090 Uiso 1 1 calc R . . C28 C 0.2393(8) 0.1109(13) 0.5301(6) 0.077(4) Uani 1 1 d . . . H28A H 0.2635 0.0237 0.5405 0.093 Uiso 1 1 calc R . . H28B H 0.2429 0.1585 0.5716 0.093 Uiso 1 1 calc R . . C29 C 0.2974(6) 0.1771(9) 0.4859(4) 0.045(2) Uani 1 1 d . . . H29A H 0.3437 0.2372 0.5115 0.055 Uiso 1 1 calc R . . H29B H 0.3336 0.1142 0.4649 0.055 Uiso 1 1 calc R . . C30 C 0.2302(6) 0.1667(8) 0.2162(4) 0.0329(18) Uani 1 1 d . . . H30A H 0.2985 0.1523 0.2140 0.039 Uiso 1 1 calc R . . H30B H 0.2060 0.2400 0.1879 0.039 Uiso 1 1 calc R . . C31 C 0.1711(7) 0.0495(9) 0.1940(4) 0.047(2) Uani 1 1 d . . . H31A H 0.1983 0.0011 0.1610 0.057 Uiso 1 1 calc R . . H31B H 0.1033 0.0715 0.1754 0.057 Uiso 1 1 calc R . . C32 C 0.1796(6) -0.0244(8) 0.2579(4) 0.039(2) Uani 1 1 d . . . H32A H 0.1268 -0.0869 0.2556 0.047 Uiso 1 1 calc R . . H32B H 0.2423 -0.0686 0.2695 0.047 Uiso 1 1 calc R . . C33 C 0.1713(6) 0.0818(7) 0.3058(4) 0.0343(18) Uani 1 1 d . . . H33A H 0.1028 0.1019 0.3052 0.041 Uiso 1 1 calc R . . H33B H 0.2022 0.0570 0.3510 0.041 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 Pr1 0.0258(2) 0.0232(2) 0.0157(2) -0.00267(16) 0.00165(15) -0.00024(16) O1 0.028(3) 0.030(3) 0.023(3) -0.009(2) 0.002(2) 0.001(2) O2 0.033(3) 0.040(3) 0.018(3) 0.005(2) 0.003(2) 0.001(2) O3 0.040(3) 0.026(3) 0.018(3) -0.006(2) 0.005(2) -0.007(2) C1 0.032(4) 0.041(4) 0.019(4) 0.003(3) 0.001(3) 0.006(3) C2 0.019(3) 0.032(4) 0.022(4) -0.002(3) -0.003(3) 0.002(3) C3 0.031(4) 0.030(4) 0.027(4) -0.010(3) 0.002(3) 0.001(3) C4 0.041(4) 0.027(4) 0.029(4) 0.001(3) 0.004(3) 0.003(3) C5 0.037(4) 0.042(5) 0.023(4) 0.000(3) 0.000(3) 0.000(4) C6 0.037(4) 0.046(5) 0.025(4) -0.009(4) 0.002(3) -0.003(4) C7 0.028(4) 0.026(4) 0.033(4) -0.002(3) -0.005(3) 0.002(3) C8 0.034(4) 0.035(4) 0.019(4) -0.010(3) -0.001(3) -0.002(3) C9 0.044(5) 0.034(4) 0.017(4) -0.013(3) -0.001(3) -0.003(4) C10 0.057(5) 0.037(5) 0.023(4) -0.008(4) 0.007(4) 0.001(4) C11 0.061(6) 0.033(5) 0.032(5) -0.005(4) 0.004(4) 0.011(4) C12 0.061(6) 0.059(6) 0.034(5) 0.003(4) 0.014(4) 0.028(5) C13 0.051(5) 0.058(6) 0.027(4) 0.006(4) 0.015(4) 0.012(4) C14 0.040(5) 0.043(5) 0.019(4) 0.000(3) 0.002(3) 0.007(4) C15 0.043(5) 0.027(4) 0.029(4) 0.000(3) 0.015(4) 0.000(3) C16 0.032(4) 0.036(4) 0.020(4) 0.003(3) 0.010(3) -0.002(3) C17 0.039(5) 0.035(4) 0.029(4) 0.005(4) 0.009(3) 0.000(4) C18 0.027(4) 0.054(6) 0.030(4) 0.013(4) 0.004(3) -0.003(4) C19 0.047(5) 0.040(5) 0.028(4) -0.005(4) 0.006(4) -0.020(4) C20 0.045(5) 0.035(5) 0.036(5) 0.000(4) 0.007(4) -0.005(4) C21 0.032(4) 0.038(5) 0.027(4) 0.007(4) 0.003(3) 0.001(4) C22 0.041(5) 0.039(5) 0.034(5) -0.016(4) 0.002(4) 0.009(4) C23 0.037(4) 0.036(5) 0.038(5) -0.003(4) 0.005(4) 0.011(4) C24 0.034(4) 0.045(5) 0.034(5) -0.003(4) 0.000(3) 0.005(4) C25 0.031(4) 0.035(4) 0.026(4) -0.005(3) -0.002(3) -0.004(3) C26 0.038(4) 0.042(5) 0.034(5) 0.008(4) 0.012(4) 0.004(4) C27 0.054(6) 0.099(9) 0.080(8) 0.061(7) 0.028(6) 0.019(6) C28 0.056(7) 0.108(10) 0.067(8) 0.059(7) 0.007(6) -0.001(6) C29 0.045(5) 0.053(6) 0.035(5) 0.016(4) 0.000(4) 0.004(4) C30 0.038(4) 0.039(5) 0.023(4) -0.009(3) 0.008(3) -0.002(4) C31 0.052(5) 0.056(6) 0.036(5) -0.018(4) 0.014(4) -0.015(5) C32 0.039(5) 0.033(5) 0.046(5) -0.016(4) 0.013(4) -0.006(4) C33 0.041(5) 0.032(4) 0.031(4) -0.010(3) 0.010(4) -0.010(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pr1 C1 2.591(7) . ? Pr1 C8 2.591(7) . ? Pr1 C15 2.596(7) . ? Pr1 O3 2.612(5) . ? Pr1 O2 2.628(5) . ? Pr1 O1 2.644(5) . ? Pr1 C2 2.989(7) . ? Pr1 C16 2.991(7) . ? Pr1 C9 3.013(7) . ? O1 C22 1.463(9) . ? O1 C25 1.463(8) . ? O2 C29 1.453(9) . ? O2 C26 1.471(9) . ? O3 C33 1.458(9) . ? O3 C30 1.473(8) . ? C1 C2 1.434(10) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C7 1.417(10) . ? C2 C3 1.423(11) . ? C3 C4 1.390(11) . ? C3 H3A 0.9500 . ? C4 C5 1.390(11) . ? C4 H4A 0.9500 . ? C5 C6 1.390(12) . ? C5 H5A 0.9500 . ? C6 C7 1.380(11) . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? C8 C9 1.438(11) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C14 1.415(11) . ? C9 C10 1.422(12) . ? C10 C11 1.370(12) . ? C10 H10A 0.9500 . ? C11 C12 1.391(13) . ? C11 H11A 0.9500 . ? C12 C13 1.398(13) . ? C12 H12A 0.9500 . ? C13 C14 1.384(12) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? C15 C16 1.448(11) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.418(11) . ? C16 C21 1.419(11) . ? C17 C18 1.388(12) . ? C17 H17A 0.9500 . ? C18 C19 1.392(12) . ? C18 H18A 0.9500 . ? C19 C20 1.394(12) . ? C19 H19A 0.9500 . ? C20 C21 1.380(11) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? C22 C23 1.509(11) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.528(12) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.510(11) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.501(12) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.418(15) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.517(13) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.512(12) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.523(13) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.518(11) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pr1 C8 111.3(2) . . ? C1 Pr1 C15 113.2(2) . . ? C8 Pr1 C15 114.7(3) . . ? C1 Pr1 O3 84.5(2) . . ? C8 Pr1 O3 149.4(2) . . ? C15 Pr1 O3 79.5(2) . . ? C1 Pr1 O2 79.6(2) . . ? C8 Pr1 O2 82.1(2) . . ? C15 Pr1 O2 150.2(2) . . ? O3 Pr1 O2 75.07(15) . . ? C1 Pr1 O1 150.1(2) . . ? C8 Pr1 O1 78.7(2) . . ? C15 Pr1 O1 85.0(2) . . ? O3 Pr1 O1 75.56(15) . . ? O2 Pr1 O1 73.94(16) . . ? C1 Pr1 C2 28.7(2) . . ? C8 Pr1 C2 125.3(2) . . ? C15 Pr1 C2 84.7(2) . . ? O3 Pr1 C2 81.28(18) . . ? O2 Pr1 C2 106.15(18) . . ? O1 Pr1 C2 156.02(17) . . ? C1 Pr1 C16 125.5(2) . . ? C8 Pr1 C16 85.9(2) . . ? C15 Pr1 C16 29.0(2) . . ? O3 Pr1 C16 106.48(18) . . ? O2 Pr1 C16 154.78(18) . . ? O1 Pr1 C16 82.01(18) . . ? C2 Pr1 C16 98.9(2) . . ? C1 Pr1 C9 83.2(2) . . ? C8 Pr1 C9 28.5(2) . . ? C15 Pr1 C9 126.1(2) . . ? O3 Pr1 C9 154.39(19) . . ? O2 Pr1 C9 80.64(19) . . ? O1 Pr1 C9 105.54(18) . . ? C2 Pr1 C9 98.0(2) . . ? C16 Pr1 C9 99.0(2) . . ? C22 O1 C25 107.8(5) . . ? C22 O1 Pr1 125.4(4) . . ? C25 O1 Pr1 125.8(4) . . ? C29 O2 C26 108.2(6) . . ? C29 O2 Pr1 126.2(5) . . ? C26 O2 Pr1 125.2(4) . . ? C33 O3 C30 107.3(5) . . ? C33 O3 Pr1 127.9(4) . . ? C30 O3 Pr1 124.7(4) . . ? C2 C1 Pr1 91.2(4) . . ? C2 C1 H1A 113.4 . . ? Pr1 C1 H1A 113.4 . . ? C2 C1 H1B 113.4 . . ? Pr1 C1 H1B 113.4 . . ? H1A C1 H1B 110.7 . . ? C7 C2 C3 115.4(7) . . ? C7 C2 C1 121.2(7) . . ? C3 C2 C1 123.0(7) . . ? C7 C2 Pr1 108.3(5) . . ? C3 C2 Pr1 96.9(4) . . ? C1 C2 Pr1 60.1(4) . . ? C4 C3 C2 121.8(7) . . ? C4 C3 H3A 119.1 . . ? C2 C3 H3A 119.1 . . ? C5 C4 C3 121.3(8) . . ? C5 C4 H4A 119.4 . . ? C3 C4 H4A 119.4 . . ? C6 C5 C4 117.8(7) . . ? C6 C5 H5A 121.1 . . ? C4 C5 H5A 121.1 . . ? C7 C6 C5 121.7(7) . . ? C7 C6 H6A 119.1 . . ? C5 C6 H6A 119.1 . . ? C6 C7 C2 122.0(7) . . ? C6 C7 H7A 119.0 . . ? C2 C7 H7A 119.0 . . ? C9 C8 Pr1 92.3(4) . . ? C9 C8 H8A 113.2 . . ? Pr1 C8 H8A 113.2 . . ? C9 C8 H8B 113.2 . . ? Pr1 C8 H8B 113.2 . . ? H8A C8 H8B 110.6 . . ? C14 C9 C10 115.2(7) . . ? C14 C9 C8 122.8(7) . . ? C10 C9 C8 121.7(7) . . ? C14 C9 Pr1 110.6(5) . . ? C10 C9 Pr1 96.9(4) . . ? C8 C9 Pr1 59.2(4) . . ? C11 C10 C9 122.1(8) . . ? C11 C10 H10A 119.0 . . ? C9 C10 H10A 119.0 . . ? C10 C11 C12 121.7(8) . . ? C10 C11 H11A 119.1 . . ? C12 C11 H11A 119.1 . . ? C11 C12 C13 117.7(8) . . ? C11 C12 H12A 121.1 . . ? C13 C12 H12A 121.1 . . ? C14 C13 C12 120.9(8) . . ? C14 C13 H13A 119.6 . . ? C12 C13 H13A 119.6 . . ? C13 C14 C9 122.3(8) . . ? C13 C14 H14A 118.8 . . ? C9 C14 H14A 118.8 . . ? C16 C15 Pr1 90.8(4) . . ? C16 C15 H15A 113.5 . . ? Pr1 C15 H15A 113.5 . . ? C16 C15 H15B 113.5 . . ? Pr1 C15 H15B 113.5 . . ? H15A C15 H15B 110.8 . . ? C17 C16 C21 115.7(7) . . ? C17 C16 C15 121.9(7) . . ? C21 C16 C15 122.0(7) . . ? C17 C16 Pr1 103.1(5) . . ? C21 C16 Pr1 101.8(5) . . ? C15 C16 Pr1 60.2(4) . . ? C18 C17 C16 121.8(8) . . ? C18 C17 H17A 119.1 . . ? C16 C17 H17A 119.1 . . ? C17 C18 C19 121.2(8) . . ? C17 C18 H18A 119.4 . . ? C19 C18 H18A 119.4 . . ? C18 C19 C20 118.0(7) . . ? C18 C19 H19A 121.0 . . ? C20 C19 H19A 121.0 . . ? C21 C20 C19 121.4(8) . . ? C21 C20 H20A 119.3 . . ? C19 C20 H20A 119.3 . . ? C20 C21 C16 121.9(7) . . ? C20 C21 H21A 119.0 . . ? C16 C21 H21A 119.0 . . ? O1 C22 C23 106.1(6) . . ? O1 C22 H22A 110.5 . . ? C23 C22 H22A 110.5 . . ? O1 C22 H22B 110.5 . . ? C23 C22 H22B 110.5 . . ? H22A C22 H22B 108.7 . . ? C22 C23 C24 102.0(6) . . ? C22 C23 H23A 111.4 . . ? C24 C23 H23A 111.4 . . ? C22 C23 H23B 111.4 . . ? C24 C23 H23B 111.4 . . ? H23A C23 H23B 109.2 . . ? C25 C24 C23 101.6(6) . . ? C25 C24 H24A 111.5 . . ? C23 C24 H24A 111.5 . . ? C25 C24 H24B 111.5 . . ? C23 C24 H24B 111.5 . . ? H24A C24 H24B 109.3 . . ? O1 C25 C24 106.5(6) . . ? O1 C25 H25A 110.4 . . ? C24 C25 H25A 110.4 . . ? O1 C25 H25B 110.4 . . ? C24 C25 H25B 110.4 . . ? H25A C25 H25B 108.6 . . ? O2 C26 C27 104.0(7) . . ? O2 C26 H26A 111.0 . . ? C27 C26 H26A 111.0 . . ? O2 C26 H26B 111.0 . . ? C27 C26 H26B 111.0 . . ? H26A C26 H26B 109.0 . . ? C28 C27 C26 106.7(9) . . ? C28 C27 H27A 110.4 . . ? C26 C27 H27A 110.4 . . ? C28 C27 H27B 110.4 . . ? C26 C27 H27B 110.4 . . ? H27A C27 H27B 108.6 . . ? C27 C28 C29 105.3(8) . . ? C27 C28 H28A 110.7 . . ? C29 C28 H28A 110.7 . . ? C27 C28 H28B 110.7 . . ? C29 C28 H28B 110.7 . . ? H28A C28 H28B 108.8 . . ? O2 C29 C28 106.4(7) . . ? O2 C29 H29A 110.4 . . ? C28 C29 H29A 110.4 . . ? O2 C29 H29B 110.4 . . ? C28 C29 H29B 110.4 . . ? H29A C29 H29B 108.6 . . ? O3 C30 C31 106.5(6) . . ? O3 C30 H30A 110.4 . . ? C31 C30 H30A 110.4 . . ? O3 C30 H30B 110.4 . . ? C31 C30 H30B 110.4 . . ? H30A C30 H30B 108.6 . . ? C30 C31 C32 101.9(7) . . ? C30 C31 H31A 111.4 . . ? C32 C31 H31A 111.4 . . ? C30 C31 H31B 111.4 . . ? C32 C31 H31B 111.4 . . ? H31A C31 H31B 109.2 . . ? C33 C32 C31 101.1(7) . . ? C33 C32 H32A 111.6 . . ? C31 C32 H32A 111.6 . . ? C33 C32 H32B 111.6 . . ? C31 C32 H32B 111.6 . . ? H32A C32 H32B 109.4 . . ? O3 C33 C32 106.2(6) . . ? O3 C33 H33A 110.5 . . ? C32 C33 H33A 110.5 . . ? O3 C33 H33B 110.5 . . ? C32 C33 H33B 110.5 . . ? H33A C33 H33B 108.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Pr1 O1 C22 67.5(7) . . . . ? C8 Pr1 O1 C22 -179.0(6) . . . . ? C15 Pr1 O1 C22 -62.6(6) . . . . ? O3 Pr1 O1 C22 17.8(6) . . . . ? O2 Pr1 O1 C22 96.1(6) . . . . ? C2 Pr1 O1 C22 2.3(8) . . . . ? C16 Pr1 O1 C22 -91.6(6) . . . . ? C9 Pr1 O1 C22 171.3(6) . . . . ? C1 Pr1 O1 C25 -125.0(6) . . . . ? C8 Pr1 O1 C25 -11.5(5) . . . . ? C15 Pr1 O1 C25 104.9(5) . . . . ? O3 Pr1 O1 C25 -174.7(5) . . . . ? O2 Pr1 O1 C25 -96.4(5) . . . . ? C2 Pr1 O1 C25 169.9(5) . . . . ? C16 Pr1 O1 C25 75.9(5) . . . . ? C9 Pr1 O1 C25 -21.2(6) . . . . ? C1 Pr1 O2 C29 -170.1(6) . . . . ? C8 Pr1 O2 C29 -56.6(6) . . . . ? C15 Pr1 O2 C29 70.7(8) . . . . ? O3 Pr1 O2 C29 102.8(6) . . . . ? O1 Pr1 O2 C29 23.9(6) . . . . ? C2 Pr1 O2 C29 178.9(6) . . . . ? C16 Pr1 O2 C29 5.7(8) . . . . ? C9 Pr1 O2 C29 -85.4(6) . . . . ? C1 Pr1 O2 C26 1.1(6) . . . . ? C8 Pr1 O2 C26 114.6(6) . . . . ? C15 Pr1 O2 C26 -118.1(6) . . . . ? O3 Pr1 O2 C26 -86.0(6) . . . . ? O1 Pr1 O2 C26 -164.9(6) . . . . ? C2 Pr1 O2 C26 -9.9(6) . . . . ? C16 Pr1 O2 C26 177.0(6) . . . . ? C9 Pr1 O2 C26 85.8(6) . . . . ? C1 Pr1 O3 C33 -66.6(6) . . . . ? C8 Pr1 O3 C33 57.2(7) . . . . ? C15 Pr1 O3 C33 178.5(6) . . . . ? O2 Pr1 O3 C33 14.1(5) . . . . ? O1 Pr1 O3 C33 91.0(6) . . . . ? C2 Pr1 O3 C33 -95.3(6) . . . . ? C16 Pr1 O3 C33 167.9(6) . . . . ? C9 Pr1 O3 C33 -4.9(8) . . . . ? C1 Pr1 O3 C30 107.9(5) . . . . ? C8 Pr1 O3 C30 -128.3(6) . . . . ? C15 Pr1 O3 C30 -7.0(5) . . . . ? O2 Pr1 O3 C30 -171.4(5) . . . . ? O1 Pr1 O3 C30 -94.5(5) . . . . ? C2 Pr1 O3 C30 79.2(5) . . . . ? C16 Pr1 O3 C30 -17.6(5) . . . . ? C9 Pr1 O3 C30 169.6(5) . . . . ? C8 Pr1 C1 C2 125.2(5) . . . . ? C15 Pr1 C1 C2 -5.7(5) . . . . ? O3 Pr1 C1 C2 -81.8(5) . . . . ? O2 Pr1 C1 C2 -157.6(5) . . . . ? O1 Pr1 C1 C2 -129.7(4) . . . . ? C16 Pr1 C1 C2 24.6(6) . . . . ? C9 Pr1 C1 C2 120.7(5) . . . . ? Pr1 C1 C2 C7 94.3(6) . . . . ? Pr1 C1 C2 C3 -78.0(7) . . . . ? C1 Pr1 C2 C7 -116.0(7) . . . . ? C8 Pr1 C2 C7 175.3(5) . . . . ? C15 Pr1 C2 C7 58.7(5) . . . . ? O3 Pr1 C2 C7 -21.4(5) . . . . ? O2 Pr1 C2 C7 -93.0(5) . . . . ? O1 Pr1 C2 C7 -6.3(8) . . . . ? C16 Pr1 C2 C7 84.0(5) . . . . ? C9 Pr1 C2 C7 -175.6(5) . . . . ? C1 Pr1 C2 C3 124.3(7) . . . . ? C8 Pr1 C2 C3 55.6(5) . . . . ? C15 Pr1 C2 C3 -61.0(5) . . . . ? O3 Pr1 C2 C3 -141.1(5) . . . . ? O2 Pr1 C2 C3 147.3(4) . . . . ? O1 Pr1 C2 C3 -126.0(5) . . . . ? C16 Pr1 C2 C3 -35.7(5) . . . . ? C9 Pr1 C2 C3 64.8(5) . . . . ? C8 Pr1 C2 C1 -68.7(5) . . . . ? C15 Pr1 C2 C1 174.7(5) . . . . ? O3 Pr1 C2 C1 94.6(5) . . . . ? O2 Pr1 C2 C1 23.0(5) . . . . ? O1 Pr1 C2 C1 109.7(6) . . . . ? C16 Pr1 C2 C1 -160.0(5) . . . . ? C9 Pr1 C2 C1 -59.5(5) . . . . ? C7 C2 C3 C4 0.2(10) . . . . ? C1 C2 C3 C4 172.9(7) . . . . ? Pr1 C2 C3 C4 114.2(7) . . . . ? C2 C3 C4 C5 -0.4(12) . . . . ? C3 C4 C5 C6 0.7(12) . . . . ? C4 C5 C6 C7 -0.9(12) . . . . ? C5 C6 C7 C2 0.6(12) . . . . ? C3 C2 C7 C6 -0.3(10) . . . . ? C1 C2 C7 C6 -173.2(7) . . . . ? Pr1 C2 C7 C6 -107.6(7) . . . . ? C1 Pr1 C8 C9 -9.5(6) . . . . ? C15 Pr1 C8 C9 120.8(5) . . . . ? O3 Pr1 C8 C9 -126.8(5) . . . . ? O2 Pr1 C8 C9 -85.0(5) . . . . ? O1 Pr1 C8 C9 -160.1(5) . . . . ? C2 Pr1 C8 C9 19.2(6) . . . . ? C16 Pr1 C8 C9 117.3(5) . . . . ? Pr1 C8 C9 C14 95.9(7) . . . . ? Pr1 C8 C9 C10 -78.3(7) . . . . ? C1 Pr1 C9 C14 54.4(6) . . . . ? C8 Pr1 C9 C14 -116.8(8) . . . . ? C15 Pr1 C9 C14 168.3(5) . . . . ? O3 Pr1 C9 C14 -7.6(8) . . . . ? O2 Pr1 C9 C14 -26.2(5) . . . . ? O1 Pr1 C9 C14 -96.5(5) . . . . ? C2 Pr1 C9 C14 79.0(6) . . . . ? C16 Pr1 C9 C14 179.4(5) . . . . ? C1 Pr1 C9 C10 -65.9(5) . . . . ? C8 Pr1 C9 C10 123.0(8) . . . . ? C15 Pr1 C9 C10 48.0(6) . . . . ? O3 Pr1 C9 C10 -127.8(5) . . . . ? O2 Pr1 C9 C10 -146.4(5) . . . . ? O1 Pr1 C9 C10 143.2(5) . . . . ? C2 Pr1 C9 C10 -41.3(5) . . . . ? C16 Pr1 C9 C10 59.1(5) . . . . ? C1 Pr1 C9 C8 171.1(5) . . . . ? C15 Pr1 C9 C8 -75.0(6) . . . . ? O3 Pr1 C9 C8 109.2(6) . . . . ? O2 Pr1 C9 C8 90.6(5) . . . . ? O1 Pr1 C9 C8 20.3(5) . . . . ? C2 Pr1 C9 C8 -164.2(5) . . . . ? C16 Pr1 C9 C8 -63.9(5) . . . . ? C14 C9 C10 C11 -0.6(11) . . . . ? C8 C9 C10 C11 174.0(7) . . . . ? Pr1 C9 C10 C11 116.0(7) . . . . ? C9 C10 C11 C12 0.0(13) . . . . ? C10 C11 C12 C13 0.3(14) . . . . ? C11 C12 C13 C14 0.1(14) . . . . ? C12 C13 C14 C9 -0.9(14) . . . . ? C10 C9 C14 C13 1.1(11) . . . . ? C8 C9 C14 C13 -173.5(8) . . . . ? Pr1 C9 C14 C13 -107.5(8) . . . . ? C1 Pr1 C15 C16 122.0(5) . . . . ? C8 Pr1 C15 C16 -7.3(5) . . . . ? O3 Pr1 C15 C16 -158.7(5) . . . . ? O2 Pr1 C15 C16 -127.1(5) . . . . ? O1 Pr1 C15 C16 -82.5(5) . . . . ? C2 Pr1 C15 C16 119.2(5) . . . . ? C9 Pr1 C15 C16 23.2(6) . . . . ? Pr1 C15 C16 C17 87.3(7) . . . . ? Pr1 C15 C16 C21 -85.4(7) . . . . ? C1 Pr1 C16 C17 167.3(5) . . . . ? C8 Pr1 C16 C17 53.9(5) . . . . ? C15 Pr1 C16 C17 -119.4(8) . . . . ? O3 Pr1 C16 C17 -97.5(5) . . . . ? O2 Pr1 C16 C17 -7.7(8) . . . . ? O1 Pr1 C16 C17 -25.2(5) . . . . ? C2 Pr1 C16 C17 179.0(5) . . . . ? C9 Pr1 C16 C17 79.3(5) . . . . ? C1 Pr1 C16 C21 47.1(6) . . . . ? C8 Pr1 C16 C21 -66.3(5) . . . . ? C15 Pr1 C16 C21 120.3(7) . . . . ? O3 Pr1 C16 C21 142.2(5) . . . . ? O2 Pr1 C16 C21 -127.9(5) . . . . ? O1 Pr1 C16 C21 -145.5(5) . . . . ? C2 Pr1 C16 C21 58.8(5) . . . . ? C9 Pr1 C16 C21 -40.9(5) . . . . ? C1 Pr1 C16 C15 -73.2(5) . . . . ? C8 Pr1 C16 C15 173.4(5) . . . . ? O3 Pr1 C16 C15 21.9(5) . . . . ? O2 Pr1 C16 C15 111.8(6) . . . . ? O1 Pr1 C16 C15 94.2(5) . . . . ? C2 Pr1 C16 C15 -61.6(5) . . . . ? C9 Pr1 C16 C15 -161.2(5) . . . . ? C21 C16 C17 C18 0.3(11) . . . . ? C15 C16 C17 C18 -172.9(7) . . . . ? Pr1 C16 C17 C18 -109.9(7) . . . . ? C16 C17 C18 C19 0.3(12) . . . . ? C17 C18 C19 C20 -1.2(12) . . . . ? C18 C19 C20 C21 1.4(12) . . . . ? C19 C20 C21 C16 -0.9(12) . . . . ? C17 C16 C21 C20 0.0(11) . . . . ? C15 C16 C21 C20 173.1(7) . . . . ? Pr1 C16 C21 C20 111.0(7) . . . . ? C25 O1 C22 C23 13.2(8) . . . . ? Pr1 O1 C22 C23 -177.4(5) . . . . ? O1 C22 C23 C24 -33.0(9) . . . . ? C22 C23 C24 C25 39.3(8) . . . . ? C22 O1 C25 C24 12.4(8) . . . . ? Pr1 O1 C25 C24 -157.0(5) . . . . ? C23 C24 C25 O1 -32.4(8) . . . . ? C29 O2 C26 C27 -18.3(10) . . . . ? Pr1 O2 C26 C27 169.1(7) . . . . ? O2 C26 C27 C28 30.2(12) . . . . ? C26 C27 C28 C29 -29.6(14) . . . . ? C26 O2 C29 C28 0.9(10) . . . . ? Pr1 O2 C29 C28 173.4(7) . . . . ? C27 C28 C29 O2 18.0(13) . . . . ? C33 O3 C30 C31 9.1(8) . . . . ? Pr1 O3 C30 C31 -166.3(5) . . . . ? O3 C30 C31 C32 -31.3(8) . . . . ? C30 C31 C32 C33 40.2(8) . . . . ? C30 O3 C33 C32 17.1(8) . . . . ? Pr1 O3 C33 C32 -167.6(5) . . . . ? C31 C32 C33 O3 -36.0(8) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.020 _refine_diff_density_min -1.268 _refine_diff_density_rms 0.141 # Attachment '4.cif' data_4 _database_code_depnum_ccdc_archive 'CCDC 736118' _refine_special_details ; Disorder at c28 is suggested by the presence of a Q peak of 1.03 e but although the thermal ellipsoids of C27 and C28 are larger than neighbouring atoms they are well within tolerance limits. No splitting messages were present in the listing file and the Q peak is not in a chemically sensible position. Considering a heavy atom is present, any disorder if present is minor and therefore ill defined, and the electron density is at a location too close to existing atoms, therefore a disorder model was not used. ; _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H45 Nd O3' _chemical_formula_sum 'C33 H45 Nd O3' _chemical_formula_weight 633.93 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' O O 0.0106 0.0060 '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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.0886(9) _cell_length_b 10.5094(7) _cell_length_c 20.6877(13) _cell_angle_alpha 90.00 _cell_angle_beta 101.409(2) _cell_angle_gamma 90.00 _cell_volume 3002.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8865 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 27.51 _exptl_crystal_description Column _exptl_crystal_colour Green _exptl_crystal_size_max 0.59 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.402 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1308 _exptl_absorpt_coefficient_mu 1.759 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.40 _exptl_absorpt_correction_T_max 0.64 _exptl_absorpt_process_details '(SADABS; Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 18188 _diffrn_reflns_av_R_equivalents 0.0210 _diffrn_reflns_av_sigmaI/netI 0.0264 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 27.55 _reflns_number_total 6844 _reflns_number_gt 6023 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'enCIFer(Allen et al.,2004);PLATON(Spek,2003)' _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^)+(0.0352P)^2^+1.6642P] 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 6844 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0320 _refine_ls_R_factor_gt 0.0268 _refine_ls_wR_factor_ref 0.0663 _refine_ls_wR_factor_gt 0.0638 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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 Nd1 Nd 0.270812(8) 0.100493(11) 0.348533(6) 0.02108(5) Uani 1 1 d . . . O1 O 0.22002(11) 0.30941(16) 0.28487(8) 0.0264(3) Uani 1 1 d . . . C25 C 0.22927(19) 0.3305(3) 0.21681(12) 0.0320(6) Uani 1 1 d . . . H25A H 0.2041 0.2564 0.1891 0.038 Uiso 1 1 calc R . . H25B H 0.2980 0.3437 0.2142 0.038 Uiso 1 1 calc R . . C24 C 0.1703(2) 0.4482(3) 0.19398(14) 0.0431(7) Uani 1 1 d . . . H24A H 0.1021 0.4264 0.1751 0.052 Uiso 1 1 calc R . . H24B H 0.1981 0.4960 0.1608 0.052 Uiso 1 1 calc R . . C23 C 0.1785(2) 0.5235(3) 0.25774(15) 0.0390(7) Uani 1 1 d . . . H23A H 0.2411 0.5692 0.2689 0.047 Uiso 1 1 calc R . . H23B H 0.1248 0.5852 0.2551 0.047 Uiso 1 1 calc R . . C22 C 0.1719(2) 0.4188(2) 0.30681(14) 0.0330(6) Uani 1 1 d . . . H22A H 0.2046 0.4447 0.3517 0.040 Uiso 1 1 calc R . . H22B H 0.1034 0.3988 0.3074 0.040 Uiso 1 1 calc R . . O2 O 0.22956(12) 0.25618(17) 0.43661(8) 0.0285(4) Uani 1 1 d . . . C29 C 0.13300(19) 0.2768(3) 0.44980(14) 0.0367(6) Uani 1 1 d . . . H29A H 0.1108 0.2010 0.4711 0.044 Uiso 1 1 calc R . . H29B H 0.0862 0.2945 0.4084 0.044 Uiso 1 1 calc R . . C28 C 0.1421(3) 0.3891(5) 0.4949(2) 0.0869(17) Uani 1 1 d . . . H28A H 0.1278 0.4689 0.4694 0.104 Uiso 1 1 calc R . . H28B H 0.0969 0.3815 0.5258 0.104 Uiso 1 1 calc R . . C27 C 0.2404(3) 0.3878(4) 0.5300(2) 0.0747(14) Uani 1 1 d . . . H27A H 0.2460 0.3400 0.5719 0.090 Uiso 1 1 calc R . . H27B H 0.2639 0.4757 0.5404 0.090 Uiso 1 1 calc R . . C26 C 0.2984(2) 0.3240(3) 0.48570(14) 0.0423(7) Uani 1 1 d . . . H26A H 0.3338 0.3880 0.4645 0.051 Uiso 1 1 calc R . . H26B H 0.3459 0.2643 0.5112 0.051 Uiso 1 1 calc R . . O3 O 0.42202(11) 0.24796(16) 0.38086(8) 0.0266(4) Uani 1 1 d . . . C33 C 0.50919(17) 0.2182(2) 0.43014(12) 0.0297(5) Uani 1 1 d . . . H33A H 0.5256 0.1269 0.4285 0.036 Uiso 1 1 calc R . . H33B H 0.4993 0.2388 0.4750 0.036 Uiso 1 1 calc R . . C32 C 0.58858(18) 0.2999(3) 0.41232(14) 0.0369(6) Uani 1 1 d . . . H32A H 0.6195 0.2576 0.3791 0.044 Uiso 1 1 calc R . . H32B H 0.6387 0.3203 0.4517 0.044 Uiso 1 1 calc R . . C31 C 0.5335(2) 0.4183(3) 0.38424(14) 0.0361(6) Uani 1 1 d . . . H31A H 0.5200 0.4748 0.4197 0.043 Uiso 1 1 calc R . . H31B H 0.5692 0.4665 0.3556 0.043 Uiso 1 1 calc R . . C30 C 0.44134(19) 0.3610(3) 0.34500(14) 0.0344(6) Uani 1 1 d . . . H30A H 0.3871 0.4222 0.3413 0.041 Uiso 1 1 calc R . . H30B H 0.4498 0.3382 0.3001 0.041 Uiso 1 1 calc R . . C1 C 0.36362(17) -0.0151(2) 0.45062(12) 0.0297(5) Uani 1 1 d . . . H1A H 0.4155 -0.0712 0.4409 0.036 Uiso 1 1 calc R . . H1B H 0.3897 0.0432 0.4874 0.036 Uiso 1 1 calc R . . C2 C 0.27937(19) -0.0844(2) 0.46080(12) 0.0289(5) Uani 1 1 d . . . C7 C 0.24531(19) -0.1930(3) 0.42291(13) 0.0338(6) Uani 1 1 d . . . H7A H 0.2824 -0.2261 0.3931 0.041 Uiso 1 1 calc R . . C6 C 0.1593(2) -0.2524(3) 0.42797(14) 0.0428(7) Uani 1 1 d . . . H6A H 0.1388 -0.3252 0.4017 0.051 Uiso 1 1 calc R . . C5 C 0.1029(2) -0.2075(3) 0.47057(15) 0.0481(8) Uani 1 1 d . . . H5A H 0.0438 -0.2484 0.4737 0.058 Uiso 1 1 calc R . . C4 C 0.1343(2) -0.1014(3) 0.50873(14) 0.0441(7) Uani 1 1 d . . . H4A H 0.0966 -0.0698 0.5386 0.053 Uiso 1 1 calc R . . C3 C 0.21995(19) -0.0408(3) 0.50385(12) 0.0334(6) Uani 1 1 d . . . H3A H 0.2393 0.0323 0.5302 0.040 Uiso 1 1 calc R . . C8 C 0.08782(17) 0.0602(3) 0.33438(12) 0.0292(5) Uani 1 1 d . . . H8A H 0.0713 -0.0046 0.3651 0.035 Uiso 1 1 calc R . . H8B H 0.0496 0.1388 0.3359 0.035 Uiso 1 1 calc R . . C9 C 0.08338(16) 0.0127(2) 0.26846(12) 0.0260(5) Uani 1 1 d . . . C14 C 0.05853(18) 0.0944(2) 0.21292(13) 0.0296(5) Uani 1 1 d . . . H14A H 0.0387 0.1791 0.2193 0.036 Uiso 1 1 calc R . . C13 C 0.06243(19) 0.0542(3) 0.15012(13) 0.0340(6) Uani 1 1 d . . . H13A H 0.0447 0.1114 0.1142 0.041 Uiso 1 1 calc R . . C12 C 0.09190(19) -0.0687(3) 0.13839(13) 0.0322(6) Uani 1 1 d . . . H12A H 0.0957 -0.0954 0.0951 0.039 Uiso 1 1 calc R . . C11 C 0.11544(18) -0.1509(3) 0.19137(13) 0.0311(5) Uani 1 1 d . . . H11A H 0.1343 -0.2357 0.1842 0.037 Uiso 1 1 calc R . . C10 C 0.11197(18) -0.1113(2) 0.25484(13) 0.0284(5) Uani 1 1 d . . . H10A H 0.1294 -0.1697 0.2902 0.034 Uiso 1 1 calc R . . C15 C 0.33630(18) 0.0583(2) 0.24306(12) 0.0281(5) Uani 1 1 d . . . H15A H 0.2868 0.0247 0.2063 0.034 Uiso 1 1 calc R . . H15B H 0.3698 0.1326 0.2284 0.034 Uiso 1 1 calc R . . C16 C 0.40187(17) -0.0380(2) 0.27561(11) 0.0260(5) Uani 1 1 d . . . C21 C 0.37472(18) -0.1658(3) 0.28054(13) 0.0315(5) Uani 1 1 d . . . H21A H 0.3126 -0.1925 0.2578 0.038 Uiso 1 1 calc R . . C20 C 0.4355(2) -0.2542(3) 0.31738(14) 0.0375(6) Uani 1 1 d . . . H20A H 0.4150 -0.3402 0.3184 0.045 Uiso 1 1 calc R . . C19 C 0.5257(2) -0.2190(3) 0.35278(14) 0.0383(6) Uani 1 1 d . . . H19A H 0.5664 -0.2790 0.3793 0.046 Uiso 1 1 calc R . . C18 C 0.55499(19) -0.0940(3) 0.34846(14) 0.0371(6) Uani 1 1 d . . . H18A H 0.6170 -0.0684 0.3719 0.045 Uiso 1 1 calc R . . C17 C 0.49556(17) -0.0057(3) 0.31067(13) 0.0317(5) Uani 1 1 d . . . H17A H 0.5182 0.0790 0.3082 0.038 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 Nd1 0.01910(7) 0.02069(7) 0.02232(7) 0.00273(5) 0.00133(5) 0.00010(4) O1 0.0265(8) 0.0258(9) 0.0269(8) 0.0066(7) 0.0057(7) 0.0051(7) C25 0.0291(13) 0.0390(15) 0.0281(13) 0.0094(11) 0.0064(10) 0.0036(11) C24 0.0396(16) 0.0509(18) 0.0383(16) 0.0190(14) 0.0068(12) 0.0124(13) C23 0.0336(14) 0.0290(14) 0.0559(18) 0.0149(13) 0.0127(13) 0.0074(11) C22 0.0342(14) 0.0272(13) 0.0390(15) 0.0061(11) 0.0109(11) 0.0077(10) O2 0.0255(8) 0.0348(10) 0.0249(9) -0.0046(7) 0.0041(7) -0.0008(7) C29 0.0312(14) 0.0443(17) 0.0369(15) -0.0103(12) 0.0121(11) -0.0068(12) C28 0.053(2) 0.113(4) 0.103(3) -0.077(3) 0.035(2) -0.025(2) C27 0.046(2) 0.109(4) 0.065(2) -0.056(2) 0.0003(18) 0.006(2) C26 0.0346(14) 0.0523(19) 0.0374(15) -0.0156(13) 0.0010(12) -0.0028(13) O3 0.0212(8) 0.0270(9) 0.0290(9) 0.0079(7) -0.0014(7) -0.0031(6) C33 0.0244(12) 0.0301(13) 0.0314(13) 0.0058(10) -0.0025(10) -0.0001(10) C32 0.0262(12) 0.0386(15) 0.0419(15) 0.0069(12) -0.0031(11) -0.0049(11) C31 0.0329(14) 0.0341(15) 0.0379(15) 0.0053(11) -0.0011(11) -0.0103(11) C30 0.0296(13) 0.0325(14) 0.0375(15) 0.0139(11) -0.0021(11) -0.0070(11) C1 0.0261(12) 0.0303(13) 0.0308(13) 0.0097(10) 0.0006(10) 0.0003(10) C2 0.0303(13) 0.0301(13) 0.0235(12) 0.0095(10) -0.0014(10) -0.0008(10) C7 0.0387(14) 0.0330(14) 0.0287(13) 0.0072(11) 0.0045(11) -0.0001(11) C6 0.0522(18) 0.0382(16) 0.0365(15) 0.0010(12) 0.0048(13) -0.0143(13) C5 0.0472(17) 0.059(2) 0.0393(16) -0.0037(14) 0.0126(13) -0.0274(15) C4 0.0408(16) 0.063(2) 0.0301(15) -0.0054(13) 0.0109(12) -0.0150(14) C3 0.0357(14) 0.0382(15) 0.0239(13) 0.0006(11) 0.0001(10) -0.0073(11) C8 0.0223(12) 0.0340(13) 0.0298(13) -0.0024(10) 0.0020(10) -0.0035(10) C9 0.0163(10) 0.0320(13) 0.0279(12) 0.0011(10) 0.0001(9) -0.0038(9) C14 0.0233(12) 0.0291(13) 0.0346(14) 0.0032(10) 0.0012(10) 0.0019(9) C13 0.0330(14) 0.0371(14) 0.0301(14) 0.0097(11) 0.0018(11) 0.0012(11) C12 0.0308(13) 0.0359(14) 0.0286(13) -0.0005(11) 0.0027(10) -0.0024(11) C11 0.0293(13) 0.0272(13) 0.0351(14) 0.0001(11) 0.0024(10) -0.0013(10) C10 0.0259(12) 0.0279(13) 0.0292(13) 0.0061(10) 0.0000(10) -0.0038(9) C15 0.0275(12) 0.0272(12) 0.0306(13) 0.0026(10) 0.0080(10) 0.0014(10) C16 0.0250(12) 0.0307(13) 0.0237(12) -0.0031(10) 0.0079(9) 0.0019(10) C21 0.0259(12) 0.0332(14) 0.0346(14) -0.0030(11) 0.0041(10) -0.0001(10) C20 0.0372(15) 0.0315(14) 0.0436(16) 0.0029(12) 0.0079(12) 0.0075(11) C19 0.0361(14) 0.0410(16) 0.0357(15) -0.0019(12) 0.0023(11) 0.0151(12) C18 0.0231(12) 0.0509(18) 0.0358(15) -0.0107(12) 0.0022(11) 0.0053(11) C17 0.0248(12) 0.0346(14) 0.0368(14) -0.0083(11) 0.0088(10) 0.0002(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 C1 2.560(2) . ? Nd1 C15 2.570(2) . ? Nd1 C8 2.572(2) . ? Nd1 O1 2.5874(16) . ? Nd1 O2 2.5988(17) . ? Nd1 O3 2.6122(16) . ? Nd1 C9 2.973(2) . ? Nd1 C16 2.984(2) . ? Nd1 C2 3.013(2) . ? O1 C22 1.452(3) . ? O1 C25 1.456(3) . ? C25 C24 1.513(4) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C24 C23 1.523(4) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C23 C22 1.512(4) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? O2 C26 1.446(3) . ? O2 C29 1.456(3) . ? C29 C28 1.494(4) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C28 C27 1.431(5) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C27 C26 1.501(4) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? O3 C30 1.455(3) . ? O3 C33 1.466(3) . ? C33 C32 1.512(4) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C32 C31 1.520(4) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C31 C30 1.513(4) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C1 C2 1.443(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C7 1.413(4) . ? C2 C3 1.414(4) . ? C7 C6 1.386(4) . ? C7 H7A 0.9500 . ? C6 C5 1.381(4) . ? C6 H6A 0.9500 . ? C5 C4 1.387(4) . ? C5 H5A 0.9500 . ? C4 C3 1.386(4) . ? C4 H4A 0.9500 . ? C3 H3A 0.9500 . ? C8 C9 1.442(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.409(3) . ? C9 C14 1.422(3) . ? C14 C13 1.377(4) . ? C14 H14A 0.9500 . ? C13 C12 1.393(4) . ? C13 H13A 0.9500 . ? C12 C11 1.383(4) . ? C12 H12A 0.9500 . ? C11 C10 1.387(4) . ? C11 H11A 0.9500 . ? C10 H10A 0.9500 . ? C15 C16 1.444(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C21 1.406(4) . ? C16 C17 1.416(3) . ? C21 C20 1.385(4) . ? C21 H21A 0.9500 . ? C20 C19 1.386(4) . ? C20 H20A 0.9500 . ? C19 C18 1.386(4) . ? C19 H19A 0.9500 . ? C18 C17 1.384(4) . ? C18 H18A 0.9500 . ? C17 H17A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Nd1 C15 114.08(8) . . ? C1 Nd1 C8 110.65(8) . . ? C15 Nd1 C8 113.27(8) . . ? C1 Nd1 O1 150.16(7) . . ? C15 Nd1 O1 79.85(7) . . ? C8 Nd1 O1 84.94(7) . . ? C1 Nd1 O2 82.47(7) . . ? C15 Nd1 O2 150.63(7) . . ? C8 Nd1 O2 79.94(7) . . ? O1 Nd1 O2 75.23(5) . . ? C1 Nd1 O3 79.21(7) . . ? C15 Nd1 O3 84.73(7) . . ? C8 Nd1 O3 151.09(7) . . ? O1 Nd1 O3 75.90(5) . . ? O2 Nd1 O3 74.40(5) . . ? C1 Nd1 C9 124.38(7) . . ? C15 Nd1 C9 84.37(7) . . ? C8 Nd1 C9 29.01(7) . . ? O1 Nd1 C9 81.61(6) . . ? O2 Nd1 C9 106.80(6) . . ? O3 Nd1 C9 156.40(6) . . ? C1 Nd1 C16 85.37(8) . . ? C15 Nd1 C16 28.93(7) . . ? C8 Nd1 C16 124.66(8) . . ? O1 Nd1 C16 107.04(6) . . ? O2 Nd1 C16 155.24(6) . . ? O3 Nd1 C16 82.19(6) . . ? C9 Nd1 C16 97.88(7) . . ? C1 Nd1 C2 28.57(7) . . ? C15 Nd1 C2 125.24(8) . . ? C8 Nd1 C2 82.40(8) . . ? O1 Nd1 C2 154.79(6) . . ? O2 Nd1 C2 81.14(7) . . ? O3 Nd1 C2 106.21(6) . . ? C9 Nd1 C2 97.18(7) . . ? C16 Nd1 C2 98.08(7) . . ? C22 O1 C25 108.56(18) . . ? C22 O1 Nd1 127.72(14) . . ? C25 O1 Nd1 123.54(14) . . ? O1 C25 C24 106.1(2) . . ? O1 C25 H25A 110.5 . . ? C24 C25 H25A 110.5 . . ? O1 C25 H25B 110.5 . . ? C24 C25 H25B 110.5 . . ? H25A C25 H25B 108.7 . . ? C25 C24 C23 102.2(2) . . ? C25 C24 H24A 111.3 . . ? C23 C24 H24A 111.3 . . ? C25 C24 H24B 111.3 . . ? C23 C24 H24B 111.3 . . ? H24A C24 H24B 109.2 . . ? C22 C23 C24 101.5(2) . . ? C22 C23 H23A 111.5 . . ? C24 C23 H23A 111.5 . . ? C22 C23 H23B 111.5 . . ? C24 C23 H23B 111.5 . . ? H23A C23 H23B 109.3 . . ? O1 C22 C23 105.8(2) . . ? O1 C22 H22A 110.6 . . ? C23 C22 H22A 110.6 . . ? O1 C22 H22B 110.6 . . ? C23 C22 H22B 110.6 . . ? H22A C22 H22B 108.7 . . ? C26 O2 C29 108.48(19) . . ? C26 O2 Nd1 126.22(15) . . ? C29 O2 Nd1 124.88(14) . . ? O2 C29 C28 105.5(2) . . ? O2 C29 H29A 110.7 . . ? C28 C29 H29A 110.7 . . ? O2 C29 H29B 110.7 . . ? C28 C29 H29B 110.7 . . ? H29A C29 H29B 108.8 . . ? C27 C28 C29 105.4(3) . . ? C27 C28 H28A 110.7 . . ? C29 C28 H28A 110.7 . . ? C27 C28 H28B 110.7 . . ? C29 C28 H28B 110.7 . . ? H28A C28 H28B 108.8 . . ? C28 C27 C26 106.4(3) . . ? C28 C27 H27A 110.4 . . ? C26 C27 H27A 110.4 . . ? C28 C27 H27B 110.4 . . ? C26 C27 H27B 110.4 . . ? H27A C27 H27B 108.6 . . ? O2 C26 C27 106.2(2) . . ? O2 C26 H26A 110.5 . . ? C27 C26 H26A 110.5 . . ? O2 C26 H26B 110.5 . . ? C27 C26 H26B 110.5 . . ? H26A C26 H26B 108.7 . . ? C30 O3 C33 108.24(17) . . ? C30 O3 Nd1 125.41(13) . . ? C33 O3 Nd1 125.46(13) . . ? O3 C33 C32 105.54(19) . . ? O3 C33 H33A 110.6 . . ? C32 C33 H33A 110.6 . . ? O3 C33 H33B 110.6 . . ? C32 C33 H33B 110.6 . . ? H33A C33 H33B 108.8 . . ? C33 C32 C31 102.2(2) . . ? C33 C32 H32A 111.3 . . ? C31 C32 H32A 111.3 . . ? C33 C32 H32B 111.3 . . ? C31 C32 H32B 111.3 . . ? H32A C32 H32B 109.2 . . ? C30 C31 C32 101.5(2) . . ? C30 C31 H31A 111.5 . . ? C32 C31 H31A 111.5 . . ? C30 C31 H31B 111.5 . . ? C32 C31 H31B 111.5 . . ? H31A C31 H31B 109.3 . . ? O3 C30 C31 106.2(2) . . ? O3 C30 H30A 110.5 . . ? C31 C30 H30A 110.5 . . ? O3 C30 H30B 110.5 . . ? C31 C30 H30B 110.5 . . ? H30A C30 H30B 108.7 . . ? C2 C1 Nd1 93.40(14) . . ? C2 C1 H1A 113.0 . . ? Nd1 C1 H1A 113.0 . . ? C2 C1 H1B 113.0 . . ? Nd1 C1 H1B 113.0 . . ? H1A C1 H1B 110.4 . . ? C7 C2 C3 115.7(2) . . ? C7 C2 C1 121.7(2) . . ? C3 C2 C1 122.3(2) . . ? C7 C2 Nd1 97.79(15) . . ? C3 C2 Nd1 109.74(17) . . ? C1 C2 Nd1 58.03(12) . . ? C6 C7 C2 121.9(3) . . ? C6 C7 H7A 119.1 . . ? C2 C7 H7A 119.1 . . ? C5 C6 C7 121.1(3) . . ? C5 C6 H6A 119.5 . . ? C7 C6 H6A 119.5 . . ? C6 C5 C4 118.6(3) . . ? C6 C5 H5A 120.7 . . ? C4 C5 H5A 120.7 . . ? C3 C4 C5 120.8(3) . . ? C3 C4 H4A 119.6 . . ? C5 C4 H4A 119.6 . . ? C4 C3 C2 122.0(3) . . ? C4 C3 H3A 119.0 . . ? C2 C3 H3A 119.0 . . ? C9 C8 Nd1 91.13(14) . . ? C9 C8 H8A 113.4 . . ? Nd1 C8 H8A 113.4 . . ? C9 C8 H8B 113.4 . . ? Nd1 C8 H8B 113.4 . . ? H8A C8 H8B 110.7 . . ? C10 C9 C14 115.6(2) . . ? C10 C9 C8 123.3(2) . . ? C14 C9 C8 120.8(2) . . ? C10 C9 Nd1 98.11(14) . . ? C14 C9 Nd1 108.20(15) . . ? C8 C9 Nd1 59.86(12) . . ? C13 C14 C9 121.8(2) . . ? C13 C14 H14A 119.1 . . ? C9 C14 H14A 119.1 . . ? C14 C13 C12 121.2(2) . . ? C14 C13 H13A 119.4 . . ? C12 C13 H13A 119.4 . . ? C11 C12 C13 118.3(3) . . ? C11 C12 H12A 120.9 . . ? C13 C12 H12A 120.9 . . ? C12 C11 C10 121.0(3) . . ? C12 C11 H11A 119.5 . . ? C10 C11 H11A 119.5 . . ? C11 C10 C9 122.1(2) . . ? C11 C10 H10A 119.0 . . ? C9 C10 H10A 119.0 . . ? C16 C15 Nd1 91.66(14) . . ? C16 C15 H15A 113.3 . . ? Nd1 C15 H15A 113.3 . . ? C16 C15 H15B 113.3 . . ? Nd1 C15 H15B 113.3 . . ? H15A C15 H15B 110.7 . . ? C21 C16 C17 115.6(2) . . ? C21 C16 C15 123.1(2) . . ? C17 C16 C15 121.0(2) . . ? C21 C16 Nd1 103.00(15) . . ? C17 C16 Nd1 103.37(15) . . ? C15 C16 Nd1 59.41(12) . . ? C20 C21 C16 122.2(2) . . ? C20 C21 H21A 118.9 . . ? C16 C21 H21A 118.9 . . ? C21 C20 C19 120.9(3) . . ? C21 C20 H20A 119.5 . . ? C19 C20 H20A 119.5 . . ? C18 C19 C20 118.2(3) . . ? C18 C19 H19A 120.9 . . ? C20 C19 H19A 120.9 . . ? C17 C18 C19 121.2(3) . . ? C17 C18 H18A 119.4 . . ? C19 C18 H18A 119.4 . . ? C18 C17 C16 121.8(3) . . ? C18 C17 H17A 119.1 . . ? C16 C17 H17A 119.1 . . ? 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 C1 Nd1 O1 C22 -56.2(2) . . . . ? C15 Nd1 O1 C22 -177.6(2) . . . . ? C8 Nd1 O1 C22 67.68(19) . . . . ? O2 Nd1 O1 C22 -13.24(18) . . . . ? O3 Nd1 O1 C22 -90.50(19) . . . . ? C9 Nd1 O1 C22 96.70(19) . . . . ? C16 Nd1 O1 C22 -167.58(18) . . . . ? C2 Nd1 O1 C22 7.7(3) . . . . ? C1 Nd1 O1 C25 129.12(19) . . . . ? C15 Nd1 O1 C25 7.73(17) . . . . ? C8 Nd1 O1 C25 -107.03(17) . . . . ? O2 Nd1 O1 C25 172.06(17) . . . . ? O3 Nd1 O1 C25 94.79(17) . . . . ? C9 Nd1 O1 C25 -78.00(17) . . . . ? C16 Nd1 O1 C25 17.72(18) . . . . ? C2 Nd1 O1 C25 -167.05(17) . . . . ? C22 O1 C25 C24 -8.9(3) . . . . ? Nd1 O1 C25 C24 166.64(17) . . . . ? O1 C25 C24 C23 30.2(3) . . . . ? C25 C24 C23 C22 -39.0(3) . . . . ? C25 O1 C22 C23 -16.4(3) . . . . ? Nd1 O1 C22 C23 168.27(16) . . . . ? C24 C23 C22 O1 34.6(3) . . . . ? C1 Nd1 O2 C26 57.5(2) . . . . ? C15 Nd1 O2 C26 -69.7(3) . . . . ? C8 Nd1 O2 C26 170.1(2) . . . . ? O1 Nd1 O2 C26 -102.5(2) . . . . ? O3 Nd1 O2 C26 -23.4(2) . . . . ? C9 Nd1 O2 C26 -178.8(2) . . . . ? C16 Nd1 O2 C26 -3.8(3) . . . . ? C2 Nd1 O2 C26 86.3(2) . . . . ? C1 Nd1 O2 C29 -114.3(2) . . . . ? C15 Nd1 O2 C29 118.5(2) . . . . ? C8 Nd1 O2 C29 -1.68(19) . . . . ? O1 Nd1 O2 C29 85.69(19) . . . . ? O3 Nd1 O2 C29 164.9(2) . . . . ? C9 Nd1 O2 C29 9.4(2) . . . . ? C16 Nd1 O2 C29 -175.57(19) . . . . ? C2 Nd1 O2 C29 -85.46(19) . . . . ? C26 O2 C29 C28 16.7(4) . . . . ? Nd1 O2 C29 C28 -170.3(3) . . . . ? O2 C29 C28 C27 -27.7(5) . . . . ? C29 C28 C27 C26 27.7(5) . . . . ? C29 O2 C26 C27 0.0(4) . . . . ? Nd1 O2 C26 C27 -172.9(2) . . . . ? C28 C27 C26 O2 -17.6(5) . . . . ? C1 Nd1 O3 C30 178.4(2) . . . . ? C15 Nd1 O3 C30 62.6(2) . . . . ? C8 Nd1 O3 C30 -68.2(2) . . . . ? O1 Nd1 O3 C30 -18.24(19) . . . . ? O2 Nd1 O3 C30 -96.54(19) . . . . ? C9 Nd1 O3 C30 -0.2(3) . . . . ? C16 Nd1 O3 C30 91.61(19) . . . . ? C2 Nd1 O3 C30 -172.20(19) . . . . ? C1 Nd1 O3 C33 10.40(18) . . . . ? C15 Nd1 O3 C33 -105.36(18) . . . . ? C8 Nd1 O3 C33 123.8(2) . . . . ? O1 Nd1 O3 C33 173.81(18) . . . . ? O2 Nd1 O3 C33 95.51(18) . . . . ? C9 Nd1 O3 C33 -168.15(18) . . . . ? C16 Nd1 O3 C33 -76.35(18) . . . . ? C2 Nd1 O3 C33 19.84(19) . . . . ? C30 O3 C33 C32 -12.4(3) . . . . ? Nd1 O3 C33 C32 157.30(16) . . . . ? O3 C33 C32 C31 32.9(3) . . . . ? C33 C32 C31 C30 -39.9(3) . . . . ? C33 O3 C30 C31 -13.4(3) . . . . ? Nd1 O3 C30 C31 176.90(16) . . . . ? C32 C31 C30 O3 33.4(3) . . . . ? C15 Nd1 C1 C2 -120.05(16) . . . . ? C8 Nd1 C1 C2 9.06(19) . . . . ? O1 Nd1 C1 C2 126.93(16) . . . . ? O2 Nd1 C1 C2 85.29(16) . . . . ? O3 Nd1 C1 C2 160.76(17) . . . . ? C9 Nd1 C1 C2 -19.9(2) . . . . ? C16 Nd1 C1 C2 -116.33(17) . . . . ? Nd1 C1 C2 C7 78.6(2) . . . . ? Nd1 C1 C2 C3 -94.4(2) . . . . ? C1 Nd1 C2 C7 -122.7(3) . . . . ? C15 Nd1 C2 C7 -47.30(19) . . . . ? C8 Nd1 C2 C7 65.90(17) . . . . ? O1 Nd1 C2 C7 126.41(18) . . . . ? O2 Nd1 C2 C7 146.84(17) . . . . ? O3 Nd1 C2 C7 -142.35(16) . . . . ? C9 Nd1 C2 C7 40.86(17) . . . . ? C16 Nd1 C2 C7 -58.19(17) . . . . ? C1 Nd1 C2 C3 116.5(3) . . . . ? C15 Nd1 C2 C3 -168.19(16) . . . . ? C8 Nd1 C2 C3 -54.99(18) . . . . ? O1 Nd1 C2 C3 5.5(3) . . . . ? O2 Nd1 C2 C3 25.95(17) . . . . ? O3 Nd1 C2 C3 96.76(17) . . . . ? C9 Nd1 C2 C3 -80.03(18) . . . . ? C16 Nd1 C2 C3 -179.08(17) . . . . ? C15 Nd1 C2 C1 75.35(18) . . . . ? C8 Nd1 C2 C1 -171.45(17) . . . . ? O1 Nd1 C2 C1 -110.94(19) . . . . ? O2 Nd1 C2 C1 -90.51(16) . . . . ? O3 Nd1 C2 C1 -19.70(17) . . . . ? C9 Nd1 C2 C1 163.51(16) . . . . ? C16 Nd1 C2 C1 64.46(17) . . . . ? C3 C2 C7 C6 -0.1(4) . . . . ? C1 C2 C7 C6 -173.6(2) . . . . ? Nd1 C2 C7 C6 -116.5(2) . . . . ? C2 C7 C6 C5 0.1(4) . . . . ? C7 C6 C5 C4 -0.3(5) . . . . ? C6 C5 C4 C3 0.6(5) . . . . ? C5 C4 C3 C2 -0.7(5) . . . . ? C7 C2 C3 C4 0.4(4) . . . . ? C1 C2 C3 C4 173.8(3) . . . . ? Nd1 C2 C3 C4 109.8(3) . . . . ? C1 Nd1 C8 C9 -124.38(15) . . . . ? C15 Nd1 C8 C9 5.16(18) . . . . ? O1 Nd1 C8 C9 81.82(15) . . . . ? O2 Nd1 C8 C9 157.68(16) . . . . ? O3 Nd1 C8 C9 130.04(15) . . . . ? C16 Nd1 C8 C9 -25.43(19) . . . . ? C2 Nd1 C8 C9 -120.03(16) . . . . ? Nd1 C8 C9 C10 79.3(2) . . . . ? Nd1 C8 C9 C14 -94.2(2) . . . . ? C1 Nd1 C9 C10 -54.60(18) . . . . ? C15 Nd1 C9 C10 60.82(16) . . . . ? C8 Nd1 C9 C10 -123.9(2) . . . . ? O1 Nd1 C9 C10 141.35(16) . . . . ? O2 Nd1 C9 C10 -146.93(15) . . . . ? O3 Nd1 C9 C10 123.67(18) . . . . ? C16 Nd1 C9 C10 35.17(16) . . . . ? C2 Nd1 C9 C10 -64.06(16) . . . . ? C1 Nd1 C9 C14 -174.98(16) . . . . ? C15 Nd1 C9 C14 -59.56(17) . . . . ? C8 Nd1 C9 C14 115.7(2) . . . . ? O1 Nd1 C9 C14 20.97(17) . . . . ? O2 Nd1 C9 C14 92.68(17) . . . . ? O3 Nd1 C9 C14 3.3(3) . . . . ? C16 Nd1 C9 C14 -85.22(17) . . . . ? C2 Nd1 C9 C14 175.55(17) . . . . ? C1 Nd1 C9 C8 69.34(18) . . . . ? C15 Nd1 C9 C8 -175.24(16) . . . . ? O1 Nd1 C9 C8 -94.71(16) . . . . ? O2 Nd1 C9 C8 -22.99(16) . . . . ? O3 Nd1 C9 C8 -112.39(19) . . . . ? C16 Nd1 C9 C8 159.11(16) . . . . ? C2 Nd1 C9 C8 59.88(16) . . . . ? C10 C9 C14 C13 0.0(3) . . . . ? C8 C9 C14 C13 173.9(2) . . . . ? Nd1 C9 C14 C13 108.7(2) . . . . ? C9 C14 C13 C12 -0.6(4) . . . . ? C14 C13 C12 C11 1.3(4) . . . . ? C13 C12 C11 C10 -1.4(4) . . . . ? C12 C11 C10 C9 0.9(4) . . . . ? C14 C9 C10 C11 -0.1(3) . . . . ? C8 C9 C10 C11 -173.9(2) . . . . ? Nd1 C9 C10 C11 -114.8(2) . . . . ? C1 Nd1 C15 C16 7.69(18) . . . . ? C8 Nd1 C15 C16 -120.09(15) . . . . ? O1 Nd1 C15 C16 159.96(16) . . . . ? O2 Nd1 C15 C16 127.78(15) . . . . ? O3 Nd1 C15 C16 83.38(15) . . . . ? C9 Nd1 C15 C16 -117.58(15) . . . . ? C2 Nd1 C15 C16 -22.76(18) . . . . ? Nd1 C15 C16 C21 85.8(2) . . . . ? Nd1 C15 C16 C17 -87.6(2) . . . . ? C1 Nd1 C16 C21 66.11(16) . . . . ? C15 Nd1 C16 C21 -120.9(2) . . . . ? C8 Nd1 C16 C21 -45.86(19) . . . . ? O1 Nd1 C16 C21 -141.58(15) . . . . ? O2 Nd1 C16 C21 126.82(17) . . . . ? O3 Nd1 C16 C21 145.84(16) . . . . ? C9 Nd1 C16 C21 -57.99(16) . . . . ? C2 Nd1 C16 C21 40.47(16) . . . . ? C1 Nd1 C16 C17 -54.58(17) . . . . ? C15 Nd1 C16 C17 118.4(2) . . . . ? C8 Nd1 C16 C17 -166.55(16) . . . . ? O1 Nd1 C16 C17 97.73(17) . . . . ? O2 Nd1 C16 C17 6.1(3) . . . . ? O3 Nd1 C16 C17 25.14(16) . . . . ? C9 Nd1 C16 C17 -178.68(17) . . . . ? C2 Nd1 C16 C17 -80.23(17) . . . . ? C1 Nd1 C16 C15 -172.96(16) . . . . ? C8 Nd1 C16 C15 75.07(17) . . . . ? O1 Nd1 C16 C15 -20.66(16) . . . . ? O2 Nd1 C16 C15 -112.25(18) . . . . ? O3 Nd1 C16 C15 -93.24(15) . . . . ? C9 Nd1 C16 C15 62.93(16) . . . . ? C2 Nd1 C16 C15 161.39(15) . . . . ? C17 C16 C21 C20 0.2(4) . . . . ? C15 C16 C21 C20 -173.6(2) . . . . ? Nd1 C16 C21 C20 -111.8(2) . . . . ? C16 C21 C20 C19 1.8(4) . . . . ? C21 C20 C19 C18 -2.3(4) . . . . ? C20 C19 C18 C17 0.9(4) . . . . ? C19 C18 C17 C16 1.0(4) . . . . ? C21 C16 C17 C18 -1.5(4) . . . . ? C15 C16 C17 C18 172.3(2) . . . . ? Nd1 C16 C17 C18 110.2(2) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.027 _refine_diff_density_min -0.896 _refine_diff_density_rms 0.080 # Attachment '5.cif' data_5 _database_code_depnum_ccdc_archive 'CCDC 736119' _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H45 O3 Sm' _chemical_formula_sum 'C33 H45 O3 Sm' _chemical_formula_weight 640.04 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' O O 0.0106 0.0060 '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 'P2(1)/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.1881(7) _cell_length_b 11.2673(6) _cell_length_c 18.8608(9) _cell_angle_alpha 90.00 _cell_angle_beta 100.381(2) _cell_angle_gamma 90.00 _cell_volume 2965.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3945 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 24.48 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.433 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1316 _exptl_absorpt_coefficient_mu 2.010 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.64 _exptl_absorpt_correction_T_max 0.85 _exptl_absorpt_process_details '(SADABS; Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 18412 _diffrn_reflns_av_R_equivalents 0.0483 _diffrn_reflns_av_sigmaI/netI 0.0666 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 27.52 _reflns_number_total 6770 _reflns_number_gt 4741 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'enCIFer(Allen et al.,2004);PLATON(Spek,2003)' _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^)+(0.0218P)^2^+1.8105P] 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 6770 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0726 _refine_ls_R_factor_gt 0.0345 _refine_ls_wR_factor_ref 0.0750 _refine_ls_wR_factor_gt 0.0619 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 Sm1 Sm 0.239269(13) 0.682244(18) 0.245155(11) 0.02144(6) Uani 1 1 d . . . C1 C 0.1889(3) 0.8461(4) 0.3228(2) 0.0284(10) Uani 1 1 d . . . H1A H 0.2441 0.8789 0.3568 0.034 Uiso 1 1 calc R . . H1B H 0.1549 0.9110 0.2933 0.034 Uiso 1 1 calc R . . C2 C 0.1247(3) 0.7783(4) 0.3599(2) 0.0254(9) Uani 1 1 d . . . C3 C 0.0249(3) 0.7817(4) 0.3398(2) 0.0289(10) Uani 1 1 d . . . H3A H -0.0025 0.8354 0.3030 0.035 Uiso 1 1 calc R . . C4 C -0.0352(3) 0.7114(4) 0.3706(2) 0.0398(12) Uani 1 1 d . . . H4A H -0.1025 0.7168 0.3548 0.048 Uiso 1 1 calc R . . C5 C 0.0016(3) 0.6321(4) 0.4249(2) 0.0395(12) Uani 1 1 d . . . H5A H -0.0399 0.5829 0.4463 0.047 Uiso 1 1 calc R . . C6 C 0.0989(3) 0.6260(4) 0.4470(2) 0.0392(12) Uani 1 1 d . . . H6A H 0.1253 0.5724 0.4842 0.047 Uiso 1 1 calc R . . C7 C 0.1587(3) 0.6973(4) 0.4155(2) 0.0326(10) Uani 1 1 d . . . H7A H 0.2259 0.6915 0.4320 0.039 Uiso 1 1 calc R . . C8 C 0.1811(3) 0.4829(4) 0.2793(2) 0.0287(10) Uani 1 1 d . . . H8A H 0.1344 0.4957 0.3117 0.034 Uiso 1 1 calc R . . H8B H 0.1465 0.4440 0.2351 0.034 Uiso 1 1 calc R . . C9 C 0.2555(3) 0.4015(4) 0.3149(2) 0.0260(9) Uani 1 1 d . . . C10 C 0.2900(3) 0.4042(4) 0.3901(2) 0.0264(9) Uani 1 1 d . . . H10A H 0.2638 0.4600 0.4189 0.032 Uiso 1 1 calc R . . C11 C 0.3612(3) 0.3272(4) 0.4225(2) 0.0354(10) Uani 1 1 d . . . H11A H 0.3824 0.3301 0.4732 0.042 Uiso 1 1 calc R . . C12 C 0.4015(3) 0.2464(4) 0.3817(3) 0.0394(12) Uani 1 1 d . . . H12A H 0.4504 0.1938 0.4039 0.047 Uiso 1 1 calc R . . C13 C 0.3696(3) 0.2435(4) 0.3083(3) 0.0355(11) Uani 1 1 d . . . H13A H 0.3974 0.1888 0.2798 0.043 Uiso 1 1 calc R . . C14 C 0.2987(3) 0.3177(4) 0.2758(2) 0.0306(9) Uani 1 1 d . . . H14A H 0.2779 0.3126 0.2251 0.037 Uiso 1 1 calc R . . C15 C 0.4144(3) 0.6253(4) 0.2576(2) 0.0305(10) Uani 1 1 d . . . H15A H 0.4283 0.5416 0.2716 0.037 Uiso 1 1 calc R . . H15B H 0.4440 0.6480 0.2159 0.037 Uiso 1 1 calc R . . C16 C 0.4319(2) 0.7077(4) 0.3167(2) 0.0251(10) Uani 1 1 d . . . C17 C 0.4485(3) 0.8303(4) 0.3059(2) 0.0298(10) Uani 1 1 d . . . H17A H 0.4579 0.8564 0.2597 0.036 Uiso 1 1 calc R . . C18 C 0.4514(3) 0.9118(4) 0.3601(2) 0.0344(11) Uani 1 1 d . . . H18A H 0.4619 0.9931 0.3506 0.041 Uiso 1 1 calc R . . C19 C 0.4392(3) 0.8785(5) 0.4285(2) 0.0384(12) Uani 1 1 d . . . H19A H 0.4409 0.9358 0.4656 0.046 Uiso 1 1 calc R . . C20 C 0.4246(3) 0.7604(5) 0.4415(2) 0.0382(12) Uani 1 1 d . . . H20A H 0.4174 0.7360 0.4884 0.046 Uiso 1 1 calc R . . C21 C 0.4202(3) 0.6762(4) 0.3873(2) 0.0329(10) Uani 1 1 d . . . H21A H 0.4090 0.5955 0.3978 0.040 Uiso 1 1 calc R . . O1 O 0.23483(18) 0.5862(3) 0.12157(14) 0.0288(7) Uani 1 1 d . . . C22 C 0.1562(3) 0.5807(5) 0.0608(2) 0.0455(13) Uani 1 1 d . . . H22A H 0.1406 0.6612 0.0412 0.055 Uiso 1 1 calc R . . H22B H 0.0985 0.5472 0.0761 0.055 Uiso 1 1 calc R . . C23 C 0.1863(4) 0.5050(5) 0.0061(3) 0.0624(17) Uani 1 1 d . . . H23A H 0.2149 0.5529 -0.0287 0.075 Uiso 1 1 calc R . . H23B H 0.1314 0.4596 -0.0205 0.075 Uiso 1 1 calc R . . C24 C 0.2598(4) 0.4230(5) 0.0481(3) 0.0507(14) Uani 1 1 d . . . H24A H 0.2292 0.3550 0.0683 0.061 Uiso 1 1 calc R . . H24B H 0.3052 0.3931 0.0182 0.061 Uiso 1 1 calc R . . C25 C 0.3082(3) 0.5051(4) 0.1066(2) 0.0389(12) Uani 1 1 d . . . H25A H 0.3355 0.4596 0.1504 0.047 Uiso 1 1 calc R . . H25B H 0.3606 0.5494 0.0901 0.047 Uiso 1 1 calc R . . O2 O 0.07067(17) 0.7024(3) 0.18022(14) 0.0274(7) Uani 1 1 d . . . C26 C 0.0340(3) 0.8076(4) 0.1403(2) 0.0313(10) Uani 1 1 d . . . H26A H 0.0757 0.8301 0.1056 0.038 Uiso 1 1 calc R . . H26B H 0.0309 0.8751 0.1734 0.038 Uiso 1 1 calc R . . C27 C -0.0649(3) 0.7753(4) 0.1011(2) 0.0304(10) Uani 1 1 d . . . H27A H -0.0625 0.7349 0.0548 0.036 Uiso 1 1 calc R . . H27B H -0.1067 0.8459 0.0920 0.036 Uiso 1 1 calc R . . C28 C -0.0981(3) 0.6915(4) 0.1548(2) 0.0303(10) Uani 1 1 d . . . H28A H -0.1205 0.7361 0.1939 0.036 Uiso 1 1 calc R . . H28B H -0.1503 0.6393 0.1308 0.036 Uiso 1 1 calc R . . C29 C -0.0095(3) 0.6214(4) 0.1833(2) 0.0312(10) Uani 1 1 d . . . H29A H -0.0094 0.5957 0.2335 0.037 Uiso 1 1 calc R . . H29B H -0.0053 0.5503 0.1532 0.037 Uiso 1 1 calc R . . O3 O 0.27065(19) 0.8554(2) 0.16438(14) 0.0271(7) Uani 1 1 d . . . C30 C 0.3248(3) 0.8424(4) 0.1065(2) 0.0327(11) Uani 1 1 d . . . H30A H 0.2818 0.8210 0.0609 0.039 Uiso 1 1 calc R . . H30B H 0.3740 0.7797 0.1182 0.039 Uiso 1 1 calc R . . C31 C 0.3715(4) 0.9614(5) 0.0993(3) 0.0482(13) Uani 1 1 d . . . H31A H 0.4353 0.9659 0.1307 0.058 Uiso 1 1 calc R . . H31B H 0.3785 0.9766 0.0488 0.058 Uiso 1 1 calc R . . C32 C 0.3034(4) 1.0470(5) 0.1231(3) 0.0492(13) Uani 1 1 d . . . H32A H 0.2521 1.0692 0.0824 0.059 Uiso 1 1 calc R . . H32B H 0.3372 1.1198 0.1431 0.059 Uiso 1 1 calc R . . C33 C 0.2624(3) 0.9810(4) 0.1806(2) 0.0347(11) Uani 1 1 d . . . H33A H 0.2990 0.9997 0.2291 0.042 Uiso 1 1 calc R . . H33B H 0.1945 1.0031 0.1789 0.042 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 0.02076(11) 0.02084(10) 0.02248(10) -0.00138(11) 0.00327(7) -0.00017(10) C1 0.029(2) 0.030(3) 0.026(2) -0.0050(18) 0.0051(18) 0.0010(18) C2 0.030(2) 0.025(2) 0.021(2) -0.0092(16) 0.0057(18) 0.0001(17) C3 0.027(2) 0.030(3) 0.031(2) 0.0011(18) 0.0078(18) 0.0027(18) C4 0.030(2) 0.051(4) 0.038(3) -0.006(2) 0.005(2) -0.002(2) C5 0.047(3) 0.040(3) 0.035(3) -0.001(2) 0.017(2) -0.009(2) C6 0.046(3) 0.038(3) 0.033(3) 0.006(2) 0.007(2) 0.001(2) C7 0.034(2) 0.038(3) 0.026(2) -0.004(2) 0.0043(18) 0.002(2) C8 0.028(2) 0.026(3) 0.034(2) -0.0024(18) 0.0096(19) -0.0013(18) C9 0.023(2) 0.020(2) 0.035(2) -0.0008(18) 0.0060(18) -0.0046(17) C10 0.027(2) 0.019(2) 0.035(2) -0.0020(17) 0.0096(18) -0.0039(17) C11 0.034(2) 0.032(3) 0.037(2) -0.001(2) -0.0024(19) -0.002(2) C12 0.028(2) 0.032(3) 0.055(3) -0.005(2) 0.000(2) 0.005(2) C13 0.023(2) 0.034(3) 0.051(3) -0.009(2) 0.010(2) -0.0003(19) C14 0.030(2) 0.030(2) 0.033(2) -0.008(2) 0.0092(17) -0.004(2) C15 0.020(2) 0.034(3) 0.039(3) -0.005(2) 0.0067(18) -0.0010(18) C16 0.0146(18) 0.031(3) 0.029(2) 0.0011(18) 0.0016(16) -0.0030(16) C17 0.026(2) 0.033(3) 0.030(2) 0.000(2) 0.0036(17) -0.007(2) C18 0.026(2) 0.029(3) 0.046(3) -0.004(2) 0.003(2) -0.0093(19) C19 0.032(3) 0.046(3) 0.036(3) -0.014(2) 0.004(2) -0.009(2) C20 0.029(2) 0.061(4) 0.024(2) 0.002(2) 0.0031(19) -0.009(2) C21 0.025(2) 0.035(3) 0.037(2) 0.011(2) 0.0017(18) -0.008(2) O1 0.0277(15) 0.0306(18) 0.0275(15) -0.0084(12) 0.0037(12) 0.0047(13) C22 0.039(3) 0.060(4) 0.034(3) -0.015(2) -0.004(2) 0.008(2) C23 0.085(4) 0.063(4) 0.033(3) -0.014(3) -0.005(3) 0.018(3) C24 0.073(4) 0.037(3) 0.041(3) -0.014(2) 0.009(3) 0.001(3) C25 0.047(3) 0.035(3) 0.037(3) -0.003(2) 0.013(2) 0.011(2) O2 0.0210(14) 0.028(2) 0.0323(15) 0.0028(13) 0.0026(12) 0.0014(12) C26 0.030(2) 0.031(3) 0.033(2) 0.000(2) 0.0044(18) 0.005(2) C27 0.027(2) 0.033(3) 0.030(2) 0.0025(18) 0.0024(18) 0.0083(18) C28 0.022(2) 0.032(3) 0.037(2) -0.003(2) 0.0028(17) 0.003(2) C29 0.026(2) 0.027(3) 0.041(3) -0.004(2) 0.0040(19) 0.0003(18) O3 0.0305(15) 0.0244(18) 0.0279(15) 0.0000(12) 0.0096(13) -0.0024(12) C30 0.037(2) 0.039(3) 0.024(2) 0.0020(19) 0.0114(19) -0.001(2) C31 0.063(3) 0.043(3) 0.045(3) 0.003(2) 0.026(3) -0.010(3) C32 0.068(3) 0.037(3) 0.047(3) 0.005(2) 0.025(3) -0.012(3) C33 0.039(3) 0.025(3) 0.041(3) -0.003(2) 0.011(2) -0.004(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 Sm1 O2 2.494(2) . ? Sm1 C8 2.517(4) . ? Sm1 C15 2.536(4) . ? Sm1 C1 2.537(4) . ? Sm1 O1 2.560(3) . ? Sm1 O3 2.563(3) . ? Sm1 C16 2.836(3) . ? C1 C2 1.460(6) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.400(5) . ? C2 C7 1.408(6) . ? C3 C4 1.368(6) . ? C3 H3A 0.9500 . ? C4 C5 1.388(6) . ? C4 H4A 0.9500 . ? C5 C6 1.371(6) . ? C5 H5A 0.9500 . ? C6 C7 1.380(6) . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? C8 C9 1.467(5) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C14 1.405(6) . ? C9 C10 1.414(5) . ? C10 C11 1.388(6) . ? C10 H10A 0.9500 . ? C11 C12 1.380(6) . ? C11 H11A 0.9500 . ? C12 C13 1.378(6) . ? C12 H12A 0.9500 . ? C13 C14 1.366(6) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? C15 C16 1.437(6) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C21 1.417(5) . ? C16 C17 1.423(6) . ? C17 C18 1.370(6) . ? C17 H17A 0.9500 . ? C18 C19 1.384(6) . ? C18 H18A 0.9500 . ? C19 C20 1.376(7) . ? C19 H19A 0.9500 . ? C20 C21 1.387(6) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? O1 C22 1.449(5) . ? O1 C25 1.451(5) . ? C22 C23 1.461(6) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.507(7) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.507(6) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? O2 C26 1.450(5) . ? O2 C29 1.467(5) . ? C26 C27 1.508(5) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.520(6) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.500(5) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? O3 C30 1.452(5) . ? O3 C33 1.458(5) . ? C30 C31 1.512(6) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.490(7) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.515(6) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? 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 O2 Sm1 C8 82.95(11) . . ? O2 Sm1 C15 154.94(12) . . ? C8 Sm1 C15 96.41(14) . . ? O2 Sm1 C1 82.64(11) . . ? C8 Sm1 C1 111.24(14) . . ? C15 Sm1 C1 120.24(13) . . ? O2 Sm1 O1 74.18(9) . . ? C8 Sm1 O1 84.27(12) . . ? C15 Sm1 O1 80.82(11) . . ? C1 Sm1 O1 150.40(11) . . ? O2 Sm1 O3 83.83(9) . . ? C8 Sm1 O3 158.67(11) . . ? C15 Sm1 O3 88.59(12) . . ? C1 Sm1 O3 83.48(11) . . ? O1 Sm1 O3 76.05(9) . . ? O2 Sm1 C16 168.93(10) . . ? C8 Sm1 C16 107.51(12) . . ? C15 Sm1 C16 30.37(12) . . ? C1 Sm1 C16 89.97(12) . . ? O1 Sm1 C16 109.83(10) . . ? O3 Sm1 C16 87.15(10) . . ? C2 C1 Sm1 99.3(3) . . ? C2 C1 H1A 111.9 . . ? Sm1 C1 H1A 111.9 . . ? C2 C1 H1B 111.9 . . ? Sm1 C1 H1B 111.9 . . ? H1A C1 H1B 109.6 . . ? C3 C2 C7 114.4(4) . . ? C3 C2 C1 123.0(4) . . ? C7 C2 C1 122.4(4) . . ? C4 C3 C2 123.2(4) . . ? C4 C3 H3A 118.4 . . ? C2 C3 H3A 118.4 . . ? C3 C4 C5 120.4(4) . . ? C3 C4 H4A 119.8 . . ? C5 C4 H4A 119.8 . . ? C6 C5 C4 118.7(4) . . ? C6 C5 H5A 120.6 . . ? C4 C5 H5A 120.6 . . ? C5 C6 C7 120.3(4) . . ? C5 C6 H6A 119.9 . . ? C7 C6 H6A 119.9 . . ? C6 C7 C2 123.0(4) . . ? C6 C7 H7A 118.5 . . ? C2 C7 H7A 118.5 . . ? C9 C8 Sm1 115.7(3) . . ? C9 C8 H8A 108.4 . . ? Sm1 C8 H8A 108.4 . . ? C9 C8 H8B 108.4 . . ? Sm1 C8 H8B 108.4 . . ? H8A C8 H8B 107.4 . . ? C14 C9 C10 115.9(4) . . ? C14 C9 C8 121.7(4) . . ? C10 C9 C8 122.4(4) . . ? C11 C10 C9 121.5(4) . . ? C11 C10 H10A 119.3 . . ? C9 C10 H10A 119.3 . . ? C12 C11 C10 120.5(4) . . ? C12 C11 H11A 119.7 . . ? C10 C11 H11A 119.7 . . ? C13 C12 C11 118.8(4) . . ? C13 C12 H12A 120.6 . . ? C11 C12 H12A 120.6 . . ? C14 C13 C12 121.3(4) . . ? C14 C13 H13A 119.3 . . ? C12 C13 H13A 119.3 . . ? C13 C14 C9 122.1(4) . . ? C13 C14 H14A 119.0 . . ? C9 C14 H14A 119.0 . . ? C16 C15 Sm1 86.5(2) . . ? C16 C15 H15A 114.2 . . ? Sm1 C15 H15A 114.2 . . ? C16 C15 H15B 114.2 . . ? Sm1 C15 H15B 114.2 . . ? H15A C15 H15B 111.4 . . ? C21 C16 C17 115.4(4) . . ? C21 C16 C15 122.3(4) . . ? C17 C16 C15 121.7(4) . . ? C21 C16 Sm1 98.9(2) . . ? C17 C16 Sm1 101.5(2) . . ? C15 C16 Sm1 63.16(19) . . ? C18 C17 C16 121.8(4) . . ? C18 C17 H17A 119.1 . . ? C16 C17 H17A 119.1 . . ? C17 C18 C19 121.5(5) . . ? C17 C18 H18A 119.3 . . ? C19 C18 H18A 119.3 . . ? C20 C19 C18 118.5(4) . . ? C20 C19 H19A 120.8 . . ? C18 C19 H19A 120.8 . . ? C19 C20 C21 121.2(4) . . ? C19 C20 H20A 119.4 . . ? C21 C20 H20A 119.4 . . ? C20 C21 C16 121.6(4) . . ? C20 C21 H21A 119.2 . . ? C16 C21 H21A 119.2 . . ? C22 O1 C25 107.2(3) . . ? C22 O1 Sm1 128.8(2) . . ? C25 O1 Sm1 122.9(2) . . ? O1 C22 C23 107.6(4) . . ? O1 C22 H22A 110.2 . . ? C23 C22 H22A 110.2 . . ? O1 C22 H22B 110.2 . . ? C23 C22 H22B 110.2 . . ? H22A C22 H22B 108.5 . . ? C22 C23 C24 104.4(4) . . ? C22 C23 H23A 110.9 . . ? C24 C23 H23A 110.9 . . ? C22 C23 H23B 110.9 . . ? C24 C23 H23B 110.9 . . ? H23A C23 H23B 108.9 . . ? C25 C24 C23 100.9(4) . . ? C25 C24 H24A 111.6 . . ? C23 C24 H24A 111.6 . . ? C25 C24 H24B 111.6 . . ? C23 C24 H24B 111.6 . . ? H24A C24 H24B 109.4 . . ? O1 C25 C24 106.3(4) . . ? O1 C25 H25A 110.5 . . ? C24 C25 H25A 110.5 . . ? O1 C25 H25B 110.5 . . ? C24 C25 H25B 110.5 . . ? H25A C25 H25B 108.7 . . ? C26 O2 C29 108.8(3) . . ? C26 O2 Sm1 123.5(2) . . ? C29 O2 Sm1 127.2(2) . . ? O2 C26 C27 105.7(3) . . ? O2 C26 H26A 110.6 . . ? C27 C26 H26A 110.6 . . ? O2 C26 H26B 110.6 . . ? C27 C26 H26B 110.6 . . ? H26A C26 H26B 108.7 . . ? C26 C27 C28 101.3(3) . . ? C26 C27 H27A 111.5 . . ? C28 C27 H27A 111.5 . . ? C26 C27 H27B 111.5 . . ? C28 C27 H27B 111.5 . . ? H27A C27 H27B 109.3 . . ? C29 C28 C27 103.0(3) . . ? C29 C28 H28A 111.2 . . ? C27 C28 H28A 111.2 . . ? C29 C28 H28B 111.2 . . ? C27 C28 H28B 111.2 . . ? H28A C28 H28B 109.1 . . ? O2 C29 C28 105.3(3) . . ? O2 C29 H29A 110.7 . . ? C28 C29 H29A 110.7 . . ? O2 C29 H29B 110.7 . . ? C28 C29 H29B 110.7 . . ? H29A C29 H29B 108.8 . . ? C30 O3 C33 109.2(3) . . ? C30 O3 Sm1 122.9(2) . . ? C33 O3 Sm1 125.8(2) . . ? O3 C30 C31 106.1(3) . . ? O3 C30 H30A 110.5 . . ? C31 C30 H30A 110.5 . . ? O3 C30 H30B 110.5 . . ? C31 C30 H30B 110.5 . . ? H30A C30 H30B 108.7 . . ? C32 C31 C30 103.2(4) . . ? C32 C31 H31A 111.1 . . ? C30 C31 H31A 111.1 . . ? C32 C31 H31B 111.1 . . ? C30 C31 H31B 111.1 . . ? H31A C31 H31B 109.1 . . ? C31 C32 C33 104.6(4) . . ? C31 C32 H32A 110.8 . . ? C33 C32 H32A 110.8 . . ? C31 C32 H32B 110.8 . . ? C33 C32 H32B 110.8 . . ? H32A C32 H32B 108.9 . . ? O3 C33 C32 105.7(4) . . ? O3 C33 H33A 110.6 . . ? C32 C33 H33A 110.6 . . ? O3 C33 H33B 110.6 . . ? C32 C33 H33B 110.6 . . ? H33A C33 H33B 108.7 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.242 _refine_diff_density_min -0.874 _refine_diff_density_rms 0.126 # Attachment '6.cif' data_6 _database_code_depnum_ccdc_archive 'CCDC 736120' _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H45 Gd O3' _chemical_formula_sum 'C33 H45 Gd O3' _chemical_formula_weight 646.94 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' O O 0.0106 0.0060 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 17.3415(15) _cell_length_b 20.8466(18) _cell_length_c 8.5133(7) _cell_angle_alpha 90.00 _cell_angle_beta 92.891(2) _cell_angle_gamma 90.00 _cell_volume 3073.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4545 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 27.49 _exptl_crystal_description Columnn _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.398 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1324 _exptl_absorpt_coefficient_mu 2.187 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.47 _exptl_absorpt_correction_T_max 0.76 _exptl_absorpt_process_details '(SADABS; Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 7292 _diffrn_reflns_av_R_equivalents 0.0241 _diffrn_reflns_av_sigmaI/netI 0.0421 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3958 _reflns_number_gt 3628 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'enCIFer(Allen et al.,2004);PLATON(Spek,2003)' _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^)+(0.0467P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.006(16) _refine_ls_number_reflns 3958 _refine_ls_number_parameters 334 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0351 _refine_ls_R_factor_gt 0.0299 _refine_ls_wR_factor_ref 0.0762 _refine_ls_wR_factor_gt 0.0723 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.003 _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 0.25294(3) 0.779344(11) 1.25296(3) 0.02635(9) Uani 1 1 d . . . O1 O 0.3734(2) 0.8064(2) 1.4035(6) 0.0346(10) Uani 1 1 d . . . O2 O 0.2142(4) 0.8627(3) 1.4438(7) 0.0318(15) Uani 1 1 d . . . O3 O 0.2436(3) 0.71325(19) 1.4913(6) 0.0293(10) Uani 1 1 d . . . C1 C 0.2701(6) 0.8632(5) 1.0493(12) 0.039(2) Uani 1 1 d . . . H1A H 0.2453 0.8467 0.9501 0.047 Uiso 1 1 calc R . . H1B H 0.2396 0.9009 1.0801 0.047 Uiso 1 1 calc R . . C2 C 0.3464(4) 0.8870(3) 1.0113(7) 0.0346(15) Uani 1 1 d . . . C3 C 0.3767(5) 0.9448(3) 1.0699(10) 0.0449(18) Uani 1 1 d . . . H3A H 0.3446 0.9715 1.1294 0.054 Uiso 1 1 calc R . . C4 C 0.4513(5) 0.9653(4) 1.0454(11) 0.055(2) Uani 1 1 d . . . H4A H 0.4702 1.0039 1.0925 0.066 Uiso 1 1 calc R . . C5 C 0.4976(5) 0.9297(5) 0.9528(11) 0.059(2) Uani 1 1 d . . . H5A H 0.5482 0.9441 0.9327 0.071 Uiso 1 1 calc R . . C6 C 0.4705(5) 0.8735(5) 0.8900(10) 0.061(3) Uani 1 1 d . . . H6A H 0.5029 0.8488 0.8263 0.073 Uiso 1 1 calc R . . C7 C 0.3957(4) 0.8509(4) 0.9169(8) 0.0431(17) Uani 1 1 d . . . H7A H 0.3783 0.8115 0.8719 0.052 Uiso 1 1 calc R . . C8 C 0.1143(5) 0.7651(4) 1.1622(9) 0.0385(16) Uani 1 1 d . . . H8A H 0.1132 0.7498 1.0521 0.046 Uiso 1 1 calc R . . H8B H 0.0926 0.7304 1.2259 0.046 Uiso 1 1 calc R . . C9 C 0.0622(4) 0.8199(3) 1.1678(9) 0.0371(16) Uani 1 1 d . . . C10 C 0.0556(5) 0.8657(3) 1.0471(10) 0.0416(18) Uani 1 1 d . . . H10A H 0.0848 0.8597 0.9567 0.050 Uiso 1 1 calc R . . C11 C 0.0086(4) 0.9195(4) 1.0535(11) 0.053(2) Uani 1 1 d . . . H11A H 0.0047 0.9482 0.9668 0.063 Uiso 1 1 calc R . . C12 C -0.0324(5) 0.9314(4) 1.1847(12) 0.059(2) Uani 1 1 d . . . H12A H -0.0635 0.9687 1.1915 0.071 Uiso 1 1 calc R . . C13 C -0.0269(4) 0.8876(4) 1.3060(11) 0.058(2) Uani 1 1 d . . . H13A H -0.0550 0.8953 1.3970 0.070 Uiso 1 1 calc R . . C14 C 0.0179(4) 0.8330(4) 1.3004(9) 0.0410(16) Uani 1 1 d . . . H14A H 0.0193 0.8038 1.3862 0.049 Uiso 1 1 calc R . . C15 C 0.3102(5) 0.6951(4) 1.0883(10) 0.0473(19) Uani 1 1 d . . . H15A H 0.2928 0.7004 0.9765 0.057 Uiso 1 1 calc R . . H15B H 0.3673 0.6973 1.0969 0.057 Uiso 1 1 calc R . . C16 C 0.2836(4) 0.6357(3) 1.1484(8) 0.0397(17) Uani 1 1 d . . . C17 C 0.3303(5) 0.5952(4) 1.2506(10) 0.054(2) Uani 1 1 d . . . H17A H 0.3833 0.6053 1.2701 0.064 Uiso 1 1 calc R . . C18 C 0.3003(8) 0.5422(5) 1.3209(13) 0.066(4) Uani 1 1 d . . . H18A H 0.3327 0.5174 1.3907 0.079 Uiso 1 1 calc R . . C19 C 0.2237(7) 0.5236(4) 1.2932(11) 0.059(2) Uani 1 1 d . . . H19A H 0.2038 0.4870 1.3441 0.070 Uiso 1 1 calc R . . C20 C 0.1774(7) 0.5593(5) 1.1909(13) 0.056(3) Uani 1 1 d . . . H20A H 0.1254 0.5466 1.1686 0.067 Uiso 1 1 calc R . . C21 C 0.2062(4) 0.6141(3) 1.1193(8) 0.0393(16) Uani 1 1 d . . . H21A H 0.1729 0.6378 1.0487 0.047 Uiso 1 1 calc R . . C22 C 0.4013(5) 0.8707(3) 1.4437(9) 0.0395(16) Uani 1 1 d . . . H22A H 0.3940 0.8800 1.5560 0.047 Uiso 1 1 calc R . . H22B H 0.3730 0.9032 1.3788 0.047 Uiso 1 1 calc R . . C23 C 0.4875(5) 0.8715(4) 1.4106(11) 0.048(2) Uani 1 1 d . . . H23A H 0.5006 0.9098 1.3484 0.058 Uiso 1 1 calc R . . H23B H 0.5199 0.8712 1.5097 0.058 Uiso 1 1 calc R . . C24 C 0.4987(4) 0.8105(4) 1.3176(10) 0.0448(18) Uani 1 1 d . . . H24A H 0.5520 0.7939 1.3332 0.054 Uiso 1 1 calc R . . H24B H 0.4867 0.8172 1.2038 0.054 Uiso 1 1 calc R . . C25 C 0.4408(5) 0.7659(3) 1.3886(11) 0.0421(18) Uani 1 1 d . . . H25A H 0.4288 0.7290 1.3186 0.051 Uiso 1 1 calc R . . H25B H 0.4603 0.7499 1.4925 0.051 Uiso 1 1 calc R . . C26 C 0.1879(4) 0.9266(3) 1.3972(8) 0.0360(15) Uani 1 1 d . . . H26A H 0.1489 0.9241 1.3084 0.043 Uiso 1 1 calc R . . H26B H 0.2317 0.9531 1.3651 0.043 Uiso 1 1 calc R . . C27 C 0.1528(5) 0.9546(4) 1.5421(10) 0.0459(18) Uani 1 1 d . . . H27A H 0.1587 1.0018 1.5456 0.055 Uiso 1 1 calc R . . H27B H 0.0974 0.9436 1.5452 0.055 Uiso 1 1 calc R . . C28 C 0.1997(5) 0.9227(3) 1.6760(10) 0.052(2) Uani 1 1 d . . . H28A H 0.2495 0.9449 1.6972 0.062 Uiso 1 1 calc R . . H28B H 0.1708 0.9220 1.7734 0.062 Uiso 1 1 calc R . . C29 C 0.2116(5) 0.8560(3) 1.6146(8) 0.0414(17) Uani 1 1 d . . . H29A H 0.2606 0.8377 1.6595 0.050 Uiso 1 1 calc R . . H29B H 0.1686 0.8276 1.6420 0.050 Uiso 1 1 calc R . . C30 C 0.3056(4) 0.6864(3) 1.5951(8) 0.0333(14) Uani 1 1 d . . . H30A H 0.3258 0.7193 1.6705 0.040 Uiso 1 1 calc R . . H30B H 0.3486 0.6710 1.5329 0.040 Uiso 1 1 calc R . . C31 C 0.2695(4) 0.6311(3) 1.6813(9) 0.0347(15) Uani 1 1 d . . . H31A H 0.2744 0.5903 1.6232 0.042 Uiso 1 1 calc R . . H31B H 0.2934 0.6261 1.7887 0.042 Uiso 1 1 calc R . . C32 C 0.1864(4) 0.6515(3) 1.6860(8) 0.0375(16) Uani 1 1 d . . . H32A H 0.1793 0.6831 1.7710 0.045 Uiso 1 1 calc R . . H32B H 0.1522 0.6142 1.7014 0.045 Uiso 1 1 calc R . . C33 C 0.1707(4) 0.6817(3) 1.5242(9) 0.0364(15) Uani 1 1 d . . . H33A H 0.1572 0.6485 1.4442 0.044 Uiso 1 1 calc R . . H33B H 0.1280 0.7132 1.5261 0.044 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 0.02430(14) 0.03626(14) 0.01848(13) 0.0004(2) 0.00099(8) -0.0003(2) O1 0.023(2) 0.043(3) 0.037(3) -0.001(2) -0.0042(19) 0.000(2) O2 0.040(4) 0.036(3) 0.020(3) 0.004(2) 0.001(2) 0.007(2) O3 0.032(3) 0.032(2) 0.024(3) 0.0082(18) -0.001(2) 0.0005(19) C1 0.043(6) 0.044(5) 0.030(5) 0.011(4) 0.000(4) 0.001(4) C2 0.039(4) 0.050(4) 0.016(3) 0.017(3) 0.008(3) 0.009(3) C3 0.047(5) 0.042(4) 0.046(5) 0.008(4) 0.009(4) 0.005(3) C4 0.055(5) 0.051(4) 0.059(6) 0.019(4) 0.007(4) -0.009(4) C5 0.043(5) 0.080(6) 0.055(5) 0.030(5) 0.012(4) 0.003(4) C6 0.045(5) 0.101(7) 0.037(5) 0.021(5) 0.011(4) 0.034(5) C7 0.046(4) 0.060(4) 0.023(4) 0.008(3) 0.002(3) 0.014(3) C8 0.031(4) 0.054(5) 0.030(4) -0.001(3) -0.003(3) 0.000(3) C9 0.019(4) 0.045(4) 0.047(4) -0.003(3) -0.004(3) -0.010(3) C10 0.037(5) 0.040(4) 0.047(5) 0.007(3) -0.006(4) -0.005(4) C11 0.033(4) 0.047(5) 0.075(6) 0.012(4) -0.020(4) -0.007(3) C12 0.034(4) 0.051(5) 0.093(8) -0.009(5) -0.001(4) 0.000(3) C13 0.034(4) 0.073(6) 0.067(6) -0.012(5) 0.008(4) -0.002(4) C14 0.029(4) 0.058(4) 0.036(4) 0.001(4) 0.001(3) -0.004(3) C15 0.055(5) 0.048(4) 0.040(5) -0.017(4) 0.006(4) -0.005(4) C16 0.053(5) 0.044(4) 0.023(3) -0.007(3) 0.012(3) 0.014(3) C17 0.060(5) 0.054(5) 0.046(5) -0.019(4) -0.008(4) 0.025(4) C18 0.110(11) 0.047(6) 0.041(6) -0.010(5) -0.003(6) 0.042(6) C19 0.105(8) 0.032(4) 0.041(5) -0.004(4) 0.016(5) 0.009(4) C20 0.072(7) 0.059(6) 0.037(5) -0.010(5) 0.017(5) 0.002(5) C21 0.054(5) 0.039(4) 0.025(4) -0.005(3) 0.005(3) 0.010(3) C22 0.036(4) 0.044(4) 0.039(4) -0.001(3) 0.002(3) -0.006(3) C23 0.028(4) 0.061(5) 0.054(6) 0.015(4) -0.009(4) -0.010(4) C24 0.027(4) 0.065(5) 0.043(5) 0.010(4) 0.009(3) -0.002(3) C25 0.027(4) 0.044(4) 0.055(5) 0.001(3) 0.001(4) -0.001(3) C26 0.042(4) 0.033(3) 0.033(4) 0.004(3) 0.001(3) 0.005(3) C27 0.060(5) 0.043(4) 0.035(4) -0.001(4) 0.004(4) 0.012(4) C28 0.075(6) 0.042(4) 0.038(5) -0.002(3) 0.005(4) 0.006(4) C29 0.052(5) 0.047(4) 0.026(4) 0.002(3) 0.009(3) 0.007(3) C30 0.032(4) 0.038(3) 0.029(4) 0.007(3) 0.001(3) 0.004(3) C31 0.036(4) 0.031(3) 0.038(4) 0.002(3) 0.009(3) 0.005(3) C32 0.034(4) 0.050(4) 0.029(4) 0.007(3) 0.008(3) 0.001(3) C33 0.032(4) 0.043(4) 0.034(4) 0.000(3) 0.006(3) -0.008(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 Gd1 O1 2.461(5) . ? Gd1 O3 2.465(4) . ? Gd1 C15 2.485(8) . ? Gd1 C1 2.490(10) . ? Gd1 O2 2.494(6) . ? Gd1 C8 2.506(9) . ? O1 C25 1.450(9) . ? O1 C22 1.460(9) . ? O2 C26 1.456(9) . ? O2 C29 1.464(9) . ? O3 C33 1.465(8) . ? O3 C30 1.467(8) . ? C1 C2 1.465(11) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.396(11) . ? C2 C7 1.419(9) . ? C3 C4 1.388(11) . ? C3 H3A 0.9500 . ? C4 C5 1.373(12) . ? C4 H4A 0.9500 . ? C5 C6 1.362(13) . ? C5 H5A 0.9500 . ? C6 C7 1.410(11) . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? C8 C9 1.458(10) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.404(10) . ? C9 C14 1.423(10) . ? C10 C11 1.389(11) . ? C10 H10A 0.9500 . ? C11 C12 1.376(13) . ? C11 H11A 0.9500 . ? C12 C13 1.378(13) . ? C12 H12A 0.9500 . ? C13 C14 1.381(11) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? C15 C16 1.427(10) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C21 1.426(11) . ? C16 C17 1.432(11) . ? C17 C18 1.372(15) . ? C17 H17A 0.9500 . ? C18 C19 1.392(16) . ? C18 H18A 0.9500 . ? C19 C20 1.373(16) . ? C19 H19A 0.9500 . ? C20 C21 1.400(13) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? C22 C23 1.535(10) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.516(12) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.516(10) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.519(10) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.519(12) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.504(9) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.519(9) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.504(9) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.527(10) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? 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 O1 Gd1 O3 77.79(16) . . ? O1 Gd1 C15 95.9(3) . . ? O3 Gd1 C15 96.6(2) . . ? O1 Gd1 C1 94.2(3) . . ? O3 Gd1 C1 168.7(3) . . ? C15 Gd1 C1 92.2(3) . . ? O1 Gd1 O2 75.59(18) . . ? O3 Gd1 O2 79.76(18) . . ? C15 Gd1 O2 171.2(3) . . ? C1 Gd1 O2 90.6(2) . . ? O1 Gd1 C8 164.6(2) . . ? O3 Gd1 C8 94.9(2) . . ? C15 Gd1 C8 98.5(3) . . ? C1 Gd1 C8 90.9(3) . . ? O2 Gd1 C8 89.8(2) . . ? C25 O1 C22 107.2(5) . . ? C25 O1 Gd1 119.2(5) . . ? C22 O1 Gd1 126.5(4) . . ? C26 O2 C29 109.5(5) . . ? C26 O2 Gd1 123.4(4) . . ? C29 O2 Gd1 127.1(4) . . ? C33 O3 C30 109.1(5) . . ? C33 O3 Gd1 120.1(4) . . ? C30 O3 Gd1 129.2(4) . . ? C2 C1 Gd1 122.2(6) . . ? C2 C1 H1A 106.8 . . ? Gd1 C1 H1A 106.8 . . ? C2 C1 H1B 106.8 . . ? Gd1 C1 H1B 106.8 . . ? H1A C1 H1B 106.6 . . ? C3 C2 C7 115.7(7) . . ? C3 C2 C1 122.8(7) . . ? C7 C2 C1 121.4(7) . . ? C4 C3 C2 123.3(7) . . ? C4 C3 H3A 118.4 . . ? C2 C3 H3A 118.4 . . ? C5 C4 C3 119.8(8) . . ? C5 C4 H4A 120.1 . . ? C3 C4 H4A 120.1 . . ? C6 C5 C4 119.4(8) . . ? C6 C5 H5A 120.3 . . ? C4 C5 H5A 120.3 . . ? C5 C6 C7 121.7(8) . . ? C5 C6 H6A 119.2 . . ? C7 C6 H6A 119.2 . . ? C6 C7 C2 120.1(8) . . ? C6 C7 H7A 120.0 . . ? C2 C7 H7A 120.0 . . ? C9 C8 Gd1 118.9(5) . . ? C9 C8 H8A 107.6 . . ? Gd1 C8 H8A 107.6 . . ? C9 C8 H8B 107.6 . . ? Gd1 C8 H8B 107.6 . . ? H8A C8 H8B 107.0 . . ? C10 C9 C14 115.0(7) . . ? C10 C9 C8 122.4(7) . . ? C14 C9 C8 122.4(7) . . ? C11 C10 C9 123.1(9) . . ? C11 C10 H10A 118.4 . . ? C9 C10 H10A 118.4 . . ? C12 C11 C10 120.4(9) . . ? C12 C11 H11A 119.8 . . ? C10 C11 H11A 119.8 . . ? C11 C12 C13 118.0(8) . . ? C11 C12 H12A 121.0 . . ? C13 C12 H12A 121.0 . . ? C12 C13 C14 122.6(8) . . ? C12 C13 H13A 118.7 . . ? C14 C13 H13A 118.7 . . ? C13 C14 C9 120.8(7) . . ? C13 C14 H14A 119.6 . . ? C9 C14 H14A 119.6 . . ? C16 C15 Gd1 105.4(5) . . ? C16 C15 H15A 110.7 . . ? Gd1 C15 H15A 110.7 . . ? C16 C15 H15B 110.7 . . ? Gd1 C15 H15B 110.7 . . ? H15A C15 H15B 108.8 . . ? C21 C16 C15 122.0(7) . . ? C21 C16 C17 114.7(7) . . ? C15 C16 C17 123.2(8) . . ? C18 C17 C16 121.7(9) . . ? C18 C17 H17A 119.2 . . ? C16 C17 H17A 119.2 . . ? C17 C18 C19 122.0(10) . . ? C17 C18 H18A 119.0 . . ? C19 C18 H18A 119.0 . . ? C20 C19 C18 118.7(9) . . ? C20 C19 H19A 120.7 . . ? C18 C19 H19A 120.7 . . ? C19 C20 C21 120.6(11) . . ? C19 C20 H20A 119.7 . . ? C21 C20 H20A 119.7 . . ? C20 C21 C16 122.3(8) . . ? C20 C21 H21A 118.8 . . ? C16 C21 H21A 118.8 . . ? O1 C22 C23 106.4(6) . . ? O1 C22 H22A 110.5 . . ? C23 C22 H22A 110.5 . . ? O1 C22 H22B 110.5 . . ? C23 C22 H22B 110.5 . . ? H22A C22 H22B 108.6 . . ? C24 C23 C22 103.7(6) . . ? C24 C23 H23A 111.0 . . ? C22 C23 H23A 111.0 . . ? C24 C23 H23B 111.0 . . ? C22 C23 H23B 111.0 . . ? H23A C23 H23B 109.0 . . ? C23 C24 C25 101.6(6) . . ? C23 C24 H24A 111.5 . . ? C25 C24 H24A 111.5 . . ? C23 C24 H24B 111.5 . . ? C25 C24 H24B 111.5 . . ? H24A C24 H24B 109.3 . . ? O1 C25 C24 103.4(6) . . ? O1 C25 H25A 111.1 . . ? C24 C25 H25A 111.1 . . ? O1 C25 H25B 111.1 . . ? C24 C25 H25B 111.1 . . ? H25A C25 H25B 109.1 . . ? O2 C26 C27 105.3(6) . . ? O2 C26 H26A 110.7 . . ? C27 C26 H26A 110.7 . . ? O2 C26 H26B 110.7 . . ? C27 C26 H26B 110.7 . . ? H26A C26 H26B 108.8 . . ? C28 C27 C26 102.7(6) . . ? C28 C27 H27A 111.2 . . ? C26 C27 H27A 111.2 . . ? C28 C27 H27B 111.2 . . ? C26 C27 H27B 111.2 . . ? H27A C27 H27B 109.1 . . ? C29 C28 C27 102.8(7) . . ? C29 C28 H28A 111.2 . . ? C27 C28 H28A 111.2 . . ? C29 C28 H28B 111.2 . . ? C27 C28 H28B 111.2 . . ? H28A C28 H28B 109.1 . . ? O2 C29 C28 105.5(6) . . ? O2 C29 H29A 110.6 . . ? C28 C29 H29A 110.6 . . ? O2 C29 H29B 110.6 . . ? C28 C29 H29B 110.6 . . ? H29A C29 H29B 108.8 . . ? O3 C30 C31 105.8(5) . . ? O3 C30 H30A 110.6 . . ? C31 C30 H30A 110.6 . . ? O3 C30 H30B 110.6 . . ? C31 C30 H30B 110.6 . . ? H30A C30 H30B 108.7 . . ? C32 C31 C30 102.6(5) . . ? C32 C31 H31A 111.3 . . ? C30 C31 H31A 111.3 . . ? C32 C31 H31B 111.3 . . ? C30 C31 H31B 111.3 . . ? H31A C31 H31B 109.2 . . ? C31 C32 C33 102.7(5) . . ? C31 C32 H32A 111.2 . . ? C33 C32 H32A 111.2 . . ? C31 C32 H32B 111.2 . . ? C33 C32 H32B 111.2 . . ? H32A C32 H32B 109.1 . . ? O3 C33 C32 103.9(5) . . ? O3 C33 H33A 111.0 . . ? C32 C33 H33A 111.0 . . ? O3 C33 H33B 111.0 . . ? C32 C33 H33B 111.0 . . ? H33A C33 H33B 109.0 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.757 _refine_diff_density_min -1.349 _refine_diff_density_rms 0.100 # Attachment '7.cif' data_7 _database_code_depnum_ccdc_archive 'CCDC 736121' _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H45 Dy O3' _chemical_formula_sum 'C33 H45 Dy O3' _chemical_formula_weight 652.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'Cc ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 17.3178(14) _cell_length_b 20.8516(17) _cell_length_c 8.4512(7) _cell_angle_alpha 90.00 _cell_angle_beta 93.201(2) _cell_angle_gamma 90.00 _cell_volume 3047.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 10994 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 27.50 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.49 _exptl_crystal_size_min 0.48 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.422 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1332 _exptl_absorpt_coefficient_mu 2.482 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.29 _exptl_absorpt_correction_T_max 0.30 _exptl_absorpt_process_details '(SADABS; Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 13315 _diffrn_reflns_av_R_equivalents 0.0240 _diffrn_reflns_av_sigmaI/netI 0.0430 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 27.51 _reflns_number_total 6702 _reflns_number_gt 6366 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'enCIFer(Allen et al.,2004);PLATON(Spek,2003)' _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^)+(0.0216P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment Constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.029(10) _refine_ls_number_reflns 6702 _refine_ls_number_parameters 335 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0274 _refine_ls_R_factor_gt 0.0252 _refine_ls_wR_factor_ref 0.0590 _refine_ls_wR_factor_gt 0.0583 _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_restrained_S_all 1.112 _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 Dy1 Dy 0.74807(2) 0.281200(6) 1.74830(3) 0.02313(5) Uani 1 1 d . . . C1 C 0.6943(3) 0.1957(2) 1.9101(5) 0.0418(10) Uani 1 1 d . . . H1A H 0.7125 0.2010 2.0225 0.050 Uiso 1 1 calc R . . H1B H 0.6371 0.1980 1.9032 0.050 Uiso 1 1 calc R . . C2 C 0.7198(3) 0.13402(19) 1.8507(5) 0.0360(9) Uani 1 1 d . . . C3 C 0.6732(3) 0.0955(2) 1.7503(6) 0.0491(12) Uani 1 1 d . . . H3A H 0.6207 0.1071 1.7276 0.059 Uiso 1 1 calc R . . C4 C 0.7023(4) 0.0404(3) 1.6825(7) 0.0566(18) Uani 1 1 d . . . H4A H 0.6690 0.0152 1.6145 0.068 Uiso 1 1 calc R . . C5 C 0.7784(4) 0.0211(2) 1.7112(6) 0.0583(15) Uani 1 1 d . . . H5A H 0.7980 -0.0158 1.6612 0.070 Uiso 1 1 calc R . . C6 C 0.8247(4) 0.0576(3) 1.8155(7) 0.0483(14) Uani 1 1 d . . . H6A H 0.8764 0.0447 1.8416 0.058 Uiso 1 1 calc R . . C7 C 0.7960(3) 0.11275(19) 1.8817(5) 0.0377(9) Uani 1 1 d . . . H7A H 0.8294 0.1373 1.9512 0.045 Uiso 1 1 calc R . . C8 C 0.8844(3) 0.2655(2) 1.8396(5) 0.0344(9) Uani 1 1 d . . . H8A H 0.8854 0.2505 1.9508 0.041 Uiso 1 1 calc R . . H8B H 0.9055 0.2304 1.7761 0.041 Uiso 1 1 calc R . . C9 C 0.9372(2) 0.31994(19) 1.8329(5) 0.0321(8) Uani 1 1 d . . . C10 C 0.9814(2) 0.3321(2) 1.7036(5) 0.0407(10) Uani 1 1 d . . . H10A H 0.9793 0.3026 1.6180 0.049 Uiso 1 1 calc R . . C11 C 1.0285(3) 0.3859(3) 1.6948(7) 0.0557(13) Uani 1 1 d . . . H11A H 1.0572 0.3925 1.6036 0.067 Uiso 1 1 calc R . . C12 C 1.0338(3) 0.4293(2) 1.8161(8) 0.0587(14) Uani 1 1 d . . . H12A H 1.0655 0.4663 1.8097 0.070 Uiso 1 1 calc R . . C13 C 0.9920(3) 0.4181(2) 1.9492(7) 0.0508(12) Uani 1 1 d . . . H13A H 0.9961 0.4474 2.0353 0.061 Uiso 1 1 calc R . . C14 C 0.9447(3) 0.3653(2) 1.9580(6) 0.0380(10) Uani 1 1 d . . . H14A H 0.9165 0.3590 2.0499 0.046 Uiso 1 1 calc R . . C15 C 0.7313(3) 0.3622(3) 1.9549(6) 0.0332(12) Uani 1 1 d . . . H15A H 0.7565 0.3451 2.0540 0.040 Uiso 1 1 calc R . . H15B H 0.7615 0.4003 1.9256 0.040 Uiso 1 1 calc R . . C16 C 0.6547(2) 0.38547(19) 1.9943(4) 0.0318(8) Uani 1 1 d . . . C17 C 0.6243(3) 0.4442(2) 1.9368(6) 0.0439(10) Uani 1 1 d . . . H17A H 0.6559 0.4712 1.8769 0.053 Uiso 1 1 calc R . . C18 C 0.5499(3) 0.4638(3) 1.9649(7) 0.0588(14) Uani 1 1 d . . . H18A H 0.5307 0.5030 1.9206 0.071 Uiso 1 1 calc R . . C19 C 0.5039(3) 0.4276(3) 2.0552(7) 0.0624(15) Uani 1 1 d . . . H19A H 0.4533 0.4416 2.0758 0.075 Uiso 1 1 calc R . . C20 C 0.5317(3) 0.3709(3) 2.1158(5) 0.0588(15) Uani 1 1 d . . . H20A H 0.5001 0.3459 2.1803 0.071 Uiso 1 1 calc R . . C21 C 0.6053(3) 0.3488(2) 2.0855(5) 0.0430(10) Uani 1 1 d . . . H21A H 0.6224 0.3086 2.1268 0.052 Uiso 1 1 calc R . . O1 O 0.62763(14) 0.30638(14) 1.6029(3) 0.0308(6) Uani 1 1 d . . . C22 C 0.5999(2) 0.3710(2) 1.5624(5) 0.0355(9) Uani 1 1 d . . . H22A H 0.6082 0.3807 1.4500 0.043 Uiso 1 1 calc R . . H22B H 0.6277 0.4033 1.6297 0.043 Uiso 1 1 calc R . . C23 C 0.5142(3) 0.3714(2) 1.5919(6) 0.0449(11) Uani 1 1 d . . . H23A H 0.5006 0.4095 1.6545 0.054 Uiso 1 1 calc R . . H23B H 0.4826 0.3715 1.4906 0.054 Uiso 1 1 calc R . . C24 C 0.5018(2) 0.3106(2) 1.6831(5) 0.0434(10) Uani 1 1 d . . . H24A H 0.4483 0.2944 1.6648 0.052 Uiso 1 1 calc R . . H24B H 0.5131 0.3168 1.7982 0.052 Uiso 1 1 calc R . . C25 C 0.5601(2) 0.2660(2) 1.6127(6) 0.0375(10) Uani 1 1 d . . . H25A H 0.5713 0.2286 1.6824 0.045 Uiso 1 1 calc R . . H25B H 0.5414 0.2506 1.5065 0.045 Uiso 1 1 calc R . . O2 O 0.75809(17) 0.21468(11) 1.5138(3) 0.0273(6) Uani 1 1 d . . . C26 C 0.6959(2) 0.18833(18) 1.4094(4) 0.0307(8) Uani 1 1 d . . . H26A H 0.6757 0.2213 1.3338 0.037 Uiso 1 1 calc R . . H26B H 0.6529 0.1729 1.4719 0.037 Uiso 1 1 calc R . . C27 C 0.7314(2) 0.13335(17) 1.3223(4) 0.0306(8) Uani 1 1 d . . . H27A H 0.7260 0.0924 1.3799 0.037 Uiso 1 1 calc R . . H27B H 0.7074 0.1289 1.2137 0.037 Uiso 1 1 calc R . . C28 C 0.8150(2) 0.1532(2) 1.3190(4) 0.0353(9) Uani 1 1 d . . . H28A H 0.8225 0.1848 1.2338 0.042 Uiso 1 1 calc R . . H28B H 0.8489 0.1157 1.3038 0.042 Uiso 1 1 calc R . . C29 C 0.8307(2) 0.1830(2) 1.4818(5) 0.0324(8) Uani 1 1 d . . . H29A H 0.8439 0.1497 1.5624 0.039 Uiso 1 1 calc R . . H29B H 0.8736 0.2144 1.4808 0.039 Uiso 1 1 calc R . . O3 O 0.7866(2) 0.36313(17) 1.5611(4) 0.0275(8) Uani 1 1 d . . . C30 C 0.8125(2) 0.42691(17) 1.6073(4) 0.0320(8) Uani 1 1 d . . . H30A H 0.8515 0.4247 1.6973 0.038 Uiso 1 1 calc R . . H30B H 0.7684 0.4534 1.6389 0.038 Uiso 1 1 calc R . . C31 C 0.8475(3) 0.4549(2) 1.4624(5) 0.0413(10) Uani 1 1 d . . . H31A H 0.9030 0.4441 1.4599 0.050 Uiso 1 1 calc R . . H31B H 0.8414 0.5021 1.4587 0.050 Uiso 1 1 calc R . . C32 C 0.8006(3) 0.4229(2) 1.3270(5) 0.0467(11) Uani 1 1 d . . . H32A H 0.7504 0.4448 1.3053 0.056 Uiso 1 1 calc R . . H32B H 0.8294 0.4223 1.2290 0.056 Uiso 1 1 calc R . . C33 C 0.7894(3) 0.35635(18) 1.3888(4) 0.0357(9) Uani 1 1 d . . . H33A H 0.7405 0.3377 1.3430 0.043 Uiso 1 1 calc R . . H33B H 0.8328 0.3283 1.3620 0.043 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 Dy1 0.02297(7) 0.02873(7) 0.01753(6) -0.00038(12) -0.00027(4) 0.00034(13) C1 0.046(3) 0.045(2) 0.035(2) 0.013(2) 0.008(2) 0.000(2) C2 0.050(2) 0.034(2) 0.0235(19) 0.0123(15) 0.0029(17) -0.0080(18) C3 0.059(3) 0.043(3) 0.045(3) 0.017(2) -0.004(2) -0.023(2) C4 0.097(5) 0.032(3) 0.040(3) 0.008(2) -0.005(3) -0.033(3) C5 0.107(5) 0.032(2) 0.038(3) 0.005(2) 0.020(3) -0.004(3) C6 0.063(3) 0.045(3) 0.038(3) 0.009(2) 0.013(2) -0.003(3) C7 0.051(2) 0.035(2) 0.028(2) 0.0057(16) 0.0062(17) -0.0051(18) C8 0.033(2) 0.037(2) 0.033(2) -0.0001(17) -0.0054(18) 0.0027(17) C9 0.0210(18) 0.037(2) 0.037(2) 0.0001(16) -0.0072(15) 0.0069(15) C10 0.0269(19) 0.052(3) 0.043(2) -0.001(2) 0.0003(17) 0.0040(18) C11 0.034(2) 0.067(3) 0.066(3) 0.018(3) 0.003(2) 0.000(2) C12 0.033(2) 0.045(3) 0.097(4) 0.010(3) -0.009(3) -0.003(2) C13 0.036(2) 0.041(3) 0.073(3) -0.011(2) -0.018(2) 0.008(2) C14 0.026(2) 0.041(2) 0.046(3) -0.0088(19) -0.0071(19) 0.0079(19) C15 0.033(3) 0.042(3) 0.025(2) -0.0099(19) -0.0007(18) -0.001(2) C16 0.035(2) 0.039(2) 0.0220(18) -0.0147(15) 0.0054(15) -0.0083(17) C17 0.047(3) 0.035(2) 0.050(3) -0.013(2) 0.012(2) -0.005(2) C18 0.053(3) 0.050(3) 0.073(4) -0.022(3) 0.000(3) 0.009(2) C19 0.038(3) 0.084(4) 0.065(3) -0.038(3) 0.008(2) 0.001(3) C20 0.047(3) 0.102(4) 0.029(2) -0.020(3) 0.0126(19) -0.037(3) C21 0.046(2) 0.058(3) 0.0250(19) -0.0054(18) 0.0034(17) -0.017(2) O1 0.0221(13) 0.0333(14) 0.0364(15) -0.0047(12) -0.0035(11) 0.0012(12) C22 0.031(2) 0.036(2) 0.039(2) -0.0011(17) -0.0006(17) 0.0063(18) C23 0.032(2) 0.049(3) 0.053(3) -0.010(2) -0.004(2) 0.010(2) C24 0.027(2) 0.069(3) 0.034(2) -0.011(2) 0.0008(17) 0.001(2) C25 0.024(2) 0.039(2) 0.048(3) -0.0045(18) -0.0054(18) -0.0032(16) O2 0.0318(14) 0.0272(13) 0.0226(13) -0.0045(10) -0.0001(11) 0.0035(11) C26 0.034(2) 0.0301(19) 0.0281(19) -0.0034(15) -0.0012(15) -0.0017(16) C27 0.039(2) 0.0269(18) 0.0265(18) -0.0026(14) 0.0038(16) -0.0012(16) C28 0.033(2) 0.046(2) 0.0270(19) -0.0088(17) 0.0039(15) -0.0027(18) C29 0.0291(19) 0.039(2) 0.029(2) -0.0040(16) 0.0000(15) 0.0073(17) O3 0.0354(19) 0.0264(15) 0.0202(15) -0.0028(11) -0.0024(13) -0.0063(13) C30 0.044(2) 0.0237(18) 0.0279(19) -0.0030(14) -0.0033(16) -0.0046(16) C31 0.055(3) 0.033(2) 0.036(2) 0.0023(18) 0.001(2) -0.0115(19) C32 0.071(3) 0.036(2) 0.033(2) 0.0013(18) 0.007(2) -0.008(2) C33 0.054(2) 0.032(2) 0.0223(18) -0.0027(15) 0.0076(16) -0.0078(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 Dy1 O1 2.419(3) . ? Dy1 O2 2.433(3) . ? Dy1 O3 2.447(4) . ? Dy1 C15 2.458(5) . ? Dy1 C1 2.461(4) . ? Dy1 C8 2.465(4) . ? C1 C2 1.459(6) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.393(6) . ? C2 C7 1.404(6) . ? C3 C4 1.391(8) . ? C3 H3A 0.9500 . ? C4 C5 1.385(9) . ? C4 H4A 0.9500 . ? C5 C6 1.386(8) . ? C5 H5A 0.9500 . ? C6 C7 1.383(7) . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? C8 C9 1.461(6) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.392(6) . ? C9 C14 1.418(6) . ? C10 C11 1.391(7) . ? C10 H10A 0.9500 . ? C11 C12 1.366(8) . ? C11 H11A 0.9500 . ? C12 C13 1.391(8) . ? C12 H12A 0.9500 . ? C13 C14 1.378(7) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? C15 C16 1.467(6) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C21 1.408(6) . ? C16 C17 1.408(6) . ? C17 C18 1.386(7) . ? C17 H17A 0.9500 . ? C18 C19 1.361(8) . ? C18 H18A 0.9500 . ? C19 C20 1.365(8) . ? C19 H19A 0.9500 . ? C20 C21 1.393(7) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? O1 C25 1.447(5) . ? O1 C22 1.464(5) . ? C22 C23 1.519(6) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.506(7) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.519(6) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? O2 C29 1.459(5) . ? O2 C26 1.461(4) . ? C26 C27 1.511(5) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.507(5) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.521(5) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? O3 C30 1.450(5) . ? O3 C33 1.466(5) . ? C30 C31 1.514(6) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.520(6) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.498(5) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? 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 O1 Dy1 O2 78.96(9) . . ? O1 Dy1 O3 77.19(10) . . ? O2 Dy1 O3 80.61(10) . . ? O1 Dy1 C15 94.52(14) . . ? O2 Dy1 C15 170.70(15) . . ? O3 Dy1 C15 91.54(12) . . ? O1 Dy1 C1 95.57(14) . . ? O2 Dy1 C1 94.95(13) . . ? O3 Dy1 C1 172.07(14) . . ? C15 Dy1 C1 92.3(2) . . ? O1 Dy1 C8 166.35(12) . . ? O2 Dy1 C8 93.93(13) . . ? O3 Dy1 C8 90.23(13) . . ? C15 Dy1 C8 91.05(16) . . ? C1 Dy1 C8 96.65(15) . . ? C2 C1 Dy1 108.4(3) . . ? C2 C1 H1A 110.0 . . ? Dy1 C1 H1A 110.0 . . ? C2 C1 H1B 110.0 . . ? Dy1 C1 H1B 110.0 . . ? H1A C1 H1B 108.4 . . ? C3 C2 C7 116.0(4) . . ? C3 C2 C1 122.9(4) . . ? C7 C2 C1 121.0(4) . . ? C4 C3 C2 121.1(5) . . ? C4 C3 H3A 119.5 . . ? C2 C3 H3A 119.5 . . ? C5 C4 C3 122.1(5) . . ? C5 C4 H4A 119.0 . . ? C3 C4 H4A 119.0 . . ? C4 C5 C6 117.5(5) . . ? C4 C5 H5A 121.2 . . ? C6 C5 H5A 121.2 . . ? C7 C6 C5 120.4(6) . . ? C7 C6 H6A 119.8 . . ? C5 C6 H6A 119.8 . . ? C6 C7 C2 122.9(4) . . ? C6 C7 H7A 118.6 . . ? C2 C7 H7A 118.6 . . ? C9 C8 Dy1 118.4(3) . . ? C9 C8 H8A 107.7 . . ? Dy1 C8 H8A 107.7 . . ? C9 C8 H8B 107.7 . . ? Dy1 C8 H8B 107.7 . . ? H8A C8 H8B 107.1 . . ? C10 C9 C14 115.6(4) . . ? C10 C9 C8 123.0(4) . . ? C14 C9 C8 121.3(4) . . ? C11 C10 C9 122.6(4) . . ? C11 C10 H10A 118.7 . . ? C9 C10 H10A 118.7 . . ? C12 C11 C10 120.6(5) . . ? C12 C11 H11A 119.7 . . ? C10 C11 H11A 119.7 . . ? C11 C12 C13 118.7(5) . . ? C11 C12 H12A 120.7 . . ? C13 C12 H12A 120.7 . . ? C14 C13 C12 121.0(5) . . ? C14 C13 H13A 119.5 . . ? C12 C13 H13A 119.5 . . ? C13 C14 C9 121.5(5) . . ? C13 C14 H14A 119.3 . . ? C9 C14 H14A 119.3 . . ? C16 C15 Dy1 122.2(3) . . ? C16 C15 H15A 106.8 . . ? Dy1 C15 H15A 106.8 . . ? C16 C15 H15B 106.8 . . ? Dy1 C15 H15B 106.8 . . ? H15A C15 H15B 106.6 . . ? C21 C16 C17 115.7(4) . . ? C21 C16 C15 122.0(4) . . ? C17 C16 C15 122.3(4) . . ? C18 C17 C16 122.1(5) . . ? C18 C17 H17A 119.0 . . ? C16 C17 H17A 119.0 . . ? C19 C18 C17 120.7(5) . . ? C19 C18 H18A 119.6 . . ? C17 C18 H18A 119.6 . . ? C18 C19 C20 119.0(5) . . ? C18 C19 H19A 120.5 . . ? C20 C19 H19A 120.5 . . ? C19 C20 C21 121.6(5) . . ? C19 C20 H20A 119.2 . . ? C21 C20 H20A 119.2 . . ? C20 C21 C16 120.8(5) . . ? C20 C21 H21A 119.6 . . ? C16 C21 H21A 119.6 . . ? C25 O1 C22 107.1(3) . . ? C25 O1 Dy1 121.4(2) . . ? C22 O1 Dy1 125.5(2) . . ? O1 C22 C23 106.1(3) . . ? O1 C22 H22A 110.5 . . ? C23 C22 H22A 110.5 . . ? O1 C22 H22B 110.5 . . ? C23 C22 H22B 110.5 . . ? H22A C22 H22B 108.7 . . ? C24 C23 C22 104.4(4) . . ? C24 C23 H23A 110.9 . . ? C22 C23 H23A 110.9 . . ? C24 C23 H23B 110.9 . . ? C22 C23 H23B 110.9 . . ? H23A C23 H23B 108.9 . . ? C23 C24 C25 101.4(4) . . ? C23 C24 H24A 111.5 . . ? C25 C24 H24A 111.5 . . ? C23 C24 H24B 111.5 . . ? C25 C24 H24B 111.5 . . ? H24A C24 H24B 109.3 . . ? O1 C25 C24 102.9(3) . . ? O1 C25 H25A 111.2 . . ? C24 C25 H25A 111.2 . . ? O1 C25 H25B 111.2 . . ? C24 C25 H25B 111.2 . . ? H25A C25 H25B 109.1 . . ? C29 O2 C26 109.4(3) . . ? C29 O2 Dy1 120.7(2) . . ? C26 O2 Dy1 128.5(2) . . ? O2 C26 C27 105.9(3) . . ? O2 C26 H26A 110.6 . . ? C27 C26 H26A 110.6 . . ? O2 C26 H26B 110.6 . . ? C27 C26 H26B 110.6 . . ? H26A C26 H26B 108.7 . . ? C28 C27 C26 102.6(3) . . ? C28 C27 H27A 111.3 . . ? C26 C27 H27A 111.3 . . ? C28 C27 H27B 111.3 . . ? C26 C27 H27B 111.3 . . ? H27A C27 H27B 109.2 . . ? C27 C28 C29 102.6(3) . . ? C27 C28 H28A 111.2 . . ? C29 C28 H28A 111.2 . . ? C27 C28 H28B 111.2 . . ? C29 C28 H28B 111.2 . . ? H28A C28 H28B 109.2 . . ? O2 C29 C28 103.9(3) . . ? O2 C29 H29A 111.0 . . ? C28 C29 H29A 111.0 . . ? O2 C29 H29B 111.0 . . ? C28 C29 H29B 111.0 . . ? H29A C29 H29B 109.0 . . ? C30 O3 C33 109.2(3) . . ? C30 O3 Dy1 123.9(2) . . ? C33 O3 Dy1 126.9(2) . . ? O3 C30 C31 105.5(3) . . ? O3 C30 H30A 110.6 . . ? C31 C30 H30A 110.6 . . ? O3 C30 H30B 110.6 . . ? C31 C30 H30B 110.6 . . ? H30A C30 H30B 108.8 . . ? C30 C31 C32 102.6(3) . . ? C30 C31 H31A 111.2 . . ? C32 C31 H31A 111.2 . . ? C30 C31 H31B 111.2 . . ? C32 C31 H31B 111.2 . . ? H31A C31 H31B 109.2 . . ? C33 C32 C31 102.6(3) . . ? C33 C32 H32A 111.2 . . ? C31 C32 H32A 111.2 . . ? C33 C32 H32B 111.2 . . ? C31 C32 H32B 111.2 . . ? H32A C32 H32B 109.2 . . ? O3 C33 C32 105.6(3) . . ? O3 C33 H33A 110.6 . . ? C32 C33 H33A 110.6 . . ? O3 C33 H33B 110.6 . . ? C32 C33 H33B 110.6 . . ? H33A C33 H33B 108.7 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.580 _refine_diff_density_min -0.989 _refine_diff_density_rms 0.088 # Attachment '8.cif' data_8 _database_code_depnum_ccdc_archive 'CCDC 736122' _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H45 Er O3' _chemical_formula_sum 'C33 H45 Er O3' _chemical_formula_weight 656.95 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 17.3188(9) _cell_length_b 20.8807(11) _cell_length_c 8.4120(5) _cell_angle_alpha 90.00 _cell_angle_beta 93.353(2) _cell_angle_gamma 90.00 _cell_volume 3036.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5784 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 27.44 _exptl_crystal_description Column _exptl_crystal_colour Pink _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.437 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1340 _exptl_absorpt_coefficient_mu 2.793 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.31 _exptl_absorpt_correction_T_max 0.75 _exptl_absorpt_process_details '(SADABS; Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 9569 _diffrn_reflns_av_R_equivalents 0.0222 _diffrn_reflns_av_sigmaI/netI 0.0406 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_max 27.54 _reflns_number_total 4861 _reflns_number_gt 4484 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'enCIFer(Allen et al.,2004);PLATON(Spek,2003)' _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^)+(0.0145P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.008(9) _refine_ls_number_reflns 4861 _refine_ls_number_parameters 334 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0267 _refine_ls_R_factor_gt 0.0220 _refine_ls_wR_factor_ref 0.0481 _refine_ls_wR_factor_gt 0.0462 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Er1 Er 0.24955(2) 0.217795(6) 0.75146(2) 0.02320(5) Uani 1 1 d . . . O1 O 0.2117(2) 0.1371(2) 0.9378(5) 0.0304(11) Uani 1 1 d . . . O2 O 0.23885(16) 0.28377(12) 0.9830(4) 0.0261(6) Uani 1 1 d . . . O3 O 0.36924(16) 0.19325(15) 0.8945(4) 0.0313(7) Uani 1 1 d . . . C1 C 0.2684(4) 0.1378(3) 0.5447(8) 0.0348(16) Uani 1 1 d . . . H1A H 0.2386 0.0995 0.5739 0.042 Uiso 1 1 calc R . . H1B H 0.2425 0.1549 0.4455 0.042 Uiso 1 1 calc R . . C2 C 0.3426(3) 0.1154(2) 0.5038(5) 0.0334(10) Uani 1 1 d . . . C3 C 0.3734(3) 0.0568(2) 0.5571(7) 0.0439(12) Uani 1 1 d . . . H3A H 0.3420 0.0293 0.6162 0.053 Uiso 1 1 calc R . . C4 C 0.4476(3) 0.0369(3) 0.5278(8) 0.0588(15) Uani 1 1 d . . . H4A H 0.4666 -0.0027 0.5699 0.071 Uiso 1 1 calc R . . C5 C 0.4936(3) 0.0739(3) 0.4389(8) 0.0647(18) Uani 1 1 d . . . H5A H 0.5442 0.0601 0.4174 0.078 Uiso 1 1 calc R . . C6 C 0.4657(3) 0.1311(3) 0.3811(6) 0.0576(16) Uani 1 1 d . . . H6A H 0.4973 0.1568 0.3180 0.069 Uiso 1 1 calc R . . C7 C 0.3917(3) 0.1527(3) 0.4128(5) 0.0433(11) Uani 1 1 d . . . H7A H 0.3743 0.1930 0.3726 0.052 Uiso 1 1 calc R . . C8 C 0.3022(3) 0.3039(2) 0.5932(6) 0.0367(10) Uani 1 1 d . . . H8A H 0.3594 0.3022 0.6023 0.044 Uiso 1 1 calc R . . H8B H 0.2851 0.2981 0.4798 0.044 Uiso 1 1 calc R . . C9 C 0.2761(3) 0.3658(2) 0.6484(5) 0.0355(10) Uani 1 1 d . . . C10 C 0.2000(3) 0.3882(2) 0.6158(6) 0.0382(11) Uani 1 1 d . . . H10A H 0.1664 0.3641 0.5456 0.046 Uiso 1 1 calc R . . C11 C 0.1722(4) 0.4437(3) 0.6815(8) 0.0488(17) Uani 1 1 d . . . H11A H 0.1206 0.4573 0.6555 0.059 Uiso 1 1 calc R . . C12 C 0.2199(4) 0.4793(2) 0.7854(7) 0.0599(17) Uani 1 1 d . . . H12A H 0.2010 0.5168 0.8342 0.072 Uiso 1 1 calc R . . C13 C 0.2953(5) 0.4596(3) 0.8172(8) 0.060(2) Uani 1 1 d . . . H13A H 0.3285 0.4845 0.8865 0.072 Uiso 1 1 calc R . . C14 C 0.3234(3) 0.4049(3) 0.7508(6) 0.0472(13) Uani 1 1 d . . . H14A H 0.3758 0.3930 0.7742 0.057 Uiso 1 1 calc R . . C15 C 0.1147(3) 0.2339(2) 0.6583(6) 0.0341(10) Uani 1 1 d . . . H15A H 0.0939 0.2692 0.7216 0.041 Uiso 1 1 calc R . . H15B H 0.1143 0.2488 0.5466 0.041 Uiso 1 1 calc R . . C16 C 0.0611(2) 0.1801(2) 0.6638(5) 0.0308(9) Uani 1 1 d . . . C17 C 0.0529(3) 0.1347(2) 0.5404(7) 0.0393(12) Uani 1 1 d . . . H17A H 0.0810 0.1405 0.4478 0.047 Uiso 1 1 calc R . . C18 C 0.0054(3) 0.0822(3) 0.5499(7) 0.0493(14) Uani 1 1 d . . . H18A H 0.0012 0.0526 0.4640 0.059 Uiso 1 1 calc R . . C19 C -0.0365(3) 0.0718(3) 0.6833(9) 0.0589(16) Uani 1 1 d . . . H19A H -0.0681 0.0349 0.6910 0.071 Uiso 1 1 calc R . . C20 C -0.0310(3) 0.1158(3) 0.8032(7) 0.0536(14) Uani 1 1 d . . . H20A H -0.0604 0.1101 0.8939 0.064 Uiso 1 1 calc R . . C21 C 0.0168(2) 0.1688(2) 0.7951(6) 0.0394(11) Uani 1 1 d . . . H21A H 0.0195 0.1984 0.8811 0.047 Uiso 1 1 calc R . . C22 C 0.2086(3) 0.1438(2) 1.1107(5) 0.0366(10) Uani 1 1 d . . . H22A H 0.1651 0.1718 1.1374 0.044 Uiso 1 1 calc R . . H22B H 0.2574 0.1622 1.1577 0.044 Uiso 1 1 calc R . . C23 C 0.1970(3) 0.0770(2) 1.1707(6) 0.0483(13) Uani 1 1 d . . . H23A H 0.1684 0.0773 1.2693 0.058 Uiso 1 1 calc R . . H23B H 0.2472 0.0550 1.1923 0.058 Uiso 1 1 calc R . . C24 C 0.1502(3) 0.0449(2) 1.0357(6) 0.0418(11) Uani 1 1 d . . . H24A H 0.0946 0.0559 1.0378 0.050 Uiso 1 1 calc R . . H24B H 0.1562 -0.0022 1.0396 0.050 Uiso 1 1 calc R . . C25 C 0.1858(3) 0.07317(19) 0.8899(5) 0.0328(10) Uani 1 1 d . . . H25A H 0.2299 0.0468 0.8587 0.039 Uiso 1 1 calc R . . H25B H 0.1470 0.0755 0.7989 0.039 Uiso 1 1 calc R . . C26 C 0.3017(2) 0.3104(2) 1.0868(5) 0.0316(9) Uani 1 1 d . . . H26A H 0.3442 0.3260 1.0230 0.038 Uiso 1 1 calc R . . H26B H 0.3226 0.2776 1.1625 0.038 Uiso 1 1 calc R . . C27 C 0.2660(2) 0.36534(19) 1.1750(5) 0.0328(10) Uani 1 1 d . . . H27A H 0.2902 0.3698 1.2841 0.039 Uiso 1 1 calc R . . H27B H 0.2712 0.4063 1.1173 0.039 Uiso 1 1 calc R . . C28 C 0.1820(2) 0.3453(2) 1.1783(5) 0.0350(10) Uani 1 1 d . . . H28A H 0.1746 0.3135 1.2635 0.042 Uiso 1 1 calc R . . H28B H 0.1480 0.3826 1.1938 0.042 Uiso 1 1 calc R . . C29 C 0.1666(2) 0.3161(2) 1.0158(5) 0.0343(10) Uani 1 1 d . . . H29A H 0.1233 0.2852 1.0160 0.041 Uiso 1 1 calc R . . H29B H 0.1539 0.3497 0.9353 0.041 Uiso 1 1 calc R . . C30 C 0.3966(3) 0.1285(2) 0.9349(6) 0.0377(11) Uani 1 1 d . . . H30A H 0.3688 0.0963 0.8666 0.045 Uiso 1 1 calc R . . H30B H 0.3882 0.1186 1.0477 0.045 Uiso 1 1 calc R . . C31 C 0.4827(3) 0.1283(3) 0.9058(7) 0.0448(14) Uani 1 1 d . . . H31A H 0.5142 0.1276 1.0079 0.054 Uiso 1 1 calc R . . H31B H 0.4963 0.0907 0.8415 0.054 Uiso 1 1 calc R . . C32 C 0.4953(3) 0.1899(3) 0.8164(6) 0.0436(12) Uani 1 1 d . . . H32A H 0.5486 0.2062 0.8367 0.052 Uiso 1 1 calc R . . H32B H 0.4845 0.1843 0.7003 0.052 Uiso 1 1 calc R . . C33 C 0.4370(3) 0.2336(2) 0.8864(7) 0.0407(12) Uani 1 1 d . . . H33A H 0.4554 0.2486 0.9936 0.049 Uiso 1 1 calc R . . H33B H 0.4260 0.2712 0.8170 0.049 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 Er1 0.02335(7) 0.02648(8) 0.01943(7) -0.00026(16) -0.00154(5) 0.00028(15) O1 0.040(2) 0.025(2) 0.025(2) -0.0019(15) -0.0017(17) -0.0039(15) O2 0.0286(15) 0.0227(15) 0.0267(16) -0.0039(12) 0.0007(13) 0.0004(12) O3 0.0238(15) 0.0317(16) 0.0379(18) -0.0041(15) -0.0043(13) 0.0022(13) C1 0.042(3) 0.037(3) 0.025(3) -0.002(2) -0.004(2) -0.008(2) C2 0.039(2) 0.039(3) 0.023(2) -0.0185(19) 0.0011(18) -0.008(2) C3 0.047(3) 0.033(3) 0.054(3) -0.011(2) 0.013(3) -0.006(2) C4 0.058(3) 0.052(4) 0.067(4) -0.024(3) 0.003(3) 0.006(3) C5 0.043(3) 0.091(5) 0.061(4) -0.038(4) 0.005(3) 0.001(3) C6 0.047(3) 0.096(5) 0.031(3) -0.016(3) 0.011(2) -0.032(3) C7 0.046(3) 0.056(3) 0.027(2) -0.009(2) 0.000(2) -0.014(2) C8 0.044(3) 0.037(3) 0.030(3) 0.007(2) 0.003(2) 0.001(2) C9 0.048(3) 0.032(2) 0.027(2) 0.0139(19) 0.0044(19) -0.009(2) C10 0.054(3) 0.033(3) 0.028(2) 0.0053(19) 0.005(2) -0.006(2) C11 0.064(4) 0.038(4) 0.046(4) 0.002(3) 0.012(3) 0.001(3) C12 0.114(6) 0.023(3) 0.044(4) 0.008(2) 0.018(3) -0.005(3) C13 0.098(6) 0.041(4) 0.037(4) 0.011(3) -0.018(4) -0.031(4) C14 0.054(3) 0.039(3) 0.048(3) 0.011(3) -0.006(2) -0.016(2) C15 0.028(2) 0.043(3) 0.031(3) 0.003(2) -0.0042(19) 0.005(2) C16 0.022(2) 0.031(2) 0.038(3) 0.0034(19) -0.0082(18) 0.0077(17) C17 0.028(3) 0.038(3) 0.050(3) -0.006(2) -0.010(2) 0.009(2) C18 0.034(3) 0.038(3) 0.073(4) -0.012(3) -0.022(3) 0.007(2) C19 0.035(3) 0.043(3) 0.097(5) 0.013(3) -0.010(3) -0.004(2) C20 0.034(3) 0.064(4) 0.062(4) 0.015(3) 0.001(3) -0.002(2) C21 0.025(2) 0.050(3) 0.043(3) -0.001(2) -0.001(2) 0.0025(19) C22 0.056(3) 0.028(2) 0.026(2) 0.0002(18) 0.002(2) -0.008(2) C23 0.079(4) 0.038(3) 0.029(3) 0.000(2) 0.005(3) -0.008(2) C24 0.054(3) 0.034(3) 0.037(3) 0.002(2) -0.001(2) -0.012(2) C25 0.043(3) 0.024(2) 0.031(2) -0.0043(18) -0.0082(19) -0.0033(18) C26 0.034(2) 0.030(2) 0.030(2) -0.0037(19) -0.0032(18) -0.0006(18) C27 0.041(2) 0.026(2) 0.031(2) -0.0036(18) 0.0040(19) -0.0032(18) C28 0.033(2) 0.042(3) 0.031(2) -0.006(2) 0.0082(18) 0.001(2) C29 0.032(2) 0.038(3) 0.033(3) -0.002(2) 0.0042(19) 0.0066(19) C30 0.034(3) 0.036(3) 0.041(3) 0.001(2) -0.006(2) 0.006(2) C31 0.030(3) 0.051(4) 0.052(4) -0.014(3) -0.003(2) 0.011(3) C32 0.027(3) 0.068(3) 0.035(3) -0.008(3) -0.003(2) 0.002(2) C33 0.025(2) 0.046(3) 0.051(3) -0.001(2) -0.003(2) -0.0036(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Er1 O3 2.391(3) . ? Er1 O2 2.402(3) . ? Er1 O1 2.418(4) . ? Er1 C15 2.442(5) . ? Er1 C8 2.445(5) . ? Er1 C1 2.446(7) . ? O1 C25 1.457(5) . ? O1 C22 1.465(6) . ? O2 C29 1.462(5) . ? O2 C26 1.465(5) . ? O3 C33 1.449(5) . ? O3 C30 1.466(5) . ? C1 C2 1.430(8) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.398(7) . ? C2 C7 1.412(6) . ? C3 C4 1.387(7) . ? C3 H3A 0.9500 . ? C4 C5 1.363(9) . ? C4 H4A 0.9500 . ? C5 C6 1.368(8) . ? C5 H5A 0.9500 . ? C6 C7 1.399(7) . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? C8 C9 1.455(6) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.410(6) . ? C9 C14 1.413(7) . ? C10 C11 1.383(8) . ? C10 H10A 0.9500 . ? C11 C12 1.384(9) . ? C11 H11A 0.9500 . ? C12 C13 1.381(10) . ? C12 H12A 0.9500 . ? C13 C14 1.374(9) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? C15 C16 1.461(6) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C21 1.401(7) . ? C16 C17 1.406(7) . ? C17 C18 1.377(7) . ? C17 H17A 0.9500 . ? C18 C19 1.388(8) . ? C18 H18A 0.9500 . ? C19 C20 1.364(8) . ? C19 H19A 0.9500 . ? C20 C21 1.385(7) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? C22 C23 1.501(6) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.512(7) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.523(7) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.518(6) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.517(6) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.505(6) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.525(6) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.512(8) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.505(7) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? 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 O3 Er1 O2 79.66(10) . . ? O3 Er1 O1 77.54(12) . . ? O2 Er1 O1 80.65(13) . . ? O3 Er1 C15 167.28(13) . . ? O2 Er1 C15 93.65(14) . . ? O1 Er1 C15 90.76(14) . . ? O3 Er1 C8 95.28(15) . . ? O2 Er1 C8 93.93(14) . . ? O1 Er1 C8 171.63(16) . . ? C15 Er1 C8 95.98(16) . . ? O3 Er1 C1 93.67(17) . . ? O2 Er1 C1 171.05(18) . . ? O1 Er1 C1 92.14(12) . . ? C15 Er1 C1 91.7(2) . . ? C8 Er1 C1 92.6(2) . . ? C25 O1 C22 109.5(4) . . ? C25 O1 Er1 123.4(3) . . ? C22 O1 Er1 127.1(3) . . ? C29 O2 C26 109.1(3) . . ? C29 O2 Er1 121.7(2) . . ? C26 O2 Er1 127.6(2) . . ? C33 O3 C30 107.2(3) . . ? C33 O3 Er1 122.2(3) . . ? C30 O3 Er1 125.0(2) . . ? C2 C1 Er1 123.7(4) . . ? C2 C1 H1A 106.4 . . ? Er1 C1 H1A 106.4 . . ? C2 C1 H1B 106.4 . . ? Er1 C1 H1B 106.4 . . ? H1A C1 H1B 106.5 . . ? C3 C2 C7 115.3(4) . . ? C3 C2 C1 122.8(5) . . ? C7 C2 C1 121.9(5) . . ? C4 C3 C2 123.0(5) . . ? C4 C3 H3A 118.5 . . ? C2 C3 H3A 118.5 . . ? C5 C4 C3 120.4(6) . . ? C5 C4 H4A 119.8 . . ? C3 C4 H4A 119.8 . . ? C4 C5 C6 118.9(5) . . ? C4 C5 H5A 120.5 . . ? C6 C5 H5A 120.5 . . ? C5 C6 C7 121.5(5) . . ? C5 C6 H6A 119.2 . . ? C7 C6 H6A 119.2 . . ? C6 C7 C2 120.9(5) . . ? C6 C7 H7A 119.6 . . ? C2 C7 H7A 119.6 . . ? C9 C8 Er1 110.3(3) . . ? C9 C8 H8A 109.6 . . ? Er1 C8 H8A 109.6 . . ? C9 C8 H8B 109.6 . . ? Er1 C8 H8B 109.6 . . ? H8A C8 H8B 108.1 . . ? C10 C9 C14 115.5(5) . . ? C10 C9 C8 122.5(4) . . ? C14 C9 C8 121.8(5) . . ? C11 C10 C9 123.0(5) . . ? C11 C10 H10A 118.5 . . ? C9 C10 H10A 118.5 . . ? C10 C11 C12 119.5(6) . . ? C10 C11 H11A 120.2 . . ? C12 C11 H11A 120.2 . . ? C13 C12 C11 119.1(6) . . ? C13 C12 H12A 120.5 . . ? C11 C12 H12A 120.5 . . ? C14 C13 C12 121.5(6) . . ? C14 C13 H13A 119.2 . . ? C12 C13 H13A 119.2 . . ? C13 C14 C9 121.4(5) . . ? C13 C14 H14A 119.3 . . ? C9 C14 H14A 119.3 . . ? C16 C15 Er1 118.9(3) . . ? C16 C15 H15A 107.6 . . ? Er1 C15 H15A 107.6 . . ? C16 C15 H15B 107.6 . . ? Er1 C15 H15B 107.6 . . ? H15A C15 H15B 107.0 . . ? C21 C16 C17 115.7(4) . . ? C21 C16 C15 122.2(4) . . ? C17 C16 C15 122.1(5) . . ? C18 C17 C16 121.9(6) . . ? C18 C17 H17A 119.0 . . ? C16 C17 H17A 119.0 . . ? C17 C18 C19 120.9(6) . . ? C17 C18 H18A 119.5 . . ? C19 C18 H18A 119.5 . . ? C20 C19 C18 118.4(5) . . ? C20 C19 H19A 120.8 . . ? C18 C19 H19A 120.8 . . ? C19 C20 C21 121.2(5) . . ? C19 C20 H20A 119.4 . . ? C21 C20 H20A 119.4 . . ? C20 C21 C16 121.9(5) . . ? C20 C21 H21A 119.1 . . ? C16 C21 H21A 119.1 . . ? O1 C22 C23 105.0(4) . . ? O1 C22 H22A 110.8 . . ? C23 C22 H22A 110.8 . . ? O1 C22 H22B 110.8 . . ? C23 C22 H22B 110.8 . . ? H22A C22 H22B 108.8 . . ? C22 C23 C24 103.6(4) . . ? C22 C23 H23A 111.0 . . ? C24 C23 H23A 111.0 . . ? C22 C23 H23B 111.0 . . ? C24 C23 H23B 111.0 . . ? H23A C23 H23B 109.0 . . ? C23 C24 C25 102.1(4) . . ? C23 C24 H24A 111.4 . . ? C25 C24 H24A 111.4 . . ? C23 C24 H24B 111.4 . . ? C25 C24 H24B 111.4 . . ? H24A C24 H24B 109.2 . . ? O1 C25 C24 105.3(4) . . ? O1 C25 H25A 110.7 . . ? C24 C25 H25A 110.7 . . ? O1 C25 H25B 110.7 . . ? C24 C25 H25B 110.7 . . ? H25A C25 H25B 108.8 . . ? O2 C26 C27 105.6(3) . . ? O2 C26 H26A 110.6 . . ? C27 C26 H26A 110.6 . . ? O2 C26 H26B 110.6 . . ? C27 C26 H26B 110.6 . . ? H26A C26 H26B 108.8 . . ? C28 C27 C26 102.6(3) . . ? C28 C27 H27A 111.2 . . ? C26 C27 H27A 111.2 . . ? C28 C27 H27B 111.2 . . ? C26 C27 H27B 111.2 . . ? H27A C27 H27B 109.2 . . ? C29 C28 C27 102.4(3) . . ? C29 C28 H28A 111.3 . . ? C27 C28 H28A 111.3 . . ? C29 C28 H28B 111.3 . . ? C27 C28 H28B 111.3 . . ? H28A C28 H28B 109.2 . . ? O2 C29 C28 104.5(3) . . ? O2 C29 H29A 110.9 . . ? C28 C29 H29A 110.9 . . ? O2 C29 H29B 110.9 . . ? C28 C29 H29B 110.9 . . ? H29A C29 H29B 108.9 . . ? O3 C30 C31 105.7(4) . . ? O3 C30 H30A 110.6 . . ? C31 C30 H30A 110.6 . . ? O3 C30 H30B 110.6 . . ? C31 C30 H30B 110.6 . . ? H30A C30 H30B 108.7 . . ? C32 C31 C30 104.4(4) . . ? C32 C31 H31A 110.9 . . ? C30 C31 H31A 110.9 . . ? C32 C31 H31B 110.9 . . ? C30 C31 H31B 110.9 . . ? H31A C31 H31B 108.9 . . ? C33 C32 C31 101.6(4) . . ? C33 C32 H32A 111.5 . . ? C31 C32 H32A 111.5 . . ? C33 C32 H32B 111.5 . . ? C31 C32 H32B 111.5 . . ? H32A C32 H32B 109.3 . . ? O3 C33 C32 103.3(4) . . ? O3 C33 H33A 111.1 . . ? C32 C33 H33A 111.1 . . ? O3 C33 H33B 111.1 . . ? C32 C33 H33B 111.1 . . ? H33A C33 H33B 109.1 . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.911 _refine_diff_density_min -0.487 _refine_diff_density_rms 0.079 # Attachment '9.cif' data_9 _database_code_depnum_ccdc_archive 'CCDC 736123' _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H44 O2 Yb, C27 H47 O5 Yb' _chemical_formula_sum 'C63 H91 O7 Yb2' _chemical_formula_weight 1306.44 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' O O 0.0106 0.0060 '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 Monoclinic _symmetry_space_group_name_H-M 'P2(1)/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 16.737(3) _cell_length_b 20.454(3) _cell_length_c 17.827(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.144(3) _cell_angle_gamma 90.00 _cell_volume 6093.6(16) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3160 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 25.43 _exptl_crystal_description COLUMN _exptl_crystal_colour COLOURLESS _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.424 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2660 _exptl_absorpt_coefficient_mu 3.099 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.64 _exptl_absorpt_correction_T_max 0.91 _exptl_absorpt_process_details '(SADABS; Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 28783 _diffrn_reflns_av_R_equivalents 0.0980 _diffrn_reflns_av_sigmaI/netI 0.1226 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 24.00 _reflns_number_total 9527 _reflns_number_gt 5599 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'enCIFer(Allen et al.,2004);PLATON(Spek,2003)' _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^)+(0.0734P)^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 9527 _refine_ls_number_parameters 707 _refine_ls_number_restraints 223 _refine_ls_R_factor_all 0.1225 _refine_ls_R_factor_gt 0.0566 _refine_ls_wR_factor_ref 0.1554 _refine_ls_wR_factor_gt 0.1240 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 0.983 _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 0.54248(3) 0.21911(3) 0.38609(3) 0.03204(17) Uani 1 1 d . . . Yb2 Yb 1.03372(3) 0.32693(3) 0.40319(3) 0.03571(18) Uani 1 1 d . B . O1 O 0.5430(5) 0.1047(4) 0.3676(4) 0.047(2) Uani 1 1 d . A . O2 O 0.5405(4) 0.3322(4) 0.3981(4) 0.040(2) Uani 1 1 d . A . O3 O 1.1457(5) 0.3074(5) 0.4885(4) 0.054(3) Uani 1 1 d . . . O4 O 1.0999(5) 0.3042(4) 0.2882(4) 0.046(2) Uani 1 1 d . . . O5 O 1.0313(6) 0.2043(4) 0.4054(5) 0.055(3) Uani 1 1 d D . . O6 O 0.9059(4) 0.3328(4) 0.3322(4) 0.042(2) Uani 1 1 d . . . O7 O 0.9527(5) 0.3182(5) 0.5095(4) 0.053(2) Uani 1 1 d . . . C1 C 0.3949(7) 0.2246(7) 0.3943(7) 0.052(4) Uani 1 1 d . A . H1A H 0.3835 0.2451 0.4429 0.063 Uiso 1 1 calc R . . H1B H 0.3732 0.2540 0.3540 0.063 Uiso 1 1 calc R . . C2 C 0.3514(7) 0.1630(7) 0.3884(8) 0.046(3) Uani 1 1 d . . . C3 C 0.3199(8) 0.1395(8) 0.3222(8) 0.058(4) Uani 1 1 d . A . H3A H 0.3244 0.1657 0.2786 0.070 Uiso 1 1 calc R . . C4 C 0.2821(9) 0.0806(9) 0.3140(11) 0.077(5) Uani 1 1 d . . . H4A H 0.2634 0.0657 0.2657 0.092 Uiso 1 1 calc R A . C5 C 0.2715(10) 0.0430(9) 0.3766(14) 0.094(7) Uani 1 1 d . A . H5A H 0.2455 0.0018 0.3715 0.112 Uiso 1 1 calc R . . C6 C 0.2985(9) 0.0650(9) 0.4474(13) 0.091(6) Uani 1 1 d . . . H6A H 0.2896 0.0400 0.4911 0.109 Uiso 1 1 calc R A . C7 C 0.3383(8) 0.1236(8) 0.4527(8) 0.062(4) Uani 1 1 d . A . H7A H 0.3577 0.1384 0.5008 0.075 Uiso 1 1 calc R . . C8 C 0.5592(8) 0.1970(6) 0.5242(6) 0.042(3) Uani 1 1 d . A . H8A H 0.5185 0.1649 0.5386 0.050 Uiso 1 1 calc R . . H8B H 0.6128 0.1779 0.5361 0.050 Uiso 1 1 calc R . . C9 C 0.5507(7) 0.2568(6) 0.5667(6) 0.034(3) Uani 1 1 d . . . C10 C 0.6111(8) 0.3041(8) 0.5724(7) 0.056(4) Uani 1 1 d . A . H10A H 0.6599 0.2961 0.5492 0.067 Uiso 1 1 calc R . . C11 C 0.6018(10) 0.3619(8) 0.6109(7) 0.062(4) Uani 1 1 d . . . H11A H 0.6454 0.3916 0.6156 0.074 Uiso 1 1 calc R A . C12 C 0.5315(11) 0.3776(8) 0.6425(8) 0.067(5) Uani 1 1 d . A . H12A H 0.5244 0.4184 0.6667 0.081 Uiso 1 1 calc R . . C13 C 0.4695(9) 0.3297(8) 0.6375(7) 0.056(4) Uani 1 1 d . . . H13A H 0.4199 0.3383 0.6591 0.067 Uiso 1 1 calc R A . C14 C 0.4809(7) 0.2723(7) 0.6021(6) 0.042(3) Uani 1 1 d . A . H14A H 0.4392 0.2409 0.6013 0.051 Uiso 1 1 calc R . . C15 C 0.5251(8) 0.2230(7) 0.2470(6) 0.047(3) Uani 1 1 d . A . H15A H 0.5696 0.1986 0.2257 0.056 Uiso 1 1 calc R . . H15B H 0.4747 0.2002 0.2314 0.056 Uiso 1 1 calc R . . C16 C 0.5225(8) 0.2904(7) 0.2139(6) 0.043(3) Uani 1 1 d . . . C17 C 0.5908(9) 0.3200(8) 0.1886(7) 0.055(4) Uani 1 1 d . A . H17A H 0.6400 0.2969 0.1946 0.067 Uiso 1 1 calc R . . C18 C 0.5913(11) 0.3789(8) 0.1564(9) 0.074(5) Uani 1 1 d . . . H18A H 0.6398 0.3960 0.1392 0.088 Uiso 1 1 calc R A . C19 C 0.5241(13) 0.4139(8) 0.1482(8) 0.076(5) Uani 1 1 d . A . H19A H 0.5246 0.4557 0.1251 0.091 Uiso 1 1 calc R . . C20 C 0.4548(10) 0.3892(9) 0.1731(8) 0.069(5) Uani 1 1 d . . . H20A H 0.4071 0.4144 0.1678 0.083 Uiso 1 1 calc R A . C21 C 0.4529(9) 0.3278(9) 0.2063(7) 0.062(4) Uani 1 1 d . A . H21A H 0.4042 0.3113 0.2237 0.074 Uiso 1 1 calc R . . C22 C 0.6916(6) 0.2313(5) 0.3783(7) 0.043(3) Uani 0.59(2) 1 d PDU A 1 H22A H 0.7031 0.2500 0.3288 0.052 Uiso 0.59(2) 1 calc PR A 1 H22B H 0.7120 0.2622 0.4176 0.052 Uiso 0.59(2) 1 calc PR A 1 C23 C 0.7356(10) 0.1660(6) 0.3885(10) 0.047(3) Uani 0.59(2) 1 d PGDU A 1 C24 C 0.7452(10) 0.1258(8) 0.3268(8) 0.053(4) Uani 0.59(2) 1 d PGU A 1 H24A H 0.7254 0.1392 0.2783 0.064 Uiso 0.59(2) 1 calc PR A 1 C25 C 0.7837(10) 0.0659(7) 0.3362(9) 0.064(5) Uani 0.59(2) 1 d PGU A 1 H25A H 0.7903 0.0384 0.2940 0.076 Uiso 0.59(2) 1 calc PR A 1 C26 C 0.8127(10) 0.0462(6) 0.4072(11) 0.064(5) Uani 0.59(2) 1 d PGU A 1 H26A H 0.8390 0.0053 0.4136 0.077 Uiso 0.59(2) 1 calc PR A 1 C27 C 0.8031(9) 0.0865(8) 0.4689(8) 0.058(5) Uani 0.59(2) 1 d PGU A 1 H27A H 0.8229 0.0731 0.5174 0.070 Uiso 0.59(2) 1 calc PR A 1 C28 C 0.7645(10) 0.1464(7) 0.4595(8) 0.050(4) Uani 0.59(2) 1 d PGU A 1 H28A H 0.7580 0.1739 0.5017 0.060 Uiso 0.59(2) 1 calc PR A 1 C22A C 0.6916(6) 0.2313(5) 0.3783(7) 0.043(3) Uani 0.41(2) 1 d PU A 2 H22C H 0.7023 0.2604 0.3357 0.052 Uiso 0.41(2) 1 calc PR A 2 H22D H 0.7137 0.2525 0.4248 0.052 Uiso 0.41(2) 1 calc PR A 2 C23A C 0.7327(13) 0.1699(9) 0.3687(13) 0.052(4) Uani 0.41(2) 1 d PGU A 2 C24A C 0.7382(13) 0.1482(9) 0.2953(12) 0.055(5) Uani 0.41(2) 1 d PGU A 2 H24B H 0.7185 0.1746 0.2545 0.066 Uiso 0.41(2) 1 calc PR A 2 C25A C 0.7725(12) 0.0877(10) 0.2816(12) 0.064(6) Uani 0.41(2) 1 d PGU A 2 H25B H 0.7763 0.0729 0.2314 0.077 Uiso 0.41(2) 1 calc PR A 2 C26A C 0.8013(12) 0.0491(9) 0.3412(13) 0.069(6) Uani 0.41(2) 1 d PGU A 2 H26B H 0.8248 0.0078 0.3318 0.082 Uiso 0.41(2) 1 calc PR A 2 C27A C 0.7958(12) 0.0709(10) 0.4146(12) 0.067(6) Uani 0.41(2) 1 d PGU A 2 H27B H 0.8155 0.0445 0.4554 0.081 Uiso 0.41(2) 1 calc PR A 2 C28A C 0.7615(13) 0.1313(10) 0.4283(12) 0.059(5) Uani 0.41(2) 1 d PGU A 2 H28B H 0.7577 0.1462 0.4785 0.071 Uiso 0.41(2) 1 calc PR A 2 C29 C 0.5644(11) 0.0615(7) 0.4290(8) 0.074(5) Uani 1 1 d . . . H29A H 0.5234 0.0623 0.4669 0.088 Uiso 1 1 calc R A . H29B H 0.6168 0.0739 0.4535 0.088 Uiso 1 1 calc R . . C30 C 0.5689(12) -0.0066(8) 0.3922(8) 0.089(6) Uani 1 1 d . A . H30A H 0.6234 -0.0160 0.3760 0.107 Uiso 1 1 calc R . . H30B H 0.5524 -0.0415 0.4265 0.107 Uiso 1 1 calc R . . C31 C 0.5113(11) 0.0010(8) 0.3275(11) 0.092(6) Uani 1 1 d . . . H31A H 0.5227 -0.0302 0.2871 0.110 Uiso 1 1 calc R A . H31B H 0.4558 -0.0058 0.3425 0.110 Uiso 1 1 calc R . . C32 C 0.5235(10) 0.0687(7) 0.3033(7) 0.071(5) Uani 1 1 d . A . H32A H 0.5673 0.0709 0.2683 0.085 Uiso 1 1 calc R . . H32B H 0.4741 0.0860 0.2774 0.085 Uiso 1 1 calc R . . C33 C 0.6058(7) 0.3774(5) 0.3812(7) 0.047(3) Uani 0.50 1 d PDU A 1 H33A H 0.6350 0.3607 0.3383 0.056 Uiso 0.50 1 calc PR A 1 H33B H 0.6440 0.3816 0.4253 0.056 Uiso 0.50 1 calc PR A 1 C34 C 0.5686(6) 0.4424(5) 0.3620(7) 0.051(2) Uani 0.50 1 d PDU A 1 H34A H 0.5413 0.4432 0.3113 0.062 Uiso 0.50 1 calc PR A 1 H34B H 0.6071 0.4790 0.3677 0.062 Uiso 0.50 1 calc PR A 1 C35 C 0.5111(12) 0.4402(7) 0.4236(11) 0.046(4) Uani 0.50 1 d PDU A 1 H35A H 0.5395 0.4471 0.4732 0.055 Uiso 0.50 1 calc PR A 1 H35B H 0.4693 0.4741 0.4160 0.055 Uiso 0.50 1 calc PR A 1 C36 C 0.4752(7) 0.3730(5) 0.4187(7) 0.046(3) Uani 0.50 1 d PDU A 1 H36A H 0.4553 0.3594 0.4676 0.055 Uiso 0.50 1 calc PR A 1 H36B H 0.4304 0.3713 0.3801 0.055 Uiso 0.50 1 calc PR A 1 C33A C 0.6058(7) 0.3774(5) 0.3812(7) 0.047(3) Uani 0.50 1 d PDU A 2 H33C H 0.6350 0.3607 0.3383 0.056 Uiso 0.50 1 calc PR A 2 H33D H 0.6440 0.3816 0.4253 0.056 Uiso 0.50 1 calc PR A 2 C34A C 0.5686(6) 0.4424(5) 0.3620(7) 0.051(2) Uani 0.50 1 d PDU A 2 H34C H 0.5603 0.4474 0.3069 0.062 Uiso 0.50 1 calc PR A 2 H34D H 0.6033 0.4784 0.3816 0.062 Uiso 0.50 1 calc PR A 2 C35A C 0.4900(10) 0.4430(6) 0.3986(14) 0.052(4) Uani 0.50 1 d PDU A 2 H35C H 0.4930 0.4709 0.4441 0.063 Uiso 0.50 1 calc PR A 2 H35D H 0.4468 0.4597 0.3635 0.063 Uiso 0.50 1 calc PR A 2 C36A C 0.4752(7) 0.3730(5) 0.4187(7) 0.046(3) Uani 0.50 1 d PDU A 2 H36C H 0.4688 0.3695 0.4734 0.055 Uiso 0.50 1 calc PR A 2 H36D H 0.4250 0.3578 0.3924 0.055 Uiso 0.50 1 calc PR A 2 C37 C 1.0460(7) 0.4519(7) 0.3989(6) 0.048(4) Uani 1 1 d . . . H37A H 1.0346 0.4681 0.3471 0.057 Uiso 1 1 calc R B . H37B H 1.0079 0.4725 0.4323 0.057 Uiso 1 1 calc R . . C38 C 1.1269(8) 0.4670(7) 0.4240(7) 0.048(3) Uani 1 1 d . B . C39 C 1.1866(9) 0.4729(7) 0.3728(8) 0.063(4) Uani 1 1 d . . . H39A H 1.1720 0.4693 0.3207 0.076 Uiso 1 1 calc R B . C40 C 1.2654(9) 0.4837(8) 0.3944(9) 0.078(5) Uani 1 1 d . B . H40A H 1.3042 0.4866 0.3575 0.094 Uiso 1 1 calc R . . C41 C 1.2888(9) 0.4906(9) 0.4705(9) 0.076(5) Uani 1 1 d . . . H41A H 1.3432 0.4977 0.4865 0.092 Uiso 1 1 calc R B . C42 C 1.2301(9) 0.4866(8) 0.5212(8) 0.064(4) Uani 1 1 d . B . H42A H 1.2440 0.4917 0.5733 0.076 Uiso 1 1 calc R . . C43 C 1.1514(7) 0.4756(7) 0.4980(7) 0.047(3) Uani 1 1 d . . . H43A H 1.1125 0.4738 0.5348 0.057 Uiso 1 1 calc R B . C44 C 1.1447(7) 0.3091(9) 0.5678(8) 0.078(4) Uani 0.50 1 d PDU B 1 H44A H 1.1195 0.2685 0.5854 0.094 Uiso 0.50 1 calc PR B 1 H44B H 1.1113 0.3464 0.5826 0.094 Uiso 0.50 1 calc PR B 1 C45 C 1.2263(9) 0.316(2) 0.6062(13) 0.080(5) Uani 0.50 1 d PDU B 1 H45A H 1.2407 0.3617 0.6175 0.096 Uiso 0.50 1 calc PR B 1 H45B H 1.2325 0.2890 0.6525 0.096 Uiso 0.50 1 calc PR B 1 C46 C 1.2715(17) 0.2880(18) 0.5432(9) 0.082(5) Uani 0.50 1 d PDU B 1 H46A H 1.2743 0.2398 0.5473 0.099 Uiso 0.50 1 calc PR B 1 H46B H 1.3268 0.3054 0.5454 0.099 Uiso 0.50 1 calc PR B 1 C47 C 1.2286(8) 0.3071(9) 0.4704(7) 0.076(4) Uani 0.50 1 d PDU B 1 H47A H 1.2457 0.3510 0.4539 0.091 Uiso 0.50 1 calc PR B 1 H47B H 1.2383 0.2750 0.4304 0.091 Uiso 0.50 1 calc PR B 1 C44A C 1.1447(7) 0.3091(9) 0.5678(8) 0.078(4) Uani 0.50 1 d PDU B 2 H44C H 1.1040 0.2795 0.5875 0.094 Uiso 0.50 1 calc PR B 2 H44D H 1.1375 0.3539 0.5874 0.094 Uiso 0.50 1 calc PR B 2 C45A C 1.2284(9) 0.2841(15) 0.5824(17) 0.079(5) Uani 0.50 1 d PDU B 2 H45C H 1.2444 0.2881 0.6365 0.095 Uiso 0.50 1 calc PR B 2 H45D H 1.2312 0.2374 0.5683 0.095 Uiso 0.50 1 calc PR B 2 C46A C 1.2837(15) 0.3235(18) 0.5369(10) 0.077(5) Uani 0.50 1 d PDU B 2 H46C H 1.3382 0.3049 0.5348 0.092 Uiso 0.50 1 calc PR B 2 H46D H 1.2857 0.3706 0.5497 0.092 Uiso 0.50 1 calc PR B 2 C47A C 1.2286(8) 0.3071(9) 0.4704(7) 0.076(4) Uani 0.50 1 d PDU B 2 H47C H 1.2364 0.3393 0.4299 0.091 Uiso 0.50 1 calc PR B 2 H47D H 1.2426 0.2634 0.4512 0.091 Uiso 0.50 1 calc PR B 2 C48 C 1.1519(8) 0.2522(7) 0.2722(7) 0.054(4) Uani 1 1 d . B . H48A H 1.1259 0.2210 0.2361 0.065 Uiso 1 1 calc R . . H48B H 1.1698 0.2285 0.3185 0.065 Uiso 1 1 calc R . . C49 C 1.2212(8) 0.2870(9) 0.2381(8) 0.073(5) Uani 1 1 d . . . H49A H 1.2630 0.2976 0.2776 0.087 Uiso 1 1 calc R B . H49B H 1.2451 0.2587 0.2003 0.087 Uiso 1 1 calc R . . C50 C 1.1898(9) 0.3474(9) 0.2024(8) 0.072(5) Uani 1 1 d . B . H50A H 1.1905 0.3448 0.1470 0.087 Uiso 1 1 calc R . . H50B H 1.2210 0.3860 0.2202 0.087 Uiso 1 1 calc R . . C51 C 1.1022(8) 0.3499(7) 0.2288(7) 0.057(4) Uani 1 1 d . B . H51A H 1.0892 0.3943 0.2464 0.069 Uiso 1 1 calc R . . H51B H 1.0635 0.3378 0.1871 0.069 Uiso 1 1 calc R . . C52 C 0.9880(9) 0.1674(7) 0.3484(7) 0.059(4) Uani 1 1 d D B . H52A H 0.9931 0.1877 0.2984 0.071 Uiso 1 1 calc R . . H52B H 0.9305 0.1652 0.3588 0.071 Uiso 1 1 calc R . . C53 C 1.0259(10) 0.0982(7) 0.3508(6) 0.072(5) Uani 1 1 d D . . H53A H 1.0739 0.0960 0.3209 0.087 Uiso 1 1 calc R B . H53B H 0.9871 0.0643 0.3332 0.087 Uiso 1 1 calc R . . C54 C 1.0481(10) 0.0922(7) 0.4373(6) 0.077(5) Uani 1 1 d D B . H54A H 1.0008 0.0808 0.4657 0.092 Uiso 1 1 calc R . . H54B H 1.0907 0.0594 0.4478 0.092 Uiso 1 1 calc R . . C55 C 1.0774(9) 0.1616(7) 0.4552(8) 0.074(5) Uani 1 1 d D B . H55A H 1.0689 0.1727 0.5083 0.089 Uiso 1 1 calc R . . H55B H 1.1352 0.1656 0.4468 0.089 Uiso 1 1 calc R . . C56 C 0.8775(9) 0.3020(7) 0.2621(6) 0.057(4) Uani 1 1 d . B . H56A H 0.8415 0.2649 0.2718 0.068 Uiso 1 1 calc R . . H56B H 0.9229 0.2859 0.2340 0.068 Uiso 1 1 calc R . . C57 C 0.8337(9) 0.3546(8) 0.2199(8) 0.065(4) Uani 1 1 d . . . H57A H 0.7855 0.3367 0.1925 0.078 Uiso 1 1 calc R B . H57B H 0.8684 0.3749 0.1832 0.078 Uiso 1 1 calc R . . C58 C 0.8101(10) 0.4047(9) 0.2780(9) 0.082(5) Uani 1 1 d . B . H58A H 0.7512 0.4085 0.2789 0.098 Uiso 1 1 calc R . . H58B H 0.8329 0.4482 0.2674 0.098 Uiso 1 1 calc R . . C59 C 0.8458(7) 0.3774(7) 0.3522(7) 0.051(4) Uani 1 1 d . B . H59A H 0.8692 0.4129 0.3841 0.061 Uiso 1 1 calc R . . H59B H 0.8042 0.3548 0.3800 0.061 Uiso 1 1 calc R . . C60 C 0.9378(9) 0.3659(7) 0.5645(7) 0.064(4) Uani 1 1 d . B . H60A H 0.9443 0.4105 0.5442 0.077 Uiso 1 1 calc R . . H60B H 0.9747 0.3604 0.6094 0.077 Uiso 1 1 calc R . . C61 C 0.8501(11) 0.3540(11) 0.5844(10) 0.102(7) Uani 1 1 d . . . H61A H 0.8410 0.3673 0.6367 0.123 Uiso 1 1 calc R B . H61B H 0.8119 0.3772 0.5495 0.123 Uiso 1 1 calc R . . C62 C 0.8448(10) 0.2857(11) 0.5753(11) 0.101(7) Uani 1 1 d . B . H62A H 0.7900 0.2738 0.5564 0.121 Uiso 1 1 calc R . . H62B H 0.8553 0.2641 0.6246 0.121 Uiso 1 1 calc R . . C63 C 0.9044(9) 0.2617(9) 0.5210(8) 0.078(5) Uani 1 1 d . B . H63A H 0.9370 0.2253 0.5429 0.094 Uiso 1 1 calc R . . H63B H 0.8771 0.2469 0.4733 0.094 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 Yb1 0.0354(3) 0.0308(3) 0.0301(3) 0.0000(2) 0.0032(2) -0.0020(3) Yb2 0.0307(3) 0.0442(4) 0.0324(3) -0.0028(2) 0.0029(2) 0.0012(3) O1 0.058(6) 0.033(5) 0.051(5) -0.001(4) 0.016(4) -0.004(5) O2 0.037(5) 0.034(5) 0.049(5) -0.002(4) 0.013(4) 0.002(4) O3 0.030(5) 0.085(8) 0.045(5) 0.002(5) -0.008(4) -0.011(5) O4 0.053(6) 0.053(6) 0.032(4) -0.002(4) 0.009(4) -0.002(5) O5 0.080(7) 0.028(6) 0.055(6) 0.013(4) -0.016(5) -0.008(5) O6 0.035(5) 0.043(6) 0.046(5) -0.004(4) -0.012(4) -0.006(4) O7 0.048(5) 0.064(7) 0.050(5) -0.006(5) 0.018(4) -0.004(5) C1 0.032(7) 0.062(11) 0.064(9) 0.003(8) 0.009(6) 0.001(7) C2 0.021(7) 0.050(10) 0.067(9) -0.007(7) 0.006(6) -0.011(6) C3 0.035(8) 0.066(12) 0.074(10) -0.009(8) 0.010(7) -0.015(8) C4 0.057(11) 0.063(14) 0.109(14) -0.024(11) 0.001(10) 0.005(10) C5 0.053(11) 0.039(12) 0.19(2) -0.028(14) 0.015(13) -0.011(9) C6 0.053(11) 0.068(14) 0.154(18) 0.034(13) 0.017(11) -0.026(10) C7 0.045(9) 0.063(12) 0.080(10) 0.018(9) 0.004(7) -0.008(8) C8 0.049(8) 0.046(9) 0.029(6) 0.008(6) -0.005(5) 0.003(7) C9 0.046(8) 0.030(8) 0.023(6) 0.013(5) -0.013(5) -0.007(6) C10 0.052(9) 0.077(12) 0.038(7) -0.001(7) -0.005(6) -0.020(8) C11 0.078(12) 0.062(12) 0.044(8) 0.006(8) -0.009(8) -0.034(9) C12 0.114(15) 0.033(10) 0.054(9) -0.003(7) -0.002(9) 0.013(10) C13 0.063(10) 0.067(12) 0.038(7) -0.002(7) 0.006(6) 0.022(9) C14 0.052(8) 0.047(9) 0.030(6) 0.003(6) 0.014(6) -0.001(7) C15 0.055(8) 0.054(10) 0.032(6) 0.004(6) 0.004(6) -0.009(7) C16 0.058(9) 0.045(9) 0.028(6) -0.016(6) 0.006(6) -0.001(8) C17 0.060(10) 0.064(12) 0.042(8) -0.004(7) 0.000(7) -0.001(9) C18 0.103(14) 0.039(11) 0.080(11) 0.022(9) 0.012(10) -0.002(10) C19 0.135(18) 0.041(11) 0.052(9) 0.001(7) -0.001(11) -0.003(12) C20 0.073(12) 0.091(15) 0.041(8) 0.004(9) -0.017(8) 0.032(11) C21 0.066(10) 0.078(13) 0.041(8) -0.010(8) -0.011(7) 0.002(10) C22 0.033(6) 0.037(6) 0.060(6) -0.002(5) 0.005(5) -0.011(5) C23 0.035(7) 0.038(7) 0.070(8) 0.001(6) 0.014(6) -0.009(6) C24 0.045(8) 0.038(8) 0.079(9) -0.001(7) 0.016(8) -0.002(7) C25 0.059(9) 0.039(8) 0.094(9) 0.001(8) 0.018(8) 0.003(7) C26 0.055(9) 0.041(9) 0.098(10) 0.008(7) 0.020(8) 0.005(7) C27 0.048(9) 0.039(9) 0.088(9) 0.011(7) 0.010(8) -0.002(7) C28 0.039(8) 0.038(8) 0.075(8) 0.008(7) 0.014(7) -0.008(7) C22A 0.033(6) 0.037(6) 0.060(6) -0.002(5) 0.005(5) -0.011(5) C23A 0.040(8) 0.039(8) 0.076(9) 0.003(7) 0.003(8) -0.007(7) C24A 0.046(10) 0.037(10) 0.083(10) -0.004(8) 0.001(9) -0.003(8) C25A 0.055(11) 0.042(10) 0.093(12) -0.003(9) -0.004(10) 0.005(9) C26A 0.061(11) 0.043(11) 0.100(13) 0.000(9) -0.008(11) 0.007(9) C27A 0.057(11) 0.047(10) 0.097(12) 0.005(9) -0.001(11) 0.004(9) C28A 0.046(10) 0.044(10) 0.088(11) 0.009(8) 0.002(10) -0.001(8) C29 0.127(15) 0.042(10) 0.052(9) 0.000(8) 0.003(9) 0.016(10) C30 0.164(19) 0.042(11) 0.063(10) 0.005(8) 0.011(11) 0.014(12) C31 0.096(14) 0.027(11) 0.148(17) -0.024(10) -0.032(12) -0.005(10) C32 0.111(13) 0.050(11) 0.048(8) -0.016(8) -0.031(8) 0.016(10) C33 0.038(6) 0.038(6) 0.065(6) 0.007(5) 0.009(5) -0.004(5) C34 0.046(5) 0.041(5) 0.067(6) 0.005(5) 0.005(4) 0.001(5) C35 0.042(7) 0.038(7) 0.058(8) -0.005(7) 0.000(6) 0.001(6) C36 0.048(6) 0.034(6) 0.056(6) -0.001(5) 0.005(5) 0.006(5) C33A 0.038(6) 0.038(6) 0.065(6) 0.007(5) 0.009(5) -0.004(5) C34A 0.046(5) 0.041(5) 0.067(6) 0.005(5) 0.005(4) 0.001(5) C35A 0.047(7) 0.040(7) 0.071(8) 0.007(7) 0.008(7) 0.004(7) C36A 0.048(6) 0.034(6) 0.056(6) -0.001(5) 0.005(5) 0.006(5) C37 0.048(8) 0.060(10) 0.036(7) -0.026(6) 0.003(6) 0.011(7) C38 0.055(9) 0.042(9) 0.046(8) -0.016(6) 0.006(7) -0.008(7) C39 0.063(10) 0.060(11) 0.066(9) -0.019(8) 0.006(8) -0.018(9) C40 0.063(11) 0.092(15) 0.081(12) -0.032(10) 0.028(9) -0.029(10) C41 0.058(10) 0.097(15) 0.073(11) -0.015(10) -0.002(8) -0.025(10) C42 0.060(10) 0.080(13) 0.050(8) -0.011(8) -0.001(7) -0.002(9) C43 0.041(8) 0.051(10) 0.052(8) -0.002(7) 0.021(6) 0.004(7) C44 0.055(6) 0.127(12) 0.051(7) -0.003(7) -0.006(6) -0.007(7) C45 0.057(8) 0.130(13) 0.053(8) -0.007(9) -0.012(7) -0.002(9) C46 0.050(8) 0.131(13) 0.064(8) -0.017(9) -0.015(7) 0.007(9) C47 0.041(7) 0.126(12) 0.060(6) -0.020(7) -0.006(5) 0.007(7) C44A 0.055(6) 0.127(12) 0.051(7) -0.003(7) -0.006(6) -0.007(7) C45A 0.055(8) 0.125(13) 0.057(8) -0.011(9) -0.010(7) -0.002(9) C46A 0.044(8) 0.122(13) 0.062(8) -0.015(9) -0.009(7) 0.004(9) C47A 0.041(7) 0.126(12) 0.060(6) -0.020(7) -0.006(5) 0.007(7) C48 0.060(9) 0.066(11) 0.038(7) 0.000(7) 0.012(6) 0.033(8) C49 0.044(9) 0.112(16) 0.063(9) 0.008(10) 0.010(7) 0.027(10) C50 0.066(11) 0.098(15) 0.054(9) -0.005(9) 0.014(8) -0.024(10) C51 0.069(10) 0.059(11) 0.045(8) -0.003(7) 0.012(7) 0.007(8) C52 0.067(10) 0.053(11) 0.059(9) -0.003(8) 0.005(7) 0.002(9) C53 0.111(13) 0.065(12) 0.038(8) -0.023(7) -0.025(8) -0.001(10) C54 0.113(14) 0.068(13) 0.048(9) 0.037(8) -0.011(8) -0.019(11) C55 0.071(11) 0.080(14) 0.070(10) 0.012(9) -0.018(8) 0.002(10) C56 0.072(10) 0.075(12) 0.021(6) -0.006(6) -0.006(6) 0.005(8) C57 0.078(11) 0.058(11) 0.057(9) 0.006(8) -0.020(8) -0.012(9) C58 0.071(11) 0.073(14) 0.103(13) 0.037(11) 0.020(10) 0.020(10) C59 0.031(7) 0.068(11) 0.055(8) -0.018(7) 0.000(6) 0.010(7) C60 0.095(12) 0.054(11) 0.045(8) -0.003(7) 0.023(8) 0.017(9) C61 0.087(14) 0.125(19) 0.102(14) 0.032(13) 0.072(11) 0.056(14) C62 0.057(11) 0.13(2) 0.116(15) 0.045(15) 0.043(10) 0.024(13) C63 0.063(10) 0.105(16) 0.071(10) 0.021(10) 0.030(8) -0.029(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 O2 2.324(8) . ? Yb1 O1 2.364(8) . ? Yb1 C15 2.481(10) . ? Yb1 C1 2.485(11) . ? Yb1 C8 2.504(10) . ? Yb1 C22 2.520(11) . ? Yb2 O3 2.382(8) . ? Yb2 O7 2.396(8) . ? Yb2 O4 2.428(7) . ? Yb2 O6 2.428(7) . ? Yb2 O5 2.508(9) . ? Yb2 C37 2.566(14) . ? O1 C32 1.386(14) . ? O1 C29 1.437(15) . ? O2 C36 1.438(13) . ? O2 C33 1.475(13) . ? O3 C44 1.415(15) . ? O3 C47 1.443(15) . ? O4 C48 1.413(14) . ? O4 C51 1.415(15) . ? O5 C52 1.431(13) . ? O5 C55 1.440(13) . ? O6 C59 1.418(14) . ? O6 C56 1.455(13) . ? O7 C60 1.417(15) . ? O7 C63 1.431(16) . ? C1 C2 1.457(18) . ? C2 C3 1.354(18) . ? C2 C7 1.428(18) . ? C3 C4 1.37(2) . ? C4 C5 1.37(2) . ? C5 C6 1.39(2) . ? C6 C7 1.37(2) . ? C8 C9 1.449(16) . ? C9 C14 1.394(16) . ? C9 C10 1.398(17) . ? C10 C11 1.38(2) . ? C11 C12 1.37(2) . ? C12 C13 1.43(2) . ? C13 C14 1.351(18) . ? C15 C16 1.499(17) . ? C16 C17 1.389(18) . ? C16 C21 1.394(18) . ? C17 C18 1.335(19) . ? C18 C19 1.33(2) . ? C19 C20 1.36(2) . ? C20 C21 1.39(2) . ? C22 C23 1.5300(10) . ? C23 C24 1.3900 . ? C23 C28 1.3900 . ? C24 C25 1.3900 . ? C25 C26 1.3900 . ? C26 C27 1.3900 . ? C27 C28 1.3900 . ? C23A C24A 1.3900 . ? C23A C28A 1.3900 . ? C24A C25A 1.3900 . ? C25A C26A 1.3900 . ? C26A C27A 1.3900 . ? C27A C28A 1.3900 . ? C29 C30 1.54(2) . ? C30 C31 1.47(2) . ? C31 C32 1.47(2) . ? C33 C34 1.5000(8) . ? C34 C35 1.5002(10) . ? C35 C36 1.5001(11) . ? C37 C38 1.435(16) . ? C38 C43 1.370(16) . ? C38 C39 1.396(17) . ? C39 C40 1.372(19) . ? C40 C41 1.399(19) . ? C41 C42 1.374(19) . ? C42 C43 1.378(17) . ? C44 C45 1.5000(11) . ? C45 C46 1.4999(10) . ? C46 C47 1.5001(10) . ? C45A C46A 1.5000(10) . ? C48 C49 1.515(19) . ? C49 C50 1.47(2) . ? C50 C51 1.565(18) . ? C52 C53 1.551(14) . ? C53 C54 1.570(13) . ? C54 C55 1.531(15) . ? C56 C57 1.482(18) . ? C57 C58 1.52(2) . ? C58 C59 1.526(18) . ? C60 C61 1.55(2) . ? C61 C62 1.41(2) . ? C62 C63 1.51(2) . ? 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 O2 Yb1 O1 177.2(3) . . ? O2 Yb1 C15 93.4(4) . . ? O1 Yb1 C15 83.9(4) . . ? O2 Yb1 C1 86.0(4) . . ? O1 Yb1 C1 93.7(4) . . ? C15 Yb1 C1 89.7(4) . . ? O2 Yb1 C8 95.2(3) . . ? O1 Yb1 C8 87.5(4) . . ? C15 Yb1 C8 171.4(4) . . ? C1 Yb1 C8 90.5(4) . . ? O2 Yb1 C22 85.8(3) . . ? O1 Yb1 C22 94.5(3) . . ? C15 Yb1 C22 90.3(4) . . ? C1 Yb1 C22 171.7(4) . . ? C8 Yb1 C22 90.8(4) . . ? O3 Yb2 O7 86.7(3) . . ? O3 Yb2 O4 97.3(3) . . ? O7 Yb2 O4 163.2(3) . . ? O3 Yb2 O6 168.8(3) . . ? O7 Yb2 O6 84.0(3) . . ? O4 Yb2 O6 89.9(3) . . ? O3 Yb2 O5 80.5(3) . . ? O7 Yb2 O5 84.4(3) . . ? O4 Yb2 O5 80.2(3) . . ? O6 Yb2 O5 92.5(3) . . ? O3 Yb2 C37 97.2(4) . . ? O7 Yb2 C37 98.5(3) . . ? O4 Yb2 C37 97.2(3) . . ? O6 Yb2 C37 90.3(3) . . ? O5 Yb2 C37 176.2(3) . . ? C32 O1 C29 110.0(10) . . ? C32 O1 Yb1 129.7(8) . . ? C29 O1 Yb1 120.4(8) . . ? C36 O2 C33 105.7(8) . . ? C36 O2 Yb1 128.0(6) . . ? C33 O2 Yb1 126.1(6) . . ? C44 O3 C47 106.8(8) . . ? C44 O3 Yb2 125.6(7) . . ? C47 O3 Yb2 126.1(7) . . ? C48 O4 C51 107.7(9) . . ? C48 O4 Yb2 129.0(7) . . ? C51 O4 Yb2 122.6(8) . . ? C52 O5 C55 110.6(11) . . ? C52 O5 Yb2 121.6(7) . . ? C55 O5 Yb2 127.4(8) . . ? C59 O6 C56 106.9(9) . . ? C59 O6 Yb2 121.2(7) . . ? C56 O6 Yb2 131.6(7) . . ? C60 O7 C63 109.6(10) . . ? C60 O7 Yb2 128.7(8) . . ? C63 O7 Yb2 121.5(8) . . ? C2 C1 Yb1 116.8(9) . . ? C3 C2 C7 115.5(13) . . ? C3 C2 C1 122.6(13) . . ? C7 C2 C1 121.9(13) . . ? C2 C3 C4 124.1(16) . . ? C3 C4 C5 119.2(17) . . ? C4 C5 C6 120.3(17) . . ? C7 C6 C5 118.5(17) . . ? C6 C7 C2 122.2(15) . . ? C9 C8 Yb1 110.7(7) . . ? C14 C9 C10 115.4(12) . . ? C14 C9 C8 122.6(11) . . ? C10 C9 C8 122.0(12) . . ? C11 C10 C9 121.9(13) . . ? C12 C11 C10 121.9(14) . . ? C11 C12 C13 116.8(14) . . ? C14 C13 C12 120.3(13) . . ? C13 C14 C9 123.6(13) . . ? C16 C15 Yb1 115.0(8) . . ? C17 C16 C21 115.3(14) . . ? C17 C16 C15 121.5(13) . . ? C21 C16 C15 123.2(13) . . ? C18 C17 C16 123.9(15) . . ? C19 C18 C17 120.4(17) . . ? C18 C19 C20 119.6(16) . . ? C19 C20 C21 120.9(15) . . ? C20 C21 C16 119.9(15) . . ? C23 C22 Yb1 112.2(9) . . ? C24 C23 C28 120.0 . . ? C24 C23 C22 119.9(11) . . ? C28 C23 C22 120.1(11) . . ? C23 C24 C25 120.0 . . ? C24 C25 C26 120.0 . . ? C25 C26 C27 120.0 . . ? C28 C27 C26 120.0 . . ? C27 C28 C23 120.0 . . ? C24A C23A C28A 120.0 . . ? C25A C24A C23A 120.0 . . ? C24A C25A C26A 120.0 . . ? C25A C26A C27A 120.0 . . ? C28A C27A C26A 120.0 . . ? C27A C28A C23A 120.0 . . ? O1 C29 C30 104.3(11) . . ? C31 C30 C29 101.2(14) . . ? C32 C31 C30 103.6(13) . . ? O1 C32 C31 106.7(12) . . ? O2 C33 C34 107.4(9) . . ? C33 C34 C35 94.6(11) . . ? C36 C35 C34 104.8(9) . . ? O2 C36 C35 103.8(11) . . ? C38 C37 Yb2 106.3(9) . . ? C43 C38 C39 115.6(13) . . ? C43 C38 C37 123.7(12) . . ? C39 C38 C37 120.7(12) . . ? C40 C39 C38 122.8(13) . . ? C39 C40 C41 120.1(14) . . ? C42 C41 C40 117.4(14) . . ? C41 C42 C43 121.2(13) . . ? C38 C43 C42 122.7(12) . . ? O3 C44 C45 113.4(13) . . ? C46 C45 C44 96.2(17) . . ? C45 C46 C47 108.2(17) . . ? O3 C47 C46 103.1(15) . . ? O4 C48 C49 102.8(12) . . ? C50 C49 C48 107.7(11) . . ? C49 C50 C51 102.5(12) . . ? O4 C51 C50 105.5(11) . . ? O5 C52 C53 105.7(10) . . ? C52 C53 C54 100.0(10) . . ? C55 C54 C53 100.8(10) . . ? O5 C55 C54 106.2(10) . . ? O6 C56 C57 104.6(11) . . ? C56 C57 C58 106.4(11) . . ? C57 C58 C59 103.9(12) . . ? O6 C59 C58 105.5(10) . . ? O7 C60 C61 104.8(13) . . ? C62 C61 C60 100.7(13) . . ? C61 C62 C63 110.9(15) . . ? O7 C63 C62 103.1(15) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.083 _refine_diff_density_min -1.323 _refine_diff_density_rms 0.164