Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_requested_category FM loop_ _publ_author_name F.G.N.Cloke A.G.Avent B.R.Elvidge P.B.Hitchcock _publ_contact_author_name 'Prof F.G.N. Cloke' _publ_contact_author_email F.G.CLOKE@SUSSEX.AC.UK data_[Y{ArN(CH2)3NAr}(CH2C6H5)(THF)2]_[7] _database_code_depnum_ccdc_archive 'CCDC 228144' _audit_creation_date 2002-09-18T17:02:49-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common ; [Y(CH2Ph)(thf)2{C6H3iPr2N(CH2)3NC6H3iPr2}] ; _chemical_formula_moiety 'C42 H63 N2 O2 Y1' _chemical_formula_sum 'C42 H63 N2 O2 Y' _chemical_formula_weight 716.85 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1) _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.1530(2) _cell_length_b 19.1733(4) _cell_length_c 11.5265(3) _cell_angle_alpha 90 _cell_angle_beta 99.595(1) _cell_angle_gamma 90 _cell_volume 1994.52(8) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8485 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.194 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.497 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.6216 _exptl_absorpt_correction_T_max 0.7243 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0492 _diffrn_reflns_av_unetI/netI 0.0574 _diffrn_reflns_number 13142 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.74 _diffrn_reflns_theta_max 25.02 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.985 _diffrn_measured_fraction_theta_max 0.985 _reflns_number_total 6240 _reflns_number_gt 5548 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0313P)^2^+1.6991P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 6240 _refine_ls_number_parameters 424 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0524 _refine_ls_R_factor_gt 0.0422 _refine_ls_wR_factor_ref 0.097 _refine_ls_wR_factor_gt 0.0916 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.016(6) _refine_diff_density_max 0.324 _refine_diff_density_min -0.269 _refine_diff_density_rms 0.05 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Y Y 0.15175(4) 0.39274(2) 0.30412(3) 0.02927(10) Uani 1 1 d . . . O1 O 0.2703(5) 0.46197(19) 0.4720(3) 0.0620(10) Uani 1 1 d . . . O2 O 0.3412(4) 0.31984(19) 0.4098(3) 0.0550(9) Uani 1 1 d . . . N1 N 0.1369(4) 0.32169(19) 0.1511(3) 0.0313(8) Uani 1 1 d . . . N2 N 0.1147(4) 0.48577(18) 0.1927(3) 0.0302(8) Uani 1 1 d . . . C1 C 0.0442(5) 0.3450(2) 0.0415(4) 0.0406(11) Uani 1 1 d . . . H1A H -0.0204 0.3059 0.0089 0.049 Uiso 1 1 calc R . . H1B H 0.1093 0.3565 -0.0162 0.049 Uiso 1 1 calc R . . C2 C -0.0522(4) 0.4076(2) 0.0548(3) 0.0324(11) Uani 1 1 d . . . H2A H -0.1284 0.4111 -0.0168 0.039 Uiso 1 1 calc R . . H2B H -0.1045 0.3989 0.122 0.039 Uiso 1 1 calc R . . C3 C 0.0249(5) 0.4773(2) 0.0741(4) 0.0358(10) Uani 1 1 d . . . H3A H 0.0903 0.4832 0.0145 0.043 Uiso 1 1 calc R . . H3B H -0.0506 0.5147 0.0615 0.043 Uiso 1 1 calc R . . C4 C 0.1982(4) 0.2546(2) 0.1420(4) 0.0320(9) Uani 1 1 d . . . C5 C 0.3394(5) 0.2458(2) 0.1071(4) 0.0422(11) Uani 1 1 d . . . C6 C 0.4012(5) 0.1794(3) 0.1110(5) 0.0553(13) Uani 1 1 d . . . H6 H 0.4967 0.1738 0.0904 0.066 Uiso 1 1 calc R . . C7 C 0.3292(5) 0.1214(3) 0.1437(5) 0.0519(13) Uani 1 1 d . . . H7 H 0.3758 0.077 0.1485 0.062 Uiso 1 1 calc R . . C8 C 0.1875(5) 0.1292(2) 0.1694(4) 0.0427(11) Uani 1 1 d . . . H8 H 0.1351 0.0892 0.1885 0.051 Uiso 1 1 calc R . . C9 C 0.1205(5) 0.1941(2) 0.1680(4) 0.0338(9) Uani 1 1 d . . . C10 C 0.4182(5) 0.3060(3) 0.0582(5) 0.0537(14) Uani 1 1 d . . . H10 H 0.3767 0.3503 0.085 0.064 Uiso 1 1 calc R . . C11 C 0.5838(6) 0.3074(4) 0.0990(8) 0.101(3) Uani 1 1 d . . . H11A H 0.6264 0.3476 0.064 0.152 Uiso 1 1 calc R . . H11B H 0.6277 0.2644 0.0744 0.152 Uiso 1 1 calc R . . H11C H 0.6048 0.3112 0.1849 0.152 Uiso 1 1 calc R . . C12 C 0.3879(8) 0.3059(3) -0.0788(6) 0.0783(19) Uani 1 1 d . . . H12A H 0.4398 0.3452 -0.108 0.117 Uiso 1 1 calc R . . H12B H 0.2812 0.3103 -0.1068 0.117 Uiso 1 1 calc R . . H12C H 0.4237 0.2621 -0.1077 0.117 Uiso 1 1 calc R . . C13 C -0.0389(5) 0.1974(2) 0.1887(4) 0.0408(10) Uani 1 1 d . . . H13 H -0.0704 0.2474 0.1856 0.049 Uiso 1 1 calc R . . C14 C -0.0558(7) 0.1679(3) 0.3090(6) 0.0683(18) Uani 1 1 d . . . H14A H -0.1597 0.1712 0.3193 0.102 Uiso 1 1 calc R . . H14B H 0.0061 0.1947 0.3709 0.102 Uiso 1 1 calc R . . H14C H -0.0247 0.119 0.3138 0.102 Uiso 1 1 calc R . . C15 C -0.1391(5) 0.1580(3) 0.0916(6) 0.0682(17) Uani 1 1 d . . . H15A H -0.2419 0.1606 0.1052 0.102 Uiso 1 1 calc R . . H15B H -0.1082 0.109 0.0921 0.102 Uiso 1 1 calc R . . H15C H -0.1318 0.1789 0.0152 0.102 Uiso 1 1 calc R . . C16 C 0.1822(5) 0.5529(2) 0.2041(4) 0.0309(9) Uani 1 1 d . . . C17 C 0.1063(5) 0.6111(2) 0.2380(4) 0.0351(9) Uani 1 1 d . . . C18 C 0.1771(5) 0.6755(2) 0.2510(4) 0.0454(11) Uani 1 1 d . . . H18 H 0.1259 0.7145 0.2754 0.054 Uiso 1 1 calc R . . C19 C 0.3187(6) 0.6841(3) 0.2294(5) 0.0540(13) Uani 1 1 d . . . H19 H 0.3653 0.7285 0.2388 0.065 Uiso 1 1 calc R . . C20 C 0.3928(6) 0.6273(3) 0.1938(5) 0.0526(13) Uani 1 1 d . . . H20 H 0.4905 0.6332 0.1778 0.063 Uiso 1 1 calc R . . C21 C 0.3284(5) 0.5620(2) 0.1809(4) 0.0383(10) Uani 1 1 d . . . C22 C -0.0519(5) 0.6062(3) 0.2593(4) 0.0399(11) Uani 1 1 d . . . H22 H -0.0867 0.5572 0.2424 0.048 Uiso 1 1 calc R . . C23 C -0.1531(6) 0.6543(3) 0.1787(7) 0.079(2) Uani 1 1 d . . . H23A H -0.2545 0.6497 0.1947 0.118 Uiso 1 1 calc R . . H23B H -0.1507 0.6418 0.0966 0.118 Uiso 1 1 calc R . . H23C H -0.1196 0.7026 0.1927 0.118 Uiso 1 1 calc R . . C24 C -0.0625(9) 0.6226(4) 0.3884(6) 0.088(2) Uani 1 1 d . . . H24A H -0.166 0.6188 0.3998 0.132 Uiso 1 1 calc R . . H24B H -0.0266 0.67 0.4074 0.132 Uiso 1 1 calc R . . H24C H -0.0018 0.5893 0.44 0.132 Uiso 1 1 calc R . . C25 C 0.4153(5) 0.5016(2) 0.1423(5) 0.0471(12) Uani 1 1 d . . . H25 H 0.3543 0.4586 0.145 0.057 Uiso 1 1 calc R . . C26 C 0.5623(8) 0.4899(5) 0.2241(8) 0.111(3) Uani 1 1 d . . . H26A H 0.6139 0.4502 0.1959 0.166 Uiso 1 1 calc R . . H26B H 0.5435 0.4802 0.3038 0.166 Uiso 1 1 calc R . . H26C H 0.6238 0.5318 0.2252 0.166 Uiso 1 1 calc R . . C27 C 0.4428(10) 0.5099(4) 0.0169(7) 0.100(3) Uani 1 1 d . . . H27A H 0.4985 0.4696 -0.0045 0.15 Uiso 1 1 calc R . . H27B H 0.4999 0.5526 0.0105 0.15 Uiso 1 1 calc R . . H27C H 0.3477 0.5129 -0.0365 0.15 Uiso 1 1 calc R . . C28 C -0.0772(5) 0.3617(3) 0.3772(4) 0.0502(12) Uani 1 1 d . . . H28A H -0.161 0.3757 0.3158 0.06 Uiso 1 1 calc R . . H28B H -0.0799 0.3102 0.3823 0.06 Uiso 1 1 calc R . . C29 C -0.1084(4) 0.3892(4) 0.4902(3) 0.0427(9) Uani 1 1 d . . . C30 C -0.1664(5) 0.4548(3) 0.5004(4) 0.0452(11) Uani 1 1 d . . . H30 H -0.1909 0.4826 0.4317 0.054 Uiso 1 1 calc R . . C31 C -0.1901(7) 0.4815(3) 0.6062(5) 0.0621(14) Uani 1 1 d . . . H31 H -0.2259 0.5278 0.61 0.075 Uiso 1 1 calc R . . C32 C -0.1623(9) 0.4415(4) 0.7074(5) 0.080(2) Uani 1 1 d . . . H32 H -0.1818 0.4592 0.7803 0.096 Uiso 1 1 calc R . . C33 C -0.1069(10) 0.3764(3) 0.7003(5) 0.089(2) Uani 1 1 d . . . H33 H -0.0849 0.3487 0.7694 0.106 Uiso 1 1 calc R . . C34 C -0.0817(7) 0.3497(3) 0.5939(4) 0.0632(15) Uani 1 1 d . . . H34 H -0.0454 0.3034 0.5911 0.076 Uiso 1 1 calc R . . C35 C 0.2568(11) 0.4392(5) 0.5890(5) 0.130(4) Uani 1 1 d . . . H35A H 0.1511 0.4392 0.5982 0.156 Uiso 1 1 calc R . . H35B H 0.2953 0.3911 0.6019 0.156 Uiso 1 1 calc R . . C36 C 0.3364(14) 0.4839(6) 0.6711(6) 0.150(5) Uani 1 1 d . . . H36A H 0.4251 0.4599 0.7136 0.18 Uiso 1 1 calc R . . H36B H 0.2743 0.4989 0.7291 0.18 Uiso 1 1 calc R . . C37 C 0.3796(9) 0.5433(4) 0.6085(6) 0.096(2) Uani 1 1 d . . . H37A H 0.3239 0.5852 0.6258 0.115 Uiso 1 1 calc R . . H37B H 0.4869 0.5526 0.6321 0.115 Uiso 1 1 calc R . . C38 C 0.3469(13) 0.5269(4) 0.4871(7) 0.117(4) Uani 1 1 d . . . H38A H 0.4399 0.5238 0.4542 0.14 Uiso 1 1 calc R . . H38B H 0.2848 0.5641 0.4446 0.14 Uiso 1 1 calc R . . C39 C 0.3123(11) 0.2550(4) 0.4641(9) 0.102(3) Uani 1 1 d . . . H39A H 0.2846 0.2642 0.5421 0.123 Uiso 1 1 calc R . . H39B H 0.2283 0.2309 0.4149 0.123 Uiso 1 1 calc R . . C40 C 0.4343(11) 0.2135(6) 0.4770(12) 0.167(5) Uani 1 1 d . . . H40A H 0.416 0.1731 0.423 0.201 Uiso 1 1 calc R . . H40B H 0.4563 0.1956 0.5586 0.201 Uiso 1 1 calc R . . C41 C 0.5581(9) 0.2532(6) 0.4509(10) 0.143(4) Uani 1 1 d . . . H41A H 0.5981 0.232 0.3845 0.171 Uiso 1 1 calc R . . H41B H 0.6379 0.255 0.5203 0.171 Uiso 1 1 calc R . . C42 C 0.4983(7) 0.3268(5) 0.4183(10) 0.124(4) Uani 1 1 d . . . H42A H 0.5383 0.3609 0.48 0.148 Uiso 1 1 calc R . . H42B H 0.5248 0.342 0.3424 0.148 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 Y 0.03663(18) 0.02380(16) 0.02664(16) -0.0008(2) 0.00309(12) -0.0017(3) O1 0.087(3) 0.056(2) 0.0355(18) -0.0106(17) -0.0136(18) -0.022(2) O2 0.055(2) 0.049(2) 0.056(2) 0.0100(17) -0.0062(17) 0.0052(17) N1 0.038(2) 0.026(2) 0.0294(19) -0.0010(15) 0.0049(16) 0.0029(15) N2 0.036(2) 0.0197(18) 0.0341(19) 0.0013(15) 0.0027(16) -0.0055(15) C1 0.053(3) 0.032(2) 0.035(2) -0.005(2) 0.003(2) 0.001(2) C2 0.0322(18) 0.035(3) 0.0284(18) 0.0003(17) 0.0012(15) -0.0022(18) C3 0.042(2) 0.032(2) 0.032(2) 0.0064(19) 0.001(2) -0.002(2) C4 0.034(2) 0.027(2) 0.033(2) -0.0083(18) 0.0007(19) 0.0008(18) C5 0.036(2) 0.030(2) 0.060(3) -0.014(2) 0.008(2) -0.004(2) C6 0.035(3) 0.042(3) 0.088(4) -0.015(3) 0.009(3) 0.003(2) C7 0.044(3) 0.031(3) 0.079(4) -0.003(3) 0.006(3) 0.011(2) C8 0.052(3) 0.026(2) 0.050(3) -0.003(2) 0.008(2) 0.002(2) C9 0.036(2) 0.030(2) 0.035(2) -0.0055(19) 0.0046(19) 0.0009(19) C10 0.042(3) 0.032(3) 0.093(4) -0.016(3) 0.027(3) -0.010(2) C11 0.047(3) 0.074(5) 0.185(8) -0.018(5) 0.024(4) -0.018(3) C12 0.099(5) 0.048(4) 0.102(5) -0.009(3) 0.058(4) -0.011(3) C13 0.048(3) 0.028(2) 0.049(3) -0.005(2) 0.016(2) -0.005(2) C14 0.082(4) 0.056(4) 0.080(4) 0.013(3) 0.053(4) 0.003(3) C15 0.039(3) 0.066(4) 0.099(4) -0.037(3) 0.011(3) -0.006(3) C16 0.034(2) 0.023(2) 0.035(2) 0.0038(18) 0.0050(19) -0.0006(18) C17 0.040(2) 0.028(2) 0.038(2) 0.0001(18) 0.008(2) 0.0001(18) C18 0.055(3) 0.025(2) 0.058(3) -0.009(2) 0.015(2) -0.003(2) C19 0.056(3) 0.027(3) 0.081(4) -0.003(2) 0.014(3) -0.012(2) C20 0.038(3) 0.040(3) 0.080(4) 0.004(3) 0.011(3) -0.007(2) C21 0.033(2) 0.029(2) 0.052(3) 0.005(2) 0.005(2) 0.0005(19) C22 0.041(3) 0.035(3) 0.048(3) -0.003(2) 0.020(2) -0.001(2) C23 0.044(3) 0.065(4) 0.131(6) 0.028(4) 0.024(4) 0.017(3) C24 0.125(6) 0.068(4) 0.088(5) -0.019(4) 0.070(4) -0.033(4) C25 0.039(3) 0.029(2) 0.077(3) 0.006(2) 0.022(3) 0.000(2) C26 0.075(5) 0.099(6) 0.146(7) -0.002(5) -0.016(5) 0.044(4) C27 0.138(7) 0.077(5) 0.099(5) 0.029(4) 0.061(5) 0.053(5) C28 0.063(3) 0.048(3) 0.046(3) -0.008(2) 0.029(2) -0.011(2) C29 0.059(2) 0.034(2) 0.0379(19) -0.009(3) 0.0161(17) -0.016(3) C30 0.057(3) 0.045(3) 0.035(2) -0.001(2) 0.012(2) -0.008(2) C31 0.092(4) 0.036(3) 0.060(3) -0.008(2) 0.019(3) 0.006(3) C32 0.152(7) 0.054(4) 0.041(3) -0.011(3) 0.038(4) -0.007(4) C33 0.186(7) 0.045(5) 0.041(3) 0.008(2) 0.038(4) 0.000(4) C34 0.112(5) 0.035(3) 0.048(3) 0.004(2) 0.029(3) 0.007(3) C35 0.190(9) 0.151(8) 0.044(4) -0.004(4) 0.008(5) -0.098(7) C36 0.272(14) 0.123(8) 0.047(4) -0.027(5) 0.002(6) -0.052(8) C37 0.112(6) 0.084(5) 0.081(5) -0.040(4) -0.015(4) -0.013(4) C38 0.198(10) 0.062(5) 0.073(5) -0.002(4) -0.030(6) -0.043(6) C39 0.120(6) 0.060(5) 0.116(6) 0.047(5) -0.009(5) 0.003(5) C40 0.116(8) 0.106(8) 0.268(15) 0.096(9) -0.001(9) 0.041(6) C41 0.075(5) 0.153(9) 0.203(10) 0.094(8) 0.032(6) 0.056(6) C42 0.043(4) 0.127(8) 0.198(9) 0.067(7) 0.010(5) 0.007(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Y N2 2.191(3) . ? Y N1 2.215(4) . ? Y O2 2.396(3) . ? Y O1 2.447(3) . ? Y C28 2.458(4) . ? O1 C38 1.424(9) . ? O1 C35 1.442(7) . ? O2 C42 1.431(7) . ? O2 C39 1.436(8) . ? N1 C4 1.414(5) . ? N1 C1 1.469(6) . ? N2 C16 1.424(5) . ? N2 C3 1.482(5) . ? C1 C2 1.513(6) . ? C2 C3 1.509(6) . ? C4 C9 1.420(6) . ? C4 C5 1.427(6) . ? C5 C6 1.390(7) . ? C5 C10 1.519(7) . ? C6 C7 1.375(7) . ? C7 C8 1.387(7) . ? C8 C9 1.386(6) . ? C9 C13 1.518(6) . ? C10 C11 1.510(8) . ? C10 C12 1.557(9) . ? C13 C15 1.524(7) . ? C13 C14 1.529(7) . ? C16 C17 1.404(6) . ? C16 C21 1.419(6) . ? C17 C18 1.391(6) . ? C17 C22 1.511(6) . ? C18 C19 1.370(7) . ? C19 C20 1.382(8) . ? C20 C21 1.380(7) . ? C21 C25 1.513(6) . ? C22 C23 1.512(7) . ? C22 C24 1.540(8) . ? C25 C27 1.517(8) . ? C25 C26 1.525(8) . ? C28 C29 1.477(6) . ? C29 C30 1.378(8) . ? C29 C34 1.401(7) . ? C30 C31 1.373(7) . ? C31 C32 1.384(8) . ? C32 C33 1.355(9) . ? C33 C34 1.383(7) . ? C35 C36 1.389(10) . ? C36 C37 1.439(12) . ? C37 C38 1.417(11) . ? C39 C40 1.359(12) . ? C40 C41 1.437(12) . ? C41 C42 1.537(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Y N1 92.92(14) . . ? N2 Y O2 143.22(13) . . ? N1 Y O2 89.37(13) . . ? N2 Y O1 91.53(12) . . ? N1 Y O1 157.50(14) . . ? O2 Y O1 74.12(12) . . ? N2 Y C28 109.90(16) . . ? N1 Y C28 100.47(14) . . ? O2 Y C28 105.72(16) . . ? O1 Y C28 98.70(15) . . ? C38 O1 C35 105.5(5) . . ? C38 O1 Y 135.6(4) . . ? C35 O1 Y 118.7(4) . . ? C42 O2 C39 107.8(6) . . ? C42 O2 Y 127.9(4) . . ? C39 O2 Y 123.8(4) . . ? C4 N1 C1 113.1(3) . . ? C4 N1 Y 130.2(3) . . ? C1 N1 Y 116.6(3) . . ? C16 N2 C3 110.5(3) . . ? C16 N2 Y 131.3(3) . . ? C3 N2 Y 117.3(3) . . ? N1 C1 C2 114.7(3) . . ? C3 C2 C1 116.8(4) . . ? N2 C3 C2 114.0(3) . . ? N1 C4 C9 120.6(4) . . ? N1 C4 C5 121.3(4) . . ? C9 C4 C5 118.1(4) . . ? C6 C5 C4 118.8(5) . . ? C6 C5 C10 119.6(4) . . ? C4 C5 C10 121.5(4) . . ? C7 C6 C5 122.5(5) . . ? C6 C7 C8 118.7(4) . . ? C9 C8 C7 121.5(4) . . ? C8 C9 C4 120.0(4) . . ? C8 C9 C13 118.1(4) . . ? C4 C9 C13 121.8(4) . . ? C11 C10 C5 114.3(5) . . ? C11 C10 C12 108.4(5) . . ? C5 C10 C12 111.1(4) . . ? C9 C13 C15 109.9(4) . . ? C9 C13 C14 111.9(4) . . ? C15 C13 C14 110.0(5) . . ? C17 C16 C21 118.7(4) . . ? C17 C16 N2 121.1(4) . . ? C21 C16 N2 120.2(4) . . ? C18 C17 C16 119.5(4) . . ? C18 C17 C22 118.7(4) . . ? C16 C17 C22 121.8(4) . . ? C19 C18 C17 121.7(4) . . ? C18 C19 C20 119.0(4) . . ? C21 C20 C19 121.7(5) . . ? C20 C21 C16 119.4(4) . . ? C20 C21 C25 119.3(4) . . ? C16 C21 C25 121.3(4) . . ? C23 C22 C17 111.6(4) . . ? C23 C22 C24 109.7(5) . . ? C17 C22 C24 111.1(5) . . ? C21 C25 C27 112.3(4) . . ? C21 C25 C26 112.5(5) . . ? C27 C25 C26 109.6(6) . . ? C29 C28 Y 121.2(3) . . ? C30 C29 C34 115.8(4) . . ? C30 C29 C28 122.3(5) . . ? C34 C29 C28 121.9(6) . . ? C31 C30 C29 122.4(4) . . ? C30 C31 C32 120.5(5) . . ? C33 C32 C31 118.5(5) . . ? C32 C33 C34 120.9(5) . . ? C33 C34 C29 121.7(5) . . ? C36 C35 O1 109.5(7) . . ? C35 C36 C37 107.7(6) . . ? C38 C37 C36 106.8(6) . . ? C37 C38 O1 109.5(7) . . ? C40 C39 O2 110.3(8) . . ? C39 C40 C41 109.2(8) . . ? C40 C41 C42 106.1(6) . . ? O2 C42 C41 104.1(6) . . ? #===END data_[Y{ArN(CH2)3NAr}{N(SiMe3)2}(THF)]_[8] _database_code_depnum_ccdc_archive 'CCDC 228145' _audit_creation_date 2002-07-25T15:59:29-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common ; '[Y(thf){N(SiMe3)2}{C6H3iPr2N(CH2)3NC6H3iPr2}]' ; _chemical_formula_moiety 'C37 H66 N3 O1 Si2 Y1' _chemical_formula_sum 'C37 H66 N3 O Si2 Y' _chemical_formula_weight 714.02 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1) _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.0609(4) _cell_length_b 17.1207(6) _cell_length_c 11.3288(4) _cell_angle_alpha 90 _cell_angle_beta 106.524(2) _cell_angle_gamma 90 _cell_volume 2056.74(13) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 17233 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 23.534 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.153 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.505 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.5856 _exptl_absorpt_correction_T_max 0.7371 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.042 _diffrn_reflns_av_unetI/netI 0.0538 _diffrn_reflns_number 10087 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.75 _diffrn_reflns_theta_max 23.52 _diffrn_reflns_theta_full 23.52 _diffrn_measured_fraction_theta_full 0.959 _diffrn_measured_fraction_theta_max 0.959 _reflns_number_total 5629 _reflns_number_gt 5132 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0426P)^2^+1.7256P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 5629 _refine_ls_number_parameters 397 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0497 _refine_ls_R_factor_gt 0.0418 _refine_ls_wR_factor_ref 0.1009 _refine_ls_wR_factor_gt 0.0958 _refine_ls_goodness_of_fit_ref 1.03 _refine_ls_restrained_S_all 1.03 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.019(6) _refine_diff_density_max 0.309 _refine_diff_density_min -0.329 _refine_diff_density_rms 0.046 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Y Y 0.70574(4) 0.90229(2) 0.27573(4) 0.03447(13) Uani 1 1 d . . . Si1 Si 0.77333(15) 0.81520(9) 0.55288(14) 0.0519(4) Uani 1 1 d . . . Si2 Si 0.62425(13) 0.95971(9) 0.54628(12) 0.0433(3) Uani 1 1 d . . . O O 0.5880(3) 0.7898(2) 0.2136(4) 0.0532(9) Uani 1 1 d . . . N1 N 0.6144(4) 0.9893(2) 0.1377(4) 0.0436(10) Uani 1 1 d . . . N2 N 0.8725(3) 0.8878(2) 0.2095(3) 0.0378(10) Uani 1 1 d . . . N3 N 0.7017(3) 0.8970(3) 0.4749(3) 0.0414(8) Uani 1 1 d . . . C1 C 0.6477(6) 0.9874(4) 0.0219(5) 0.0617(17) Uani 1 1 d . . . H1A H 0.6948 1.0357 0.0161 0.074 Uiso 1 1 calc R . . H1B H 0.5688 0.9882 -0.0467 0.074 Uiso 1 1 calc R . . C2 C 0.7259(5) 0.9182(4) 0.0035(4) 0.0587(17) Uani 1 1 d . . . H2A H 0.6823 0.87 0.0174 0.07 Uiso 1 1 calc R . . H2B H 0.7263 0.9178 -0.0838 0.07 Uiso 1 1 calc R . . C3 C 0.8604(4) 0.9136(3) 0.0822(4) 0.0450(12) Uani 1 1 d . . . H3A H 0.9071 0.8769 0.0439 0.054 Uiso 1 1 calc R . . H3B H 0.8998 0.9658 0.0848 0.054 Uiso 1 1 calc R . . C4 C 0.5269(5) 1.0514(3) 0.1352(5) 0.0429(12) Uani 1 1 d . . . C5 C 0.3959(5) 1.0386(3) 0.0895(5) 0.0425(12) Uani 1 1 d . . . C6 C 0.3133(5) 1.0996(3) 0.0918(5) 0.0499(13) Uani 1 1 d . . . H6 H 0.225 1.0909 0.0622 0.06 Uiso 1 1 calc R . . C7 C 0.3569(6) 1.1722(4) 0.1361(5) 0.0624(16) Uani 1 1 d . . . H7 H 0.299 1.2128 0.138 0.075 Uiso 1 1 calc R . . C8 C 0.4853(6) 1.1857(3) 0.1779(5) 0.0595(16) Uani 1 1 d . . . H8 H 0.5149 1.2362 0.2075 0.071 Uiso 1 1 calc R . . C9 C 0.5725(6) 1.1268(3) 0.1776(5) 0.0486(14) Uani 1 1 d . . . C10 C 0.3418(5) 0.9600(3) 0.0366(5) 0.0508(13) Uani 1 1 d . . . H10 H 0.4119 0.9209 0.0571 0.061 Uiso 1 1 calc R . . C11 C 0.2386(6) 0.9308(4) 0.0911(6) 0.0709(19) Uani 1 1 d . . . H11A H 0.2072 0.8803 0.0545 0.106 Uiso 1 1 calc R . . H11B H 0.1692 0.9686 0.0733 0.106 Uiso 1 1 calc R . . H11C H 0.2733 0.925 0.1804 0.106 Uiso 1 1 calc R . . C12 C 0.2879(7) 0.9624(4) -0.1033(6) 0.0764(19) Uani 1 1 d . . . H12A H 0.2548 0.9107 -0.1333 0.115 Uiso 1 1 calc R . . H12B H 0.3547 0.9769 -0.1404 0.115 Uiso 1 1 calc R . . H12C H 0.2198 1.001 -0.1259 0.115 Uiso 1 1 calc R . . C13 C 0.7141(6) 1.1435(4) 0.2266(6) 0.0635(16) Uani 1 1 d . . . H13 H 0.7609 1.0954 0.2155 0.076 Uiso 1 1 calc R . . C14 C 0.7514(9) 1.1635(8) 0.3615(8) 0.152(5) Uani 1 1 d . . . H14A H 0.8424 1.1731 0.3901 0.228 Uiso 1 1 calc R . . H14B H 0.73 1.1199 0.4079 0.228 Uiso 1 1 calc R . . H14C H 0.7061 1.2104 0.3744 0.228 Uiso 1 1 calc R . . C15 C 0.7519(8) 1.2100(5) 0.1537(10) 0.117(3) Uani 1 1 d . . . H15A H 0.843 1.219 0.1847 0.176 Uiso 1 1 calc R . . H15B H 0.7068 1.2577 0.1633 0.176 Uiso 1 1 calc R . . H15C H 0.7302 1.1957 0.0663 0.176 Uiso 1 1 calc R . . C16 C 0.9994(4) 0.8661(3) 0.2721(4) 0.0358(10) Uani 1 1 d . . . C17 C 1.0478(4) 0.7935(3) 0.2476(4) 0.0384(11) Uani 1 1 d . . . C18 C 1.1691(5) 0.7722(3) 0.3151(5) 0.0445(12) Uani 1 1 d . . . H18 H 1.2018 0.7232 0.2996 0.053 Uiso 1 1 calc R . . C19 C 1.2443(5) 0.8212(4) 0.4052(5) 0.0523(14) Uani 1 1 d . . . H19 H 1.3268 0.8058 0.4509 0.063 Uiso 1 1 calc R . . C20 C 1.1963(5) 0.8920(4) 0.4263(5) 0.0560(15) Uani 1 1 d . . . H20 H 1.2472 0.9255 0.4873 0.067 Uiso 1 1 calc R . . C21 C 1.0756(5) 0.9166(3) 0.3616(4) 0.0456(13) Uani 1 1 d . . . C22 C 0.9707(4) 0.7359(3) 0.1537(4) 0.0393(11) Uani 1 1 d . . . H22 H 0.8843 0.7582 0.1192 0.047 Uiso 1 1 calc R . . C23 C 0.9576(6) 0.6570(3) 0.2115(6) 0.0569(14) Uani 1 1 d . . . H23A H 0.9065 0.622 0.1484 0.085 Uiso 1 1 calc R . . H23B H 0.9166 0.6642 0.2769 0.085 Uiso 1 1 calc R . . H23C H 1.0414 0.6341 0.2465 0.085 Uiso 1 1 calc R . . C24 C 1.0279(5) 0.7233(3) 0.0468(5) 0.0544(14) Uani 1 1 d . . . H24A H 0.9756 0.6865 -0.0123 0.082 Uiso 1 1 calc R . . H24B H 1.1134 0.7021 0.0785 0.082 Uiso 1 1 calc R . . H24C H 1.0315 0.7733 0.0057 0.082 Uiso 1 1 calc R . . C25 C 1.0304(6) 0.9973(3) 0.3867(6) 0.0596(16) Uani 1 1 d . . . H25 H 0.9374 0.999 0.3463 0.072 Uiso 1 1 calc R . . C26 C 1.0893(9) 1.0597(4) 0.3259(9) 0.103(3) Uani 1 1 d . . . H26A H 1.0733 1.0476 0.2383 0.154 Uiso 1 1 calc R . . H26B H 1.1805 1.0614 0.3653 0.154 Uiso 1 1 calc R . . H26C H 1.0523 1.1106 0.3349 0.154 Uiso 1 1 calc R . . C27 C 1.0497(10) 1.0145(5) 0.5196(8) 0.108(3) Uani 1 1 d . . . H27A H 1.0183 1.067 0.5285 0.162 Uiso 1 1 calc R . . H27B H 1.1398 1.0116 0.5632 0.162 Uiso 1 1 calc R . . H27C H 1.0037 0.9761 0.5544 0.162 Uiso 1 1 calc R . . C28 C 0.8800(7) 0.7709(3) 0.4698(6) 0.0693(18) Uani 1 1 d . . . H28A H 0.8318 0.7593 0.3847 0.104 Uiso 1 1 calc R . . H28B H 0.9161 0.7224 0.5112 0.104 Uiso 1 1 calc R . . H28C H 0.948 0.8076 0.47 0.104 Uiso 1 1 calc R . . C29 C 0.8752(7) 0.8339(5) 0.7121(6) 0.081(2) Uani 1 1 d . . . H29A H 0.9354 0.8756 0.7103 0.122 Uiso 1 1 calc R . . H29B H 0.9212 0.7862 0.7453 0.122 Uiso 1 1 calc R . . H29C H 0.8225 0.8498 0.7643 0.122 Uiso 1 1 calc R . . C30 C 0.6595(7) 0.7352(4) 0.5620(6) 0.0736(18) Uani 1 1 d . . . H30A H 0.6047 0.7238 0.4793 0.11 Uiso 1 1 calc R . . H30B H 0.6079 0.7521 0.6148 0.11 Uiso 1 1 calc R . . H30C H 0.7066 0.6881 0.5968 0.11 Uiso 1 1 calc R . . C31 C 0.7373(6) 1.0297(4) 0.6480(6) 0.0660(17) Uani 1 1 d . . . H31A H 0.8023 1.0004 0.7089 0.099 Uiso 1 1 calc R . . H31B H 0.6917 1.0635 0.6905 0.099 Uiso 1 1 calc R . . H31C H 0.7772 1.0617 0.5979 0.099 Uiso 1 1 calc R . . C32 C 0.5399(5) 0.9121(4) 0.6498(4) 0.0568(14) Uani 1 1 d . . . H32A H 0.6002 0.8817 0.7133 0.085 Uiso 1 1 calc R . . H32B H 0.474 0.8775 0.6011 0.085 Uiso 1 1 calc R . . H32C H 0.5016 0.9524 0.689 0.085 Uiso 1 1 calc R . . C33 C 0.4992(5) 1.0152(3) 0.4308(5) 0.0590(15) Uani 1 1 d . . . H33A H 0.5368 1.0421 0.3735 0.088 Uiso 1 1 calc R . . H33B H 0.461 1.0536 0.4734 0.088 Uiso 1 1 calc R . . H33C H 0.4342 0.9789 0.385 0.088 Uiso 1 1 calc R . . C34 C 0.6121(9) 0.7232(6) 0.1478(10) 0.136(5) Uani 1 1 d . . . H34A H 0.7041 0.7151 0.1643 0.163 Uiso 1 1 calc R . . H34B H 0.5748 0.7306 0.0581 0.163 Uiso 1 1 calc R . . C35 C 0.5557(9) 0.6570(5) 0.1896(12) 0.123(4) Uani 1 1 d . . . H35A H 0.6174 0.6309 0.2592 0.147 Uiso 1 1 calc R . . H35B H 0.5252 0.6187 0.1223 0.147 Uiso 1 1 calc R . . C36 C 0.4490(7) 0.6890(4) 0.2294(8) 0.081(2) Uani 1 1 d . . . H36A H 0.3676 0.6746 0.17 0.097 Uiso 1 1 calc R . . H36B H 0.4507 0.6685 0.3116 0.097 Uiso 1 1 calc R . . C37 C 0.4658(6) 0.7753(3) 0.2338(7) 0.0697(18) Uani 1 1 d . . . H37A H 0.3979 0.8008 0.1689 0.084 Uiso 1 1 calc R . . H37B H 0.464 0.796 0.3149 0.084 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 Y 0.0316(2) 0.0426(2) 0.0334(2) -0.0013(3) 0.01593(16) 0.0014(3) Si1 0.0603(10) 0.0606(9) 0.0416(8) 0.0079(7) 0.0256(7) 0.0103(8) Si2 0.0390(8) 0.0561(9) 0.0373(8) -0.0104(6) 0.0151(6) -0.0010(6) O 0.049(2) 0.055(2) 0.067(2) -0.0153(19) 0.0342(19) -0.0147(17) N1 0.041(2) 0.058(3) 0.034(2) 0.0016(19) 0.0153(19) 0.009(2) N2 0.0330(19) 0.045(3) 0.039(2) -0.0007(18) 0.0162(16) 0.0029(18) N3 0.047(2) 0.046(2) 0.0356(19) -0.007(2) 0.0191(16) -0.003(2) C1 0.058(4) 0.100(5) 0.030(3) 0.014(3) 0.016(3) 0.032(3) C2 0.049(3) 0.095(5) 0.035(3) -0.003(3) 0.015(2) 0.016(3) C3 0.047(3) 0.050(3) 0.045(3) 0.003(3) 0.024(2) 0.011(3) C4 0.047(3) 0.051(3) 0.036(3) 0.006(2) 0.021(2) 0.006(2) C5 0.037(3) 0.054(3) 0.041(3) 0.009(2) 0.018(2) 0.007(2) C6 0.041(3) 0.060(3) 0.052(3) 0.009(3) 0.018(3) 0.007(3) C7 0.073(4) 0.061(4) 0.061(4) 0.000(3) 0.032(3) 0.021(3) C8 0.081(5) 0.055(4) 0.051(4) -0.004(3) 0.031(3) 0.001(3) C9 0.049(3) 0.061(4) 0.041(3) -0.002(3) 0.021(3) 0.002(3) C10 0.042(3) 0.049(3) 0.064(4) 0.015(3) 0.019(3) 0.008(2) C11 0.046(3) 0.081(5) 0.088(5) 0.010(3) 0.023(3) -0.008(3) C12 0.104(5) 0.057(4) 0.069(4) -0.005(3) 0.025(4) -0.008(4) C13 0.057(4) 0.077(4) 0.063(4) -0.013(3) 0.028(3) -0.018(3) C14 0.090(6) 0.297(14) 0.071(6) -0.057(7) 0.026(5) -0.084(8) C15 0.087(6) 0.121(7) 0.156(9) 0.022(6) 0.055(6) -0.029(5) C16 0.028(2) 0.044(3) 0.039(3) 0.000(2) 0.016(2) -0.004(2) C17 0.033(3) 0.048(3) 0.037(3) 0.002(2) 0.015(2) -0.004(2) C18 0.033(3) 0.056(3) 0.046(3) 0.006(2) 0.015(2) 0.005(2) C19 0.033(3) 0.070(4) 0.049(3) 0.001(3) 0.003(2) -0.001(3) C20 0.038(3) 0.081(4) 0.047(3) -0.012(3) 0.009(2) -0.015(3) C21 0.044(3) 0.050(4) 0.046(3) -0.007(2) 0.018(2) -0.007(2) C22 0.034(3) 0.042(3) 0.045(3) -0.001(2) 0.016(2) 0.001(2) C23 0.054(3) 0.051(3) 0.067(4) -0.004(3) 0.019(3) -0.002(3) C24 0.050(3) 0.065(4) 0.052(3) -0.013(3) 0.019(3) -0.003(3) C25 0.051(3) 0.062(4) 0.070(4) -0.028(3) 0.025(3) -0.013(3) C26 0.139(8) 0.054(4) 0.140(8) -0.009(4) 0.081(7) -0.001(5) C27 0.149(8) 0.096(6) 0.094(6) -0.037(5) 0.059(6) 0.004(5) C28 0.094(5) 0.063(4) 0.067(4) 0.024(3) 0.049(4) 0.031(3) C29 0.071(4) 0.118(6) 0.051(4) 0.013(4) 0.012(3) 0.032(4) C30 0.097(5) 0.063(4) 0.072(4) 0.018(3) 0.040(4) 0.003(4) C31 0.066(4) 0.061(4) 0.072(4) -0.026(3) 0.022(3) -0.005(3) C32 0.045(3) 0.087(4) 0.040(3) -0.003(3) 0.014(2) 0.003(3) C33 0.048(3) 0.067(4) 0.066(4) 0.003(3) 0.024(3) 0.005(3) C34 0.103(7) 0.159(9) 0.183(10) -0.129(8) 0.100(7) -0.065(6) C35 0.094(7) 0.063(5) 0.227(12) -0.059(6) 0.072(7) -0.013(5) C36 0.065(4) 0.071(4) 0.114(6) -0.013(4) 0.036(4) -0.018(3) C37 0.046(3) 0.059(4) 0.121(6) 0.004(4) 0.051(4) 0.000(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Y N1 2.188(4) . ? Y N2 2.194(3) . ? Y N3 2.272(3) . ? Y O 2.320(3) . ? Si1 N3 1.723(5) . ? Si1 C28 1.866(6) . ? Si1 C29 1.862(7) . ? Si1 C30 1.883(7) . ? Si2 N3 1.713(4) . ? Si2 C33 1.870(6) . ? Si2 C31 1.873(6) . ? Si2 C32 1.879(5) . ? O C34 1.428(8) . ? O C37 1.455(6) . ? N1 C4 1.433(6) . ? N1 C1 1.460(6) . ? N2 C16 1.430(6) . ? N2 C3 1.477(6) . ? C1 C2 1.516(8) . ? C2 C3 1.503(7) . ? C4 C5 1.411(7) . ? C4 C9 1.418(8) . ? C5 C6 1.392(7) . ? C5 C10 1.525(8) . ? C6 C7 1.375(8) . ? C7 C8 1.383(8) . ? C8 C9 1.396(8) . ? C9 C13 1.533(8) . ? C10 C11 1.527(8) . ? C10 C12 1.527(8) . ? C13 C14 1.505(10) . ? C13 C15 1.533(10) . ? C16 C17 1.412(7) . ? C16 C21 1.413(7) . ? C17 C18 1.391(7) . ? C17 C22 1.522(7) . ? C18 C19 1.398(8) . ? C19 C20 1.371(8) . ? C20 C21 1.393(7) . ? C21 C25 1.524(7) . ? C22 C23 1.527(7) . ? C22 C24 1.533(7) . ? C25 C27 1.488(9) . ? C25 C26 1.515(9) . ? C34 C35 1.437(13) . ? C35 C36 1.482(10) . ? C36 C37 1.489(8) . ? 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 Y N2 95.43(14) . . ? N1 Y N3 127.00(16) . . ? N2 Y N3 126.24(13) . . ? N1 Y O 104.09(15) . . ? N2 Y O 104.87(13) . . ? N3 Y O 95.74(15) . . ? N3 Si1 C28 109.7(2) . . ? N3 Si1 C29 114.8(3) . . ? C28 Si1 C29 105.3(3) . . ? N3 Si1 C30 113.7(3) . . ? C28 Si1 C30 105.1(3) . . ? C29 Si1 C30 107.6(3) . . ? N3 Si2 C33 111.0(2) . . ? N3 Si2 C31 110.8(2) . . ? C33 Si2 C31 109.7(3) . . ? N3 Si2 C32 115.2(3) . . ? C33 Si2 C32 104.9(3) . . ? C31 Si2 C32 104.8(3) . . ? C34 O C37 105.5(5) . . ? C34 O Y 130.5(4) . . ? C37 O Y 124.0(3) . . ? C4 N1 C1 110.0(4) . . ? C4 N1 Y 133.7(3) . . ? C1 N1 Y 116.3(3) . . ? C16 N2 C3 111.4(3) . . ? C16 N2 Y 131.4(3) . . ? C3 N2 Y 116.6(3) . . ? Si2 N3 Si1 119.1(2) . . ? Si2 N3 Y 126.7(2) . . ? Si1 N3 Y 113.9(2) . . ? N1 C1 C2 116.2(4) . . ? C3 C2 C1 117.7(5) . . ? N2 C3 C2 113.2(4) . . ? C5 C4 C9 119.6(5) . . ? C5 C4 N1 120.6(5) . . ? C9 C4 N1 119.8(5) . . ? C6 C5 C4 119.2(5) . . ? C6 C5 C10 118.9(5) . . ? C4 C5 C10 121.9(4) . . ? C7 C6 C5 121.4(5) . . ? C6 C7 C8 119.7(5) . . ? C7 C8 C9 121.3(6) . . ? C8 C9 C4 118.7(6) . . ? C8 C9 C13 120.0(5) . . ? C4 C9 C13 121.3(5) . . ? C5 C10 C11 112.6(5) . . ? C5 C10 C12 112.2(4) . . ? C11 C10 C12 108.2(5) . . ? C14 C13 C9 111.5(5) . . ? C14 C13 C15 109.9(7) . . ? C9 C13 C15 110.5(6) . . ? C17 C16 C21 119.8(4) . . ? C17 C16 N2 120.3(4) . . ? C21 C16 N2 119.8(4) . . ? C18 C17 C16 118.9(4) . . ? C18 C17 C22 118.4(4) . . ? C16 C17 C22 122.7(4) . . ? C17 C18 C19 121.7(5) . . ? C20 C19 C18 118.6(5) . . ? C19 C20 C21 122.4(5) . . ? C20 C21 C16 118.6(5) . . ? C20 C21 C25 119.5(5) . . ? C16 C21 C25 121.9(5) . . ? C17 C22 C23 112.1(4) . . ? C17 C22 C24 111.6(4) . . ? C23 C22 C24 109.0(4) . . ? C27 C25 C26 111.3(6) . . ? C27 C25 C21 114.1(6) . . ? C26 C25 C21 110.4(5) . . ? O C34 C35 107.1(6) . . ? C34 C35 C36 105.5(7) . . ? C37 C36 C35 105.9(6) . . ? O C37 C36 106.0(5) . . ? data_nov1502 _database_code_depnum_ccdc_archive 'CCDC 228146' _audit_creation_date 2002-11-12T14:39:33-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common (Y(C6H3iPr2N(CH2)3NC6H3iPr2)2K(C7H8)) _chemical_formula_moiety 'C61 H88 K N4 Y' _chemical_formula_sum 'C61 H88 K N4 Y' _chemical_formula_weight 1005.36 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_Int_Tables_number 14 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 12.2379(2) _cell_length_b 13.0294(2) _cell_length_c 36.6872(6) _cell_angle_alpha 90 _cell_angle_beta 98.851(1) _cell_angle_gamma 90 _cell_volume 5780.20(16) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 72736 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 22.465 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.155 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2160 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.12 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.8328 _exptl_absorpt_correction_T_max 0.9065 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0746 _diffrn_reflns_av_unetI/netI 0.0813 _diffrn_reflns_number 24408 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 3.72 _diffrn_reflns_theta_max 22.61 _diffrn_reflns_theta_full 22.61 _diffrn_measured_fraction_theta_full 0.976 _diffrn_measured_fraction_theta_max 0.976 _reflns_number_total 7471 _reflns_number_gt 5283 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The C6 ring of the toluene was included as a rigid body. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0446P)^2^+11.2075P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 7471 _refine_ls_number_parameters 592 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1098 _refine_ls_R_factor_gt 0.0677 _refine_ls_wR_factor_ref 0.1477 _refine_ls_wR_factor_gt 0.1314 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.579 _refine_diff_density_min -0.435 _refine_diff_density_rms 0.063 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 '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' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Y Y 0.25911(4) 0.34991(4) 0.872992(13) 0.03712(18) Uani 1 1 d . . . K K 0.72051(16) 0.09294(15) 0.89937(5) 0.1032(6) Uani 1 1 d . . . N1 N 0.2971(4) 0.4879(3) 0.90780(11) 0.0429(11) Uani 1 1 d . . . N2 N 0.4291(4) 0.2817(4) 0.89095(11) 0.0423(11) Uani 1 1 d . . . N3 N 0.2175(4) 0.3743(3) 0.81183(11) 0.0474(12) Uani 1 1 d . . . N4 N 0.1130(4) 0.2493(3) 0.87786(11) 0.0438(12) Uani 1 1 d . . . C1 C 0.4156(5) 0.5018(5) 0.92247(15) 0.0514(16) Uani 1 1 d . . . H1A H 0.4334 0.4634 0.9456 0.062 Uiso 1 1 calc R . . H1B H 0.4298 0.5746 0.928 0.062 Uiso 1 1 calc R . . C2 C 0.4907(5) 0.4657(5) 0.89536(15) 0.0551(16) Uani 1 1 d . . . H2A H 0.4543 0.4827 0.8704 0.066 Uiso 1 1 calc R . . H2B H 0.5591 0.506 0.9 0.066 Uiso 1 1 calc R . . C3 C 0.5228(4) 0.3528(5) 0.89564(15) 0.0506(15) Uani 1 1 d . . . H3A H 0.5666 0.3407 0.8758 0.061 Uiso 1 1 calc R . . H3B H 0.57 0.3374 0.9191 0.061 Uiso 1 1 calc R . . C4 C 0.2280(4) 0.5573(4) 0.92351(15) 0.0444(14) Uani 1 1 d . . . C5 C 0.1890(5) 0.6462(5) 0.90395(16) 0.0599(17) Uani 1 1 d . . . C6 C 0.1194(6) 0.7129(5) 0.91941(19) 0.072(2) Uani 1 1 d . . . H6 H 0.0919 0.7717 0.9062 0.086 Uiso 1 1 calc R . . C7 C 0.0903(6) 0.6943(5) 0.95343(19) 0.0680(19) Uani 1 1 d . . . H7 H 0.0439 0.7403 0.9635 0.082 Uiso 1 1 calc R . . C8 C 0.1290(5) 0.6086(5) 0.97258(17) 0.0592(17) Uani 1 1 d . . . H8 H 0.1092 0.5965 0.996 0.071 Uiso 1 1 calc R . . C9 C 0.1972(5) 0.5389(4) 0.95826(14) 0.0454(15) Uani 1 1 d . . . C10 C 0.2205(9) 0.6732(5) 0.8661(2) 0.096(3) Uani 1 1 d . . . H10 H 0.2251 0.608 0.8526 0.115 Uiso 1 1 calc R . . C11 C 0.1381(9) 0.7422(6) 0.8419(2) 0.129(4) Uani 1 1 d . . . H11A H 0.0656 0.7104 0.8385 0.194 Uiso 1 1 calc R . . H11B H 0.1621 0.7518 0.8182 0.194 Uiso 1 1 calc R . . H11C H 0.1344 0.8083 0.8539 0.194 Uiso 1 1 calc R . . C12 C 0.3344(8) 0.7231(7) 0.8704(3) 0.130(4) Uani 1 1 d . . . H12A H 0.3531 0.7385 0.8463 0.194 Uiso 1 1 calc R . . H12B H 0.3889 0.6765 0.8833 0.194 Uiso 1 1 calc R . . H12C H 0.3336 0.7862 0.8845 0.194 Uiso 1 1 calc R . . C13 C 0.2388(5) 0.4450(4) 0.98084(14) 0.0483(15) Uani 1 1 d . . . H13 H 0.278 0.4005 0.9652 0.058 Uiso 1 1 calc R . . C14 C 0.1454(5) 0.3829(5) 0.99266(17) 0.0664(19) Uani 1 1 d . . . H14A H 0.1757 0.3235 1.0066 0.1 Uiso 1 1 calc R . . H14B H 0.0955 0.3606 0.971 0.1 Uiso 1 1 calc R . . H14C H 0.1054 0.4251 1.0079 0.1 Uiso 1 1 calc R . . C15 C 0.3216(5) 0.4760(5) 1.01485(15) 0.0621(18) Uani 1 1 d . . . H15A H 0.3477 0.415 1.0287 0.093 Uiso 1 1 calc R . . H15B H 0.2857 0.5212 1.0303 0.093 Uiso 1 1 calc R . . H15C H 0.3838 0.5112 1.007 0.093 Uiso 1 1 calc R . . C16 C 0.4621(5) 0.1804(5) 0.90105(15) 0.0466(15) Uani 1 1 d . . . C17 C 0.4617(5) 0.1014(5) 0.87405(15) 0.0545(16) Uani 1 1 d . . . C18 C 0.4858(6) 0.0018(6) 0.88492(19) 0.075(2) Uani 1 1 d . . . H18 H 0.4821 -0.0499 0.8669 0.09 Uiso 1 1 calc R . . C19 C 0.5153(7) -0.0241(5) 0.9216(2) 0.088(2) Uani 1 1 d . . . H19 H 0.5309 -0.0926 0.9285 0.105 Uiso 1 1 calc R . . C20 C 0.5213(6) 0.0521(5) 0.94772(18) 0.074(2) Uani 1 1 d . . . H20 H 0.5437 0.0347 0.9726 0.089 Uiso 1 1 calc R . . C21 C 0.4956(5) 0.1530(5) 0.93889(15) 0.0520(15) Uani 1 1 d . . . C22 C 0.4425(5) 0.1286(5) 0.83298(15) 0.0676(19) Uani 1 1 d . . . H22 H 0.3962 0.1912 0.8296 0.081 Uiso 1 1 calc R . . C23 C 0.3828(6) 0.0432(6) 0.80894(19) 0.098(3) Uani 1 1 d . . . H23A H 0.3715 0.0646 0.7833 0.147 Uiso 1 1 calc R . . H23B H 0.3118 0.0298 0.8166 0.147 Uiso 1 1 calc R . . H23C H 0.4273 -0.0187 0.8117 0.147 Uiso 1 1 calc R . . C24 C 0.5536(6) 0.1526(7) 0.82076(18) 0.096(3) Uani 1 1 d . . . H24A H 0.5418 0.1708 0.7948 0.143 Uiso 1 1 calc R . . H24B H 0.6011 0.0927 0.8246 0.143 Uiso 1 1 calc R . . H24C H 0.5885 0.2095 0.8352 0.143 Uiso 1 1 calc R . . C25 C 0.4994(5) 0.2310(5) 0.97005(14) 0.0525(16) Uani 1 1 d . . . H25 H 0.4799 0.2989 0.9588 0.063 Uiso 1 1 calc R . . C26 C 0.4161(6) 0.2059(5) 0.99552(18) 0.083(2) Uani 1 1 d . . . H26A H 0.42 0.2577 1.0147 0.124 Uiso 1 1 calc R . . H26B H 0.433 0.1392 1.0067 0.124 Uiso 1 1 calc R . . H26C H 0.3422 0.2048 0.9814 0.124 Uiso 1 1 calc R . . C27 C 0.6150(6) 0.2388(5) 0.99240(17) 0.076(2) Uani 1 1 d . . . H27A H 0.615 0.2898 1.0117 0.114 Uiso 1 1 calc R . . H27B H 0.6671 0.2589 0.9763 0.114 Uiso 1 1 calc R . . H27C H 0.6364 0.1728 1.0035 0.114 Uiso 1 1 calc R . . C28 C 0.1779(5) 0.2812(5) 0.79181(15) 0.0571(17) Uani 1 1 d . . . H28A H 0.2338 0.2588 0.777 0.068 Uiso 1 1 calc R . . H28B H 0.1105 0.2977 0.7747 0.068 Uiso 1 1 calc R . . C29 C 0.1534(5) 0.1929(4) 0.81637(15) 0.0490(15) Uani 1 1 d . . . H29A H 0.2222 0.1745 0.8324 0.059 Uiso 1 1 calc R . . H29B H 0.1311 0.1334 0.8006 0.059 Uiso 1 1 calc R . . C30 C 0.0643(5) 0.2112(5) 0.84079(14) 0.0508(15) Uani 1 1 d . . . H30A H 0.0108 0.2615 0.8289 0.061 Uiso 1 1 calc R . . H30B H 0.0247 0.1469 0.8434 0.061 Uiso 1 1 calc R . . C31 C 0.2181(5) 0.4615(5) 0.78860(14) 0.0534(16) Uani 1 1 d . . . C32 C 0.1185(6) 0.5102(5) 0.77297(15) 0.0570(17) Uani 1 1 d . . . C33 C 0.1231(7) 0.5972(6) 0.75148(17) 0.075(2) Uani 1 1 d . . . H33 H 0.0569 0.6289 0.7408 0.09 Uiso 1 1 calc R . . C34 C 0.2228(8) 0.6386(6) 0.74532(19) 0.090(2) Uani 1 1 d . . . H34 H 0.2246 0.698 0.7309 0.108 Uiso 1 1 calc R . . C35 C 0.3176(7) 0.5917(7) 0.76056(19) 0.088(2) Uani 1 1 d . . . H35 H 0.3854 0.6211 0.757 0.106 Uiso 1 1 calc R . . C36 C 0.3192(6) 0.5023(6) 0.78114(15) 0.0680(19) Uani 1 1 d . . . C37 C 0.0063(6) 0.4711(5) 0.77911(19) 0.0705(19) Uani 1 1 d . . . H37 H 0.0182 0.4153 0.7976 0.085 Uiso 1 1 calc R . . C38 C -0.0637(6) 0.5536(6) 0.7938(2) 0.104(3) Uani 1 1 d . . . H38A H -0.1339 0.5243 0.7976 0.156 Uiso 1 1 calc R . . H38B H -0.0768 0.6091 0.776 0.156 Uiso 1 1 calc R . . H38C H -0.0251 0.5798 0.8169 0.156 Uiso 1 1 calc R . . C39 C -0.0586(7) 0.4253(6) 0.7428(2) 0.103(3) Uani 1 1 d . . . H39A H -0.1296 0.3997 0.7475 0.154 Uiso 1 1 calc R . . H39B H -0.0164 0.3694 0.7344 0.154 Uiso 1 1 calc R . . H39C H -0.0701 0.4782 0.724 0.154 Uiso 1 1 calc R . . C40 C 0.4286(6) 0.4479(7) 0.79265(19) 0.090(3) Uani 1 1 d . . . H40 H 0.4216 0.4054 0.8145 0.108 Uiso 1 1 calc R . . C41 C 0.4513(7) 0.3754(8) 0.7618(2) 0.124(3) Uani 1 1 d . . . H41A H 0.5208 0.34 0.7693 0.186 Uiso 1 1 calc R . . H41B H 0.4554 0.4148 0.7396 0.186 Uiso 1 1 calc R . . H41C H 0.3919 0.3256 0.7569 0.186 Uiso 1 1 calc R . . C42 C 0.5260(7) 0.5214(8) 0.8033(2) 0.136(4) Uani 1 1 d . . . H42A H 0.5932 0.4822 0.8105 0.205 Uiso 1 1 calc R . . H42B H 0.512 0.564 0.8238 0.205 Uiso 1 1 calc R . . H42C H 0.5344 0.5646 0.7824 0.205 Uiso 1 1 calc R . . C43 C 0.0427(5) 0.2300(4) 0.90426(14) 0.0422(14) Uani 1 1 d . . . C44 C 0.0677(5) 0.1504(5) 0.93027(16) 0.0551(16) Uani 1 1 d . . . C45 C -0.0024(6) 0.1315(5) 0.95586(16) 0.0626(18) Uani 1 1 d . . . H45 H 0.0145 0.0782 0.9731 0.075 Uiso 1 1 calc R . . C46 C -0.0965(6) 0.1895(6) 0.95654(18) 0.069(2) Uani 1 1 d . . . H46 H -0.1433 0.1755 0.974 0.083 Uiso 1 1 calc R . . C47 C -0.1213(5) 0.2676(5) 0.93170(17) 0.0638(18) Uani 1 1 d . . . H47 H -0.1852 0.3071 0.9323 0.077 Uiso 1 1 calc R . . C48 C -0.0533(5) 0.2897(5) 0.90535(14) 0.0469(15) Uani 1 1 d . . . C49 C 0.1723(6) 0.0865(5) 0.93104(18) 0.071(2) Uani 1 1 d . . . H49 H 0.2332 0.1353 0.9291 0.085 Uiso 1 1 calc R . . C50 C 0.2059(7) 0.0258(6) 0.9672(2) 0.105(3) Uani 1 1 d . . . H50A H 0.2732 -0.0123 0.9658 0.157 Uiso 1 1 calc R . . H50B H 0.1472 -0.0216 0.9706 0.157 Uiso 1 1 calc R . . H50C H 0.2184 0.0731 0.9878 0.157 Uiso 1 1 calc R . . C51 C 0.1688(7) 0.0121(6) 0.8991(2) 0.103(3) Uani 1 1 d . . . H51A H 0.2383 -0.0248 0.9012 0.154 Uiso 1 1 calc R . . H51B H 0.1569 0.0498 0.876 0.154 Uiso 1 1 calc R . . H51C H 0.1088 -0.0363 0.8995 0.154 Uiso 1 1 calc R . . C52 C -0.0841(5) 0.3774(5) 0.87890(16) 0.0555(17) Uani 1 1 d . . . H52 H -0.0231 0.3866 0.8643 0.067 Uiso 1 1 calc R . . C53 C -0.0976(6) 0.4786(5) 0.89903(19) 0.084(2) Uani 1 1 d . . . H53A H -0.1165 0.5329 0.8811 0.127 Uiso 1 1 calc R . . H53B H -0.0288 0.4954 0.9148 0.127 Uiso 1 1 calc R . . H53C H -0.1561 0.4715 0.9139 0.127 Uiso 1 1 calc R . . C54 C -0.1893(5) 0.3514(6) 0.85182(18) 0.082(2) Uani 1 1 d . . . H54A H -0.2073 0.408 0.8348 0.123 Uiso 1 1 calc R . . H54B H -0.2501 0.34 0.8655 0.123 Uiso 1 1 calc R . . H54C H -0.1768 0.2899 0.8382 0.123 Uiso 1 1 calc R . . C55 C 0.8763(10) -0.0804(13) 0.8894(5) 0.306(17) Uani 1 1 d G . . H55 H 0.9319 -0.0498 0.9064 0.368 Uiso 1 1 calc R . . C56 C 0.8619(11) -0.0507(8) 0.8525(5) 0.276(14) Uani 1 1 d G . . H56 H 0.9078 0 0.8447 0.331 Uiso 1 1 calc R . . C57 C 0.7797(13) -0.0960(12) 0.8273(3) 0.196(6) Uani 1 1 d G . . H57 H 0.7699 -0.0759 0.8024 0.236 Uiso 1 1 calc R . . C58 C 0.7118(9) -0.1709(12) 0.8389(5) 0.224(8) Uani 1 1 d G . . H58 H 0.6562 -0.2015 0.8218 0.269 Uiso 1 1 calc R . . C59 C 0.7262(13) -0.2006(8) 0.8757(6) 0.212(9) Uani 1 1 d G . . C60 C 0.8084(16) -0.1554(14) 0.9009(3) 0.37(2) Uani 1 1 d G . . H60 H 0.8181 -0.1755 0.9258 0.448 Uiso 1 1 calc R . . C61 C 0.680(3) -0.267(2) 0.8937(9) 0.50(3) Uani 1 1 d . . . H61A H 0.6215 -0.3007 0.8773 0.757 Uiso 0.5 1 calc PR . . H61B H 0.6498 -0.2331 0.9134 0.757 Uiso 0.5 1 calc PR . . H61C H 0.7347 -0.3172 0.9041 0.757 Uiso 0.5 1 calc PR . . H61D H 0.7158 -0.2666 0.9192 0.757 Uiso 0.5 1 calc PR . . H61E H 0.6876 -0.3343 0.8831 0.757 Uiso 0.5 1 calc PR . . H61F H 0.6026 -0.2502 0.8925 0.757 Uiso 0.5 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y 0.0387(3) 0.0444(3) 0.0277(3) -0.0016(3) 0.0033(2) -0.0010(3) K 0.0879(14) 0.0948(14) 0.1163(15) -0.0148(11) -0.0183(11) 0.0117(11) N1 0.041(3) 0.041(3) 0.046(3) -0.009(2) 0.006(2) -0.003(2) N2 0.034(3) 0.056(3) 0.037(3) -0.004(2) 0.006(2) 0.002(3) N3 0.054(3) 0.054(3) 0.032(2) 0.002(2) 0.000(2) -0.004(2) N4 0.046(3) 0.050(3) 0.035(3) -0.011(2) 0.003(2) -0.006(2) C1 0.051(4) 0.057(4) 0.046(3) -0.003(3) 0.006(3) -0.014(3) C2 0.047(4) 0.070(5) 0.049(4) 0.010(3) 0.010(3) -0.005(3) C3 0.035(3) 0.071(4) 0.047(3) 0.011(3) 0.011(3) 0.007(4) C4 0.044(4) 0.039(4) 0.048(3) -0.012(3) -0.001(3) -0.003(3) C5 0.084(5) 0.039(4) 0.056(4) -0.013(4) 0.007(3) -0.001(4) C6 0.111(6) 0.037(4) 0.062(5) -0.001(4) -0.001(4) 0.009(4) C7 0.074(5) 0.063(5) 0.065(5) -0.011(4) 0.004(4) 0.016(4) C8 0.060(4) 0.068(5) 0.050(4) -0.013(4) 0.012(3) 0.005(4) C9 0.044(4) 0.050(4) 0.041(3) -0.008(3) 0.004(3) -0.006(3) C10 0.184(10) 0.046(5) 0.066(5) 0.004(4) 0.041(6) 0.013(5) C11 0.225(12) 0.097(7) 0.056(5) 0.014(5) -0.012(6) 0.006(7) C12 0.144(9) 0.117(8) 0.142(8) 0.056(7) 0.067(7) 0.013(7) C13 0.052(4) 0.052(4) 0.042(3) -0.007(3) 0.010(3) 0.005(3) C14 0.074(5) 0.068(5) 0.060(4) -0.002(3) 0.017(3) -0.014(4) C15 0.066(5) 0.066(4) 0.051(4) -0.002(3) -0.002(3) 0.003(4) C16 0.042(4) 0.053(4) 0.046(4) -0.004(3) 0.009(3) 0.005(3) C17 0.050(4) 0.064(4) 0.050(4) -0.015(4) 0.009(3) 0.006(3) C18 0.095(6) 0.063(5) 0.068(5) -0.021(4) 0.018(4) 0.010(4) C19 0.136(7) 0.054(5) 0.072(5) -0.004(4) 0.012(5) 0.016(5) C20 0.113(6) 0.057(5) 0.054(4) -0.002(4) 0.013(4) 0.022(4) C21 0.063(4) 0.049(4) 0.044(3) 0.002(3) 0.009(3) 0.009(3) C22 0.068(5) 0.090(5) 0.044(4) -0.017(4) 0.004(3) 0.019(4) C23 0.098(6) 0.115(7) 0.076(5) -0.047(5) -0.007(4) 0.035(5) C24 0.090(6) 0.145(7) 0.056(4) 0.002(5) 0.026(4) 0.024(6) C25 0.074(5) 0.047(4) 0.037(3) -0.002(3) 0.009(3) 0.009(3) C26 0.121(7) 0.070(5) 0.065(4) -0.008(4) 0.037(4) 0.012(5) C27 0.092(6) 0.071(5) 0.057(4) -0.005(4) -0.016(4) 0.014(4) C28 0.058(4) 0.074(5) 0.038(3) -0.009(3) 0.004(3) 0.006(4) C29 0.051(4) 0.053(4) 0.042(3) -0.013(3) 0.006(3) -0.003(3) C30 0.053(4) 0.053(4) 0.046(3) -0.016(3) 0.006(3) -0.011(3) C31 0.065(5) 0.066(4) 0.027(3) 0.004(3) 0.003(3) -0.013(4) C32 0.071(5) 0.059(4) 0.039(3) 0.002(3) 0.001(3) -0.002(4) C33 0.084(6) 0.080(5) 0.056(4) 0.016(4) -0.001(4) 0.002(4) C34 0.122(8) 0.096(6) 0.053(4) 0.027(4) 0.020(5) -0.008(6) C35 0.090(6) 0.118(7) 0.057(5) 0.026(5) 0.012(4) -0.027(5) C36 0.072(5) 0.098(6) 0.032(3) 0.021(4) 0.004(3) -0.013(4) C37 0.069(5) 0.060(5) 0.080(5) 0.017(4) 0.002(4) 0.004(4) C38 0.087(6) 0.090(6) 0.141(8) 0.024(6) 0.037(5) 0.010(5) C39 0.091(6) 0.089(6) 0.110(6) 0.015(5) -0.044(5) -0.011(5) C40 0.060(5) 0.151(8) 0.060(5) 0.046(5) 0.011(4) -0.007(5) C41 0.096(7) 0.174(10) 0.111(7) 0.050(7) 0.048(5) 0.034(6) C42 0.074(6) 0.248(12) 0.086(6) 0.071(7) 0.008(5) -0.044(7) C43 0.047(4) 0.043(4) 0.036(3) -0.008(3) 0.003(3) -0.008(3) C44 0.061(4) 0.053(4) 0.053(4) -0.005(4) 0.012(3) -0.009(4) C45 0.079(5) 0.057(4) 0.051(4) 0.002(3) 0.006(4) -0.017(4) C46 0.071(5) 0.088(6) 0.054(4) -0.001(4) 0.022(4) -0.021(4) C47 0.060(5) 0.079(5) 0.056(4) -0.008(4) 0.019(3) -0.006(4) C48 0.042(4) 0.056(4) 0.042(3) -0.008(3) 0.007(3) -0.015(3) C49 0.087(6) 0.055(4) 0.070(5) 0.012(4) 0.011(4) -0.008(4) C50 0.100(7) 0.089(6) 0.124(7) 0.056(5) 0.015(5) 0.012(5) C51 0.122(7) 0.066(5) 0.125(7) -0.002(5) 0.033(6) 0.021(5) C52 0.045(4) 0.067(5) 0.056(4) 0.000(3) 0.013(3) 0.002(3) C53 0.088(6) 0.080(5) 0.088(5) 0.000(4) 0.020(4) 0.016(4) C54 0.053(4) 0.113(6) 0.076(5) 0.014(5) 0.000(4) -0.006(4) C55 0.27(3) 0.33(3) 0.30(3) -0.17(2) -0.04(2) 0.14(3) C56 0.164(19) 0.178(15) 0.49(4) -0.15(2) 0.07(2) -0.039(13) C57 0.198(17) 0.164(14) 0.230(17) 0.014(14) 0.040(15) 0.010(11) C58 0.227(18) 0.181(17) 0.29(3) 0.020(15) 0.136(17) -0.010(14) C59 0.23(2) 0.130(12) 0.32(2) 0.084(16) 0.16(2) 0.061(13) C60 0.126(16) 0.166(19) 0.85(7) 0.02(3) 0.14(3) 0.035(14) C61 0.60(5) 0.29(3) 0.76(6) 0.25(3) 0.55(5) 0.17(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Y N1 2.213(4) . ? Y N3 2.246(4) . ? Y N4 2.246(4) . ? Y N2 2.265(4) . ? K C55 3.014(11) . ? K C18 3.078(8) . ? K C46 3.090(7) 1_655 ? K C47 3.102(7) 1_655 ? K C19 3.150(8) . ? K C17 3.163(6) . ? K C56 3.219(11) . ? K C20 3.272(7) . ? K C24 3.358(7) . ? K C16 3.371(6) . ? K C21 3.394(6) . ? N1 C4 1.419(6) . ? N1 C1 1.478(7) . ? N2 C16 1.414(7) . ? N2 C3 1.463(7) . ? N3 C31 1.422(7) . ? N3 C28 1.461(7) . ? N4 C43 1.413(6) . ? N4 C30 1.484(6) . ? C1 C2 1.529(7) . ? C2 C3 1.522(8) . ? C4 C9 1.405(7) . ? C4 C5 1.407(8) . ? C5 C6 1.397(9) . ? C5 C10 1.539(9) . ? C6 C7 1.371(9) . ? C7 C8 1.364(8) . ? C8 C9 1.390(8) . ? C9 C13 1.521(8) . ? C10 C12 1.524(11) . ? C10 C11 1.529(11) . ? C13 C14 1.517(8) . ? C13 C15 1.535(7) . ? C16 C17 1.427(8) . ? C16 C21 1.431(7) . ? C17 C18 1.377(9) . ? C17 C22 1.530(8) . ? C18 C19 1.379(9) . ? C19 C20 1.374(9) . ? C20 C21 1.379(8) . ? C21 C25 1.524(8) . ? C22 C24 1.528(9) . ? C22 C23 1.533(9) . ? C25 C26 1.520(8) . ? C25 C27 1.526(8) . ? C28 C29 1.520(8) . ? C29 C30 1.532(7) . ? C31 C36 1.412(8) . ? C31 C32 1.415(8) . ? C32 C33 1.387(9) . ? C32 C37 1.514(9) . ? C33 C34 1.383(10) . ? C34 C35 1.354(10) . ? C35 C36 1.387(9) . ? C36 C40 1.516(9) . ? C37 C38 1.523(9) . ? C37 C39 1.560(9) . ? C40 C42 1.532(11) . ? C40 C41 1.533(11) . ? C43 C44 1.410(8) . ? C43 C48 1.415(8) . ? C44 C45 1.388(8) . ? C44 C49 1.525(9) . ? C45 C46 1.381(9) . ? C46 C47 1.368(9) . ? C46 K 3.090(7) 1_455 ? C47 C48 1.399(8) . ? C47 K 3.102(6) 1_455 ? C48 C52 1.510(8) . ? C49 C51 1.518(9) . ? C49 C50 1.544(9) . ? C52 C53 1.532(8) . ? C52 C54 1.538(8) . ? C55 C56 1.39 . ? C55 C60 1.39 . ? C56 C57 1.39 . ? C57 C58 1.39 . ? C58 C59 1.39 . ? C59 C61 1.27(2) . ? C59 C60 1.39 . ? 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 Y N3 117.20(16) . . ? N1 Y N4 121.81(15) . . ? N3 Y N4 95.80(16) . . ? N1 Y N2 92.80(16) . . ? N3 Y N2 113.77(15) . . ? N4 Y N2 117.06(17) . . ? C55 K C18 106.3(4) . . ? C55 K C46 89.0(3) . 1_655 ? C18 K C46 146.46(19) . 1_655 ? C55 K C47 103.1(3) . 1_655 ? C18 K C47 149.28(19) . 1_655 ? C46 K C47 25.52(16) 1_655 1_655 ? C55 K C19 102.3(4) . . ? C18 K C19 25.55(17) . . ? C46 K C19 123.01(19) 1_655 . ? C47 K C19 137.01(18) 1_655 . ? C55 K C17 127.9(3) . . ? C18 K C17 25.44(16) . . ? C46 K C17 140.65(19) 1_655 . ? C47 K C17 128.64(19) 1_655 . ? C19 K C17 44.81(18) . . ? C55 K C56 25.50(8) . . ? C18 K C56 104.3(3) . . ? C46 K C56 101.9(4) 1_655 . ? C47 K C56 106.0(3) 1_655 . ? C19 K C56 111.8(3) . . ? C17 K C56 117.4(3) . . ? C55 K C20 118.8(5) . . ? C18 K C20 43.70(17) . . ? C46 K C20 102.75(18) 1_655 . ? C47 K C20 112.66(17) 1_655 . ? C19 K C20 24.62(16) . . ? C17 K C20 50.85(16) . . ? C56 K C20 134.5(2) . . ? C55 K C24 112.4(3) . . ? C18 K C24 60.9(2) . . ? C46 K C24 140.3(2) 1_655 . ? C47 K C24 114.8(2) 1_655 . ? C19 K C24 86.0(2) . . ? C17 K C24 44.81(16) . . ? C56 K C24 89.0(4) . . ? C20 K C24 95.61(18) . . ? C55 K C16 150.2(3) . . ? C18 K C16 43.97(16) . . ? C46 K C16 115.70(18) 1_655 . ? C47 K C16 106.08(17) 1_655 . ? C19 K C16 51.04(17) . . ? C17 K C16 24.98(14) . . ? C56 K C16 142.1(4) . . ? C20 K C16 42.75(15) . . ? C24 K C16 59.29(15) . . ? C55 K C21 142.6(4) . . ? C18 K C21 50.65(16) . . ? C46 K C21 99.58(17) 1_655 . ? C47 K C21 99.60(16) 1_655 . ? C19 K C21 43.11(17) . . ? C17 K C21 43.62(14) . . ? C56 K C21 154.1(3) . . ? C20 K C21 23.79(14) . . ? C24 K C21 83.54(15) . . ? C16 K C21 24.42(13) . . ? C4 N1 C1 112.7(4) . . ? C4 N1 Y 131.8(3) . . ? C1 N1 Y 114.6(3) . . ? C16 N2 C3 111.9(4) . . ? C16 N2 Y 130.9(4) . . ? C3 N2 Y 117.0(3) . . ? C31 N3 C28 113.2(4) . . ? C31 N3 Y 133.7(3) . . ? C28 N3 Y 113.1(3) . . ? C43 N4 C30 111.6(4) . . ? C43 N4 Y 137.2(3) . . ? C30 N4 Y 109.5(3) . . ? N1 C1 C2 112.3(4) . . ? C3 C2 C1 118.3(5) . . ? N2 C3 C2 114.5(5) . . ? C9 C4 C5 119.0(5) . . ? C9 C4 N1 121.4(5) . . ? C5 C4 N1 119.6(5) . . ? C6 C5 C4 119.0(6) . . ? C6 C5 C10 118.6(6) . . ? C4 C5 C10 122.4(6) . . ? C7 C6 C5 121.3(6) . . ? C8 C7 C6 119.7(6) . . ? C7 C8 C9 121.4(6) . . ? C8 C9 C4 119.5(5) . . ? C8 C9 C13 119.3(5) . . ? C4 C9 C13 121.1(5) . . ? C12 C10 C11 108.7(7) . . ? C12 C10 C5 110.8(7) . . ? C11 C10 C5 115.0(7) . . ? C14 C13 C9 112.4(5) . . ? C14 C13 C15 109.9(5) . . ? C9 C13 C15 110.8(5) . . ? N2 C16 C17 121.4(5) . . ? N2 C16 C21 121.0(5) . . ? C17 C16 C21 117.6(5) . . ? N2 C16 K 122.8(3) . . ? C17 C16 K 69.3(3) . . ? C21 C16 K 78.7(3) . . ? C18 C17 C16 120.1(6) . . ? C18 C17 C22 119.8(6) . . ? C16 C17 C22 120.0(6) . . ? C18 C17 K 73.8(4) . . ? C16 C17 K 85.7(3) . . ? C22 C17 K 107.0(4) . . ? C17 C18 C19 121.7(6) . . ? C17 C18 K 80.7(4) . . ? C19 C18 K 80.2(5) . . ? C20 C19 C18 118.8(7) . . ? C20 C19 K 82.7(5) . . ? C18 C19 K 74.3(4) . . ? C19 C20 C21 122.6(6) . . ? C19 C20 K 72.7(4) . . ? C21 C20 K 83.1(4) . . ? C20 C21 C16 119.1(5) . . ? C20 C21 C25 118.7(5) . . ? C16 C21 C25 122.2(5) . . ? C20 C21 K 73.2(4) . . ? C16 C21 K 76.9(3) . . ? C25 C21 K 122.8(4) . . ? C24 C22 C17 109.1(5) . . ? C24 C22 C23 110.3(6) . . ? C17 C22 C23 112.7(6) . . ? C22 C24 K 98.7(4) . . ? C26 C25 C21 111.8(5) . . ? C26 C25 C27 109.8(5) . . ? C21 C25 C27 111.5(5) . . ? N3 C28 C29 114.2(4) . . ? C28 C29 C30 116.9(5) . . ? N4 C30 C29 111.5(4) . . ? C36 C31 C32 118.7(6) . . ? C36 C31 N3 120.2(6) . . ? C32 C31 N3 121.2(5) . . ? C33 C32 C31 119.2(6) . . ? C33 C32 C37 118.5(6) . . ? C31 C32 C37 122.3(6) . . ? C34 C33 C32 121.7(7) . . ? C35 C34 C33 118.6(7) . . ? C34 C35 C36 122.9(7) . . ? C35 C36 C31 118.8(7) . . ? C35 C36 C40 118.9(7) . . ? C31 C36 C40 122.2(6) . . ? C32 C37 C38 112.8(6) . . ? C32 C37 C39 110.8(6) . . ? C38 C37 C39 109.3(6) . . ? C36 C40 C42 113.4(8) . . ? C36 C40 C41 109.5(6) . . ? C42 C40 C41 110.6(7) . . ? C44 C43 N4 120.2(5) . . ? C44 C43 C48 118.6(5) . . ? N4 C43 C48 121.2(5) . . ? C45 C44 C43 119.8(6) . . ? C45 C44 C49 119.7(6) . . ? C43 C44 C49 120.5(5) . . ? C46 C45 C44 121.2(6) . . ? C47 C46 C45 119.7(6) . . ? C47 C46 K 77.7(4) . 1_455 ? C45 C46 K 106.5(4) . 1_455 ? C46 C47 C48 121.2(6) . . ? C46 C47 K 76.7(4) . 1_455 ? C48 C47 K 106.8(4) . 1_455 ? C47 C48 C43 119.5(6) . . ? C47 C48 C52 118.9(6) . . ? C43 C48 C52 121.6(5) . . ? C51 C49 C44 114.2(6) . . ? C51 C49 C50 108.0(6) . . ? C44 C49 C50 114.1(6) . . ? C48 C52 C53 112.1(5) . . ? C48 C52 C54 110.5(5) . . ? C53 C52 C54 111.0(5) . . ? C56 C55 C60 120 . . ? C56 C55 K 85.5(6) . . ? C60 C55 K 94.0(5) . . ? C57 C56 C55 120 . . ? C57 C56 K 102.1(4) . . ? C55 C56 K 69.0(5) . . ? C56 C57 C58 120 . . ? C57 C58 C59 120 . . ? C61 C59 C60 106(2) . . ? C61 C59 C58 134(2) . . ? C60 C59 C58 120 . . ? C59 C60 C55 120 . . ? C59 C60 K 101.4(4) . . ? C55 C60 K 61.9(4) . . ? #===END data_[{YI(thf)2(C6H3iPr2NCH2CH2NC6H3iPr2)}2].2.5(toluene)_[10] _database_code_depnum_ccdc_archive 'CCDC 228147' _audit_creation_date 2002-09-30T15:08:21-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common ; '[{YI(thf)2(C6H3iPr2NCH2CH2NC6H3iPr2)}2].2.5(toluene)' ; _chemical_formula_moiety '(C68 H108 I2 N4 O4 Y2) 2.5(C7 H8)' _chemical_formula_sum 'C85.50 H128 I2 N4 O4 Y2' _chemical_formula_weight 1707.54 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.2250(4) _cell_length_b 14.2440(4) _cell_length_c 25.3516(9) _cell_angle_alpha 78.418(1) _cell_angle_beta 80.205(1) _cell_angle_gamma 85.201(2) _cell_volume 4256.0(2) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 256334 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 22.722 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.332 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1770 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.13 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.7061 _exptl_absorpt_correction_T_max 0.8209 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0732 _diffrn_reflns_av_unetI/netI 0.0699 _diffrn_reflns_number 34631 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.76 _diffrn_reflns_theta_max 23.05 _diffrn_reflns_theta_full 23.05 _diffrn_measured_fraction_theta_full 0.957 _diffrn_measured_fraction_theta_max 0.957 _reflns_number_total 11404 _reflns_number_gt 9046 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; There are two independent dimers both on inversion centres. There are two toluene solvate molecules in general positions included with rigid C6 rings and 1,2 and 1,3 distance constraints(SADI) on the methyl carbon. There is another toluene disordered across an inversion centre included with distance constraints(SADI) and with H atoms omitted. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+73.3600P] 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 'riding; omitted for disordered toluene' _refine_ls_extinction_method none _refine_ls_number_reflns 11404 _refine_ls_number_parameters 760 _refine_ls_number_restraints 27 _refine_ls_R_factor_all 0.1288 _refine_ls_R_factor_gt 0.1027 _refine_ls_wR_factor_ref 0.2173 _refine_ls_wR_factor_gt 0.2078 _refine_ls_goodness_of_fit_ref 1.266 _refine_ls_restrained_S_all 1.267 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.205 _refine_diff_density_min -1.097 _refine_diff_density_rms 0.13 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 I I 0.06689(8) 0.41616(7) 0.05996(4) 0.0470(3) Uani 1 1 d . . . Y Y -0.05416(10) 0.61690(9) 0.06151(5) 0.0328(3) Uani 1 1 d . . . O1 O -0.1860(8) 0.7403(6) 0.0302(4) 0.046(3) Uani 1 1 d . C . O2 O -0.2228(7) 0.5354(7) 0.0930(4) 0.046(2) Uani 1 1 d . . . N1 N 0.0969(8) 0.7000(7) 0.0492(4) 0.032(3) Uani 1 1 d . . . N2 N -0.0640(9) 0.6497(8) 0.1441(4) 0.037(3) Uani 1 1 d . . . C1 C 0.0867(12) 0.7544(11) 0.0937(6) 0.047(4) Uani 1 1 d . . . H1A H 0.0417 0.8138 0.0844 0.057 Uiso 1 1 calc R . . H1B H 0.1608 0.7722 0.0967 0.057 Uiso 1 1 calc R . . C2 C 0.0354(13) 0.7000(12) 0.1476(6) 0.057(4) Uani 1 1 d . . . H2A H 0.0907 0.6527 0.1624 0.068 Uiso 1 1 calc R . . H2B H 0.0141 0.7445 0.1728 0.068 Uiso 1 1 calc R . . C3 C 0.2013(11) 0.7099(10) 0.0147(6) 0.040(3) Uani 1 1 d . . . C4 C 0.2082(11) 0.7734(10) -0.0366(6) 0.043(4) Uani 1 1 d . . . C5 C 0.3129(15) 0.7858(12) -0.0705(8) 0.071(5) Uani 1 1 d . . . H5 H 0.3198 0.8287 -0.1042 0.085 Uiso 1 1 calc R . . C6 C 0.4071(14) 0.7317(15) -0.0523(8) 0.071(5) Uani 1 1 d . . . H6 H 0.4764 0.7354 -0.0751 0.085 Uiso 1 1 calc R . . C7 C 0.3976(13) 0.6773(14) -0.0045(9) 0.069(5) Uani 1 1 d . . . H7 H 0.4629 0.6469 0.0071 0.082 Uiso 1 1 calc R . . C8 C 0.2990(11) 0.6603(11) 0.0310(6) 0.047(4) Uani 1 1 d . . . C9 C 0.1093(13) 0.8333(10) -0.0566(7) 0.055(4) Uani 1 1 d . . . H9 H 0.042 0.8041 -0.0341 0.066 Uiso 1 1 calc R . . C10 C 0.0992(18) 0.8334(15) -0.1156(8) 0.088(6) Uani 1 1 d . . . H10A H 0.0334 0.8719 -0.1248 0.132 Uiso 1 1 calc R . . H10B H 0.0932 0.7682 -0.1201 0.132 Uiso 1 1 calc R . . H10C H 0.1645 0.8603 -0.1393 0.132 Uiso 1 1 calc R . . C11 C 0.1065(18) 0.9354(11) -0.0468(8) 0.081(6) Uani 1 1 d . . . H11A H 0.0418 0.9712 -0.0594 0.122 Uiso 1 1 calc R . . H11B H 0.1733 0.9661 -0.0666 0.122 Uiso 1 1 calc R . . H11C H 0.1027 0.9342 -0.0081 0.122 Uiso 1 1 calc R . . C12 C 0.2962(13) 0.5893(12) 0.0837(7) 0.057(4) Uani 1 1 d . . . H12 H 0.2174 0.5769 0.0985 0.069 Uiso 1 1 calc R . . C13 C 0.3439(15) 0.6341(15) 0.1253(8) 0.086(6) Uani 1 1 d . . . H13A H 0.3414 0.5885 0.1595 0.129 Uiso 1 1 calc R . . H13B H 0.2999 0.6919 0.1315 0.129 Uiso 1 1 calc R . . H13C H 0.4203 0.65 0.111 0.129 Uiso 1 1 calc R . . C14 C 0.3560(15) 0.4947(13) 0.0782(9) 0.081(6) Uani 1 1 d . . . H14A H 0.3496 0.4526 0.1137 0.121 Uiso 1 1 calc R . . H14B H 0.4338 0.5045 0.0639 0.121 Uiso 1 1 calc R . . H14C H 0.3231 0.4656 0.0535 0.121 Uiso 1 1 calc R . . C15 C -0.1261(11) 0.6224(11) 0.1977(6) 0.044(4) Uani 1 1 d . . . C16 C -0.1031(12) 0.5320(11) 0.2304(6) 0.043(4) Uani 1 1 d . . . C17 C -0.1595(16) 0.5128(14) 0.2823(7) 0.071(5) Uani 1 1 d . . . H17 H -0.1434 0.4534 0.3042 0.085 Uiso 1 1 calc R . . C18 C -0.2391(18) 0.5750(18) 0.3050(8) 0.085(7) Uani 1 1 d . . . H18 H -0.2766 0.5594 0.341 0.102 Uiso 1 1 calc R . . C19 C -0.2585(14) 0.6580(17) 0.2724(8) 0.074(6) Uani 1 1 d . . . H19 H -0.3124 0.7009 0.2869 0.089 Uiso 1 1 calc R . . C20 C -0.2074(12) 0.6876(13) 0.2192(7) 0.060(5) Uani 1 1 d . . . C21 C -0.0191(14) 0.4584(12) 0.2107(7) 0.062(5) Uani 1 1 d . . . H21 H 0.0063 0.4828 0.1715 0.075 Uiso 1 1 calc R . . C22 C -0.0680(16) 0.3620(12) 0.2150(8) 0.075(5) Uani 1 1 d . . . H22A H -0.1314 0.3709 0.1958 0.112 Uiso 1 1 calc R . . H22B H -0.0917 0.3345 0.2531 0.112 Uiso 1 1 calc R . . H22C H -0.0122 0.3191 0.1989 0.112 Uiso 1 1 calc R . . C23 C 0.0824(17) 0.4460(17) 0.2383(11) 0.111(8) Uani 1 1 d . . . H23A H 0.1344 0.3988 0.2237 0.167 Uiso 1 1 calc R . . H23B H 0.0607 0.4242 0.2772 0.167 Uiso 1 1 calc R . . H23C H 0.1173 0.5068 0.2318 0.167 Uiso 1 1 calc R . . C24 C -0.2386(19) 0.7784(17) 0.1872(9) 0.096(7) Uani 1 1 d . . . H24 H -0.2044 0.7773 0.149 0.115 Uiso 1 1 calc R . . C25 C -0.191(2) 0.8657(17) 0.2035(11) 0.131(10) Uani 1 1 d . . . H25A H -0.2139 0.9247 0.1805 0.196 Uiso 1 1 calc R . . H25B H -0.1108 0.8585 0.1985 0.196 Uiso 1 1 calc R . . H25C H -0.2199 0.8677 0.2413 0.196 Uiso 1 1 calc R . . C26 C -0.3641(19) 0.801(2) 0.1868(12) 0.142(12) Uani 1 1 d . . . H26A H -0.3757 0.8631 0.1643 0.213 Uiso 1 1 calc R . . H26B H -0.4017 0.8007 0.2237 0.213 Uiso 1 1 calc R . . H26C H -0.3939 0.752 0.1722 0.213 Uiso 1 1 calc R . . C27 C -0.1754(12) 0.8409(10) 0.0278(7) 0.055(4) Uani 1 1 d . . . H27A H -0.0997 0.8546 0.0307 0.066 Uiso 1 1 calc R A 1 H27B H -0.228 0.8651 0.0563 0.066 Uiso 1 1 calc R A 1 C30 C -0.2815(13) 0.7338(13) 0.0039(8) 0.069(5) Uani 1 1 d . . . H30A H -0.3507 0.7438 0.0285 0.083 Uiso 1 1 calc R B 1 H30B H -0.2808 0.6703 -0.0055 0.083 Uiso 1 1 calc R B 1 C31 C -0.3170(13) 0.5731(13) 0.1274(8) 0.069(5) Uani 1 1 d . . . H31A H -0.3746 0.6026 0.1059 0.083 Uiso 1 1 calc R . . H31B H -0.2936 0.6213 0.1454 0.083 Uiso 1 1 calc R . . C32 C -0.3584(15) 0.4899(16) 0.1678(8) 0.084(6) Uani 1 1 d . . . H32A H -0.4381 0.4991 0.1805 0.1 Uiso 1 1 calc R . . H32B H -0.3188 0.4785 0.1992 0.1 Uiso 1 1 calc R . . C33 C -0.3355(16) 0.4069(16) 0.1371(8) 0.088(6) Uani 1 1 d . . . H33A H -0.3061 0.3496 0.1599 0.106 Uiso 1 1 calc R . . H33B H -0.4033 0.3913 0.1257 0.106 Uiso 1 1 calc R . . C34 C -0.2524(15) 0.4420(12) 0.0895(8) 0.071(6) Uani 1 1 d . . . H34A H -0.1863 0.398 0.0888 0.086 Uiso 1 1 calc R . . H34B H -0.2831 0.4451 0.0559 0.086 Uiso 1 1 calc R . . C28 C -0.205(3) 0.885(3) -0.0318(17) 0.104(14) Uiso 0.58(2) 1 d P C 1 H28A H -0.249 0.9455 -0.0316 0.125 Uiso 0.58(2) 1 calc PR C 1 H28B H -0.1374 0.8959 -0.0584 0.125 Uiso 0.58(2) 1 calc PR C 1 C29 C -0.274(4) 0.809(3) -0.0461(19) 0.119(16) Uiso 0.58(2) 1 d P C 1 H29A H -0.3476 0.836 -0.053 0.142 Uiso 0.58(2) 1 calc PR C 1 H29B H -0.2353 0.7841 -0.078 0.142 Uiso 0.58(2) 1 calc PR C 1 C28A C -0.295(3) 0.881(2) 0.0407(15) 0.045(10) Uiso 0.42(2) 1 d P C 2 H28C H -0.3148 0.8855 0.0793 0.054 Uiso 0.42(2) 1 calc PR C 2 H28D H -0.3067 0.9446 0.0183 0.054 Uiso 0.42(2) 1 calc PR C 2 C29A C -0.360(3) 0.809(2) 0.0268(15) 0.048(11) Uiso 0.42(2) 1 d P C 2 H29C H -0.4067 0.8402 -0.0003 0.057 Uiso 0.42(2) 1 calc PR C 2 H29D H -0.4088 0.7783 0.0594 0.057 Uiso 0.42(2) 1 calc PR C 2 I1B I -0.40418(8) -0.04048(6) 0.43688(4) 0.0464(3) Uani 1 1 d . . 3 Y1B Y -0.51324(10) 0.16393(9) 0.44333(5) 0.0309(3) Uani 1 1 d . . 3 O1B O -0.6683(8) 0.1132(6) 0.4101(4) 0.047(3) Uani 1 1 d . D 3 O2B O -0.6628(7) 0.2660(6) 0.4775(4) 0.046(3) Uani 1 1 d . E 3 N1B N -0.4658(8) 0.2571(7) 0.3629(4) 0.031(2) Uani 1 1 d . F 3 N2B N -0.3703(9) 0.2338(7) 0.4577(4) 0.032(3) Uani 1 1 d . F 3 C1B C -0.3654(11) 0.3094(10) 0.3594(5) 0.038(3) Uani 1 1 d . F 3 H1B1 H -0.3718 0.3723 0.3356 0.046 Uiso 1 1 calc R F 3 H1B2 H -0.3004 0.2736 0.3433 0.046 Uiso 1 1 calc R F 3 C2B C -0.3496(11) 0.3223(8) 0.4152(5) 0.034(3) Uani 1 1 d . F 3 H2B1 H -0.2734 0.3408 0.4136 0.04 Uiso 1 1 calc R F 3 H2B2 H -0.4003 0.3747 0.4258 0.04 Uiso 1 1 calc R F 3 C3B C -0.5012(11) 0.2722(9) 0.3116(5) 0.034(3) Uani 1 1 d . F 3 C4B C -0.5697(11) 0.3538(9) 0.2936(5) 0.035(3) Uani 1 1 d . F 3 C5B C -0.6077(11) 0.3641(10) 0.2443(6) 0.043(4) Uani 1 1 d . F 3 H5B H -0.6532 0.4183 0.2328 0.052 Uiso 1 1 calc R F 3 C6B C -0.5800(13) 0.2958(11) 0.2118(6) 0.049(4) Uani 1 1 d . F 3 H6B H -0.6079 0.3028 0.1788 0.059 Uiso 1 1 calc R F 3 C7B C -0.5121(13) 0.2185(10) 0.2278(6) 0.046(4) Uani 1 1 d . F 3 H7B H -0.4923 0.1732 0.205 0.055 Uiso 1 1 calc R F 3 C8B C -0.4719(12) 0.2047(9) 0.2755(6) 0.042(4) Uani 1 1 d . F 3 H8B H -0.537 0.1674 0.2941 0.05 Uiso 1 1 calc R F 3 C9B C -0.5982(11) 0.4320(9) 0.3278(6) 0.047(4) Uani 1 1 d . F 3 C10B C -0.7234(13) 0.4523(12) 0.3420(8) 0.064(5) Uani 1 1 d . F 3 H10D H -0.737 0.5024 0.3636 0.097 Uiso 1 1 calc R F 3 H10E H -0.7576 0.3944 0.3628 0.097 Uiso 1 1 calc R F 3 H10F H -0.755 0.4731 0.3088 0.097 Uiso 1 1 calc R F 3 C11B C -0.5461(14) 0.5257(11) 0.2974(7) 0.061(5) Uani 1 1 d . F 3 H11D H -0.5651 0.5746 0.3196 0.091 Uiso 1 1 calc R F 3 H11E H -0.5741 0.5465 0.2632 0.091 Uiso 1 1 calc R F 3 H11F H -0.4659 0.5153 0.2903 0.091 Uiso 1 1 calc R F 3 C12B C -0.3948(13) 0.1180(10) 0.2911(6) 0.053(4) Uani 1 1 d . F 3 H12B H -0.389 0.1108 0.3302 0.064 Uiso 1 1 calc R F 3 C13B C -0.2784(15) 0.1359(16) 0.2573(9) 0.097(7) Uani 1 1 d . F 3 H13D H -0.228 0.0815 0.2674 0.145 Uiso 1 1 calc R F 3 H13E H -0.251 0.1934 0.2644 0.145 Uiso 1 1 calc R F 3 H13F H -0.2831 0.1441 0.2188 0.145 Uiso 1 1 calc R F 3 C14B C -0.4333(18) 0.0250(12) 0.2818(8) 0.086(6) Uani 1 1 d . F 3 H14D H -0.3809 -0.0273 0.2928 0.129 Uiso 1 1 calc R F 3 H14E H -0.4375 0.0304 0.2434 0.129 Uiso 1 1 calc R F 3 H14F H -0.5061 0.0124 0.3031 0.129 Uiso 1 1 calc R F 3 C15B C -0.2872(11) 0.2129(9) 0.4919(6) 0.037(3) Uani 1 1 d . F 3 C16B C -0.3066(12) 0.2336(9) 0.5453(6) 0.040(3) Uani 1 1 d . F 3 C17B C -0.2192(16) 0.2146(12) 0.5764(6) 0.056(5) Uani 1 1 d . F 3 H17B H -0.2313 0.2275 0.6119 0.067 Uiso 1 1 calc R F 3 C18B C -0.1226(14) 0.1799(10) 0.5573(7) 0.048(4) Uani 1 1 d . F 3 H18B H -0.0666 0.1697 0.5793 0.057 Uiso 1 1 calc R F 3 C19B C -0.0989(12) 0.1576(11) 0.5072(7) 0.056(4) Uani 1 1 d . F 3 H19B H -0.0276 0.1325 0.4949 0.067 Uiso 1 1 calc R F 3 C20B C -0.1821(11) 0.1722(9) 0.4733(6) 0.040(4) Uani 1 1 d . F 3 C21B C -0.4170(12) 0.2814(9) 0.5663(6) 0.044(4) Uani 1 1 d . F 3 H21B H -0.4727 0.2682 0.5449 0.052 Uiso 1 1 calc R F 3 C22B C -0.4066(16) 0.3921(10) 0.5553(7) 0.066(5) Uani 1 1 d . F 3 H22D H -0.4772 0.4226 0.5683 0.099 Uiso 1 1 calc R F 3 H22E H -0.3866 0.4154 0.5164 0.099 Uiso 1 1 calc R F 3 H22F H -0.3496 0.4071 0.5742 0.099 Uiso 1 1 calc R F 3 C23B C -0.4599(16) 0.2436(12) 0.6264(7) 0.072(5) Uani 1 1 d . F 3 H23D H -0.5305 0.2766 0.637 0.109 Uiso 1 1 calc R F 3 H23E H -0.4066 0.2551 0.6485 0.109 Uiso 1 1 calc R F 3 H23F H -0.4698 0.1753 0.632 0.109 Uiso 1 1 calc R F 3 C24B C -0.1540(12) 0.1432(10) 0.4182(6) 0.047(4) Uani 1 1 d . F 3 H24B H -0.224 0.1447 0.4033 0.056 Uiso 1 1 calc R F 3 C25B C -0.0749(14) 0.2124(14) 0.3773(8) 0.078(6) Uani 1 1 d . F 3 H25D H -0.0598 0.1915 0.3425 0.118 Uiso 1 1 calc R F 3 H25E H -0.0058 0.2125 0.3912 0.118 Uiso 1 1 calc R F 3 H25F H -0.1095 0.2767 0.3724 0.118 Uiso 1 1 calc R F 3 C26B C -0.1001(14) 0.0407(12) 0.4220(8) 0.072(5) Uani 1 1 d . F 3 H26D H -0.0846 0.0247 0.3859 0.108 Uiso 1 1 calc R F 3 H26E H -0.1506 -0.0044 0.4457 0.108 Uiso 1 1 calc R F 3 H26F H -0.0313 0.0374 0.4367 0.108 Uiso 1 1 calc R F 3 C27B C -0.7438(12) 0.1798(11) 0.3803(7) 0.054(4) Uani 1 1 d . D 3 H27C H -0.7101 0.2416 0.3654 0.065 Uiso 1 1 calc R D 3 H27D H -0.8137 0.1907 0.4042 0.065 Uiso 1 1 calc R D 3 C28B C -0.7640(13) 0.1333(13) 0.3357(7) 0.063(5) Uani 1 1 d . D 3 H28E H -0.7061 0.1471 0.3037 0.075 Uiso 1 1 calc R D 3 H28F H -0.8367 0.154 0.3248 0.075 Uiso 1 1 calc R D 3 C29B C -0.7596(15) 0.0267(14) 0.3621(8) 0.073(5) Uani 1 1 d . D 3 H29E H -0.8349 0.0036 0.3734 0.087 Uiso 1 1 calc R D 3 H29F H -0.7183 -0.0114 0.3363 0.087 Uiso 1 1 calc R D 3 C30B C -0.7033(15) 0.0186(12) 0.4096(8) 0.073(6) Uani 1 1 d . D 3 H30C H -0.7541 -0.0045 0.4431 0.088 Uiso 1 1 calc R D 3 H30D H -0.6388 -0.0268 0.4071 0.088 Uiso 1 1 calc R D 3 C31B C -0.7745(12) 0.2431(12) 0.5044(7) 0.063(5) Uani 1 1 d . E 3 H31C H -0.7826 0.1736 0.5133 0.075 Uiso 1 1 calc R E 3 H31D H -0.8299 0.273 0.4816 0.075 Uiso 1 1 calc R E 3 C32B C -0.7862(16) 0.2853(16) 0.5561(8) 0.092(7) Uani 1 1 d . E 3 H32C H -0.8636 0.3057 0.5676 0.11 Uiso 1 1 calc R E 3 H32D H -0.7606 0.2382 0.5859 0.11 Uiso 1 1 calc R E 3 C33B C -0.7129(16) 0.3706(14) 0.5399(8) 0.076(6) Uani 1 1 d . E 3 H33C H -0.7582 0.4309 0.5381 0.091 Uiso 1 1 calc R E 3 H33D H -0.6622 0.3682 0.5662 0.091 Uiso 1 1 calc R E 3 C34B C -0.6494(12) 0.3626(8) 0.4850(5) 0.052(4) Uani 1 1 d . E 3 H34C H -0.6789 0.4102 0.4566 0.062 Uiso 1 1 calc R E 3 H34D H -0.5707 0.3734 0.4834 0.062 Uiso 1 1 calc R E 3 C1C C -0.2624(12) 0.9385(8) -0.1413(5) 0.48(5) Uiso 1 1 d R E 4 C2C C -0.2207(12) 1.0065(8) -0.1187(5) 0.36(3) Uiso 1 1 d RD E 4 H2C H -0.1436 1.0131 -0.1234 0.428 Uiso 1 1 calc R E 4 C3C C -0.2929(12) 1.0649(8) -0.0893(5) 0.36(3) Uiso 1 1 d R E 4 H3C H -0.2647 1.1109 -0.074 0.431 Uiso 1 1 calc R E 4 C4C C -0.4070(12) 1.0553(8) -0.0824(5) 0.26(2) Uiso 1 1 d R E 4 H4C H -0.4558 1.0947 -0.0624 0.314 Uiso 1 1 calc R E 4 C5C C -0.4487(12) 0.9873(8) -0.1050(5) 0.44(5) Uiso 1 1 d R E 4 H5C H -0.5258 0.9807 -0.1003 0.526 Uiso 1 1 calc R E 4 C6C C -0.3765(12) 0.9289(8) -0.1344(5) 0.31(3) Uiso 1 1 d RD E 4 H6C H -0.4047 0.8829 -0.1497 0.369 Uiso 1 1 calc R E 4 C7C C -0.1892(15) 0.8846(14) -0.1752(7) 0.44(5) Uiso 1 1 d D E 4 H7C1 H -0.232 0.8459 -0.1908 0.657 Uiso 0.5 1 calc PR E 4 H7C2 H -0.1395 0.8431 -0.1536 0.657 Uiso 0.5 1 calc PR E 4 H7C3 H -0.1461 0.928 -0.2042 0.657 Uiso 0.5 1 calc PR E 4 H7C4 H -0.1131 0.8987 -0.1749 0.657 Uiso 0.5 1 calc PR E 4 H7C5 H -0.2056 0.9016 -0.2121 0.657 Uiso 0.5 1 calc PR E 4 H7C6 H -0.199 0.8167 -0.1615 0.657 Uiso 0.5 1 calc PR E 4 C8C C 0.2060(15) 0.8117(14) 0.2577(7) 0.226(19) Uiso 1 1 d R E 4 C9C C 0.1647(15) 0.7207(14) 0.2744(7) 0.235(19) Uiso 1 1 d RD E 4 H9C H 0.2105 0.6664 0.2681 0.282 Uiso 1 1 calc R E 4 C10C C 0.0556(15) 0.7099(14) 0.3005(7) 0.211(17) Uiso 1 1 d R E 4 H10G H 0.0277 0.6483 0.3118 0.253 Uiso 1 1 calc R E 4 C11C C -0.0121(15) 0.7901(14) 0.3099(7) 0.27(2) Uiso 1 1 d R E 4 H11G H -0.0858 0.7829 0.3275 0.328 Uiso 1 1 calc R E 4 C12C C 0.0293(15) 0.8812(14) 0.2932(7) 0.27(2) Uiso 1 1 d R E 4 H12C H -0.0165 0.9354 0.2995 0.327 Uiso 1 1 calc R E 4 C13C C 0.1383(15) 0.8919(14) 0.2671(7) 0.200(16) Uiso 1 1 d RD E 4 H13G H 0.1663 0.9535 0.2558 0.24 Uiso 1 1 calc R E 4 C14C C 0.318(3) 0.8223(18) 0.234(2) 0.30(3) Uiso 1 1 d D E 4 H14G H 0.3339 0.8898 0.2252 0.455 Uiso 0.5 1 calc PR E 4 H14H H 0.332 0.7965 0.2003 0.455 Uiso 0.5 1 calc PR E 4 H14I H 0.366 0.7878 0.2587 0.455 Uiso 0.5 1 calc PR E 4 H14J H 0.3541 0.7597 0.231 0.455 Uiso 0.5 1 calc PR E 4 H14K H 0.3559 0.8529 0.2559 0.455 Uiso 0.5 1 calc PR E 4 H14L H 0.3219 0.8616 0.1974 0.455 Uiso 0.5 1 calc PR E 4 C15C C 0.000(3) 0.507(2) 0.5269(9) 0.105(15) Uiso 0.5 1 d PD . 4 C16C C 0.062(3) 0.579(2) 0.5245(13) 0.070(10) Uiso 0.5 1 d PD . 4 C17C C 0.017(2) 0.527(2) 0.5733(10) 0.139(10) Uiso 1 1 d D G 4 C18C C -0.045(3) 0.453(2) 0.5722(9) 0.098(14) Uiso 0.5 1 d PD G 4 C19C C -0.0587(18) 0.4340(15) 0.5248(9) 0.091(6) Uiso 1 1 d D . 4 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 I 0.0572(7) 0.0434(6) 0.0429(6) -0.0172(5) -0.0099(5) 0.0086(5) Y 0.0281(7) 0.0354(8) 0.0383(8) -0.0170(6) -0.0021(6) -0.0029(6) O1 0.047(6) 0.039(6) 0.059(7) -0.024(5) -0.014(5) 0.012(5) O2 0.038(6) 0.049(6) 0.053(6) -0.024(5) 0.010(5) -0.014(5) N1 0.019(6) 0.044(7) 0.037(7) -0.020(5) -0.005(5) -0.001(5) N2 0.034(7) 0.044(7) 0.034(7) -0.013(5) -0.001(5) -0.003(5) C1 0.042(9) 0.052(9) 0.052(10) -0.025(8) 0.002(7) -0.008(7) C2 0.060(11) 0.067(11) 0.054(11) -0.030(9) -0.014(8) -0.005(9) C3 0.037(9) 0.046(9) 0.038(9) -0.015(7) 0.007(7) -0.014(7) C4 0.031(8) 0.039(8) 0.065(11) -0.031(8) 0.009(7) -0.014(7) C5 0.076(14) 0.054(11) 0.074(13) -0.001(9) 0.007(10) -0.015(10) C6 0.037(10) 0.120(17) 0.047(11) -0.009(11) 0.009(8) 0.007(10) C7 0.034(10) 0.085(14) 0.095(16) -0.040(12) -0.013(10) 0.006(9) C8 0.029(9) 0.050(9) 0.063(11) -0.016(8) 0.000(7) -0.008(7) C9 0.057(11) 0.041(9) 0.057(11) -0.007(8) 0.016(8) -0.004(8) C10 0.106(17) 0.087(15) 0.072(14) -0.018(12) -0.017(12) 0.005(12) C11 0.121(17) 0.037(10) 0.083(14) -0.017(9) -0.006(12) 0.013(10) C12 0.038(9) 0.068(11) 0.059(11) -0.003(9) -0.004(8) 0.009(8) C13 0.059(12) 0.120(17) 0.087(15) -0.018(13) -0.036(11) -0.006(12) C14 0.058(12) 0.081(14) 0.106(16) -0.016(12) -0.029(11) 0.011(10) C15 0.039(9) 0.059(10) 0.044(9) -0.030(8) -0.006(7) -0.006(7) C16 0.042(9) 0.051(9) 0.037(9) -0.016(7) 0.002(7) -0.014(7) C17 0.085(14) 0.074(13) 0.046(11) -0.004(9) 0.008(10) -0.016(11) C18 0.090(16) 0.121(19) 0.047(12) -0.031(13) 0.020(11) -0.044(14) C19 0.057(12) 0.122(18) 0.045(12) -0.045(12) 0.018(9) 0.009(12) C20 0.037(9) 0.088(13) 0.059(11) -0.029(10) -0.014(8) 0.021(9) C21 0.073(12) 0.067(12) 0.047(10) -0.013(9) -0.003(9) -0.007(9) C22 0.083(14) 0.055(11) 0.086(14) -0.014(10) -0.013(11) 0.001(10) C23 0.069(14) 0.122(19) 0.16(2) -0.046(17) -0.054(15) 0.028(13) C24 0.115(18) 0.110(17) 0.069(13) -0.052(13) -0.017(12) 0.048(15) C25 0.14(2) 0.096(19) 0.14(2) -0.013(17) 0.012(18) 0.034(17) C26 0.101(19) 0.17(3) 0.19(3) -0.11(2) -0.079(19) 0.097(19) C27 0.030(8) 0.049(10) 0.086(13) -0.021(9) -0.008(8) 0.015(7) C30 0.042(10) 0.082(13) 0.096(15) -0.042(12) -0.022(10) 0.015(9) C31 0.037(10) 0.090(14) 0.084(14) -0.049(12) 0.016(9) -0.003(9) C32 0.058(12) 0.128(18) 0.061(13) -0.024(13) 0.024(10) -0.038(12) C33 0.070(14) 0.107(17) 0.082(15) -0.006(13) 0.007(11) -0.037(12) C34 0.068(12) 0.056(11) 0.094(14) -0.038(10) 0.021(10) -0.036(9) I1B 0.0547(7) 0.0322(5) 0.0443(6) -0.0044(4) 0.0082(5) 0.0042(4) Y1B 0.0261(7) 0.0262(7) 0.0391(8) -0.0069(6) -0.0015(6) -0.0005(5) O1B 0.040(6) 0.040(6) 0.063(7) -0.006(5) -0.015(5) -0.004(5) O2B 0.038(6) 0.034(6) 0.055(6) -0.003(5) 0.014(5) 0.008(4) N1B 0.024(6) 0.036(6) 0.031(6) -0.008(5) 0.001(5) 0.001(5) N2B 0.041(7) 0.022(6) 0.033(6) -0.004(5) -0.009(5) 0.010(5) C1B 0.035(8) 0.036(8) 0.040(9) 0.001(6) -0.005(6) -0.002(6) C2B 0.032(8) 0.019(7) 0.047(9) -0.001(6) -0.005(6) 0.002(6) C3B 0.041(8) 0.031(8) 0.026(8) -0.002(6) 0.004(6) -0.002(6) C4B 0.038(8) 0.036(8) 0.026(8) -0.002(6) 0.002(6) -0.007(6) C5B 0.036(8) 0.034(8) 0.054(10) 0.009(7) -0.012(7) -0.001(6) C6B 0.063(11) 0.056(10) 0.032(9) -0.007(8) -0.014(7) -0.023(8) C7B 0.076(11) 0.033(8) 0.028(8) -0.006(7) -0.006(8) 0.001(8) C8B 0.049(9) 0.025(7) 0.046(10) 0.000(7) 0.004(7) -0.013(6) C9B 0.037(9) 0.028(8) 0.069(11) -0.005(7) 0.005(7) 0.002(6) C10B 0.049(10) 0.057(11) 0.084(13) -0.020(9) -0.002(9) 0.012(8) C11B 0.067(11) 0.051(10) 0.076(12) -0.026(9) -0.023(9) -0.006(8) C12B 0.073(12) 0.038(9) 0.043(9) -0.007(7) 0.002(8) 0.006(8) C13B 0.063(13) 0.109(17) 0.105(17) -0.021(14) 0.010(12) 0.025(12) C14B 0.113(17) 0.051(11) 0.088(15) -0.022(10) 0.007(12) -0.001(11) C15B 0.034(8) 0.029(7) 0.047(9) 0.000(6) -0.010(7) -0.013(6) C16B 0.052(9) 0.023(7) 0.046(9) -0.013(6) -0.002(7) -0.005(6) C17B 0.079(13) 0.061(11) 0.036(9) 0.004(8) -0.028(9) -0.040(10) C18B 0.058(11) 0.043(9) 0.044(10) 0.014(8) -0.038(9) -0.009(8) C19B 0.032(9) 0.052(10) 0.079(13) 0.001(9) -0.014(8) 0.002(7) C20B 0.024(8) 0.037(8) 0.055(10) 0.002(7) -0.004(7) -0.002(6) C21B 0.061(10) 0.035(8) 0.041(9) -0.016(7) -0.008(7) -0.014(7) C22B 0.103(15) 0.039(9) 0.058(11) -0.021(8) 0.002(10) -0.013(9) C23B 0.089(14) 0.064(12) 0.056(11) -0.020(9) 0.025(10) -0.019(10) C24B 0.033(8) 0.051(9) 0.057(10) -0.005(8) -0.018(7) 0.001(7) C25B 0.047(11) 0.099(15) 0.075(13) 0.009(11) 0.002(9) -0.012(10) C26B 0.060(12) 0.076(13) 0.074(13) -0.015(10) -0.007(10) 0.023(10) C27B 0.034(9) 0.052(10) 0.072(12) -0.001(9) -0.012(8) 0.003(7) C28B 0.041(10) 0.096(14) 0.050(11) -0.004(10) -0.010(8) -0.015(9) C29B 0.063(12) 0.084(14) 0.079(14) -0.027(11) -0.014(10) -0.019(10) C30B 0.073(13) 0.051(11) 0.105(16) -0.004(10) -0.040(12) -0.026(9) C31B 0.027(9) 0.060(11) 0.091(14) -0.004(10) 0.003(9) 0.004(8) C32B 0.069(14) 0.100(16) 0.084(15) -0.016(13) 0.024(11) 0.043(13) C33B 0.067(13) 0.085(14) 0.073(13) -0.032(11) 0.002(10) 0.019(11) C34B 0.071(11) 0.026(8) 0.053(10) -0.013(7) 0.000(8) 0.014(7) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 I Y 3.1120(16) . ? I Y 3.2385(16) 2_565 ? Y N2 2.216(10) . ? Y N1 2.220(10) . ? Y O2 2.388(9) . ? Y O1 2.391(9) . ? Y I 3.2385(16) 2_565 ? O1 C27 1.437(17) . ? O1 C30 1.457(17) . ? O2 C34 1.431(16) . ? O2 C31 1.456(16) . ? N1 C3 1.419(16) . ? N1 C1 1.475(16) . ? N2 C15 1.436(18) . ? N2 C2 1.485(18) . ? C1 C2 1.49(2) . ? C3 C8 1.42(2) . ? C3 C4 1.42(2) . ? C4 C5 1.42(2) . ? C4 C9 1.52(2) . ? C5 C6 1.42(2) . ? C6 C7 1.29(2) . ? C7 C8 1.38(2) . ? C8 C12 1.50(2) . ? C9 C10 1.52(2) . ? C9 C11 1.52(2) . ? C12 C14 1.50(2) . ? C12 C13 1.55(2) . ? C15 C20 1.42(2) . ? C15 C16 1.42(2) . ? C16 C17 1.36(2) . ? C16 C21 1.50(2) . ? C17 C18 1.39(3) . ? C18 C19 1.33(3) . ? C19 C20 1.38(2) . ? C20 C24 1.44(3) . ? C21 C23 1.51(2) . ? C21 C22 1.52(2) . ? C24 C26 1.54(3) . ? C24 C25 1.57(3) . ? C27 C28A 1.53(4) . ? C27 C28 1.60(4) . ? C30 C29 1.48(4) . ? C30 C29A 1.51(4) . ? C31 C32 1.46(2) . ? C32 C33 1.52(3) . ? C33 C34 1.47(2) . ? C28 C29 1.55(5) . ? C28A C29A 1.48(5) . ? I1B Y1B 3.1224(15) . ? I1B Y1B 3.2317(16) 2_456 ? Y1B N2B 2.198(11) . ? Y1B N1B 2.212(10) . ? Y1B O2B 2.394(8) . ? Y1B O1B 2.417(9) . ? Y1B I1B 3.2317(16) 2_456 ? O1B C30B 1.450(17) . ? O1B C27B 1.459(16) . ? O2B C31B 1.451(17) . ? O2B C34B 1.452(15) . ? N1B C3B 1.411(16) . ? N1B C1B 1.469(16) . ? N2B C15B 1.420(16) . ? N2B C2B 1.493(15) . ? C1B C2B 1.511(18) . ? C3B C4B 1.419(18) . ? C3B C8B 1.440(18) . ? C4B C5B 1.381(19) . ? C4B C9B 1.528(19) . ? C5B C6B 1.38(2) . ? C6B C7B 1.36(2) . ? C7B C8B 1.355(19) . ? C8B C12B 1.519(19) . ? C9B C10B 1.53(2) . ? C9B C11B 1.53(2) . ? C12B C14B 1.52(2) . ? C12B C13B 1.54(2) . ? C15B C20B 1.410(18) . ? C15B C16B 1.421(19) . ? C16B C17B 1.41(2) . ? C16B C21B 1.521(19) . ? C17B C18B 1.29(2) . ? C18B C19B 1.35(2) . ? C19B C20B 1.42(2) . ? C20B C24B 1.51(2) . ? C21B C23B 1.53(2) . ? C21B C22B 1.556(19) . ? C24B C26B 1.54(2) . ? C24B C25B 1.55(2) . ? C27B C28B 1.48(2) . ? C28B C29B 1.53(2) . ? C29B C30B 1.47(2) . ? C31B C32B 1.53(3) . ? C32B C33B 1.52(3) . ? C33B C34B 1.49(2) . ? C1C C2C 1.39 . ? C1C C6C 1.39 . ? C1C C7C 1.42(2) . ? C2C C3C 1.39 . ? C3C C4C 1.39 . ? C4C C5C 1.39 . ? C5C C6C 1.39 . ? C8C C13C 1.39 . ? C8C C9C 1.39 . ? C8C C14C 1.41(3) . ? C9C C10C 1.39 . ? C10C C11C 1.39 . ? C11C C12C 1.39 . ? C12C C13C 1.39 . ? C15C C16C 1.309(19) . ? C15C C18C 1.31(2) . ? C15C C17C 1.31(2) . ? C15C C19C 1.329(18) . ? C15C C15C 1.42(4) 2_566 ? C15C C19C 1.51(4) 2_566 ? C16C C19C 1.31(3) 2_566 ? C16C C17C 1.36(2) . ? C17C C18C 1.35(2) . ? C18C C19C 1.325(19) . ? C19C C16C 1.31(3) 2_566 ? C19C C15C 1.51(4) 2_566 ? 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 Y I Y 102.69(4) . 2_565 ? N2 Y N1 79.8(4) . . ? N2 Y O2 88.4(4) . . ? N1 Y O2 168.2(3) . . ? N2 Y O1 96.7(4) . . ? N1 Y O1 100.8(4) . . ? O2 Y O1 79.6(3) . . ? N2 Y I 108.5(3) . . ? N1 Y I 97.1(3) . . ? O2 Y I 87.3(2) . . ? O1 Y I 151.3(2) . . ? N2 Y I 173.3(3) . 2_565 ? N1 Y I 103.1(3) . 2_565 ? O2 Y I 88.5(2) . 2_565 ? O1 Y I 76.9(2) . 2_565 ? I Y I 77.31(4) . 2_565 ? C27 O1 C30 105.9(11) . . ? C27 O1 Y 124.3(8) . . ? C30 O1 Y 129.3(9) . . ? C34 O2 C31 105.1(11) . . ? C34 O2 Y 131.7(9) . . ? C31 O2 Y 122.9(9) . . ? C3 N1 C1 112.3(10) . . ? C3 N1 Y 139.2(8) . . ? C1 N1 Y 108.2(8) . . ? C15 N2 C2 109.4(11) . . ? C15 N2 Y 138.9(8) . . ? C2 N2 Y 110.5(8) . . ? N1 C1 C2 113.4(12) . . ? N2 C2 C1 112.8(12) . . ? C8 C3 N1 121.5(13) . . ? C8 C3 C4 119.4(12) . . ? N1 C3 C4 119.0(12) . . ? C5 C4 C3 119.3(14) . . ? C5 C4 C9 117.2(15) . . ? C3 C4 C9 123.4(12) . . ? C4 C5 C6 118.3(17) . . ? C7 C6 C5 120.1(16) . . ? C6 C7 C8 125.3(17) . . ? C7 C8 C3 117.4(15) . . ? C7 C8 C12 120.8(15) . . ? C3 C8 C12 121.8(13) . . ? C10 C9 C4 114.6(13) . . ? C10 C9 C11 110.6(15) . . ? C4 C9 C11 111.7(14) . . ? C14 C12 C8 114.4(14) . . ? C14 C12 C13 110.0(14) . . ? C8 C12 C13 109.4(14) . . ? C20 C15 C16 119.6(14) . . ? C20 C15 N2 120.0(14) . . ? C16 C15 N2 120.4(12) . . ? C17 C16 C15 117.7(14) . . ? C17 C16 C21 119.3(15) . . ? C15 C16 C21 123.0(13) . . ? C16 C17 C18 124.5(18) . . ? C19 C18 C17 115.3(17) . . ? C18 C19 C20 126.6(18) . . ? C19 C20 C15 116.3(17) . . ? C19 C20 C24 121.3(16) . . ? C15 C20 C24 122.4(16) . . ? C16 C21 C23 112.7(15) . . ? C16 C21 C22 112.9(14) . . ? C23 C21 C22 110.5(16) . . ? C20 C24 C26 116(2) . . ? C20 C24 C25 112.8(18) . . ? C26 C24 C25 107.5(18) . . ? O1 C27 C28A 104.5(16) . . ? O1 C27 C28 100.8(18) . . ? C28A C27 C28 78(2) . . ? O1 C30 C29 108(2) . . ? O1 C30 C29A 99.9(17) . . ? C29 C30 C29A 82(2) . . ? O2 C31 C32 105.1(14) . . ? C31 C32 C33 104.2(15) . . ? C34 C33 C32 104.4(15) . . ? O2 C34 C33 108.9(14) . . ? C29 C28 C27 106(3) . . ? C30 C29 C28 102(3) . . ? C29A C28A C27 102(2) . . ? C28A C29A C30 110(3) . . ? Y1B I1B Y1B 103.33(4) . 2_456 ? N2B Y1B N1B 78.7(4) . . ? N2B Y1B O2B 100.4(3) . . ? N1B Y1B O2B 97.3(3) . . ? N2B Y1B O1B 167.8(3) . . ? N1B Y1B O1B 89.3(4) . . ? O2B Y1B O1B 78.3(3) . . ? N2B Y1B I1B 99.7(2) . . ? N1B Y1B I1B 107.5(3) . . ? O2B Y1B I1B 150.6(2) . . ? O1B Y1B I1B 86.4(2) . . ? N2B Y1B I1B 101.6(3) . 2_456 ? N1B Y1B I1B 175.7(3) . 2_456 ? O2B Y1B I1B 78.4(2) . 2_456 ? O1B Y1B I1B 90.1(2) . 2_456 ? I1B Y1B I1B 76.67(4) . 2_456 ? C30B O1B C27B 104.9(11) . . ? C30B O1B Y1B 131.7(9) . . ? C27B O1B Y1B 123.2(8) . . ? C31B O2B C34B 105.2(10) . . ? C31B O2B Y1B 129.9(8) . . ? C34B O2B Y1B 123.8(7) . . ? C3B N1B C1B 110.4(10) . . ? C3B N1B Y1B 135.8(8) . . ? C1B N1B Y1B 113.4(8) . . ? C15B N2B C2B 112.7(10) . . ? C15B N2B Y1B 137.7(8) . . ? C2B N2B Y1B 109.2(7) . . ? N1B C1B C2B 110.5(11) . . ? N2B C2B C1B 112.9(10) . . ? N1B C3B C4B 121.5(11) . . ? N1B C3B C8B 121.8(11) . . ? C4B C3B C8B 116.7(12) . . ? C5B C4B C3B 120.1(12) . . ? C5B C4B C9B 119.9(12) . . ? C3B C4B C9B 119.9(12) . . ? C4B C5B C6B 121.0(13) . . ? C7B C6B C5B 119.6(13) . . ? C8B C7B C6B 122.0(13) . . ? C7B C8B C3B 120.5(13) . . ? C7B C8B C12B 120.0(13) . . ? C3B C8B C12B 119.5(13) . . ? C10B C9B C4B 112.7(12) . . ? C10B C9B C11B 108.2(12) . . ? C4B C9B C11B 110.4(12) . . ? C14B C12B C8B 113.7(14) . . ? C14B C12B C13B 108.6(14) . . ? C8B C12B C13B 108.7(13) . . ? C20B C15B N2B 120.7(12) . . ? C20B C15B C16B 118.1(12) . . ? N2B C15B C16B 121.2(12) . . ? C17B C16B C15B 118.4(14) . . ? C17B C16B C21B 121.6(14) . . ? C15B C16B C21B 119.9(12) . . ? C18B C17B C16B 121.8(15) . . ? C17B C18B C19B 123.0(14) . . ? C18B C19B C20B 119.5(14) . . ? C15B C20B C19B 119.2(14) . . ? C15B C20B C24B 122.6(12) . . ? C19B C20B C24B 118.2(13) . . ? C16B C21B C23B 113.7(13) . . ? C16B C21B C22B 109.5(12) . . ? C23B C21B C22B 110.8(12) . . ? C20B C24B C26B 112.2(13) . . ? C20B C24B C25B 112.3(13) . . ? C26B C24B C25B 108.2(13) . . ? O1B C27B C28B 105.5(12) . . ? C27B C28B C29B 102.2(13) . . ? C30B C29B C28B 106.4(14) . . ? O1B C30B C29B 107.6(14) . . ? O2B C31B C32B 103.2(14) . . ? C33B C32B C31B 104.3(15) . . ? C34B C33B C32B 105.4(14) . . ? O2B C34B C33B 106.3(12) . . ? C2C C1C C6C 120 . . ? C2C C1C C7C 119.8(7) . . ? C6C C1C C7C 120.0(6) . . ? C3C C2C C1C 120 . . ? C2C C3C C4C 120 . . ? C5C C4C C3C 120 . . ? C6C C5C C4C 120 . . ? C5C C6C C1C 120 . . ? C13C C8C C9C 120 . . ? C13C C8C C14C 119.9(8) . . ? C9C C8C C14C 120.0(8) . . ? C10C C9C C8C 120 . . ? C9C C10C C11C 120 . . ? C12C C11C C10C 120 . . ? C13C C12C C11C 120 . . ? C12C C13C C8C 120 . . ? C16C C15C C18C 124.5(13) . . ? C17C C15C C19C 122.3(13) . . ? C16C C15C C15C 109(2) . 2_566 ? C18C C15C C15C 127(2) . 2_566 ? C17C C15C C19C 117.1(18) . 2_566 ? C19C C15C C19C 120.4(19) . 2_566 ? C19C C16C C17C 129(2) 2_566 . ? C18C C17C C16C 117.4(12) . . ? C19C C18C C17C 119.7(13) . . ? C16C C19C C15C 114(2) 2_566 . ? C18C C19C C15C 118.7(18) . 2_566 ? #'[Y(thf){CH(SiMe3)2}{C6H3iPr2NCH2CH2NC6H3iPr2}].1/2(pentane)' [11] data_dec602 _database_code_depnum_ccdc_archive 'CCDC 228148' _audit_creation_date 2002-12-13T09:51:45-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common (Y(thf)(CH(SiMe3)2)(C6H3iPr2NCH2CH2NC6H3iPr2)).1/2(pentane) _chemical_formula_moiety '(C37 H65 N2 O1 Si2 Y1).1/2(C5 H12)' _chemical_formula_sum 'C39.5 H71 N2 O Si2 Y' _chemical_formula_weight 735.07 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.5573(2) _cell_length_b 17.9434(3) _cell_length_c 19.4501(3) _cell_angle_alpha 90 _cell_angle_beta 99.444(1) _cell_angle_gamma 90 _cell_volume 4323.11(12) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 20312 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.129 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1588 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.433 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.8258 _exptl_absorpt_correction_T_max 0.9733 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.115 _diffrn_reflns_av_unetI/netI 0.0741 _diffrn_reflns_number 44698 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.78 _diffrn_reflns_theta_max 25.02 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _reflns_number_total 7568 _reflns_number_gt 5579 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The pentane solvent is disordered across an inversion centre and was refined with isotropic C atoms,no H atoms, fixed bond lengths,1,3 distance constraints. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0313P)^2^+9.6290P] 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 'riding; omitted for solvate' _refine_ls_extinction_method none _refine_ls_number_reflns 7568 _refine_ls_number_parameters 408 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0921 _refine_ls_R_factor_gt 0.0575 _refine_ls_wR_factor_ref 0.1207 _refine_ls_wR_factor_gt 0.1085 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.984 _refine_diff_density_min -0.447 _refine_diff_density_rms 0.078 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Y Y 0.02855(3) 0.22873(2) 0.228101(19) 0.01848(12) Uani 1 1 d . . . Si1 Si -0.10535(10) 0.08920(7) 0.13956(6) 0.0278(3) Uani 1 1 d . . . Si2 Si -0.03592(11) 0.20423(7) 0.03226(6) 0.0329(3) Uani 1 1 d . . . O O 0.1922(2) 0.16706(16) 0.26000(15) 0.0320(7) Uani 1 1 d . . . N1 N 0.0690(3) 0.34513(18) 0.23605(16) 0.0219(7) Uani 1 1 d . . . N2 N -0.0351(3) 0.25656(17) 0.32264(16) 0.0219(7) Uani 1 1 d . . . C1 C 0.0752(4) 0.3688(2) 0.3090(2) 0.0303(10) Uani 1 1 d . . . H1A H 0.0687 0.4238 0.3106 0.036 Uiso 1 1 calc R . . H1B H 0.1468 0.355 0.3353 0.036 Uiso 1 1 calc R . . C2 C -0.0120(4) 0.3341(2) 0.3439(2) 0.0336(11) Uani 1 1 d . . . H2A H 0.0109 0.3359 0.3951 0.04 Uiso 1 1 calc R . . H2B H -0.0789 0.3639 0.3324 0.04 Uiso 1 1 calc R . . C3 C 0.0841(3) 0.4012(2) 0.18685(19) 0.0205(9) Uani 1 1 d . . . C4 C 0.1840(3) 0.4070(2) 0.1626(2) 0.0227(9) Uani 1 1 d . . . C5 C 0.1943(4) 0.4582(2) 0.1098(2) 0.0299(10) Uani 1 1 d . . . H5 H 0.2609 0.4613 0.0929 0.036 Uiso 1 1 calc R . . C6 C 0.1108(4) 0.5038(2) 0.0818(2) 0.0336(11) Uani 1 1 d . . . H6 H 0.1193 0.538 0.0459 0.04 Uiso 1 1 calc R . . C7 C 0.0136(3) 0.4992(2) 0.1068(2) 0.0299(10) Uani 1 1 d . . . H7 H -0.0441 0.5312 0.0879 0.036 Uiso 1 1 calc R . . C8 C -0.0012(3) 0.4490(2) 0.1585(2) 0.0260(9) Uani 1 1 d . . . C9 C 0.2797(3) 0.3603(2) 0.1952(2) 0.0299(10) Uani 1 1 d . . . H9 H 0.2505 0.3157 0.2166 0.036 Uiso 1 1 calc R . . C10 C 0.3495(5) 0.3321(4) 0.1442(3) 0.077(2) Uani 1 1 d . . . H10A H 0.3791 0.3745 0.1218 0.115 Uiso 1 1 calc R . . H10B H 0.3056 0.3014 0.1086 0.115 Uiso 1 1 calc R . . H10C H 0.4087 0.3021 0.1691 0.115 Uiso 1 1 calc R . . C11 C 0.3481(5) 0.4038(4) 0.2543(3) 0.0699(18) Uani 1 1 d . . . H11A H 0.3041 0.4161 0.2899 0.105 Uiso 1 1 calc R . . H11B H 0.3741 0.4499 0.2357 0.105 Uiso 1 1 calc R . . H11C H 0.4099 0.3734 0.275 0.105 Uiso 1 1 calc R . . C12 C -0.1104(3) 0.4454(3) 0.1833(2) 0.0327(11) Uani 1 1 d . . . H12 H -0.1084 0.4015 0.2152 0.039 Uiso 1 1 calc R . . C13 C -0.1313(4) 0.5137(3) 0.2246(3) 0.0556(15) Uani 1 1 d . . . H13A H -0.1312 0.5581 0.1953 0.083 Uiso 1 1 calc R . . H13B H -0.0746 0.5183 0.2655 0.083 Uiso 1 1 calc R . . H13C H -0.2016 0.5089 0.2399 0.083 Uiso 1 1 calc R . . C14 C -0.2043(4) 0.4331(4) 0.1234(3) 0.0610(16) Uani 1 1 d . . . H14A H -0.1933 0.3862 0.0995 0.092 Uiso 1 1 calc R . . H14B H -0.2074 0.4745 0.0903 0.092 Uiso 1 1 calc R . . H14C H -0.2722 0.4306 0.1419 0.092 Uiso 1 1 calc R . . C15 C -0.1082(3) 0.2225(2) 0.36204(19) 0.0232(9) Uani 1 1 d . . . C16 C -0.0685(3) 0.1775(2) 0.4206(2) 0.0301(10) Uani 1 1 d . . . C17 C -0.1403(4) 0.1437(3) 0.4575(2) 0.0377(12) Uani 1 1 d . . . H17 H -0.1133 0.112 0.4955 0.045 Uiso 1 1 calc R . . C18 C -0.2507(4) 0.1549(3) 0.4404(2) 0.0379(12) Uani 1 1 d . . . H18 H -0.299 0.1323 0.467 0.046 Uiso 1 1 calc R . . C19 C -0.2888(4) 0.1993(3) 0.3842(2) 0.0333(11) Uani 1 1 d . . . H19 H -0.3645 0.207 0.3722 0.04 Uiso 1 1 calc R . . C20 C -0.2206(3) 0.2334(2) 0.3442(2) 0.0263(9) Uani 1 1 d . . . C21 C 0.0530(4) 0.1674(3) 0.4445(3) 0.0488(14) Uani 1 1 d . . . H21 H 0.0909 0.1928 0.4097 0.059 Uiso 1 1 calc R . . C22 C 0.0905(5) 0.2042(4) 0.5152(3) 0.076(2) Uani 1 1 d . . . H22A H 0.0537 0.181 0.5504 0.113 Uiso 1 1 calc R . . H22B H 0.0732 0.2575 0.5121 0.113 Uiso 1 1 calc R . . H22C H 0.1687 0.1978 0.5285 0.113 Uiso 1 1 calc R . . C23 C 0.0854(5) 0.0862(4) 0.4467(3) 0.0720(19) Uani 1 1 d . . . H23A H 0.05 0.0599 0.481 0.108 Uiso 1 1 calc R . . H23B H 0.1639 0.0822 0.46 0.108 Uiso 1 1 calc R . . H23C H 0.0632 0.0639 0.4006 0.108 Uiso 1 1 calc R . . C24 C -0.2685(3) 0.2807(2) 0.2819(2) 0.0333(10) Uani 1 1 d . . . H24 H -0.2073 0.3005 0.2602 0.04 Uiso 1 1 calc R . . C25 C -0.3407(4) 0.2347(3) 0.2269(3) 0.0516(13) Uani 1 1 d . . . H25A H -0.4007 0.2138 0.2471 0.077 Uiso 1 1 calc R . . H25B H -0.2985 0.1942 0.211 0.077 Uiso 1 1 calc R . . H25C H -0.3692 0.2667 0.1873 0.077 Uiso 1 1 calc R . . C26 C -0.3303(5) 0.3476(3) 0.3047(3) 0.0616(16) Uani 1 1 d . . . H26A H -0.2813 0.3782 0.3376 0.092 Uiso 1 1 calc R . . H26B H -0.3898 0.3298 0.3273 0.092 Uiso 1 1 calc R . . H26C H -0.3594 0.3775 0.2638 0.092 Uiso 1 1 calc R . . C27 C -0.0732(3) 0.1853(2) 0.1180(2) 0.0257(9) Uani 1 1 d . . . H27 H -0.144 0.2115 0.1155 0.031 Uiso 1 1 calc R . . C28 C -0.0221(4) 0.0173(3) 0.1038(2) 0.0403(12) Uani 1 1 d . . . H28A H 0.0543 0.0256 0.1222 0.06 Uiso 1 1 calc R . . H28B H -0.0336 0.0209 0.0528 0.06 Uiso 1 1 calc R . . H28C H -0.0434 -0.0324 0.1175 0.06 Uiso 1 1 calc R . . C29 C -0.0748(4) 0.0766(2) 0.2378(2) 0.0322(11) Uani 1 1 d . . . H29A H -0.1195 0.1109 0.26 0.048 Uiso 1 1 calc R . . H29B H 0.0017 0.0872 0.2544 0.048 Uiso 1 1 calc R . . H29C H -0.0909 0.0252 0.2496 0.048 Uiso 1 1 calc R . . C30 C -0.2498(4) 0.0635(3) 0.1110(3) 0.0484(13) Uani 1 1 d . . . H30A H -0.2682 0.0686 0.0603 0.073 Uiso 1 1 calc R . . H30B H -0.2958 0.0966 0.1335 0.073 Uiso 1 1 calc R . . H30C H -0.2613 0.0118 0.1243 0.073 Uiso 1 1 calc R . . C31 C -0.0400(5) 0.3062(3) 0.0119(2) 0.0473(13) Uani 1 1 d . . . H31A H 0.0105 0.3327 0.0474 0.071 Uiso 1 1 calc R . . H31B H -0.1132 0.3252 0.0116 0.071 Uiso 1 1 calc R . . H31C H -0.0193 0.3142 -0.034 0.071 Uiso 1 1 calc R . . C32 C 0.1038(4) 0.1714(3) 0.0264(3) 0.0596(16) Uani 1 1 d . . . H32A H 0.1084 0.1175 0.0343 0.089 Uiso 1 1 calc R . . H32B H 0.1557 0.1968 0.0618 0.089 Uiso 1 1 calc R . . H32C H 0.1204 0.1828 -0.02 0.089 Uiso 1 1 calc R . . C33 C -0.1291(5) 0.1596(3) -0.0423(2) 0.0537(15) Uani 1 1 d . . . H33A H -0.2026 0.1785 -0.0434 0.08 Uiso 1 1 calc R . . H33B H -0.1285 0.1055 -0.036 0.08 Uiso 1 1 calc R . . H33C H -0.1047 0.1718 -0.0863 0.08 Uiso 1 1 calc R . . C34 C 0.2691(4) 0.1830(3) 0.3229(2) 0.0443(13) Uani 1 1 d . . . H34A H 0.2601 0.1477 0.3606 0.053 Uiso 1 1 calc R . . H34B H 0.2599 0.2345 0.3392 0.053 Uiso 1 1 calc R . . C35 C 0.3777(4) 0.1735(3) 0.3010(3) 0.0443(13) Uani 1 1 d . . . H35A H 0.432 0.1563 0.3406 0.053 Uiso 1 1 calc R . . H35B H 0.4026 0.2209 0.2831 0.053 Uiso 1 1 calc R . . C36 C 0.3589(4) 0.1156(4) 0.2446(3) 0.0671(18) Uani 1 1 d . . . H36A H 0.4017 0.1271 0.2074 0.081 Uiso 1 1 calc R . . H36B H 0.38 0.0656 0.2638 0.081 Uiso 1 1 calc R . . C37 C 0.2444(5) 0.1178(4) 0.2173(4) 0.078(2) Uani 1 1 d . . . H37A H 0.2329 0.136 0.1686 0.094 Uiso 1 1 calc R . . H37B H 0.2133 0.0671 0.2177 0.094 Uiso 1 1 calc R . . C38 C -0.6113(15) 0.0755(11) 0.0579(10) 0.113(6) Uiso 0.5 1 d PD . . C39 C -0.5405(15) 0.0568(9) 0.0068(10) 0.124(7) Uiso 0.5 1 d PD . . C40 C -0.5009(10) -0.0212(6) 0.0160(6) 0.062(3) Uiso 0.5 1 d PD . . C41 C -0.4340(15) -0.0395(9) -0.0444(9) 0.106(6) Uiso 0.5 1 d PD . . C42 C -0.4144(15) -0.1232(10) -0.0452(10) 0.118(6) Uiso 0.5 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y 0.0185(2) 0.0196(2) 0.01737(19) -0.00011(17) 0.00299(14) 0.00074(18) Si1 0.0301(7) 0.0277(7) 0.0242(6) -0.0041(5) 0.0007(5) -0.0043(5) Si2 0.0449(8) 0.0322(7) 0.0210(6) 0.0018(5) 0.0034(6) 0.0053(6) O 0.0189(15) 0.0339(17) 0.0413(18) -0.0028(14) -0.0008(13) 0.0048(13) N1 0.0238(18) 0.0213(18) 0.0210(18) 0.0017(14) 0.0051(15) -0.0041(14) N2 0.0221(17) 0.0228(19) 0.0215(17) -0.0014(14) 0.0053(14) -0.0018(14) C1 0.038(3) 0.032(3) 0.019(2) -0.0012(18) 0.0020(19) -0.012(2) C2 0.046(3) 0.030(3) 0.027(2) -0.0045(19) 0.013(2) -0.009(2) C3 0.022(2) 0.019(2) 0.019(2) -0.0034(17) -0.0007(17) -0.0045(17) C4 0.023(2) 0.022(2) 0.023(2) 0.0002(17) 0.0013(18) -0.0024(17) C5 0.031(2) 0.032(3) 0.027(2) 0.0020(19) 0.007(2) -0.005(2) C6 0.045(3) 0.028(2) 0.026(2) 0.0076(19) 0.001(2) -0.001(2) C7 0.030(2) 0.025(2) 0.032(2) 0.0029(19) -0.002(2) 0.0048(19) C8 0.027(2) 0.023(2) 0.027(2) -0.0052(18) 0.0026(19) -0.0007(18) C9 0.022(2) 0.036(3) 0.032(2) 0.005(2) 0.0044(19) -0.0035(19) C10 0.073(4) 0.106(5) 0.054(4) 0.016(4) 0.018(3) 0.055(4) C11 0.049(4) 0.087(5) 0.064(4) 0.000(3) -0.019(3) 0.005(3) C12 0.022(2) 0.036(3) 0.040(3) 0.001(2) 0.004(2) 0.003(2) C13 0.043(3) 0.064(4) 0.063(4) -0.021(3) 0.018(3) -0.004(3) C14 0.029(3) 0.089(5) 0.064(4) -0.020(3) 0.003(3) -0.008(3) C15 0.026(2) 0.023(2) 0.022(2) -0.0040(18) 0.0105(18) 0.0012(18) C16 0.032(2) 0.036(3) 0.024(2) 0.0044(19) 0.011(2) 0.005(2) C17 0.041(3) 0.045(3) 0.029(3) 0.010(2) 0.012(2) 0.005(2) C18 0.039(3) 0.043(3) 0.036(3) 0.002(2) 0.020(2) -0.009(2) C19 0.023(2) 0.043(3) 0.035(3) -0.004(2) 0.009(2) -0.002(2) C20 0.025(2) 0.028(2) 0.026(2) -0.0053(19) 0.0048(18) 0.000(2) C21 0.036(3) 0.075(4) 0.039(3) 0.031(3) 0.015(2) 0.020(3) C22 0.049(4) 0.074(5) 0.091(5) -0.009(4) -0.025(3) 0.005(3) C23 0.059(4) 0.091(5) 0.061(4) -0.010(4) -0.002(3) 0.039(4) C24 0.025(2) 0.037(3) 0.037(3) 0.004(2) 0.002(2) 0.004(2) C25 0.044(3) 0.068(4) 0.038(3) 0.005(3) -0.005(2) 0.001(3) C26 0.059(4) 0.050(4) 0.074(4) 0.010(3) 0.006(3) 0.024(3) C27 0.028(2) 0.027(2) 0.020(2) -0.0034(18) -0.0024(18) 0.0025(19) C28 0.053(3) 0.030(3) 0.037(3) -0.003(2) 0.007(2) -0.002(2) C29 0.040(3) 0.026(2) 0.032(3) -0.0005(19) 0.008(2) -0.014(2) C30 0.036(3) 0.056(3) 0.048(3) -0.003(3) -0.007(2) -0.014(3) C31 0.075(4) 0.039(3) 0.029(3) 0.006(2) 0.012(3) 0.000(3) C32 0.060(4) 0.069(4) 0.056(4) 0.019(3) 0.029(3) 0.013(3) C33 0.087(4) 0.048(3) 0.021(3) -0.002(2) -0.004(3) 0.002(3) C34 0.027(3) 0.073(4) 0.029(3) -0.004(2) -0.007(2) 0.008(2) C35 0.022(2) 0.061(4) 0.047(3) 0.009(3) -0.001(2) 0.001(2) C36 0.041(3) 0.109(5) 0.051(4) -0.014(3) 0.006(3) 0.025(3) C37 0.052(4) 0.082(5) 0.097(5) -0.051(4) 0.003(4) 0.022(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Y N1 2.149(3) . ? Y N2 2.180(3) . ? Y O 2.327(3) . ? Y C27 2.434(4) . ? Si1 C27 1.835(4) . ? Si1 C28 1.865(5) . ? Si1 C30 1.866(5) . ? Si1 C29 1.900(4) . ? Si2 C27 1.837(4) . ? Si2 C31 1.871(5) . ? Si2 C32 1.872(5) . ? Si2 C33 1.886(5) . ? O C37 1.442(6) . ? O C34 1.457(5) . ? N1 C3 1.422(5) . ? N1 C1 1.471(5) . ? N2 C15 1.426(5) . ? N2 C2 1.467(5) . ? C1 C2 1.514(6) . ? C3 C8 1.413(6) . ? C3 C4 1.414(5) . ? C4 C5 1.398(6) . ? C4 C9 1.517(6) . ? C5 C6 1.370(6) . ? C6 C7 1.387(6) . ? C7 C8 1.385(6) . ? C8 C12 1.529(6) . ? C9 C10 1.515(6) . ? C9 C11 1.530(7) . ? C12 C13 1.511(6) . ? C12 C14 1.532(6) . ? C15 C20 1.411(5) . ? C15 C16 1.418(6) . ? C16 C17 1.381(6) . ? C16 C21 1.531(6) . ? C17 C18 1.387(6) . ? C18 C19 1.374(6) . ? C19 C20 1.389(6) . ? C20 C24 1.520(6) . ? C21 C23 1.511(8) . ? C21 C22 1.528(8) . ? C24 C25 1.526(7) . ? C24 C26 1.534(7) . ? C34 C35 1.502(6) . ? C35 C36 1.502(7) . ? C36 C37 1.449(7) . ? C38 C39 1.476(15) . ? C39 C40 1.486(15) . ? C40 C41 1.587(15) . ? C41 C42 1.522(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Y N2 80.32(12) . . ? N1 Y O 104.78(11) . . ? N2 Y O 108.31(11) . . ? N1 Y C27 117.26(13) . . ? N2 Y C27 127.08(13) . . ? O Y C27 113.29(12) . . ? C27 Si1 C28 114.0(2) . . ? C27 Si1 C30 113.8(2) . . ? C28 Si1 C30 107.2(2) . . ? C27 Si1 C29 109.01(18) . . ? C28 Si1 C29 105.1(2) . . ? C30 Si1 C29 107.2(2) . . ? C27 Si2 C31 111.8(2) . . ? C27 Si2 C32 112.2(2) . . ? C31 Si2 C32 106.7(3) . . ? C27 Si2 C33 113.7(2) . . ? C31 Si2 C33 105.1(2) . . ? C32 Si2 C33 106.8(3) . . ? C37 O C34 107.6(4) . . ? C37 O Y 127.1(3) . . ? C34 O Y 124.4(3) . . ? C3 N1 C1 116.9(3) . . ? C3 N1 Y 134.0(2) . . ? C1 N1 Y 109.0(2) . . ? C15 N2 C2 111.7(3) . . ? C15 N2 Y 135.5(2) . . ? C2 N2 Y 111.8(2) . . ? N1 C1 C2 112.7(3) . . ? N2 C2 C1 112.9(3) . . ? C8 C3 C4 118.8(4) . . ? C8 C3 N1 121.1(3) . . ? C4 C3 N1 120.1(3) . . ? C5 C4 C3 119.2(4) . . ? C5 C4 C9 120.5(4) . . ? C3 C4 C9 120.3(3) . . ? C6 C5 C4 121.8(4) . . ? C5 C6 C7 119.0(4) . . ? C8 C7 C6 121.5(4) . . ? C7 C8 C3 119.7(4) . . ? C7 C8 C12 119.5(4) . . ? C3 C8 C12 120.8(4) . . ? C10 C9 C4 114.5(4) . . ? C10 C9 C11 110.4(4) . . ? C4 C9 C11 109.9(4) . . ? C13 C12 C8 112.1(4) . . ? C13 C12 C14 110.1(4) . . ? C8 C12 C14 112.5(4) . . ? C20 C15 C16 118.8(4) . . ? C20 C15 N2 121.0(4) . . ? C16 C15 N2 120.2(3) . . ? C17 C16 C15 119.6(4) . . ? C17 C16 C21 119.5(4) . . ? C15 C16 C21 120.9(4) . . ? C16 C17 C18 121.6(4) . . ? C19 C18 C17 118.6(4) . . ? C18 C19 C20 122.3(4) . . ? C19 C20 C15 119.1(4) . . ? C19 C20 C24 119.5(4) . . ? C15 C20 C24 121.4(4) . . ? C23 C21 C22 110.5(4) . . ? C23 C21 C16 111.9(5) . . ? C22 C21 C16 111.5(4) . . ? C20 C24 C25 111.7(4) . . ? C20 C24 C26 111.1(4) . . ? C25 C24 C26 110.8(4) . . ? Si1 C27 Si2 118.6(2) . . ? Si1 C27 Y 101.75(17) . . ? Si2 C27 Y 124.4(2) . . ? O C34 C35 104.4(4) . . ? C34 C35 C36 104.1(4) . . ? C37 C36 C35 106.0(4) . . ? O C37 C36 108.9(5) . . ? C38 C39 C40 111.2(14) . . ? C39 C40 C41 108.3(10) . . ? C42 C41 C40 108.5(12) . . ? #===END #===END data_[Y3{ArNH(CH2)2NAr}2{ArN(CH2)2NAr}(mu-H)3(mu3-H)2(THF)]_[14] _database_code_depnum_ccdc_archive 'CCDC 228149' _audit_creation_date 2003-04-10T17:36:11-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C87 H141 N6 O1 Y3' _chemical_formula_sum 'C87 H141 N6 O1 Y3' _chemical_formula_weight 1553.79 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_Int_Tables_number 14 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 25.4497(7) _cell_length_b 14.2389(3) _cell_length_c 25.1449(5) _cell_angle_alpha 90 _cell_angle_beta 105.140(1) _cell_angle_gamma 90 _cell_volume 8795.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 41601 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 24.108 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.173 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3320 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.007 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.8511 _exptl_absorpt_correction_T_max 0.9663 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.25549E-1 _diffrn_orient_matrix_ub_12 -0.549283E-1 _diffrn_orient_matrix_ub_13 0.89928E-2 _diffrn_orient_matrix_ub_21 0.132827E-1 _diffrn_orient_matrix_ub_22 0.12859E-1 _diffrn_orient_matrix_ub_23 -0.330651E-1 _diffrn_orient_matrix_ub_31 0.294654E-1 _diffrn_orient_matrix_ub_32 0.418306E-1 _diffrn_orient_matrix_ub_33 0.219729E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.1862 _diffrn_reflns_av_unetI/netI 0.1717 _diffrn_reflns_number 41296 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.74 _diffrn_reflns_theta_max 24.13 _diffrn_reflns_theta_full 24.13 _diffrn_measured_fraction_theta_full 0.953 _diffrn_measured_fraction_theta_max 0.953 _reflns_number_total 13369 _reflns_number_gt 7396 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Very weak higher angle data. The five hydride hydrogens and two hydrogens on N were refined isotropic; other H atoms were riding. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0266P)^2^+39.4813P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 13369 _refine_ls_number_parameters 902 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.173 _refine_ls_R_factor_gt 0.0843 _refine_ls_wR_factor_ref 0.1724 _refine_ls_wR_factor_gt 0.1396 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.811 _refine_diff_density_min -0.545 _refine_diff_density_rms 0.099 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Y1 Y 0.25021(3) 0.54907(6) 0.32399(3) 0.0282(2) Uani 1 1 d . . . H1X H 0.183(2) 0.534(4) 0.362(2) 0.011(16) Uiso 1 1 d . . . H2X H 0.239(2) 0.304(4) 0.413(2) 0.001(15) Uiso 1 1 d . . . H3X H 0.311(3) 0.442(5) 0.329(3) 0.03(2) Uiso 1 1 d . . . H4X H 0.218(3) 0.401(5) 0.332(3) 0.05(2) Uiso 1 1 d . . . H5X H 0.270(4) 0.450(7) 0.390(4) 0.10(4) Uiso 1 1 d . . . Y2 Y 0.30456(3) 0.33384(6) 0.37667(3) 0.0264(2) Uani 1 1 d . . . Y3 Y 0.18145(3) 0.40849(6) 0.39677(3) 0.0295(2) Uani 1 1 d . . . O O 0.2742(2) 0.2015(4) 0.3194(2) 0.0363(15) Uani 1 1 d . . . N1 N 0.2202(3) 0.6162(5) 0.2437(3) 0.0327(17) Uani 1 1 d . . . N2 N 0.2964(3) 0.6802(5) 0.3413(3) 0.0341(18) Uani 1 1 d . . . N3 N 0.3943(3) 0.2648(5) 0.3632(3) 0.0336(18) Uani 1 1 d . . . H3N H 0.396(3) 0.219(5) 0.388(3) 0.03(2) Uiso 1 1 d . . . N4 N 0.3705(3) 0.3287(5) 0.4543(2) 0.0269(16) Uani 1 1 d . . . N5 N 0.1043(3) 0.3370(5) 0.3589(3) 0.0351(17) Uani 1 1 d . . . N6 N 0.1051(3) 0.4959(6) 0.4295(3) 0.038(2) Uani 1 1 d . . . H6N H 0.094(4) 0.541(6) 0.405(4) 0.05(3) Uiso 1 1 d . . . C1 C 0.2580(5) 0.6928(8) 0.2414(4) 0.075(4) Uani 1 1 d . . . H1B H 0.2836 0.6695 0.2207 0.09 Uiso 1 1 calc R . . H1A H 0.2366 0.744 0.2193 0.09 Uiso 1 1 calc R . . C2 C 0.2887(6) 0.7319(10) 0.2896(4) 0.122(7) Uani 1 1 d . . . H2B H 0.2722 0.7932 0.2942 0.147 Uiso 1 1 calc R . . H2A H 0.3253 0.7451 0.2844 0.147 Uiso 1 1 calc R . . C3 C 0.1734(4) 0.6153(6) 0.1976(3) 0.035(2) Uani 1 1 d . . . C4 C 0.1239(4) 0.6509(7) 0.2034(4) 0.042(2) Uani 1 1 d . . . C5 C 0.0777(4) 0.6440(7) 0.1578(4) 0.056(3) Uani 1 1 d . . . H5 H 0.0436 0.6661 0.1614 0.068 Uiso 1 1 calc R . . C6 C 0.0808(4) 0.6063(8) 0.1083(4) 0.057(3) Uani 1 1 d . . . H6 H 0.0494 0.6024 0.0781 0.068 Uiso 1 1 calc R . . C7 C 0.1302(4) 0.5744(7) 0.1035(4) 0.048(3) Uani 1 1 d . . . H7 H 0.1323 0.5498 0.069 0.058 Uiso 1 1 calc R . . C8 C 0.1776(4) 0.5764(6) 0.1469(4) 0.042(2) Uani 1 1 d . . . C9 C 0.1187(4) 0.6968(7) 0.2555(4) 0.044(3) Uani 1 1 d . . . H9 H 0.1538 0.6867 0.2841 0.053 Uiso 1 1 calc R . . C10 C 0.0737(4) 0.6563(8) 0.2781(4) 0.069(3) Uani 1 1 d . . . H10C H 0.0386 0.6639 0.2507 0.103 Uiso 1 1 calc R . . H10B H 0.0728 0.6895 0.312 0.103 Uiso 1 1 calc R . . H10A H 0.0806 0.5894 0.2861 0.103 Uiso 1 1 calc R . . C11 C 0.1111(5) 0.8043(7) 0.2469(4) 0.069(3) Uani 1 1 d . . . H11C H 0.1427 0.8305 0.2367 0.103 Uiso 1 1 calc R . . H11B H 0.1078 0.8336 0.2811 0.103 Uiso 1 1 calc R . . H11A H 0.0781 0.8166 0.2175 0.103 Uiso 1 1 calc R . . C12 C 0.2300(4) 0.5355(8) 0.1386(3) 0.048(3) Uani 1 1 d . . . H12 H 0.2592 0.5453 0.1735 0.057 Uiso 1 1 calc R . . C13 C 0.2470(5) 0.5864(8) 0.0929(4) 0.073(3) Uani 1 1 d . . . H13C H 0.2185 0.5795 0.0583 0.109 Uiso 1 1 calc R . . H13B H 0.281 0.5595 0.0886 0.109 Uiso 1 1 calc R . . H13A H 0.2524 0.6532 0.1022 0.109 Uiso 1 1 calc R . . C14 C 0.2248(5) 0.4311(8) 0.1277(5) 0.072(3) Uani 1 1 d . . . H14C H 0.216 0.3995 0.1589 0.107 Uiso 1 1 calc R . . H14B H 0.2593 0.4067 0.123 0.107 Uiso 1 1 calc R . . H14A H 0.1958 0.4195 0.0941 0.107 Uiso 1 1 calc R . . C15 C 0.3268(4) 0.7309(6) 0.3881(3) 0.036(2) Uani 1 1 d . . . C16 C 0.2998(5) 0.7787(6) 0.4226(4) 0.048(3) Uani 1 1 d . . . C17 C 0.3307(5) 0.8260(7) 0.4689(4) 0.064(3) Uani 1 1 d . . . H17 H 0.3128 0.8595 0.4917 0.076 Uiso 1 1 calc R . . C18 C 0.3864(5) 0.8251(7) 0.4820(5) 0.067(3) Uani 1 1 d . . . H18 H 0.4064 0.8558 0.5145 0.081 Uiso 1 1 calc R . . C19 C 0.4141(5) 0.7799(7) 0.4485(4) 0.057(3) Uani 1 1 d . . . H19 H 0.4527 0.7803 0.4575 0.068 Uiso 1 1 calc R . . C20 C 0.3833(4) 0.7327(6) 0.4003(4) 0.039(2) Uani 1 1 d . . . C21 C 0.2378(5) 0.7771(8) 0.4103(4) 0.063(3) Uani 1 1 d . . . H21 H 0.2243 0.7404 0.3754 0.075 Uiso 1 1 calc R . . C22 C 0.2131(6) 0.8714(10) 0.3998(8) 0.158(8) Uani 1 1 d . . . H22C H 0.2266 0.9109 0.4324 0.237 Uiso 1 1 calc R . . H22B H 0.1734 0.866 0.3918 0.237 Uiso 1 1 calc R . . H22A H 0.2229 0.8998 0.3682 0.237 Uiso 1 1 calc R . . C23 C 0.2185(6) 0.7252(13) 0.4547(7) 0.138(7) Uani 1 1 d . . . H23C H 0.2293 0.7605 0.4893 0.207 Uiso 1 1 calc R . . H23B H 0.235 0.6626 0.46 0.207 Uiso 1 1 calc R . . H23A H 0.1788 0.7193 0.4433 0.207 Uiso 1 1 calc R . . C24 C 0.4145(4) 0.6795(7) 0.3660(4) 0.054(3) Uani 1 1 d . . . H24 H 0.3887 0.6679 0.3291 0.065 Uiso 1 1 calc R . . C25 C 0.4622(7) 0.7326(11) 0.3565(9) 0.165(9) Uani 1 1 d . . . H25C H 0.4893 0.7419 0.3917 0.248 Uiso 1 1 calc R . . H25B H 0.4499 0.7938 0.34 0.248 Uiso 1 1 calc R . . H25A H 0.4784 0.6967 0.3316 0.248 Uiso 1 1 calc R . . C26 C 0.4327(7) 0.5878(8) 0.3901(5) 0.119(6) Uani 1 1 d . . . H26C H 0.4504 0.5535 0.3658 0.179 Uiso 1 1 calc R . . H26B H 0.4012 0.5518 0.3945 0.179 Uiso 1 1 calc R . . H26A H 0.4585 0.5965 0.4262 0.179 Uiso 1 1 calc R . . C27 C 0.4369(3) 0.3226(6) 0.4009(3) 0.037(2) Uani 1 1 d . . . H27B H 0.4343 0.3886 0.3882 0.045 Uiso 1 1 calc R . . H27A H 0.4735 0.2985 0.4015 0.045 Uiso 1 1 calc R . . C28 C 0.4279(3) 0.3170(7) 0.4573(3) 0.039(2) Uani 1 1 d . . . H28B H 0.4406 0.2553 0.474 0.046 Uiso 1 1 calc R . . H28A H 0.4493 0.3666 0.481 0.046 Uiso 1 1 calc R . . C29 C 0.4102(3) 0.2209(6) 0.3178(3) 0.031(2) Uani 1 1 d . . . C30 C 0.4187(3) 0.2744(6) 0.2745(3) 0.031(2) Uani 1 1 d . . . C31 C 0.4345(3) 0.2263(7) 0.2331(3) 0.039(2) Uani 1 1 d . . . H31 H 0.4408 0.2611 0.2032 0.046 Uiso 1 1 calc R . . C32 C 0.4412(4) 0.1311(8) 0.2336(4) 0.051(3) Uani 1 1 d . . . H32 H 0.4525 0.1008 0.2048 0.061 Uiso 1 1 calc R . . C33 C 0.4316(4) 0.0801(7) 0.2760(4) 0.053(3) Uani 1 1 d . . . H33 H 0.4358 0.0138 0.276 0.063 Uiso 1 1 calc R . . C34 C 0.4159(4) 0.1223(7) 0.3191(4) 0.044(2) Uani 1 1 d . . . C35 C 0.4096(4) 0.3796(6) 0.2700(3) 0.040(2) Uani 1 1 d . . . H35 H 0.3957 0.3994 0.302 0.048 Uiso 1 1 calc R . . C36 C 0.4635(4) 0.4323(7) 0.2747(4) 0.060(3) Uani 1 1 d . . . H36C H 0.4776 0.4164 0.2431 0.091 Uiso 1 1 calc R . . H36B H 0.4901 0.4139 0.3089 0.091 Uiso 1 1 calc R . . H36A H 0.4571 0.5001 0.2751 0.091 Uiso 1 1 calc R . . C37 C 0.3675(4) 0.4084(7) 0.2178(4) 0.053(3) Uani 1 1 d . . . H37C H 0.3796 0.3891 0.1856 0.079 Uiso 1 1 calc R . . H37B H 0.3629 0.4768 0.2174 0.079 Uiso 1 1 calc R . . H37A H 0.3326 0.3781 0.2168 0.079 Uiso 1 1 calc R . . C38 C 0.4070(5) 0.0611(7) 0.3656(5) 0.071(4) Uani 1 1 d . . . H38 H 0.3834 0.0985 0.384 0.085 Uiso 1 1 calc R . . C39 C 0.3770(6) -0.0290(10) 0.3472(6) 0.127(6) Uani 1 1 d . . . H39C H 0.3996 -0.0703 0.3312 0.19 Uiso 1 1 calc R . . H39B H 0.3429 -0.0154 0.3196 0.19 Uiso 1 1 calc R . . H39A H 0.369 -0.0601 0.379 0.19 Uiso 1 1 calc R . . C40 C 0.4583(6) 0.0422(10) 0.4086(5) 0.107(5) Uani 1 1 d . . . H40C H 0.4499 0.0101 0.4398 0.16 Uiso 1 1 calc R . . H40B H 0.4768 0.1016 0.421 0.16 Uiso 1 1 calc R . . H40A H 0.482 0.0022 0.3932 0.16 Uiso 1 1 calc R . . C41 C 0.3615(3) 0.3302(6) 0.5083(3) 0.034(2) Uani 1 1 d . . . C42 C 0.3486(4) 0.2467(6) 0.5317(3) 0.038(2) Uani 1 1 d . . . C43 C 0.3375(4) 0.2491(7) 0.5838(4) 0.048(3) Uani 1 1 d . . . H43 H 0.3269 0.1932 0.5988 0.058 Uiso 1 1 calc R . . C44 C 0.3417(4) 0.3319(8) 0.6129(4) 0.050(3) Uani 1 1 d . . . H44 H 0.3342 0.3331 0.6479 0.06 Uiso 1 1 calc R . . C45 C 0.3569(4) 0.4124(7) 0.5912(4) 0.046(3) Uani 1 1 d . . . H45 H 0.3603 0.4689 0.6119 0.055 Uiso 1 1 calc R . . C47 C 0.3481(4) 0.1525(7) 0.5041(4) 0.055(3) Uani 1 1 d . . . H47 H 0.3572 0.1635 0.4683 0.066 Uiso 1 1 calc R . . C48 C 0.2915(5) 0.1048(7) 0.4910(4) 0.076(4) Uani 1 1 d . . . H48C H 0.2811 0.0936 0.5254 0.115 Uiso 1 1 calc R . . H48B H 0.293 0.0448 0.4724 0.115 Uiso 1 1 calc R . . H48A H 0.2645 0.1457 0.467 0.115 Uiso 1 1 calc R . . C49 C 0.3916(5) 0.0859(8) 0.5384(5) 0.084(4) Uani 1 1 d . . . H49C H 0.4277 0.1146 0.544 0.126 Uiso 1 1 calc R . . H49B H 0.3907 0.0262 0.5188 0.126 Uiso 1 1 calc R . . H49A H 0.3843 0.0746 0.5742 0.126 Uiso 1 1 calc R . . C50 C 0.3825(4) 0.5052(6) 0.5167(4) 0.043(2) Uani 1 1 d . . . H50 H 0.3874 0.492 0.4792 0.051 Uiso 1 1 calc R . . C51 C 0.3389(4) 0.5787(7) 0.5102(4) 0.050(3) Uani 1 1 d . . . H51C H 0.3053 0.5558 0.4848 0.076 Uiso 1 1 calc R . . H51B H 0.3507 0.6363 0.4954 0.076 Uiso 1 1 calc R . . H51A H 0.3323 0.5918 0.5462 0.076 Uiso 1 1 calc R . . C52 C 0.4370(4) 0.5453(8) 0.5521(5) 0.073(3) Uani 1 1 d . . . H52C H 0.4338 0.5578 0.5895 0.109 Uiso 1 1 calc R . . H52B H 0.4454 0.6039 0.5356 0.109 Uiso 1 1 calc R . . H52A H 0.4661 0.4997 0.5537 0.109 Uiso 1 1 calc R . . C92 C 0.3676(3) 0.4141(6) 0.5393(3) 0.037(2) Uani 1 1 d . . . C53 C 0.0529(4) 0.3871(8) 0.3566(4) 0.056(3) Uani 1 1 d . . . H53B H 0.0224 0.3417 0.3485 0.068 Uiso 1 1 calc R . . H53A H 0.046 0.4338 0.3264 0.068 Uiso 1 1 calc R . . C54 C 0.0552(4) 0.4358(8) 0.4097(4) 0.057(3) Uani 1 1 d . . . H54B H 0.0543 0.3882 0.4381 0.069 Uiso 1 1 calc R . . H54A H 0.0224 0.4758 0.4049 0.069 Uiso 1 1 calc R . . C55 C 0.0953(3) 0.2563(7) 0.3248(4) 0.038(2) Uani 1 1 d . . . C56 C 0.0983(4) 0.1671(7) 0.3493(4) 0.046(2) Uani 1 1 d . . . C57 C 0.0891(4) 0.0883(8) 0.3148(5) 0.059(3) Uani 1 1 d . . . H57 H 0.0911 0.0278 0.3311 0.07 Uiso 1 1 calc R . . C58 C 0.0774(4) 0.0942(8) 0.2584(5) 0.060(3) Uani 1 1 d . . . H58 H 0.071 0.0395 0.236 0.072 Uiso 1 1 calc R . . C59 C 0.0753(4) 0.1812(8) 0.2359(4) 0.053(3) Uani 1 1 d . . . H59 H 0.0672 0.1864 0.197 0.064 Uiso 1 1 calc R . . C60 C 0.0845(3) 0.2628(6) 0.2670(4) 0.040(2) Uani 1 1 d . . . C61 C 0.1119(4) 0.1554(8) 0.4111(4) 0.057(3) Uani 1 1 d . . . H61 H 0.1356 0.2105 0.4259 0.068 Uiso 1 1 calc R . . C62 C 0.0640(5) 0.1665(13) 0.4341(5) 0.121(6) Uani 1 1 d . . . H62C H 0.0483 0.2293 0.4252 0.182 Uiso 1 1 calc R . . H62B H 0.0755 0.1588 0.4742 0.182 Uiso 1 1 calc R . . H62A H 0.0366 0.1189 0.4181 0.182 Uiso 1 1 calc R . . C63 C 0.1450(6) 0.0728(11) 0.4352(5) 0.117(6) Uani 1 1 d . . . H63C H 0.1573 0.0799 0.4753 0.175 Uiso 1 1 calc R . . H63B H 0.1767 0.0682 0.42 0.175 Uiso 1 1 calc R . . H63A H 0.123 0.0157 0.4261 0.175 Uiso 1 1 calc R . . C64 C 0.0824(4) 0.3581(7) 0.2382(4) 0.046(3) Uani 1 1 d . . . H64 H 0.0951 0.4066 0.2675 0.056 Uiso 1 1 calc R . . C65 C 0.0250(4) 0.3848(8) 0.2060(4) 0.062(3) Uani 1 1 d . . . H65C H 0.011 0.3377 0.1774 0.093 Uiso 1 1 calc R . . H65B H 0.0257 0.4464 0.1888 0.093 Uiso 1 1 calc R . . H65A H 0.0013 0.3874 0.2311 0.093 Uiso 1 1 calc R . . C66 C 0.1208(4) 0.3621(7) 0.2000(4) 0.060(3) Uani 1 1 d . . . H66C H 0.1086 0.317 0.1699 0.091 Uiso 1 1 calc R . . H66B H 0.1579 0.3462 0.2211 0.091 Uiso 1 1 calc R . . H66A H 0.1204 0.4255 0.1848 0.091 Uiso 1 1 calc R . . C67 C 0.1071(4) 0.5303(7) 0.4849(3) 0.038(2) Uani 1 1 d . . . C68 C 0.1357(4) 0.4732(7) 0.5285(3) 0.044(2) Uani 1 1 d . . . C69 C 0.1369(5) 0.5013(9) 0.5816(4) 0.072(3) Uani 1 1 d . . . H69 H 0.155 0.4631 0.6118 0.086 Uiso 1 1 calc R . . C70 C 0.1122(5) 0.5843(10) 0.5917(5) 0.090(4) Uani 1 1 d . . . H70 H 0.1143 0.6031 0.6285 0.108 Uiso 1 1 calc R . . C71 C 0.0847(5) 0.6387(9) 0.5484(5) 0.081(4) Uani 1 1 d . . . H71 H 0.0676 0.6951 0.5554 0.097 Uiso 1 1 calc R . . C72 C 0.0813(4) 0.6123(7) 0.4933(4) 0.050(3) Uani 1 1 d . . . C73 C 0.1681(4) 0.3895(7) 0.5186(4) 0.043(2) Uani 1 1 d . . . H73 H 0.1483 0.3614 0.4824 0.051 Uiso 1 1 calc R . . C74 C 0.2230(4) 0.4223(7) 0.5131(4) 0.048(3) Uani 1 1 d . . . H74C H 0.2178 0.467 0.4825 0.072 Uiso 1 1 calc R . . H74B H 0.2439 0.3682 0.5059 0.072 Uiso 1 1 calc R . . H74A H 0.2428 0.4531 0.5473 0.072 Uiso 1 1 calc R . . C75 C 0.1759(5) 0.3121(8) 0.5617(4) 0.073(4) Uani 1 1 d . . . H75C H 0.1957 0.3372 0.5976 0.11 Uiso 1 1 calc R . . H75B H 0.1966 0.2605 0.5513 0.11 Uiso 1 1 calc R . . H75A H 0.1402 0.289 0.5638 0.11 Uiso 1 1 calc R . . C76 C 0.0479(4) 0.6743(8) 0.4475(4) 0.058(3) Uani 1 1 d . . . H76 H 0.0517 0.6493 0.4115 0.07 Uiso 1 1 calc R . . C77 C -0.0118(4) 0.6712(9) 0.4468(5) 0.081(4) Uani 1 1 d . . . H77C H -0.0249 0.6063 0.4412 0.121 Uiso 1 1 calc R . . H77B H -0.0327 0.7105 0.4167 0.121 Uiso 1 1 calc R . . H77A H -0.0163 0.6946 0.4819 0.121 Uiso 1 1 calc R . . C78 C 0.0670(6) 0.7762(9) 0.4526(6) 0.107(5) Uani 1 1 d . . . H78C H 0.045 0.8127 0.4217 0.161 Uiso 1 1 calc R . . H78B H 0.1053 0.779 0.4522 0.161 Uiso 1 1 calc R . . H78A H 0.0628 0.8025 0.4873 0.161 Uiso 1 1 calc R . . C79 C 0.2368(4) 0.1282(7) 0.3282(4) 0.061(3) Uani 1 1 d . . . H79B H 0.2026 0.1562 0.3325 0.073 Uiso 1 1 calc R . . H79A H 0.2537 0.091 0.3616 0.073 Uiso 1 1 calc R . . C80 C 0.2262(4) 0.0672(7) 0.2770(4) 0.064(3) Uani 1 1 d . . . H80B H 0.1902 0.0361 0.2697 0.077 Uiso 1 1 calc R . . H80A H 0.2548 0.019 0.2801 0.077 Uiso 1 1 calc R . . C81 C 0.2277(5) 0.1395(9) 0.2326(5) 0.078(4) Uani 1 1 d . . . H81B H 0.2374 0.1095 0.201 0.093 Uiso 1 1 calc R . . H81A H 0.192 0.1711 0.2193 0.093 Uiso 1 1 calc R . . C82 C 0.2713(4) 0.2090(8) 0.2612(4) 0.059(3) Uani 1 1 d . . . H82B H 0.3068 0.193 0.2543 0.07 Uiso 1 1 calc R . . H82A H 0.2613 0.2737 0.2479 0.07 Uiso 1 1 calc R . . C83 C 0.4162(8) 0.6405(18) 0.1480(8) 0.163(8) Uani 1 1 d . . . H83C H 0.3943 0.5996 0.1651 0.245 Uiso 1 1 calc R . . H83B H 0.4533 0.6157 0.1554 0.245 Uiso 1 1 calc R . . H83A H 0.4 0.6426 0.1081 0.245 Uiso 1 1 calc R . . C84 C 0.4175(7) 0.7319(15) 0.1700(10) 0.156(9) Uani 1 1 d . . . H84B H 0.4407 0.7714 0.1529 0.188 Uiso 1 1 calc R . . H84A H 0.4355 0.7285 0.2099 0.188 Uiso 1 1 calc R . . C85 C 0.3617(9) 0.7832(15) 0.1626(7) 0.129(7) Uani 1 1 d . . . H85B H 0.345 0.793 0.1227 0.155 Uiso 1 1 calc R . . H85A H 0.3371 0.7422 0.1768 0.155 Uiso 1 1 calc R . . C86 C 0.3657(11) 0.8633(16) 0.1874(9) 0.174(10) Uani 1 1 d . . . H86B H 0.3903 0.9046 0.1733 0.209 Uiso 1 1 calc R . . H86A H 0.382 0.8538 0.2273 0.209 Uiso 1 1 calc R . . C87 C 0.3063(8) 0.9156(13) 0.1784(7) 0.155(8) Uani 1 1 d . . . H87C H 0.2905 0.9272 0.139 0.233 Uiso 1 1 calc R . . H87B H 0.3112 0.9755 0.1983 0.233 Uiso 1 1 calc R . . H87A H 0.2818 0.8753 0.1925 0.233 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y1 0.0244(5) 0.0310(5) 0.0315(5) 0.0029(4) 0.0116(4) 0.0010(4) Y2 0.0190(4) 0.0306(5) 0.0291(5) -0.0012(4) 0.0057(3) 0.0002(4) Y3 0.0189(5) 0.0402(5) 0.0312(5) 0.0034(4) 0.0098(3) 0.0004(4) O 0.032(4) 0.037(4) 0.042(4) -0.011(3) 0.011(3) -0.009(3) N1 0.021(4) 0.045(5) 0.035(4) -0.001(3) 0.014(3) 0.000(3) N2 0.039(5) 0.034(4) 0.031(4) 0.004(3) 0.013(3) -0.006(4) N3 0.022(4) 0.043(5) 0.037(5) -0.002(4) 0.010(3) -0.001(4) N4 0.023(4) 0.032(4) 0.026(4) 0.001(3) 0.008(3) 0.005(3) N5 0.021(4) 0.047(5) 0.036(4) -0.002(4) 0.005(3) -0.004(4) N6 0.016(4) 0.068(6) 0.035(5) 0.002(4) 0.013(3) 0.007(4) C1 0.085(9) 0.092(9) 0.041(6) 0.019(6) 0.003(6) -0.056(7) C2 0.167(15) 0.124(12) 0.041(7) 0.034(7) -0.034(8) -0.108(11) C3 0.032(6) 0.045(6) 0.026(5) 0.002(4) 0.002(4) 0.003(4) C4 0.038(6) 0.052(6) 0.038(6) 0.003(4) 0.011(5) 0.009(5) C5 0.035(6) 0.084(8) 0.048(7) 0.002(6) 0.007(5) 0.006(5) C6 0.046(7) 0.087(8) 0.030(6) -0.001(5) -0.003(5) 0.004(6) C7 0.037(6) 0.074(8) 0.037(6) -0.004(5) 0.017(5) -0.003(5) C8 0.034(6) 0.049(6) 0.039(6) 0.003(5) 0.002(4) 0.002(5) C9 0.022(5) 0.069(7) 0.045(6) -0.005(5) 0.015(4) 0.016(5) C10 0.055(8) 0.094(9) 0.063(7) 0.000(6) 0.026(6) 0.010(7) C11 0.075(9) 0.063(8) 0.064(7) -0.003(6) 0.013(6) 0.018(6) C12 0.032(6) 0.087(8) 0.025(5) -0.007(5) 0.010(4) 0.005(5) C13 0.077(9) 0.083(9) 0.072(8) -0.024(7) 0.045(7) -0.025(7) C14 0.063(8) 0.073(9) 0.095(9) 0.001(7) 0.049(7) 0.017(6) C15 0.047(6) 0.030(5) 0.028(5) 0.002(4) 0.005(4) -0.006(4) C16 0.075(8) 0.025(6) 0.043(6) -0.008(4) 0.014(5) -0.003(5) C17 0.102(10) 0.027(6) 0.056(7) -0.008(5) 0.011(7) 0.019(6) C18 0.082(10) 0.035(7) 0.066(8) -0.012(6) -0.017(7) -0.001(6) C19 0.067(8) 0.038(6) 0.052(7) 0.013(5) -0.010(6) -0.005(6) C20 0.048(7) 0.022(5) 0.043(6) 0.000(4) 0.007(5) -0.007(4) C21 0.067(9) 0.065(8) 0.060(7) -0.007(6) 0.022(6) 0.021(6) C22 0.097(13) 0.073(11) 0.26(2) 0.005(12) -0.026(13) 0.015(9) C23 0.102(13) 0.190(18) 0.148(15) 0.050(13) 0.080(12) 0.036(12) C24 0.047(7) 0.068(8) 0.042(6) 0.004(5) 0.001(5) -0.008(6) C25 0.147(16) 0.094(12) 0.33(3) 0.015(13) 0.197(18) 0.005(11) C26 0.223(19) 0.051(8) 0.102(11) 0.000(7) 0.075(11) 0.057(10) C27 0.028(5) 0.038(6) 0.049(6) -0.018(4) 0.016(4) -0.011(4) C28 0.024(5) 0.055(6) 0.036(5) -0.004(4) 0.006(4) -0.003(4) C29 0.017(5) 0.031(6) 0.045(6) -0.012(4) 0.008(4) 0.002(4) C30 0.015(5) 0.038(6) 0.038(5) -0.001(4) 0.007(4) -0.005(4) C31 0.024(5) 0.055(7) 0.036(5) -0.003(5) 0.006(4) -0.009(5) C32 0.038(6) 0.070(8) 0.049(7) -0.021(6) 0.019(5) 0.013(5) C33 0.050(7) 0.038(6) 0.072(8) -0.010(6) 0.020(6) 0.013(5) C34 0.034(6) 0.051(7) 0.048(6) 0.000(5) 0.012(5) 0.000(5) C35 0.038(6) 0.050(6) 0.035(5) 0.006(4) 0.015(4) 0.001(5) C36 0.051(7) 0.056(7) 0.077(8) -0.003(6) 0.021(6) -0.024(5) C37 0.051(7) 0.051(6) 0.054(6) 0.009(5) 0.010(5) 0.003(5) C38 0.108(11) 0.045(7) 0.072(8) 0.022(6) 0.047(8) 0.019(7) C39 0.081(11) 0.108(12) 0.165(15) 0.078(11) -0.014(10) -0.032(9) C40 0.107(12) 0.120(12) 0.073(9) 0.047(8) -0.013(8) -0.052(9) C41 0.027(5) 0.037(6) 0.036(5) -0.002(4) 0.003(4) 0.003(4) C42 0.040(6) 0.045(6) 0.026(5) 0.007(4) 0.008(4) 0.013(5) C43 0.055(7) 0.044(7) 0.045(6) 0.016(5) 0.014(5) 0.000(5) C44 0.041(6) 0.064(7) 0.040(6) 0.013(6) 0.003(5) 0.013(6) C45 0.053(7) 0.048(7) 0.034(5) -0.012(5) 0.008(5) 0.003(5) C47 0.076(8) 0.048(7) 0.043(6) 0.011(5) 0.017(5) -0.002(6) C48 0.109(11) 0.052(8) 0.061(7) 0.007(6) 0.009(7) -0.020(7) C49 0.094(10) 0.049(7) 0.097(9) 0.007(7) 0.005(8) 0.023(7) C50 0.040(6) 0.046(6) 0.048(6) -0.023(5) 0.023(5) -0.022(5) C51 0.061(7) 0.044(6) 0.043(6) 0.002(5) 0.009(5) -0.015(5) C52 0.063(8) 0.068(8) 0.087(9) -0.015(7) 0.019(6) -0.026(7) C92 0.031(5) 0.042(6) 0.035(5) -0.003(4) 0.005(4) 0.002(4) C53 0.022(6) 0.086(8) 0.060(7) -0.002(6) 0.010(5) -0.002(5) C54 0.019(5) 0.105(9) 0.050(6) -0.014(6) 0.012(5) 0.000(6) C55 0.009(5) 0.053(7) 0.052(6) 0.005(5) 0.007(4) -0.004(4) C56 0.033(6) 0.053(7) 0.052(6) 0.004(6) 0.009(5) -0.001(5) C57 0.036(6) 0.051(7) 0.092(9) 0.025(7) 0.022(6) -0.002(5) C58 0.049(7) 0.050(7) 0.073(8) 0.000(6) 0.003(6) -0.018(6) C59 0.035(6) 0.063(8) 0.059(7) -0.003(6) 0.009(5) -0.006(5) C60 0.019(5) 0.043(6) 0.059(7) -0.007(5) 0.014(5) -0.012(4) C61 0.042(7) 0.061(7) 0.066(7) 0.019(6) 0.010(5) 0.006(6) C62 0.056(9) 0.219(18) 0.080(10) 0.040(11) 0.002(7) 0.014(11) C63 0.100(12) 0.172(16) 0.073(9) 0.042(10) 0.013(8) 0.047(11) C64 0.038(6) 0.056(7) 0.041(6) 0.001(5) 0.004(5) -0.008(5) C65 0.042(7) 0.071(8) 0.065(7) 0.011(6) 0.000(5) -0.012(6) C66 0.066(8) 0.061(7) 0.061(7) -0.009(5) 0.027(6) -0.012(6) C67 0.029(5) 0.060(7) 0.034(5) -0.001(5) 0.024(4) 0.010(5) C68 0.041(6) 0.066(7) 0.028(5) 0.004(5) 0.017(4) 0.006(5) C69 0.063(8) 0.109(10) 0.040(7) 0.013(6) 0.007(6) 0.018(7) C70 0.093(10) 0.132(12) 0.041(7) -0.014(7) 0.012(7) 0.046(9) C71 0.076(9) 0.119(11) 0.054(8) -0.010(7) 0.026(7) 0.044(8) C72 0.039(6) 0.076(8) 0.038(6) 0.002(5) 0.015(5) 0.015(5) C73 0.027(6) 0.063(7) 0.036(5) 0.013(5) 0.006(4) 0.004(5) C74 0.034(6) 0.074(7) 0.035(5) -0.005(5) 0.007(4) 0.009(5) C75 0.070(8) 0.095(10) 0.058(7) 0.023(6) 0.023(6) 0.016(7) C76 0.059(8) 0.073(8) 0.048(6) 0.009(6) 0.023(5) 0.023(6) C77 0.046(7) 0.123(11) 0.078(8) 0.022(8) 0.024(6) 0.024(7) C78 0.080(11) 0.089(11) 0.152(14) 0.030(10) 0.029(9) 0.011(8) C79 0.062(8) 0.052(7) 0.075(8) -0.014(6) 0.028(6) -0.023(6) C80 0.051(7) 0.053(7) 0.083(8) -0.026(6) 0.007(6) -0.019(6) C81 0.064(9) 0.089(9) 0.066(8) -0.015(7) -0.009(6) -0.009(7) C82 0.056(7) 0.070(7) 0.046(7) -0.008(5) 0.009(5) -0.015(6) C83 0.121(17) 0.22(2) 0.158(18) 0.034(17) 0.046(14) 0.021(17) C84 0.065(12) 0.131(17) 0.24(2) -0.018(16) -0.018(13) 0.004(12) C85 0.18(2) 0.125(16) 0.100(13) 0.037(12) 0.065(13) -0.050(16) C86 0.28(3) 0.119(18) 0.17(2) 0.027(15) 0.13(2) -0.01(2) C87 0.20(2) 0.137(16) 0.181(18) 0.069(13) 0.143(17) 0.024(15) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y1 N1 2.184(7) . ? Y1 N2 2.189(7) . ? Y1 H1X 2.18(6) . ? Y1 H3X 2.15(7) . ? Y1 H4X 2.30(8) . ? Y1 H5X 2.13(10) . ? Y2 N4 2.218(6) . ? Y2 O 2.375(5) . ? Y2 N3 2.589(7) . ? Y2 H2X 2.14(5) . ? Y2 H3X 1.98(6) . ? Y2 H4X 2.39(8) . ? Y2 H5X 1.94(10) . ? Y3 N5 2.196(7) . ? Y3 N6 2.615(7) . ? Y3 H1X 1.98(6) . ? Y3 H2X 2.06(5) . ? Y3 H4X 2.07(7) . ? Y3 H5X 2.38(10) . ? O C82 1.448(10) . ? O C79 1.468(10) . ? N1 C3 1.429(10) . ? N1 C1 1.466(11) . ? N2 C15 1.424(10) . ? N2 C2 1.463(11) . ? N3 C29 1.449(10) . ? N3 C27 1.487(10) . ? N3 H3N 0.89(7) . ? N4 C41 1.437(10) . ? N4 C28 1.453(10) . ? N5 C55 1.416(11) . ? N5 C53 1.478(11) . ? N6 C67 1.465(10) . ? N6 C54 1.505(11) . ? N6 H6N 0.90(8) . ? C1 C2 1.376(13) . ? C1 H1B 0.99 . ? C1 H1A 0.99 . ? C2 H2B 0.99 . ? C2 H2A 0.99 . ? C3 C4 1.399(12) . ? C3 C8 1.419(11) . ? C4 C5 1.416(12) . ? C4 C9 1.502(12) . ? C5 C6 1.377(12) . ? C5 H5 0.95 . ? C6 C7 1.369(13) . ? C6 H6 0.95 . ? C7 C8 1.400(12) . ? C7 H7 0.95 . ? C8 C12 1.517(12) . ? C9 C10 1.517(13) . ? C9 C11 1.551(13) . ? C9 H9 1 . ? C10 H10C 0.98 . ? C10 H10B 0.98 . ? C10 H10A 0.98 . ? C11 H11C 0.98 . ? C11 H11B 0.98 . ? C11 H11A 0.98 . ? C12 C14 1.511(14) . ? C12 C13 1.515(13) . ? C12 H12 1 . ? C13 H13C 0.98 . ? C13 H13B 0.98 . ? C13 H13A 0.98 . ? C14 H14C 0.98 . ? C14 H14B 0.98 . ? C14 H14A 0.98 . ? C15 C20 1.389(12) . ? C15 C16 1.413(13) . ? C16 C17 1.397(13) . ? C16 C21 1.527(14) . ? C17 C18 1.368(15) . ? C17 H17 0.95 . ? C18 C19 1.389(15) . ? C18 H18 0.95 . ? C19 C20 1.428(12) . ? C19 H19 0.95 . ? C20 C24 1.518(13) . ? C21 C22 1.477(16) . ? C21 C23 1.523(16) . ? C21 H21 1 . ? C22 H22C 0.98 . ? C22 H22B 0.98 . ? C22 H22A 0.98 . ? C23 H23C 0.98 . ? C23 H23B 0.98 . ? C23 H23A 0.98 . ? C24 C26 1.464(14) . ? C24 C25 1.501(15) . ? C24 H24 1 . ? C25 H25C 0.98 . ? C25 H25B 0.98 . ? C25 H25A 0.98 . ? C26 H26C 0.98 . ? C26 H26B 0.98 . ? C26 H26A 0.98 . ? C27 C28 1.497(11) . ? C27 H27B 0.99 . ? C27 H27A 0.99 . ? C28 H28B 0.99 . ? C28 H28A 0.99 . ? C29 C30 1.391(11) . ? C29 C34 1.411(12) . ? C30 C31 1.391(12) . ? C30 C35 1.515(12) . ? C31 C32 1.366(13) . ? C31 H31 0.95 . ? C32 C33 1.364(13) . ? C32 H32 0.95 . ? C33 C34 1.385(13) . ? C33 H33 0.95 . ? C34 C38 1.521(13) . ? C35 C37 1.519(11) . ? C35 C36 1.540(12) . ? C35 H35 1 . ? C36 H36C 0.98 . ? C36 H36B 0.98 . ? C36 H36A 0.98 . ? C37 H37C 0.98 . ? C37 H37B 0.98 . ? C37 H37A 0.98 . ? C38 C40 1.487(15) . ? C38 C39 1.502(16) . ? C38 H38 1 . ? C39 H39C 0.98 . ? C39 H39B 0.98 . ? C39 H39A 0.98 . ? C40 H40C 0.98 . ? C40 H40B 0.98 . ? C40 H40A 0.98 . ? C41 C42 1.403(11) . ? C41 C92 1.412(11) . ? C42 C43 1.410(12) . ? C42 C47 1.508(12) . ? C43 C44 1.378(13) . ? C43 H43 0.95 . ? C44 C45 1.368(12) . ? C44 H44 0.95 . ? C45 C92 1.401(12) . ? C45 H45 0.95 . ? C47 C49 1.540(13) . ? C47 C48 1.549(14) . ? C47 H47 1 . ? C48 H48C 0.98 . ? C48 H48B 0.98 . ? C48 H48A 0.98 . ? C49 H49C 0.98 . ? C49 H49B 0.98 . ? C49 H49A 0.98 . ? C50 C51 1.502(12) . ? C50 C92 1.504(12) . ? C50 C52 1.548(12) . ? C50 H50 1 . ? C51 H51C 0.98 . ? C51 H51B 0.98 . ? C51 H51A 0.98 . ? C52 H52C 0.98 . ? C52 H52B 0.98 . ? C52 H52A 0.98 . ? C53 C54 1.492(12) . ? C53 H53B 0.99 . ? C53 H53A 0.99 . ? C54 H54B 0.99 . ? C54 H54A 0.99 . ? C55 C56 1.405(12) . ? C55 C60 1.410(12) . ? C56 C57 1.402(14) . ? C56 C61 1.511(13) . ? C57 C58 1.371(13) . ? C57 H57 0.95 . ? C58 C59 1.358(13) . ? C58 H58 0.95 . ? C59 C60 1.385(12) . ? C59 H59 0.95 . ? C60 C64 1.532(12) . ? C61 C63 1.481(15) . ? C61 C62 1.488(15) . ? C61 H61 1 . ? C62 H62C 0.98 . ? C62 H62B 0.98 . ? C62 H62A 0.98 . ? C63 H63C 0.98 . ? C63 H63B 0.98 . ? C63 H63A 0.98 . ? C64 C65 1.522(12) . ? C64 C66 1.539(13) . ? C64 H64 1 . ? C65 H65C 0.98 . ? C65 H65B 0.98 . ? C65 H65A 0.98 . ? C66 H66C 0.98 . ? C66 H66B 0.98 . ? C66 H66A 0.98 . ? C67 C72 1.381(12) . ? C67 C68 1.407(12) . ? C68 C69 1.386(13) . ? C68 C73 1.507(12) . ? C69 C70 1.393(15) . ? C69 H69 0.95 . ? C70 C71 1.370(15) . ? C70 H70 0.95 . ? C71 C72 1.417(13) . ? C71 H71 0.95 . ? C72 C76 1.524(13) . ? C73 C74 1.514(12) . ? C73 C75 1.521(12) . ? C73 H73 1 . ? C74 H74C 0.98 . ? C74 H74B 0.98 . ? C74 H74A 0.98 . ? C75 H75C 0.98 . ? C75 H75B 0.98 . ? C75 H75A 0.98 . ? C76 C77 1.515(14) . ? C76 C78 1.525(16) . ? C76 H76 1 . ? C77 H77C 0.98 . ? C77 H77B 0.98 . ? C77 H77A 0.98 . ? C78 H78C 0.98 . ? C78 H78B 0.98 . ? C78 H78A 0.98 . ? C79 C80 1.518(13) . ? C79 H79B 0.99 . ? C79 H79A 0.99 . ? C80 C81 1.526(14) . ? C80 H80B 0.99 . ? C80 H80A 0.99 . ? C81 C82 1.521(13) . ? C81 H81B 0.99 . ? C81 H81A 0.99 . ? C82 H82B 0.99 . ? C82 H82A 0.99 . ? C83 C84 1.41(2) . ? C83 H83C 0.98 . ? C83 H83B 0.98 . ? C83 H83A 0.98 . ? C84 C85 1.56(2) . ? C84 H84B 0.99 . ? C84 H84A 0.99 . ? C85 C86 1.29(2) . ? C85 H85B 0.99 . ? C85 H85A 0.99 . ? C86 C87 1.65(3) . ? C86 H86B 0.99 . ? C86 H86A 0.99 . ? C87 H87C 0.98 . ? C87 H87B 0.98 . ? C87 H87A 0.98 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Y1 N2 81.4(2) . . ? N1 Y1 H1X 109.2(15) . . ? N2 Y1 H1X 116.1(15) . . ? N1 Y1 H3X 116.0(17) . . ? N2 Y1 H3X 104.4(18) . . ? H1X Y1 H3X 122(2) . . ? N1 Y1 H4X 116.2(18) . . ? N2 Y1 H4X 162.3(18) . . ? H1X Y1 H4X 62(2) . . ? H3X Y1 H4X 67(3) . . ? N1 Y1 H5X 164(3) . . ? N2 Y1 H5X 114(3) . . ? H1X Y1 H5X 69(3) . . ? H3X Y1 H5X 58(3) . . ? H4X Y1 H5X 49(3) . . ? N4 Y2 O 124.0(2) . . ? N4 Y2 N3 67.1(2) . . ? O Y2 N3 77.1(2) . . ? N4 Y2 H2X 96.1(14) . . ? O Y2 H2X 86.5(14) . . ? N3 Y2 H2X 142.1(14) . . ? N4 Y2 H3X 112.9(19) . . ? O Y2 H3X 108.6(18) . . ? N3 Y2 H3X 90.0(19) . . ? H2X Y2 H3X 128(2) . . ? N4 Y2 H4X 144.8(18) . . ? O Y2 H4X 85.3(18) . . ? N3 Y2 H4X 145.8(18) . . ? H2X Y2 H4X 64(2) . . ? H3X Y2 H4X 68(3) . . ? N4 Y2 H5X 99(3) . . ? O Y2 H5X 134(3) . . ? N3 Y2 H5X 143(3) . . ? H2X Y2 H5X 70(3) . . ? H3X Y2 H5X 63(3) . . ? H4X Y2 H5X 49(3) . . ? N5 Y3 N6 72.8(3) . . ? N5 Y3 H1X 110.3(17) . . ? N6 Y3 H1X 79.2(17) . . ? N5 Y3 H2X 105.4(15) . . ? N6 Y3 H2X 146.2(15) . . ? H1X Y3 H2X 130(2) . . ? N5 Y3 H4X 100(2) . . ? N6 Y3 H4X 143(2) . . ? H1X Y3 H4X 69(3) . . ? H2X Y3 H4X 71(3) . . ? N5 Y3 H5X 147(2) . . ? N6 Y3 H5X 134(2) . . ? H1X Y3 H5X 67(3) . . ? H2X Y3 H5X 64(3) . . ? H4X Y3 H5X 48(3) . . ? C82 O C79 109.9(7) . . ? C82 O Y2 118.5(5) . . ? C79 O Y2 126.4(5) . . ? C3 N1 C1 113.1(7) . . ? C3 N1 Y1 139.7(5) . . ? C1 N1 Y1 106.7(5) . . ? C15 N2 C2 113.4(7) . . ? C15 N2 Y1 138.1(5) . . ? C2 N2 Y1 108.2(6) . . ? C29 N3 C27 115.7(7) . . ? C29 N3 Y2 134.8(5) . . ? C27 N3 Y2 103.1(5) . . ? C29 N3 H3N 105(5) . . ? C27 N3 H3N 94(5) . . ? Y2 N3 H3N 94(5) . . ? C41 N4 C28 110.9(6) . . ? C41 N4 Y2 124.2(5) . . ? C28 N4 Y2 124.8(5) . . ? C55 N5 C53 111.5(7) . . ? C55 N5 Y3 128.5(5) . . ? C53 N5 Y3 118.4(6) . . ? C67 N6 C54 108.8(7) . . ? C67 N6 Y3 128.0(5) . . ? C54 N6 Y3 104.9(5) . . ? C67 N6 H6N 111(6) . . ? C54 N6 H6N 96(6) . . ? Y3 N6 H6N 104(6) . . ? C2 C1 N1 119.7(9) . . ? C2 C1 H1B 107.4 . . ? N1 C1 H1B 107.4 . . ? C2 C1 H1A 107.4 . . ? N1 C1 H1A 107.4 . . ? H1B C1 H1A 106.9 . . ? C1 C2 N2 119.5(9) . . ? C1 C2 H2B 107.4 . . ? N2 C2 H2B 107.4 . . ? C1 C2 H2A 107.4 . . ? N2 C2 H2A 107.4 . . ? H2B C2 H2A 107 . . ? C4 C3 C8 121.1(8) . . ? C4 C3 N1 119.6(7) . . ? C8 C3 N1 119.3(8) . . ? C3 C4 C5 118.0(8) . . ? C3 C4 C9 122.5(8) . . ? C5 C4 C9 119.5(8) . . ? C6 C5 C4 121.8(9) . . ? C6 C5 H5 119.1 . . ? C4 C5 H5 119.1 . . ? C7 C6 C5 118.6(9) . . ? C7 C6 H6 120.7 . . ? C5 C6 H6 120.7 . . ? C6 C7 C8 123.3(9) . . ? C6 C7 H7 118.3 . . ? C8 C7 H7 118.3 . . ? C7 C8 C3 117.0(8) . . ? C7 C8 C12 119.7(8) . . ? C3 C8 C12 123.2(8) . . ? C4 C9 C10 114.1(8) . . ? C4 C9 C11 110.1(8) . . ? C10 C9 C11 110.5(8) . . ? C4 C9 H9 107.3 . . ? C10 C9 H9 107.3 . . ? C11 C9 H9 107.3 . . ? C9 C10 H10C 109.5 . . ? C9 C10 H10B 109.5 . . ? H10C C10 H10B 109.5 . . ? C9 C10 H10A 109.5 . . ? H10C C10 H10A 109.5 . . ? H10B C10 H10A 109.5 . . ? C9 C11 H11C 109.5 . . ? C9 C11 H11B 109.5 . . ? H11C C11 H11B 109.5 . . ? C9 C11 H11A 109.5 . . ? H11C C11 H11A 109.5 . . ? H11B C11 H11A 109.5 . . ? C14 C12 C13 111.2(8) . . ? C14 C12 C8 111.4(8) . . ? C13 C12 C8 110.8(8) . . ? C14 C12 H12 107.8 . . ? C13 C12 H12 107.8 . . ? C8 C12 H12 107.8 . . ? C12 C13 H13C 109.5 . . ? C12 C13 H13B 109.5 . . ? H13C C13 H13B 109.5 . . ? C12 C13 H13A 109.5 . . ? H13C C13 H13A 109.5 . . ? H13B C13 H13A 109.5 . . ? C12 C14 H14C 109.5 . . ? C12 C14 H14B 109.5 . . ? H14C C14 H14B 109.5 . . ? C12 C14 H14A 109.5 . . ? H14C C14 H14A 109.5 . . ? H14B C14 H14A 109.5 . . ? C20 C15 C16 119.8(8) . . ? C20 C15 N2 120.0(8) . . ? C16 C15 N2 120.3(8) . . ? C17 C16 C15 119.1(10) . . ? C17 C16 C21 120.2(10) . . ? C15 C16 C21 120.7(8) . . ? C18 C17 C16 121.2(11) . . ? C18 C17 H17 119.4 . . ? C16 C17 H17 119.4 . . ? C17 C18 C19 121.1(10) . . ? C17 C18 H18 119.5 . . ? C19 C18 H18 119.5 . . ? C18 C19 C20 118.7(10) . . ? C18 C19 H19 120.7 . . ? C20 C19 H19 120.7 . . ? C15 C20 C19 120.2(9) . . ? C15 C20 C24 122.0(8) . . ? C19 C20 C24 117.7(9) . . ? C22 C21 C23 111.6(12) . . ? C22 C21 C16 113.0(11) . . ? C23 C21 C16 111.9(10) . . ? C22 C21 H21 106.6 . . ? C23 C21 H21 106.6 . . ? C16 C21 H21 106.6 . . ? C21 C22 H22C 109.5 . . ? C21 C22 H22B 109.5 . . ? H22C C22 H22B 109.5 . . ? C21 C22 H22A 109.5 . . ? H22C C22 H22A 109.5 . . ? H22B C22 H22A 109.5 . . ? C21 C23 H23C 109.5 . . ? C21 C23 H23B 109.5 . . ? H23C C23 H23B 109.5 . . ? C21 C23 H23A 109.5 . . ? H23C C23 H23A 109.5 . . ? H23B C23 H23A 109.5 . . ? C26 C24 C25 109.5(12) . . ? C26 C24 C20 111.5(9) . . ? C25 C24 C20 113.8(10) . . ? C26 C24 H24 107.2 . . ? C25 C24 H24 107.2 . . ? C20 C24 H24 107.2 . . ? C24 C25 H25C 109.5 . . ? C24 C25 H25B 109.5 . . ? H25C C25 H25B 109.5 . . ? C24 C25 H25A 109.5 . . ? H25C C25 H25A 109.5 . . ? H25B C25 H25A 109.5 . . ? C24 C26 H26C 109.5 . . ? C24 C26 H26B 109.5 . . ? H26C C26 H26B 109.5 . . ? C24 C26 H26A 109.5 . . ? H26C C26 H26A 109.5 . . ? H26B C26 H26A 109.5 . . ? N3 C27 C28 108.0(7) . . ? N3 C27 H27B 110.1 . . ? C28 C27 H27B 110.1 . . ? N3 C27 H27A 110.1 . . ? C28 C27 H27A 110.1 . . ? H27B C27 H27A 108.4 . . ? N4 C28 C27 110.1(7) . . ? N4 C28 H28B 109.6 . . ? C27 C28 H28B 109.6 . . ? N4 C28 H28A 109.6 . . ? C27 C28 H28A 109.6 . . ? H28B C28 H28A 108.2 . . ? C30 C29 C34 121.8(8) . . ? C30 C29 N3 120.8(8) . . ? C34 C29 N3 117.3(8) . . ? C31 C30 C29 116.7(8) . . ? C31 C30 C35 120.0(8) . . ? C29 C30 C35 123.3(8) . . ? C32 C31 C30 122.8(9) . . ? C32 C31 H31 118.6 . . ? C30 C31 H31 118.6 . . ? C33 C32 C31 119.2(9) . . ? C33 C32 H32 120.4 . . ? C31 C32 H32 120.4 . . ? C32 C33 C34 121.9(9) . . ? C32 C33 H33 119.1 . . ? C34 C33 H33 119.1 . . ? C33 C34 C29 117.5(9) . . ? C33 C34 C38 119.0(9) . . ? C29 C34 C38 123.5(9) . . ? C30 C35 C37 113.0(7) . . ? C30 C35 C36 111.2(8) . . ? C37 C35 C36 110.4(8) . . ? C30 C35 H35 107.3 . . ? C37 C35 H35 107.3 . . ? C36 C35 H35 107.3 . . ? C35 C36 H36C 109.5 . . ? C35 C36 H36B 109.5 . . ? H36C C36 H36B 109.5 . . ? C35 C36 H36A 109.5 . . ? H36C C36 H36A 109.5 . . ? H36B C36 H36A 109.5 . . ? C35 C37 H37C 109.5 . . ? C35 C37 H37B 109.5 . . ? H37C C37 H37B 109.5 . . ? C35 C37 H37A 109.5 . . ? H37C C37 H37A 109.5 . . ? H37B C37 H37A 109.5 . . ? C40 C38 C39 110.3(10) . . ? C40 C38 C34 112.5(10) . . ? C39 C38 C34 114.8(10) . . ? C40 C38 H38 106.2 . . ? C39 C38 H38 106.2 . . ? C34 C38 H38 106.2 . . ? C38 C39 H39C 109.5 . . ? C38 C39 H39B 109.5 . . ? H39C C39 H39B 109.5 . . ? C38 C39 H39A 109.5 . . ? H39C C39 H39A 109.5 . . ? H39B C39 H39A 109.5 . . ? C38 C40 H40C 109.5 . . ? C38 C40 H40B 109.5 . . ? H40C C40 H40B 109.5 . . ? C38 C40 H40A 109.5 . . ? H40C C40 H40A 109.5 . . ? H40B C40 H40A 109.5 . . ? C42 C41 C92 119.4(8) . . ? C42 C41 N4 119.8(7) . . ? C92 C41 N4 120.8(8) . . ? C41 C42 C43 119.6(8) . . ? C41 C42 C47 122.4(8) . . ? C43 C42 C47 118.0(8) . . ? C44 C43 C42 120.5(9) . . ? C44 C43 H43 119.8 . . ? C42 C43 H43 119.8 . . ? C45 C44 C43 119.8(9) . . ? C45 C44 H44 120.1 . . ? C43 C44 H44 120.1 . . ? C44 C45 C92 122.0(9) . . ? C44 C45 H45 119 . . ? C92 C45 H45 119 . . ? C42 C47 C49 111.8(8) . . ? C42 C47 C48 112.6(9) . . ? C49 C47 C48 110.0(9) . . ? C42 C47 H47 107.4 . . ? C49 C47 H47 107.4 . . ? C48 C47 H47 107.4 . . ? C47 C48 H48C 109.5 . . ? C47 C48 H48B 109.5 . . ? H48C C48 H48B 109.5 . . ? C47 C48 H48A 109.5 . . ? H48C C48 H48A 109.5 . . ? H48B C48 H48A 109.5 . . ? C47 C49 H49C 109.5 . . ? C47 C49 H49B 109.5 . . ? H49C C49 H49B 109.5 . . ? C47 C49 H49A 109.5 . . ? H49C C49 H49A 109.5 . . ? H49B C49 H49A 109.5 . . ? C51 C50 C92 112.9(7) . . ? C51 C50 C52 109.2(8) . . ? C92 C50 C52 112.2(8) . . ? C51 C50 H50 107.4 . . ? C92 C50 H50 107.4 . . ? C52 C50 H50 107.4 . . ? C50 C51 H51C 109.5 . . ? C50 C51 H51B 109.5 . . ? H51C C51 H51B 109.5 . . ? C50 C51 H51A 109.5 . . ? H51C C51 H51A 109.5 . . ? H51B C51 H51A 109.5 . . ? C50 C52 H52C 109.5 . . ? C50 C52 H52B 109.5 . . ? H52C C52 H52B 109.5 . . ? C50 C52 H52A 109.5 . . ? H52C C52 H52A 109.5 . . ? H52B C52 H52A 109.5 . . ? C45 C92 C41 118.6(8) . . ? C45 C92 C50 119.8(8) . . ? C41 C92 C50 121.6(7) . . ? N5 C53 C54 111.3(7) . . ? N5 C53 H53B 109.4 . . ? C54 C53 H53B 109.4 . . ? N5 C53 H53A 109.4 . . ? C54 C53 H53A 109.4 . . ? H53B C53 H53A 108 . . ? C53 C54 N6 113.2(7) . . ? C53 C54 H54B 108.9 . . ? N6 C54 H54B 108.9 . . ? C53 C54 H54A 108.9 . . ? N6 C54 H54A 108.9 . . ? H54B C54 H54A 107.8 . . ? C56 C55 C60 119.1(9) . . ? C56 C55 N5 119.0(8) . . ? C60 C55 N5 121.9(8) . . ? C57 C56 C55 118.1(9) . . ? C57 C56 C61 120.4(9) . . ? C55 C56 C61 121.6(9) . . ? C58 C57 C56 123.2(10) . . ? C58 C57 H57 118.4 . . ? C56 C57 H57 118.4 . . ? C59 C58 C57 117.4(10) . . ? C59 C58 H58 121.3 . . ? C57 C58 H58 121.3 . . ? C58 C59 C60 123.3(10) . . ? C58 C59 H59 118.4 . . ? C60 C59 H59 118.4 . . ? C59 C60 C55 119.0(9) . . ? C59 C60 C64 119.8(9) . . ? C55 C60 C64 121.3(8) . . ? C63 C61 C62 111.3(11) . . ? C63 C61 C56 117.4(10) . . ? C62 C61 C56 113.4(9) . . ? C63 C61 H61 104.4 . . ? C62 C61 H61 104.4 . . ? C56 C61 H61 104.4 . . ? C61 C62 H62C 109.5 . . ? C61 C62 H62B 109.5 . . ? H62C C62 H62B 109.5 . . ? C61 C62 H62A 109.5 . . ? H62C C62 H62A 109.5 . . ? H62B C62 H62A 109.5 . . ? C61 C63 H63C 109.5 . . ? C61 C63 H63B 109.5 . . ? H63C C63 H63B 109.5 . . ? C61 C63 H63A 109.5 . . ? H63C C63 H63A 109.5 . . ? H63B C63 H63A 109.5 . . ? C65 C64 C60 112.5(8) . . ? C65 C64 C66 109.7(8) . . ? C60 C64 C66 112.2(8) . . ? C65 C64 H64 107.4 . . ? C60 C64 H64 107.4 . . ? C66 C64 H64 107.4 . . ? C64 C65 H65C 109.5 . . ? C64 C65 H65B 109.5 . . ? H65C C65 H65B 109.5 . . ? C64 C65 H65A 109.5 . . ? H65C C65 H65A 109.5 . . ? H65B C65 H65A 109.5 . . ? C64 C66 H66C 109.5 . . ? C64 C66 H66B 109.5 . . ? H66C C66 H66B 109.5 . . ? C64 C66 H66A 109.5 . . ? H66C C66 H66A 109.5 . . ? H66B C66 H66A 109.5 . . ? C72 C67 C68 122.6(8) . . ? C72 C67 N6 121.9(8) . . ? C68 C67 N6 115.4(8) . . ? C69 C68 C67 117.4(9) . . ? C69 C68 C73 120.9(9) . . ? C67 C68 C73 121.5(8) . . ? C68 C69 C70 121.5(10) . . ? C68 C69 H69 119.2 . . ? C70 C69 H69 119.2 . . ? C71 C70 C69 119.7(10) . . ? C71 C70 H70 120.1 . . ? C69 C70 H70 120.1 . . ? C70 C71 C72 120.9(11) . . ? C70 C71 H71 119.5 . . ? C72 C71 H71 119.5 . . ? C67 C72 C71 117.7(9) . . ? C67 C72 C76 124.6(8) . . ? C71 C72 C76 117.7(9) . . ? C68 C73 C74 109.2(8) . . ? C68 C73 C75 115.4(8) . . ? C74 C73 C75 109.7(8) . . ? C68 C73 H73 107.4 . . ? C74 C73 H73 107.4 . . ? C75 C73 H73 107.4 . . ? C73 C74 H74C 109.5 . . ? C73 C74 H74B 109.5 . . ? H74C C74 H74B 109.5 . . ? C73 C74 H74A 109.5 . . ? H74C C74 H74A 109.5 . . ? H74B C74 H74A 109.5 . . ? C73 C75 H75C 109.5 . . ? C73 C75 H75B 109.5 . . ? H75C C75 H75B 109.5 . . ? C73 C75 H75A 109.5 . . ? H75C C75 H75A 109.5 . . ? H75B C75 H75A 109.5 . . ? C77 C76 C72 110.6(9) . . ? C77 C76 C78 109.0(10) . . ? C72 C76 C78 112.7(10) . . ? C77 C76 H76 108.2 . . ? C72 C76 H76 108.2 . . ? C78 C76 H76 108.2 . . ? C76 C77 H77C 109.5 . . ? C76 C77 H77B 109.5 . . ? H77C C77 H77B 109.5 . . ? C76 C77 H77A 109.5 . . ? H77C C77 H77A 109.5 . . ? H77B C77 H77A 109.5 . . ? C76 C78 H78C 109.5 . . ? C76 C78 H78B 109.5 . . ? H78C C78 H78B 109.5 . . ? C76 C78 H78A 109.5 . . ? H78C C78 H78A 109.5 . . ? H78B C78 H78A 109.5 . . ? O C79 C80 104.9(8) . . ? O C79 H79B 110.8 . . ? C80 C79 H79B 110.8 . . ? O C79 H79A 110.8 . . ? C80 C79 H79A 110.8 . . ? H79B C79 H79A 108.8 . . ? C79 C80 C81 101.6(8) . . ? C79 C80 H80B 111.4 . . ? C81 C80 H80B 111.4 . . ? C79 C80 H80A 111.4 . . ? C81 C80 H80A 111.4 . . ? H80B C80 H80A 109.3 . . ? C82 C81 C80 104.3(8) . . ? C82 C81 H81B 110.9 . . ? C80 C81 H81B 110.9 . . ? C82 C81 H81A 110.9 . . ? C80 C81 H81A 110.9 . . ? H81B C81 H81A 108.9 . . ? O C82 C81 105.6(8) . . ? O C82 H82B 110.6 . . ? C81 C82 H82B 110.6 . . ? O C82 H82A 110.6 . . ? C81 C82 H82A 110.6 . . ? H82B C82 H82A 108.8 . . ? C84 C83 H83C 109.5 . . ? C84 C83 H83B 109.5 . . ? H83C C83 H83B 109.5 . . ? C84 C83 H83A 109.5 . . ? H83C C83 H83A 109.5 . . ? H83B C83 H83A 109.5 . . ? C83 C84 C85 117.1(17) . . ? C83 C84 H84B 108 . . ? C85 C84 H84B 108 . . ? C83 C84 H84A 108 . . ? C85 C84 H84A 108 . . ? H84B C84 H84A 107.3 . . ? C86 C85 C84 114(2) . . ? C86 C85 H85B 108.8 . . ? C84 C85 H85B 108.8 . . ? C86 C85 H85A 108.8 . . ? C84 C85 H85A 108.8 . . ? H85B C85 H85A 107.7 . . ? C85 C86 C87 112(2) . . ? C85 C86 H86B 109.1 . . ? C87 C86 H86B 109.1 . . ? C85 C86 H86A 109.1 . . ? C87 C86 H86A 109.1 . . ? H86B C86 H86A 107.9 . . ? C86 C87 H87C 109.5 . . ? C86 C87 H87B 109.5 . . ? H87C C87 H87B 109.5 . . ? C86 C87 H87A 109.5 . . ? H87C C87 H87A 109.5 . . ? H87B C87 H87A 109.5 . . ? #===END data_[Y(thf)(OC6H2MetBu2)(C6H3iPr2NCH2CH2NC6H3iPr2)]_[15] _database_code_depnum_ccdc_archive 'CCDC 228150' _audit_creation_date 2003-03-27T10:10:15-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common ; '[Y(thf)(OC6H2MetBu2)(C6H3iPr2NCH2CH2NC6H3iPr2)]' ; _chemical_formula_moiety 'C45 H69 N2 O2 Y1' _chemical_formula_sum 'C45 H69 N2 O2 Y1' _chemical_formula_weight 758.93 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 10.2131(3) _cell_length_b 23.5543(6) _cell_length_c 18.5374(7) _cell_angle_alpha 90 _cell_angle_beta 101.190(1) _cell_angle_gamma 90 _cell_volume 4374.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 22492 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 22.986 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.152 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1632 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.368 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.8089 _exptl_absorpt_correction_T_max 0.9546 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0999 _diffrn_reflns_av_unetI/netI 0.083 _diffrn_reflns_number 19710 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.76 _diffrn_reflns_theta_max 22.98 _diffrn_reflns_theta_full 22.98 _diffrn_measured_fraction_theta_full 0.931 _diffrn_measured_fraction_theta_max 0.931 _reflns_number_total 5660 _reflns_number_gt 3978 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0452P)^2^+9.0223P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 5660 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1024 _refine_ls_R_factor_gt 0.0606 _refine_ls_wR_factor_ref 0.1423 _refine_ls_wR_factor_gt 0.1222 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.689 _refine_diff_density_min -0.314 _refine_diff_density_rms 0.064 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Y Y 0.13282(5) 0.16424(2) 0.23546(3) 0.03335(19) Uani 1 1 d . . . O1 O 0.0817(4) 0.11973(14) 0.3220(2) 0.0424(10) Uani 1 1 d . . . O2 O -0.0740(4) 0.16576(17) 0.1572(2) 0.0518(11) Uani 1 1 d . . . N1 N 0.2149(4) 0.24956(17) 0.2390(3) 0.0356(11) Uani 1 1 d . . . N2 N 0.2909(4) 0.14676(16) 0.1757(2) 0.0300(10) Uani 1 1 d . . . C1 C 0.2618(6) 0.2510(2) 0.1687(3) 0.0457(16) Uani 1 1 d . . . H1A H 0.3121 0.2867 0.166 0.055 Uiso 1 1 calc R . . H1B H 0.1835 0.2513 0.1277 0.055 Uiso 1 1 calc R . . C2 C 0.3496(6) 0.2014(2) 0.1591(4) 0.0445(16) Uani 1 1 d . . . H2A H 0.364 0.2007 0.1078 0.053 Uiso 1 1 calc R . . H2B H 0.4377 0.2062 0.1919 0.053 Uiso 1 1 calc R . . C3 C 0.2206(6) 0.3020(2) 0.2783(4) 0.0410(15) Uani 1 1 d . . . C4 C 0.3332(6) 0.3143(2) 0.3327(4) 0.0441(16) Uani 1 1 d . . . C5 C 0.3337(7) 0.3652(3) 0.3719(4) 0.0580(18) Uani 1 1 d . . . H5 H 0.4088 0.3741 0.4091 0.07 Uiso 1 1 calc R . . C6 C 0.2282(8) 0.4026(3) 0.3580(4) 0.064(2) Uani 1 1 d . . . H6 H 0.2299 0.4365 0.3859 0.077 Uiso 1 1 calc R . . C7 C 0.1227(8) 0.3906(3) 0.3043(5) 0.068(2) Uani 1 1 d . . . H7 H 0.0507 0.4168 0.2947 0.081 Uiso 1 1 calc R . . C8 C 0.1150(6) 0.3409(2) 0.2623(4) 0.0529(18) Uani 1 1 d . . . C9 C 0.4535(6) 0.2763(3) 0.3467(4) 0.0493(16) Uani 1 1 d . . . H9 H 0.4251 0.2386 0.324 0.059 Uiso 1 1 calc R . . C10 C 0.5114(8) 0.2659(3) 0.4279(4) 0.071(2) Uani 1 1 d . . . H10A H 0.5884 0.2404 0.4324 0.107 Uiso 1 1 calc R . . H10B H 0.4433 0.2484 0.4514 0.107 Uiso 1 1 calc R . . H10C H 0.5397 0.3021 0.452 0.107 Uiso 1 1 calc R . . C11 C 0.5628(7) 0.2994(3) 0.3082(4) 0.066(2) Uani 1 1 d . . . H11A H 0.64 0.2738 0.3175 0.098 Uiso 1 1 calc R . . H11B H 0.59 0.3372 0.3274 0.098 Uiso 1 1 calc R . . H11C H 0.5282 0.3018 0.2552 0.098 Uiso 1 1 calc R . . C12 C -0.0030(6) 0.3313(3) 0.2007(5) 0.069(2) Uani 1 1 d . . . H12 H 0.0011 0.2909 0.1846 0.083 Uiso 1 1 calc R . . C13 C 0.0059(9) 0.3689(4) 0.1340(6) 0.114(4) Uani 1 1 d . . . H13A H -0.071 0.3614 0.0945 0.171 Uiso 1 1 calc R . . H13B H 0.0885 0.3603 0.1167 0.171 Uiso 1 1 calc R . . H13C H 0.0059 0.4089 0.1483 0.171 Uiso 1 1 calc R . . C14 C -0.1370(8) 0.3392(4) 0.2248(7) 0.126(4) Uani 1 1 d . . . H14A H -0.2099 0.3323 0.1829 0.189 Uiso 1 1 calc R . . H14B H -0.1432 0.3781 0.2427 0.189 Uiso 1 1 calc R . . H14C H -0.1435 0.3123 0.2643 0.189 Uiso 1 1 calc R . . C15 C 0.3756(5) 0.1007(2) 0.1676(3) 0.0318(13) Uani 1 1 d . . . C16 C 0.4692(5) 0.0804(2) 0.2294(3) 0.0335(13) Uani 1 1 d . . . C17 C 0.5546(5) 0.0364(2) 0.2194(4) 0.0436(15) Uani 1 1 d . . . H17 H 0.6182 0.0229 0.2602 0.052 Uiso 1 1 calc R . . C18 C 0.5484(6) 0.0119(2) 0.1513(4) 0.0455(16) Uani 1 1 d . . . H18 H 0.6079 -0.0179 0.1452 0.055 Uiso 1 1 calc R . . C19 C 0.4565(6) 0.0306(2) 0.0925(4) 0.0481(16) Uani 1 1 d . . . H19 H 0.4518 0.0127 0.0462 0.058 Uiso 1 1 calc R . . C20 C 0.3698(5) 0.0750(2) 0.0983(3) 0.0391(14) Uani 1 1 d . . . C21 C 0.4809(6) 0.1053(2) 0.3052(3) 0.0444(15) Uani 1 1 d . . . H21 H 0.4095 0.1347 0.3027 0.053 Uiso 1 1 calc R . . C22 C 0.4599(7) 0.0613(3) 0.3632(4) 0.074(2) Uani 1 1 d . . . H22A H 0.4675 0.08 0.411 0.111 Uiso 1 1 calc R . . H22B H 0.5279 0.0316 0.3665 0.111 Uiso 1 1 calc R . . H22C H 0.371 0.0444 0.3489 0.111 Uiso 1 1 calc R . . C23 C 0.6145(6) 0.1349(3) 0.3299(4) 0.0532(17) Uani 1 1 d . . . H23A H 0.6189 0.1509 0.3791 0.08 Uiso 1 1 calc R . . H23B H 0.6236 0.1655 0.2953 0.08 Uiso 1 1 calc R . . H23C H 0.687 0.1074 0.3312 0.08 Uiso 1 1 calc R . . C24 C 0.2719(6) 0.0951(3) 0.0310(3) 0.0495(16) Uani 1 1 d . . . H24 H 0.2198 0.1273 0.0463 0.059 Uiso 1 1 calc R . . C25 C 0.3439(8) 0.1171(3) -0.0290(4) 0.074(2) Uani 1 1 d . . . H25A H 0.2778 0.1301 -0.0714 0.111 Uiso 1 1 calc R . . H25B H 0.3974 0.0865 -0.0443 0.111 Uiso 1 1 calc R . . H25C H 0.4023 0.1488 -0.0095 0.111 Uiso 1 1 calc R . . C26 C 0.1729(7) 0.0478(3) 0.0010(4) 0.077(2) Uani 1 1 d . . . H26A H 0.1102 0.0617 -0.0422 0.115 Uiso 1 1 calc R . . H26B H 0.1235 0.0365 0.0391 0.115 Uiso 1 1 calc R . . H26C H 0.2218 0.0151 -0.0128 0.115 Uiso 1 1 calc R . . C27 C 0.0089(5) 0.0882(2) 0.3611(3) 0.0308(13) Uani 1 1 d . . . C28 C -0.0274(5) 0.0318(2) 0.3398(3) 0.0318(13) Uani 1 1 d . . . C29 C -0.1070(5) 0.0032(2) 0.3812(3) 0.0365(14) Uani 1 1 d . . . H29 H -0.1344 -0.0344 0.3669 0.044 Uiso 1 1 calc R . . C30 C -0.1483(5) 0.0261(2) 0.4412(3) 0.0406(15) Uani 1 1 d . . . C31 C -0.1071(5) 0.0814(2) 0.4617(3) 0.0407(14) Uani 1 1 d . . . H31 H -0.1337 0.098 0.5033 0.049 Uiso 1 1 calc R . . C32 C -0.0278(5) 0.1133(2) 0.4227(3) 0.0351(14) Uani 1 1 d . . . C33 C 0.0180(6) -0.0016(2) 0.2773(3) 0.0401(15) Uani 1 1 d . . . C34 C 0.0947(8) 0.0305(3) 0.2269(4) 0.077(2) Uani 1 1 d . . . H34A H 0.1723 0.0493 0.2566 0.115 Uiso 1 1 calc R . . H34B H 0.0362 0.059 0.1986 0.115 Uiso 1 1 calc R . . H34C H 0.1246 0.0037 0.193 0.115 Uiso 1 1 calc R . . C35 C 0.1162(8) -0.0487(3) 0.3128(5) 0.082(2) Uani 1 1 d . . . H35A H 0.1931 -0.0313 0.3449 0.123 Uiso 1 1 calc R . . H35B H 0.1466 -0.0704 0.2741 0.123 Uiso 1 1 calc R . . H35C H 0.0706 -0.0742 0.3418 0.123 Uiso 1 1 calc R . . C36 C -0.0976(8) -0.0295(4) 0.2286(5) 0.091(3) Uani 1 1 d . . . H36A H -0.0661 -0.0503 0.1894 0.136 Uiso 1 1 calc R . . H36B H -0.1623 -0.0006 0.2068 0.136 Uiso 1 1 calc R . . H36C H -0.1404 -0.056 0.2576 0.136 Uiso 1 1 calc R . . C37 C -0.2327(6) -0.0069(3) 0.4851(4) 0.0528(17) Uani 1 1 d . . . H37A H -0.2515 0.0168 0.5253 0.079 Uiso 0.5 1 calc PR . . H37B H -0.1844 -0.0411 0.5054 0.079 Uiso 0.5 1 calc PR . . H37C H -0.3168 -0.0179 0.453 0.079 Uiso 0.5 1 calc PR . . H37D H -0.2503 -0.0449 0.4638 0.079 Uiso 0.5 1 calc PR . . H37E H -0.3174 0.0129 0.4837 0.079 Uiso 0.5 1 calc PR . . H37F H -0.1851 -0.0103 0.5362 0.079 Uiso 0.5 1 calc PR . . C38 C 0.0161(6) 0.1738(2) 0.4485(4) 0.0455(16) Uani 1 1 d . . . C39 C 0.1694(6) 0.1771(3) 0.4671(4) 0.067(2) Uani 1 1 d . . . H39A H 0.2039 0.1485 0.5044 0.1 Uiso 1 1 calc R . . H39B H 0.1967 0.215 0.4862 0.1 Uiso 1 1 calc R . . H39C H 0.2053 0.17 0.4226 0.1 Uiso 1 1 calc R . . C40 C -0.0395(7) 0.2178(2) 0.3900(4) 0.0602(19) Uani 1 1 d . . . H40A H -0.0104 0.2558 0.4078 0.09 Uiso 1 1 calc R . . H40B H -0.1372 0.2161 0.3797 0.09 Uiso 1 1 calc R . . H40C H -0.0065 0.2098 0.3448 0.09 Uiso 1 1 calc R . . C41 C -0.0344(8) 0.1910(3) 0.5185(4) 0.076(2) Uani 1 1 d . . . H41A H -0.0013 0.1638 0.5579 0.114 Uiso 1 1 calc R . . H41B H -0.1322 0.1909 0.5083 0.114 Uiso 1 1 calc R . . H41C H -0.0018 0.2291 0.5337 0.114 Uiso 1 1 calc R . . C42 C -0.1055(8) 0.1624(5) 0.0792(5) 0.115(4) Uani 1 1 d . . . H42A H -0.0448 0.1356 0.0609 0.138 Uiso 1 1 calc R . . H42B H -0.097 0.2002 0.0571 0.138 Uiso 1 1 calc R . . C43 C -0.2440(9) 0.1422(5) 0.0606(5) 0.116(4) Uani 1 1 d . . . H43A H -0.2901 0.1587 0.0133 0.14 Uiso 1 1 calc R . . H43B H -0.2467 0.1003 0.0565 0.14 Uiso 1 1 calc R . . C44 C -0.3055(7) 0.1609(4) 0.1197(4) 0.077(2) Uani 1 1 d . . . H44A H -0.3772 0.1343 0.1267 0.092 Uiso 1 1 calc R . . H44B H -0.3444 0.1992 0.1096 0.092 Uiso 1 1 calc R . . C45 C -0.1962(6) 0.1617(3) 0.1864(4) 0.069(2) Uani 1 1 d . . . H45A H -0.2056 0.1948 0.218 0.083 Uiso 1 1 calc R . . H45B H -0.197 0.1265 0.2156 0.083 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 Y 0.0297(3) 0.0323(3) 0.0400(4) 0.0023(3) 0.0116(2) -0.0015(2) O1 0.047(2) 0.036(2) 0.046(3) 0.0022(18) 0.015(2) -0.0042(17) O2 0.028(2) 0.075(3) 0.053(3) 0.012(2) 0.009(2) -0.002(2) N1 0.041(3) 0.028(2) 0.041(3) 0.002(2) 0.016(2) 0.0006(19) N2 0.025(2) 0.030(2) 0.034(3) 0.0028(19) 0.005(2) 0.0009(18) C1 0.054(4) 0.040(3) 0.046(4) 0.004(3) 0.019(3) 0.000(3) C2 0.046(4) 0.036(3) 0.055(5) 0.006(3) 0.020(3) 0.003(3) C3 0.045(4) 0.026(3) 0.058(5) 0.002(3) 0.026(3) -0.002(3) C4 0.059(4) 0.035(3) 0.044(4) -0.001(3) 0.024(4) -0.007(3) C5 0.075(5) 0.050(4) 0.054(5) -0.009(3) 0.024(4) -0.009(4) C6 0.093(6) 0.038(4) 0.070(6) -0.014(4) 0.035(5) -0.002(4) C7 0.077(5) 0.033(4) 0.105(7) -0.001(4) 0.046(5) 0.008(3) C8 0.057(4) 0.031(3) 0.078(5) 0.004(3) 0.032(4) 0.008(3) C9 0.055(4) 0.048(4) 0.045(5) -0.008(3) 0.008(3) -0.004(3) C10 0.079(5) 0.073(5) 0.060(6) -0.009(4) 0.009(4) 0.003(4) C11 0.053(4) 0.070(5) 0.077(6) -0.008(4) 0.023(4) -0.006(3) C12 0.050(4) 0.042(4) 0.109(7) 0.001(4) 0.002(4) 0.017(3) C13 0.091(7) 0.105(7) 0.129(9) 0.035(6) -0.024(6) 0.003(5) C14 0.057(5) 0.116(7) 0.206(13) -0.007(7) 0.029(7) 0.021(5) C15 0.032(3) 0.027(3) 0.037(4) 0.004(2) 0.008(3) -0.003(2) C16 0.029(3) 0.037(3) 0.035(4) 0.004(2) 0.007(3) -0.002(2) C17 0.036(3) 0.038(3) 0.053(5) 0.014(3) -0.002(3) 0.007(3) C18 0.038(4) 0.035(3) 0.062(5) -0.009(3) 0.008(3) 0.010(3) C19 0.049(4) 0.043(3) 0.053(5) -0.011(3) 0.010(3) 0.003(3) C20 0.033(3) 0.042(3) 0.042(4) 0.000(3) 0.007(3) 0.001(3) C21 0.040(4) 0.058(4) 0.035(4) 0.006(3) 0.005(3) 0.009(3) C22 0.062(5) 0.113(6) 0.045(5) 0.021(4) 0.002(4) -0.015(4) C23 0.046(4) 0.065(4) 0.045(5) -0.006(3) 0.000(3) 0.002(3) C24 0.058(4) 0.051(4) 0.037(4) -0.005(3) 0.001(3) 0.010(3) C25 0.093(6) 0.078(5) 0.052(5) 0.003(4) 0.016(4) 0.017(4) C26 0.079(5) 0.075(5) 0.063(6) -0.008(4) -0.021(4) 0.002(4) C27 0.032(3) 0.032(3) 0.030(4) 0.003(2) 0.008(3) -0.002(2) C28 0.030(3) 0.031(3) 0.032(4) 0.002(2) 0.003(3) 0.000(2) C29 0.041(3) 0.032(3) 0.032(4) 0.003(3) -0.004(3) 0.000(2) C30 0.032(3) 0.044(3) 0.044(4) 0.013(3) 0.002(3) 0.000(3) C31 0.034(3) 0.059(4) 0.028(4) -0.001(3) 0.002(3) 0.011(3) C32 0.026(3) 0.040(3) 0.036(4) -0.002(3) -0.001(3) 0.002(2) C33 0.045(3) 0.028(3) 0.048(4) -0.003(3) 0.011(3) -0.002(2) C34 0.120(7) 0.052(4) 0.069(6) -0.013(4) 0.047(5) -0.001(4) C35 0.090(6) 0.083(5) 0.078(6) -0.001(4) 0.026(5) 0.033(4) C36 0.076(6) 0.120(7) 0.077(7) -0.049(5) 0.016(5) -0.014(5) C37 0.047(4) 0.064(4) 0.046(4) 0.023(3) 0.006(3) -0.005(3) C38 0.043(4) 0.041(4) 0.052(4) -0.012(3) 0.007(3) -0.006(3) C39 0.048(4) 0.064(4) 0.083(6) -0.021(4) -0.002(4) -0.011(3) C40 0.072(5) 0.038(4) 0.071(6) -0.007(3) 0.017(4) -0.002(3) C41 0.094(6) 0.068(5) 0.071(6) -0.035(4) 0.031(5) -0.013(4) C42 0.046(5) 0.244(12) 0.055(7) 0.033(7) 0.011(4) 0.010(6) C43 0.068(6) 0.218(12) 0.063(7) -0.033(7) 0.011(5) -0.004(6) C44 0.043(4) 0.112(6) 0.074(6) 0.013(5) 0.009(4) 0.002(4) C45 0.028(3) 0.117(6) 0.067(6) -0.007(5) 0.017(4) -0.004(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Y O1 2.066(4) . ? Y N2 2.168(4) . ? Y N1 2.173(4) . ? Y O2 2.319(4) . ? O1 C27 1.356(6) . ? O2 C42 1.421(9) . ? O2 C45 1.457(7) . ? N1 C3 1.428(7) . ? N1 C1 1.475(7) . ? N2 C15 1.414(6) . ? N2 C2 1.477(6) . ? C1 C2 1.506(7) . ? C3 C8 1.403(8) . ? C3 C4 1.405(9) . ? C4 C5 1.400(8) . ? C4 C9 1.502(8) . ? C5 C6 1.377(9) . ? C6 C7 1.347(10) . ? C7 C8 1.400(9) . ? C8 C12 1.508(10) . ? C9 C10 1.527(9) . ? C9 C11 1.536(8) . ? C12 C14 1.531(10) . ? C12 C13 1.537(11) . ? C15 C20 1.411(8) . ? C15 C16 1.425(7) . ? C16 C17 1.390(7) . ? C16 C21 1.506(8) . ? C17 C18 1.378(8) . ? C18 C19 1.366(8) . ? C19 C20 1.387(7) . ? C20 C24 1.516(8) . ? C21 C23 1.522(8) . ? C21 C22 1.536(8) . ? C24 C26 1.533(9) . ? C24 C25 1.537(9) . ? C27 C32 1.399(7) . ? C27 C28 1.414(7) . ? C28 C29 1.395(7) . ? C28 C33 1.545(8) . ? C29 C30 1.375(8) . ? C30 C31 1.399(8) . ? C30 C37 1.510(7) . ? C31 C32 1.404(8) . ? C32 C38 1.542(7) . ? C33 C36 1.493(9) . ? C33 C34 1.531(8) . ? C33 C35 1.554(9) . ? C38 C40 1.529(9) . ? C38 C39 1.539(8) . ? C38 C41 1.540(9) . ? C42 C43 1.469(11) . ? C43 C44 1.435(11) . ? C44 C45 1.496(10) . ? 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 Y N2 128.75(14) . . ? O1 Y N1 126.86(16) . . ? N2 Y N1 82.53(15) . . ? O1 Y O2 98.99(15) . . ? N2 Y O2 111.21(15) . . ? N1 Y O2 107.70(16) . . ? C27 O1 Y 160.1(4) . . ? C42 O2 C45 109.4(5) . . ? C42 O2 Y 129.4(4) . . ? C45 O2 Y 120.6(4) . . ? C3 N1 C1 116.2(4) . . ? C3 N1 Y 142.4(4) . . ? C1 N1 Y 100.6(3) . . ? C15 N2 C2 111.4(4) . . ? C15 N2 Y 137.0(3) . . ? C2 N2 Y 108.3(3) . . ? N1 C1 C2 112.9(5) . . ? N2 C2 C1 112.1(4) . . ? C8 C3 C4 120.3(5) . . ? C8 C3 N1 120.2(6) . . ? C4 C3 N1 119.5(5) . . ? C5 C4 C3 118.0(6) . . ? C5 C4 C9 120.0(6) . . ? C3 C4 C9 121.8(5) . . ? C6 C5 C4 121.7(7) . . ? C7 C6 C5 119.3(6) . . ? C6 C7 C8 122.5(7) . . ? C7 C8 C3 118.1(7) . . ? C7 C8 C12 119.8(6) . . ? C3 C8 C12 122.1(6) . . ? C4 C9 C10 114.4(5) . . ? C4 C9 C11 110.7(5) . . ? C10 C9 C11 109.7(6) . . ? C8 C12 C14 112.9(7) . . ? C8 C12 C13 111.1(6) . . ? C14 C12 C13 111.1(7) . . ? C20 C15 N2 120.5(5) . . ? C20 C15 C16 119.4(5) . . ? N2 C15 C16 120.0(5) . . ? C17 C16 C15 118.9(5) . . ? C17 C16 C21 118.4(5) . . ? C15 C16 C21 122.7(5) . . ? C18 C17 C16 121.0(5) . . ? C19 C18 C17 119.9(5) . . ? C18 C19 C20 122.1(6) . . ? C19 C20 C15 118.6(5) . . ? C19 C20 C24 120.0(5) . . ? C15 C20 C24 121.4(5) . . ? C16 C21 C23 111.3(5) . . ? C16 C21 C22 113.3(5) . . ? C23 C21 C22 109.7(5) . . ? C20 C24 C26 110.8(5) . . ? C20 C24 C25 111.6(5) . . ? C26 C24 C25 111.0(6) . . ? O1 C27 C32 117.8(5) . . ? O1 C27 C28 120.4(5) . . ? C32 C27 C28 121.8(5) . . ? C29 C28 C27 116.8(5) . . ? C29 C28 C33 117.2(5) . . ? C27 C28 C33 125.9(5) . . ? C30 C29 C28 123.9(5) . . ? C29 C30 C31 117.5(5) . . ? C29 C30 C37 122.0(5) . . ? C31 C30 C37 120.5(6) . . ? C30 C31 C32 122.1(5) . . ? C27 C32 C31 117.9(5) . . ? C27 C32 C38 122.4(5) . . ? C31 C32 C38 119.7(5) . . ? C36 C33 C34 106.6(6) . . ? C36 C33 C28 111.2(5) . . ? C34 C33 C28 118.1(5) . . ? C36 C33 C35 108.1(6) . . ? C34 C33 C35 104.3(5) . . ? C28 C33 C35 108.0(5) . . ? C40 C38 C39 110.2(5) . . ? C40 C38 C41 106.3(5) . . ? C39 C38 C41 106.9(6) . . ? C40 C38 C32 111.2(5) . . ? C39 C38 C32 109.8(4) . . ? C41 C38 C32 112.3(5) . . ? O2 C42 C43 106.0(7) . . ? C44 C43 C42 105.4(8) . . ? C43 C44 C45 105.5(6) . . ? O2 C45 C44 104.5(6) . . ? #===END data_[Si{ArN(CH2)NAr}PhH]_[16] _database_code_depnum_ccdc_archive 'CCDC 228151' _audit_creation_date 2003-06-13T09:33:35-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C32 H44 N2 Si1' _chemical_formula_sum 'C32 H44 N2 Si1' _chemical_formula_weight 484.78 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 16.7778(3) _cell_length_b 9.6378(1) _cell_length_c 19.7477(3) _cell_angle_alpha 90 _cell_angle_beta 109.171(1) _cell_angle_gamma 90 _cell_volume 3016.14(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 17916 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.068 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.099 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.295495E-1 _diffrn_orient_matrix_ub_12 -0.83542E-2 _diffrn_orient_matrix_ub_13 0.528017E-1 _diffrn_orient_matrix_ub_21 -0.555617E-1 _diffrn_orient_matrix_ub_22 0.42002E-2 _diffrn_orient_matrix_ub_23 0.8415E-2 _diffrn_orient_matrix_ub_31 -0.46473E-2 _diffrn_orient_matrix_ub_32 -0.103336 _diffrn_orient_matrix_ub_33 -0.39267E-2 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0608 _diffrn_reflns_av_unetI/netI 0.0354 _diffrn_reflns_number 27657 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.75 _diffrn_reflns_theta_max 25.02 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _reflns_number_total 5266 _reflns_number_gt 4375 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The H on Si was refined ; other H atoms were riding. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0428P)^2^+1.1643P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 5266 _refine_ls_number_parameters 320 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0542 _refine_ls_R_factor_gt 0.0414 _refine_ls_wR_factor_ref 0.1059 _refine_ls_wR_factor_gt 0.0984 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.199 _refine_diff_density_min -0.263 _refine_diff_density_rms 0.033 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' 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 Si Si 0.28880(3) 0.48351(4) 0.02390(2) 0.02704(13) Uani 1 1 d . . . H1 H 0.2904(10) 0.4273(16) -0.0400(8) 0.032(4) Uiso 1 1 d . . . N1 N 0.25794(8) 0.65342(13) 0.01277(7) 0.0298(3) Uani 1 1 d . . . N2 N 0.20764(8) 0.43527(12) 0.05405(7) 0.0286(3) Uani 1 1 d . . . C1 C 0.19013(11) 0.68427(17) 0.04239(9) 0.0368(4) Uani 1 1 d . . . H1A H 0.1499 0.7515 0.0114 0.044 Uiso 1 1 calc R . . H1B H 0.2139 0.7247 0.091 0.044 Uiso 1 1 calc R . . C2 C 0.14555(10) 0.54748(16) 0.04558(10) 0.0360(4) Uani 1 1 d . . . H2A H 0.124 0.5479 0.0866 0.043 Uiso 1 1 calc R . . H2B H 0.0973 0.5339 0.001 0.043 Uiso 1 1 calc R . . C3 C 0.28122(10) 0.75580(16) -0.03007(8) 0.0320(4) Uani 1 1 d . . . C4 C 0.24060(10) 0.75644(18) -0.10480(9) 0.0371(4) Uani 1 1 d . . . C5 C 0.26701(12) 0.8523(2) -0.14596(10) 0.0466(5) Uani 1 1 d . . . H5 H 0.2406 0.8533 -0.1965 0.056 Uiso 1 1 calc R . . C6 C 0.33054(12) 0.9453(2) -0.11463(10) 0.0487(5) Uani 1 1 d . . . H6 H 0.3484 1.0088 -0.1436 0.058 Uiso 1 1 calc R . . C7 C 0.36835(12) 0.94649(19) -0.04132(10) 0.0447(4) Uani 1 1 d . . . H7 H 0.4115 1.0123 -0.0201 0.054 Uiso 1 1 calc R . . C8 C 0.34460(10) 0.85313(17) 0.00243(9) 0.0359(4) Uani 1 1 d . . . C9 C 0.16867(11) 0.6580(2) -0.14119(10) 0.0476(5) Uani 1 1 d . . . H9 H 0.1624 0.593 -0.1038 0.057 Uiso 1 1 calc R . . C10 C 0.18609(17) 0.5709(3) -0.19912(12) 0.0746(7) Uani 1 1 d . . . H10A H 0.1382 0.509 -0.2209 0.112 Uiso 1 1 calc R . . H10B H 0.2372 0.5156 -0.1778 0.112 Uiso 1 1 calc R . . H10C H 0.1941 0.6321 -0.236 0.112 Uiso 1 1 calc R . . C11 C 0.08546(14) 0.7380(3) -0.17173(14) 0.0818(8) Uani 1 1 d . . . H11A H 0.0398 0.6729 -0.1949 0.123 Uiso 1 1 calc R . . H11B H 0.0906 0.8059 -0.207 0.123 Uiso 1 1 calc R . . H11C H 0.0729 0.7863 -0.1328 0.123 Uiso 1 1 calc R . . C12 C 0.38885(11) 0.85768(19) 0.08257(9) 0.0429(4) Uani 1 1 d . . . H12 H 0.3575 0.7951 0.1054 0.051 Uiso 1 1 calc R . . C13 C 0.38720(17) 1.0042(2) 0.11246(12) 0.0698(7) Uani 1 1 d . . . H13A H 0.4161 1.0037 0.1644 0.105 Uiso 1 1 calc R . . H13B H 0.3286 1.0337 0.1024 0.105 Uiso 1 1 calc R . . H13C H 0.4158 1.0686 0.0897 0.105 Uiso 1 1 calc R . . C14 C 0.47905(12) 0.8028(2) 0.10187(10) 0.0590(6) Uani 1 1 d . . . H14A H 0.5064 0.8062 0.154 0.088 Uiso 1 1 calc R . . H14B H 0.5108 0.8603 0.0787 0.088 Uiso 1 1 calc R . . H14C H 0.4778 0.7067 0.0853 0.088 Uiso 1 1 calc R . . C15 C 0.17750(9) 0.29781(15) 0.06128(8) 0.0297(3) Uani 1 1 d . . . C16 C 0.13681(10) 0.21819(17) -0.00028(9) 0.0358(4) Uani 1 1 d . . . C17 C 0.10831(11) 0.08574(18) 0.00934(10) 0.0450(5) Uani 1 1 d . . . H17 H 0.0821 0.0297 -0.0315 0.054 Uiso 1 1 calc R . . C18 C 0.11720(11) 0.03469(18) 0.07629(11) 0.0463(5) Uani 1 1 d . . . H18 H 0.0971 -0.0555 0.0814 0.056 Uiso 1 1 calc R . . C19 C 0.15530(11) 0.11441(17) 0.13606(10) 0.0397(4) Uani 1 1 d . . . H19 H 0.1606 0.0788 0.1822 0.048 Uiso 1 1 calc R . . C20 C 0.18622(10) 0.24681(16) 0.12993(9) 0.0319(4) Uani 1 1 d . . . C21 C 0.12299(10) 0.27041(19) -0.07564(9) 0.0402(4) Uani 1 1 d . . . H21 H 0.1449 0.3676 -0.0717 0.048 Uiso 1 1 calc R . . C22 C 0.17243(13) 0.1846(2) -0.11334(11) 0.0561(5) Uani 1 1 d . . . H22A H 0.1624 0.2212 -0.1617 0.084 Uiso 1 1 calc R . . H22B H 0.1538 0.0877 -0.1164 0.084 Uiso 1 1 calc R . . H22C H 0.2328 0.1897 -0.0861 0.084 Uiso 1 1 calc R . . C23 C 0.02926(12) 0.2745(2) -0.12074(11) 0.0602(6) Uani 1 1 d . . . H23A H 0.0231 0.3093 -0.1688 0.09 Uiso 1 1 calc R . . H23B H -0.0008 0.3362 -0.0979 0.09 Uiso 1 1 calc R . . H23C H 0.0055 0.1809 -0.1243 0.09 Uiso 1 1 calc R . . C24 C 0.22791(10) 0.32994(16) 0.19775(9) 0.0334(4) Uani 1 1 d . . . H24 H 0.2458 0.4211 0.1832 0.04 Uiso 1 1 calc R . . C25 C 0.16649(13) 0.3594(2) 0.23855(11) 0.0504(5) Uani 1 1 d . . . H25A H 0.1952 0.4134 0.2817 0.076 Uiso 1 1 calc R . . H25B H 0.1467 0.2715 0.2522 0.076 Uiso 1 1 calc R . . H25C H 0.1182 0.4122 0.2078 0.076 Uiso 1 1 calc R . . C26 C 0.30683(12) 0.25698(19) 0.24647(10) 0.0466(5) Uani 1 1 d . . . H26A H 0.3324 0.3132 0.2895 0.07 Uiso 1 1 calc R . . H26B H 0.3474 0.2451 0.2208 0.07 Uiso 1 1 calc R . . H26C H 0.2913 0.1659 0.2604 0.07 Uiso 1 1 calc R . . C27 C 0.39538(10) 0.44451(16) 0.08760(9) 0.0319(4) Uani 1 1 d . . . C28 C 0.41952(11) 0.4738(2) 0.16062(9) 0.0422(4) Uani 1 1 d . . . H28 H 0.3795 0.5124 0.18 0.051 Uiso 1 1 calc R . . C29 C 0.50107(13) 0.4477(2) 0.20561(11) 0.0577(6) Uani 1 1 d . . . H29 H 0.5164 0.4671 0.2554 0.069 Uiso 1 1 calc R . . C30 C 0.55974(13) 0.3935(3) 0.17786(12) 0.0671(7) Uani 1 1 d . . . H30 H 0.6156 0.3761 0.2086 0.08 Uiso 1 1 calc R . . C31 C 0.53803(12) 0.3647(2) 0.10625(13) 0.0623(6) Uani 1 1 d . . . H31 H 0.5789 0.328 0.0873 0.075 Uiso 1 1 calc R . . C32 C 0.45643(11) 0.38916(19) 0.06134(10) 0.0429(4) Uani 1 1 d . . . H32 H 0.4417 0.3679 0.0118 0.052 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 Si 0.0264(2) 0.0292(2) 0.0259(2) -0.00278(17) 0.00914(17) -0.00008(17) N1 0.0328(7) 0.0292(7) 0.0305(7) 0.0030(5) 0.0146(6) 0.0011(6) N2 0.0287(7) 0.0236(6) 0.0352(7) -0.0030(5) 0.0128(6) -0.0002(5) C1 0.0443(10) 0.0294(8) 0.0451(10) -0.0006(7) 0.0259(8) 0.0029(7) C2 0.0345(9) 0.0298(8) 0.0487(10) -0.0001(7) 0.0205(8) 0.0040(7) C3 0.0351(9) 0.0320(8) 0.0317(9) 0.0040(7) 0.0148(7) 0.0034(7) C4 0.0372(9) 0.0404(9) 0.0326(9) 0.0047(7) 0.0101(7) 0.0059(7) C5 0.0512(11) 0.0554(12) 0.0326(10) 0.0121(8) 0.0130(8) 0.0082(9) C6 0.0562(12) 0.0494(11) 0.0445(11) 0.0155(9) 0.0221(9) -0.0018(9) C7 0.0500(11) 0.0455(10) 0.0418(10) 0.0059(8) 0.0194(9) -0.0092(8) C8 0.0396(9) 0.0364(9) 0.0352(9) 0.0030(7) 0.0172(7) -0.0039(7) C9 0.0454(10) 0.0547(11) 0.0354(10) 0.0044(8) 0.0035(8) -0.0017(9) C10 0.0910(18) 0.0815(17) 0.0477(13) -0.0208(12) 0.0180(12) -0.0196(14) C11 0.0479(13) 0.0927(19) 0.0854(18) 0.0062(15) -0.0046(12) 0.0002(13) C12 0.0526(11) 0.0463(10) 0.0328(9) -0.0028(8) 0.0182(8) -0.0215(9) C13 0.111(2) 0.0564(13) 0.0538(13) -0.0161(11) 0.0433(13) -0.0306(13) C14 0.0526(12) 0.0794(15) 0.0391(11) 0.0109(10) 0.0072(9) -0.0220(11) C15 0.0244(7) 0.0241(8) 0.0404(9) -0.0039(7) 0.0105(7) -0.0002(6) C16 0.0290(8) 0.0322(9) 0.0425(10) -0.0069(7) 0.0068(7) 0.0008(7) C17 0.0395(10) 0.0317(9) 0.0551(12) -0.0132(8) 0.0039(8) -0.0063(8) C18 0.0440(10) 0.0275(9) 0.0636(13) -0.0006(9) 0.0125(9) -0.0067(8) C19 0.0414(10) 0.0278(8) 0.0490(11) 0.0013(8) 0.0134(8) -0.0041(7) C20 0.0294(8) 0.0260(8) 0.0413(9) -0.0018(7) 0.0130(7) -0.0012(6) C21 0.0353(9) 0.0408(10) 0.0382(10) -0.0103(8) 0.0036(7) -0.0010(7) C22 0.0550(12) 0.0617(13) 0.0485(12) -0.0182(10) 0.0128(9) 0.0008(10) C23 0.0405(11) 0.0756(15) 0.0518(12) -0.0030(11) -0.0023(9) 0.0007(10) C24 0.0388(9) 0.0276(8) 0.0361(9) -0.0013(7) 0.0156(7) -0.0047(7) C25 0.0606(12) 0.0460(11) 0.0556(12) -0.0080(9) 0.0341(10) -0.0097(9) C26 0.0531(11) 0.0383(10) 0.0415(10) -0.0008(8) 0.0062(9) -0.0012(8) C27 0.0293(8) 0.0325(8) 0.0338(9) 0.0044(7) 0.0102(7) -0.0021(7) C28 0.0359(9) 0.0542(11) 0.0357(9) 0.0038(8) 0.0107(7) -0.0064(8) C29 0.0481(12) 0.0805(15) 0.0365(11) 0.0140(10) 0.0028(9) -0.0130(11) C30 0.0342(11) 0.0950(18) 0.0628(15) 0.0302(13) 0.0034(10) 0.0051(11) C31 0.0365(10) 0.0800(16) 0.0715(15) 0.0214(12) 0.0194(10) 0.0194(10) C32 0.0355(9) 0.0476(10) 0.0470(11) 0.0062(8) 0.0153(8) 0.0072(8) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Si N1 1.7098(13) . ? Si N2 1.7196(13) . ? Si C27 1.8557(16) . ? N1 C3 1.435(2) . ? N1 C1 1.4704(19) . ? N2 C15 1.4418(19) . ? N2 C2 1.4725(19) . ? C1 C2 1.527(2) . ? C3 C8 1.405(2) . ? C3 C4 1.408(2) . ? C4 C5 1.396(2) . ? C4 C9 1.517(2) . ? C5 C6 1.374(3) . ? C6 C7 1.377(3) . ? C7 C8 1.393(2) . ? C8 C12 1.512(2) . ? C9 C10 1.523(3) . ? C9 C11 1.534(3) . ? C12 C14 1.528(3) . ? C12 C13 1.534(3) . ? C15 C20 1.404(2) . ? C15 C16 1.410(2) . ? C16 C17 1.398(2) . ? C16 C21 1.515(2) . ? C17 C18 1.372(3) . ? C18 C19 1.377(3) . ? C19 C20 1.398(2) . ? C20 C24 1.520(2) . ? C21 C22 1.527(3) . ? C21 C23 1.532(2) . ? C24 C26 1.529(2) . ? C24 C25 1.529(2) . ? C27 C28 1.393(2) . ? C27 C32 1.397(2) . ? C28 C29 1.388(3) . ? C29 C30 1.377(3) . ? C30 C31 1.368(3) . ? C31 C32 1.385(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 N1 Si N2 93.59(6) . . ? N1 Si C27 117.70(7) . . ? N2 Si C27 114.02(7) . . ? C3 N1 C1 119.44(12) . . ? C3 N1 Si 127.22(10) . . ? C1 N1 Si 112.56(10) . . ? C15 N2 C2 115.35(12) . . ? C15 N2 Si 128.76(10) . . ? C2 N2 Si 111.92(10) . . ? N1 C1 C2 107.17(12) . . ? N2 C2 C1 107.51(12) . . ? C8 C3 C4 120.60(15) . . ? C8 C3 N1 120.10(14) . . ? C4 C3 N1 119.29(14) . . ? C5 C4 C3 118.45(16) . . ? C5 C4 C9 119.56(15) . . ? C3 C4 C9 121.98(15) . . ? C6 C5 C4 121.15(17) . . ? C5 C6 C7 120.01(17) . . ? C6 C7 C8 121.33(17) . . ? C7 C8 C3 118.40(15) . . ? C7 C8 C12 119.23(15) . . ? C3 C8 C12 122.36(14) . . ? C4 C9 C10 112.42(17) . . ? C4 C9 C11 110.58(17) . . ? C10 C9 C11 110.86(18) . . ? C8 C12 C14 110.89(15) . . ? C8 C12 C13 111.40(16) . . ? C14 C12 C13 111.34(17) . . ? C20 C15 C16 120.64(14) . . ? C20 C15 N2 119.26(13) . . ? C16 C15 N2 120.06(14) . . ? C17 C16 C15 118.05(16) . . ? C17 C16 C21 119.21(15) . . ? C15 C16 C21 122.74(15) . . ? C18 C17 C16 121.64(16) . . ? C17 C18 C19 119.92(16) . . ? C18 C19 C20 121.07(17) . . ? C19 C20 C15 118.65(15) . . ? C19 C20 C24 118.78(15) . . ? C15 C20 C24 122.57(14) . . ? C16 C21 C22 111.49(15) . . ? C16 C21 C23 112.12(15) . . ? C22 C21 C23 110.41(15) . . ? C20 C24 C26 111.41(13) . . ? C20 C24 C25 111.57(14) . . ? C26 C24 C25 110.39(15) . . ? C28 C27 C32 117.54(15) . . ? C28 C27 Si 123.27(13) . . ? C32 C27 Si 119.12(13) . . ? C29 C28 C27 121.08(18) . . ? C30 C29 C28 119.83(19) . . ? C31 C30 C29 120.39(18) . . ? C30 C31 C32 119.93(19) . . ? C31 C32 C27 121.22(18) . . ? #===END data_[Y(thf)(OC6H2tBu2Me)(C6H3iPr2N(CH2)3NC6H3iPr2)] _database_code_depnum_ccdc_archive 'CCDC 228152' _audit_creation_date 2002-03-19T09:17:06-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common ; '[Y(thf)(OC6H2tBu2Me)(C6H3iPr2N(CH2)3NC6H3iPr2)]' ; _chemical_formula_moiety 'C46 H63 N2 O2 Y1' _chemical_formula_sum 'C46 H63 N2 O2 Y' _chemical_formula_weight 764.89 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_Int_Tables_number 14 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 9.7063(2) _cell_length_b 24.9099(6) _cell_length_c 18.6024(4) _cell_angle_alpha 90 _cell_angle_beta 97.802(1) _cell_angle_gamma 90 _cell_volume 4456.11(17) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 20353 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 24.108 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.14 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1632 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.344 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.7229 _exptl_absorpt_correction_T_max 0.7957 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.34786E-2 _diffrn_orient_matrix_ub_12 -0.8333E-3 _diffrn_orient_matrix_ub_13 0.534684E-1 _diffrn_orient_matrix_ub_21 -0.58334E-1 _diffrn_orient_matrix_ub_22 -0.332019E-1 _diffrn_orient_matrix_ub_23 -0.60649E-2 _diffrn_orient_matrix_ub_31 0.860153E-1 _diffrn_orient_matrix_ub_32 -0.225507E-1 _diffrn_orient_matrix_ub_33 0.69538E-2 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0973 _diffrn_reflns_av_unetI/netI 0.0726 _diffrn_reflns_number 26024 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.76 _diffrn_reflns_theta_max 24.14 _diffrn_reflns_theta_full 24.14 _diffrn_measured_fraction_theta_full 0.946 _diffrn_measured_fraction_theta_max 0.946 _reflns_number_total 6731 _reflns_number_gt 4644 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0371P)^2^+10.5033P] 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 riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.0012(4) _refine_ls_number_reflns 6731 _refine_ls_number_parameters 461 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1055 _refine_ls_R_factor_gt 0.061 _refine_ls_wR_factor_ref 0.1361 _refine_ls_wR_factor_gt 0.1164 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.484 _refine_diff_density_min -0.366 _refine_diff_density_rms 0.071 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Y Y 0.50645(5) 0.141374(17) 0.25134(2) 0.02810(17) Uani 1 1 d . . . O1 O 0.6247(3) 0.12244(12) 0.16878(16) 0.0328(8) Uani 1 1 d . . . O2 O 0.2931(3) 0.12068(14) 0.18455(17) 0.0405(9) Uani 1 1 d . . . N1 N 0.5320(4) 0.09577(16) 0.35104(19) 0.0343(10) Uani 1 1 d . . . N2 N 0.4707(4) 0.21859(15) 0.3015(2) 0.0386(10) Uani 1 1 d . . . C1 C 0.4721(6) 0.1194(2) 0.4132(3) 0.0442(14) Uani 1 1 d . . . H1A H 0.5479 0.1355 0.4473 0.053 Uiso 1 1 calc R . . H1B H 0.4299 0.0903 0.4393 0.053 Uiso 1 1 calc R . . C2 C 0.3634(6) 0.1615(2) 0.3910(3) 0.0455(14) Uani 1 1 d . . . H2A H 0.3068 0.166 0.431 0.055 Uiso 1 1 calc R . . H2B H 0.301 0.148 0.3484 0.055 Uiso 1 1 calc R . . C3 C 0.4164(7) 0.2166(2) 0.3722(3) 0.0574(17) Uani 1 1 d . . . H3A H 0.3396 0.2429 0.3713 0.069 Uiso 1 1 calc R . . H3B H 0.4912 0.2277 0.4109 0.069 Uiso 1 1 calc R . . C4 C 0.6109(6) 0.0487(2) 0.3718(2) 0.0400(13) Uani 1 1 d . . . C5 C 0.5415(7) -0.0011(2) 0.3731(3) 0.0486(15) Uani 1 1 d . . . C6 C 0.6190(9) -0.0471(2) 0.3899(3) 0.069(2) Uani 1 1 d . . . H6 H 0.5732 -0.0808 0.39 0.083 Uiso 1 1 calc R . . C7 C 0.7606(10) -0.0447(3) 0.4063(4) 0.080(2) Uani 1 1 d . . . H7 H 0.8116 -0.0768 0.4175 0.096 Uiso 1 1 calc R . . C8 C 0.8312(8) 0.0039(3) 0.4071(3) 0.0687(19) Uani 1 1 d . . . H8 H 0.9295 0.0049 0.4187 0.082 Uiso 1 1 calc R . . C9 C 0.7561(6) 0.0514(2) 0.3905(3) 0.0463(14) Uani 1 1 d . . . C10 C 0.3842(7) -0.0052(2) 0.3570(3) 0.0581(17) Uani 1 1 d . . . H10 H 0.3474 0.0323 0.3514 0.07 Uiso 1 1 calc R . . C11 C 0.3185(8) -0.0309(3) 0.4176(3) 0.073(2) Uani 1 1 d . . . H11A H 0.2174 -0.0321 0.4042 0.109 Uiso 1 1 calc R . . H11B H 0.3411 -0.0097 0.4621 0.109 Uiso 1 1 calc R . . H11C H 0.3544 -0.0674 0.4259 0.109 Uiso 1 1 calc R . . C12 C 0.3350(10) -0.0345(4) 0.2868(4) 0.129(4) Uani 1 1 d . . . H12A H 0.3761 -0.0178 0.247 0.193 Uiso 1 1 calc R . . H12B H 0.2334 -0.0325 0.2766 0.193 Uiso 1 1 calc R . . H12C H 0.3637 -0.0722 0.2915 0.193 Uiso 1 1 calc R . . C13 C 0.8314(6) 0.1046(3) 0.3941(3) 0.0562(16) Uani 1 1 d . . . H13 H 0.7597 0.1328 0.3796 0.067 Uiso 1 1 calc R . . C14 C 0.9379(8) 0.1086(4) 0.3413(4) 0.106(3) Uani 1 1 d . . . H14A H 0.9823 0.144 0.3457 0.16 Uiso 1 1 calc R . . H14B H 0.8914 0.1037 0.2916 0.16 Uiso 1 1 calc R . . H14C H 1.0087 0.0807 0.3525 0.16 Uiso 1 1 calc R . . C15 C 0.8998(10) 0.1185(4) 0.4703(4) 0.107(3) Uani 1 1 d . . . H15A H 0.9459 0.1535 0.4697 0.16 Uiso 1 1 calc R . . H15B H 0.9688 0.091 0.4873 0.16 Uiso 1 1 calc R . . H15C H 0.8289 0.12 0.503 0.16 Uiso 1 1 calc R . . C16 C 0.5016(5) 0.2722(2) 0.2812(3) 0.0371(12) Uani 1 1 d . . . C17 C 0.6264(6) 0.2968(2) 0.3096(3) 0.0431(14) Uani 1 1 d . . . C18 C 0.6574(7) 0.3477(2) 0.2829(3) 0.0547(16) Uani 1 1 d . . . H18 H 0.7438 0.3641 0.3004 0.066 Uiso 1 1 calc R . . C19 C 0.5654(7) 0.3741(2) 0.2322(3) 0.0580(17) Uani 1 1 d . . . H19 H 0.5886 0.4082 0.2146 0.07 Uiso 1 1 calc R . . C20 C 0.4397(6) 0.3507(2) 0.2069(3) 0.0471(14) Uani 1 1 d . . . H20 H 0.3755 0.3695 0.1729 0.057 Uiso 1 1 calc R . . C21 C 0.4047(6) 0.3001(2) 0.2303(3) 0.0402(13) Uani 1 1 d . . . C22 C 0.7254(6) 0.2716(2) 0.3699(3) 0.0532(15) Uani 1 1 d . . . H22 H 0.6961 0.2335 0.3749 0.064 Uiso 1 1 calc R . . C23 C 0.8775(7) 0.2713(3) 0.3571(3) 0.084(2) Uani 1 1 d . . . H23A H 0.9342 0.2538 0.3981 0.125 Uiso 1 1 calc R . . H23B H 0.9095 0.3083 0.3526 0.125 Uiso 1 1 calc R . . H23C H 0.8863 0.2516 0.3123 0.125 Uiso 1 1 calc R . . C24 C 0.7143(7) 0.3002(3) 0.4422(3) 0.0639(18) Uani 1 1 d . . . H24A H 0.7775 0.2831 0.4811 0.096 Uiso 1 1 calc R . . H24B H 0.6186 0.2976 0.4532 0.096 Uiso 1 1 calc R . . H24C H 0.7397 0.3381 0.4384 0.096 Uiso 1 1 calc R . . C25 C 0.2638(6) 0.2773(2) 0.2029(3) 0.0554(16) Uani 1 1 d . . . H25 H 0.2695 0.2375 0.2094 0.067 Uiso 1 1 calc R . . C26 C 0.1554(8) 0.2980(5) 0.2478(4) 0.128(4) Uani 1 1 d . . . H26A H 0.0647 0.2824 0.2296 0.192 Uiso 1 1 calc R . . H26B H 0.1501 0.3372 0.2441 0.192 Uiso 1 1 calc R . . H26C H 0.1817 0.2876 0.2987 0.192 Uiso 1 1 calc R . . C27 C 0.2146(7) 0.2882(3) 0.1236(3) 0.0677(19) Uani 1 1 d . . . H27A H 0.1233 0.2716 0.1099 0.102 Uiso 1 1 calc R . . H27B H 0.2812 0.273 0.094 0.102 Uiso 1 1 calc R . . H27C H 0.2075 0.327 0.1155 0.102 Uiso 1 1 calc R . . C28 C 0.6827(5) 0.1144(2) 0.1069(2) 0.0311(11) Uani 1 1 d . . . C29 C 0.7230(5) 0.1588(2) 0.0674(2) 0.0350(12) Uani 1 1 d . . . C30 C 0.7780(5) 0.1485(2) 0.0027(2) 0.0396(13) Uani 1 1 d . . . H30 H 0.8038 0.1782 -0.0247 0.048 Uiso 1 1 calc R . . C31 C 0.7963(5) 0.0976(2) -0.0227(3) 0.0411(13) Uani 1 1 d . . . C32 C 0.7582(5) 0.0551(2) 0.0179(3) 0.0426(13) Uani 1 1 d . . . H32 H 0.7712 0.0197 0.0009 0.051 Uiso 1 1 calc R . . C33 C 0.7015(5) 0.0611(2) 0.0826(2) 0.0368(12) Uani 1 1 d . . . C34 C 0.7099(5) 0.2168(2) 0.0937(3) 0.0378(12) Uani 1 1 d . . . C35 C 0.7949(6) 0.2243(2) 0.1689(3) 0.0540(15) Uani 1 1 d . . . H35A H 0.7623 0.1989 0.2031 0.081 Uiso 1 1 calc R . . H35B H 0.7831 0.2611 0.1858 0.081 Uiso 1 1 calc R . . H35C H 0.8934 0.2177 0.1658 0.081 Uiso 1 1 calc R . . C36 C 0.5573(6) 0.2315(2) 0.0949(3) 0.0503(15) Uani 1 1 d . . . H36A H 0.5158 0.2063 0.1263 0.075 Uiso 1 1 calc R . . H36B H 0.5071 0.2295 0.0456 0.075 Uiso 1 1 calc R . . H36C H 0.5511 0.268 0.1136 0.075 Uiso 1 1 calc R . . C37 C 0.7664(7) 0.2577(2) 0.0435(3) 0.0602(17) Uani 1 1 d . . . H37A H 0.7558 0.294 0.0623 0.09 Uiso 1 1 calc R . . H37B H 0.7146 0.2547 -0.0053 0.09 Uiso 1 1 calc R . . H37C H 0.8651 0.2505 0.0416 0.09 Uiso 1 1 calc R . . C38 C 0.8546(7) 0.0884(3) -0.0934(3) 0.0594(17) Uani 1 1 d . . . H38A H 0.8599 0.0498 -0.1026 0.089 Uiso 0.5 1 calc PR . . H38B H 0.9479 0.1041 -0.09 0.089 Uiso 0.5 1 calc PR . . H38C H 0.7938 0.1054 -0.1333 0.089 Uiso 0.5 1 calc PR . . H38D H 0.8745 0.1231 -0.1147 0.089 Uiso 0.5 1 calc PR . . H38E H 0.7865 0.0688 -0.1273 0.089 Uiso 0.5 1 calc PR . . H38F H 0.9406 0.0674 -0.084 0.089 Uiso 0.5 1 calc PR . . C39 C 0.6597(6) 0.0112(2) 0.1237(3) 0.0448(14) Uani 1 1 d . . . C40 C 0.5034(6) 0.0111(3) 0.1284(3) 0.0627(18) Uani 1 1 d . . . H40A H 0.4796 -0.021 0.1546 0.094 Uiso 1 1 calc R . . H40B H 0.4516 0.0109 0.0794 0.094 Uiso 1 1 calc R . . H40C H 0.4791 0.0433 0.1543 0.094 Uiso 1 1 calc R . . C41 C 0.7426(7) 0.0089(2) 0.2001(3) 0.0614(17) Uani 1 1 d . . . H41A H 0.7148 -0.0229 0.2255 0.092 Uiso 1 1 calc R . . H41B H 0.7236 0.0412 0.2272 0.092 Uiso 1 1 calc R . . H41C H 0.8422 0.007 0.1963 0.092 Uiso 1 1 calc R . . C42 C 0.6890(9) -0.0415(2) 0.0857(3) 0.077(2) Uani 1 1 d . . . H42A H 0.6605 -0.0719 0.1136 0.115 Uiso 1 1 calc R . . H42B H 0.7887 -0.0441 0.0824 0.115 Uiso 1 1 calc R . . H42C H 0.6367 -0.042 0.0368 0.115 Uiso 1 1 calc R . . C43 C 0.2661(6) 0.1282(3) 0.1057(3) 0.0595(17) Uani 1 1 d . . . C44 C 0.1363(8) 0.0957(4) 0.0830(4) 0.114(4) Uani 1 1 d . . . C45 C 0.0688(8) 0.0850(4) 0.1472(4) 0.104(3) Uani 1 1 d . . . C46 C 0.1650(6) 0.1054(4) 0.2116(4) 0.088(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y 0.0349(3) 0.0296(3) 0.0211(2) 0.0001(2) 0.00836(17) -0.0016(2) O1 0.0362(19) 0.0377(19) 0.0257(17) 0.0004(15) 0.0087(14) 0.0007(15) O2 0.039(2) 0.051(2) 0.0306(18) -0.0025(16) 0.0015(15) -0.0033(17) N1 0.046(3) 0.034(2) 0.024(2) 0.0016(18) 0.0094(19) 0.000(2) N2 0.061(3) 0.029(2) 0.028(2) -0.0008(19) 0.015(2) -0.002(2) C1 0.067(4) 0.044(3) 0.026(3) 0.007(2) 0.023(3) -0.002(3) C2 0.061(4) 0.041(3) 0.039(3) 0.004(3) 0.023(3) 0.004(3) C3 0.105(5) 0.034(3) 0.041(3) 0.002(3) 0.035(3) -0.003(3) C4 0.059(4) 0.043(3) 0.019(2) 0.001(2) 0.010(2) 0.006(3) C5 0.078(4) 0.043(4) 0.026(3) 0.001(2) 0.010(3) -0.003(3) C6 0.123(7) 0.039(4) 0.049(4) 0.004(3) 0.020(4) 0.010(4) C7 0.117(7) 0.058(5) 0.069(5) 0.011(4) 0.028(5) 0.041(5) C8 0.074(5) 0.092(6) 0.043(4) 0.012(4) 0.017(3) 0.029(4) C9 0.050(4) 0.062(4) 0.029(3) 0.005(3) 0.015(3) 0.011(3) C10 0.083(5) 0.054(4) 0.034(3) 0.010(3) 0.000(3) -0.025(3) C11 0.105(6) 0.070(5) 0.043(4) 0.004(3) 0.011(4) -0.018(4) C12 0.155(9) 0.188(10) 0.046(4) -0.019(5) 0.025(5) -0.096(8) C13 0.041(3) 0.084(5) 0.044(3) 0.007(3) 0.010(3) -0.006(3) C14 0.097(6) 0.146(8) 0.085(6) -0.027(5) 0.049(5) -0.052(6) C15 0.146(8) 0.124(7) 0.048(4) -0.004(4) 0.004(5) -0.050(6) C16 0.052(3) 0.033(3) 0.029(2) -0.009(2) 0.015(2) -0.006(3) C17 0.063(4) 0.043(3) 0.024(3) -0.007(2) 0.007(3) -0.007(3) C18 0.069(4) 0.049(4) 0.046(3) -0.010(3) 0.007(3) -0.029(3) C19 0.091(5) 0.040(3) 0.044(3) 0.003(3) 0.014(3) -0.015(3) C20 0.069(4) 0.035(3) 0.037(3) 0.000(3) 0.007(3) 0.000(3) C21 0.056(3) 0.030(3) 0.036(3) 0.002(2) 0.010(3) -0.002(3) C22 0.071(4) 0.057(4) 0.030(3) -0.006(3) 0.001(3) -0.008(3) C23 0.075(5) 0.120(7) 0.052(4) -0.012(4) 0.000(4) -0.006(5) C24 0.095(5) 0.064(4) 0.031(3) -0.007(3) 0.003(3) -0.008(4) C25 0.061(4) 0.040(3) 0.063(4) 0.005(3) -0.003(3) -0.009(3) C26 0.071(5) 0.239(12) 0.080(6) -0.034(7) 0.034(5) -0.059(7) C27 0.058(4) 0.077(5) 0.063(4) -0.007(4) -0.007(3) 0.009(4) C28 0.032(3) 0.042(3) 0.020(2) -0.004(2) 0.007(2) 0.003(2) C29 0.033(3) 0.045(3) 0.027(3) -0.001(2) 0.005(2) -0.001(2) C30 0.042(3) 0.053(4) 0.026(3) -0.001(3) 0.013(2) -0.008(3) C31 0.042(3) 0.055(4) 0.029(3) -0.005(3) 0.013(2) -0.004(3) C32 0.048(3) 0.045(3) 0.034(3) -0.009(3) 0.005(3) 0.004(3) C33 0.041(3) 0.050(3) 0.021(2) 0.001(2) 0.008(2) 0.004(3) C34 0.045(3) 0.038(3) 0.033(3) -0.004(2) 0.015(2) -0.005(2) C35 0.058(4) 0.063(4) 0.043(3) -0.010(3) 0.012(3) -0.010(3) C36 0.064(4) 0.048(4) 0.040(3) 0.007(3) 0.012(3) 0.003(3) C37 0.082(5) 0.050(4) 0.054(4) 0.003(3) 0.029(3) -0.012(3) C38 0.074(4) 0.071(4) 0.039(3) -0.007(3) 0.028(3) 0.000(4) C39 0.069(4) 0.040(3) 0.026(3) 0.002(2) 0.013(3) 0.009(3) C40 0.064(4) 0.058(4) 0.070(4) 0.002(3) 0.022(3) -0.019(3) C41 0.088(5) 0.062(4) 0.034(3) 0.012(3) 0.011(3) 0.018(4) C42 0.146(7) 0.038(4) 0.053(4) 0.001(3) 0.037(4) 0.014(4) C43 0.061(4) 0.085(5) 0.029(3) 0.003(3) -0.007(3) -0.013(3) C44 0.064(5) 0.224(11) 0.056(4) -0.037(6) 0.008(4) -0.061(6) C45 0.069(5) 0.165(9) 0.075(5) -0.001(5) -0.005(4) -0.038(6) C46 0.034(3) 0.169(8) 0.064(4) 0.007(5) 0.013(3) -0.028(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Y O1 2.092(3) . ? Y N1 2.160(4) . ? Y N2 2.186(4) . ? Y O2 2.324(3) . ? O1 C28 1.364(5) . ? O2 C46 1.453(7) . ? O2 C43 1.467(6) . ? N1 C4 1.426(6) . ? N1 C1 1.485(6) . ? N2 C16 1.430(6) . ? N2 C3 1.481(6) . ? C1 C2 1.506(7) . ? C2 C3 1.523(7) . ? C4 C9 1.406(7) . ? C4 C5 1.412(7) . ? C5 C6 1.384(8) . ? C5 C10 1.519(8) . ? C6 C7 1.368(10) . ? C7 C8 1.390(10) . ? C8 C9 1.402(8) . ? C9 C13 1.511(8) . ? C10 C11 1.510(8) . ? C10 C12 1.516(8) . ? C13 C15 1.522(8) . ? C13 C14 1.523(8) . ? C16 C17 1.397(7) . ? C16 C21 1.421(7) . ? C17 C18 1.408(7) . ? C17 C22 1.511(7) . ? C18 C19 1.376(8) . ? C19 C20 1.376(8) . ? C20 C21 1.392(7) . ? C21 C25 1.504(7) . ? C22 C23 1.527(8) . ? C22 C24 1.538(7) . ? C25 C27 1.512(8) . ? C25 C26 1.520(9) . ? C28 C29 1.412(7) . ? C28 C33 1.422(7) . ? C29 C30 1.403(7) . ? C29 C34 1.537(7) . ? C30 C31 1.373(7) . ? C31 C32 1.381(7) . ? C31 C38 1.519(7) . ? C32 C33 1.397(7) . ? C33 C39 1.541(7) . ? C34 C36 1.529(7) . ? C34 C37 1.531(7) . ? C34 C35 1.536(7) . ? C39 C40 1.531(8) . ? C39 C42 1.536(7) . ? C39 C41 1.537(7) . ? C43 C44 1.509(9) . ? C44 C45 1.462(10) . ? C45 C46 1.504(9) . ? 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 Y N1 120.08(14) . . ? O1 Y N2 130.28(14) . . ? N1 Y N2 95.87(14) . . ? O1 Y O2 95.48(12) . . ? N1 Y O2 109.42(13) . . ? N2 Y O2 103.99(14) . . ? C28 O1 Y 169.6(3) . . ? C46 O2 C43 109.5(4) . . ? C46 O2 Y 128.0(3) . . ? C43 O2 Y 122.1(3) . . ? C4 N1 C1 111.6(4) . . ? C4 N1 Y 131.3(3) . . ? C1 N1 Y 116.7(3) . . ? C16 N2 C3 112.2(4) . . ? C16 N2 Y 131.0(3) . . ? C3 N2 Y 116.5(3) . . ? N1 C1 C2 113.3(4) . . ? C1 C2 C3 116.5(5) . . ? N2 C3 C2 114.0(4) . . ? C9 C4 C5 120.2(5) . . ? C9 C4 N1 120.7(5) . . ? C5 C4 N1 119.1(5) . . ? C6 C5 C4 119.0(6) . . ? C6 C5 C10 119.2(6) . . ? C4 C5 C10 121.7(5) . . ? C7 C6 C5 120.8(7) . . ? C6 C7 C8 121.3(6) . . ? C7 C8 C9 119.5(7) . . ? C8 C9 C4 119.1(6) . . ? C8 C9 C13 119.8(6) . . ? C4 C9 C13 121.1(5) . . ? C11 C10 C12 108.9(5) . . ? C11 C10 C5 113.4(5) . . ? C12 C10 C5 113.2(6) . . ? C9 C13 C15 112.8(5) . . ? C9 C13 C14 113.3(6) . . ? C15 C13 C14 109.7(6) . . ? C17 C16 C21 119.9(5) . . ? C17 C16 N2 120.8(5) . . ? C21 C16 N2 119.3(4) . . ? C16 C17 C18 118.5(5) . . ? C16 C17 C22 122.0(5) . . ? C18 C17 C22 119.4(5) . . ? C19 C18 C17 121.5(5) . . ? C20 C19 C18 119.7(5) . . ? C19 C20 C21 121.3(5) . . ? C20 C21 C16 119.0(5) . . ? C20 C21 C25 119.0(5) . . ? C16 C21 C25 122.0(5) . . ? C17 C22 C23 114.6(5) . . ? C17 C22 C24 110.1(5) . . ? C23 C22 C24 108.9(5) . . ? C21 C25 C27 114.6(5) . . ? C21 C25 C26 110.6(5) . . ? C27 C25 C26 109.0(6) . . ? O1 C28 C29 120.0(4) . . ? O1 C28 C33 119.4(4) . . ? C29 C28 C33 120.6(4) . . ? C30 C29 C28 117.9(5) . . ? C30 C29 C34 120.1(4) . . ? C28 C29 C34 122.0(4) . . ? C31 C30 C29 123.1(5) . . ? C30 C31 C32 117.6(4) . . ? C30 C31 C38 121.3(5) . . ? C32 C31 C38 121.1(5) . . ? C31 C32 C33 123.7(5) . . ? C32 C33 C28 117.2(5) . . ? C32 C33 C39 120.1(5) . . ? C28 C33 C39 122.7(4) . . ? C36 C34 C37 106.2(5) . . ? C36 C34 C35 111.0(4) . . ? C37 C34 C35 106.4(4) . . ? C36 C34 C29 110.6(4) . . ? C37 C34 C29 112.3(4) . . ? C35 C34 C29 110.3(4) . . ? C40 C39 C42 105.8(5) . . ? C40 C39 C41 110.2(5) . . ? C42 C39 C41 106.7(5) . . ? C40 C39 C33 111.1(4) . . ? C42 C39 C33 112.5(4) . . ? C41 C39 C33 110.4(5) . . ? O2 C43 C44 103.9(5) . . ? C45 C44 C43 108.6(6) . . ? C44 C45 C46 106.9(6) . . ? O2 C46 C45 106.3(5) . . ? #===END