# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_a00122d _database_code_depnum_ccdc_archive 'CCDC 840581' #TrackingRef 'a00122d (CCDC 840581).cif' _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H74 N4' _chemical_formula_weight 803.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.22(3) _cell_length_b 15.72(3) _cell_length_c 18.26(3) _cell_angle_alpha 84.17(3) _cell_angle_beta 75.17(2) _cell_angle_gamma 77.17(3) _cell_volume 4112(13) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3577 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 24.75 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 0.973 _exptl_crystal_F_000 1314 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.100 _exptl_absorpt_coefficient_mu 0.056 _shelx_estimated_absorpt_T_min 0.978 _shelx_estimated_absorpt_T_max 0.994 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 17247 _diffrn_reflns_av_unetI/netI 0.0664 _diffrn_reflns_av_R_equivalents 0.0264 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.155 _diffrn_reflns_theta_max 25.050 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.973 _diffrn_measured_fraction_theta_full 0.952 _diffrn_reflns_Laue_measured_fraction_max 0.973 _diffrn_reflns_Laue_measured_fraction_full 0.952 _diffrn_reflns_point_group_measured_fraction_max 0.973 _diffrn_reflns_point_group_measured_fraction_full 0.952 _reflns_number_total 14163 _reflns_number_gt 7022 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; In this data, 3 DFIX and 15 ISOR instructions were used to restrain the N-H bonds, isopropyl groups and Ph ring so that there were 93 restraints in the data. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+4.8500P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 14163 _refine_ls_number_parameters 844 _refine_ls_number_restraints 93 _refine_ls_R_factor_all 0.1306 _refine_ls_R_factor_gt 0.0753 _refine_ls_wR_factor_ref 0.1825 _refine_ls_wR_factor_gt 0.1700 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.040 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.0529(2) 0.7119(2) 0.3314(2) 0.0568(9) Uani 1 1 d . . . . . C2 C 1.0448(3) 0.7307(2) 0.4060(2) 0.0608(9) Uani 1 1 d . . . . . C3 C 1.1256(3) 0.7324(3) 0.4272(3) 0.0834(13) Uani 1 1 d . . . . . H3 H 1.1223 0.7446 0.4767 0.100 Uiso 1 1 calc R U . . . C4 C 1.2090(3) 0.7166(3) 0.3771(4) 0.0962(15) Uani 1 1 d . . . . . H4 H 1.2625 0.7180 0.3923 0.115 Uiso 1 1 calc R U . . . C5 C 1.2152(3) 0.6990(3) 0.3058(3) 0.0908(14) Uani 1 1 d . . . . . H5 H 1.2734 0.6892 0.2721 0.109 Uiso 1 1 calc R U . . . C6 C 1.1385(3) 0.6946(2) 0.2799(2) 0.0652(10) Uani 1 1 d . . . . . C7 C 0.9521(3) 0.7529(2) 0.4597(2) 0.0697(10) Uani 1 1 d . . . . . H7 H 0.9109 0.7225 0.4437 0.084 Uiso 1 1 calc R U . . . C8 C 0.9513(3) 0.7224(3) 0.5416(2) 0.1022(15) Uani 1 1 d . . . . . H8A H 0.9768 0.6609 0.5440 0.153 Uiso 1 1 calc R U . . . H8B H 0.8886 0.7337 0.5718 0.153 Uiso 1 1 calc R U . . . H8C H 0.9879 0.7534 0.5605 0.153 Uiso 1 1 calc R U . . . C9 C 0.9125(3) 0.8494(3) 0.4524(3) 0.1017(15) Uani 1 1 d . . . . . H9A H 0.9542 0.8818 0.4627 0.153 Uiso 1 1 calc R U . . . H9B H 0.8534 0.8634 0.4880 0.153 Uiso 1 1 calc R U . . . H9C H 0.9048 0.8645 0.4018 0.153 Uiso 1 1 calc R U . . . C10 C 1.1471(3) 0.6769(3) 0.1992(2) 0.0852(13) Uani 1 1 d . . . . . H10 H 1.0904 0.6586 0.1970 0.102 Uiso 1 1 calc R U . . . C11 C 1.1528(4) 0.7601(4) 0.1493(3) 0.139(2) Uani 1 1 d . . . . . H11A H 1.0970 0.8031 0.1657 0.209 Uiso 1 1 calc R U . . . H11B H 1.1595 0.7477 0.0976 0.209 Uiso 1 1 calc R U . . . H11C H 1.2053 0.7822 0.1533 0.209 Uiso 1 1 calc R U . . . C12 C 1.2281(3) 0.6044(4) 0.1692(3) 0.130(2) Uani 1 1 d . . . . . H12A H 1.2851 0.6235 0.1641 0.195 Uiso 1 1 calc R U . . . H12B H 1.2245 0.5893 0.1205 0.195 Uiso 1 1 calc R U . . . H12C H 1.2262 0.5542 0.2037 0.195 Uiso 1 1 calc R U . . . C13 C 0.9286(3) 0.4942(2) 0.3433(2) 0.0607(10) Uani 1 1 d . . . . . C14 C 0.9704(3) 0.4321(2) 0.2904(2) 0.0728(11) Uani 1 1 d . . . . . C15 C 0.9327(4) 0.3575(3) 0.2956(3) 0.0911(14) Uani 1 1 d . . . . . H15 H 0.9594 0.3150 0.2601 0.109 Uiso 1 1 calc R U . . . C16 C 0.8581(4) 0.3466(3) 0.3514(3) 0.0973(16) Uani 1 1 d . . . . . H16 H 0.8339 0.2967 0.3541 0.117 Uiso 1 1 calc R U . . . C17 C 0.8181(3) 0.4078(3) 0.4038(3) 0.0861(13) Uani 1 1 d . . . . . H17 H 0.7663 0.3995 0.4416 0.103 Uiso 1 1 calc R U . . . C18 C 0.8532(3) 0.4827(2) 0.4019(2) 0.0675(10) Uani 1 1 d . . . . . C19 C 1.0551(3) 0.4419(3) 0.2300(3) 0.0903(13) Uani 1 1 d . . . . . H19 H 1.0593 0.5036 0.2264 0.108 Uiso 1 1 calc R U . . . C20 C 1.0523(4) 0.4185(4) 0.1521(3) 0.141(2) Uani 1 1 d . . . . . H20A H 1.0531 0.3572 0.1525 0.211 Uiso 1 1 calc R U . . . H20B H 1.1054 0.4320 0.1152 0.211 Uiso 1 1 calc R U . . . H20C H 0.9967 0.4515 0.1394 0.211 Uiso 1 1 calc R U . . . C21 C 1.1419(4) 0.3892(4) 0.2524(3) 0.144(2) Uani 1 1 d . . . . . H21A H 1.1363 0.3293 0.2631 0.216 Uiso 1 1 calc R U . . . H21B H 1.1488 0.4125 0.2967 0.216 Uiso 1 1 calc R U . . . H21C H 1.1953 0.3927 0.2115 0.216 Uiso 1 1 calc R U . . . C22 C 0.8120(3) 0.5464(3) 0.4629(3) 0.0849(13) Uani 1 1 d . . . . . H22 H 0.8335 0.6007 0.4440 0.102 Uiso 1 1 calc R U . . . C23 C 0.7067(4) 0.5685(4) 0.4815(4) 0.169(3) Uani 1 1 d . U . . . H23A H 0.6862 0.5822 0.4353 0.253 Uiso 1 1 calc R U . . . H23B H 0.6845 0.6180 0.5129 0.253 Uiso 1 1 calc R U . . . H23C H 0.6828 0.5194 0.5079 0.253 Uiso 1 1 calc R U . . . C24 C 0.8477(5) 0.5145(4) 0.5330(3) 0.143(2) Uani 1 1 d . U . . . H24A H 0.8307 0.4596 0.5516 0.215 Uiso 1 1 calc R U . . . H24B H 0.8210 0.5566 0.5714 0.215 Uiso 1 1 calc R U . . . H24C H 0.9141 0.5072 0.5205 0.215 Uiso 1 1 calc R U . . . C25 C 0.9314(2) 0.6522(2) 0.31213(18) 0.0488(8) Uani 1 1 d . . . . . C26 C 0.8419(2) 0.6682(2) 0.29044(17) 0.0449(7) Uani 1 1 d . . . . . C27 C 0.8258(2) 0.6239(2) 0.23670(19) 0.0566(9) Uani 1 1 d . . . . . H27 H 0.8709 0.5770 0.2152 0.068 Uiso 1 1 calc R U . . . C28 C 0.7443(2) 0.6467(2) 0.2133(2) 0.0600(9) Uani 1 1 d . . . . . H28 H 0.7356 0.6170 0.1750 0.072 Uiso 1 1 calc R U . . . C29 C 0.6755(2) 0.7142(2) 0.24695(18) 0.0483(8) Uani 1 1 d . . . . . C30 C 0.6906(2) 0.7565(2) 0.3018(2) 0.0599(9) Uani 1 1 d . . . . . H30 H 0.6439 0.8008 0.3259 0.072 Uiso 1 1 calc R U . . . C31 C 0.7739(2) 0.7353(2) 0.3229(2) 0.0600(9) Uani 1 1 d . . . . . H31 H 0.7837 0.7668 0.3595 0.072 Uiso 1 1 calc R U . . . C32 C 0.5905(2) 0.7397(2) 0.2184(2) 0.0549(9) Uani 1 1 d . . . . . C33 C 0.5287(3) 0.7695(3) 0.1090(2) 0.0783(12) Uani 1 1 d . . . . . C34 C 0.5179(4) 0.7026(5) 0.0714(3) 0.117(2) Uani 1 1 d . . . . . C35 C 0.4492(5) 0.7176(5) 0.0295(4) 0.150(2) Uani 1 1 d . U . . . H35 H 0.4410 0.6746 0.0019 0.180 Uiso 1 1 calc R U . . . C36 C 0.3960(5) 0.7998(6) 0.0327(4) 0.152(3) Uani 1 1 d . U . . . H36 H 0.3495 0.8099 0.0063 0.182 Uiso 1 1 calc R U . . . C37 C 0.4015(4) 0.8683(5) 0.0687(3) 0.133(2) Uani 1 1 d . . . . . H37 H 0.3613 0.9222 0.0678 0.159 Uiso 1 1 calc R U . . . C38 C 0.4730(3) 0.8521(4) 0.1080(3) 0.0954(15) Uani 1 1 d . . . . . C39 C 0.5784(6) 0.6133(5) 0.0715(4) 0.142(2) Uani 1 1 d . . . . . H39 H 0.6084 0.6092 0.1135 0.170 Uiso 1 1 calc R U . . . C40 C 0.6528(6) 0.6025(5) 0.0013(5) 0.209(4) Uani 1 1 d . U . . . H40A H 0.6260 0.6104 -0.0417 0.314 Uiso 1 1 calc R U . . . H40B H 0.6907 0.5449 0.0021 0.314 Uiso 1 1 calc R U . . . H40C H 0.6904 0.6451 -0.0022 0.314 Uiso 1 1 calc R U . . . C41 C 0.5256(6) 0.5420(6) 0.0852(5) 0.212(4) Uani 1 1 d . U . . . H41A H 0.4824 0.5527 0.0534 0.317 Uiso 1 1 calc R U . . . H41B H 0.4924 0.5399 0.1374 0.317 Uiso 1 1 calc R U . . . H41C H 0.5679 0.4872 0.0735 0.317 Uiso 1 1 calc R U . . . C42 C 0.4880(4) 0.9253(4) 0.1467(3) 0.116(2) Uani 1 1 d . . . . . H42 H 0.5128 0.8991 0.1901 0.139 Uiso 1 1 calc R U . . . C43 C 0.5594(5) 0.9733(5) 0.0967(4) 0.183(3) Uani 1 1 d . U . . . H43A H 0.6148 0.9319 0.0759 0.275 Uiso 1 1 calc R U . . . H43B H 0.5738 1.0130 0.1264 0.275 Uiso 1 1 calc R U . . . H43C H 0.5348 1.0054 0.0563 0.275 Uiso 1 1 calc R U . . . C44 C 0.4032(5) 0.9930(5) 0.1770(5) 0.228(4) Uani 1 1 d . U . . . H44A H 0.3702 1.0125 0.1380 0.342 Uiso 1 1 calc R U . . . H44B H 0.4213 1.0416 0.1927 0.342 Uiso 1 1 calc R U . . . H44C H 0.3637 0.9681 0.2195 0.342 Uiso 1 1 calc R U . . . C45 C 0.4856(2) 0.7227(3) 0.3448(2) 0.0622(10) Uani 1 1 d . . . . . C46 C 0.4537(3) 0.7864(3) 0.3975(2) 0.0695(10) Uani 1 1 d . . . . . C47 C 0.4275(3) 0.7593(3) 0.4723(2) 0.0910(14) Uani 1 1 d . . . . . H47 H 0.4063 0.8011 0.5089 0.109 Uiso 1 1 calc R U . . . C48 C 0.4313(3) 0.6746(4) 0.4948(3) 0.1013(16) Uani 1 1 d . . . . . H48 H 0.4125 0.6590 0.5461 0.122 Uiso 1 1 calc R U . . . C49 C 0.4623(3) 0.6120(3) 0.4433(3) 0.0909(14) Uani 1 1 d . . . . . H49 H 0.4649 0.5536 0.4593 0.109 Uiso 1 1 calc R U . . . C50 C 0.4904(3) 0.6348(3) 0.3660(2) 0.0731(11) Uani 1 1 d . . . . . C51 C 0.4439(3) 0.8822(3) 0.3751(3) 0.0884(13) Uani 1 1 d . . . . . H51 H 0.4805 0.8876 0.3228 0.106 Uiso 1 1 calc R U . . . C52 C 0.4790(4) 0.9333(4) 0.4242(3) 0.135(2) Uani 1 1 d . . . . . H52A H 0.4388 0.9360 0.4742 0.202 Uiso 1 1 calc R U . . . H52B H 0.4794 0.9915 0.4023 0.202 Uiso 1 1 calc R U . . . H52C H 0.5408 0.9047 0.4269 0.202 Uiso 1 1 calc R U . . . C53 C 0.3437(4) 0.9203(3) 0.3757(4) 0.137(2) Uani 1 1 d . . . . . H53A H 0.3269 0.8957 0.3365 0.206 Uiso 1 1 calc R U . . . H53B H 0.3353 0.9825 0.3670 0.206 Uiso 1 1 calc R U . . . H53C H 0.3050 0.9069 0.4241 0.206 Uiso 1 1 calc R U . . . C54 C 0.5210(3) 0.5646(3) 0.3111(3) 0.0971(14) Uani 1 1 d . . . . . H54 H 0.5486 0.5906 0.2619 0.116 Uiso 1 1 calc R U . . . C55 C 0.5916(5) 0.4907(4) 0.3296(4) 0.179(3) Uani 1 1 d . U . . . H55A H 0.6407 0.5125 0.3407 0.269 Uiso 1 1 calc R U . . . H55B H 0.6164 0.4539 0.2872 0.269 Uiso 1 1 calc R U . . . H55C H 0.5637 0.4576 0.3730 0.269 Uiso 1 1 calc R U . . . C56 C 0.4395(5) 0.5290(5) 0.3012(4) 0.186(3) Uani 1 1 d . U . . . H56A H 0.4004 0.5182 0.3501 0.279 Uiso 1 1 calc R U . . . H56B H 0.4625 0.4755 0.2752 0.279 Uiso 1 1 calc R U . . . H56C H 0.4043 0.5710 0.2721 0.279 Uiso 1 1 calc R U . . . C57 C 0.9793(3) 0.2285(2) 0.0816(2) 0.0666(10) Uani 1 1 d . . . . . C58 C 1.0678(3) 0.2198(3) 0.0348(2) 0.0770(11) Uani 1 1 d . . . . . C59 C 1.0836(4) 0.2814(3) -0.0244(3) 0.1104(17) Uani 1 1 d . . . . . H59 H 1.1426 0.2759 -0.0567 0.132 Uiso 1 1 calc R U . . . C60 C 1.0163(5) 0.3492(4) -0.0369(3) 0.129(2) Uani 1 1 d . . . . . H60 H 1.0284 0.3882 -0.0782 0.155 Uiso 1 1 calc R U . . . C61 C 0.9314(4) 0.3601(3) 0.0110(3) 0.1139(18) Uani 1 1 d . . . . . H61 H 0.8862 0.4085 0.0036 0.137 Uiso 1 1 calc R U . . . C62 C 0.9097(3) 0.3008(3) 0.0712(2) 0.0798(12) Uani 1 1 d . . . . . C63 C 1.1469(3) 0.1482(3) 0.0458(3) 0.0881(13) Uani 1 1 d . . . . . H63 H 1.1221 0.1076 0.0861 0.106 Uiso 1 1 calc R U . . . C64 C 1.1900(3) 0.0981(3) -0.0250(3) 0.1209(19) Uani 1 1 d . . . . . H64A H 1.2190 0.1353 -0.0644 0.181 Uiso 1 1 calc R U . . . H64B H 1.1427 0.0784 -0.0409 0.181 Uiso 1 1 calc R U . . . H64C H 1.2358 0.0486 -0.0147 0.181 Uiso 1 1 calc R U . . . C65 C 1.2170(4) 0.1861(4) 0.0727(4) 0.141(2) Uani 1 1 d . . . . . H65A H 1.2354 0.2325 0.0378 0.212 Uiso 1 1 calc R U . . . H65B H 1.2705 0.1411 0.0750 0.212 Uiso 1 1 calc R U . . . H65C H 1.1889 0.2085 0.1221 0.212 Uiso 1 1 calc R U . . . C66 C 0.8156(4) 0.3128(3) 0.1223(3) 0.0971(15) Uani 1 1 d . . . . . H66 H 0.8204 0.2742 0.1674 0.116 Uiso 1 1 calc R U . . . C67 C 0.7810(4) 0.4060(4) 0.1497(4) 0.154(2) Uani 1 1 d . U . . . H67A H 0.8287 0.4234 0.1667 0.232 Uiso 1 1 calc R U . . . H67B H 0.7267 0.4080 0.1907 0.232 Uiso 1 1 calc R U . . . H67C H 0.7659 0.4450 0.1086 0.232 Uiso 1 1 calc R U . . . C68 C 0.7466(4) 0.2872(4) 0.0895(4) 0.158(3) Uani 1 1 d . . . . . H68A H 0.7423 0.3216 0.0436 0.237 Uiso 1 1 calc R U . . . H68B H 0.6872 0.2970 0.1251 0.237 Uiso 1 1 calc R U . . . H68C H 0.7656 0.2265 0.0786 0.237 Uiso 1 1 calc R U . . . C69 C 0.9556(2) 0.0895(2) 0.13761(19) 0.0554(9) Uani 1 1 d . . . . . C70 C 0.9777(2) 0.0443(2) 0.06682(19) 0.0544(9) Uani 1 1 d . . . . . C71 C 1.0369(2) -0.0356(2) 0.0593(2) 0.0599(9) Uani 1 1 d . . . . . H71 H 1.0626 -0.0605 0.0995 0.072 Uiso 1 1 calc R U . . . C72 C 1.0591(2) -0.0795(2) -0.00569(19) 0.0608(9) Uani 1 1 d . . . . . H72 H 1.0994 -0.1337 -0.0091 0.073 Uiso 1 1 calc R U . . . C73 C 0.9098(3) 0.0629(2) 0.2766(2) 0.0614(9) Uani 1 1 d . . . . . C74 C 0.9784(3) 0.0626(2) 0.3132(2) 0.0685(10) Uani 1 1 d . . . . . C75 C 0.9514(4) 0.0827(3) 0.3891(3) 0.0929(14) Uani 1 1 d . . . . . H75 H 0.9964 0.0832 0.4152 0.111 Uiso 1 1 calc R U . . . C76 C 0.8619(5) 0.1012(3) 0.4252(3) 0.1098(18) Uani 1 1 d . . . . . H76 H 0.8450 0.1135 0.4763 0.132 Uiso 1 1 calc R U . . . C77 C 0.7972(4) 0.1020(3) 0.3885(3) 0.1066(17) Uani 1 1 d . . . . . H77 H 0.7351 0.1163 0.4144 0.128 Uiso 1 1 calc R U . . . C78 C 0.8184(3) 0.0825(3) 0.3129(3) 0.0841(12) Uani 1 1 d . . . . . C79 C 1.0781(3) 0.0387(3) 0.2748(3) 0.0828(12) Uani 1 1 d . . . . . H79 H 1.0813 0.0424 0.2203 0.099 Uiso 1 1 calc R U . . . C80 C 1.1191(4) -0.0548(4) 0.2937(4) 0.151(2) Uani 1 1 d . U . . . H80A H 1.1253 -0.0603 0.3451 0.227 Uiso 1 1 calc R U . . . H80B H 1.1791 -0.0720 0.2600 0.227 Uiso 1 1 calc R U . . . H80C H 1.0790 -0.0918 0.2881 0.227 Uiso 1 1 calc R U . . . C81 C 1.1366(4) 0.0987(4) 0.2865(4) 0.157(2) Uani 1 1 d . U . . . H81A H 1.1122 0.1572 0.2700 0.235 Uiso 1 1 calc R U . . . H81B H 1.1992 0.0803 0.2576 0.235 Uiso 1 1 calc R U . . . H81C H 1.1359 0.0973 0.3393 0.235 Uiso 1 1 calc R U . . . C82 C 0.7432(4) 0.0818(5) 0.2721(3) 0.131(2) Uani 1 1 d . . . . . H82 H 0.7716 0.0830 0.2175 0.158 Uiso 1 1 calc R U . . . C83 C 0.7038(5) -0.0005(6) 0.2919(5) 0.209(4) Uani 1 1 d . U . . . H83A H 0.7478 -0.0459 0.3100 0.314 Uiso 1 1 calc R U . . . H83B H 0.6914 -0.0188 0.2476 0.314 Uiso 1 1 calc R U . . . H83C H 0.6471 0.0112 0.3307 0.314 Uiso 1 1 calc R U . . . C84 C 0.6644(5) 0.1620(6) 0.2877(4) 0.203(3) Uani 1 1 d . U . . . H84A H 0.6240 0.1642 0.2546 0.304 Uiso 1 1 calc R U . . . H84B H 0.6898 0.2139 0.2789 0.304 Uiso 1 1 calc R U . . . H84C H 0.6298 0.1585 0.3395 0.304 Uiso 1 1 calc R U . . . N1 N 0.97047(18) 0.71833(17) 0.30611(15) 0.0519(7) Uani 1 1 d . . . . . N2 N 0.96679(19) 0.57102(18) 0.33804(17) 0.0570(7) Uani 1 1 d D . . . . H2N H 1.0190(15) 0.568(2) 0.3463(19) 0.068 Uiso 1 1 d D U . . . N3 N 0.60259(19) 0.7533(2) 0.14520(16) 0.0638(8) Uani 1 1 d . . . . . N4 N 0.5072(2) 0.7490(2) 0.26604(17) 0.0652(8) Uani 1 1 d D . . . . H4N H 0.4588(17) 0.768(2) 0.255(2) 0.078 Uiso 1 1 d D U . . . N5 N 0.9551(2) 0.17041(18) 0.14466(15) 0.0609(8) Uani 1 1 d . . . . . N6 N 0.9351(2) 0.03619(19) 0.20053(17) 0.0600(8) Uani 1 1 d D . . . . H6N H 0.930(2) -0.0137(15) 0.190(2) 0.072 Uiso 1 1 d D U . . . 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 0.057(2) 0.0423(19) 0.079(3) 0.0085(18) -0.032(2) -0.0132(16) C2 0.069(3) 0.049(2) 0.075(3) 0.0039(18) -0.034(2) -0.0188(18) C3 0.099(4) 0.073(3) 0.100(3) 0.011(2) -0.059(3) -0.030(3) C4 0.068(3) 0.098(4) 0.139(5) 0.019(3) -0.055(3) -0.027(3) C5 0.059(3) 0.094(3) 0.118(4) 0.018(3) -0.028(3) -0.016(2) C6 0.052(2) 0.058(2) 0.087(3) 0.005(2) -0.022(2) -0.0109(18) C7 0.084(3) 0.059(2) 0.071(3) -0.0020(19) -0.027(2) -0.013(2) C8 0.127(4) 0.105(4) 0.074(3) 0.008(3) -0.029(3) -0.024(3) C9 0.118(4) 0.073(3) 0.105(4) -0.008(3) -0.029(3) 0.004(3) C10 0.068(3) 0.099(3) 0.081(3) -0.004(3) -0.012(2) -0.009(2) C11 0.173(6) 0.125(5) 0.088(4) 0.020(3) -0.010(4) -0.002(4) C12 0.096(4) 0.123(5) 0.147(5) -0.031(4) -0.005(4) 0.010(3) C13 0.072(3) 0.042(2) 0.078(3) 0.0080(19) -0.041(2) -0.0124(19) C14 0.094(3) 0.048(2) 0.081(3) 0.004(2) -0.037(3) -0.010(2) C15 0.131(4) 0.053(3) 0.105(4) -0.001(2) -0.055(3) -0.021(3) C16 0.131(5) 0.061(3) 0.128(4) 0.024(3) -0.071(4) -0.044(3) C17 0.088(3) 0.068(3) 0.112(4) 0.019(3) -0.040(3) -0.028(3) C18 0.068(3) 0.052(2) 0.089(3) 0.014(2) -0.031(2) -0.018(2) C19 0.117(4) 0.059(3) 0.089(3) -0.014(2) -0.021(3) -0.006(3) C20 0.183(6) 0.139(5) 0.093(4) -0.025(4) -0.034(4) -0.008(4) C21 0.100(4) 0.168(6) 0.147(5) 0.023(4) -0.036(4) 0.002(4) C22 0.077(3) 0.070(3) 0.098(3) 0.012(3) -0.001(3) -0.025(2) C23 0.118(5) 0.164(5) 0.203(6) -0.035(5) 0.015(4) -0.034(4) C24 0.216(6) 0.110(4) 0.101(4) -0.013(3) -0.047(4) -0.013(4) C25 0.050(2) 0.0452(19) 0.050(2) -0.0019(15) -0.0148(16) -0.0046(16) C26 0.0445(19) 0.0425(18) 0.0487(19) -0.0008(15) -0.0143(15) -0.0082(15) C27 0.048(2) 0.059(2) 0.060(2) -0.0113(18) -0.0149(17) 0.0026(17) C28 0.058(2) 0.066(2) 0.060(2) -0.0135(18) -0.0221(18) -0.0067(19) C29 0.046(2) 0.0507(19) 0.0464(19) 0.0005(16) -0.0104(16) -0.0089(16) C30 0.045(2) 0.059(2) 0.074(2) -0.0189(19) -0.0165(18) 0.0036(17) C31 0.057(2) 0.056(2) 0.072(2) -0.0179(19) -0.0229(19) -0.0059(18) C32 0.044(2) 0.058(2) 0.062(2) 0.0030(18) -0.0152(18) -0.0066(16) C33 0.058(3) 0.116(4) 0.063(3) 0.020(3) -0.023(2) -0.021(3) C34 0.109(4) 0.168(6) 0.106(4) 0.033(4) -0.070(3) -0.060(4) C35 0.158(4) 0.173(4) 0.145(4) -0.007(3) -0.065(3) -0.055(4) C36 0.133(4) 0.176(5) 0.159(4) 0.019(4) -0.064(3) -0.039(4) C37 0.095(4) 0.170(6) 0.119(5) 0.062(4) -0.042(4) -0.009(4) C38 0.064(3) 0.136(5) 0.074(3) 0.035(3) -0.016(2) -0.012(3) C39 0.179(7) 0.151(6) 0.138(6) -0.001(5) -0.089(5) -0.066(6) C40 0.202(7) 0.200(7) 0.185(6) 0.009(6) 0.005(6) -0.025(6) C41 0.251(7) 0.207(7) 0.213(7) -0.018(6) -0.078(6) -0.093(6) C42 0.099(4) 0.118(4) 0.084(3) 0.038(3) -0.006(3) 0.037(3) C43 0.189(6) 0.186(6) 0.166(6) 0.003(5) -0.005(5) -0.069(5) C44 0.177(6) 0.204(7) 0.225(7) -0.002(6) -0.005(5) 0.067(5) C45 0.045(2) 0.082(3) 0.057(2) 0.023(2) -0.0132(17) -0.0185(19) C46 0.061(2) 0.083(3) 0.060(3) 0.000(2) -0.007(2) -0.014(2) C47 0.099(3) 0.107(4) 0.057(3) -0.001(3) -0.002(2) -0.020(3) C48 0.109(4) 0.125(5) 0.058(3) 0.019(3) -0.008(3) -0.025(3) C49 0.090(3) 0.097(4) 0.079(3) 0.038(3) -0.019(3) -0.025(3) C50 0.066(3) 0.079(3) 0.067(3) 0.015(2) -0.013(2) -0.012(2) C51 0.090(3) 0.085(3) 0.080(3) 0.000(2) -0.006(3) -0.014(3) C52 0.163(6) 0.121(5) 0.132(5) -0.016(4) -0.033(4) -0.053(4) C53 0.100(4) 0.108(4) 0.193(6) 0.029(4) -0.046(4) -0.002(3) C54 0.105(4) 0.082(3) 0.098(4) 0.023(3) -0.023(3) -0.021(3) C55 0.171(5) 0.148(5) 0.162(5) 0.016(4) -0.022(4) 0.055(4) C56 0.170(6) 0.173(6) 0.231(7) -0.060(5) -0.055(5) -0.037(5) C57 0.087(3) 0.047(2) 0.061(2) -0.0027(18) -0.012(2) -0.010(2) C58 0.091(3) 0.060(2) 0.074(3) 0.004(2) -0.008(2) -0.019(2) C59 0.125(4) 0.091(4) 0.097(4) 0.020(3) -0.001(3) -0.025(3) C60 0.155(6) 0.092(4) 0.112(4) 0.042(3) -0.007(4) -0.016(4) C61 0.143(5) 0.078(3) 0.103(4) 0.020(3) -0.034(4) 0.008(3) C62 0.105(3) 0.060(3) 0.068(3) -0.006(2) -0.018(2) -0.003(2) C63 0.078(3) 0.075(3) 0.104(4) 0.004(3) -0.009(3) -0.020(2) C64 0.100(4) 0.104(4) 0.123(4) -0.012(3) 0.027(3) -0.007(3) C65 0.106(4) 0.129(5) 0.201(7) 0.008(4) -0.056(4) -0.033(4) C66 0.098(4) 0.080(3) 0.094(3) -0.015(3) -0.015(3) 0.019(3) C67 0.155(5) 0.123(4) 0.163(5) -0.055(4) -0.033(4) 0.032(4) C68 0.109(5) 0.186(7) 0.176(6) -0.079(5) -0.011(4) -0.020(4) C69 0.056(2) 0.053(2) 0.052(2) -0.0028(18) -0.0062(17) -0.0073(17) C70 0.061(2) 0.047(2) 0.051(2) -0.0044(16) -0.0089(17) -0.0082(17) C71 0.072(2) 0.049(2) 0.055(2) -0.0009(17) -0.0190(19) -0.0019(18) C72 0.071(2) 0.046(2) 0.057(2) -0.0045(18) -0.0126(19) 0.0028(18) C73 0.076(3) 0.050(2) 0.052(2) -0.0044(17) -0.003(2) -0.0136(19) C74 0.090(3) 0.055(2) 0.061(3) -0.0089(19) -0.013(2) -0.019(2) C75 0.134(5) 0.084(3) 0.070(3) -0.012(2) -0.021(3) -0.040(3) C76 0.154(6) 0.104(4) 0.066(3) -0.027(3) 0.009(4) -0.046(4) C77 0.099(4) 0.110(4) 0.087(4) -0.018(3) 0.026(3) -0.021(3) C78 0.077(3) 0.092(3) 0.071(3) -0.010(2) 0.003(3) -0.013(2) C79 0.089(3) 0.088(3) 0.080(3) -0.012(2) -0.032(3) -0.020(3) C80 0.127(4) 0.103(4) 0.204(6) 0.014(4) -0.025(4) -0.006(3) C81 0.128(4) 0.142(5) 0.207(6) -0.053(4) -0.011(4) -0.059(4) C82 0.075(4) 0.174(6) 0.117(5) -0.005(4) 0.008(3) -0.003(4) C83 0.182(6) 0.223(7) 0.263(8) 0.003(6) -0.094(6) -0.087(6) C84 0.140(5) 0.242(7) 0.197(6) 0.002(6) -0.039(5) 0.016(5) N1 0.0506(17) 0.0471(16) 0.0621(18) 0.0015(13) -0.0211(14) -0.0114(13) N2 0.0522(18) 0.0446(16) 0.079(2) 0.0034(14) -0.0290(16) -0.0067(14) N3 0.0520(18) 0.089(2) 0.0502(18) 0.0068(16) -0.0185(15) -0.0114(16) N4 0.0473(19) 0.085(2) 0.0575(19) 0.0142(16) -0.0169(16) -0.0036(17) N5 0.075(2) 0.0502(18) 0.0523(18) -0.0060(14) -0.0082(15) -0.0089(15) N6 0.073(2) 0.0530(18) 0.0520(19) -0.0074(16) -0.0071(15) -0.0155(16) _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 C6 1.387(5) . ? C1 C2 1.392(5) . ? C1 N1 1.425(4) . ? C2 C3 1.386(5) . ? C2 C7 1.489(5) . ? C3 C4 1.350(6) . ? C3 H3 0.9300 . ? C4 C5 1.334(7) . ? C4 H4 0.9300 . ? C5 C6 1.384(6) . ? C5 H5 0.9300 . ? C6 C10 1.494(6) . ? C7 C9 1.509(6) . ? C7 C8 1.520(6) . ? C7 H7 0.9800 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C12 1.508(6) . ? C10 C11 1.523(6) . ? C10 H10 0.9800 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.377(5) . ? C13 C18 1.385(5) . ? C13 N2 1.437(5) . ? C14 C15 1.401(6) . ? C14 C19 1.493(6) . ? C15 C16 1.347(7) . ? C15 H15 0.9300 . ? C16 C17 1.355(6) . ? C16 H16 0.9300 . ? C17 C18 1.391(6) . ? C17 H17 0.9300 . ? C18 C22 1.491(6) . ? C19 C20 1.517(6) . ? C19 C21 1.523(6) . ? C19 H19 0.9800 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C24 1.514(7) . ? C22 C23 1.516(7) . ? C22 H22 0.9800 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 N1 1.290(4) . ? C25 N2 1.359(4) . ? C25 C26 1.476(5) . ? C26 C27 1.359(5) . ? C26 C31 1.365(5) . ? C27 C28 1.375(5) . ? C27 H27 0.9300 . ? C28 C29 1.381(5) . ? C28 H28 0.9300 . ? C29 C30 1.349(5) . ? C29 C32 1.476(5) . ? C30 C31 1.379(5) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 N3 1.303(5) . ? C32 N4 1.328(5) . ? C33 C34 1.374(7) . ? C33 C38 1.386(7) . ? C33 N3 1.409(5) . ? C34 C35 1.412(7) . ? C34 C39 1.499(8) . ? C35 C36 1.362(9) . ? C35 H35 0.9300 . ? C36 C37 1.346(9) . ? C36 H36 0.9300 . ? C37 C38 1.416(7) . ? C37 H37 0.9300 . ? C38 C42 1.497(7) . ? C39 C40 1.473(9) . ? C39 C41 1.484(9) . ? C39 H39 0.9800 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 C44 1.499(8) . ? C42 C43 1.515(8) . ? C42 H42 0.9800 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 C46 1.382(5) . ? C45 C50 1.386(6) . ? C45 N4 1.429(5) . ? C46 C47 1.373(6) . ? C46 C51 1.504(6) . ? C47 C48 1.346(7) . ? C47 H47 0.9300 . ? C48 C49 1.352(6) . ? C48 H48 0.9300 . ? C49 C50 1.400(6) . ? C49 H49 0.9300 . ? C50 C54 1.482(6) . ? C51 C53 1.507(7) . ? C51 C52 1.521(6) . ? C51 H51 0.9800 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C54 C55 1.474(7) . ? C54 C56 1.526(7) . ? C54 H54 0.9800 . ? C55 H55A 0.9600 . ? C55 H55B 0.9600 . ? C55 H55C 0.9600 . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C57 C58 1.384(6) . ? C57 C62 1.405(5) . ? C57 N5 1.419(5) . ? C58 C59 1.388(6) . ? C58 C63 1.494(6) . ? C59 C60 1.349(7) . ? C59 H59 0.9300 . ? C60 C61 1.348(7) . ? C60 H60 0.9300 . ? C61 C62 1.388(6) . ? C61 H61 0.9300 . ? C62 C66 1.480(6) . ? C63 C64 1.505(6) . ? C63 C65 1.529(6) . ? C63 H63 0.9800 . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 0.9600 . ? C65 H65A 0.9600 . ? C65 H65B 0.9600 . ? C65 H65C 0.9600 . ? C66 C68 1.476(7) . ? C66 C67 1.530(7) . ? C66 H66 0.9800 . ? C67 H67A 0.9600 . ? C67 H67B 0.9600 . ? C67 H67C 0.9600 . ? C68 H68A 0.9600 . ? C68 H68B 0.9600 . ? C68 H68C 0.9600 . ? C69 N5 1.290(5) . ? C69 N6 1.362(4) . ? C69 C70 1.465(5) . ? C70 C71 1.370(5) . ? C70 C72 1.386(5) 2_755 ? C71 C72 1.362(5) . ? C71 H71 0.9300 . ? C72 C70 1.386(5) 2_755 ? C72 H72 0.9300 . ? C73 C78 1.359(6) . ? C73 C74 1.375(5) . ? C73 N6 1.424(5) . ? C74 C75 1.389(6) . ? C74 C79 1.480(6) . ? C75 C76 1.333(7) . ? C75 H75 0.9300 . ? C76 C77 1.324(7) . ? C76 H76 0.9300 . ? C77 C78 1.385(7) . ? C77 H77 0.9300 . ? C78 C82 1.521(7) . ? C79 C81 1.498(6) . ? C79 C80 1.506(7) . ? C79 H79 0.9800 . ? C80 H80A 0.9600 . ? C80 H80B 0.9600 . ? C80 H80C 0.9600 . ? C81 H81A 0.9600 . ? C81 H81B 0.9600 . ? C81 H81C 0.9600 . ? C82 C83 1.516(9) . ? C82 C84 1.529(8) . ? C82 H82 0.9800 . ? C83 H83A 0.9600 . ? C83 H83B 0.9600 . ? C83 H83C 0.9600 . ? C84 H84A 0.9600 . ? C84 H84B 0.9600 . ? C84 H84C 0.9600 . ? N2 H2N 0.836(18) . ? N4 H4N 0.798(18) . ? N6 H6N 0.846(18) . ? 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 C6 C1 C2 121.7(3) . . ? C6 C1 N1 119.4(4) . . ? C2 C1 N1 118.7(3) . . ? C3 C2 C1 117.5(4) . . ? C3 C2 C7 121.4(4) . . ? C1 C2 C7 121.0(3) . . ? C4 C3 C2 121.1(5) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C5 C4 C3 120.3(4) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C4 C5 C6 122.6(5) . . ? C4 C5 H5 118.7 . . ? C6 C5 H5 118.7 . . ? C5 C6 C1 116.7(4) . . ? C5 C6 C10 121.5(4) . . ? C1 C6 C10 121.7(3) . . ? C2 C7 C9 110.0(3) . . ? C2 C7 C8 114.2(4) . . ? C9 C7 C8 111.8(4) . . ? C2 C7 H7 106.8 . . ? C9 C7 H7 106.8 . . ? C8 C7 H7 106.8 . . ? 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 113.0(4) . . ? C6 C10 C11 110.3(4) . . ? C12 C10 C11 110.8(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 . . ? C14 C13 C18 121.5(4) . . ? C14 C13 N2 118.4(4) . . ? C18 C13 N2 120.1(4) . . ? C13 C14 C15 118.1(4) . . ? C13 C14 C19 121.5(4) . . ? C15 C14 C19 120.3(4) . . ? C16 C15 C14 120.8(5) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? C15 C16 C17 120.6(5) . . ? C15 C16 H16 119.7 . . ? C17 C16 H16 119.7 . . ? C16 C17 C18 121.2(5) . . ? C16 C17 H17 119.4 . . ? C18 C17 H17 119.4 . . ? C13 C18 C17 117.8(4) . . ? C13 C18 C22 121.9(4) . . ? C17 C18 C22 120.4(4) . . ? C14 C19 C20 113.7(4) . . ? C14 C19 C21 110.4(4) . . ? C20 C19 C21 110.6(4) . . ? C14 C19 H19 107.2 . . ? C20 C19 H19 107.2 . . ? C21 C19 H19 107.2 . . ? 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 110.7(4) . . ? C18 C22 C23 113.1(4) . . ? C24 C22 C23 111.5(5) . . ? C18 C22 H22 107.1 . . ? C24 C22 H22 107.1 . . ? C23 C22 H22 107.1 . . ? 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 . . ? N1 C25 N2 124.0(3) . . ? N1 C25 C26 116.6(3) . . ? N2 C25 C26 119.3(3) . . ? C27 C26 C31 118.5(3) . . ? C27 C26 C25 123.8(3) . . ? C31 C26 C25 117.6(3) . . ? C26 C27 C28 121.6(3) . . ? C26 C27 H27 119.2 . . ? C28 C27 H27 119.2 . . ? C27 C28 C29 119.5(3) . . ? C27 C28 H28 120.2 . . ? C29 C28 H28 120.2 . . ? C30 C29 C28 118.8(3) . . ? C30 C29 C32 122.8(3) . . ? C28 C29 C32 118.3(3) . . ? C29 C30 C31 121.2(3) . . ? C29 C30 H30 119.4 . . ? C31 C30 H30 119.4 . . ? C26 C31 C30 120.3(3) . . ? C26 C31 H31 119.8 . . ? C30 C31 H31 119.8 . . ? N3 C32 N4 123.1(3) . . ? N3 C32 C29 116.3(3) . . ? N4 C32 C29 120.6(3) . . ? C34 C33 C38 121.7(5) . . ? C34 C33 N3 117.9(4) . . ? C38 C33 N3 120.3(5) . . ? C33 C34 C35 119.9(7) . . ? C33 C34 C39 122.2(5) . . ? C35 C34 C39 118.0(6) . . ? C36 C35 C34 114.9(7) . . ? C36 C35 H35 122.5 . . ? C34 C35 H35 122.5 . . ? C37 C36 C35 128.8(7) . . ? C37 C36 H36 115.6 . . ? C35 C36 H36 115.6 . . ? C36 C37 C38 115.0(7) . . ? C36 C37 H37 122.5 . . ? C38 C37 H37 122.5 . . ? C33 C38 C37 119.6(6) . . ? C33 C38 C42 121.2(4) . . ? C37 C38 C42 119.2(6) . . ? C40 C39 C41 111.9(7) . . ? C40 C39 C34 110.5(6) . . ? C41 C39 C34 113.3(7) . . ? C40 C39 H39 106.9 . . ? C41 C39 H39 106.9 . . ? C34 C39 H39 106.9 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C39 C41 H41A 109.5 . . ? C39 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C39 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C38 C42 C44 115.9(6) . . ? C38 C42 C43 112.8(5) . . ? C44 C42 C43 107.0(6) . . ? C38 C42 H42 106.8 . . ? C44 C42 H42 106.8 . . ? C43 C42 H42 106.8 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C46 C45 C50 121.7(4) . . ? C46 C45 N4 118.6(4) . . ? C50 C45 N4 119.5(4) . . ? C47 C46 C45 117.3(4) . . ? C47 C46 C51 120.4(4) . . ? C45 C46 C51 122.3(4) . . ? C48 C47 C46 122.5(5) . . ? C48 C47 H47 118.7 . . ? C46 C47 H47 118.7 . . ? C47 C48 C49 120.4(5) . . ? C47 C48 H48 119.8 . . ? C49 C48 H48 119.8 . . ? C48 C49 C50 120.3(5) . . ? C48 C49 H49 119.9 . . ? C50 C49 H49 119.9 . . ? C45 C50 C49 117.9(4) . . ? C45 C50 C54 123.4(4) . . ? C49 C50 C54 118.6(4) . . ? C46 C51 C53 108.8(4) . . ? C46 C51 C52 113.9(4) . . ? C53 C51 C52 110.9(5) . . ? C46 C51 H51 107.7 . . ? C53 C51 H51 107.7 . . ? C52 C51 H51 107.7 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C51 C53 H53A 109.5 . . ? C51 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C51 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C55 C54 C50 114.5(5) . . ? C55 C54 C56 108.5(5) . . ? C50 C54 C56 111.8(5) . . ? C55 C54 H54 107.2 . . ? C50 C54 H54 107.2 . . ? C56 C54 H54 107.2 . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C54 C56 H56A 109.5 . . ? C54 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C54 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C58 C57 C62 120.1(4) . . ? C58 C57 N5 123.2(3) . . ? C62 C57 N5 116.5(4) . . ? C57 C58 C59 118.1(4) . . ? C57 C58 C63 123.2(4) . . ? C59 C58 C63 118.8(4) . . ? C60 C59 C58 122.2(5) . . ? C60 C59 H59 118.9 . . ? C58 C59 H59 118.9 . . ? C61 C60 C59 119.6(5) . . ? C61 C60 H60 120.2 . . ? C59 C60 H60 120.2 . . ? C60 C61 C62 121.7(5) . . ? C60 C61 H61 119.2 . . ? C62 C61 H61 119.2 . . ? C61 C62 C57 118.1(4) . . ? C61 C62 C66 121.0(4) . . ? C57 C62 C66 120.9(4) . . ? C58 C63 C64 111.0(4) . . ? C58 C63 C65 109.6(4) . . ? C64 C63 C65 112.8(4) . . ? C58 C63 H63 107.7 . . ? C64 C63 H63 107.7 . . ? C65 C63 H63 107.7 . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C63 C65 H65A 109.5 . . ? C63 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C63 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C68 C66 C62 113.5(4) . . ? C68 C66 C67 110.5(5) . . ? C62 C66 C67 112.0(5) . . ? C68 C66 H66 106.8 . . ? C62 C66 H66 106.8 . . ? C67 C66 H66 106.8 . . ? C66 C67 H67A 109.5 . . ? C66 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C66 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C66 C68 H68A 109.5 . . ? C66 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C66 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? N5 C69 N6 119.9(3) . . ? N5 C69 C70 127.0(3) . . ? N6 C69 C70 113.0(3) . . ? C71 C70 C72 117.7(3) . 2_755 ? C71 C70 C69 119.9(3) . . ? C72 C70 C69 122.4(3) 2_755 . ? C72 C71 C70 121.5(3) . . ? C72 C71 H71 119.2 . . ? C70 C71 H71 119.2 . . ? C71 C72 C70 120.8(3) . 2_755 ? C71 C72 H72 119.6 . . ? C70 C72 H72 119.6 2_755 . ? C78 C73 C74 121.5(4) . . ? C78 C73 N6 119.1(4) . . ? C74 C73 N6 119.2(4) . . ? C73 C74 C75 117.8(4) . . ? C73 C74 C79 121.8(4) . . ? C75 C74 C79 120.3(4) . . ? C76 C75 C74 121.0(5) . . ? C76 C75 H75 119.5 . . ? C74 C75 H75 119.5 . . ? C77 C76 C75 120.1(5) . . ? C77 C76 H76 120.0 . . ? C75 C76 H76 120.0 . . ? C76 C77 C78 122.4(5) . . ? C76 C77 H77 118.8 . . ? C78 C77 H77 118.8 . . ? C73 C78 C77 117.2(5) . . ? C73 C78 C82 121.1(4) . . ? C77 C78 C82 121.7(5) . . ? C74 C79 C81 115.0(4) . . ? C74 C79 C80 111.7(4) . . ? C81 C79 C80 110.9(5) . . ? C74 C79 H79 106.2 . . ? C81 C79 H79 106.2 . . ? C80 C79 H79 106.2 . . ? C79 C80 H80A 109.5 . . ? C79 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C79 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? C79 C81 H81A 109.5 . . ? C79 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C79 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C83 C82 C78 112.1(5) . . ? C83 C82 C84 109.6(6) . . ? C78 C82 C84 112.2(6) . . ? C83 C82 H82 107.6 . . ? C78 C82 H82 107.6 . . ? C84 C82 H82 107.6 . . ? C82 C83 H83A 109.5 . . ? C82 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C82 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? C82 C84 H84A 109.5 . . ? C82 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C82 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? C25 N1 C1 121.2(3) . . ? C25 N2 C13 126.7(3) . . ? C25 N2 H2N 112(2) . . ? C13 N2 H2N 121(2) . . ? C32 N3 C33 122.7(3) . . ? C32 N4 C45 127.6(3) . . ? C32 N4 H4N 126(3) . . ? C45 N4 H4N 106(3) . . ? C69 N5 C57 122.8(3) . . ? C69 N6 C73 125.1(3) . . ? C69 N6 H6N 113(3) . . ? C73 N6 H6N 121(3) . . ? _refine_diff_density_max 0.301 _refine_diff_density_min -0.212 _refine_diff_density_rms 0.042 _shelxl_version_number 2013-2 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.103 0.162 0.819 32 9 ' ' 2 0.125 0.012 0.437 7 0 ' ' 3 0.211 0.971 0.123 13 0 ' ' 4 0.416 0.224 0.290 332 41 ' ' 5 0.584 0.776 0.710 332 41 ' ' 6 0.310 0.842 0.239 10 0 ' ' 7 0.690 0.158 0.761 10 0 ' ' 8 0.789 0.028 0.877 13 0 ' ' 9 0.896 0.838 0.181 32 9 ' ' 10 0.875 0.988 0.562 7 0 ' ' _platon_squeeze_details ; The disordered solvents within the void were not crystallographically well defined. The SQUEEZE routine of the program PLATON was used in order to eliminate the contribution of disordered solvents molecules, thereby a final model based only on the ordered part of the crystal structure was obtained. The SQUEEZE routine suggested that a total potential solvent area volume of 793.7 Ang^3^, and a void electron population of 102 per cell. Because the solvent involved in the recrystallization is toluene, the amount of the disordered solvent was 2 per cell suggested by electron count. The overall formula should be (C56H74N4).0.667(C7H8), considering the contribution of solvent. ; data_a01231c _database_code_depnum_ccdc_archive 'CCDC 840582' #TrackingRef 'a01231c (CCDC 840582).cif' _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C128 H156 Lu2 N12 O6' _chemical_formula_weight 2308.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_H-M_alt 'C 2/c' _space_group_name_Hall '-C 2yc' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.567(8) _cell_length_b 42.621(16) _cell_length_c 15.651(6) _cell_angle_alpha 90 _cell_angle_beta 93.747(5) _cell_angle_gamma 90 _cell_volume 13025(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 916 _cell_measurement_theta_min 2.241 _cell_measurement_theta_max 24.403 _exptl_crystal_description rod _exptl_crystal_colour colorless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.177 _exptl_crystal_F_000 4792 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.050 _exptl_absorpt_coefficient_mu 1.560 _shelx_estimated_absorpt_T_min 0.746 _shelx_estimated_absorpt_T_max 0.926 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 26920 _diffrn_reflns_av_unetI/netI 0.1028 _diffrn_reflns_av_R_equivalents 0.0638 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -50 _diffrn_reflns_limit_k_max 50 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.617 _diffrn_reflns_theta_max 25.000 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measured_fraction_theta_full 0.967 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_Laue_measured_fraction_full 0.967 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_point_group_measured_fraction_full 0.967 _reflns_number_total 11421 _reflns_number_gt 6613 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; In this data, 8 ISOR instructions were used to restrain the isopropyl groups and Ph ring so that there were 48 restraints in the data. C63 belongs to the coordinated THF, so that it has a larger Ueq value, which results in the Alert Level A. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0416P)^2^] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 11421 _refine_ls_number_parameters 607 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.0986 _refine_ls_R_factor_gt 0.0513 _refine_ls_wR_factor_ref 0.1112 _refine_ls_wR_factor_gt 0.1034 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Lu1 Lu 0.73840(2) 0.12104(2) 0.06491(2) 0.04328(10) Uani 1 1 d . . . . . N1 N 0.6349(3) 0.14639(11) 0.0955(3) 0.0438(13) Uani 1 1 d . . . . . N2 N 0.6631(2) 0.09973(11) 0.1548(3) 0.0398(12) Uani 1 1 d . . . . . N3 N 0.8589(3) 0.12328(14) 0.0915(4) 0.0633(16) Uani 1 1 d . . . . . N4 N 0.7655(3) 0.06871(12) 0.0218(4) 0.0537(15) Uani 1 1 d . . . . . N5 N 0.9094(4) 0.17791(18) 0.3801(5) 0.098(2) Uani 1 1 d . . . . . N6 N 0.6617(6) 0.0696(2) -0.2850(5) 0.122(3) Uani 1 1 d . . . . . O1 O 0.7524(3) 0.16495(11) -0.0238(3) 0.0664(14) Uani 1 1 d . . . . . O2 O 0.7122(3) 0.10264(11) -0.0671(3) 0.0638(14) Uani 1 1 d . . . . . O3 O 0.7926(2) 0.15128(11) 0.1701(3) 0.0594(13) Uani 1 1 d . . . . . C1 C 0.8526(4) 0.14259(17) 0.1533(5) 0.0576(19) Uani 1 1 d . . . . . C2 C 0.9130(4) 0.15670(18) 0.2028(5) 0.077(2) Uani 1 1 d . . . . . H2A H 0.9224 0.1445 0.2545 0.092 Uiso 1 1 calc R U . . . H2B H 0.9526 0.1549 0.1689 0.092 Uiso 1 1 calc R U . . . C3 C 0.9054(3) 0.19004(12) 0.2274(5) 0.077(2) Uani 1 1 d G . . . . C4 C 0.9019(3) 0.21171(19) 0.1608(3) 0.097(3) Uani 1 1 d G . . . . H4 H 0.9027 0.2049 0.1045 0.116 Uiso 1 1 calc R U . . . C5 C 0.8973(3) 0.24356(17) 0.1786(5) 0.114(4) Uani 1 1 d G U . . . H5 H 0.8949 0.2581 0.1341 0.137 Uiso 1 1 calc R U . . . C6 C 0.8961(3) 0.25375(11) 0.2628(6) 0.132(4) Uani 1 1 d G . . . . H6 H 0.8930 0.2751 0.2747 0.158 Uiso 1 1 calc R U . . . C7 C 0.8996(3) 0.23209(17) 0.3294(4) 0.121(4) Uani 1 1 d G . . . . H7 H 0.8988 0.2389 0.3857 0.145 Uiso 1 1 calc R U . . . C8 C 0.9042(3) 0.20023(15) 0.3116(4) 0.079(2) Uani 1 1 d G . . . . C9 C 0.9393(6) 0.1884(3) 0.4664(6) 0.145(5) Uani 1 1 d . . . . . H9A H 0.9817 0.1992 0.4598 0.218 Uiso 1 1 calc R U . . . H9B H 0.9475 0.1704 0.5026 0.218 Uiso 1 1 calc R U . . . H9C H 0.9077 0.2022 0.4919 0.218 Uiso 1 1 calc R U . . . C10 C 0.8462(6) 0.1602(2) 0.3893(6) 0.118(4) Uani 1 1 d . . . . . H10A H 0.8277 0.1536 0.3339 0.176 Uiso 1 1 calc R U . . . H10B H 0.8135 0.1732 0.4155 0.176 Uiso 1 1 calc R U . . . H10C H 0.8559 0.1421 0.4246 0.176 Uiso 1 1 calc R U . . . C11 C 0.9215(2) 0.10989(13) 0.0694(4) 0.068(2) Uani 1 1 d G . . . . C12 C 0.9568(3) 0.09006(14) 0.1274(3) 0.096(3) Uani 1 1 d G . . . . H12 H 0.9409 0.0869 0.1814 0.116 Uiso 1 1 calc R U . . . C13 C 1.0159(3) 0.07495(14) 0.1046(5) 0.123(4) Uani 1 1 d G . . . . H13 H 1.0395 0.0617 0.1434 0.147 Uiso 1 1 calc R U . . . C14 C 1.0397(2) 0.07966(16) 0.0238(6) 0.131(5) Uani 1 1 d G . . . . H14 H 1.0792 0.0695 0.0085 0.157 Uiso 1 1 calc R U . . . C15 C 1.0044(4) 0.09949(18) -0.0342(4) 0.136(4) Uani 1 1 d G . . . . H15 H 1.0203 0.1026 -0.0882 0.163 Uiso 1 1 calc R U . . . C16 C 0.9453(3) 0.11460(14) -0.0114(4) 0.100(3) Uani 1 1 d G . . . . H16 H 0.9217 0.1279 -0.0501 0.120 Uiso 1 1 calc R U . . . C17 C 0.7412(4) 0.07572(16) -0.0568(4) 0.0520(18) Uani 1 1 d . . . . . C18 C 0.8004(3) 0.03957(10) 0.0465(3) 0.061(2) Uani 1 1 d G . . . . C19 C 0.7693(3) 0.01961(13) 0.1026(4) 0.090(3) Uani 1 1 d G . . . . H19 H 0.7265 0.0245 0.1212 0.108 Uiso 1 1 calc R U . . . C20 C 0.8024(4) -0.00773(13) 0.1307(4) 0.132(4) Uani 1 1 d G . . . . H20 H 0.7816 -0.0211 0.1682 0.158 Uiso 1 1 calc R U . . . C21 C 0.8664(4) -0.01510(12) 0.1029(4) 0.136(4) Uani 1 1 d G . . . . H21 H 0.8885 -0.0334 0.1217 0.163 Uiso 1 1 calc R U . . . C22 C 0.8975(3) 0.00486(15) 0.0468(4) 0.122(4) Uani 1 1 d G . . . . H22 H 0.9403 -0.0001 0.0282 0.146 Uiso 1 1 calc R U . . . C23 C 0.8644(3) 0.03220(13) 0.0186(3) 0.087(3) Uani 1 1 d G . . . . H23 H 0.8852 0.0456 -0.0189 0.104 Uiso 1 1 calc R U . . . C24 C 0.7443(4) 0.05530(17) -0.1360(5) 0.075(2) Uani 1 1 d . . . . . H24A H 0.7740 0.0375 -0.1226 0.091 Uiso 1 1 calc R U . . . H24B H 0.6989 0.0473 -0.1519 0.091 Uiso 1 1 calc R U . . . C25 C 0.7699(4) 0.07241(13) -0.2095(4) 0.084(3) Uani 1 1 d G . . . . C26 C 0.8387(4) 0.08074(17) -0.2048(4) 0.134(4) Uani 1 1 d G . . . . H26 H 0.8668 0.0754 -0.1567 0.161 Uiso 1 1 calc R U . . . C27 C 0.8656(4) 0.09701(19) -0.2719(6) 0.164(5) Uani 1 1 d G U . . . H27 H 0.9117 0.1026 -0.2687 0.196 Uiso 1 1 calc R U . . . C28 C 0.8237(5) 0.10494(16) -0.3437(4) 0.160(5) Uani 1 1 d G U . . . H28 H 0.8416 0.1158 -0.3886 0.192 Uiso 1 1 calc R U . . . C29 C 0.7548(5) 0.09660(17) -0.3485(4) 0.141(5) Uani 1 1 d G . . . . H29 H 0.7268 0.1019 -0.3966 0.169 Uiso 1 1 calc R U . . . C30 C 0.7280(3) 0.08034(16) -0.2814(5) 0.103(3) Uani 1 1 d G . . . . C31 C 0.6171(6) 0.0881(3) -0.2370(7) 0.157(5) Uani 1 1 d . U . . . H31A H 0.6386 0.0922 -0.1812 0.235 Uiso 1 1 calc R U . . . H31B H 0.5750 0.0770 -0.2313 0.235 Uiso 1 1 calc R U . . . H31C H 0.6077 0.1076 -0.2661 0.235 Uiso 1 1 calc R U . . . C32 C 0.6322(6) 0.0625(3) -0.3713(7) 0.162(5) Uani 1 1 d . U . . . H32A H 0.6642 0.0502 -0.4012 0.243 Uiso 1 1 calc R U . . . H32B H 0.6228 0.0817 -0.4018 0.243 Uiso 1 1 calc R U . . . H32C H 0.5905 0.0509 -0.3674 0.243 Uiso 1 1 calc R U . . . C33 C 0.5972(2) 0.17510(8) 0.0864(3) 0.0482(17) Uani 1 1 d G . . . . C34 C 0.5575(3) 0.18037(11) 0.0109(3) 0.061(2) Uani 1 1 d G . . . . C35 C 0.5250(2) 0.20909(14) -0.0029(3) 0.080(3) Uani 1 1 d G . . . . H35 H 0.4984 0.2126 -0.0535 0.097 Uiso 1 1 calc R U . . . C36 C 0.5322(3) 0.23254(10) 0.0587(4) 0.092(3) Uani 1 1 d G . . . . H36 H 0.5105 0.2518 0.0494 0.110 Uiso 1 1 calc R U . . . C37 C 0.5720(3) 0.22727(9) 0.1342(3) 0.083(3) Uani 1 1 d G . . . . H37 H 0.5768 0.2430 0.1755 0.100 Uiso 1 1 calc R U . . . C38 C 0.6045(2) 0.19855(11) 0.1481(2) 0.0552(19) Uani 1 1 d G . . . . C39 C 0.6498(4) 0.19474(15) 0.2350(4) 0.0594(19) Uani 1 1 d . . . . . H39A H 0.6660 0.1730 0.2384 0.071 Uiso 1 1 calc R U . . . C40 C 0.6089(4) 0.20100(18) 0.3133(4) 0.087(3) Uani 1 1 d . . . . . H40A H 0.5698 0.1873 0.3119 0.130 Uiso 1 1 calc R U . . . H40B H 0.5938 0.2224 0.3127 0.130 Uiso 1 1 calc R U . . . H40C H 0.6373 0.1971 0.3646 0.130 Uiso 1 1 calc R U . . . C41 C 0.7127(4) 0.21610(18) 0.2371(5) 0.082(2) Uani 1 1 d . . . . . H41A H 0.7393 0.2133 0.2904 0.123 Uiso 1 1 calc R U . . . H41B H 0.6983 0.2376 0.2318 0.123 Uiso 1 1 calc R U . . . H41C H 0.7401 0.2108 0.1905 0.123 Uiso 1 1 calc R U . . . C42 C 0.5476(5) 0.1558(2) -0.0556(6) 0.099(3) Uani 1 1 d . . . . . H42A H 0.5712 0.1370 -0.0332 0.119 Uiso 1 1 calc R U . . . C43 C 0.4771(6) 0.1471(3) -0.0759(7) 0.171(5) Uani 1 1 d . U . . . H43A H 0.4750 0.1311 -0.1190 0.257 Uiso 1 1 calc R U . . . H43B H 0.4518 0.1652 -0.0968 0.257 Uiso 1 1 calc R U . . . H43C H 0.4575 0.1394 -0.0253 0.257 Uiso 1 1 calc R U . . . C44 C 0.5805(5) 0.1649(2) -0.1350(7) 0.130(4) Uani 1 1 d . . . . . H44A H 0.6279 0.1696 -0.1214 0.194 Uiso 1 1 calc R U . . . H44B H 0.5579 0.1831 -0.1596 0.194 Uiso 1 1 calc R U . . . H44C H 0.5768 0.1479 -0.1753 0.194 Uiso 1 1 calc R U . . . C45 C 0.6466(3) 0.07124(14) 0.1952(4) 0.0448(16) Uani 1 1 d . . . . . C46 C 0.6841(4) 0.06219(16) 0.2706(4) 0.0568(19) Uani 1 1 d . . . . . C47 C 0.6740(4) 0.03317(19) 0.3043(5) 0.076(2) Uani 1 1 d . . . . . H47A H 0.7008 0.0273 0.3529 0.091 Uiso 1 1 calc R U . . . C48 C 0.6276(5) 0.0127(2) 0.2712(6) 0.095(3) Uani 1 1 d . . . . . H48A H 0.6217 -0.0067 0.2969 0.114 Uiso 1 1 calc R U . . . C49 C 0.5883(4) 0.02116(17) 0.1974(6) 0.083(3) Uani 1 1 d . . . . . H49A H 0.5554 0.0072 0.1747 0.100 Uiso 1 1 calc R U . . . C50 C 0.5966(4) 0.05064(15) 0.1551(5) 0.056(2) Uani 1 1 d . . . . . C51 C 0.5552(4) 0.05826(17) 0.0707(5) 0.062(2) Uani 1 1 d . . . . . H51A H 0.5618 0.0806 0.0585 0.074 Uiso 1 1 calc R U . . . C52 C 0.4788(4) 0.05281(18) 0.0766(5) 0.083(3) Uani 1 1 d . . . . . H52A H 0.4625 0.0655 0.1218 0.125 Uiso 1 1 calc R U . . . H52B H 0.4707 0.0311 0.0885 0.125 Uiso 1 1 calc R U . . . H52C H 0.4549 0.0585 0.0233 0.125 Uiso 1 1 calc R U . . . C53 C 0.5813(4) 0.0395(2) -0.0043(5) 0.099(3) Uani 1 1 d . . . . . H53A H 0.6297 0.0428 -0.0067 0.149 Uiso 1 1 calc R U . . . H53B H 0.5581 0.0465 -0.0569 0.149 Uiso 1 1 calc R U . . . H53C H 0.5725 0.0176 0.0038 0.149 Uiso 1 1 calc R U . . . C54 C 0.7371(4) 0.08362(19) 0.3101(4) 0.065(2) Uani 1 1 d . . . . . H54A H 0.7275 0.1048 0.2883 0.078 Uiso 1 1 calc R U . . . C55 C 0.7332(5) 0.0843(2) 0.4057(5) 0.118(4) Uani 1 1 d . . . . . H55A H 0.6885 0.0911 0.4194 0.178 Uiso 1 1 calc R U . . . H55B H 0.7670 0.0985 0.4303 0.178 Uiso 1 1 calc R U . . . H55C H 0.7418 0.0636 0.4284 0.178 Uiso 1 1 calc R U . . . C56 C 0.8066(4) 0.0740(2) 0.2830(6) 0.101(3) Uani 1 1 d . . . . . H56A H 0.8060 0.0736 0.2217 0.151 Uiso 1 1 calc R U . . . H56B H 0.8177 0.0535 0.3051 0.151 Uiso 1 1 calc R U . . . H56C H 0.8404 0.0888 0.3051 0.151 Uiso 1 1 calc R U . . . C57 C 0.6185(3) 0.12362(15) 0.1498(4) 0.0417(14) Uani 1 1 d . . . . . C58 C 0.5570(3) 0.12486(12) 0.2009(4) 0.0367(14) Uani 1 1 d . . . . . C59 C 0.4913(3) 0.12535(14) 0.1616(4) 0.0444(16) Uani 1 1 d . . . . . H59A H 0.4852 0.1263 0.1022 0.053 Uiso 1 1 calc R U . . . C60 C 0.4350(3) 0.12437(14) 0.2101(4) 0.0477(16) Uani 1 1 d . . . . . H60A H 0.3913 0.1234 0.1831 0.057 Uiso 1 1 calc R U . . . C61 C 0.7510(4) 0.19727(17) 0.0030(5) 0.082(3) Uani 1 1 d . . . . . H61A H 0.7756 0.1999 0.0584 0.098 Uiso 1 1 calc R U . . . H61B H 0.7041 0.2043 0.0071 0.098 Uiso 1 1 calc R U . . . C62 C 0.7846(6) 0.2152(2) -0.0635(6) 0.124(4) Uani 1 1 d . U . . . H62A H 0.7532 0.2307 -0.0892 0.149 Uiso 1 1 calc R U . . . H62B H 0.8246 0.2260 -0.0384 0.149 Uiso 1 1 calc R U . . . C63 C 0.8038(7) 0.1936(3) -0.1263(8) 0.183(5) Uani 1 1 d . U . . . H63A H 0.8533 0.1931 -0.1273 0.219 Uiso 1 1 calc R U . . . H63B H 0.7850 0.2002 -0.1823 0.219 Uiso 1 1 calc R U . . . C64 C 0.7785(5) 0.16286(19) -0.1065(5) 0.097(3) Uani 1 1 d . . . . . H64A H 0.7426 0.1566 -0.1487 0.116 Uiso 1 1 calc R U . . . H64B H 0.8152 0.1475 -0.1063 0.116 Uiso 1 1 calc R U . . . 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 Lu1 0.03418(15) 0.04802(15) 0.04794(16) -0.00369(17) 0.00503(11) -0.00257(18) N1 0.038(3) 0.038(3) 0.057(3) -0.002(3) 0.008(3) -0.001(3) N2 0.037(3) 0.039(3) 0.044(3) 0.004(2) 0.008(3) 0.003(3) N3 0.031(3) 0.085(4) 0.074(4) -0.029(4) 0.005(3) 0.001(3) N4 0.047(4) 0.049(3) 0.066(4) -0.004(3) 0.015(3) 0.001(3) N5 0.080(6) 0.097(6) 0.117(7) -0.028(5) 0.005(5) -0.007(5) N6 0.162(10) 0.117(7) 0.079(6) -0.023(5) -0.048(6) -0.001(7) O1 0.081(4) 0.058(3) 0.063(3) 0.002(3) 0.024(3) -0.010(3) O2 0.084(4) 0.054(3) 0.051(3) -0.008(2) -0.010(3) 0.010(3) O3 0.030(3) 0.079(3) 0.069(3) -0.027(2) 0.004(2) -0.004(2) C1 0.038(4) 0.067(5) 0.067(5) -0.015(4) -0.006(4) -0.008(4) C2 0.038(5) 0.104(6) 0.087(6) -0.039(5) -0.009(4) 0.005(4) C3 0.042(5) 0.104(7) 0.084(6) -0.044(6) -0.004(5) -0.009(5) C4 0.076(7) 0.114(8) 0.100(7) -0.017(6) -0.003(6) -0.026(6) C5 0.112(6) 0.115(6) 0.115(5) -0.011(5) 0.005(5) -0.016(5) C6 0.116(9) 0.079(7) 0.201(13) -0.003(8) 0.023(9) -0.037(7) C7 0.109(9) 0.102(8) 0.153(10) -0.067(8) 0.019(7) -0.039(7) C8 0.049(5) 0.082(6) 0.106(7) -0.015(6) 0.000(5) -0.010(5) C9 0.157(11) 0.185(11) 0.087(7) -0.042(7) -0.039(7) -0.006(9) C10 0.144(11) 0.113(8) 0.095(7) 0.004(6) 0.004(7) -0.015(8) C11 0.039(5) 0.082(6) 0.082(6) -0.024(4) 0.003(4) -0.007(4) C12 0.058(6) 0.117(8) 0.112(7) -0.026(6) -0.011(6) 0.030(6) C13 0.060(7) 0.136(9) 0.168(11) -0.057(8) -0.032(7) 0.031(6) C14 0.047(6) 0.156(11) 0.190(13) -0.074(10) 0.015(8) 0.010(7) C15 0.074(8) 0.177(12) 0.160(11) -0.040(9) 0.034(8) 0.018(8) C16 0.075(7) 0.120(8) 0.108(7) -0.022(6) 0.024(6) 0.007(6) C17 0.058(5) 0.049(4) 0.049(4) -0.003(4) 0.002(4) -0.009(4) C18 0.061(5) 0.049(4) 0.070(5) -0.010(4) -0.002(4) 0.011(4) C19 0.087(7) 0.068(5) 0.120(7) 0.022(5) 0.039(6) 0.019(5) C20 0.135(10) 0.079(7) 0.182(11) 0.036(7) 0.019(9) 0.042(7) C21 0.136(11) 0.097(8) 0.174(11) 0.033(8) 0.012(9) 0.052(8) C22 0.105(9) 0.094(7) 0.167(11) 0.010(7) 0.009(8) 0.055(7) C23 0.074(6) 0.076(6) 0.112(7) -0.002(5) 0.020(6) 0.019(5) C24 0.086(7) 0.071(5) 0.067(5) -0.022(4) -0.009(5) 0.000(5) C25 0.105(8) 0.077(6) 0.070(6) -0.032(5) 0.009(6) -0.004(6) C26 0.133(11) 0.186(12) 0.090(7) -0.002(7) 0.049(7) -0.041(9) C27 0.152(7) 0.179(7) 0.162(7) -0.002(5) 0.021(5) 0.000(5) C28 0.162(7) 0.175(7) 0.143(7) 0.001(5) 0.021(5) -0.005(5) C29 0.194(14) 0.171(11) 0.059(7) 0.006(7) 0.013(8) -0.016(10) C30 0.135(10) 0.099(7) 0.071(7) -0.025(6) -0.030(7) -0.014(7) C31 0.158(9) 0.161(9) 0.149(8) -0.026(7) -0.004(8) 0.016(8) C32 0.184(9) 0.152(8) 0.143(8) -0.012(7) -0.032(8) 0.002(8) C33 0.037(4) 0.044(4) 0.065(5) 0.006(3) 0.012(4) -0.003(3) C34 0.054(5) 0.062(5) 0.066(5) 0.021(4) -0.016(4) -0.008(4) C35 0.072(6) 0.071(6) 0.096(6) 0.029(5) -0.010(5) -0.005(5) C36 0.081(7) 0.074(6) 0.121(8) 0.044(6) 0.008(6) 0.022(5) C37 0.093(7) 0.042(4) 0.119(8) -0.006(5) 0.044(6) 0.006(5) C38 0.043(4) 0.045(4) 0.080(5) 0.005(4) 0.026(4) 0.001(4) C39 0.061(5) 0.045(4) 0.073(5) -0.007(4) 0.011(4) -0.005(4) C40 0.108(7) 0.085(6) 0.070(5) -0.007(4) 0.028(5) -0.004(5) C41 0.070(6) 0.089(6) 0.087(6) -0.018(5) 0.001(5) -0.015(5) C42 0.108(9) 0.082(6) 0.099(7) 0.008(6) -0.054(7) -0.013(6) C43 0.184(10) 0.183(9) 0.140(8) 0.017(7) -0.045(7) -0.078(8) C44 0.113(9) 0.142(10) 0.131(9) -0.057(8) -0.009(8) -0.005(8) C45 0.037(4) 0.040(4) 0.059(4) -0.002(3) 0.014(3) 0.008(3) C46 0.041(4) 0.063(5) 0.066(5) 0.018(4) -0.002(4) 0.004(4) C47 0.056(6) 0.073(6) 0.097(6) 0.025(5) -0.001(5) 0.003(5) C48 0.095(8) 0.067(6) 0.124(8) 0.043(6) 0.012(7) 0.023(6) C49 0.072(6) 0.041(4) 0.141(8) -0.013(5) 0.038(6) -0.020(4) C50 0.050(5) 0.044(4) 0.078(5) -0.012(4) 0.023(4) 0.003(4) C51 0.054(5) 0.062(5) 0.068(5) -0.013(4) -0.006(4) -0.015(4) C52 0.062(6) 0.084(6) 0.103(6) -0.023(5) -0.009(5) -0.012(5) C53 0.089(7) 0.118(7) 0.091(6) -0.034(6) 0.004(6) -0.020(6) C54 0.048(5) 0.086(6) 0.060(5) 0.010(4) -0.004(4) -0.001(4) C55 0.116(9) 0.153(10) 0.083(7) 0.030(6) -0.018(6) -0.037(7) C56 0.050(6) 0.124(8) 0.125(8) 0.002(6) -0.018(5) -0.006(5) C57 0.037(4) 0.045(4) 0.043(3) -0.010(3) 0.002(3) -0.007(3) C58 0.029(3) 0.029(3) 0.053(4) -0.001(3) 0.009(3) 0.001(3) C59 0.035(4) 0.061(4) 0.037(3) 0.004(3) -0.002(3) 0.004(3) C60 0.036(4) 0.060(4) 0.047(4) 0.001(3) -0.001(3) 0.004(4) C61 0.096(7) 0.055(5) 0.097(6) -0.003(4) 0.037(5) -0.016(5) C62 0.137(6) 0.103(5) 0.136(6) 0.010(5) 0.034(5) -0.018(5) C63 0.208(8) 0.164(8) 0.182(8) 0.003(6) 0.067(6) -0.023(6) C64 0.134(9) 0.075(6) 0.087(6) 0.012(5) 0.051(6) -0.017(6) _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 Lu1 O2 2.238(4) . ? Lu1 N2 2.291(5) . ? Lu1 O3 2.295(4) . ? Lu1 O1 2.357(5) . ? Lu1 N3 2.370(5) . ? Lu1 N1 2.371(5) . ? Lu1 N4 2.399(5) . ? Lu1 C1 2.711(7) . ? Lu1 C17 2.716(7) . ? Lu1 C57 2.773(6) . ? N1 C57 1.342(7) . ? N1 C33 1.431(6) . ? N2 C57 1.340(7) . ? N2 C45 1.415(7) . ? N3 C1 1.282(8) . ? N3 C11 1.415(6) . ? N4 C17 1.323(8) . ? N4 C18 1.458(6) . ? N5 C8 1.432(9) . ? N5 C10 1.465(11) . ? N5 C9 1.504(10) . ? N6 C30 1.373(10) . ? N6 C31 1.427(12) . ? N6 C32 1.465(11) . ? O1 C64 1.425(8) . ? O1 C61 1.441(8) . ? O2 C17 1.286(7) . ? O3 C1 1.275(7) . ? C1 C2 1.496(8) . ? C2 C3 1.482(8) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.3900 . ? C3 C8 1.3900 . ? C4 C5 1.3900 . ? C4 H4 0.9300 . ? C5 C6 1.3900 . ? C5 H5 0.9300 . ? C6 C7 1.3900 . ? C6 H6 0.9300 . ? C7 C8 1.3900 . ? C7 H7 0.9300 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.3900 . ? C11 C16 1.3900 . ? C12 C13 1.3900 . ? C12 H12 0.9300 . ? C13 C14 1.3900 . ? C13 H13 0.9300 . ? C14 C15 1.3900 . ? C14 H14 0.9300 . ? C15 C16 1.3900 . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C24 1.520(9) . ? C18 C19 1.3900 . ? C18 C23 1.3900 . ? C19 C20 1.3900 . ? C19 H19 0.9300 . ? C20 C21 1.3900 . ? C20 H20 0.9300 . ? C21 C22 1.3900 . ? C21 H21 0.9300 . ? C22 C23 1.3900 . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C25 1.477(8) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.3900 . ? C25 C30 1.3900 . ? C26 C27 1.3900 . ? C26 H26 0.9300 . ? C27 C28 1.3900 . ? C27 H27 0.9300 . ? C28 C29 1.3900 . ? C28 H28 0.9300 . ? C29 C30 1.3900 . ? C29 H29 0.9300 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 C34 1.3900 . ? C33 C38 1.3900 . ? C34 C35 1.3900 . ? C34 C42 1.480(9) . ? C35 C36 1.3900 . ? C35 H35 0.9300 . ? C36 C37 1.3900 . ? C36 H36 0.9300 . ? C37 C38 1.3900 . ? C37 H37 0.9300 . ? C38 C39 1.584(8) . ? C39 C41 1.529(9) . ? C39 C40 1.532(9) . ? C39 H39A 0.9800 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 C43 1.443(13) . ? C42 C44 1.488(12) . ? C42 H42A 0.9800 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 C46 1.402(8) . ? C45 C50 1.430(9) . ? C46 C47 1.364(9) . ? C46 C54 1.485(9) . ? C47 C48 1.339(11) . ? C47 H47A 0.9300 . ? C48 C49 1.393(11) . ? C48 H48A 0.9300 . ? C49 C50 1.434(9) . ? C49 H49A 0.9300 . ? C50 C51 1.539(9) . ? C51 C52 1.522(9) . ? C51 C53 1.533(9) . ? C51 H51A 0.9800 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C54 C55 1.502(9) . ? C54 C56 1.508(10) . ? C54 H54A 0.9800 . ? C55 H55A 0.9600 . ? C55 H55B 0.9600 . ? C55 H55C 0.9600 . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C57 C58 1.489(7) . ? C58 C59 1.388(7) . ? C58 C60 1.393(7) 2_655 ? C59 C60 1.378(8) . ? C59 H59A 0.9300 . ? C60 C58 1.393(7) 2_655 ? C60 H60A 0.9300 . ? C61 C62 1.479(10) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C62 C63 1.413(13) . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C63 C64 1.443(13) . ? C63 H63A 0.9700 . ? C63 H63B 0.9700 . ? C64 H64A 0.9700 . ? C64 H64B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Lu1 N2 108.09(18) . . ? O2 Lu1 O3 157.85(17) . . ? N2 Lu1 O3 93.88(16) . . ? O2 Lu1 O1 76.28(17) . . ? N2 Lu1 O1 141.35(17) . . ? O3 Lu1 O1 84.86(17) . . ? O2 Lu1 N3 109.97(19) . . ? N2 Lu1 N3 125.51(19) . . ? O3 Lu1 N3 56.19(17) . . ? O1 Lu1 N3 85.32(19) . . ? O2 Lu1 N1 101.48(17) . . ? N2 Lu1 N1 57.63(17) . . ? O3 Lu1 N1 87.70(16) . . ? O1 Lu1 N1 83.74(17) . . ? N3 Lu1 N1 143.06(18) . . ? O2 Lu1 N4 57.05(18) . . ? N2 Lu1 N4 88.11(17) . . ? O3 Lu1 N4 128.58(18) . . ? O1 Lu1 N4 122.42(19) . . ? N3 Lu1 N4 81.45(19) . . ? N1 Lu1 N4 133.43(17) . . ? O2 Lu1 C1 136.2(2) . . ? N2 Lu1 C1 111.3(2) . . ? O3 Lu1 C1 27.97(17) . . ? O1 Lu1 C1 84.70(19) . . ? N3 Lu1 C1 28.23(18) . . ? N1 Lu1 C1 115.4(2) . . ? N4 Lu1 C1 105.6(2) . . ? O2 Lu1 C17 28.02(17) . . ? N2 Lu1 C17 101.09(18) . . ? O3 Lu1 C17 150.79(19) . . ? O1 Lu1 C17 98.23(19) . . ? N3 Lu1 C17 94.9(2) . . ? N1 Lu1 C17 121.51(19) . . ? N4 Lu1 C17 29.15(17) . . ? C1 Lu1 C17 123.0(2) . . ? O2 Lu1 C57 107.82(17) . . ? N2 Lu1 C57 28.73(16) . . ? O3 Lu1 C57 90.00(16) . . ? O1 Lu1 C57 112.66(18) . . ? N3 Lu1 C57 141.07(18) . . ? N1 Lu1 C57 28.92(16) . . ? N4 Lu1 C57 112.39(18) . . ? C1 Lu1 C57 115.94(19) . . ? C17 Lu1 C57 114.89(18) . . ? C57 N1 C33 122.5(5) . . ? C57 N1 Lu1 92.4(4) . . ? C33 N1 Lu1 144.2(3) . . ? C57 N2 C45 120.8(5) . . ? C57 N2 Lu1 96.0(3) . . ? C45 N2 Lu1 142.0(4) . . ? C1 N3 C11 124.8(6) . . ? C1 N3 Lu1 90.9(4) . . ? C11 N3 Lu1 144.0(4) . . ? C17 N4 C18 124.9(5) . . ? C17 N4 Lu1 88.8(4) . . ? C18 N4 Lu1 145.7(4) . . ? C8 N5 C10 113.5(7) . . ? C8 N5 C9 118.6(7) . . ? C10 N5 C9 110.2(8) . . ? C30 N6 C31 113.7(8) . . ? C30 N6 C32 114.9(9) . . ? C31 N6 C32 112.6(10) . . ? C64 O1 C61 109.8(6) . . ? C64 O1 Lu1 123.2(4) . . ? C61 O1 Lu1 125.6(4) . . ? C17 O2 Lu1 97.1(4) . . ? C1 O3 Lu1 94.5(4) . . ? O3 C1 N3 118.5(6) . . ? O3 C1 C2 118.9(6) . . ? N3 C1 C2 122.5(7) . . ? O3 C1 Lu1 57.6(3) . . ? N3 C1 Lu1 60.9(4) . . ? C2 C1 Lu1 175.8(5) . . ? C3 C2 C1 115.5(6) . . ? C3 C2 H2A 108.4 . . ? C1 C2 H2A 108.4 . . ? C3 C2 H2B 108.4 . . ? C1 C2 H2B 108.4 . . ? H2A C2 H2B 107.5 . . ? C4 C3 C8 120.0 . . ? C4 C3 C2 116.3(6) . . ? C8 C3 C2 123.6(6) . . ? C3 C4 C5 120.0 . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C4 C5 C6 120.0 . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C7 C6 C5 120.0 . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C6 C7 C8 120.0 . . ? C6 C7 H7 120.0 . . ? C8 C7 H7 120.0 . . ? C7 C8 C3 120.0 . . ? C7 C8 N5 120.1(6) . . ? C3 C8 N5 119.9(6) . . ? N5 C9 H9A 109.5 . . ? N5 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N5 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N5 C10 H10A 109.5 . . ? N5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C16 120.0 . . ? C12 C11 N3 119.1(5) . . ? C16 C11 N3 120.7(5) . . ? C11 C12 C13 120.0 . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C12 C13 C14 120.0 . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C15 C14 C13 120.0 . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C16 C15 C14 120.0 . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C15 C16 C11 120.0 . . ? C15 C16 H16 120.0 . . ? C11 C16 H16 120.0 . . ? O2 C17 N4 116.5(6) . . ? O2 C17 C24 116.7(6) . . ? N4 C17 C24 126.8(7) . . ? O2 C17 Lu1 54.8(3) . . ? N4 C17 Lu1 62.0(3) . . ? C24 C17 Lu1 169.6(5) . . ? C19 C18 C23 120.0 . . ? C19 C18 N4 118.2(4) . . ? C23 C18 N4 121.7(4) . . ? C20 C19 C18 120.0 . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C21 C20 C19 120.0 . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C22 C21 C20 120.0 . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C21 C22 C23 120.0 . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C22 C23 C18 120.0 . . ? C22 C23 H23 120.0 . . ? C18 C23 H23 120.0 . . ? C25 C24 C17 112.7(6) . . ? C25 C24 H24A 109.0 . . ? C17 C24 H24A 109.0 . . ? C25 C24 H24B 109.0 . . ? C17 C24 H24B 109.0 . . ? H24A C24 H24B 107.8 . . ? C26 C25 C30 120.0 . . ? C26 C25 C24 117.5(6) . . ? C30 C25 C24 122.5(6) . . ? C27 C26 C25 120.0 . . ? C27 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C26 C27 C28 120.0 . . ? C26 C27 H27 120.0 . . ? C28 C27 H27 120.0 . . ? C29 C28 C27 120.0 . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C28 C29 C30 120.0 . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? N6 C30 C29 122.5(7) . . ? N6 C30 C25 117.3(7) . . ? C29 C30 C25 120.0 . . ? N6 C31 H31A 109.5 . . ? N6 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N6 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N6 C32 H32A 109.5 . . ? N6 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N6 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 C38 120.0 . . ? C34 C33 N1 118.6(4) . . ? C38 C33 N1 121.1(4) . . ? C33 C34 C35 120.0 . . ? C33 C34 C42 121.6(5) . . ? C35 C34 C42 118.4(5) . . ? C34 C35 C36 120.0 . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? C37 C36 C35 120.0 . . ? C37 C36 H36 120.0 . . ? C35 C36 H36 120.0 . . ? C36 C37 C38 120.0 . . ? C36 C37 H37 120.0 . . ? C38 C37 H37 120.0 . . ? C37 C38 C33 120.0 . . ? C37 C38 C39 116.7(4) . . ? C33 C38 C39 123.3(4) . . ? C41 C39 C40 110.0(6) . . ? C41 C39 C38 111.2(5) . . ? C40 C39 C38 112.1(6) . . ? C41 C39 H39A 107.8 . . ? C40 C39 H39A 107.8 . . ? C38 C39 H39A 107.8 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C39 C41 H41A 109.5 . . ? C39 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C39 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C43 C42 C34 114.5(10) . . ? C43 C42 C44 110.0(9) . . ? C34 C42 C44 111.0(8) . . ? C43 C42 H42A 107.0 . . ? C34 C42 H42A 107.0 . . ? C44 C42 H42A 107.0 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C46 C45 N2 119.4(6) . . ? C46 C45 C50 120.4(6) . . ? N2 C45 C50 120.0(6) . . ? C47 C46 C45 119.5(7) . . ? C47 C46 C54 120.8(7) . . ? C45 C46 C54 119.6(6) . . ? C48 C47 C46 123.7(8) . . ? C48 C47 H47A 118.2 . . ? C46 C47 H47A 118.2 . . ? C47 C48 C49 118.4(8) . . ? C47 C48 H48A 120.8 . . ? C49 C48 H48A 120.8 . . ? C48 C49 C50 122.5(8) . . ? C48 C49 H49A 118.8 . . ? C50 C49 H49A 118.8 . . ? C45 C50 C49 115.5(7) . . ? C45 C50 C51 123.7(6) . . ? C49 C50 C51 120.8(7) . . ? C52 C51 C53 110.2(6) . . ? C52 C51 C50 112.2(6) . . ? C53 C51 C50 111.4(6) . . ? C52 C51 H51A 107.6 . . ? C53 C51 H51A 107.6 . . ? C50 C51 H51A 107.6 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C51 C53 H53A 109.5 . . ? C51 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C51 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C46 C54 C55 110.3(7) . . ? C46 C54 C56 109.4(7) . . ? C55 C54 C56 113.0(7) . . ? C46 C54 H54A 108.0 . . ? C55 C54 H54A 108.0 . . ? C56 C54 H54A 108.0 . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C54 C56 H56A 109.5 . . ? C54 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C54 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? N2 C57 N1 113.9(5) . . ? N2 C57 C58 122.7(5) . . ? N1 C57 C58 123.4(6) . . ? N2 C57 Lu1 55.3(3) . . ? N1 C57 Lu1 58.7(3) . . ? C58 C57 Lu1 176.1(4) . . ? C59 C58 C60 119.0(5) . 2_655 ? C59 C58 C57 121.3(5) . . ? C60 C58 C57 119.7(5) 2_655 . ? C60 C59 C58 120.3(5) . . ? C60 C59 H59A 119.8 . . ? C58 C59 H59A 119.8 . . ? C59 C60 C58 120.6(5) . 2_655 ? C59 C60 H60A 119.7 . . ? C58 C60 H60A 119.7 2_655 . ? O1 C61 C62 105.7(6) . . ? O1 C61 H61A 110.6 . . ? C62 C61 H61A 110.6 . . ? O1 C61 H61B 110.6 . . ? C62 C61 H61B 110.6 . . ? H61A C61 H61B 108.7 . . ? C63 C62 C61 107.8(9) . . ? C63 C62 H62A 110.1 . . ? C61 C62 H62A 110.1 . . ? C63 C62 H62B 110.1 . . ? C61 C62 H62B 110.1 . . ? H62A C62 H62B 108.5 . . ? C62 C63 C64 109.3(10) . . ? C62 C63 H63A 109.8 . . ? C64 C63 H63A 109.8 . . ? C62 C63 H63B 109.8 . . ? C64 C63 H63B 109.8 . . ? H63A C63 H63B 108.3 . . ? O1 C64 C63 106.6(8) . . ? O1 C64 H64A 110.4 . . ? C63 C64 H64A 110.4 . . ? O1 C64 H64B 110.4 . . ? C63 C64 H64B 110.4 . . ? H64A C64 H64B 108.6 . . ? _refine_diff_density_max 1.205 _refine_diff_density_min -0.700 _refine_diff_density_rms 0.094 _shelxl_version_number 2013-2 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.164 0.250 -0.086 854 164 ' ' 2 0.664 0.750 -0.086 854 164 ' ' 3 0.000 -0.011 0.250 128 15 ' ' 4 0.500 0.489 0.250 128 15 ' ' 5 0.000 0.011 0.750 128 15 ' ' 6 0.500 0.511 0.750 128 15 ' ' _platon_squeeze_details ; The disordered solvents within the void were not crystallographically well defined. The SQUEEZE routine of the program PLATON was used in order to eliminate the contribution of disordered solvents molecules, thereby a final model based only on the ordered part of the crystal structure was obtained. The SQUEEZE routine suggested that a total potential solvent area volume of 2238.8 Ang^3^, and a void electron population of 387 per cell. Because the solvent involved in the recrystallization is toluene, the amount of the disordered solvent was 8 per cell suggested by electron count. The overall formula should be (C128H156Lu2N12O6).2(C7H8), considering the contribution of solvent. ; data_a10122a _database_code_depnum_ccdc_archive 'CCDC 840583' #TrackingRef 'a10122a (CCDC 840583).cif' _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C120 H140 N12 S4 Y2' _chemical_formula_weight 2056.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' _space_group_crystal_system orthorhombic _space_group_IT_number 70 _space_group_name_H-M_alt 'F d d d' _space_group_name_Hall '-F 2uv 2vw' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+3/4, -y+3/4, z' '-x+3/4, y, -z+3/4' 'x, -y+3/4, -z+3/4' 'x, y+1/2, z+1/2' '-x+3/4, -y+5/4, z+1/2' '-x+3/4, y+1/2, -z+5/4' 'x, -y+5/4, -z+5/4' 'x+1/2, y, z+1/2' '-x+5/4, -y+3/4, z+1/2' '-x+5/4, y, -z+5/4' 'x+1/2, -y+3/4, -z+5/4' 'x+1/2, y+1/2, z' '-x+5/4, -y+5/4, z' '-x+5/4, y+1/2, -z+3/4' 'x+1/2, -y+5/4, -z+3/4' '-x, -y, -z' 'x-3/4, y-3/4, -z' 'x-3/4, -y, z-3/4' '-x, y-3/4, z-3/4' '-x, -y+1/2, -z+1/2' 'x-3/4, y-1/4, -z+1/2' 'x-3/4, -y+1/2, z-1/4' '-x, y-1/4, z-1/4' '-x+1/2, -y, -z+1/2' 'x-1/4, y-3/4, -z+1/2' 'x-1/4, -y, z-1/4' '-x+1/2, y-3/4, z-1/4' '-x+1/2, -y+1/2, -z' 'x-1/4, y-1/4, -z' 'x-1/4, -y+1/2, z-3/4' '-x+1/2, y-1/4, z-3/4' _cell_length_a 11.625(3) _cell_length_b 36.414(10) _cell_length_c 63.656(18) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 26947(13) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5579 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 24.18 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.014 _exptl_crystal_F_000 8688 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_min 0.080 _exptl_absorpt_coefficient_mu 0.963 _shelx_estimated_absorpt_T_min 0.831 _shelx_estimated_absorpt_T_max 0.927 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 27109 _diffrn_reflns_av_unetI/netI 0.0689 _diffrn_reflns_av_R_equivalents 0.0614 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -43 _diffrn_reflns_limit_k_max 41 _diffrn_reflns_limit_l_min -75 _diffrn_reflns_limit_l_max 64 _diffrn_reflns_theta_min 1.280 _diffrn_reflns_theta_max 24.998 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measured_fraction_theta_full 0.974 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_Laue_measured_fraction_full 0.974 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_point_group_measured_fraction_full 0.974 _reflns_number_total 5944 _reflns_number_gt 3383 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; In this data, 1 DFIX and 4 ISOR instructions were used to restrain the amino and isopropyl groups so that there were 25 restraints in the data. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+48.0000P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 5944 _refine_ls_number_parameters 319 _refine_ls_number_restraints 25 _refine_ls_R_factor_all 0.0913 _refine_ls_R_factor_gt 0.0542 _refine_ls_wR_factor_ref 0.1342 _refine_ls_wR_factor_gt 0.1259 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 0.6250 0.1250 0.21475(2) 0.04818(18) Uani 1 2 d S T P . . N1 N 0.5544(2) 0.14583(8) 0.18204(4) 0.0456(7) Uani 1 1 d . . . . . N2 N 0.8057(3) 0.10720(9) 0.23013(5) 0.0552(8) Uani 1 1 d . . . . . N3 N 0.8828(6) 0.12289(17) 0.28579(8) 0.1298(18) Uani 1 1 d D . . . . S1 S 0.75628(10) 0.17644(3) 0.23394(2) 0.0760(4) Uani 1 1 d . . . . . C1 C 0.6250 0.1250 0.17057(7) 0.0435(12) Uani 1 2 d S T P . . C2 C 0.6250 0.1250 0.14712(7) 0.0436(12) Uani 1 2 d S T P . . C3 C 0.6243(3) 0.15723(10) 0.13583(5) 0.0509(9) Uani 1 1 d . . . . . H3 H 0.6227 0.1795 0.1430 0.061 Uiso 1 1 calc R U . . . C4 C 0.4570(3) 0.16348(10) 0.17307(5) 0.0478(9) Uani 1 1 d . . . . . C5 C 0.3641(3) 0.14256(11) 0.16591(6) 0.0551(10) Uani 1 1 d . . . . . C6 C 0.2688(4) 0.16092(14) 0.15816(7) 0.0727(12) Uani 1 1 d . . . . . H6 H 0.2065 0.1475 0.1531 0.087 Uiso 1 1 calc R U . . . C7 C 0.2647(4) 0.19855(15) 0.15779(8) 0.0857(15) Uani 1 1 d . . . . . H7 H 0.1997 0.2105 0.1527 0.103 Uiso 1 1 calc R U . . . C8 C 0.3571(4) 0.21844(13) 0.16495(7) 0.0806(14) Uani 1 1 d . . . . . H8 H 0.3544 0.2440 0.1645 0.097 Uiso 1 1 calc R U . . . C9 C 0.4535(4) 0.20142(11) 0.17279(7) 0.0628(11) Uani 1 1 d . . . . . C10 C 0.3608(3) 0.10088(11) 0.16718(7) 0.0648(11) Uani 1 1 d . . . . . H10 H 0.4389 0.0926 0.1706 0.078 Uiso 1 1 calc R U . . . C11 C 0.3273(4) 0.08283(13) 0.14624(7) 0.0879(15) Uani 1 1 d . . . . . H11A H 0.3322 0.0566 0.1476 0.132 Uiso 1 1 calc R U . . . H11B H 0.3787 0.0910 0.1354 0.132 Uiso 1 1 calc R U . . . H11C H 0.2499 0.0896 0.1427 0.132 Uiso 1 1 calc R U . . . C12 C 0.2831(4) 0.08759(12) 0.18466(7) 0.0827(14) Uani 1 1 d . . . . . H12A H 0.3084 0.0978 0.1978 0.124 Uiso 1 1 calc R U . . . H12B H 0.2860 0.0613 0.1854 0.124 Uiso 1 1 calc R U . . . H12C H 0.2056 0.0953 0.1819 0.124 Uiso 1 1 calc R U . . . C13 C 0.5607(6) 0.22361(13) 0.17987(11) 0.120(2) Uani 1 1 d . . . . . H13 H 0.6235 0.2065 0.1830 0.144 Uiso 1 1 calc R U . . . C14 C 0.6010(8) 0.2509(3) 0.16400(15) 0.252(6) Uani 1 1 d . U . . . H14A H 0.5596 0.2735 0.1658 0.378 Uiso 1 1 calc R U . . . H14B H 0.5875 0.2415 0.1501 0.378 Uiso 1 1 calc R U . . . H14C H 0.6818 0.2553 0.1659 0.378 Uiso 1 1 calc R U . . . C15 C 0.5346(7) 0.2439(2) 0.19825(10) 0.190(4) Uani 1 1 d . U . . . H15A H 0.6014 0.2574 0.2026 0.285 Uiso 1 1 calc R U . . . H15B H 0.5116 0.2274 0.2092 0.285 Uiso 1 1 calc R U . . . H15C H 0.4731 0.2608 0.1953 0.285 Uiso 1 1 calc R U . . . C16 C 0.8442(3) 0.13806(12) 0.23702(6) 0.0588(11) Uani 1 1 d . . . . . C17 C 0.9635(4) 0.14280(13) 0.24629(7) 0.0769(13) Uani 1 1 d . . . . . H17A H 0.9912 0.1188 0.2506 0.092 Uiso 1 1 calc R U . . . H17B H 1.0142 0.1515 0.2353 0.092 Uiso 1 1 calc R U . . . C18 C 0.9744(4) 0.16839(13) 0.26463(7) 0.0683(12) Uani 1 1 d . . . . . C19 C 1.0298(4) 0.20179(15) 0.26309(9) 0.0926(15) Uani 1 1 d . . . . . H19 H 1.0591 0.2088 0.2501 0.111 Uiso 1 1 calc R U . . . C20 C 1.0438(5) 0.22511(15) 0.27980(13) 0.109(2) Uani 1 1 d . . . . . H20 H 1.0812 0.2475 0.2782 0.131 Uiso 1 1 calc R U . . . C21 C 1.0018(7) 0.2147(2) 0.29871(12) 0.133(3) Uani 1 1 d . . . . . H21 H 1.0102 0.2300 0.3103 0.159 Uiso 1 1 calc R U . . . C22 C 0.9479(7) 0.1822(2) 0.30086(10) 0.131(2) Uani 1 1 d . . . . . H22 H 0.9197 0.1754 0.3140 0.157 Uiso 1 1 calc R U . . . C23 C 0.9337(5) 0.15869(15) 0.28406(9) 0.0906(15) Uani 1 1 d . . . . . C24 C 0.9586(8) 0.0967(2) 0.29631(16) 0.218(4) Uani 1 1 d . U . . . H24A H 0.9678 0.1037 0.3107 0.327 Uiso 1 1 calc R U . . . H24B H 1.0322 0.0966 0.2895 0.327 Uiso 1 1 calc R U . . . H24C H 0.9254 0.0726 0.2956 0.327 Uiso 1 1 calc R U . . . C25 C 0.7718(8) 0.1238(3) 0.29460(17) 0.252(5) Uani 1 1 d D U . . . H25A H 0.7763 0.1326 0.3088 0.379 Uiso 1 1 calc R U . . . H25B H 0.7396 0.0995 0.2945 0.379 Uiso 1 1 calc R U . . . H25C H 0.7238 0.1399 0.2865 0.379 Uiso 1 1 calc R U . . . C26 C 0.8733(4) 0.07422(10) 0.23106(6) 0.0542(10) Uani 1 1 d . . . . . C27 C 0.8452(4) 0.04793(12) 0.24579(7) 0.0686(12) Uani 1 1 d . . . . . H27 H 0.7866 0.0523 0.2554 0.082 Uiso 1 1 calc R U . . . C28 C 0.9045(4) 0.01516(12) 0.24613(8) 0.0758(13) Uani 1 1 d . . . . . H28 H 0.8856 -0.0026 0.2560 0.091 Uiso 1 1 calc R U . . . C29 C 0.9904(4) 0.00846(13) 0.23214(8) 0.0823(14) Uani 1 1 d . . . . . H29 H 1.0302 -0.0137 0.2326 0.099 Uiso 1 1 calc R U . . . C30 C 1.0183(4) 0.03440(13) 0.21730(7) 0.0783(14) Uani 1 1 d . . . . . H30 H 1.0759 0.0298 0.2075 0.094 Uiso 1 1 calc R U . . . C31 C 0.9599(4) 0.06740(12) 0.21710(6) 0.0672(12) Uani 1 1 d . . . . . H31 H 0.9799 0.0853 0.2073 0.081 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y1 0.0457(3) 0.0541(3) 0.0447(3) 0.000 0.000 0.0064(3) N1 0.0406(18) 0.0509(18) 0.0454(18) 0.0011(15) 0.0010(15) 0.0059(15) N2 0.052(2) 0.055(2) 0.059(2) -0.0025(17) -0.0122(16) 0.0045(17) N3 0.148(5) 0.120(4) 0.121(4) 0.001(3) 0.021(4) -0.028(4) S1 0.0718(8) 0.0608(7) 0.0954(9) -0.0204(6) -0.0211(7) 0.0118(6) C1 0.033(3) 0.050(3) 0.047(3) 0.000 0.000 -0.004(3) C2 0.037(3) 0.056(3) 0.038(3) 0.000 0.000 0.000(3) C3 0.052(2) 0.053(2) 0.0481(19) -0.0057(17) -0.002(2) -0.001(2) C4 0.044(2) 0.057(3) 0.043(2) 0.0009(18) 0.0027(18) 0.010(2) C5 0.043(2) 0.069(3) 0.053(2) -0.0008(19) -0.003(2) 0.007(2) C6 0.052(3) 0.086(4) 0.080(3) 0.003(3) -0.011(2) 0.008(3) C7 0.067(3) 0.097(4) 0.092(4) 0.015(3) -0.003(3) 0.034(3) C8 0.080(4) 0.063(3) 0.099(4) 0.013(3) 0.002(3) 0.016(3) C9 0.059(3) 0.054(3) 0.075(3) 0.003(2) -0.001(2) 0.008(2) C10 0.042(2) 0.071(3) 0.082(3) -0.006(2) -0.006(2) 0.001(2) C11 0.073(3) 0.099(4) 0.092(4) -0.022(3) 0.002(3) -0.011(3) C12 0.094(4) 0.082(3) 0.072(3) 0.004(3) -0.004(3) -0.009(3) C13 0.174(7) 0.042(3) 0.144(6) 0.011(3) -0.036(5) 0.006(4) C14 0.269(10) 0.245(10) 0.242(9) -0.129(8) 0.127(8) -0.154(8) C15 0.195(8) 0.276(9) 0.099(5) -0.028(6) 0.039(5) -0.144(7) C16 0.059(3) 0.065(3) 0.052(2) -0.005(2) -0.007(2) 0.002(2) C17 0.062(3) 0.089(3) 0.080(3) -0.010(3) -0.020(2) 0.000(3) C18 0.062(3) 0.071(3) 0.072(3) -0.006(3) -0.012(2) 0.000(2) C19 0.083(4) 0.091(4) 0.103(4) 0.010(3) -0.005(3) -0.004(3) C20 0.112(5) 0.071(4) 0.145(6) -0.013(4) -0.044(5) -0.009(3) C21 0.179(8) 0.111(6) 0.109(6) -0.035(5) -0.046(5) 0.019(5) C22 0.179(7) 0.121(6) 0.092(5) -0.011(4) 0.011(4) -0.015(5) C23 0.106(4) 0.082(4) 0.084(4) -0.007(3) 0.003(3) -0.011(3) C24 0.224(10) 0.138(7) 0.293(11) 0.077(7) -0.015(8) -0.033(7) C25 0.171(8) 0.255(10) 0.332(12) -0.014(9) 0.101(9) -0.071(8) C26 0.051(2) 0.054(2) 0.057(2) 0.0067(19) -0.009(2) 0.005(2) C27 0.059(3) 0.068(3) 0.078(3) 0.005(2) 0.002(2) 0.007(2) C28 0.074(3) 0.064(3) 0.089(3) 0.023(3) -0.001(3) 0.004(2) C29 0.081(4) 0.065(3) 0.100(4) 0.012(3) -0.009(3) 0.025(3) C30 0.077(3) 0.078(3) 0.080(3) 0.012(3) 0.005(3) 0.027(3) C31 0.063(3) 0.069(3) 0.069(3) 0.020(2) 0.001(2) 0.014(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 Y1 N1 2.363(3) . ? Y1 N1 2.363(3) 14_545 ? Y1 N2 2.406(3) . ? Y1 N2 2.406(3) 14_545 ? Y1 S1 2.7076(12) . ? Y1 S1 2.7078(12) 14_545 ? Y1 C1 2.812(5) . ? Y1 C16 2.955(4) 14_545 ? Y1 C16 2.955(4) . ? N1 C1 1.335(4) . ? N1 C4 1.422(4) . ? N2 C16 1.287(5) . ? N2 C26 1.437(5) . ? N3 C25 1.407(7) . ? N3 C23 1.436(7) . ? N3 C24 1.460(9) . ? S1 C16 1.743(4) . ? C1 N1 1.335(4) 14_545 ? C1 C2 1.493(6) . ? C2 C3 1.376(4) . ? C2 C3 1.376(4) 14_545 ? C3 C3 1.379(7) 11_554 ? C3 H3 0.9300 . ? C4 C9 1.382(5) . ? C4 C5 1.398(5) . ? C5 C6 1.385(5) . ? C5 C10 1.520(5) . ? C6 C7 1.371(6) . ? C6 H6 0.9300 . ? C7 C8 1.373(6) . ? C7 H7 0.9300 . ? C8 C9 1.375(6) . ? C8 H8 0.9300 . ? C9 C13 1.551(7) . ? C10 C12 1.512(5) . ? C10 C11 1.536(6) . ? C10 H10 0.9800 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C15 1.418(8) . ? C13 C14 1.492(9) . ? C13 H13 0.9800 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C17 1.517(6) . ? C17 C18 1.499(6) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C23 1.370(6) . ? C18 C19 1.380(6) . ? C19 C20 1.371(7) . ? C19 H19 0.9300 . ? C20 C21 1.353(8) . ? C20 H20 0.9300 . ? C21 C22 1.345(8) . ? C21 H21 0.9300 . ? C22 C23 1.380(7) . ? C22 H22 0.9300 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C31 1.366(5) . ? C26 C27 1.380(5) . ? C27 C28 1.379(6) . ? C27 H27 0.9300 . ? C28 C29 1.360(6) . ? C28 H28 0.9300 . ? C29 C30 1.375(6) . ? C29 H29 0.9300 . ? C30 C31 1.380(5) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Y1 N1 56.45(14) . 14_545 ? N1 Y1 N2 138.43(10) . . ? N1 Y1 N2 88.22(10) 14_545 . ? N1 Y1 N2 88.21(10) . 14_545 ? N1 Y1 N2 138.43(10) 14_545 14_545 ? N2 Y1 N2 131.99(15) . 14_545 ? N1 Y1 S1 111.80(8) . . ? N1 Y1 S1 115.09(8) 14_545 . ? N2 Y1 S1 60.71(8) . . ? N2 Y1 S1 97.01(8) 14_545 . ? N1 Y1 S1 115.09(8) . 14_545 ? N1 Y1 S1 111.80(8) 14_545 14_545 ? N2 Y1 S1 97.01(8) . 14_545 ? N2 Y1 S1 60.71(8) 14_545 14_545 ? S1 Y1 S1 126.34(6) . 14_545 ? N1 Y1 C1 28.23(7) . . ? N1 Y1 C1 28.22(7) 14_545 . ? N2 Y1 C1 114.01(7) . . ? N2 Y1 C1 114.01(7) 14_545 . ? S1 Y1 C1 116.83(3) . . ? S1 Y1 C1 116.83(3) 14_545 . ? N1 Y1 C16 100.07(10) . 14_545 ? N1 Y1 C16 132.12(11) 14_545 14_545 ? N2 Y1 C16 120.95(10) . 14_545 ? N2 Y1 C16 25.21(10) 14_545 14_545 ? S1 Y1 C16 112.38(8) . 14_545 ? S1 Y1 C16 35.51(8) 14_545 14_545 ? C1 Y1 C16 118.68(8) . 14_545 ? N1 Y1 C16 132.13(11) . . ? N1 Y1 C16 100.07(10) 14_545 . ? N2 Y1 C16 25.21(10) . . ? N2 Y1 C16 120.95(10) 14_545 . ? S1 Y1 C16 35.51(8) . . ? S1 Y1 C16 112.38(8) 14_545 . ? C1 Y1 C16 118.68(8) . . ? C16 Y1 C16 122.65(15) 14_545 . ? C1 N1 C4 121.8(3) . . ? C1 N1 Y1 94.9(2) . . ? C4 N1 Y1 140.9(2) . . ? C16 N2 C26 121.7(3) . . ? C16 N2 Y1 102.0(2) . . ? C26 N2 Y1 136.0(2) . . ? C25 N3 C23 112.8(6) . . ? C25 N3 C24 112.7(7) . . ? C23 N3 C24 112.3(6) . . ? C16 S1 Y1 80.01(15) . . ? N1 C1 N1 113.7(4) 14_545 . ? N1 C1 C2 123.2(2) 14_545 . ? N1 C1 C2 123.2(2) . . ? N1 C1 Y1 56.8(2) 14_545 . ? N1 C1 Y1 56.8(2) . . ? C2 C1 Y1 180.0 . . ? C3 C2 C3 117.0(4) . 14_545 ? C3 C2 C1 121.5(2) . . ? C3 C2 C1 121.5(2) 14_545 . ? C2 C3 C3 121.5(2) . 11_554 ? C2 C3 H3 119.3 . . ? C3 C3 H3 119.3 11_554 . ? C9 C4 C5 121.2(4) . . ? C9 C4 N1 118.7(3) . . ? C5 C4 N1 120.0(3) . . ? C6 C5 C4 118.1(4) . . ? C6 C5 C10 118.7(4) . . ? C4 C5 C10 123.1(4) . . ? C7 C6 C5 121.1(4) . . ? C7 C6 H6 119.5 . . ? C5 C6 H6 119.5 . . ? C6 C7 C8 119.6(4) . . ? C6 C7 H7 120.2 . . ? C8 C7 H7 120.2 . . ? C7 C8 C9 121.4(4) . . ? C7 C8 H8 119.3 . . ? C9 C8 H8 119.3 . . ? C8 C9 C4 118.6(4) . . ? C8 C9 C13 121.7(4) . . ? C4 C9 C13 119.6(4) . . ? C12 C10 C5 112.0(3) . . ? C12 C10 C11 110.5(4) . . ? C5 C10 C11 112.8(4) . . ? C12 C10 H10 107.1 . . ? C5 C10 H10 107.1 . . ? C11 C10 H10 107.1 . . ? 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 . . ? C15 C13 C14 106.1(5) . . ? C15 C13 C9 109.9(6) . . ? C14 C13 C9 113.7(6) . . ? C15 C13 H13 109.0 . . ? C14 C13 H13 109.0 . . ? C9 C13 H13 109.0 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N2 C16 C17 123.4(4) . . ? N2 C16 S1 117.2(3) . . ? C17 C16 S1 119.3(3) . . ? N2 C16 Y1 52.8(2) . . ? C17 C16 Y1 173.4(3) . . ? S1 C16 Y1 64.47(13) . . ? C18 C17 C16 116.8(4) . . ? C18 C17 H17A 108.1 . . ? C16 C17 H17A 108.1 . . ? C18 C17 H17B 108.1 . . ? C16 C17 H17B 108.1 . . ? H17A C17 H17B 107.3 . . ? C23 C18 C19 116.9(5) . . ? C23 C18 C17 120.9(5) . . ? C19 C18 C17 122.1(5) . . ? C20 C19 C18 123.1(5) . . ? C20 C19 H19 118.5 . . ? C18 C19 H19 118.5 . . ? C21 C20 C19 118.3(6) . . ? C21 C20 H20 120.9 . . ? C19 C20 H20 120.9 . . ? C22 C21 C20 120.4(6) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C21 C22 C23 121.5(6) . . ? C21 C22 H22 119.3 . . ? C23 C22 H22 119.3 . . ? C18 C23 C22 119.9(5) . . ? C18 C23 N3 116.4(5) . . ? C22 C23 N3 123.6(6) . . ? N3 C24 H24A 109.5 . . ? N3 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N3 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N3 C25 H25A 109.5 . . ? N3 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N3 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C31 C26 C27 119.4(4) . . ? C31 C26 N2 121.9(3) . . ? C27 C26 N2 118.6(4) . . ? C28 C27 C26 119.5(4) . . ? C28 C27 H27 120.3 . . ? C26 C27 H27 120.3 . . ? C29 C28 C27 120.8(4) . . ? C29 C28 H28 119.6 . . ? C27 C28 H28 119.6 . . ? C28 C29 C30 120.0(4) . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C29 C30 C31 119.2(4) . . ? C29 C30 H30 120.4 . . ? C31 C30 H30 120.4 . . ? C26 C31 C30 121.0(4) . . ? C26 C31 H31 119.5 . . ? C30 C31 H31 119.5 . . ? _refine_diff_density_max 0.618 _refine_diff_density_min -0.368 _refine_diff_density_rms 0.054 _shelxl_version_number 2013-2 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.044 -0.125 0.125 821 202 ' ' 2 0.287 0.125 0.375 821 202 ' ' 3 0.544 -0.125 0.625 821 202 ' ' 4 0.787 0.125 0.875 821 202 ' ' 5 0.440 0.375 0.125 821 202 ' ' 6 0.940 0.375 0.625 821 202 ' ' 7 0.557 0.625 0.375 821 202 ' ' 8 0.057 0.625 0.875 821 202 ' ' _platon_squeeze_details ; The disordered solvents within the void were not crystallographically well defined. The SQUEEZE routine of the program PLATON was used in order to eliminate the contribution of disordered solvents molecules, thereby a final model based only on the ordered part of the crystal structure was obtained. The SQUEEZE routine suggested that a total potential solvent area volume of 6580.0 Ang^3^, and a void electron population of 1619 per cell. Because the solvent we used in the recrystalization of this complex is toluene, the amount of the disordered solvent was 32 per cell suggested by electron count. The overall formula should be (C120H140N12S4Y2).4(C7H8), considering the contribution of solvent. ;