# 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_complex1 #TrackingRef '16823_web_deposit_cif_file_0_TamalKumarSen_1357974721.complex 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C47 H67 N3 Si2 Zn' _chemical_formula_sum 'C47 H67 N3 Si2 Zn' _chemical_formula_weight 795.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.6449(13) _cell_length_b 22.610(2) _cell_length_c 15.8432(15) _cell_angle_alpha 90.00 _cell_angle_beta 96.468(2) _cell_angle_gamma 90.00 _cell_volume 4500.7(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8320 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 28.13 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.174 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1712 _exptl_absorpt_coefficient_mu 0.632 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.892 _exptl_absorpt_correction_T_max 0.939 _exptl_absorpt_process_details 'SADABS; BRUKER; 2008' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41248 _diffrn_reflns_av_R_equivalents 0.0566 _diffrn_reflns_av_sigmaI/netI 0.0518 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 27.00 _reflns_number_total 9831 _reflns_number_gt 7438 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0368P)^2^+2.3664P] 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 9831 _refine_ls_number_parameters 493 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0601 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.0917 _refine_ls_wR_factor_gt 0.0818 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.482606(17) 0.032820(10) 0.244987(14) 0.01449(7) Uani 1 1 d . . . Si1 Si 0.72192(4) 0.06180(3) 0.32607(4) 0.01633(13) Uani 1 1 d . . . Si2 Si 0.67556(4) -0.04079(3) 0.20844(4) 0.01759(13) Uani 1 1 d . . . N1 N 0.63870(12) 0.02214(7) 0.25580(10) 0.0157(4) Uani 1 1 d . . . N2 N 0.32278(11) 0.13362(7) 0.20789(10) 0.0110(3) Uani 1 1 d . . . C1I C 0.33236(15) 0.13415(9) 0.39186(12) 0.0165(4) Uani 1 1 d . . . H1I H 0.3869 0.1473 0.3567 0.020 Uiso 1 1 calc R . . N4 N 0.39557(12) 0.20634(7) 0.14745(10) 0.0111(3) Uani 1 1 d . . . C1 C 0.38702(16) -0.03558(10) 0.26440(14) 0.0236(5) Uani 1 1 d . . . H1A H 0.3140 -0.0233 0.2484 0.028 Uiso 1 1 calc R . . H1B H 0.4022 -0.0674 0.2265 0.028 Uiso 1 1 calc R . . C2 C 0.3953(2) -0.06019(11) 0.35458(16) 0.0360(6) Uani 1 1 d . . . H2A H 0.4685 -0.0686 0.3739 0.054 Uiso 1 1 calc R . . H2B H 0.3543 -0.0959 0.3550 0.054 Uiso 1 1 calc R . . H2C H 0.3685 -0.0316 0.3915 0.054 Uiso 1 1 calc R . . C3 C 0.79386(19) 0.01439(11) 0.41147(15) 0.0320(6) Uani 1 1 d . . . H3A H 0.7432 -0.0033 0.4446 0.048 Uiso 1 1 calc R . . H3B H 0.8427 0.0383 0.4475 0.048 Uiso 1 1 calc R . . H3C H 0.8324 -0.0161 0.3859 0.048 Uiso 1 1 calc R . . C4 C 0.82805(16) 0.10400(10) 0.27838(14) 0.0205(5) Uani 1 1 d . . . H4A H 0.8625 0.0784 0.2415 0.031 Uiso 1 1 calc R . . H4B H 0.8795 0.1183 0.3228 0.031 Uiso 1 1 calc R . . H4C H 0.7965 0.1368 0.2463 0.031 Uiso 1 1 calc R . . C5 C 0.64780(17) 0.11813(11) 0.38306(16) 0.0319(6) Uani 1 1 d . . . H5A H 0.6124 0.1452 0.3426 0.048 Uiso 1 1 calc R . . H5B H 0.6969 0.1395 0.4225 0.048 Uiso 1 1 calc R . . H5C H 0.5961 0.0986 0.4132 0.048 Uiso 1 1 calc R . . C6 C 0.6634(2) -0.10898(10) 0.27449(15) 0.0297(5) Uani 1 1 d . . . H6A H 0.6961 -0.1020 0.3313 0.045 Uiso 1 1 calc R . . H6B H 0.6985 -0.1414 0.2502 0.045 Uiso 1 1 calc R . . H6C H 0.5896 -0.1184 0.2758 0.045 Uiso 1 1 calc R . . C7 C 0.81798(17) -0.03986(11) 0.18405(15) 0.0287(5) Uani 1 1 d . . . H7A H 0.8297 -0.0056 0.1506 0.043 Uiso 1 1 calc R . . H7B H 0.8321 -0.0749 0.1530 0.043 Uiso 1 1 calc R . . H7C H 0.8647 -0.0386 0.2362 0.043 Uiso 1 1 calc R . . C8 C 0.59397(18) -0.05325(11) 0.10346(14) 0.0264(5) Uani 1 1 d . . . H8A H 0.5198 -0.0533 0.1113 0.040 Uiso 1 1 calc R . . H8B H 0.6126 -0.0907 0.0805 0.040 Uiso 1 1 calc R . . H8C H 0.6078 -0.0222 0.0649 0.040 Uiso 1 1 calc R . . C9 C 0.42878(14) 0.11515(9) 0.20410(12) 0.0123(4) Uani 1 1 d . . . C10 C 0.24425(14) 0.09932(9) 0.24633(12) 0.0121(4) Uani 1 1 d . . . C11 C 0.16755(14) 0.06850(9) 0.19352(12) 0.0151(4) Uani 1 1 d . . . C12 C 0.09195(15) 0.03724(9) 0.23272(13) 0.0183(4) Uani 1 1 d . . . H12 H 0.0398 0.0159 0.1996 0.022 Uiso 1 1 calc R . . C13 C 0.09281(15) 0.03728(10) 0.32009(14) 0.0211(5) Uani 1 1 d . . . H13 H 0.0411 0.0164 0.3450 0.025 Uiso 1 1 calc R . . C14 C 0.17012(15) 0.06826(10) 0.37054(13) 0.0191(4) Uani 1 1 d . . . H14 H 0.1697 0.0680 0.4292 0.023 Uiso 1 1 calc R . . C15 C 0.24852(14) 0.09979(9) 0.33502(12) 0.0150(4) Uani 1 1 d . . . C16 C 0.38644(17) 0.09578(10) 0.46267(14) 0.0255(5) Uani 1 1 d . . . H16A H 0.3354 0.0841 0.5000 0.038 Uiso 1 1 calc R . . H16B H 0.4427 0.1178 0.4941 0.038 Uiso 1 1 calc R . . H16C H 0.4154 0.0612 0.4387 0.038 Uiso 1 1 calc R . . C17 C 0.28510(18) 0.18902(11) 0.42926(15) 0.0299(5) Uani 1 1 d . . . H17A H 0.2311 0.1773 0.4639 0.045 Uiso 1 1 calc R . . H17B H 0.2542 0.2140 0.3841 0.045 Uiso 1 1 calc R . . H17C H 0.3402 0.2102 0.4633 0.045 Uiso 1 1 calc R . . C18 C 0.16512(15) 0.06722(10) 0.09760(13) 0.0183(4) Uani 1 1 d . . . H18 H 0.2202 0.0943 0.0821 0.022 Uiso 1 1 calc R . . C19 C 0.1918(2) 0.00525(11) 0.06708(15) 0.0317(6) Uani 1 1 d . . . H19A H 0.2606 -0.0064 0.0938 0.048 Uiso 1 1 calc R . . H19B H 0.1925 0.0057 0.0066 0.048 Uiso 1 1 calc R . . H19C H 0.1391 -0.0223 0.0818 0.048 Uiso 1 1 calc R . . C20 C 0.05794(17) 0.08871(11) 0.05363(14) 0.0295(5) Uani 1 1 d . . . H20A H 0.0026 0.0625 0.0671 0.044 Uiso 1 1 calc R . . H20B H 0.0602 0.0893 -0.0067 0.044 Uiso 1 1 calc R . . H20C H 0.0439 0.1279 0.0730 0.044 Uiso 1 1 calc R . . C21 C 0.30339(14) 0.18718(9) 0.17337(12) 0.0118(4) Uani 1 1 d . . . C22 C 0.20069(14) 0.21824(9) 0.15815(12) 0.0133(4) Uani 1 1 d . . . C23 C 0.12490(15) 0.21691(10) 0.21574(13) 0.0180(4) Uani 1 1 d . . . H23 H 0.1381 0.1957 0.2661 0.022 Uiso 1 1 calc R . . C24 C 0.02977(15) 0.24734(10) 0.19765(13) 0.0200(5) Uani 1 1 d . . . H24 H -0.0204 0.2464 0.2362 0.024 Uiso 1 1 calc R . . C25 C 0.00870(15) 0.27890(9) 0.12327(13) 0.0184(4) Uani 1 1 d . . . H25 H -0.0547 0.2998 0.1123 0.022 Uiso 1 1 calc R . . C26 C 0.08216(15) 0.27940(10) 0.06504(14) 0.0206(5) Uani 1 1 d . . . H26 H 0.0678 0.3000 0.0142 0.025 Uiso 1 1 calc R . . C27 C 0.17720(15) 0.24921(10) 0.08258(13) 0.0185(4) Uani 1 1 d . . . H27 H 0.2263 0.2496 0.0431 0.022 Uiso 1 1 calc R . . C28 C 0.41581(14) 0.26627(9) 0.12094(12) 0.0132(4) Uani 1 1 d . . . C29 C 0.42032(15) 0.31104(9) 0.18206(13) 0.0170(4) Uani 1 1 d . . . C30 C 0.40104(16) 0.30077(10) 0.27432(13) 0.0205(5) Uani 1 1 d . . . H30 H 0.3784 0.2596 0.2791 0.025 Uiso 1 1 calc R . . C31 C 0.5019(2) 0.30877(14) 0.33457(15) 0.0425(7) Uani 1 1 d . . . H31A H 0.5548 0.2812 0.3203 0.064 Uiso 1 1 calc R . . H31B H 0.4869 0.3019 0.3918 0.064 Uiso 1 1 calc R . . H31C H 0.5280 0.3484 0.3297 0.064 Uiso 1 1 calc R . . C32 C 0.3113(2) 0.33975(12) 0.29939(17) 0.0416(7) Uani 1 1 d . . . H32A H 0.2975 0.3302 0.3562 0.062 Uiso 1 1 calc R . . H32B H 0.2481 0.3330 0.2610 0.062 Uiso 1 1 calc R . . H32C H 0.3316 0.3806 0.2968 0.062 Uiso 1 1 calc R . . C33 C 0.44565(17) 0.36779(10) 0.15632(14) 0.0245(5) Uani 1 1 d . . . H33 H 0.4490 0.3987 0.1952 0.029 Uiso 1 1 calc R . . C34 C 0.46585(18) 0.37874(10) 0.07400(14) 0.0268(5) Uani 1 1 d . . . H34 H 0.4836 0.4168 0.0582 0.032 Uiso 1 1 calc R . . C35 C 0.45984(16) 0.33378(10) 0.01508(14) 0.0222(5) Uani 1 1 d . . . H35 H 0.4733 0.3421 -0.0402 0.027 Uiso 1 1 calc R . . C36 C 0.43419(14) 0.27626(9) 0.03612(12) 0.0155(4) Uani 1 1 d . . . C37 C 0.42746(16) 0.22830(10) -0.03128(13) 0.0184(4) Uani 1 1 d . . . H37 H 0.4140 0.1905 -0.0040 0.022 Uiso 1 1 calc R . . C38 C 0.53236(17) 0.22295(11) -0.07073(14) 0.0253(5) Uani 1 1 d . . . H38A H 0.5435 0.2581 -0.1026 0.038 Uiso 1 1 calc R . . H38B H 0.5292 0.1893 -0.1078 0.038 Uiso 1 1 calc R . . H38C H 0.5901 0.2181 -0.0265 0.038 Uiso 1 1 calc R . . C39 C 0.33667(17) 0.23930(11) -0.10218(14) 0.0256(5) Uani 1 1 d . . . H39A H 0.2701 0.2399 -0.0785 0.038 Uiso 1 1 calc R . . H39B H 0.3356 0.2082 -0.1436 0.038 Uiso 1 1 calc R . . H39C H 0.3474 0.2766 -0.1289 0.038 Uiso 1 1 calc R . . C40 C 0.47308(14) 0.16193(9) 0.16597(12) 0.0124(4) Uani 1 1 d . . . C41 C 0.58062(14) 0.16836(9) 0.13862(12) 0.0139(4) Uani 1 1 d . . . C42 C 0.64256(14) 0.21880(9) 0.15607(13) 0.0166(4) Uani 1 1 d . . . H42 H 0.6180 0.2491 0.1884 0.020 Uiso 1 1 calc R . . C43 C 0.74060(15) 0.22406(10) 0.12545(14) 0.0210(5) Uani 1 1 d . . . H43 H 0.7811 0.2581 0.1368 0.025 Uiso 1 1 calc R . . C44 C 0.77842(16) 0.17888(10) 0.07812(14) 0.0229(5) Uani 1 1 d . . . H44 H 0.8440 0.1826 0.0574 0.027 Uiso 1 1 calc R . . C45 C 0.71852(16) 0.12815(10) 0.06169(14) 0.0228(5) Uani 1 1 d . . . H45 H 0.7442 0.0976 0.0305 0.027 Uiso 1 1 calc R . . C46 C 0.61988(15) 0.12292(9) 0.09179(13) 0.0178(4) Uani 1 1 d . . . H46 H 0.5798 0.0888 0.0805 0.021 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.01253(11) 0.01100(12) 0.01971(12) 0.00227(10) 0.00081(8) 0.00004(9) Si1 0.0143(3) 0.0167(3) 0.0179(3) -0.0010(2) 0.0019(2) -0.0011(2) Si2 0.0194(3) 0.0136(3) 0.0199(3) -0.0010(2) 0.0027(2) 0.0017(2) N1 0.0130(8) 0.0143(9) 0.0198(9) -0.0002(7) 0.0008(6) -0.0002(6) N2 0.0105(7) 0.0106(8) 0.0121(8) 0.0004(7) 0.0024(6) -0.0008(6) C1I 0.0181(10) 0.0179(11) 0.0136(9) -0.0006(9) 0.0028(8) -0.0028(8) N4 0.0114(7) 0.0087(8) 0.0134(8) 0.0004(7) 0.0021(6) -0.0004(6) C1 0.0178(10) 0.0164(11) 0.0353(13) 0.0078(10) -0.0021(9) -0.0008(8) C2 0.0494(15) 0.0217(14) 0.0376(14) 0.0037(12) 0.0081(12) -0.0068(11) C3 0.0335(13) 0.0336(15) 0.0264(12) 0.0070(11) -0.0067(10) -0.0094(10) C4 0.0190(10) 0.0183(12) 0.0237(11) 0.0005(10) 0.0009(8) -0.0005(8) C5 0.0224(11) 0.0372(15) 0.0370(14) -0.0202(12) 0.0080(10) -0.0035(10) C6 0.0428(14) 0.0155(12) 0.0306(13) 0.0005(11) 0.0031(10) 0.0028(10) C7 0.0236(11) 0.0297(14) 0.0337(13) -0.0046(11) 0.0072(9) 0.0079(10) C8 0.0323(12) 0.0217(12) 0.0246(12) -0.0047(10) 0.0006(9) -0.0014(9) C9 0.0112(9) 0.0121(10) 0.0134(9) -0.0024(8) 0.0009(7) 0.0000(7) C10 0.0092(8) 0.0117(10) 0.0156(9) 0.0041(8) 0.0028(7) 0.0013(7) C11 0.0137(9) 0.0140(11) 0.0176(10) 0.0035(9) 0.0015(7) 0.0019(7) C12 0.0133(9) 0.0172(11) 0.0236(11) 0.0009(9) -0.0007(8) -0.0030(8) C13 0.0163(10) 0.0220(12) 0.0257(11) 0.0090(10) 0.0063(8) -0.0012(8) C14 0.0181(10) 0.0238(12) 0.0162(10) 0.0051(9) 0.0054(8) 0.0022(8) C15 0.0144(9) 0.0144(11) 0.0164(10) 0.0020(9) 0.0028(7) 0.0019(7) C16 0.0247(11) 0.0251(13) 0.0249(12) 0.0047(10) -0.0054(9) -0.0039(9) C17 0.0309(12) 0.0277(14) 0.0297(13) -0.0072(11) -0.0032(10) 0.0045(10) C18 0.0177(10) 0.0205(12) 0.0160(10) -0.0001(9) -0.0005(8) -0.0034(8) C19 0.0463(15) 0.0252(14) 0.0227(12) -0.0044(11) -0.0003(10) 0.0033(11) C20 0.0267(12) 0.0375(15) 0.0224(11) 0.0015(11) -0.0056(9) 0.0003(10) C21 0.0116(9) 0.0123(10) 0.0115(9) -0.0013(8) 0.0014(7) -0.0008(7) C22 0.0133(9) 0.0103(10) 0.0160(10) -0.0011(8) 0.0007(7) 0.0001(7) C23 0.0178(10) 0.0212(12) 0.0149(10) 0.0028(9) 0.0019(8) 0.0027(8) C24 0.0161(10) 0.0263(13) 0.0183(10) -0.0014(10) 0.0054(8) 0.0032(8) C25 0.0131(9) 0.0176(11) 0.0243(11) 0.0003(9) 0.0004(8) 0.0030(8) C26 0.0174(10) 0.0215(12) 0.0228(11) 0.0102(10) 0.0012(8) 0.0018(8) C27 0.0156(10) 0.0221(12) 0.0186(10) 0.0051(9) 0.0052(8) 0.0013(8) C28 0.0123(9) 0.0087(10) 0.0184(10) 0.0031(8) 0.0009(7) -0.0005(7) C29 0.0168(10) 0.0132(11) 0.0201(10) 0.0004(9) -0.0017(8) 0.0023(8) C30 0.0291(11) 0.0143(11) 0.0182(10) -0.0032(9) 0.0032(9) 0.0004(8) C31 0.0418(15) 0.063(2) 0.0214(13) 0.0042(13) -0.0022(11) -0.0104(13) C32 0.0561(17) 0.0357(16) 0.0355(14) -0.0010(13) 0.0162(13) 0.0144(13) C33 0.0341(12) 0.0125(11) 0.0254(12) -0.0017(10) -0.0034(9) -0.0019(9) C34 0.0352(13) 0.0138(12) 0.0291(12) 0.0060(10) -0.0057(10) -0.0081(9) C35 0.0270(11) 0.0211(12) 0.0178(11) 0.0063(10) -0.0003(8) -0.0070(9) C36 0.0141(9) 0.0150(11) 0.0169(10) 0.0014(9) -0.0001(7) -0.0013(7) C37 0.0237(10) 0.0159(11) 0.0166(10) 0.0016(9) 0.0063(8) -0.0027(8) C38 0.0277(12) 0.0308(14) 0.0187(11) 0.0033(10) 0.0079(9) 0.0026(9) C39 0.0253(11) 0.0317(14) 0.0198(11) -0.0051(10) 0.0026(9) -0.0042(9) C40 0.0145(9) 0.0100(10) 0.0127(9) -0.0017(8) 0.0009(7) 0.0036(7) C41 0.0121(9) 0.0142(11) 0.0154(9) 0.0046(8) 0.0013(7) 0.0003(7) C42 0.0141(9) 0.0150(11) 0.0209(10) 0.0020(9) 0.0029(8) 0.0019(8) C43 0.0145(10) 0.0199(12) 0.0283(12) 0.0061(10) 0.0015(8) -0.0026(8) C44 0.0137(10) 0.0297(13) 0.0266(12) 0.0094(10) 0.0083(8) 0.0016(8) C45 0.0231(11) 0.0232(13) 0.0240(11) 0.0006(10) 0.0111(9) 0.0077(9) C46 0.0194(10) 0.0147(11) 0.0198(10) 0.0027(9) 0.0038(8) -0.0001(8) _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 Zn1 N1 1.9767(15) . ? Zn1 C1 2.008(2) . ? Zn1 C9 2.061(2) . ? Si1 N1 1.6991(17) . ? Si1 C5 1.872(2) . ? Si1 C4 1.874(2) . ? Si1 C3 1.879(2) . ? Si2 N1 1.6981(18) . ? Si2 C8 1.877(2) . ? Si2 C6 1.879(2) . ? Si2 C7 1.884(2) . ? N2 C21 1.340(2) . ? N2 C9 1.412(2) . ? N2 C10 1.447(2) . ? C1I C16 1.519(3) . ? C1I C15 1.524(3) . ? C1I C17 1.526(3) . ? C1I H1I 0.9800 . ? N4 C21 1.350(2) . ? N4 C40 1.411(2) . ? N4 C28 1.450(2) . ? C1 C2 1.526(3) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C40 1.369(3) . ? C10 C11 1.394(3) . ? C10 C15 1.400(3) . ? C11 C12 1.390(3) . ? C11 C18 1.517(3) . ? C12 C13 1.383(3) . ? C12 H12 0.9300 . ? C13 C14 1.382(3) . ? C13 H13 0.9300 . ? C14 C15 1.390(3) . ? C14 H14 0.9300 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C20 1.531(3) . ? C18 C19 1.532(3) . ? C18 H18 0.9800 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C22 1.472(2) . ? C22 C27 1.390(3) . ? C22 C23 1.396(3) . ? C23 C24 1.387(3) . ? C23 H23 0.9300 . ? C24 C25 1.378(3) . ? C24 H24 0.9300 . ? C25 C26 1.381(3) . ? C25 H25 0.9300 . ? C26 C27 1.383(3) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C29 1.398(3) . ? C28 C36 1.407(3) . ? C29 C33 1.395(3) . ? C29 C30 1.526(3) . ? C30 C31 1.515(3) . ? C30 C32 1.525(3) . ? C30 H30 0.9800 . ? 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 1.379(3) . ? C33 H33 0.9300 . ? C34 C35 1.376(3) . ? C34 H34 0.9300 . ? C35 C36 1.390(3) . ? C35 H35 0.9300 . ? C36 C37 1.518(3) . ? C37 C39 1.533(3) . ? C37 C38 1.533(3) . ? C37 H37 0.9800 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 C41 1.480(2) . ? C41 C46 1.391(3) . ? C41 C42 1.393(3) . ? C42 C43 1.386(3) . ? C42 H42 0.9300 . ? C43 C44 1.384(3) . ? C43 H43 0.9300 . ? C44 C45 1.383(3) . ? C44 H44 0.9300 . ? C45 C46 1.390(3) . ? C45 H45 0.9300 . ? C46 H46 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 Zn1 C1 120.34(8) . . ? N1 Zn1 C9 115.38(7) . . ? C1 Zn1 C9 124.10(8) . . ? N1 Si1 C5 111.61(9) . . ? N1 Si1 C4 115.04(9) . . ? C5 Si1 C4 105.56(10) . . ? N1 Si1 C3 112.62(10) . . ? C5 Si1 C3 105.60(12) . . ? C4 Si1 C3 105.68(10) . . ? N1 Si2 C8 111.50(10) . . ? N1 Si2 C6 113.44(10) . . ? C8 Si2 C6 107.40(11) . . ? N1 Si2 C7 113.42(10) . . ? C8 Si2 C7 105.22(11) . . ? C6 Si2 C7 105.26(11) . . ? Si2 N1 Si1 123.45(10) . . ? Si2 N1 Zn1 112.65(9) . . ? Si1 N1 Zn1 122.07(9) . . ? C21 N2 C9 112.39(15) . . ? C21 N2 C10 123.60(15) . . ? C9 N2 C10 124.00(15) . . ? C16 C1I C15 111.76(17) . . ? C16 C1I C17 109.95(18) . . ? C15 C1I C17 111.54(16) . . ? C16 C1I H1I 107.8 . . ? C15 C1I H1I 107.8 . . ? C17 C1I H1I 107.8 . . ? C21 N4 C40 108.17(16) . . ? C21 N4 C28 125.07(15) . . ? C40 N4 C28 125.75(15) . . ? C2 C1 Zn1 116.44(16) . . ? C2 C1 H1A 108.2 . . ? Zn1 C1 H1A 108.2 . . ? C2 C1 H1B 108.2 . . ? Zn1 C1 H1B 108.2 . . ? H1A C1 H1B 107.3 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si1 C4 H4A 109.5 . . ? Si1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si1 C5 H5A 109.5 . . ? Si1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si2 C6 H6A 109.5 . . ? Si2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si2 C7 H7A 109.5 . . ? Si2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si2 C8 H8A 109.5 . . ? Si2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C40 C9 N2 103.17(16) . . ? C40 C9 Zn1 134.39(14) . . ? N2 C9 Zn1 122.36(13) . . ? C11 C10 C15 123.48(17) . . ? C11 C10 N2 118.64(16) . . ? C15 C10 N2 117.87(16) . . ? C12 C11 C10 116.93(18) . . ? C12 C11 C18 120.04(18) . . ? C10 C11 C18 123.02(17) . . ? C13 C12 C11 121.23(19) . . ? C13 C12 H12 119.4 . . ? C11 C12 H12 119.4 . . ? C14 C13 C12 120.30(19) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C13 C14 C15 121.06(19) . . ? C13 C14 H14 119.5 . . ? C15 C14 H14 119.5 . . ? C14 C15 C10 116.98(18) . . ? C14 C15 C1I 120.15(17) . . ? C10 C15 C1I 122.85(17) . . ? C1I C16 H16A 109.5 . . ? C1I C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C1I C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C1I C17 H17A 109.5 . . ? C1I C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C1I C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C11 C18 C20 111.51(17) . . ? C11 C18 C19 110.68(18) . . ? C20 C18 C19 111.20(18) . . ? C11 C18 H18 107.8 . . ? C20 C18 H18 107.8 . . ? C19 C18 H18 107.8 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N2 C21 N4 106.84(15) . . ? N2 C21 C22 127.97(16) . . ? N4 C21 C22 124.97(17) . . ? C27 C22 C23 118.56(18) . . ? C27 C22 C21 118.70(16) . . ? C23 C22 C21 122.73(18) . . ? C24 C23 C22 119.83(19) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C25 C24 C23 120.87(18) . . ? C25 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? C24 C25 C26 119.73(18) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 120.1 . . ? C25 C26 C27 119.8(2) . . ? C25 C26 H26 120.1 . . ? C27 C26 H26 120.1 . . ? C26 C27 C22 121.21(18) . . ? C26 C27 H27 119.4 . . ? C22 C27 H27 119.4 . . ? C29 C28 C36 123.16(18) . . ? C29 C28 N4 118.09(17) . . ? C36 C28 N4 118.70(17) . . ? C33 C29 C28 117.16(18) . . ? C33 C29 C30 119.13(19) . . ? C28 C29 C30 123.70(18) . . ? C31 C30 C32 111.4(2) . . ? C31 C30 C29 111.78(18) . . ? C32 C30 C29 111.44(18) . . ? C31 C30 H30 107.3 . . ? C32 C30 H30 107.3 . . ? C29 C30 H30 107.3 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 C29 121.0(2) . . ? C34 C33 H33 119.5 . . ? C29 C33 H33 119.5 . . ? C35 C34 C33 120.4(2) . . ? C35 C34 H34 119.8 . . ? C33 C34 H34 119.8 . . ? C34 C35 C36 121.66(19) . . ? C34 C35 H35 119.2 . . ? C36 C35 H35 119.2 . . ? C35 C36 C28 116.57(19) . . ? C35 C36 C37 119.72(18) . . ? C28 C36 C37 123.70(18) . . ? C36 C37 C39 112.19(17) . . ? C36 C37 C38 111.15(17) . . ? C39 C37 C38 108.96(17) . . ? C36 C37 H37 108.1 . . ? C39 C37 H37 108.1 . . ? C38 C37 H37 108.1 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C9 C40 N4 109.42(16) . . ? C9 C40 C41 129.81(17) . . ? N4 C40 C41 120.59(17) . . ? C46 C41 C42 118.93(17) . . ? C46 C41 C40 118.58(18) . . ? C42 C41 C40 122.47(18) . . ? C43 C42 C41 120.37(19) . . ? C43 C42 H42 119.8 . . ? C41 C42 H42 119.8 . . ? C44 C43 C42 120.2(2) . . ? C44 C43 H43 119.9 . . ? C42 C43 H43 119.9 . . ? C45 C44 C43 119.91(18) . . ? C45 C44 H44 120.0 . . ? C43 C44 H44 120.0 . . ? C44 C45 C46 120.0(2) . . ? C44 C45 H45 120.0 . . ? C46 C45 H45 120.0 . . ? C45 C46 C41 120.5(2) . . ? C45 C46 H46 119.7 . . ? C41 C46 H46 119.7 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.481 _refine_diff_density_min -0.293 _refine_diff_density_rms 0.062 _database_code_depnum_ccdc_archive 'CCDC 919364' ####################################################################### # # 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_complex2 #TrackingRef '16824_web_deposit_cif_file_1_TamalKumarSen_1357974721.complex 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H53 Al N2' _chemical_formula_sum 'C42 H53 Al N2' _chemical_formula_weight 612.84 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' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.871(2) _cell_length_b 10.967(2) _cell_length_c 18.786(4) _cell_angle_alpha 77.611(4) _cell_angle_beta 76.658(4) _cell_angle_gamma 75.050(4) _cell_volume 1885.6(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5380 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 25.06 _exptl_crystal_description block _exptl_crystal_colour white _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.079 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 664 _exptl_absorpt_coefficient_mu 0.083 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.988 _exptl_absorpt_correction_T_max 0.993 _exptl_absorpt_process_details 'SADABS; BRUKER; 2008' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25271 _diffrn_reflns_av_R_equivalents 0.0517 _diffrn_reflns_av_sigmaI/netI 0.0515 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.13 _diffrn_reflns_theta_max 25.06 _reflns_number_total 6652 _reflns_number_gt 4825 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0358P)^2^+0.9601P] 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 6652 _refine_ls_number_parameters 417 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0690 _refine_ls_R_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.1059 _refine_ls_wR_factor_gt 0.0884 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.39222(6) 0.44238(5) 0.28155(3) 0.02074(15) Uani 1 1 d . . . N1 N 0.16546(16) 0.67414(14) 0.21370(8) 0.0174(3) Uani 1 1 d . . . N2 N 0.05411(16) 0.78239(14) 0.30135(8) 0.0169(3) Uani 1 1 d . . . C1 C 0.5623(2) 0.7274(2) 0.10319(12) 0.0357(5) Uani 1 1 d . . . H1A H 0.5858 0.6405 0.1278 0.054 Uiso 1 1 calc R . . H1B H 0.6043 0.7800 0.1226 0.054 Uiso 1 1 calc R . . H1C H 0.5986 0.7315 0.0509 0.054 Uiso 1 1 calc R . . C2 C 0.3999(2) 0.77552(18) 0.11643(10) 0.0241(4) Uani 1 1 d . . . H2 H 0.3663 0.7760 0.1697 0.029 Uiso 1 1 calc R . . C3 C 0.3269(2) 0.68756(18) 0.09335(10) 0.0201(4) Uani 1 1 d . . . C4 C 0.21371(19) 0.63846(17) 0.14023(9) 0.0180(4) Uani 1 1 d . . . C5 C 0.06791(19) 0.78090(17) 0.22825(9) 0.0174(4) Uani 1 1 d . . . C6 C -0.0381(2) 0.88578(17) 0.33854(10) 0.0185(4) Uani 1 1 d . . . C7 C -0.1859(2) 0.89829(18) 0.35076(10) 0.0218(4) Uani 1 1 d . . . C8 C -0.2707(2) 1.00792(19) 0.37775(11) 0.0284(5) Uani 1 1 d . . . H8 H -0.3695 1.0200 0.3863 0.034 Uiso 1 1 calc R . . C9 C -0.2110(2) 1.0983(2) 0.39188(11) 0.0319(5) Uani 1 1 d . . . H9 H -0.2696 1.1718 0.4084 0.038 Uiso 1 1 calc R . . C10 C 0.2398(2) 1.0626(2) 0.28140(12) 0.0342(5) Uani 1 1 d . . . H10A H 0.2205 1.0536 0.2352 0.051 Uiso 1 1 calc R . . H10B H 0.3406 1.0528 0.2773 0.051 Uiso 1 1 calc R . . H10C H 0.1911 1.1458 0.2930 0.051 Uiso 1 1 calc R . . C11 C 0.1875(2) 0.95987(19) 0.34312(11) 0.0243(4) Uani 1 1 d . . . H11 H 0.2337 0.8762 0.3285 0.029 Uiso 1 1 calc R . . C12 C 0.2306(2) 0.9629(2) 0.41594(11) 0.0328(5) Uani 1 1 d . . . H12A H 0.1899 1.0455 0.4303 0.049 Uiso 1 1 calc R . . H12B H 0.3327 0.9466 0.4092 0.049 Uiso 1 1 calc R . . H12C H 0.1962 0.8984 0.4540 0.049 Uiso 1 1 calc R . . C13 C 0.0267(2) 0.97402(17) 0.35485(10) 0.0218(4) Uani 1 1 d . . . C14 C 0.14795(19) 0.67429(17) 0.33173(10) 0.0175(4) Uani 1 1 d . . . C15 C 0.1594(2) 0.65240(17) 0.41077(10) 0.0178(4) Uani 1 1 d . . . C16 C 0.2930(2) 0.63234(18) 0.42969(10) 0.0226(4) Uani 1 1 d . . . H16 H 0.3732 0.6348 0.3924 0.027 Uiso 1 1 calc R . . C17 C 0.3077(2) 0.60875(18) 0.50326(10) 0.0252(5) Uani 1 1 d . . . H17 H 0.3973 0.5957 0.5151 0.030 Uiso 1 1 calc R . . C18 C 0.1887(2) 0.60458(18) 0.55926(10) 0.0258(5) Uani 1 1 d . . . H18 H 0.1985 0.5877 0.6087 0.031 Uiso 1 1 calc R . . C19 C 0.0557(2) 0.62562(18) 0.54133(10) 0.0257(5) Uani 1 1 d . . . H19 H -0.0243 0.6237 0.5788 0.031 Uiso 1 1 calc R . . C20 C 0.0408(2) 0.64961(18) 0.46768(10) 0.0226(4) Uani 1 1 d . . . H20 H -0.0493 0.6640 0.4562 0.027 Uiso 1 1 calc R . . C21 C 0.22200(19) 0.60367(17) 0.27678(9) 0.0173(4) Uani 1 1 d . . . C22 C 0.3371(2) 0.32068(19) 0.37230(11) 0.0308(5) Uani 1 1 d . . . H22A H 0.2639 0.2838 0.3653 0.046 Uiso 1 1 calc R . . H22B H 0.3020 0.3654 0.4138 0.046 Uiso 1 1 calc R . . H22C H 0.4189 0.2541 0.3816 0.046 Uiso 1 1 calc R . . C23 C 0.5642(2) 0.4980(2) 0.29122(12) 0.0328(5) Uani 1 1 d . . . H23A H 0.5623 0.4978 0.3426 0.049 Uiso 1 1 calc R . . H23B H 0.5637 0.5828 0.2639 0.049 Uiso 1 1 calc R . . H23C H 0.6490 0.4401 0.2718 0.049 Uiso 1 1 calc R . . C24 C 0.4436(2) 0.36189(19) 0.19030(11) 0.0280(5) Uani 1 1 d . . . H24A H 0.5309 0.2983 0.1915 0.042 Uiso 1 1 calc R . . H24B H 0.4559 0.4263 0.1473 0.042 Uiso 1 1 calc R . . H24C H 0.3687 0.3223 0.1883 0.042 Uiso 1 1 calc R . . C25 C -0.00860(19) 0.87984(17) 0.17563(10) 0.0195(4) Uani 1 1 d . . . C26 C -0.0280(2) 1.00937(18) 0.17820(11) 0.0257(5) Uani 1 1 d . . . H26 H 0.0089 1.0339 0.2129 0.031 Uiso 1 1 calc R . . C27 C -0.1016(2) 1.1020(2) 0.12953(12) 0.0331(5) Uani 1 1 d . . . H27 H -0.1145 1.1881 0.1321 0.040 Uiso 1 1 calc R . . C28 C -0.1559(2) 1.0671(2) 0.07727(11) 0.0343(5) Uani 1 1 d . . . H28 H -0.2050 1.1293 0.0445 0.041 Uiso 1 1 calc R . . C29 C -0.1366(2) 0.9389(2) 0.07405(11) 0.0300(5) Uani 1 1 d . . . H29 H -0.1728 0.9149 0.0389 0.036 Uiso 1 1 calc R . . C30 C -0.0640(2) 0.84580(19) 0.12258(10) 0.0237(4) Uani 1 1 d . . . H30 H -0.0520 0.7599 0.1198 0.028 Uiso 1 1 calc R . . C31 C 0.1449(2) 0.55781(17) 0.12024(10) 0.0195(4) Uani 1 1 d . . . C32 C 0.0177(2) 0.51032(18) 0.17096(10) 0.0229(4) Uani 1 1 d . . . H32 H -0.0288 0.5721 0.2046 0.027 Uiso 1 1 calc R . . C33 C -0.0934(2) 0.5024(2) 0.12767(11) 0.0300(5) Uani 1 1 d . . . H33A H -0.1158 0.5814 0.0945 0.045 Uiso 1 1 calc R . . H33B H -0.1784 0.4871 0.1618 0.045 Uiso 1 1 calc R . . H33C H -0.0553 0.4335 0.0996 0.045 Uiso 1 1 calc R . . C34 C 0.0623(2) 0.3807(2) 0.21831(11) 0.0330(5) Uani 1 1 d . . . H34A H 0.1129 0.3189 0.1867 0.050 Uiso 1 1 calc R . . H34B H -0.0210 0.3538 0.2483 0.050 Uiso 1 1 calc R . . H34C H 0.1232 0.3876 0.2497 0.050 Uiso 1 1 calc R . . C35 C 0.1954(2) 0.52539(18) 0.04952(10) 0.0244(4) Uani 1 1 d . . . H35 H 0.1538 0.4708 0.0343 0.029 Uiso 1 1 calc R . . C36 C 0.3060(2) 0.57267(19) 0.00162(10) 0.0252(5) Uani 1 1 d . . . H36 H 0.3370 0.5504 -0.0455 0.030 Uiso 1 1 calc R . . C37 C 0.3709(2) 0.65275(18) 0.02312(10) 0.0236(4) Uani 1 1 d . . . H37 H 0.4451 0.6839 -0.0098 0.028 Uiso 1 1 calc R . . C38 C 0.3600(2) 0.91304(19) 0.07599(12) 0.0332(5) Uani 1 1 d . . . H38A H 0.3942 0.9155 0.0237 0.050 Uiso 1 1 calc R . . H38B H 0.4027 0.9674 0.0937 0.050 Uiso 1 1 calc R . . H38C H 0.2582 0.9425 0.0853 0.050 Uiso 1 1 calc R . . C39 C -0.2576(2) 0.80141(19) 0.33583(11) 0.0252(5) Uani 1 1 d . . . H39 H -0.1831 0.7330 0.3153 0.030 Uiso 1 1 calc R . . C40 C -0.3559(2) 0.8630(2) 0.27917(11) 0.0338(5) Uani 1 1 d . . . H40A H -0.4330 0.9268 0.2996 0.051 Uiso 1 1 calc R . . H40B H -0.3936 0.7984 0.2679 0.051 Uiso 1 1 calc R . . H40C H -0.3025 0.9022 0.2346 0.051 Uiso 1 1 calc R . . C41 C -0.3436(2) 0.7415(2) 0.40800(11) 0.0326(5) Uani 1 1 d . . . H41A H -0.2815 0.7015 0.4429 0.049 Uiso 1 1 calc R . . H41B H -0.3850 0.6786 0.3976 0.049 Uiso 1 1 calc R . . H41C H -0.4180 0.8071 0.4286 0.049 Uiso 1 1 calc R . . C42 C -0.0645(2) 1.08066(19) 0.38165(11) 0.0288(5) Uani 1 1 d . . . H42 H -0.0261 1.1416 0.3930 0.035 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0217(3) 0.0206(3) 0.0184(3) -0.0030(2) -0.0057(2) -0.0003(2) N1 0.0197(8) 0.0184(8) 0.0138(8) -0.0035(6) -0.0048(6) -0.0015(7) N2 0.0204(8) 0.0152(8) 0.0150(8) -0.0031(6) -0.0047(6) -0.0018(7) C1 0.0269(12) 0.0466(14) 0.0370(13) -0.0070(10) -0.0102(10) -0.0097(10) C2 0.0257(11) 0.0288(11) 0.0186(10) -0.0026(8) -0.0053(8) -0.0072(9) C3 0.0210(10) 0.0205(10) 0.0166(10) -0.0005(8) -0.0068(8) 0.0004(8) C4 0.0211(10) 0.0172(10) 0.0127(9) -0.0019(7) -0.0062(8) 0.0034(8) C5 0.0208(10) 0.0163(10) 0.0163(9) -0.0032(7) -0.0047(8) -0.0044(8) C6 0.0235(11) 0.0153(10) 0.0160(9) -0.0040(7) -0.0060(8) 0.0000(8) C7 0.0244(11) 0.0225(11) 0.0178(10) -0.0042(8) -0.0057(8) -0.0018(9) C8 0.0234(11) 0.0314(12) 0.0278(11) -0.0084(9) -0.0060(9) 0.0028(9) C9 0.0364(13) 0.0240(12) 0.0338(12) -0.0146(9) -0.0094(10) 0.0065(10) C10 0.0334(13) 0.0307(12) 0.0399(13) 0.0039(10) -0.0156(10) -0.0097(10) C11 0.0274(11) 0.0196(10) 0.0287(11) -0.0046(8) -0.0106(9) -0.0046(9) C12 0.0386(13) 0.0288(12) 0.0361(12) -0.0055(9) -0.0189(10) -0.0055(10) C13 0.0292(11) 0.0173(10) 0.0189(10) -0.0021(8) -0.0074(8) -0.0029(9) C14 0.0182(10) 0.0159(10) 0.0181(9) -0.0003(7) -0.0059(8) -0.0030(8) C15 0.0241(10) 0.0131(9) 0.0173(9) -0.0030(7) -0.0064(8) -0.0031(8) C16 0.0229(11) 0.0235(11) 0.0218(10) -0.0053(8) -0.0064(8) -0.0025(8) C17 0.0265(11) 0.0261(11) 0.0248(11) -0.0041(8) -0.0128(9) -0.0021(9) C18 0.0388(13) 0.0228(11) 0.0173(10) -0.0033(8) -0.0108(9) -0.0043(9) C19 0.0300(12) 0.0281(12) 0.0179(10) -0.0040(8) -0.0012(9) -0.0074(9) C20 0.0243(11) 0.0238(11) 0.0216(10) -0.0040(8) -0.0068(8) -0.0057(9) C21 0.0198(10) 0.0170(10) 0.0161(9) -0.0004(7) -0.0061(8) -0.0052(8) C22 0.0355(13) 0.0259(12) 0.0262(11) 0.0003(9) -0.0071(9) -0.0011(10) C23 0.0259(12) 0.0405(13) 0.0318(12) -0.0089(10) -0.0062(9) -0.0037(10) C24 0.0268(11) 0.0270(12) 0.0266(11) -0.0062(9) -0.0048(9) 0.0016(9) C25 0.0182(10) 0.0207(10) 0.0162(9) -0.0007(8) -0.0028(8) -0.0005(8) C26 0.0302(12) 0.0233(11) 0.0247(11) -0.0011(8) -0.0103(9) -0.0052(9) C27 0.0424(13) 0.0196(11) 0.0359(12) 0.0005(9) -0.0141(10) -0.0025(10) C28 0.0423(14) 0.0281(12) 0.0290(12) 0.0054(9) -0.0181(10) 0.0002(10) C29 0.0345(12) 0.0313(12) 0.0246(11) -0.0020(9) -0.0154(9) -0.0009(10) C30 0.0278(11) 0.0215(11) 0.0207(10) -0.0037(8) -0.0081(9) 0.0001(9) C31 0.0218(10) 0.0174(10) 0.0177(10) -0.0025(8) -0.0066(8) 0.0007(8) C32 0.0260(11) 0.0222(11) 0.0216(10) -0.0059(8) -0.0053(8) -0.0046(9) C33 0.0287(12) 0.0349(13) 0.0282(11) -0.0028(9) -0.0091(9) -0.0086(10) C34 0.0348(13) 0.0332(13) 0.0315(12) 0.0005(9) -0.0093(10) -0.0100(10) C35 0.0281(11) 0.0239(11) 0.0230(10) -0.0071(8) -0.0102(9) -0.0012(9) C36 0.0268(11) 0.0295(12) 0.0170(10) -0.0073(8) -0.0057(8) 0.0019(9) C37 0.0204(10) 0.0289(11) 0.0170(10) 0.0001(8) -0.0031(8) -0.0011(9) C38 0.0347(13) 0.0290(12) 0.0370(12) -0.0016(10) -0.0072(10) -0.0116(10) C39 0.0227(11) 0.0267(11) 0.0273(11) -0.0078(9) -0.0039(9) -0.0052(9) C40 0.0303(12) 0.0458(14) 0.0284(12) -0.0065(10) -0.0086(10) -0.0106(11) C41 0.0265(12) 0.0389(13) 0.0321(12) 0.0005(10) -0.0069(9) -0.0105(10) C42 0.0377(13) 0.0223(11) 0.0299(11) -0.0100(9) -0.0128(10) -0.0023(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 C22 1.988(2) . ? Al1 C24 1.998(2) . ? Al1 C23 2.003(2) . ? Al1 C21 2.1043(19) . ? N1 C5 1.344(2) . ? N1 C21 1.415(2) . ? N1 C4 1.455(2) . ? N2 C5 1.352(2) . ? N2 C14 1.406(2) . ? N2 C6 1.455(2) . ? C1 C2 1.532(3) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.523(3) . ? C2 C38 1.532(3) . ? C2 H2 0.9800 . ? C3 C37 1.393(3) . ? C3 C4 1.403(3) . ? C4 C31 1.398(3) . ? C5 C25 1.479(2) . ? C6 C7 1.398(3) . ? C6 C13 1.406(3) . ? C7 C8 1.396(3) . ? C7 C39 1.522(3) . ? C8 C9 1.373(3) . ? C8 H8 0.9300 . ? C9 C42 1.381(3) . ? C9 H9 0.9300 . ? C10 C11 1.531(3) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C13 1.523(3) . ? C11 C12 1.532(3) . ? C11 H11 0.9800 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C42 1.390(3) . ? C14 C21 1.379(3) . ? C14 C15 1.478(2) . ? C15 C20 1.393(3) . ? C15 C16 1.395(3) . ? C16 C17 1.385(3) . ? C16 H16 0.9300 . ? C17 C18 1.388(3) . ? C17 H17 0.9300 . ? C18 C19 1.380(3) . ? C18 H18 0.9300 . ? C19 C20 1.387(3) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? 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 C26 1.393(3) . ? C25 C30 1.396(3) . ? C26 C27 1.387(3) . ? C26 H26 0.9300 . ? C27 C28 1.381(3) . ? C27 H27 0.9300 . ? C28 C29 1.382(3) . ? C28 H28 0.9300 . ? C29 C30 1.382(3) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C35 1.395(3) . ? C31 C32 1.525(3) . ? C32 C34 1.524(3) . ? C32 C33 1.537(3) . ? C32 H32 0.9800 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 C36 1.382(3) . ? C35 H35 0.9300 . ? C36 C37 1.381(3) . ? C36 H36 0.9300 . ? C37 H37 0.9300 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 C40 1.537(3) . ? C39 C41 1.538(3) . ? 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 H42 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 C22 Al1 C24 112.00(9) . . ? C22 Al1 C23 108.77(9) . . ? C24 Al1 C23 107.52(9) . . ? C22 Al1 C21 107.33(8) . . ? C24 Al1 C21 112.74(8) . . ? C23 Al1 C21 108.36(9) . . ? C5 N1 C21 112.68(14) . . ? C5 N1 C4 123.72(14) . . ? C21 N1 C4 123.51(14) . . ? C5 N2 C14 108.79(14) . . ? C5 N2 C6 123.47(14) . . ? C14 N2 C6 127.64(14) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 C1 111.56(17) . . ? C3 C2 C38 111.14(16) . . ? C1 C2 C38 110.30(17) . . ? C3 C2 H2 107.9 . . ? C1 C2 H2 107.9 . . ? C38 C2 H2 107.9 . . ? C37 C3 C4 116.87(17) . . ? C37 C3 C2 120.43(17) . . ? C4 C3 C2 122.70(16) . . ? C31 C4 C3 123.74(16) . . ? C31 C4 N1 118.45(16) . . ? C3 C4 N1 117.82(16) . . ? N1 C5 N2 106.39(15) . . ? N1 C5 C25 127.76(16) . . ? N2 C5 C25 125.84(16) . . ? C7 C6 C13 123.48(17) . . ? C7 C6 N2 118.75(16) . . ? C13 C6 N2 117.57(16) . . ? C8 C7 C6 116.78(18) . . ? C8 C7 C39 119.11(18) . . ? C6 C7 C39 124.10(17) . . ? C9 C8 C7 121.3(2) . . ? C9 C8 H8 119.4 . . ? C7 C8 H8 119.4 . . ? C8 C9 C42 120.4(2) . . ? C8 C9 H9 119.8 . . ? C42 C9 H9 119.8 . . ? C11 C10 H10A 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C11 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C13 C11 C10 112.05(16) . . ? C13 C11 C12 109.98(17) . . ? C10 C11 C12 110.73(17) . . ? C13 C11 H11 108.0 . . ? C10 C11 H11 108.0 . . ? C12 C11 H11 108.0 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C42 C13 C6 116.41(18) . . ? C42 C13 C11 119.72(17) . . ? C6 C13 C11 123.86(17) . . ? C21 C14 N2 109.30(15) . . ? C21 C14 C15 129.68(16) . . ? N2 C14 C15 120.99(15) . . ? C20 C15 C16 118.39(16) . . ? C20 C15 C14 122.15(17) . . ? C16 C15 C14 119.46(16) . . ? C17 C16 C15 120.88(18) . . ? C17 C16 H16 119.6 . . ? C15 C16 H16 119.6 . . ? C16 C17 C18 119.96(18) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C19 C18 C17 119.78(17) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C18 C19 C20 120.29(18) . . ? C18 C19 H19 119.9 . . ? C20 C19 H19 119.9 . . ? C19 C20 C15 120.70(18) . . ? C19 C20 H20 119.6 . . ? C15 C20 H20 119.6 . . ? C14 C21 N1 102.81(15) . . ? C14 C21 Al1 129.04(13) . . ? N1 C21 Al1 127.86(12) . . ? Al1 C22 H22A 109.5 . . ? Al1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Al1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Al1 C23 H23A 109.5 . . ? Al1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Al1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Al1 C24 H24A 109.5 . . ? Al1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Al1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C30 118.41(17) . . ? C26 C25 C5 120.74(16) . . ? C30 C25 C5 120.85(17) . . ? C27 C26 C25 120.67(18) . . ? C27 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? C28 C27 C26 120.4(2) . . ? C28 C27 H27 119.8 . . ? C26 C27 H27 119.8 . . ? C27 C28 C29 119.38(18) . . ? C27 C28 H28 120.3 . . ? C29 C28 H28 120.3 . . ? C28 C29 C30 120.68(19) . . ? C28 C29 H29 119.7 . . ? C30 C29 H29 119.7 . . ? C29 C30 C25 120.49(19) . . ? C29 C30 H30 119.8 . . ? C25 C30 H30 119.8 . . ? C35 C31 C4 116.43(17) . . ? C35 C31 C32 120.79(17) . . ? C4 C31 C32 122.75(16) . . ? C34 C32 C31 112.41(16) . . ? C34 C32 C33 109.08(16) . . ? C31 C32 C33 112.30(16) . . ? C34 C32 H32 107.6 . . ? C31 C32 H32 107.6 . . ? C33 C32 H32 107.6 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 C31 121.45(18) . . ? C36 C35 H35 119.3 . . ? C31 C35 H35 119.3 . . ? C37 C36 C35 120.49(18) . . ? C37 C36 H36 119.8 . . ? C35 C36 H36 119.8 . . ? C36 C37 C3 121.01(18) . . ? C36 C37 H37 119.5 . . ? C3 C37 H37 119.5 . . ? C2 C38 H38A 109.5 . . ? C2 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C2 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C7 C39 C40 111.31(16) . . ? C7 C39 C41 110.91(16) . . ? C40 C39 C41 109.64(17) . . ? C7 C39 H39 108.3 . . ? C40 C39 H39 108.3 . . ? C41 C39 H39 108.3 . . ? 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 . . ? C9 C42 C13 121.58(19) . . ? C9 C42 H42 119.2 . . ? C13 C42 H42 119.2 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.205 _refine_diff_density_min -0.227 _refine_diff_density_rms 0.046 _database_code_depnum_ccdc_archive 'CCDC 919365'