# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Sjoerd Harder' _publ_contact_author_address ; Anorganische Chemie, Universit\"at Duisburg-Essen Essen 45117 GERMANY ; _publ_contact_author_email SJOERD.HARDER@UNI-DUE.DE _publ_section_title ; Syntheses and Structures of Bora-Amidinate Lanthanide(III) Complexes ; _publ_author_name 'Sjoerd Harder' # Attachment 'hasj192-NBNSmNR2.cif' data_hasj192 _database_code_depnum_ccdc_archive 'CCDC 763734' #TrackingRef 'hasj192-NBNSmNR2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (DIPP-NBN)SmNTMS2.(THF)2 _chemical_melting_point ? _chemical_formula_moiety 'C38 H69 B N3 O2 Si2 Sm, C6 H6' _chemical_formula_sum 'C44 H75 B N3 O2 Si2 Sm' _chemical_formula_weight 895.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 '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' B B 0.0013 0.0007 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.6630(2) _cell_length_b 24.3032(5) _cell_length_c 17.3539(4) _cell_angle_alpha 90.00 _cell_angle_beta 105.0460(10) _cell_angle_gamma 90.00 _cell_volume 4750.30(17) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.252 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1884 _exptl_absorpt_coefficient_mu 1.322 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6924 _exptl_absorpt_correction_T_max 0.7779 _exptl_absorpt_process_details ; BRUKER AXS SMART APEX 2 Vers. 1.0-27 R.H. Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 61959 _diffrn_reflns_av_R_equivalents 0.0894 _diffrn_reflns_av_sigmaI/netI 0.0576 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8183 _reflns_number_gt 6248 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The asymmteric unit contains one cocrystallized benzene molecule which is disordered over 2 positions (40/60). ; _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^)+(0.0256P)^2^+4.8816P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8183 _refine_ls_number_parameters 467 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0586 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.0876 _refine_ls_wR_factor_gt 0.0793 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm1 Sm 0.219373(17) 0.166463(8) 0.283505(12) 0.03019(8) Uani 1 1 d . . . N1 N 0.4051(3) 0.18680(13) 0.36300(18) 0.0297(7) Uani 1 1 d . . . N2 N 0.2214(3) 0.20479(12) 0.40272(18) 0.0287(7) Uani 1 1 d . . . N3 N 0.1797(3) 0.07495(13) 0.2531(2) 0.0435(9) Uani 1 1 d . . . B1 B 0.3481(4) 0.20764(18) 0.4213(3) 0.0300(10) Uani 1 1 d . . . Si1 Si 0.10349(12) 0.03088(5) 0.29986(9) 0.0554(4) Uani 1 1 d . . . Si2 Si 0.23611(12) 0.05566(5) 0.17569(8) 0.0534(4) Uani 1 1 d . . . O1 O 0.2085(2) 0.24168(11) 0.18591(16) 0.0392(7) Uani 1 1 d . . . O2 O 0.0034(2) 0.18286(11) 0.22946(17) 0.0429(7) Uani 1 1 d . . . C1 C 0.5308(3) 0.18387(17) 0.3818(2) 0.0337(10) Uani 1 1 d . . . C2 C 0.5875(4) 0.13197(18) 0.3969(2) 0.0389(10) Uani 1 1 d . . . C3 C 0.7116(4) 0.1295(2) 0.4185(3) 0.0513(12) Uani 1 1 d . . . H3 H 0.7495 0.0946 0.4281 0.067 Uiso 1 1 calc R . . C4 C 0.7799(4) 0.1761(2) 0.4263(3) 0.0597(14) Uani 1 1 d . . . H4 H 0.8640 0.1735 0.4422 0.078 Uiso 1 1 calc R . . C5 C 0.7259(4) 0.2264(2) 0.4108(3) 0.0543(13) Uani 1 1 d . . . H5 H 0.7736 0.2585 0.4158 0.071 Uiso 1 1 calc R . . C6 C 0.6013(3) 0.23166(18) 0.3877(2) 0.0399(10) Uani 1 1 d . . . C7 C 0.5155(4) 0.08045(18) 0.3963(3) 0.0472(12) Uani 1 1 d . . . H7 H 0.4402 0.0845 0.3532 0.057 Uiso 1 1 calc R . . C8 C 0.5760(5) 0.0273(2) 0.3801(3) 0.0712(16) Uani 1 1 d . . . H8A H 0.5990 0.0309 0.3298 0.107 Uiso 1 1 calc R . . H8B H 0.5209 -0.0036 0.3762 0.107 Uiso 1 1 calc R . . H8C H 0.6469 0.0206 0.4238 0.107 Uiso 1 1 calc R . . C9 C 0.4822(4) 0.07536(18) 0.4757(3) 0.0515(12) Uani 1 1 d . . . H9A H 0.5545 0.0706 0.5191 0.077 Uiso 1 1 calc R . . H9B H 0.4302 0.0434 0.4738 0.077 Uiso 1 1 calc R . . H9C H 0.4408 0.1088 0.4851 0.077 Uiso 1 1 calc R . . C10 C 0.5496(4) 0.28894(17) 0.3690(3) 0.0445(11) Uani 1 1 d . . . H10 H 0.4613 0.2852 0.3500 0.053 Uiso 1 1 calc R . . C11 C 0.5935(4) 0.3155(2) 0.3016(3) 0.0584(13) Uani 1 1 d . . . H11A H 0.6791 0.3222 0.3201 0.088 Uiso 1 1 calc R . . H11B H 0.5521 0.3505 0.2863 0.088 Uiso 1 1 calc R . . H11C H 0.5772 0.2908 0.2554 0.088 Uiso 1 1 calc R . . C12 C 0.5774(5) 0.3261(2) 0.4426(3) 0.0668(15) Uani 1 1 d . . . H12A H 0.5464 0.3093 0.4844 0.100 Uiso 1 1 calc R . . H12B H 0.5401 0.3621 0.4284 0.100 Uiso 1 1 calc R . . H12C H 0.6636 0.3307 0.4622 0.100 Uiso 1 1 calc R . . C13 C 0.1553(3) 0.22724(17) 0.4532(2) 0.0325(9) Uani 1 1 d . . . C14 C 0.1371(3) 0.19759(18) 0.5186(2) 0.0378(10) Uani 1 1 d . . . C15 C 0.0707(4) 0.2223(2) 0.5656(3) 0.0491(12) Uani 1 1 d . . . H15 H 0.0582 0.2027 0.6100 0.064 Uiso 1 1 calc R . . C16 C 0.0228(4) 0.2741(2) 0.5496(3) 0.0531(13) Uani 1 1 d . . . H16 H -0.0216 0.2898 0.5829 0.069 Uiso 1 1 calc R . . C17 C 0.0395(3) 0.3030(2) 0.4855(3) 0.0453(11) Uani 1 1 d . . . H17 H 0.0056 0.3386 0.4744 0.059 Uiso 1 1 calc R . . C18 C 0.1055(3) 0.28095(17) 0.4363(2) 0.0357(10) Uani 1 1 d . . . C19 C 0.1906(4) 0.14108(18) 0.5405(3) 0.0427(11) Uani 1 1 d . . . H19 H 0.2124 0.1259 0.4926 0.051 Uiso 1 1 calc R . . C20 C 0.1044(4) 0.1000(2) 0.5640(3) 0.0647(14) Uani 1 1 d . . . H20A H 0.1392 0.0631 0.5692 0.097 Uiso 1 1 calc R . . H20B H 0.0289 0.0998 0.5227 0.097 Uiso 1 1 calc R . . H20C H 0.0904 0.1112 0.6151 0.097 Uiso 1 1 calc R . . C21 C 0.3040(4) 0.1449(2) 0.6079(3) 0.0597(13) Uani 1 1 d . . . H21A H 0.3601 0.1698 0.5922 0.090 Uiso 1 1 calc R . . H21B H 0.3396 0.1083 0.6189 0.090 Uiso 1 1 calc R . . H21C H 0.2851 0.1592 0.6560 0.090 Uiso 1 1 calc R . . C22 C 0.1318(4) 0.31511(17) 0.3703(3) 0.0444(11) Uani 1 1 d . . . H22 H 0.1428 0.2892 0.3281 0.053 Uiso 1 1 calc R . . C23 C 0.2480(4) 0.34664(19) 0.4008(3) 0.0537(13) Uani 1 1 d . . . H23A H 0.2391 0.3735 0.4410 0.081 Uiso 1 1 calc R . . H23B H 0.2675 0.3659 0.3562 0.081 Uiso 1 1 calc R . . H23C H 0.3118 0.3208 0.4247 0.081 Uiso 1 1 calc R . . C24 C 0.0318(4) 0.3554(2) 0.3307(3) 0.0630(14) Uani 1 1 d . . . H24A H -0.0442 0.3357 0.3166 0.095 Uiso 1 1 calc R . . H24B H 0.0479 0.3707 0.2824 0.095 Uiso 1 1 calc R . . H24C H 0.0282 0.3852 0.3680 0.095 Uiso 1 1 calc R . . C25 C -0.0041(4) 0.0700(2) 0.3418(3) 0.0662(15) Uani 1 1 d . . . H25A H 0.0367 0.1010 0.3736 0.099 Uiso 1 1 calc R . . H25B H -0.0368 0.0456 0.3758 0.099 Uiso 1 1 calc R . . H25C H -0.0687 0.0839 0.2981 0.099 Uiso 1 1 calc R . . C26 C 0.2028(5) -0.0071(2) 0.3856(4) 0.093(2) Uani 1 1 d . . . H26A H 0.2617 -0.0282 0.3667 0.140 Uiso 1 1 calc R . . H26B H 0.1551 -0.0323 0.4088 0.140 Uiso 1 1 calc R . . H26C H 0.2435 0.0193 0.4263 0.140 Uiso 1 1 calc R . . C27 C 0.0171(5) -0.0232(2) 0.2321(4) 0.091(2) Uani 1 1 d . . . H27A H -0.0392 -0.0055 0.1870 0.136 Uiso 1 1 calc R . . H27B H -0.0265 -0.0458 0.2616 0.136 Uiso 1 1 calc R . . H27C H 0.0717 -0.0464 0.2121 0.136 Uiso 1 1 calc R . . C28 C 0.1207(5) 0.0429(2) 0.0793(3) 0.0764(17) Uani 1 1 d . . . H28A H 0.0755 0.0097 0.0844 0.115 Uiso 1 1 calc R . . H28B H 0.1597 0.0379 0.0361 0.115 Uiso 1 1 calc R . . H28C H 0.0667 0.0745 0.0672 0.115 Uiso 1 1 calc R . . C29 C 0.3349(5) -0.0062(2) 0.1955(4) 0.0828(18) Uani 1 1 d . . . H29A H 0.3972 -0.0007 0.2451 0.124 Uiso 1 1 calc R . . H29B H 0.3714 -0.0115 0.1512 0.124 Uiso 1 1 calc R . . H29C H 0.2879 -0.0387 0.2007 0.124 Uiso 1 1 calc R . . C30 C 0.3286(4) 0.11528(19) 0.1551(3) 0.0593(14) Uani 1 1 d . . . H30A H 0.2766 0.1465 0.1343 0.089 Uiso 1 1 calc R . . H30B H 0.3708 0.1041 0.1156 0.089 Uiso 1 1 calc R . . H30C H 0.3862 0.1261 0.2047 0.089 Uiso 1 1 calc R . . C31 C 0.3133(4) 0.2635(2) 0.1680(3) 0.0618(15) Uani 1 1 d . . . H31A H 0.3230 0.2480 0.1174 0.080 Uiso 1 1 calc R . . H31B H 0.3847 0.2545 0.2113 0.080 Uiso 1 1 calc R . . C32 C 0.2961(5) 0.3232(2) 0.1613(4) 0.0681(16) Uani 1 1 d . . . H32A H 0.3434 0.3396 0.1272 0.089 Uiso 1 1 calc R . . H32B H 0.3186 0.3410 0.2144 0.089 Uiso 1 1 calc R . . C33 C 0.1654(4) 0.3289(2) 0.1233(3) 0.0665(15) Uani 1 1 d . . . H33A H 0.1333 0.3621 0.1434 0.086 Uiso 1 1 calc R . . H33B H 0.1495 0.3316 0.0646 0.086 Uiso 1 1 calc R . . C34 C 0.1116(4) 0.27791(19) 0.1469(3) 0.0556(13) Uani 1 1 d . . . H34A H 0.0623 0.2871 0.1837 0.072 Uiso 1 1 calc R . . H34B H 0.0605 0.2597 0.0991 0.072 Uiso 1 1 calc R . . C35 C -0.0803(4) 0.2103(2) 0.2660(3) 0.0541(13) Uani 1 1 d . . . H35A H -0.0693 0.2507 0.2658 0.070 Uiso 1 1 calc R . . H35B H -0.0690 0.1979 0.3218 0.070 Uiso 1 1 calc R . . C36 C -0.2006(4) 0.1949(2) 0.2166(3) 0.0643(14) Uani 1 1 d . . . H36A H -0.2581 0.2251 0.2146 0.084 Uiso 1 1 calc R . . H36B H -0.2300 0.1614 0.2376 0.084 Uiso 1 1 calc R . . C37 C -0.1799(4) 0.1844(2) 0.1342(3) 0.0699(15) Uani 1 1 d . . . H37A H -0.2413 0.1597 0.1019 0.091 Uiso 1 1 calc R . . H37B H -0.1791 0.2193 0.1048 0.091 Uiso 1 1 calc R . . C38 C -0.0612(4) 0.15785(19) 0.1546(3) 0.0490(12) Uani 1 1 d . . . H38A H -0.0687 0.1176 0.1609 0.064 Uiso 1 1 calc R . . H38B H -0.0200 0.1647 0.1123 0.064 Uiso 1 1 calc R . . C39A C 0.8765(16) 0.5628(5) 0.3749(13) 0.124(8) Uiso 0.382(18) 1 d PG A 1 H39A H 0.8981 0.6004 0.3737 0.162 Uiso 0.382(18) 1 calc PR A 1 C40A C 0.823(2) 0.5355(9) 0.3043(9) 0.24(2) Uiso 0.382(18) 1 d PG A 1 H40A H 0.8080 0.5545 0.2548 0.312 Uiso 0.382(18) 1 calc PR A 1 C41A C 0.7914(19) 0.4805(9) 0.3061(9) 0.204(16) Uiso 0.382(18) 1 d PG A 1 H41A H 0.7548 0.4618 0.2578 0.265 Uiso 0.382(18) 1 calc PR A 1 C42A C 0.8133(15) 0.4527(5) 0.3785(14) 0.085(6) Uiso 0.382(18) 1 d PG A 1 H42A H 0.7917 0.4151 0.3797 0.110 Uiso 0.382(18) 1 calc PR A 1 C43A C 0.8668(16) 0.4800(7) 0.4491(9) 0.120(8) Uiso 0.382(18) 1 d PG A 1 H43A H 0.8818 0.4610 0.4985 0.155 Uiso 0.382(18) 1 calc PR A 1 C44A C 0.8984(16) 0.5350(7) 0.4473(9) 0.115(8) Uiso 0.382(18) 1 d PG A 1 H44A H 0.9350 0.5536 0.4955 0.150 Uiso 0.382(18) 1 calc PR A 1 C44B C 0.8582(9) 0.5533(4) 0.4041(6) 0.117(5) Uiso 0.618(18) 1 d PG A 2 H44B H 0.8806 0.5893 0.4241 0.152 Uiso 0.618(18) 1 calc PR A 2 C43B C 0.8399(11) 0.5122(5) 0.4553(3) 0.151(6) Uiso 0.618(18) 1 d PG A 2 H43B H 0.8496 0.5201 0.5103 0.197 Uiso 0.618(18) 1 calc PR A 2 C39B C 0.8072(11) 0.4597(4) 0.4261(6) 0.118(5) Uiso 0.618(18) 1 d PG A 2 H39B H 0.7947 0.4316 0.4611 0.154 Uiso 0.618(18) 1 calc PR A 2 C42B C 0.7930(8) 0.4483(3) 0.3457(6) 0.083(4) Uiso 0.618(18) 1 d PG A 2 H42B H 0.7706 0.4124 0.3257 0.108 Uiso 0.618(18) 1 calc PR A 2 C41B C 0.8113(8) 0.4894(3) 0.2945(3) 0.075(4) Uiso 0.618(18) 1 d PG A 2 H41B H 0.8015 0.4816 0.2395 0.098 Uiso 0.618(18) 1 calc PR A 2 C40B C 0.8440(8) 0.5419(3) 0.3237(5) 0.073(4) Uiso 0.618(18) 1 d PG A 2 H40B H 0.8565 0.5700 0.2887 0.095 Uiso 0.618(18) 1 calc PR A 2 H100 H 0.405(3) 0.2247(14) 0.481(2) 0.038(10) Uiso 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 Sm1 0.02939(13) 0.02780(13) 0.02992(12) -0.00096(10) 0.00150(9) -0.00006(10) N1 0.0245(17) 0.0324(18) 0.0293(18) 0.0001(15) 0.0015(14) 0.0024(15) N2 0.0277(17) 0.0289(19) 0.0286(18) -0.0001(14) 0.0057(14) -0.0017(15) N3 0.044(2) 0.030(2) 0.050(2) -0.0026(17) -0.0002(18) -0.0014(17) B1 0.031(3) 0.030(3) 0.026(2) 0.004(2) 0.001(2) 0.000(2) Si1 0.0479(8) 0.0366(8) 0.0699(10) 0.0070(7) -0.0061(7) -0.0086(7) Si2 0.0570(9) 0.0377(8) 0.0560(9) -0.0151(6) -0.0022(7) 0.0056(7) O1 0.0325(16) 0.0428(18) 0.0417(17) 0.0099(14) 0.0084(13) 0.0059(14) O2 0.0295(16) 0.0480(18) 0.0472(18) -0.0034(14) 0.0029(14) -0.0018(14) C1 0.028(2) 0.046(3) 0.026(2) 0.0004(18) 0.0062(17) 0.002(2) C2 0.035(2) 0.049(3) 0.030(2) 0.001(2) 0.0032(19) 0.011(2) C3 0.041(3) 0.068(4) 0.044(3) 0.009(2) 0.010(2) 0.019(3) C4 0.032(3) 0.092(4) 0.055(3) 0.017(3) 0.011(2) 0.010(3) C5 0.033(3) 0.075(4) 0.056(3) 0.005(3) 0.013(2) -0.009(3) C6 0.031(2) 0.052(3) 0.037(2) 0.002(2) 0.0091(19) -0.001(2) C7 0.049(3) 0.038(3) 0.045(3) -0.003(2) -0.006(2) 0.013(2) C8 0.093(4) 0.051(3) 0.058(3) -0.007(3) -0.001(3) 0.027(3) C9 0.046(3) 0.035(3) 0.067(3) 0.002(2) 0.003(2) -0.001(2) C10 0.041(3) 0.042(3) 0.051(3) 0.006(2) 0.014(2) -0.007(2) C11 0.046(3) 0.055(3) 0.074(4) 0.018(3) 0.017(3) -0.003(2) C12 0.069(4) 0.060(4) 0.071(4) -0.015(3) 0.018(3) -0.012(3) C13 0.020(2) 0.043(3) 0.029(2) -0.0045(19) -0.0011(17) -0.0034(19) C14 0.027(2) 0.049(3) 0.035(2) -0.006(2) 0.0042(19) -0.011(2) C15 0.039(3) 0.070(4) 0.043(3) -0.009(2) 0.019(2) -0.016(3) C16 0.034(3) 0.070(4) 0.060(3) -0.022(3) 0.021(2) -0.007(3) C17 0.028(2) 0.055(3) 0.051(3) -0.013(2) 0.006(2) 0.006(2) C18 0.024(2) 0.043(3) 0.034(2) -0.011(2) -0.0031(18) -0.0002(19) C19 0.045(3) 0.046(3) 0.037(2) 0.003(2) 0.009(2) -0.007(2) C20 0.063(3) 0.066(4) 0.065(3) 0.014(3) 0.017(3) -0.020(3) C21 0.050(3) 0.064(3) 0.058(3) 0.009(3) 0.003(3) 0.003(3) C22 0.050(3) 0.036(3) 0.044(3) -0.003(2) 0.007(2) 0.014(2) C23 0.053(3) 0.048(3) 0.063(3) 0.013(2) 0.019(3) 0.006(2) C24 0.068(3) 0.045(3) 0.063(3) -0.003(3) -0.006(3) 0.013(3) C25 0.072(4) 0.064(4) 0.061(3) 0.012(3) 0.014(3) -0.012(3) C26 0.065(4) 0.080(4) 0.115(5) 0.050(4) -0.013(3) -0.002(3) C27 0.082(4) 0.067(4) 0.114(5) -0.020(4) 0.009(4) -0.035(3) C28 0.083(4) 0.070(4) 0.063(4) -0.017(3) -0.004(3) 0.008(3) C29 0.082(4) 0.054(4) 0.097(5) -0.029(3) -0.005(3) 0.012(3) C30 0.074(3) 0.051(3) 0.057(3) -0.015(3) 0.024(3) 0.006(3) C31 0.045(3) 0.067(4) 0.080(4) 0.024(3) 0.027(3) 0.007(3) C32 0.058(3) 0.057(4) 0.090(4) 0.017(3) 0.018(3) -0.001(3) C33 0.057(3) 0.060(4) 0.084(4) 0.037(3) 0.022(3) 0.013(3) C34 0.047(3) 0.059(3) 0.053(3) 0.020(3) 0.000(2) 0.009(3) C35 0.039(3) 0.060(3) 0.064(3) -0.008(3) 0.014(2) 0.006(2) C36 0.038(3) 0.085(4) 0.064(4) -0.002(3) 0.003(3) 0.012(3) C37 0.045(3) 0.094(4) 0.060(4) -0.003(3) -0.006(3) 0.013(3) C38 0.038(3) 0.058(3) 0.046(3) -0.006(2) 0.001(2) -0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 N2 2.263(3) . ? Sm1 N1 2.299(3) . ? Sm1 N3 2.305(3) . ? Sm1 O1 2.473(3) . ? Sm1 O2 2.481(3) . ? Sm1 B1 2.666(5) . ? Sm1 Si2 3.3135(13) . ? N1 C1 1.419(5) . ? N1 B1 1.439(5) . ? N2 C13 1.418(5) . ? N2 B1 1.429(5) . ? N3 Si2 1.708(4) . ? N3 Si1 1.723(4) . ? B1 H100 1.15(4) . ? Si1 C25 1.867(5) . ? Si1 C27 1.873(5) . ? Si1 C26 1.875(5) . ? Si2 C29 1.871(5) . ? Si2 C28 1.881(5) . ? Si2 C30 1.895(5) . ? O1 C31 1.438(5) . ? O1 C34 1.454(5) . ? O2 C38 1.455(5) . ? O2 C35 1.457(5) . ? C1 C6 1.412(6) . ? C1 C2 1.417(6) . ? C2 C3 1.399(6) . ? C2 C7 1.506(6) . ? C3 C4 1.371(7) . ? C3 H3 0.9500 . ? C4 C5 1.370(6) . ? C4 H4 0.9500 . ? C5 C6 1.409(6) . ? C5 H5 0.9500 . ? C6 C10 1.518(6) . ? C7 C9 1.530(6) . ? C7 C8 1.533(6) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C12 1.529(6) . ? C10 C11 1.535(6) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.406(5) . ? C13 C18 1.428(5) . ? C14 C15 1.397(6) . ? C14 C19 1.516(6) . ? C15 C16 1.377(6) . ? C15 H15 0.9500 . ? C16 C17 1.371(6) . ? C16 H16 0.9500 . ? C17 C18 1.398(5) . ? C17 H17 0.9500 . ? C18 C22 1.508(6) . ? C19 C21 1.524(6) . ? C19 C20 1.545(6) . ? C19 H19 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.526(6) . ? C22 C24 1.540(6) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.464(6) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.502(7) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.494(6) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.490(6) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.531(7) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.484(6) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39A C40A 1.3900 . ? C39A C44A 1.3900 . ? C39A H39A 0.9500 . ? C40A C41A 1.3900 . ? C40A H40A 0.9500 . ? C41A C42A 1.3900 . ? C41A H41A 0.9500 . ? C42A C43A 1.3900 . ? C42A H42A 0.9500 . ? C43A C44A 1.3900 . ? C43A H43A 0.9500 . ? C44A H44A 0.9500 . ? C44B C43B 1.3900 . ? C44B C40B 1.3900 . ? C44B H44B 0.9500 . ? C43B C39B 1.3900 . ? C43B H43B 0.9500 . ? C39B C42B 1.3900 . ? C39B H39B 0.9500 . ? C42B C41B 1.3900 . ? C42B H42B 0.9500 . ? C41B C40B 1.3900 . ? C41B H41B 0.9500 . ? C40B H40B 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Sm1 N1 65.06(10) . . ? N2 Sm1 N3 124.07(12) . . ? N1 Sm1 N3 116.52(11) . . ? N2 Sm1 O1 107.96(10) . . ? N1 Sm1 O1 97.17(10) . . ? N3 Sm1 O1 125.81(11) . . ? N2 Sm1 O2 92.77(10) . . ? N1 Sm1 O2 153.89(10) . . ? N3 Sm1 O2 86.84(11) . . ? O1 Sm1 O2 75.87(9) . . ? N2 Sm1 B1 32.41(12) . . ? N1 Sm1 B1 32.65(12) . . ? N3 Sm1 B1 126.89(13) . . ? O1 Sm1 B1 104.69(11) . . ? O2 Sm1 B1 123.96(12) . . ? N2 Sm1 Si2 149.58(8) . . ? N1 Sm1 Si2 109.21(8) . . ? N3 Sm1 Si2 28.87(9) . . ? O1 Sm1 Si2 102.36(7) . . ? O2 Sm1 Si2 96.88(7) . . ? B1 Sm1 Si2 135.20(10) . . ? C1 N1 B1 119.6(3) . . ? C1 N1 Sm1 152.1(2) . . ? B1 N1 Sm1 87.8(2) . . ? C13 N2 B1 122.5(3) . . ? C13 N2 Sm1 147.6(2) . . ? B1 N2 Sm1 89.5(2) . . ? Si2 N3 Si1 123.4(2) . . ? Si2 N3 Sm1 110.46(17) . . ? Si1 N3 Sm1 126.11(19) . . ? N2 B1 N1 117.6(4) . . ? N2 B1 Sm1 58.08(19) . . ? N1 B1 Sm1 59.5(2) . . ? N2 B1 H100 122.9(17) . . ? N1 B1 H100 119.5(17) . . ? Sm1 B1 H100 178.7(18) . . ? N3 Si1 C25 110.4(2) . . ? N3 Si1 C27 113.5(2) . . ? C25 Si1 C27 107.2(3) . . ? N3 Si1 C26 113.1(2) . . ? C25 Si1 C26 106.3(3) . . ? C27 Si1 C26 105.9(3) . . ? N3 Si2 C29 114.9(2) . . ? N3 Si2 C28 114.3(2) . . ? C29 Si2 C28 107.2(2) . . ? N3 Si2 C30 107.03(18) . . ? C29 Si2 C30 107.2(2) . . ? C28 Si2 C30 105.6(3) . . ? N3 Si2 Sm1 40.67(11) . . ? C29 Si2 Sm1 132.28(18) . . ? C28 Si2 Sm1 120.18(17) . . ? C30 Si2 Sm1 66.73(14) . . ? C31 O1 C34 106.1(3) . . ? C31 O1 Sm1 121.7(2) . . ? C34 O1 Sm1 131.5(2) . . ? C38 O2 C35 109.2(3) . . ? C38 O2 Sm1 120.7(2) . . ? C35 O2 Sm1 129.7(2) . . ? C6 C1 C2 118.9(4) . . ? C6 C1 N1 121.5(4) . . ? C2 C1 N1 119.5(4) . . ? C3 C2 C1 119.3(4) . . ? C3 C2 C7 120.1(4) . . ? C1 C2 C7 120.4(4) . . ? C4 C3 C2 121.7(4) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? C5 C4 C3 119.5(4) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C4 C5 C6 121.7(5) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C5 C6 C1 118.9(4) . . ? C5 C6 C10 117.9(4) . . ? C1 C6 C10 123.2(4) . . ? C2 C7 C9 109.4(3) . . ? C2 C7 C8 114.8(4) . . ? C9 C7 C8 109.5(4) . . ? C2 C7 H7 107.6 . . ? C9 C7 H7 107.6 . . ? C8 C7 H7 107.6 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C6 C10 C12 112.2(4) . . ? C6 C10 C11 110.8(4) . . ? C12 C10 C11 110.3(4) . . ? C6 C10 H10 107.8 . . ? C12 C10 H10 107.8 . . ? C11 C10 H10 107.8 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 N2 121.5(4) . . ? C14 C13 C18 119.7(4) . . ? N2 C13 C18 118.8(3) . . ? C15 C14 C13 118.3(4) . . ? C15 C14 C19 119.9(4) . . ? C13 C14 C19 121.8(4) . . ? C16 C15 C14 122.2(4) . . ? C16 C15 H15 118.9 . . ? C14 C15 H15 118.9 . . ? C17 C16 C15 119.8(4) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C16 C17 C18 121.0(4) . . ? C16 C17 H17 119.5 . . ? C18 C17 H17 119.5 . . ? C17 C18 C13 119.0(4) . . ? C17 C18 C22 120.4(4) . . ? C13 C18 C22 120.5(3) . . ? C14 C19 C21 110.8(4) . . ? C14 C19 C20 113.4(4) . . ? C21 C19 C20 109.3(4) . . ? C14 C19 H19 107.7 . . ? C21 C19 H19 107.7 . . ? C20 C19 H19 107.7 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C18 C22 C23 110.5(4) . . ? C18 C22 C24 114.1(4) . . ? C23 C22 C24 109.7(4) . . ? C18 C22 H22 107.4 . . ? C23 C22 H22 107.4 . . ? C24 C22 H22 107.4 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si1 C25 H25A 109.5 . . ? Si1 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si1 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si1 C26 H26A 109.5 . . ? Si1 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si1 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si1 C27 H27A 109.5 . . ? Si1 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si1 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si2 C28 H28A 109.5 . . ? Si2 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si2 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si2 C29 H29A 109.5 . . ? Si2 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? Si2 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? Si2 C30 H30A 109.5 . . ? Si2 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si2 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O1 C31 C32 106.1(4) . . ? O1 C31 H31A 110.5 . . ? C32 C31 H31A 110.5 . . ? O1 C31 H31B 110.5 . . ? C32 C31 H31B 110.5 . . ? H31A C31 H31B 108.7 . . ? C31 C32 C33 103.2(4) . . ? C31 C32 H32A 111.1 . . ? C33 C32 H32A 111.1 . . ? C31 C32 H32B 111.1 . . ? C33 C32 H32B 111.1 . . ? H32A C32 H32B 109.1 . . ? C34 C33 C32 104.7(4) . . ? C34 C33 H33A 110.8 . . ? C32 C33 H33A 110.8 . . ? C34 C33 H33B 110.8 . . ? C32 C33 H33B 110.8 . . ? H33A C33 H33B 108.9 . . ? O1 C34 C33 107.4(4) . . ? O1 C34 H34A 110.2 . . ? C33 C34 H34A 110.2 . . ? O1 C34 H34B 110.2 . . ? C33 C34 H34B 110.2 . . ? H34A C34 H34B 108.5 . . ? O2 C35 C36 105.7(4) . . ? O2 C35 H35A 110.6 . . ? C36 C35 H35A 110.6 . . ? O2 C35 H35B 110.6 . . ? C36 C35 H35B 110.6 . . ? H35A C35 H35B 108.7 . . ? C35 C36 C37 103.0(4) . . ? C35 C36 H36A 111.2 . . ? C37 C36 H36A 111.2 . . ? C35 C36 H36B 111.2 . . ? C37 C36 H36B 111.2 . . ? H36A C36 H36B 109.1 . . ? C38 C37 C36 102.3(4) . . ? C38 C37 H37A 111.3 . . ? C36 C37 H37A 111.3 . . ? C38 C37 H37B 111.3 . . ? C36 C37 H37B 111.3 . . ? H37A C37 H37B 109.2 . . ? O2 C38 C37 105.4(4) . . ? O2 C38 H38A 110.7 . . ? C37 C38 H38A 110.7 . . ? O2 C38 H38B 110.7 . . ? C37 C38 H38B 110.7 . . ? H38A C38 H38B 108.8 . . ? C40A C39A C44A 120.0 . . ? C40A C39A H39A 120.0 . . ? C44A C39A H39A 120.0 . . ? C39A C40A C41A 120.0 . . ? C39A C40A H40A 120.0 . . ? C41A C40A H40A 120.0 . . ? C42A C41A C40A 120.0 . . ? C42A C41A H41A 120.0 . . ? C40A C41A H41A 120.0 . . ? C43A C42A C41A 120.0 . . ? C43A C42A H42A 120.0 . . ? C41A C42A H42A 120.0 . . ? C44A C43A C42A 120.0 . . ? C44A C43A H43A 120.0 . . ? C42A C43A H43A 120.0 . . ? C43A C44A C39A 120.0 . . ? C43A C44A H44A 120.0 . . ? C39A C44A H44A 120.0 . . ? C43B C44B C40B 120.0 . . ? C43B C44B H44B 120.0 . . ? C40B C44B H44B 120.0 . . ? C39B C43B C44B 120.0 . . ? C39B C43B H43B 120.0 . . ? C44B C43B H43B 120.0 . . ? C43B C39B C42B 120.0 . . ? C43B C39B H39B 120.0 . . ? C42B C39B H39B 120.0 . . ? C39B C42B C41B 120.0 . . ? C39B C42B H42B 120.0 . . ? C41B C42B H42B 120.0 . . ? C40B C41B C42B 120.0 . . ? C40B C41B H41B 120.0 . . ? C42B C41B H41B 120.0 . . ? C41B C40B C44B 120.0 . . ? C41B C40B H40B 120.0 . . ? C44B C40B H40B 120.0 . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.630 _refine_diff_density_min -0.572 _refine_diff_density_rms 0.083 # Attachment 'hasj250-NBNSmDMA.cif' data_hasj250 _database_code_depnum_ccdc_archive 'CCDC 763735' #TrackingRef 'hasj250-NBNSmDMA.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ((DIPP-NBN)Sm-DMA)2 _chemical_melting_point ? _chemical_formula_moiety 'C66 H94 B2 N6 Sm2' _chemical_formula_sum 'C66 H94 B2 N6 Sm2' _chemical_formula_weight 1293.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9732(8) _cell_length_b 17.9783(12) _cell_length_c 18.4408(13) _cell_angle_alpha 62.308(2) _cell_angle_beta 89.912(3) _cell_angle_gamma 76.663(3) _cell_volume 3110.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 103(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.381 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1332 _exptl_absorpt_coefficient_mu 1.913 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4361 _exptl_absorpt_correction_T_max 0.8528 _exptl_absorpt_process_details ; BRUKER AXS SMART APEX 2 Vers. 1.0-27 R.H. Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 103(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41617 _diffrn_reflns_av_R_equivalents 0.0224 _diffrn_reflns_av_sigmaI/netI 0.0301 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 30.79 _reflns_number_total 18319 _reflns_number_gt 15450 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0251P)^2^+2.2735P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18319 _refine_ls_number_parameters 729 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0334 _refine_ls_R_factor_gt 0.0238 _refine_ls_wR_factor_ref 0.0625 _refine_ls_wR_factor_gt 0.0567 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm1 Sm 0.097114(9) 0.168587(6) 0.699199(5) 0.01311(3) Uani 1 1 d . . . Sm2 Sm 0.208048(9) -0.194435(6) 0.813508(5) 0.01294(3) Uani 1 1 d . . . B1 B 0.0046(2) 0.14739(14) 0.57641(13) 0.0160(4) Uani 1 1 d . . . B2 B 0.1056(2) -0.16354(14) 0.93313(13) 0.0154(4) Uani 1 1 d . . . N1 N -0.03402(16) 0.22756(10) 0.57822(10) 0.0156(3) Uani 1 1 d . . . N2 N 0.08936(15) 0.07582(10) 0.64649(10) 0.0151(3) Uani 1 1 d . . . N3 N 0.11672(15) -0.24407(10) 0.93359(10) 0.0152(3) Uani 1 1 d . . . N4 N 0.14407(15) -0.09650(10) 0.86246(10) 0.0144(3) Uani 1 1 d . . . N5 N 0.05498(17) 0.33033(11) 0.66891(11) 0.0198(3) Uani 1 1 d . . . N6 N 0.26517(17) -0.36063(11) 0.85027(11) 0.0203(3) Uani 1 1 d . . . C1 C -0.10153(19) 0.30484(12) 0.50809(11) 0.0161(4) Uani 1 1 d . . . C2 C -0.04136(19) 0.34835(12) 0.43810(11) 0.0158(4) Uani 1 1 d . . . C3 C -0.1105(2) 0.42594(13) 0.37104(12) 0.0198(4) Uani 1 1 d . . . H3 H -0.0705 0.4538 0.3236 0.026 Uiso 1 1 calc R . . C4 C -0.2353(2) 0.46300(13) 0.37206(13) 0.0221(4) Uani 1 1 d . . . H4 H -0.2802 0.5162 0.3264 0.029 Uiso 1 1 calc R . . C5 C -0.2938(2) 0.42107(13) 0.44093(13) 0.0217(4) Uani 1 1 d . . . H5 H -0.3793 0.4465 0.4422 0.028 Uiso 1 1 calc R . . C6 C -0.23004(19) 0.34236(13) 0.50847(12) 0.0187(4) Uani 1 1 d . . . C7 C 0.0978(2) 0.31456(13) 0.43501(12) 0.0177(4) Uani 1 1 d . . . H7 H 0.1367 0.2705 0.4926 0.023 Uiso 1 1 calc R . . C8 C 0.1169(2) 0.26864(14) 0.38212(14) 0.0245(4) Uani 1 1 d . . . H8A H 0.0770 0.2203 0.4045 0.037 Uiso 1 1 calc R . . H8B H 0.2074 0.2462 0.3827 0.037 Uiso 1 1 calc R . . H8C H 0.0786 0.3100 0.3253 0.037 Uiso 1 1 calc R . . C9 C 0.1690(2) 0.38590(14) 0.40387(14) 0.0227(4) Uani 1 1 d . . . H9A H 0.1469 0.4226 0.3441 0.034 Uiso 1 1 calc R . . H9B H 0.2601 0.3590 0.4164 0.034 Uiso 1 1 calc R . . H9C H 0.1455 0.4216 0.4313 0.034 Uiso 1 1 calc R . . C10 C -0.3002(2) 0.29496(14) 0.57980(14) 0.0256(5) Uani 1 1 d . . . H10 H -0.2374 0.2609 0.6305 0.033 Uiso 1 1 calc R . . C11 C -0.3505(2) 0.22964(17) 0.56559(16) 0.0378(6) Uani 1 1 d . . . H11A H -0.4106 0.2607 0.5152 0.057 Uiso 1 1 calc R . . H11B H -0.3929 0.1976 0.6127 0.057 Uiso 1 1 calc R . . H11C H -0.2801 0.1887 0.5597 0.057 Uiso 1 1 calc R . . C12 C -0.4057(3) 0.35540(18) 0.59656(18) 0.0446(7) Uani 1 1 d . . . H12A H -0.3724 0.3993 0.6013 0.067 Uiso 1 1 calc R . . H12B H -0.4377 0.3213 0.6481 0.067 Uiso 1 1 calc R . . H12C H -0.4744 0.3843 0.5510 0.067 Uiso 1 1 calc R . . C13 C 0.13218(18) -0.00448(12) 0.65001(11) 0.0147(3) Uani 1 1 d . . . C14 C 0.26419(19) -0.03842(13) 0.65062(12) 0.0169(4) Uani 1 1 d . . . C15 C 0.3065(2) -0.11549(13) 0.64658(12) 0.0194(4) Uani 1 1 d . . . H15 H 0.3940 -0.1364 0.6458 0.025 Uiso 1 1 calc R . . C16 C 0.2240(2) -0.16271(13) 0.64358(12) 0.0200(4) Uani 1 1 d . . . H16 H 0.2541 -0.2144 0.6394 0.026 Uiso 1 1 calc R . . C17 C 0.0968(2) -0.13249(13) 0.64680(12) 0.0185(4) Uani 1 1 d . . . H17 H 0.0402 -0.1649 0.6459 0.024 Uiso 1 1 calc R . . C18 C 0.04917(18) -0.05552(12) 0.65137(11) 0.0153(3) Uani 1 1 d . . . C19 C -0.09139(19) -0.02813(13) 0.65350(12) 0.0175(4) Uani 1 1 d . . . H19 H -0.1093 0.0243 0.6618 0.023 Uiso 1 1 calc R . . C20 C -0.1361(2) -0.09972(14) 0.72538(13) 0.0228(4) Uani 1 1 d . . . H20A H -0.1283 -0.1495 0.7154 0.034 Uiso 1 1 calc R . . H20B H -0.2245 -0.0772 0.7297 0.034 Uiso 1 1 calc R . . H20C H -0.0840 -0.1182 0.7769 0.034 Uiso 1 1 calc R . . C21 C -0.1674(2) -0.00324(14) 0.57183(13) 0.0238(4) Uani 1 1 d . . . H21A H -0.1386 0.0423 0.5260 0.036 Uiso 1 1 calc R . . H21B H -0.2572 0.0183 0.5738 0.036 Uiso 1 1 calc R . . H21C H -0.1547 -0.0545 0.5637 0.036 Uiso 1 1 calc R . . C22 C 0.35553(19) 0.01527(13) 0.64527(13) 0.0199(4) Uani 1 1 d . . . H22 H 0.3282 0.0446 0.6795 0.026 Uiso 1 1 calc R . . C23 C 0.4929(2) -0.03822(16) 0.67766(15) 0.0267(5) Uani 1 1 d . . . H23A H 0.4963 -0.0876 0.7324 0.040 Uiso 1 1 calc R . . H23B H 0.5434 -0.0015 0.6815 0.040 Uiso 1 1 calc R . . H23C H 0.5267 -0.0598 0.6398 0.040 Uiso 1 1 calc R . . C24 C 0.3474(2) 0.08652(15) 0.55578(14) 0.0270(5) Uani 1 1 d . . . H24A H 0.3747 0.0596 0.5209 0.040 Uiso 1 1 calc R . . H24B H 0.4022 0.1235 0.5532 0.040 Uiso 1 1 calc R . . H24C H 0.2600 0.1220 0.5362 0.040 Uiso 1 1 calc R . . C25 C 0.09774(19) -0.31752(12) 1.00353(11) 0.0152(3) Uani 1 1 d . . . C26 C 0.18627(19) -0.36472(12) 1.07549(12) 0.0171(4) Uani 1 1 d . . . C27 C 0.1669(2) -0.44030(13) 1.14160(13) 0.0224(4) Uani 1 1 d . . . H27 H 0.2267 -0.4718 1.1897 0.029 Uiso 1 1 calc R . . C28 C 0.0630(2) -0.46952(14) 1.13794(13) 0.0253(5) Uani 1 1 d . . . H28 H 0.0515 -0.5210 1.1830 0.033 Uiso 1 1 calc R . . C29 C -0.0248(2) -0.42326(13) 1.06789(13) 0.0223(4) Uani 1 1 d . . . H29 H -0.0966 -0.4436 1.0655 0.029 Uiso 1 1 calc R . . C30 C -0.00982(19) -0.34719(12) 1.00065(12) 0.0179(4) Uani 1 1 d . . . C31 C 0.30274(19) -0.33584(13) 1.08413(12) 0.0189(4) Uani 1 1 d . . . H31 H 0.3138 -0.2912 1.0281 0.025 Uiso 1 1 calc R . . C32 C 0.2833(2) -0.29307(16) 1.13942(15) 0.0285(5) Uani 1 1 d . . . H32A H 0.2087 -0.2434 1.1159 0.043 Uiso 1 1 calc R . . H32B H 0.3577 -0.2730 1.1432 0.043 Uiso 1 1 calc R . . H32C H 0.2710 -0.3354 1.1946 0.043 Uiso 1 1 calc R . . C33 C 0.4238(2) -0.41017(15) 1.11755(16) 0.0297(5) Uani 1 1 d . . . H33A H 0.4215 -0.4498 1.1758 0.045 Uiso 1 1 calc R . . H33B H 0.4970 -0.3862 1.1121 0.045 Uiso 1 1 calc R . . H33C H 0.4304 -0.4420 1.0861 0.045 Uiso 1 1 calc R . . C34 C -0.1105(2) -0.29515(13) 0.92690(13) 0.0219(4) Uani 1 1 d . . . H34 H -0.0665 -0.2696 0.8770 0.028 Uiso 1 1 calc R . . C35 C -0.1979(2) -0.21935(15) 0.93327(15) 0.0289(5) Uani 1 1 d . . . H35A H -0.2590 -0.1842 0.8834 0.043 Uiso 1 1 calc R . . H35B H -0.1478 -0.1832 0.9387 0.043 Uiso 1 1 calc R . . H35C H -0.2428 -0.2420 0.9817 0.043 Uiso 1 1 calc R . . C36 C -0.1869(3) -0.34934(17) 0.91293(18) 0.0393(6) Uani 1 1 d . . . H36A H -0.2439 -0.3662 0.9554 0.059 Uiso 1 1 calc R . . H36B H -0.1295 -0.4017 0.9161 0.059 Uiso 1 1 calc R . . H36C H -0.2365 -0.3149 0.8583 0.059 Uiso 1 1 calc R . . C37 C 0.13363(18) -0.01683(12) 0.85888(11) 0.0143(3) Uani 1 1 d . . . C38 C 0.24432(19) 0.01057(12) 0.86415(11) 0.0156(4) Uani 1 1 d . . . C39 C 0.2340(2) 0.08669(12) 0.86881(11) 0.0177(4) Uani 1 1 d . . . H39 H 0.3085 0.1034 0.8733 0.023 Uiso 1 1 calc R . . C40 C 0.1177(2) 0.13921(12) 0.86717(11) 0.0187(4) Uani 1 1 d . . . H40 H 0.1127 0.1901 0.8722 0.024 Uiso 1 1 calc R . . C41 C 0.0091(2) 0.11557(12) 0.85807(12) 0.0184(4) Uani 1 1 d . . . H41 H -0.0707 0.1519 0.8554 0.024 Uiso 1 1 calc R . . C42 C 0.01382(18) 0.03964(12) 0.85275(11) 0.0148(3) Uani 1 1 d . . . C43 C 0.37388(19) -0.04905(13) 0.87438(12) 0.0187(4) Uani 1 1 d . . . H43 H 0.3683 -0.0782 0.8401 0.024 Uiso 1 1 calc R . . C44 C 0.4094(2) -0.12002(14) 0.96478(14) 0.0259(5) Uani 1 1 d . . . H44A H 0.4193 -0.0934 0.9995 0.039 Uiso 1 1 calc R . . H44B H 0.4890 -0.1616 0.9702 0.039 Uiso 1 1 calc R . . H44C H 0.3426 -0.1505 0.9823 0.039 Uiso 1 1 calc R . . C45 C 0.4782(2) -0.00173(15) 0.84659(15) 0.0252(4) Uani 1 1 d . . . H45A H 0.4524 0.0466 0.7903 0.038 Uiso 1 1 calc R . . H45B H 0.5559 -0.0424 0.8477 0.038 Uiso 1 1 calc R . . H45C H 0.4933 0.0210 0.8839 0.038 Uiso 1 1 calc R . . C46 C -0.11019(19) 0.01883(12) 0.84526(12) 0.0171(4) Uani 1 1 d . . . H46 H -0.0922 -0.0339 0.8374 0.022 Uiso 1 1 calc R . . C47 C -0.2020(2) 0.09314(14) 0.77146(13) 0.0233(4) Uani 1 1 d . . . H47A H -0.2284 0.1435 0.7809 0.035 Uiso 1 1 calc R . . H47B H -0.2762 0.0742 0.7649 0.035 Uiso 1 1 calc R . . H47C H -0.1602 0.1093 0.7213 0.035 Uiso 1 1 calc R . . C48 C -0.1730(2) -0.00188(15) 0.92457(13) 0.0245(4) Uani 1 1 d . . . H48A H -0.1134 -0.0479 0.9722 0.037 Uiso 1 1 calc R . . H48B H -0.2481 -0.0215 0.9211 0.037 Uiso 1 1 calc R . . H48C H -0.1977 0.0505 0.9310 0.037 Uiso 1 1 calc R . . C49 C 0.2877(2) 0.22454(14) 0.66374(14) 0.0217(4) Uani 1 1 d . . . C50 C 0.2800(2) 0.26587(13) 0.71708(12) 0.0197(4) Uani 1 1 d . . . C51 C 0.3833(2) 0.24902(15) 0.77258(14) 0.0262(5) Uani 1 1 d . . . H51 H 0.4632 0.2156 0.7710 0.034 Uiso 1 1 calc R . . C52 C 0.3726(2) 0.27946(16) 0.82940(14) 0.0304(5) Uani 1 1 d . . . H52 H 0.4441 0.2656 0.8667 0.040 Uiso 1 1 calc R . . C53 C 0.2585(3) 0.33000(15) 0.83227(13) 0.0297(5) Uani 1 1 d . . . H53 H 0.2519 0.3517 0.8706 0.039 Uiso 1 1 calc R . . C54 C 0.1544(2) 0.34857(14) 0.77886(13) 0.0230(4) Uani 1 1 d . . . H54 H 0.0758 0.3833 0.7805 0.030 Uiso 1 1 calc R . . C55 C 0.1642(2) 0.31658(13) 0.72271(12) 0.0191(4) Uani 1 1 d . . . C56 C 0.0538(2) 0.40198(13) 0.58507(13) 0.0257(5) Uani 1 1 d . . . H56A H 0.0404 0.4568 0.5870 0.038 Uiso 1 1 calc R . . H56B H -0.0145 0.4065 0.5479 0.038 Uiso 1 1 calc R . . H56C H 0.1348 0.3901 0.5648 0.038 Uiso 1 1 calc R . . C57 C -0.0673(2) 0.35002(14) 0.69775(15) 0.0276(5) Uani 1 1 d . . . H57A H -0.0663 0.3052 0.7547 0.041 Uiso 1 1 calc R . . H57B H -0.1346 0.3510 0.6622 0.041 Uiso 1 1 calc R . . H57C H -0.0825 0.4069 0.6956 0.041 Uiso 1 1 calc R . . C58 C 0.4342(2) -0.26602(15) 0.86194(14) 0.0219(4) Uani 1 1 d . . . C59 C 0.45193(19) -0.30629(13) 0.80803(13) 0.0202(4) Uani 1 1 d . . . C60 C 0.5449(2) -0.29235(15) 0.75360(14) 0.0251(4) Uani 1 1 d . . . H60 H 0.6029 -0.2617 0.7566 0.033 Uiso 1 1 calc R . . C61 C 0.5546(2) -0.32163(16) 0.69613(15) 0.0304(5) Uani 1 1 d . . . H61 H 0.6181 -0.3104 0.6603 0.040 Uiso 1 1 calc R . . C62 C 0.4728(2) -0.36706(15) 0.69019(14) 0.0292(5) Uani 1 1 d . . . H62 H 0.4802 -0.3877 0.6509 0.038 Uiso 1 1 calc R . . C63 C 0.3797(2) -0.38222(13) 0.74228(13) 0.0228(4) Uani 1 1 d . . . H63 H 0.3237 -0.4140 0.7391 0.030 Uiso 1 1 calc R . . C64 C 0.36766(19) -0.35137(13) 0.79917(12) 0.0190(4) Uani 1 1 d . . . C65 C 0.1535(2) -0.37167(15) 0.81642(16) 0.0298(5) Uani 1 1 d . . . H65A H 0.1273 -0.3254 0.7593 0.045 Uiso 1 1 calc R . . H65B H 0.0846 -0.3687 0.8496 0.045 Uiso 1 1 calc R . . H65C H 0.1741 -0.4283 0.8177 0.045 Uiso 1 1 calc R . . C66 C 0.3090(2) -0.43476(14) 0.93413(14) 0.0291(5) Uani 1 1 d . . . H66A H 0.3299 -0.4892 0.9312 0.044 Uiso 1 1 calc R . . H66B H 0.2420 -0.4356 0.9695 0.044 Uiso 1 1 calc R . . H66C H 0.3841 -0.4285 0.9572 0.044 Uiso 1 1 calc R . . H1 H -0.028(2) 0.1414(15) 0.5249(16) 0.023(6) Uiso 1 1 d . . . H2 H 0.075(2) -0.1542(16) 0.9850(16) 0.027(7) Uiso 1 1 d . . . H58B H 0.424(2) -0.3029(17) 0.9147(18) 0.027(7) Uiso 1 1 d . . . H49A H 0.371(3) 0.1920(18) 0.6615(18) 0.036(8) Uiso 1 1 d . . . H58A H 0.498(3) -0.2399(18) 0.8634(18) 0.036(8) Uiso 1 1 d . . . H49B H 0.252(2) 0.2642(16) 0.6043(16) 0.023(6) Uiso 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 Sm1 0.01774(5) 0.01224(5) 0.00852(4) -0.00428(3) 0.00163(3) -0.00390(4) Sm2 0.01583(5) 0.01258(5) 0.00946(4) -0.00496(3) 0.00223(3) -0.00267(3) B1 0.0182(10) 0.0165(10) 0.0122(9) -0.0050(8) 0.0026(7) -0.0068(8) B2 0.0174(10) 0.0139(9) 0.0120(9) -0.0050(8) 0.0030(7) -0.0020(8) N1 0.0191(8) 0.0135(7) 0.0106(7) -0.0029(6) 0.0011(6) -0.0042(6) N2 0.0176(8) 0.0144(7) 0.0133(7) -0.0067(6) 0.0021(6) -0.0040(6) N3 0.0180(8) 0.0124(7) 0.0115(7) -0.0036(6) 0.0033(6) -0.0022(6) N4 0.0181(8) 0.0132(7) 0.0112(7) -0.0053(6) 0.0026(6) -0.0039(6) N5 0.0283(9) 0.0144(8) 0.0159(8) -0.0065(7) 0.0012(7) -0.0057(7) N6 0.0233(9) 0.0159(8) 0.0202(8) -0.0082(7) 0.0060(7) -0.0032(7) C1 0.0209(9) 0.0146(8) 0.0106(8) -0.0035(7) -0.0008(7) -0.0060(7) C2 0.0218(9) 0.0158(8) 0.0116(8) -0.0066(7) 0.0018(7) -0.0076(7) C3 0.0295(11) 0.0167(9) 0.0117(8) -0.0040(7) 0.0015(7) -0.0096(8) C4 0.0288(11) 0.0150(9) 0.0155(9) -0.0020(7) -0.0039(8) -0.0047(8) C5 0.0225(10) 0.0164(9) 0.0190(10) -0.0042(8) -0.0015(8) -0.0016(8) C6 0.0205(9) 0.0171(9) 0.0145(9) -0.0040(7) 0.0009(7) -0.0060(7) C7 0.0243(10) 0.0184(9) 0.0128(8) -0.0081(7) 0.0042(7) -0.0082(8) C8 0.0328(12) 0.0240(10) 0.0242(11) -0.0162(9) 0.0070(9) -0.0105(9) C9 0.0269(11) 0.0245(10) 0.0242(10) -0.0151(9) 0.0101(8) -0.0127(9) C10 0.0199(10) 0.0244(10) 0.0202(10) -0.0012(8) 0.0042(8) -0.0044(8) C11 0.0297(13) 0.0369(13) 0.0302(13) 0.0016(11) -0.0014(10) -0.0178(11) C12 0.0326(14) 0.0392(14) 0.0365(15) -0.0032(12) 0.0161(12) 0.0030(11) C13 0.0212(9) 0.0133(8) 0.0075(7) -0.0036(6) 0.0009(6) -0.0036(7) C14 0.0201(9) 0.0179(9) 0.0114(8) -0.0062(7) 0.0026(7) -0.0045(7) C15 0.0227(10) 0.0197(9) 0.0117(8) -0.0062(7) 0.0037(7) -0.0010(8) C16 0.0310(11) 0.0154(9) 0.0114(8) -0.0066(7) 0.0021(7) -0.0015(8) C17 0.0271(10) 0.0158(9) 0.0116(8) -0.0055(7) -0.0003(7) -0.0060(8) C18 0.0205(9) 0.0138(8) 0.0091(8) -0.0037(7) -0.0005(7) -0.0037(7) C19 0.0192(9) 0.0172(9) 0.0143(9) -0.0052(7) 0.0010(7) -0.0064(7) C20 0.0252(10) 0.0240(10) 0.0157(9) -0.0054(8) 0.0024(8) -0.0095(8) C21 0.0244(10) 0.0253(10) 0.0166(9) -0.0051(8) -0.0018(8) -0.0082(9) C22 0.0197(10) 0.0215(10) 0.0190(9) -0.0097(8) 0.0049(7) -0.0062(8) C23 0.0183(10) 0.0334(12) 0.0290(12) -0.0157(10) 0.0049(8) -0.0063(9) C24 0.0271(11) 0.0276(11) 0.0249(11) -0.0095(9) 0.0095(9) -0.0116(9) C25 0.0208(9) 0.0112(8) 0.0126(8) -0.0055(7) 0.0044(7) -0.0027(7) C26 0.0219(9) 0.0135(8) 0.0134(8) -0.0057(7) 0.0032(7) -0.0016(7) C27 0.0323(11) 0.0153(9) 0.0131(9) -0.0032(7) 0.0008(8) -0.0026(8) C28 0.0387(13) 0.0169(9) 0.0169(10) -0.0039(8) 0.0067(9) -0.0105(9) C29 0.0283(11) 0.0191(9) 0.0196(10) -0.0077(8) 0.0070(8) -0.0099(8) C30 0.0209(9) 0.0154(9) 0.0156(9) -0.0067(7) 0.0048(7) -0.0033(7) C31 0.0206(9) 0.0176(9) 0.0159(9) -0.0074(7) 0.0013(7) -0.0019(7) C32 0.0276(11) 0.0355(12) 0.0319(12) -0.0240(11) 0.0046(9) -0.0075(10) C33 0.0249(11) 0.0261(11) 0.0341(13) -0.0159(10) -0.0063(9) 0.0038(9) C34 0.0195(10) 0.0211(10) 0.0195(10) -0.0054(8) 0.0018(8) -0.0052(8) C35 0.0243(11) 0.0234(11) 0.0252(11) -0.0031(9) 0.0072(9) -0.0002(9) C36 0.0336(13) 0.0346(13) 0.0419(15) -0.0108(12) -0.0100(11) -0.0114(11) C37 0.0202(9) 0.0133(8) 0.0071(7) -0.0033(6) 0.0029(6) -0.0041(7) C38 0.0199(9) 0.0158(8) 0.0089(8) -0.0040(7) 0.0010(7) -0.0049(7) C39 0.0260(10) 0.0172(9) 0.0101(8) -0.0051(7) 0.0012(7) -0.0092(8) C40 0.0329(11) 0.0128(8) 0.0104(8) -0.0052(7) 0.0047(7) -0.0071(8) C41 0.0255(10) 0.0151(9) 0.0117(8) -0.0054(7) 0.0053(7) -0.0026(7) C42 0.0190(9) 0.0148(8) 0.0077(7) -0.0032(7) 0.0039(6) -0.0042(7) C43 0.0184(9) 0.0189(9) 0.0183(9) -0.0087(8) 0.0014(7) -0.0045(7) C44 0.0247(11) 0.0224(10) 0.0214(10) -0.0052(9) -0.0045(8) -0.0011(8) C45 0.0194(10) 0.0264(11) 0.0290(11) -0.0118(9) 0.0022(8) -0.0078(8) C46 0.0195(9) 0.0154(8) 0.0114(8) -0.0034(7) 0.0028(7) -0.0023(7) C47 0.0230(10) 0.0231(10) 0.0162(9) -0.0052(8) -0.0002(8) -0.0015(8) C48 0.0232(10) 0.0278(11) 0.0154(9) -0.0047(8) 0.0060(8) -0.0063(9) C49 0.0236(10) 0.0244(10) 0.0214(10) -0.0129(9) 0.0068(8) -0.0094(8) C50 0.0281(11) 0.0175(9) 0.0146(9) -0.0053(7) 0.0063(8) -0.0128(8) C51 0.0284(11) 0.0265(11) 0.0237(11) -0.0083(9) 0.0048(9) -0.0152(9) C52 0.0382(13) 0.0358(13) 0.0187(10) -0.0085(9) -0.0012(9) -0.0226(11) C53 0.0523(15) 0.0302(12) 0.0143(9) -0.0108(9) 0.0076(9) -0.0239(11) C54 0.0377(12) 0.0187(9) 0.0153(9) -0.0076(8) 0.0072(8) -0.0134(9) C55 0.0300(11) 0.0156(9) 0.0119(8) -0.0047(7) 0.0036(7) -0.0103(8) C56 0.0456(14) 0.0156(9) 0.0141(9) -0.0054(8) -0.0028(9) -0.0085(9) C57 0.0278(11) 0.0209(10) 0.0316(12) -0.0119(9) 0.0030(9) -0.0029(9) C58 0.0200(10) 0.0256(10) 0.0214(10) -0.0142(9) 0.0000(8) -0.0015(8) C59 0.0173(9) 0.0209(9) 0.0183(9) -0.0095(8) -0.0003(7) 0.0025(7) C60 0.0178(10) 0.0294(11) 0.0272(11) -0.0150(9) 0.0028(8) -0.0013(8) C61 0.0266(12) 0.0362(13) 0.0282(12) -0.0178(10) 0.0109(9) -0.0025(10) C62 0.0384(13) 0.0268(11) 0.0220(11) -0.0153(9) 0.0055(9) 0.0002(10) C63 0.0279(11) 0.0177(9) 0.0198(10) -0.0099(8) -0.0014(8) 0.0013(8) C64 0.0213(10) 0.0163(9) 0.0158(9) -0.0074(7) 0.0014(7) 0.0010(7) C65 0.0277(12) 0.0231(11) 0.0394(14) -0.0147(10) 0.0063(10) -0.0083(9) C66 0.0417(14) 0.0179(10) 0.0212(11) -0.0072(8) 0.0112(10) -0.0013(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 N1 2.2978(16) . ? Sm1 N2 2.3035(16) . ? Sm1 C49 2.484(2) . ? Sm1 N5 2.6178(17) . ? Sm1 B1 2.700(2) . ? Sm1 C41 2.8713(19) . ? Sm1 C40 2.8898(19) . ? Sm1 C39 2.9867(19) . ? Sm1 C42 3.0159(18) . ? Sm1 C50 3.058(2) . ? Sm2 N3 2.2964(16) . ? Sm2 N4 2.3050(16) . ? Sm2 C58 2.465(2) . ? Sm2 N6 2.6523(17) . ? Sm2 B2 2.698(2) . ? Sm2 C17 2.8956(19) . ? Sm2 C16 2.9255(19) . ? Sm2 C59 2.987(2) . ? Sm2 C18 3.0469(18) . ? Sm2 C15 3.0486(19) . ? B1 N1 1.422(3) . ? B1 N2 1.448(3) . ? B1 H1 1.08(3) . ? B2 N3 1.421(3) . ? B2 N4 1.450(3) . ? B2 H2 1.09(3) . ? N1 C1 1.418(2) . ? N2 C13 1.382(2) . ? N3 C25 1.412(2) . ? N4 C37 1.380(2) . ? N5 C55 1.457(3) . ? N5 C57 1.471(3) . ? N5 C56 1.480(3) . ? N6 C64 1.455(3) . ? N6 C65 1.470(3) . ? N6 C66 1.480(3) . ? C1 C6 1.417(3) . ? C1 C2 1.418(3) . ? C2 C3 1.401(3) . ? C2 C7 1.519(3) . ? C3 C4 1.382(3) . ? C3 H3 0.9500 . ? C4 C5 1.387(3) . ? C4 H4 0.9500 . ? C5 C6 1.397(3) . ? C5 H5 0.9500 . ? C6 C10 1.519(3) . ? C7 C8 1.531(3) . ? C7 C9 1.537(3) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.529(4) . ? C10 C12 1.532(3) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C18 1.427(3) . ? C13 C14 1.434(3) . ? C14 C15 1.393(3) . ? C14 C22 1.518(3) . ? C15 C16 1.394(3) . ? C15 H15 0.9500 . ? C16 C17 1.388(3) . ? C16 H16 0.9500 . ? C17 C18 1.404(3) . ? C17 H17 0.9500 . ? C18 C19 1.513(3) . ? C19 C20 1.535(3) . ? C19 C21 1.539(3) . ? C19 H19 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.534(3) . ? C22 C24 1.535(3) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C30 1.413(3) . ? C25 C26 1.415(3) . ? C26 C27 1.404(3) . ? C26 C31 1.520(3) . ? C27 C28 1.375(3) . ? C27 H27 0.9500 . ? C28 C29 1.388(3) . ? C28 H28 0.9500 . ? C29 C30 1.401(3) . ? C29 H29 0.9500 . ? C30 C34 1.513(3) . ? C31 C32 1.526(3) . ? C31 C33 1.533(3) . ? C31 H31 1.0000 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C36 1.526(3) . ? C34 C35 1.528(3) . ? C34 H34 1.0000 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.431(3) . ? C37 C42 1.432(3) . ? C38 C39 1.389(3) . ? C38 C43 1.522(3) . ? C39 C40 1.392(3) . ? C39 H39 0.9500 . ? C40 C41 1.389(3) . ? C40 H40 0.9500 . ? C41 C42 1.403(3) . ? C41 H41 0.9500 . ? C42 C46 1.515(3) . ? C43 C45 1.530(3) . ? C43 C44 1.534(3) . ? C43 H43 1.0000 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 C47 1.531(3) . ? C46 C48 1.537(3) . ? C46 H46 1.0000 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 C50 1.475(3) . ? C49 H49A 0.98(3) . ? C49 H49B 1.00(3) . ? C50 C51 1.408(3) . ? C50 C55 1.418(3) . ? C51 C52 1.383(3) . ? C51 H51 0.9500 . ? C52 C53 1.384(4) . ? C52 H52 0.9500 . ? C53 C54 1.382(3) . ? C53 H53 0.9500 . ? C54 C55 1.393(3) . ? C54 H54 0.9500 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 C59 1.468(3) . ? C58 H58B 0.91(3) . ? C58 H58A 0.93(3) . ? C59 C60 1.411(3) . ? C59 C64 1.417(3) . ? C60 C61 1.380(3) . ? C60 H60 0.9500 . ? C61 C62 1.380(4) . ? C61 H61 0.9500 . ? C62 C63 1.387(3) . ? C62 H62 0.9500 . ? C63 C64 1.390(3) . ? C63 H63 0.9500 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Sm1 N2 64.14(6) . . ? N1 Sm1 C49 107.09(7) . . ? N2 Sm1 C49 110.41(6) . . ? N1 Sm1 N5 84.00(6) . . ? N2 Sm1 N5 146.47(5) . . ? C49 Sm1 N5 67.64(7) . . ? N1 Sm1 B1 31.77(6) . . ? N2 Sm1 B1 32.43(6) . . ? C49 Sm1 B1 110.92(7) . . ? N5 Sm1 B1 114.87(6) . . ? N1 Sm1 C41 123.58(6) . . ? N2 Sm1 C41 113.38(6) . . ? C49 Sm1 C41 123.23(7) . . ? N5 Sm1 C41 92.31(5) . . ? B1 Sm1 C41 125.48(6) . . ? N1 Sm1 C40 145.91(6) . . ? N2 Sm1 C40 131.25(5) . . ? C49 Sm1 C40 95.34(7) . . ? N5 Sm1 C40 81.19(5) . . ? B1 Sm1 C40 152.74(6) . . ? C41 Sm1 C40 27.90(6) . . ? N1 Sm1 C39 171.58(6) . . ? N2 Sm1 C39 116.07(5) . . ? C49 Sm1 C39 80.91(6) . . ? N5 Sm1 C39 97.00(5) . . ? B1 Sm1 C39 148.12(6) . . ? C41 Sm1 C39 48.11(6) . . ? C40 Sm1 C39 27.34(6) . . ? N1 Sm1 C42 116.74(5) . . ? N2 Sm1 C42 86.35(5) . . ? C49 Sm1 C42 135.99(6) . . ? N5 Sm1 C42 119.10(5) . . ? B1 Sm1 C42 104.51(6) . . ? C41 Sm1 C42 27.43(5) . . ? C40 Sm1 C42 48.77(5) . . ? C39 Sm1 C42 55.52(5) . . ? N1 Sm1 C50 120.04(5) . . ? N2 Sm1 C50 138.34(6) . . ? C49 Sm1 C50 28.54(6) . . ? N5 Sm1 C50 50.21(6) . . ? B1 Sm1 C50 136.03(6) . . ? C41 Sm1 C50 98.03(6) . . ? C40 Sm1 C50 71.23(5) . . ? C39 Sm1 C50 65.95(5) . . ? C42 Sm1 C50 118.80(5) . . ? N3 Sm2 N4 64.21(6) . . ? N3 Sm2 C58 102.88(7) . . ? N4 Sm2 C58 108.39(6) . . ? N3 Sm2 N6 82.96(5) . . ? N4 Sm2 N6 145.68(5) . . ? C58 Sm2 N6 67.83(7) . . ? N3 Sm2 B2 31.77(6) . . ? N4 Sm2 B2 32.49(6) . . ? C58 Sm2 B2 107.17(7) . . ? N6 Sm2 B2 113.91(6) . . ? N3 Sm2 C17 128.75(6) . . ? N4 Sm2 C17 113.68(6) . . ? C58 Sm2 C17 123.33(7) . . ? N6 Sm2 C17 94.17(6) . . ? B2 Sm2 C17 128.71(6) . . ? N3 Sm2 C16 151.41(6) . . ? N4 Sm2 C16 129.51(5) . . ? C58 Sm2 C16 95.78(7) . . ? N6 Sm2 C16 84.30(5) . . ? B2 Sm2 C16 154.68(6) . . ? C17 Sm2 C16 27.58(6) . . ? N3 Sm2 C59 117.96(6) . . ? N4 Sm2 C59 136.83(6) . . ? C58 Sm2 C59 29.28(6) . . ? N6 Sm2 C59 50.94(6) . . ? B2 Sm2 C59 133.64(6) . . ? C17 Sm2 C59 97.54(6) . . ? C16 Sm2 C59 71.33(6) . . ? N3 Sm2 C18 120.13(5) . . ? N4 Sm2 C18 86.64(5) . . ? C58 Sm2 C18 136.55(7) . . ? N6 Sm2 C18 120.37(5) . . ? B2 Sm2 C18 106.48(6) . . ? C17 Sm2 C18 27.17(5) . . ? C16 Sm2 C18 48.22(5) . . ? C59 Sm2 C18 118.70(5) . . ? N3 Sm2 C15 174.69(6) . . ? N4 Sm2 C15 113.02(5) . . ? C58 Sm2 C15 82.23(7) . . ? N6 Sm2 C15 100.48(5) . . ? B2 Sm2 C15 145.46(6) . . ? C17 Sm2 C15 47.33(6) . . ? C16 Sm2 C15 26.88(6) . . ? C59 Sm2 C15 67.26(6) . . ? C18 Sm2 C15 54.64(5) . . ? N1 B1 N2 116.73(18) . . ? N1 B1 Sm1 58.32(10) . . ? N2 B1 Sm1 58.54(10) . . ? N1 B1 H1 120.7(13) . . ? N2 B1 H1 122.6(13) . . ? Sm1 B1 H1 176.2(13) . . ? N3 B2 N4 116.86(17) . . ? N3 B2 Sm2 58.33(10) . . ? N4 B2 Sm2 58.66(10) . . ? N3 B2 H2 121.3(13) . . ? N4 B2 H2 121.7(13) . . ? Sm2 B2 H2 173.7(14) . . ? C1 N1 B1 121.31(17) . . ? C1 N1 Sm1 146.29(13) . . ? B1 N1 Sm1 89.91(12) . . ? C13 N2 B1 120.80(16) . . ? C13 N2 Sm1 149.89(13) . . ? B1 N2 Sm1 89.03(12) . . ? C25 N3 B2 121.81(16) . . ? C25 N3 Sm2 146.21(13) . . ? B2 N3 Sm2 89.90(11) . . ? C37 N4 B2 118.91(16) . . ? C37 N4 Sm2 152.06(12) . . ? B2 N4 Sm2 88.85(11) . . ? C55 N5 C57 114.65(17) . . ? C55 N5 C56 110.14(16) . . ? C57 N5 C56 108.25(17) . . ? C55 N5 Sm1 96.11(11) . . ? C57 N5 Sm1 105.70(12) . . ? C56 N5 Sm1 121.89(12) . . ? C64 N6 C65 114.36(18) . . ? C64 N6 C66 110.68(17) . . ? C65 N6 C66 108.63(18) . . ? C64 N6 Sm2 92.65(11) . . ? C65 N6 Sm2 105.17(12) . . ? C66 N6 Sm2 124.84(13) . . ? N1 C1 C6 120.09(17) . . ? N1 C1 C2 121.20(18) . . ? C6 C1 C2 118.64(17) . . ? C3 C2 C1 119.43(18) . . ? C3 C2 C7 118.89(17) . . ? C1 C2 C7 121.64(17) . . ? C4 C3 C2 121.78(19) . . ? C4 C3 H3 119.1 . . ? C2 C3 H3 119.1 . . ? C3 C4 C5 118.82(19) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? C4 C5 C6 121.6(2) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C5 C6 C1 119.66(18) . . ? C5 C6 C10 120.02(19) . . ? C1 C6 C10 120.23(17) . . ? C2 C7 C8 111.49(17) . . ? C2 C7 C9 113.09(17) . . ? C8 C7 C9 109.46(16) . . ? C2 C7 H7 107.5 . . ? C8 C7 H7 107.5 . . ? C9 C7 H7 107.5 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C6 C10 C11 109.7(2) . . ? C6 C10 C12 113.97(19) . . ? C11 C10 C12 111.1(2) . . ? C6 C10 H10 107.2 . . ? C11 C10 H10 107.2 . . ? C12 C10 H10 107.2 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N2 C13 C18 122.43(17) . . ? N2 C13 C14 119.90(17) . . ? C18 C13 C14 117.65(17) . . ? C15 C14 C13 120.12(18) . . ? C15 C14 C22 119.84(18) . . ? C13 C14 C22 119.63(17) . . ? C14 C15 C16 121.82(19) . . ? C14 C15 Sm2 83.22(11) . . ? C16 C15 Sm2 71.63(11) . . ? C14 C15 H15 119.1 . . ? C16 C15 H15 119.1 . . ? Sm2 C15 H15 116.5 . . ? C17 C16 C15 118.47(18) . . ? C17 C16 Sm2 75.01(11) . . ? C15 C16 Sm2 81.49(11) . . ? C17 C16 H16 120.8 . . ? C15 C16 H16 120.8 . . ? Sm2 C16 H16 113.4 . . ? C16 C17 C18 122.06(19) . . ? C16 C17 Sm2 77.41(11) . . ? C18 C17 Sm2 82.43(11) . . ? C16 C17 H17 119.0 . . ? C18 C17 H17 119.0 . . ? Sm2 C17 H17 111.2 . . ? C17 C18 C13 119.69(18) . . ? C17 C18 C19 117.57(17) . . ? C13 C18 C19 122.68(17) . . ? C17 C18 Sm2 70.40(11) . . ? C13 C18 Sm2 85.07(11) . . ? C19 C18 Sm2 116.86(11) . . ? C18 C19 C20 111.55(16) . . ? C18 C19 C21 111.68(17) . . ? C20 C19 C21 109.54(17) . . ? C18 C19 H19 108.0 . . ? C20 C19 H19 108.0 . . ? C21 C19 H19 108.0 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C14 C22 C23 114.07(18) . . ? C14 C22 C24 109.67(17) . . ? C23 C22 C24 109.82(18) . . ? C14 C22 H22 107.7 . . ? C23 C22 H22 107.7 . . ? C24 C22 H22 107.7 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N3 C25 C30 119.33(17) . . ? N3 C25 C26 121.82(18) . . ? C30 C25 C26 118.80(17) . . ? C27 C26 C25 119.71(19) . . ? C27 C26 C31 118.33(18) . . ? C25 C26 C31 121.96(17) . . ? C28 C27 C26 121.2(2) . . ? C28 C27 H27 119.4 . . ? C26 C27 H27 119.4 . . ? C27 C28 C29 119.50(19) . . ? C27 C28 H28 120.2 . . ? C29 C28 H28 120.2 . . ? C28 C29 C30 121.3(2) . . ? C28 C29 H29 119.4 . . ? C30 C29 H29 119.4 . . ? C29 C30 C25 119.50(19) . . ? C29 C30 C34 120.28(19) . . ? C25 C30 C34 120.17(17) . . ? C26 C31 C32 110.04(17) . . ? C26 C31 C33 113.23(17) . . ? C32 C31 C33 109.80(18) . . ? C26 C31 H31 107.9 . . ? C32 C31 H31 107.9 . . ? C33 C31 H31 107.9 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C30 C34 C36 113.97(18) . . ? C30 C34 C35 110.55(18) . . ? C36 C34 C35 110.5(2) . . ? C30 C34 H34 107.2 . . ? C36 C34 H34 107.2 . . ? C35 C34 H34 107.2 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N4 C37 C38 120.33(17) . . ? N4 C37 C42 121.91(17) . . ? C38 C37 C42 117.72(17) . . ? C39 C38 C37 120.09(18) . . ? C39 C38 C43 120.02(18) . . ? C37 C38 C43 119.54(17) . . ? C38 C39 C40 122.00(19) . . ? C38 C39 Sm1 82.72(11) . . ? C40 C39 Sm1 72.45(11) . . ? C38 C39 H39 119.0 . . ? C40 C39 H39 119.0 . . ? Sm1 C39 H39 116.2 . . ? C41 C40 C39 118.49(18) . . ? C41 C40 Sm1 75.31(11) . . ? C39 C40 Sm1 80.21(11) . . ? C41 C40 H40 120.8 . . ? C39 C40 H40 120.8 . . ? Sm1 C40 H40 114.5 . . ? C40 C41 C42 121.96(19) . . ? C40 C41 Sm1 76.79(11) . . ? C42 C41 Sm1 82.03(11) . . ? C40 C41 H41 119.0 . . ? C42 C41 H41 119.0 . . ? Sm1 C41 H41 112.2 . . ? C41 C42 C37 119.56(18) . . ? C41 C42 C46 117.56(17) . . ? C37 C42 C46 122.80(17) . . ? C41 C42 Sm1 70.54(10) . . ? C37 C42 Sm1 83.77(10) . . ? C46 C42 Sm1 118.47(11) . . ? C38 C43 C45 113.94(17) . . ? C38 C43 C44 109.60(17) . . ? C45 C43 C44 109.62(17) . . ? C38 C43 H43 107.8 . . ? C45 C43 H43 107.8 . . ? C44 C43 H43 107.8 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C42 C46 C47 112.31(16) . . ? C42 C46 C48 110.60(17) . . ? C47 C46 C48 109.26(17) . . ? C42 C46 H46 108.2 . . ? C47 C46 H46 108.2 . . ? C48 C46 H46 108.2 . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C46 C48 H48A 109.5 . . ? C46 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C46 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C50 C49 Sm1 97.90(13) . . ? C50 C49 H49A 117.4(17) . . ? Sm1 C49 H49A 126.4(16) . . ? C50 C49 H49B 116.0(14) . . ? Sm1 C49 H49B 93.2(14) . . ? H49A C49 H49B 104(2) . . ? C51 C50 C55 115.71(19) . . ? C51 C50 C49 122.1(2) . . ? C55 C50 C49 121.80(19) . . ? C51 C50 Sm1 137.80(14) . . ? C55 C50 Sm1 79.53(12) . . ? C49 C50 Sm1 53.55(10) . . ? C52 C51 C50 122.2(2) . . ? C52 C51 H51 118.9 . . ? C50 C51 H51 118.9 . . ? C51 C52 C53 120.5(2) . . ? C51 C52 H52 119.8 . . ? C53 C52 H52 119.8 . . ? C54 C53 C52 119.4(2) . . ? C54 C53 H53 120.3 . . ? C52 C53 H53 120.3 . . ? C53 C54 C55 120.2(2) . . ? C53 C54 H54 119.9 . . ? C55 C54 H54 119.9 . . ? C54 C55 C50 121.9(2) . . ? C54 C55 N5 121.8(2) . . ? C50 C55 N5 116.28(17) . . ? N5 C56 H56A 109.5 . . ? N5 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? N5 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? N5 C57 H57A 109.5 . . ? N5 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? N5 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C59 C58 Sm2 95.47(13) . . ? C59 C58 H58B 113.8(16) . . ? Sm2 C58 H58B 96.2(17) . . ? C59 C58 H58A 113.8(18) . . ? Sm2 C58 H58A 127.3(17) . . ? H58B C58 H58A 109(2) . . ? C60 C59 C64 115.69(19) . . ? C60 C59 C58 121.3(2) . . ? C64 C59 C58 122.52(19) . . ? C60 C59 Sm2 134.05(14) . . ? C64 C59 Sm2 80.34(12) . . ? C58 C59 Sm2 55.24(11) . . ? C61 C60 C59 122.4(2) . . ? C61 C60 H60 118.8 . . ? C59 C60 H60 118.8 . . ? C62 C61 C60 120.6(2) . . ? C62 C61 H61 119.7 . . ? C60 C61 H61 119.7 . . ? C61 C62 C63 119.1(2) . . ? C61 C62 H62 120.5 . . ? C63 C62 H62 120.5 . . ? C62 C63 C64 120.6(2) . . ? C62 C63 H63 119.7 . . ? C64 C63 H63 119.7 . . ? C63 C64 C59 121.5(2) . . ? C63 C64 N6 121.81(19) . . ? C59 C64 N6 116.61(18) . . ? N6 C65 H65A 109.5 . . ? N6 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? N6 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? N6 C66 H66A 109.5 . . ? N6 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? N6 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 30.79 _diffrn_measured_fraction_theta_full 0.940 _refine_diff_density_max 1.443 _refine_diff_density_min -0.830 _refine_diff_density_rms 0.094 # Attachment 'hasj277-NBNYDMA.cif' data_hasj277 _database_code_depnum_ccdc_archive 'CCDC 763736' #TrackingRef 'hasj277-NBNYDMA.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ((DIPP-NBN)Y(DMA)) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H100 B2 N6 Y2' _chemical_formula_weight 1249.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.1964(8) _cell_length_b 16.0669(6) _cell_length_c 23.1829(10) _cell_angle_alpha 90.00 _cell_angle_beta 92.806(2) _cell_angle_gamma 90.00 _cell_volume 6769.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 103(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.226 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2648 _exptl_absorpt_coefficient_mu 1.750 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4748 _exptl_absorpt_correction_T_max 0.8444 _exptl_absorpt_process_details ; BRUKER AXS SMART APEX 2 Vers. 1.0-27 R.H. Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 103(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 68204 _diffrn_reflns_av_R_equivalents 0.0414 _diffrn_reflns_av_sigmaI/netI 0.0382 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.12 _diffrn_reflns_theta_max 24.48 _reflns_number_total 11139 _reflns_number_gt 9167 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+23.2972P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11139 _refine_ls_number_parameters 783 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0617 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.1079 _refine_ls_wR_factor_gt 0.1036 _refine_ls_goodness_of_fit_ref 1.262 _refine_ls_restrained_S_all 1.262 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1535(2) 1.2933(3) -0.00010(18) 0.0151(9) Uani 1 1 d . . . C2 C 0.1698(2) 1.3234(3) -0.05542(17) 0.0182(9) Uani 1 1 d . . . C3 C 0.1393(2) 1.3981(3) -0.07556(19) 0.0218(10) Uani 1 1 d . . . H3 H 0.1507 1.4178 -0.1127 0.028 Uiso 1 1 calc R . . C4 C 0.0930(2) 1.4441(3) -0.04266(19) 0.0220(10) Uani 1 1 d . . . H4 H 0.0731 1.4953 -0.0567 0.029 Uiso 1 1 calc R . . C5 C 0.0758(2) 1.4148(3) 0.01093(18) 0.0183(10) Uani 1 1 d . . . H5 H 0.0429 1.4459 0.0331 0.024 Uiso 1 1 calc R . . C6 C 0.1054(2) 1.3409(3) 0.03349(18) 0.0168(9) Uani 1 1 d . . . C7 C 0.2164(3) 1.2715(3) -0.09430(19) 0.0255(11) Uani 1 1 d . . . H7 H 0.2507 1.2375 -0.0689 0.033 Uiso 1 1 calc R . . C8 C 0.1654(3) 1.2108(3) -0.1286(2) 0.0387(14) Uani 1 1 d . . . H8A H 0.1375 1.1777 -0.1017 0.058 Uiso 1 1 calc R . . H8B H 0.1950 1.1737 -0.1517 0.058 Uiso 1 1 calc R . . H8C H 0.1312 1.2424 -0.1542 0.058 Uiso 1 1 calc R . . C9 C 0.2633(3) 1.3219(4) -0.1349(2) 0.0422(14) Uani 1 1 d . . . H9A H 0.2311 1.3508 -0.1635 0.063 Uiso 1 1 calc R . . H9B H 0.2961 1.2843 -0.1547 0.063 Uiso 1 1 calc R . . H9C H 0.2926 1.3628 -0.1124 0.063 Uiso 1 1 calc R . . C10 C 0.0847(2) 1.3136(3) 0.09328(18) 0.0163(9) Uani 1 1 d . . . H10 H 0.1226 1.2726 0.1078 0.021 Uiso 1 1 calc R . . C11 C 0.0101(2) 1.2690(3) 0.09049(19) 0.0240(11) Uani 1 1 d . . . H11A H -0.0281 1.3073 0.0754 0.036 Uiso 1 1 calc R . . H11B H -0.0016 1.2507 0.1293 0.036 Uiso 1 1 calc R . . H11C H 0.0124 1.2205 0.0650 0.036 Uiso 1 1 calc R . . C12 C 0.0832(3) 1.3845(3) 0.1373(2) 0.0295(12) Uani 1 1 d . . . H12A H 0.1294 1.4158 0.1370 0.044 Uiso 1 1 calc R . . H12B H 0.0773 1.3614 0.1759 0.044 Uiso 1 1 calc R . . H12C H 0.0419 1.4217 0.1272 0.044 Uiso 1 1 calc R . . C13 C 0.1496(2) 1.0007(3) 0.06467(17) 0.0118(9) Uani 1 1 d . . . C14 C 0.1253(2) 0.9481(3) 0.01736(17) 0.0147(9) Uani 1 1 d . . . C15 C 0.0862(2) 0.8757(3) 0.02840(18) 0.0157(9) Uani 1 1 d . . . H15 H 0.0694 0.8422 -0.0033 0.020 Uiso 1 1 calc R . . C16 C 0.0970(2) 0.8992(3) 0.13005(18) 0.0154(9) Uani 1 1 d . . . H16 H 0.0879 0.8821 0.1683 0.020 Uiso 1 1 calc R . . C17 C 0.0706(2) 0.8503(3) 0.08393(18) 0.0177(10) Uani 1 1 d . . . H17 H 0.0430 0.8012 0.0902 0.023 Uiso 1 1 calc R . . C18 C 0.1363(2) 0.9725(3) 0.12187(17) 0.0144(9) Uani 1 1 d . . . C19 C 0.1359(2) 0.9710(3) -0.04527(17) 0.0167(9) Uani 1 1 d . . . H19 H 0.1700 1.0198 -0.0457 0.022 Uiso 1 1 calc R . . C20 C 0.1706(2) 0.9002(3) -0.07872(18) 0.0211(10) Uani 1 1 d . . . H20A H 0.2138 0.8789 -0.0565 0.032 Uiso 1 1 calc R . . H20B H 0.1855 0.9210 -0.1161 0.032 Uiso 1 1 calc R . . H20C H 0.1347 0.8553 -0.0849 0.032 Uiso 1 1 calc R . . C21 C 0.0638(2) 0.9963(3) -0.07661(19) 0.0244(11) Uani 1 1 d . . . H21A H 0.0293 0.9495 -0.0766 0.037 Uiso 1 1 calc R . . H21B H 0.0731 1.0117 -0.1165 0.037 Uiso 1 1 calc R . . H21C H 0.0427 1.0440 -0.0569 0.037 Uiso 1 1 calc R . . C22 C 0.1582(2) 1.0276(3) 0.17332(17) 0.0163(9) Uani 1 1 d . . . H22 H 0.2068 1.0532 0.1658 0.021 Uiso 1 1 calc R . . C23 C 0.1021(2) 1.0985(3) 0.17762(19) 0.0228(10) Uani 1 1 d . . . H23A H 0.0969 1.1277 0.1405 0.034 Uiso 1 1 calc R . . H23B H 0.1192 1.1376 0.2078 0.034 Uiso 1 1 calc R . . H23C H 0.0544 1.0754 0.1873 0.034 Uiso 1 1 calc R . . C24 C 0.1663(3) 0.9817(3) 0.23108(18) 0.0250(11) Uani 1 1 d . . . H24A H 0.1178 0.9627 0.2423 0.038 Uiso 1 1 calc R . . H24B H 0.1874 1.0194 0.2607 0.038 Uiso 1 1 calc R . . H24C H 0.1988 0.9336 0.2272 0.038 Uiso 1 1 calc R . . C25 C 0.3365(2) 0.6896(3) -0.00131(17) 0.0156(9) Uani 1 1 d . . . C26 C 0.3090(2) 0.6548(3) -0.05420(17) 0.0164(9) Uani 1 1 d . . . C27 C 0.3403(2) 0.5832(3) -0.07536(18) 0.0214(10) Uani 1 1 d . . . H27 H 0.3219 0.5612 -0.1112 0.028 Uiso 1 1 calc R . . C28 C 0.3974(3) 0.5430(3) -0.0458(2) 0.0258(11) Uani 1 1 d . . . H28 H 0.4183 0.4939 -0.0609 0.033 Uiso 1 1 calc R . . C29 C 0.4238(2) 0.5757(3) 0.00625(19) 0.0224(10) Uani 1 1 d . . . H29 H 0.4632 0.5482 0.0268 0.029 Uiso 1 1 calc R . . C30 C 0.3948(2) 0.6473(3) 0.02969(17) 0.0151(9) Uani 1 1 d . . . C31 C 0.2487(2) 0.6989(3) -0.08991(18) 0.0195(10) Uani 1 1 d . . . H31 H 0.2203 0.7338 -0.0631 0.025 Uiso 1 1 calc R . . C32 C 0.1944(3) 0.6392(3) -0.12094(19) 0.0268(11) Uani 1 1 d . . . H32A H 0.2183 0.6121 -0.1529 0.040 Uiso 1 1 calc R . . H32B H 0.1513 0.6704 -0.1361 0.040 Uiso 1 1 calc R . . H32C H 0.1787 0.5968 -0.0937 0.040 Uiso 1 1 calc R . . C33 C 0.2825(3) 0.7571(3) -0.13339(19) 0.0265(11) Uani 1 1 d . . . H33A H 0.3167 0.7954 -0.1130 0.040 Uiso 1 1 calc R . . H33B H 0.2435 0.7889 -0.1539 0.040 Uiso 1 1 calc R . . H33C H 0.3092 0.7242 -0.1612 0.040 Uiso 1 1 calc R . . C34 C 0.4259(2) 0.6771(3) 0.08821(17) 0.0183(10) Uani 1 1 d . . . H34 H 0.3912 0.7197 0.1026 0.024 Uiso 1 1 calc R . . C35 C 0.5011(2) 0.7191(3) 0.08394(19) 0.0239(11) Uani 1 1 d . . . H35A H 0.5369 0.6783 0.0713 0.036 Uiso 1 1 calc R . . H35B H 0.5174 0.7411 0.1219 0.036 Uiso 1 1 calc R . . H35C H 0.4970 0.7648 0.0560 0.036 Uiso 1 1 calc R . . C36 C 0.4319(3) 0.6074(3) 0.13313(19) 0.0245(11) Uani 1 1 d . . . H36A H 0.3842 0.5795 0.1351 0.037 Uiso 1 1 calc R . . H36B H 0.4463 0.6310 0.1710 0.037 Uiso 1 1 calc R . . H36C H 0.4691 0.5670 0.1221 0.037 Uiso 1 1 calc R . . C37 C 0.3489(2) 0.9823(3) 0.06090(17) 0.0143(9) Uani 1 1 d . . . C38 C 0.3715(2) 1.0116(3) 0.11725(18) 0.0151(9) Uani 1 1 d . . . C39 C 0.4130(2) 1.0849(3) 0.12316(19) 0.0178(10) Uani 1 1 d . . . H39 H 0.4295 1.1027 0.1607 0.023 Uiso 1 1 calc R . . C40 C 0.4305(2) 1.1320(3) 0.07582(18) 0.0188(10) Uani 1 1 d . . . H40 H 0.4585 1.1817 0.0807 0.024 Uiso 1 1 calc R . . C41 C 0.4065(2) 1.1054(3) 0.02094(19) 0.0193(10) Uani 1 1 d . . . H41 H 0.4182 1.1378 -0.0116 0.025 Uiso 1 1 calc R . . C42 C 0.3659(2) 1.0327(3) 0.01242(18) 0.0152(9) Uani 1 1 d . . . C43 C 0.3583(2) 0.9584(3) 0.16945(18) 0.0194(10) Uani 1 1 d . . . H43 H 0.3083 0.9329 0.1635 0.025 Uiso 1 1 calc R . . C44 C 0.4146(3) 0.8873(3) 0.1725(2) 0.0265(11) Uani 1 1 d . . . H44A H 0.4156 0.8601 0.1347 0.040 Uiso 1 1 calc R . . H44B H 0.4007 0.8467 0.2015 0.040 Uiso 1 1 calc R . . H44C H 0.4635 0.9098 0.1831 0.040 Uiso 1 1 calc R . . C45 C 0.3601(3) 1.0047(3) 0.22715(18) 0.0254(11) Uani 1 1 d . . . H45A H 0.4103 1.0240 0.2368 0.038 Uiso 1 1 calc R . . H45B H 0.3444 0.9672 0.2575 0.038 Uiso 1 1 calc R . . H45C H 0.3268 1.0527 0.2242 0.038 Uiso 1 1 calc R . . C46 C 0.3452(2) 1.0072(3) -0.04946(17) 0.0180(10) Uani 1 1 d . . . H46 H 0.3112 0.9584 -0.0482 0.023 Uiso 1 1 calc R . . C47 C 0.3056(2) 1.0764(3) -0.08373(19) 0.0215(10) Uani 1 1 d . . . H47A H 0.2666 1.0997 -0.0609 0.032 Uiso 1 1 calc R . . H47B H 0.2839 1.0536 -0.1199 0.032 Uiso 1 1 calc R . . H47C H 0.3408 1.1203 -0.0924 0.032 Uiso 1 1 calc R . . C48 C 0.4134(3) 0.9805(3) -0.08054(19) 0.0276(11) Uani 1 1 d . . . H48A H 0.4472 1.0278 -0.0828 0.041 Uiso 1 1 calc R . . H48B H 0.3988 0.9615 -0.1196 0.041 Uiso 1 1 calc R . . H48C H 0.4381 0.9350 -0.0591 0.041 Uiso 1 1 calc R . . C49 C 0.2772(2) 1.2141(3) 0.17170(19) 0.0186(10) Uani 1 1 d . . . C50 C 0.3511(2) 1.2524(3) 0.17850(18) 0.0176(10) Uani 1 1 d . . . C51 C 0.3992(2) 1.2353(3) 0.22638(19) 0.0210(10) Uani 1 1 d . . . H51 H 0.3818 1.2033 0.2574 0.027 Uiso 1 1 calc R . . C52 C 0.4714(3) 1.2638(3) 0.2297(2) 0.0269(11) Uani 1 1 d . . . H52 H 0.5028 1.2500 0.2623 0.035 Uiso 1 1 calc R . . C53 C 0.4976(2) 1.3121(3) 0.1860(2) 0.0287(11) Uani 1 1 d . . . H53 H 0.5467 1.3324 0.1886 0.037 Uiso 1 1 calc R . . C54 C 0.4517(2) 1.3309(3) 0.13811(19) 0.0230(10) Uani 1 1 d . . . H54 H 0.4693 1.3646 0.1081 0.030 Uiso 1 1 calc R . . C55 C 0.3800(2) 1.3005(3) 0.13396(18) 0.0173(10) Uani 1 1 d . . . C56 C 0.2813(2) 1.3843(3) 0.0928(2) 0.0245(11) Uani 1 1 d . . . H56A H 0.2543 1.3735 0.1275 0.037 Uiso 1 1 calc R . . H56B H 0.2465 1.3903 0.0595 0.037 Uiso 1 1 calc R . . H56C H 0.3100 1.4356 0.0980 0.037 Uiso 1 1 calc R . . C57 C 0.3704(3) 1.3325(3) 0.02977(19) 0.0267(11) Uani 1 1 d . . . H57A H 0.3916 1.3885 0.0327 0.040 Uiso 1 1 calc R . . H57B H 0.3355 1.3297 -0.0037 0.040 Uiso 1 1 calc R . . H57C H 0.4098 1.2917 0.0252 0.040 Uiso 1 1 calc R . . C58 C 0.2401(2) 0.7696(3) 0.17318(19) 0.0197(10) Uani 1 1 d . . . C59 C 0.1692(2) 0.7287(3) 0.18342(18) 0.0189(10) Uani 1 1 d . . . C60 C 0.1303(3) 0.7426(3) 0.23352(19) 0.0247(11) Uani 1 1 d . . . H60 H 0.1521 0.7764 0.2633 0.032 Uiso 1 1 calc R . . C61 C 0.0621(3) 0.7090(3) 0.2408(2) 0.0331(12) Uani 1 1 d . . . H61 H 0.0378 0.7199 0.2754 0.043 Uiso 1 1 calc R . . C62 C 0.0279(3) 0.6596(3) 0.1987(2) 0.0302(12) Uani 1 1 d . . . H62 H -0.0190 0.6359 0.2043 0.039 Uiso 1 1 calc R . . C63 C 0.0638(2) 0.6454(3) 0.14809(19) 0.0235(10) Uani 1 1 d . . . H63 H 0.0410 0.6118 0.1186 0.031 Uiso 1 1 calc R . . C64 C 0.1325(2) 0.6797(3) 0.14012(17) 0.0176(9) Uani 1 1 d . . . C65 C 0.2241(3) 0.6012(3) 0.0929(2) 0.0263(11) Uani 1 1 d . . . H65A H 0.2582 0.6123 0.1260 0.039 Uiso 1 1 calc R . . H65B H 0.2518 0.5969 0.0578 0.039 Uiso 1 1 calc R . . H65C H 0.1981 0.5488 0.0991 0.039 Uiso 1 1 calc R . . C66 C 0.1202(3) 0.6506(3) 0.03595(18) 0.0231(10) Uani 1 1 d . . . H66A H 0.1003 0.5943 0.0401 0.035 Uiso 1 1 calc R . . H66B H 0.1476 0.6537 0.0006 0.035 Uiso 1 1 calc R . . H66C H 0.0797 0.6908 0.0337 0.035 Uiso 1 1 calc R . . C67 C 0.2141(4) 0.4575(4) 0.2573(2) 0.0460(16) Uani 1 1 d . . . H67 H 0.1669 0.4323 0.2575 0.060 Uiso 1 1 calc R . . C68 C 0.2765(3) 0.4090(3) 0.2557(2) 0.0403(14) Uani 1 1 d . . . H68 H 0.2719 0.3501 0.2541 0.052 Uiso 1 1 calc R . . C69 C 0.3448(3) 0.4441(3) 0.2566(2) 0.0397(14) Uani 1 1 d . . . H69 H 0.3873 0.4100 0.2558 0.052 Uiso 1 1 calc R . . C70 C 0.3515(4) 0.5301(4) 0.2586(2) 0.0498(17) Uani 1 1 d . . . H70 H 0.3989 0.5551 0.2595 0.065 Uiso 1 1 calc R . . C71 C 0.2889(5) 0.5794(4) 0.2594(2) 0.065(2) Uani 1 1 d . . . H71 H 0.2931 0.6384 0.2607 0.085 Uiso 1 1 calc R . . C72 C 0.2208(5) 0.5424(4) 0.2584(2) 0.061(2) Uani 1 1 d . . . H72 H 0.1779 0.5761 0.2585 0.079 Uiso 1 1 calc R . . B1 B 0.1461(3) 1.1443(3) 0.0263(2) 0.0171(11) Uani 1 1 d . . . B2 B 0.3462(3) 0.8383(3) 0.02463(19) 0.0149(10) Uani 1 1 d . . . N1 N 0.18648(17) 1.2194(2) 0.02177(14) 0.0127(7) Uani 1 1 d . . . N2 N 0.18360(17) 1.0764(2) 0.05685(14) 0.0118(7) Uani 1 1 d . . . N3 N 0.30483(18) 0.7628(2) 0.02075(14) 0.0128(7) Uani 1 1 d . . . N4 N 0.31353(17) 0.9064(2) 0.05496(14) 0.0124(7) Uani 1 1 d . . . N5 N 0.33183(19) 1.3136(2) 0.08274(14) 0.0178(8) Uani 1 1 d . . . N6 N 0.17013(19) 0.6701(2) 0.08643(14) 0.0179(8) Uani 1 1 d . . . Y1 Y 0.28057(2) 1.16217(2) 0.073904(17) 0.01294(10) Uani 1 1 d . . . Y2 Y 0.22037(2) 0.82058(2) 0.075598(17) 0.01296(10) Uani 1 1 d . . . H49A H 0.237(2) 1.254(3) 0.1662(17) 0.015(11) Uiso 1 1 d . . . H49B H 0.265(2) 1.182(3) 0.2062(18) 0.014(11) Uiso 1 1 d . . . H1 H 0.092(2) 1.140(2) 0.0128(17) 0.013(11) Uiso 1 1 d . . . H58Q H 0.257(2) 0.801(3) 0.207(2) 0.022(12) Uiso 1 1 d . . . H58B H 0.278(2) 0.731(3) 0.1635(18) 0.020(12) Uiso 1 1 d . . . H2 H 0.400(2) 0.842(3) 0.0070(18) 0.025(12) Uiso 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 C1 0.013(2) 0.013(2) 0.020(2) 0.0000(18) -0.0027(17) -0.0002(17) C2 0.018(2) 0.020(3) 0.017(2) 0.001(2) 0.0004(17) 0.0033(19) C3 0.024(2) 0.021(3) 0.020(2) 0.006(2) 0.0017(19) 0.001(2) C4 0.018(2) 0.016(3) 0.032(3) 0.005(2) -0.0008(19) 0.0022(19) C5 0.016(2) 0.014(2) 0.025(2) -0.004(2) 0.0015(18) 0.0032(18) C6 0.012(2) 0.016(2) 0.023(2) -0.0037(19) -0.0016(17) -0.0008(18) C7 0.032(3) 0.027(3) 0.018(2) 0.003(2) 0.007(2) 0.012(2) C8 0.051(3) 0.039(3) 0.025(3) -0.009(2) -0.006(2) 0.020(3) C9 0.050(3) 0.043(4) 0.035(3) 0.016(3) 0.024(3) 0.021(3) C10 0.015(2) 0.013(2) 0.021(2) 0.0001(19) 0.0009(17) 0.0002(18) C11 0.020(2) 0.030(3) 0.022(2) 0.001(2) 0.0024(19) -0.001(2) C12 0.035(3) 0.029(3) 0.025(3) -0.006(2) 0.005(2) -0.004(2) C13 0.0048(18) 0.012(2) 0.018(2) -0.0014(18) -0.0028(16) 0.0047(17) C14 0.011(2) 0.015(2) 0.018(2) -0.0011(19) -0.0004(17) 0.0060(18) C15 0.012(2) 0.015(2) 0.019(2) -0.0029(19) -0.0038(17) 0.0042(18) C16 0.014(2) 0.015(2) 0.017(2) 0.0035(19) 0.0040(17) 0.0055(18) C17 0.015(2) 0.014(2) 0.024(2) 0.0061(19) -0.0010(18) -0.0027(18) C18 0.011(2) 0.015(2) 0.017(2) -0.0020(18) 0.0008(17) 0.0070(18) C19 0.017(2) 0.017(2) 0.016(2) -0.0006(19) 0.0001(17) 0.0014(18) C20 0.019(2) 0.024(3) 0.020(2) -0.001(2) -0.0016(18) 0.006(2) C21 0.025(2) 0.030(3) 0.018(2) 0.002(2) -0.0009(19) 0.008(2) C22 0.017(2) 0.018(2) 0.014(2) -0.0005(18) 0.0026(17) 0.0000(18) C23 0.029(3) 0.021(3) 0.019(2) -0.004(2) 0.0068(19) 0.002(2) C24 0.032(3) 0.025(3) 0.017(2) -0.001(2) -0.001(2) -0.001(2) C25 0.016(2) 0.013(2) 0.018(2) 0.0005(18) 0.0068(17) -0.0007(18) C26 0.019(2) 0.014(2) 0.016(2) 0.0008(19) 0.0018(17) 0.0030(18) C27 0.025(2) 0.023(3) 0.016(2) -0.006(2) 0.0005(19) 0.004(2) C28 0.033(3) 0.018(3) 0.027(3) -0.007(2) 0.004(2) 0.007(2) C29 0.019(2) 0.025(3) 0.023(2) 0.002(2) 0.0016(19) 0.008(2) C30 0.015(2) 0.014(2) 0.016(2) 0.0021(18) 0.0020(17) 0.0030(18) C31 0.023(2) 0.017(2) 0.019(2) 0.0000(19) 0.0016(18) 0.0062(19) C32 0.031(3) 0.029(3) 0.021(2) -0.002(2) -0.002(2) 0.006(2) C33 0.029(3) 0.026(3) 0.024(3) 0.002(2) 0.002(2) 0.008(2) C34 0.016(2) 0.019(3) 0.019(2) 0.000(2) 0.0012(17) 0.0070(19) C35 0.022(2) 0.026(3) 0.023(2) 0.002(2) -0.0005(19) 0.002(2) C36 0.026(3) 0.026(3) 0.022(2) 0.000(2) 0.001(2) 0.002(2) C37 0.0071(19) 0.016(2) 0.020(2) -0.0015(19) 0.0025(16) 0.0061(17) C38 0.0074(19) 0.015(2) 0.022(2) -0.0007(19) -0.0020(17) 0.0071(17) C39 0.009(2) 0.018(2) 0.025(2) -0.005(2) -0.0051(18) 0.0062(18) C40 0.013(2) 0.017(2) 0.026(2) -0.004(2) 0.0004(18) -0.0053(18) C41 0.016(2) 0.018(3) 0.024(2) -0.001(2) 0.0065(18) 0.0049(19) C42 0.010(2) 0.016(2) 0.019(2) 0.0006(19) 0.0009(17) 0.0064(18) C43 0.023(2) 0.018(3) 0.017(2) -0.0008(19) -0.0045(18) 0.0004(19) C44 0.030(3) 0.023(3) 0.025(3) 0.001(2) -0.011(2) 0.007(2) C45 0.032(3) 0.024(3) 0.020(2) -0.001(2) -0.006(2) 0.001(2) C46 0.020(2) 0.018(2) 0.017(2) 0.0012(19) 0.0039(18) 0.0031(19) C47 0.019(2) 0.024(3) 0.022(2) 0.003(2) 0.0009(19) 0.006(2) C48 0.030(3) 0.032(3) 0.022(2) 0.001(2) 0.009(2) 0.013(2) C49 0.018(2) 0.018(3) 0.019(2) 0.001(2) 0.0011(19) 0.000(2) C50 0.021(2) 0.014(2) 0.018(2) -0.0057(19) 0.0004(18) 0.0021(19) C51 0.028(3) 0.017(3) 0.018(2) -0.0040(19) -0.0025(19) -0.002(2) C52 0.028(3) 0.024(3) 0.027(3) -0.004(2) -0.012(2) -0.003(2) C53 0.018(2) 0.030(3) 0.037(3) -0.006(2) -0.006(2) -0.006(2) C54 0.025(2) 0.018(3) 0.026(2) -0.003(2) 0.0042(19) -0.005(2) C55 0.020(2) 0.015(2) 0.017(2) -0.0039(18) -0.0016(18) 0.0031(18) C56 0.024(2) 0.016(3) 0.032(3) 0.001(2) -0.005(2) 0.002(2) C57 0.035(3) 0.023(3) 0.022(2) 0.005(2) 0.002(2) 0.000(2) C58 0.022(2) 0.019(3) 0.017(2) -0.001(2) -0.0043(19) 0.005(2) C59 0.027(2) 0.013(2) 0.016(2) 0.0058(19) 0.0015(18) 0.0069(19) C60 0.036(3) 0.022(3) 0.016(2) 0.004(2) 0.002(2) 0.005(2) C61 0.044(3) 0.035(3) 0.021(3) 0.004(2) 0.014(2) 0.009(3) C62 0.026(3) 0.033(3) 0.033(3) 0.004(2) 0.010(2) 0.000(2) C63 0.028(3) 0.020(3) 0.023(2) 0.003(2) 0.003(2) 0.000(2) C64 0.023(2) 0.012(2) 0.018(2) 0.0052(19) 0.0056(18) 0.0073(19) C65 0.028(3) 0.015(3) 0.037(3) 0.001(2) 0.012(2) 0.004(2) C66 0.032(3) 0.018(3) 0.019(2) -0.005(2) 0.004(2) -0.003(2) C67 0.068(4) 0.055(4) 0.015(3) -0.002(3) -0.002(3) 0.015(3) C68 0.074(4) 0.027(3) 0.020(3) -0.007(2) 0.008(3) 0.003(3) C69 0.067(4) 0.029(3) 0.024(3) 0.000(2) 0.011(3) 0.006(3) C70 0.093(5) 0.039(4) 0.019(3) -0.002(3) 0.014(3) -0.019(4) C71 0.155(8) 0.017(3) 0.026(3) 0.006(3) 0.023(4) 0.017(4) C72 0.104(6) 0.055(5) 0.024(3) 0.016(3) 0.010(3) 0.030(4) B1 0.014(2) 0.021(3) 0.017(2) 0.000(2) 0.002(2) 0.007(2) B2 0.014(2) 0.018(3) 0.012(2) 0.004(2) -0.0010(18) 0.005(2) N1 0.0132(17) 0.0118(19) 0.0131(17) 0.0001(15) -0.0013(14) 0.0027(15) N2 0.0124(17) 0.0103(19) 0.0127(17) -0.0001(14) -0.0003(14) 0.0022(14) N3 0.0164(18) 0.0104(19) 0.0116(17) -0.0007(15) -0.0005(14) 0.0037(15) N4 0.0126(17) 0.0105(19) 0.0138(17) -0.0003(15) -0.0037(14) 0.0018(14) N5 0.0200(19) 0.015(2) 0.0180(18) 0.0012(16) -0.0008(15) -0.0031(16) N6 0.0223(19) 0.014(2) 0.0183(18) -0.0005(16) 0.0052(15) 0.0032(16) Y1 0.0125(2) 0.0112(2) 0.0149(2) -0.00019(17) -0.00049(15) 0.00154(17) Y2 0.0133(2) 0.0109(2) 0.0148(2) -0.00060(17) 0.00081(15) 0.00237(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.413(5) . ? C1 C2 1.416(6) . ? C1 C6 1.423(6) . ? C2 C3 1.393(6) . ? C2 C7 1.517(6) . ? C3 C4 1.379(6) . ? C3 H3 0.9500 . ? C4 C5 1.379(6) . ? C4 H4 0.9500 . ? C5 C6 1.395(6) . ? C5 H5 0.9500 . ? C6 C10 1.518(6) . ? C7 C9 1.531(7) . ? C7 C8 1.541(7) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C12 1.531(6) . ? C10 C11 1.534(6) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 N2 1.382(5) . ? C13 C18 1.432(6) . ? C13 C14 1.437(6) . ? C14 C15 1.394(6) . ? C14 C19 1.519(6) . ? C14 Y2 2.963(4) . ? C15 C17 1.393(6) . ? C15 Y2 2.771(4) . ? C15 H15 0.9500 . ? C16 C17 1.393(6) . ? C16 C18 1.396(6) . ? C16 Y2 2.917(4) . ? C16 H16 0.9500 . ? C17 Y2 2.782(4) . ? C17 H17 0.9500 . ? C18 C22 1.522(6) . ? C19 C21 1.523(6) . ? C19 C20 1.531(6) . ? C19 H19 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C24 1.529(6) . ? C22 C23 1.536(6) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 N3 1.416(5) . ? C25 C26 1.416(6) . ? C25 C30 1.425(6) . ? C26 C27 1.384(6) . ? C26 C31 1.518(6) . ? C27 C28 1.377(6) . ? C27 H27 0.9500 . ? C28 C29 1.380(6) . ? C28 H28 0.9500 . ? C29 C30 1.387(6) . ? C29 H29 0.9500 . ? C30 C34 1.521(6) . ? C31 C33 1.527(6) . ? C31 C32 1.531(6) . ? C31 H31 1.0000 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C36 1.529(6) . ? C34 C35 1.533(6) . ? C34 H34 1.0000 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 N4 1.382(5) . ? C37 C38 1.430(6) . ? C37 C42 1.431(6) . ? C38 C39 1.402(6) . ? C38 C43 1.510(6) . ? C39 C40 1.383(6) . ? C39 Y1 2.895(4) . ? C39 H39 0.9500 . ? C40 C41 1.392(6) . ? C40 Y1 2.770(4) . ? C40 H40 0.9500 . ? C41 C42 1.391(6) . ? C41 Y1 2.805(4) . ? C41 H41 0.9500 . ? C42 C46 1.521(6) . ? C42 Y1 2.998(4) . ? C43 C45 1.530(6) . ? C43 C44 1.534(6) . ? C43 H43 1.0000 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 C47 1.526(6) . ? C46 C48 1.528(6) . ? C46 H46 1.0000 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 C50 1.481(6) . ? C49 Y1 2.419(4) . ? C49 H49A 0.97(4) . ? C49 H49B 0.98(4) . ? C50 C51 1.406(6) . ? C50 C55 1.412(6) . ? C51 C52 1.389(6) . ? C51 H51 0.9500 . ? C52 C53 1.381(7) . ? C52 H52 0.9500 . ? C53 C54 1.389(6) . ? C53 H53 0.9500 . ? C54 C55 1.391(6) . ? C54 H54 0.9500 . ? C55 N5 1.457(5) . ? C56 N5 1.486(6) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 N5 1.476(5) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 C59 1.477(6) . ? C58 Y2 2.416(4) . ? C58 H58Q 0.97(5) . ? C58 H58B 0.97(5) . ? C59 C60 1.407(6) . ? C59 C64 1.417(6) . ? C60 C61 1.373(7) . ? C60 H60 0.9500 . ? C61 C62 1.381(7) . ? C61 H61 0.9500 . ? C62 C63 1.390(6) . ? C62 H62 0.9500 . ? C63 C64 1.386(6) . ? C63 H63 0.9500 . ? C64 N6 1.458(5) . ? C65 N6 1.482(5) . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 N6 1.479(5) . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 C72 1.369(9) . ? C67 C68 1.380(8) . ? C67 H67 0.9500 . ? C68 C69 1.363(8) . ? C68 H68 0.9500 . ? C69 C70 1.387(8) . ? C69 H69 0.9500 . ? C70 C71 1.390(9) . ? C70 H70 0.9500 . ? C71 C72 1.373(10) . ? C71 H71 0.9500 . ? C72 H72 0.9500 . ? B1 N1 1.420(6) . ? B1 N2 1.452(6) . ? B1 Y1 2.651(5) . ? B1 H1 1.03(4) . ? B2 N3 1.428(6) . ? B2 N4 1.445(6) . ? B2 Y2 2.643(5) . ? B2 H2 1.08(4) . ? N1 Y1 2.244(3) . ? N2 Y1 2.258(3) . ? N3 Y2 2.243(3) . ? N4 Y2 2.255(3) . ? N5 Y1 2.610(3) . ? N6 Y2 2.602(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 120.5(4) . . ? N1 C1 C6 121.1(4) . . ? C2 C1 C6 118.3(4) . . ? C3 C2 C1 120.0(4) . . ? C3 C2 C7 119.9(4) . . ? C1 C2 C7 119.9(4) . . ? C4 C3 C2 121.4(4) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C5 C4 C3 119.2(4) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? C4 C5 C6 121.9(4) . . ? C4 C5 H5 119.1 . . ? C6 C5 H5 119.1 . . ? C5 C6 C1 119.2(4) . . ? C5 C6 C10 118.7(4) . . ? C1 C6 C10 122.1(4) . . ? C2 C7 C9 114.8(4) . . ? C2 C7 C8 108.3(4) . . ? C9 C7 C8 110.9(4) . . ? C2 C7 H7 107.5 . . ? C9 C7 H7 107.5 . . ? C8 C7 H7 107.5 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C6 C10 C12 114.1(4) . . ? C6 C10 C11 110.7(3) . . ? C12 C10 C11 109.3(4) . . ? C6 C10 H10 107.5 . . ? C12 C10 H10 107.5 . . ? C11 C10 H10 107.5 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N2 C13 C18 119.7(4) . . ? N2 C13 C14 122.7(4) . . ? C18 C13 C14 117.5(4) . . ? C15 C14 C13 119.4(4) . . ? C15 C14 C19 117.9(4) . . ? C13 C14 C19 122.6(4) . . ? C15 C14 Y2 68.4(2) . . ? C13 C14 Y2 84.7(2) . . ? C19 C14 Y2 120.3(3) . . ? C17 C15 C14 122.9(4) . . ? C17 C15 Y2 75.9(2) . . ? C14 C15 Y2 83.7(2) . . ? C17 C15 H15 118.5 . . ? C14 C15 H15 118.5 . . ? Y2 C15 H15 111.7 . . ? C17 C16 C18 122.1(4) . . ? C17 C16 Y2 70.5(2) . . ? C18 C16 Y2 84.0(2) . . ? C17 C16 H16 118.9 . . ? C18 C16 H16 118.9 . . ? Y2 C16 H16 116.8 . . ? C15 C17 C16 117.8(4) . . ? C15 C17 Y2 75.0(2) . . ? C16 C17 Y2 81.3(2) . . ? C15 C17 H17 121.1 . . ? C16 C17 H17 121.1 . . ? Y2 C17 H17 113.4 . . ? C16 C18 C13 120.2(4) . . ? C16 C18 C22 120.0(4) . . ? C13 C18 C22 119.5(4) . . ? C14 C19 C21 112.0(3) . . ? C14 C19 C20 112.2(4) . . ? C21 C19 C20 108.9(3) . . ? C14 C19 H19 107.9 . . ? C21 C19 H19 107.9 . . ? C20 C19 H19 107.9 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C18 C22 C24 114.6(4) . . ? C18 C22 C23 109.5(3) . . ? C24 C22 C23 109.7(3) . . ? C18 C22 H22 107.6 . . ? C24 C22 H22 107.6 . . ? C23 C22 H22 107.6 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N3 C25 C26 120.5(4) . . ? N3 C25 C30 121.3(4) . . ? C26 C25 C30 118.1(4) . . ? C27 C26 C25 120.1(4) . . ? C27 C26 C31 119.6(4) . . ? C25 C26 C31 120.2(4) . . ? C28 C27 C26 121.8(4) . . ? C28 C27 H27 119.1 . . ? C26 C27 H27 119.1 . . ? C27 C28 C29 118.6(4) . . ? C27 C28 H28 120.7 . . ? C29 C28 H28 120.7 . . ? C28 C29 C30 122.4(4) . . ? C28 C29 H29 118.8 . . ? C30 C29 H29 118.8 . . ? C29 C30 C25 119.1(4) . . ? C29 C30 C34 118.5(4) . . ? C25 C30 C34 122.4(4) . . ? C26 C31 C33 109.9(4) . . ? C26 C31 C32 113.4(4) . . ? C33 C31 C32 110.2(4) . . ? C26 C31 H31 107.7 . . ? C33 C31 H31 107.7 . . ? C32 C31 H31 107.7 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C30 C34 C36 112.8(4) . . ? C30 C34 C35 112.0(3) . . ? C36 C34 C35 109.4(3) . . ? C30 C34 H34 107.4 . . ? C36 C34 H34 107.4 . . ? C35 C34 H34 107.4 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N4 C37 C38 119.6(4) . . ? N4 C37 C42 122.6(4) . . ? C38 C37 C42 117.9(4) . . ? C39 C38 C37 119.7(4) . . ? C39 C38 C43 120.2(4) . . ? C37 C38 C43 119.7(4) . . ? C40 C39 C38 121.7(4) . . ? C40 C39 Y1 70.9(2) . . ? C38 C39 Y1 83.6(2) . . ? C40 C39 H39 119.1 . . ? C38 C39 H39 119.1 . . ? Y1 C39 H39 116.9 . . ? C39 C40 C41 118.8(4) . . ? C39 C40 Y1 81.0(2) . . ? C41 C40 Y1 76.9(2) . . ? C39 C40 H40 120.6 . . ? C41 C40 H40 120.6 . . ? Y1 C40 H40 112.1 . . ? C42 C41 C40 121.9(4) . . ? C42 C41 Y1 84.0(2) . . ? C40 C41 Y1 74.1(2) . . ? C42 C41 H41 119.0 . . ? C40 C41 H41 119.0 . . ? Y1 C41 H41 112.9 . . ? C41 C42 C37 119.8(4) . . ? C41 C42 C46 117.7(4) . . ? C37 C42 C46 122.3(4) . . ? C41 C42 Y1 68.5(2) . . ? C37 C42 Y1 83.3(2) . . ? C46 C42 Y1 121.7(3) . . ? C38 C43 C45 115.4(4) . . ? C38 C43 C44 109.0(4) . . ? C45 C43 C44 109.6(4) . . ? C38 C43 H43 107.5 . . ? C45 C43 H43 107.5 . . ? C44 C43 H43 107.5 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C42 C46 C47 112.6(4) . . ? C42 C46 C48 110.5(4) . . ? C47 C46 C48 109.5(3) . . ? C42 C46 H46 108.0 . . ? C47 C46 H46 108.0 . . ? C48 C46 H46 108.0 . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C46 C48 H48A 109.5 . . ? C46 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C46 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C50 C49 Y1 100.3(3) . . ? C50 C49 H49A 114(2) . . ? Y1 C49 H49A 99(2) . . ? C50 C49 H49B 111(2) . . ? Y1 C49 H49B 127(2) . . ? H49A C49 H49B 105(3) . . ? C51 C50 C55 116.4(4) . . ? C51 C50 C49 122.0(4) . . ? C55 C50 C49 121.3(4) . . ? C52 C51 C50 122.0(4) . . ? C52 C51 H51 119.0 . . ? C50 C51 H51 119.0 . . ? C53 C52 C51 120.2(4) . . ? C53 C52 H52 119.9 . . ? C51 C52 H52 119.9 . . ? C52 C53 C54 119.6(4) . . ? C52 C53 H53 120.2 . . ? C54 C53 H53 120.2 . . ? C53 C54 C55 120.2(4) . . ? C53 C54 H54 119.9 . . ? C55 C54 H54 119.9 . . ? C54 C55 C50 121.5(4) . . ? C54 C55 N5 122.0(4) . . ? C50 C55 N5 116.4(4) . . ? N5 C56 H56A 109.5 . . ? N5 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? N5 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? N5 C57 H57A 109.5 . . ? N5 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? N5 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C59 C58 Y2 102.2(3) . . ? C59 C58 H58Q 110(3) . . ? Y2 C58 H58Q 127(3) . . ? C59 C58 H58B 113(3) . . ? Y2 C58 H58B 94(3) . . ? H58Q C58 H58B 109(4) . . ? C60 C59 C64 115.7(4) . . ? C60 C59 C58 122.7(4) . . ? C64 C59 C58 121.3(4) . . ? C61 C60 C59 122.3(4) . . ? C61 C60 H60 118.9 . . ? C59 C60 H60 118.9 . . ? C60 C61 C62 121.1(4) . . ? C60 C61 H61 119.4 . . ? C62 C61 H61 119.4 . . ? C61 C62 C63 118.6(4) . . ? C61 C62 H62 120.7 . . ? C63 C62 H62 120.7 . . ? C64 C63 C62 120.7(4) . . ? C64 C63 H63 119.6 . . ? C62 C63 H63 119.6 . . ? C63 C64 C59 121.6(4) . . ? C63 C64 N6 122.4(4) . . ? C59 C64 N6 116.0(4) . . ? N6 C65 H65A 109.5 . . ? N6 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? N6 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? N6 C66 H66A 109.5 . . ? N6 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? N6 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C72 C67 C68 119.5(7) . . ? C72 C67 H67 120.3 . . ? C68 C67 H67 120.3 . . ? C69 C68 C67 121.0(6) . . ? C69 C68 H68 119.5 . . ? C67 C68 H68 119.5 . . ? C68 C69 C70 119.5(6) . . ? C68 C69 H69 120.2 . . ? C70 C69 H69 120.2 . . ? C69 C70 C71 119.8(6) . . ? C69 C70 H70 120.1 . . ? C71 C70 H70 120.1 . . ? C72 C71 C70 119.5(6) . . ? C72 C71 H71 120.3 . . ? C70 C71 H71 120.3 . . ? C67 C72 C71 120.7(7) . . ? C67 C72 H72 119.6 . . ? C71 C72 H72 119.6 . . ? N1 B1 N2 116.2(4) . . ? N1 B1 Y1 57.8(2) . . ? N2 B1 Y1 58.4(2) . . ? N1 B1 H1 122(2) . . ? N2 B1 H1 121(2) . . ? Y1 B1 H1 173(2) . . ? N3 B2 N4 116.5(4) . . ? N3 B2 Y2 58.1(2) . . ? N4 B2 Y2 58.5(2) . . ? N3 B2 H2 120(2) . . ? N4 B2 H2 123(2) . . ? Y2 B2 H2 174(2) . . ? C1 N1 B1 121.9(3) . . ? C1 N1 Y1 146.8(3) . . ? B1 N1 Y1 89.8(2) . . ? C13 N2 B1 121.5(3) . . ? C13 N2 Y1 150.0(3) . . ? B1 N2 Y1 88.4(3) . . ? C25 N3 B2 120.4(3) . . ? C25 N3 Y2 148.3(3) . . ? B2 N3 Y2 89.2(2) . . ? C37 N4 B2 121.1(3) . . ? C37 N4 Y2 150.4(3) . . ? B2 N4 Y2 88.3(2) . . ? C55 N5 C57 114.6(3) . . ? C55 N5 C56 109.6(3) . . ? C57 N5 C56 107.3(3) . . ? C55 N5 Y1 97.3(2) . . ? C57 N5 Y1 108.0(3) . . ? C56 N5 Y1 120.2(3) . . ? C64 N6 C66 113.7(3) . . ? C64 N6 C65 109.3(3) . . ? C66 N6 C65 107.4(3) . . ? C64 N6 Y2 99.5(2) . . ? C66 N6 Y2 109.0(3) . . ? C65 N6 Y2 118.0(3) . . ? N1 Y1 N2 65.59(12) . . ? N1 Y1 C49 108.03(14) . . ? N2 Y1 C49 108.58(13) . . ? N1 Y1 N5 85.44(11) . . ? N2 Y1 N5 148.82(11) . . ? C49 Y1 N5 68.32(13) . . ? N1 Y1 B1 32.40(14) . . ? N2 Y1 B1 33.20(14) . . ? C49 Y1 B1 111.20(15) . . ? N5 Y1 B1 116.92(13) . . ? N1 Y1 C40 143.65(12) . . ? N2 Y1 C40 131.07(12) . . ? C49 Y1 C40 96.64(14) . . ? N5 Y1 C40 79.26(12) . . ? B1 Y1 C40 151.26(14) . . ? N1 Y1 C41 121.05(12) . . ? N2 Y1 C41 111.91(12) . . ? C49 Y1 C41 125.55(14) . . ? N5 Y1 C41 92.36(12) . . ? B1 Y1 C41 122.71(14) . . ? C40 Y1 C41 28.92(12) . . ? N1 Y1 C39 170.58(12) . . ? N2 Y1 C39 115.84(12) . . ? C49 Y1 C39 80.63(14) . . ? N5 Y1 C39 94.66(12) . . ? B1 Y1 C39 148.38(14) . . ? C40 Y1 C39 28.15(12) . . ? C41 Y1 C39 49.54(13) . . ? N1 Y1 C42 115.31(11) . . ? N2 Y1 C42 84.95(11) . . ? C49 Y1 C42 136.26(14) . . ? N5 Y1 C42 119.52(11) . . ? B1 Y1 C42 102.49(13) . . ? C40 Y1 C42 49.72(12) . . ? C41 Y1 C42 27.48(12) . . ? C39 Y1 C42 56.61(11) . . ? N3 Y2 N4 65.79(12) . . ? N3 Y2 C58 108.42(14) . . ? N4 Y2 C58 109.10(14) . . ? N3 Y2 N6 85.62(11) . . ? N4 Y2 N6 149.36(11) . . ? C58 Y2 N6 68.38(14) . . ? N3 Y2 B2 32.70(14) . . ? N4 Y2 B2 33.13(14) . . ? C58 Y2 B2 111.28(14) . . ? N6 Y2 B2 117.35(13) . . ? N3 Y2 C15 121.55(12) . . ? N4 Y2 C15 112.19(12) . . ? C58 Y2 C15 124.44(14) . . ? N6 Y2 C15 91.61(12) . . ? B2 Y2 C15 123.70(13) . . ? N3 Y2 C17 144.18(12) . . ? N4 Y2 C17 131.20(12) . . ? C58 Y2 C17 95.41(14) . . ? N6 Y2 C17 78.63(12) . . ? B2 Y2 C17 152.30(13) . . ? C15 Y2 C17 29.05(12) . . ? N3 Y2 C16 171.05(12) . . ? N4 Y2 C16 115.43(12) . . ? C58 Y2 C16 79.85(14) . . ? N6 Y2 C16 94.55(11) . . ? B2 Y2 C16 148.09(14) . . ? C15 Y2 C16 49.50(12) . . ? C17 Y2 C16 28.17(12) . . ? N3 Y2 C14 115.38(11) . . ? N4 Y2 C14 84.75(11) . . ? C58 Y2 C14 135.85(14) . . ? N6 Y2 C14 119.11(11) . . ? B2 Y2 C14 102.76(13) . . ? C15 Y2 C14 27.88(12) . . ? C17 Y2 C14 50.31(12) . . ? C16 Y2 C14 56.86(11) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 24.48 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.614 _refine_diff_density_min -0.494 _refine_diff_density_rms 0.079