# 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_2 _refine_special_details ; Anti-bumping restraints were employed to model the positional disorder of several H atoms. ; _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H74 Li2 N2 O3, 2(C4 H8 O)' _chemical_formula_sum 'C56 H90 Li2 N2 O5' _chemical_formula_weight 885.18 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' Li Li -0.0003 0.0001 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C c' _symmetry_space_group_name_Hall 'C -2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 27.1700(17) _cell_length_b 10.8660(7) _cell_length_c 18.7723(12) _cell_angle_alpha 90.00 _cell_angle_beta 105.400(1) _cell_angle_gamma 90.00 _cell_volume 5343.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 8348 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 27.49 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.100 _exptl_crystal_density_method ? _exptl_crystal_F_000 1944 _exptl_absorpt_coefficient_mu 0.068 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.683 _exptl_absorpt_correction_T_max 0.746 _exptl_absorpt_process_details 'SADABS 2007/2' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% 0 _diffrn_reflns_number 16172 _diffrn_reflns_av_R_equivalents 0.018 _diffrn_reflns_av_sigmaI/netI 0.024 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 27.53 _reflns_number_total 6110 _reflns_number_gt 5691 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36A (Bruker, 2002)' _computing_data_reduction 'Bruker SAINT; SHELXTL (Sheldrick, 2008)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'enCIFer (Allen et al., 2004); PLATON (Spek, 2009)' _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^)+(0.070P)^2^+1.875P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom, Me from difmap' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6110 _refine_ls_number_parameters 618 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0453 _refine_ls_R_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.107 _refine_ls_wR_factor_gt 0.103 _refine_ls_goodness_of_fit_ref 1.02 _refine_ls_restrained_S_all 1.03 _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 Li1 Li 0.98279(14) 0.6813(3) 0.9848(2) 0.0247(7) Uani 1 1 d . . . Li2 Li 1.00281(15) 0.8641(4) 1.0627(2) 0.0315(9) Uani 1 1 d . . . N1 N 0.93429(6) 0.80762(16) 1.01421(9) 0.0182(3) Uani 1 1 d . . . N2 N 1.01410(6) 0.85252(16) 0.96283(9) 0.0177(3) Uani 1 1 d . . . C1 C 0.92329(8) 0.85333(18) 0.94219(11) 0.0185(4) Uani 1 1 d . . . C2 C 0.87459(8) 0.87578(19) 0.89655(12) 0.0217(4) Uani 1 1 d . . . H2A H 0.8457 0.8573 0.9142 0.026 Uiso 1 1 calc R . . C3 C 0.86693(8) 0.9248(2) 0.82547(12) 0.0253(4) Uani 1 1 d . . . H3 H 0.8333 0.9392 0.7955 0.030 Uiso 1 1 calc R . . C4 C 0.90862(9) 0.9521(2) 0.79907(12) 0.0260(4) Uani 1 1 d . . . H4 H 0.9038 0.9872 0.7513 0.031 Uiso 1 1 calc R . . C5 C 0.95803(8) 0.9278(2) 0.84299(11) 0.0226(4) Uani 1 1 d . . . H5 H 0.9864 0.9458 0.8241 0.027 Uiso 1 1 calc R . . C6 C 0.96676(8) 0.87783(18) 0.91396(11) 0.0180(4) Uani 1 1 d . . . C7 C 0.89566(7) 0.82166(19) 1.05113(11) 0.0179(4) Uani 1 1 d . . . C8 C 0.87457(8) 0.71842(19) 1.07851(11) 0.0202(4) Uani 1 1 d . . . C9 C 0.83924(8) 0.73450(19) 1.11956(12) 0.0211(4) Uani 1 1 d . . . H9 H 0.8259 0.6639 1.1377 0.025 Uiso 1 1 calc R . . C10 C 0.82293(7) 0.84990(19) 1.13484(11) 0.0185(4) Uani 1 1 d . . . C11 C 0.84328(8) 0.95140(19) 1.10770(11) 0.0191(4) Uani 1 1 d . . . H11 H 0.8323 1.0313 1.1172 0.023 Uiso 1 1 calc R . . C12 C 0.87928(8) 0.94068(18) 1.06705(11) 0.0183(4) Uani 1 1 d . . . C13 C 0.88876(9) 0.5880(2) 1.06163(14) 0.0273(5) Uani 1 1 d . . . H13 H 0.9179 0.5938 1.0386 0.033 Uiso 1 1 calc R . . C14 C 0.90594(10) 0.5080(2) 1.13088(17) 0.0372(6) Uani 1 1 d . . . H14A H 0.8773 0.4964 1.1528 0.056 Uiso 1 1 calc R . . H14C H 0.9342 0.5485 1.1667 0.056 Uiso 1 1 calc R . . H14B H 0.9173 0.4277 1.1175 0.056 Uiso 1 1 calc R . . C15 C 0.84411(11) 0.5279(2) 1.00560(16) 0.0378(6) Uani 1 1 d . . . H15B H 0.8150 0.5206 1.0269 0.057 Uiso 1 1 calc R . . H15C H 0.8542 0.4458 0.9930 0.057 Uiso 1 1 calc R . . H15A H 0.8344 0.5785 0.9609 0.057 Uiso 1 1 calc R . . C16 C 0.78339(8) 0.8663(2) 1.17838(12) 0.0215(4) Uani 1 1 d . . . H16 H 0.7825 0.9555 1.1910 0.026 Uiso 1 1 calc R . . C17 C 0.79724(9) 0.7934(2) 1.25102(13) 0.0278(5) Uani 1 1 d . . . H17B H 0.7722 0.8109 1.2789 0.042 Uiso 1 1 calc R . . H17C H 0.8313 0.8175 1.2804 0.042 Uiso 1 1 calc R . . H17A H 0.7970 0.7051 1.2401 0.042 Uiso 1 1 calc R . . C18 C 0.73014(8) 0.8301(2) 1.13187(14) 0.0298(5) Uani 1 1 d . . . H18B H 0.7203 0.8831 1.0881 0.045 Uiso 1 1 calc R . . H18C H 0.7055 0.8401 1.1613 0.045 Uiso 1 1 calc R . . H18A H 0.7304 0.7441 1.1164 0.045 Uiso 1 1 calc R . . C19 C 0.90207(8) 1.05792(18) 1.04424(11) 0.0206(4) Uani 1 1 d . . . H19 H 0.9257 1.0330 1.0140 0.025 Uiso 1 1 calc R . . C20 C 0.86104(9) 1.1417(2) 0.99626(13) 0.0271(5) Uani 1 1 d . . . H20A H 0.8426 1.0970 0.9519 0.041 Uiso 1 1 calc R . . H20C H 0.8773 1.2148 0.9818 0.041 Uiso 1 1 calc R . . H20B H 0.8371 1.1670 1.0244 0.041 Uiso 1 1 calc R . . C21 C 0.93360(9) 1.1281(2) 1.11176(13) 0.0258(4) Uani 1 1 d . . . H21B H 0.9482 1.2020 1.0955 0.039 Uiso 1 1 calc R . . H21C H 0.9612 1.0752 1.1399 0.039 Uiso 1 1 calc R . . H21A H 0.9116 1.1520 1.1432 0.039 Uiso 1 1 calc R . . C22 C 1.05849(7) 0.87457(18) 0.93921(11) 0.0179(4) Uani 1 1 d . . . C23 C 1.07315(8) 0.79930(19) 0.88682(11) 0.0202(4) Uani 1 1 d . . . C24 C 1.12044(8) 0.8168(2) 0.87243(12) 0.0223(4) Uani 1 1 d . . . H24 H 1.1296 0.7652 0.8372 0.027 Uiso 1 1 calc R . . C25 C 1.15468(8) 0.9069(2) 0.90763(11) 0.0210(4) Uani 1 1 d . . . C26 C 1.13991(8) 0.98213(19) 0.95829(11) 0.0195(4) Uani 1 1 d . . . H26 H 1.1627 1.0444 0.9829 0.023 Uiso 1 1 calc R . . C27 C 1.09271(8) 0.96926(18) 0.97426(11) 0.0182(4) Uani 1 1 d . . . C28 C 1.03959(8) 0.6938(2) 0.84822(13) 0.0255(4) Uani 1 1 d . . . H28 H 1.0070 0.6970 0.8633 0.031 Uiso 1 1 calc R . . C29 C 1.02611(10) 0.7061(3) 0.76384(14) 0.0345(5) Uani 1 1 d . . . H29C H 1.0575 0.7066 0.7476 0.052 Uiso 1 1 calc R . . H29B H 1.0074 0.7831 0.7489 0.052 Uiso 1 1 calc R . . H29A H 1.0048 0.6364 0.7411 0.052 Uiso 1 1 calc R . . C30 C 1.06449(10) 0.5690(2) 0.87231(16) 0.0350(5) Uani 1 1 d . . . H30A H 1.0417 0.5031 0.8475 0.052 Uiso 1 1 calc R . . H30B H 1.0709 0.5602 0.9259 0.052 Uiso 1 1 calc R . . H30C H 1.0969 0.5637 0.8589 0.052 Uiso 1 1 calc R . . C31 C 1.20724(8) 0.9189(2) 0.89391(12) 0.0232(4) Uani 1 1 d . . . H31 H 1.2234 0.9958 0.9188 0.028 Uiso 1 1 calc R . . C32 C 1.20429(9) 0.9297(3) 0.81095(14) 0.0325(5) Uani 1 1 d . . . H32A H 1.1913 0.8525 0.7860 0.049 Uiso 1 1 calc R . . H32C H 1.2384 0.9462 0.8049 0.049 Uiso 1 1 calc R . . H32B H 1.1813 0.9972 0.7892 0.049 Uiso 1 1 calc R . . C33 C 1.24137(9) 0.8108(2) 0.92747(14) 0.0295(5) Uani 1 1 d . . . H33B H 1.2457 0.8090 0.9810 0.044 Uiso 1 1 calc R . . H33C H 1.2748 0.8202 0.9174 0.044 Uiso 1 1 calc R . . H33A H 1.2256 0.7338 0.9055 0.044 Uiso 1 1 calc R . . C34 C 1.07711(8) 1.05569(19) 1.02836(11) 0.0202(4) Uani 1 1 d . . . H2 H 1.0617 1.0037 1.0608 0.024 Uiso 1 1 calc R . . C35 C 1.12133(9) 1.1270(2) 1.07904(14) 0.0296(5) Uani 1 1 d . . . H35B H 1.1347 1.1867 1.0498 0.044 Uiso 1 1 calc R . . H35C H 1.1485 1.0694 1.1030 0.044 Uiso 1 1 calc R . . H35A H 1.1091 1.1704 1.1168 0.044 Uiso 1 1 calc R . . C36 C 1.03566(9) 1.1455(2) 0.98752(13) 0.0268(5) Uani 1 1 d . . . H36C H 1.0498 1.2004 0.9566 0.040 Uiso 1 1 calc R . . H36B H 1.0237 1.1942 1.0235 0.040 Uiso 1 1 calc R . . H36A H 1.0070 1.0991 0.9563 0.040 Uiso 1 1 calc R . . O1 O 0.95089(6) 0.54869(14) 0.91875(9) 0.0250(3) Uani 1 1 d . A . C37 C 0.95923(9) 0.4179(2) 0.93050(14) 0.0288(5) Uani 1 1 d . A . H37A H 0.9472 0.3900 0.9732 0.035 Uiso 1 1 calc R . . H37B H 0.9960 0.3980 0.9401 0.035 Uiso 1 1 calc R . . C38 C 0.92882(13) 0.3564(3) 0.85990(17) 0.0442(7) Uani 1 1 d . . . H38A H 0.9495 0.3480 0.8239 0.053 Uiso 0.787(10) 1 calc PR A 1 H38B H 0.9167 0.2740 0.8701 0.053 Uiso 0.787(10) 1 calc PR A 1 H38C H 0.9505 0.2972 0.8419 0.053 Uiso 0.213(10) 1 calc PR A 2 H38D H 0.8993 0.3116 0.8687 0.053 Uiso 0.213(10) 1 calc PR A 2 C39 C 0.88515(12) 0.4425(3) 0.83208(17) 0.0288(10) Uani 0.787(10) 1 d P A 1 H39B H 0.8580 0.4289 0.8574 0.035 Uiso 0.787(10) 1 calc PR A 1 H39A H 0.8705 0.4337 0.7781 0.035 Uiso 0.787(10) 1 calc PR A 1 C39A C 0.9124(5) 0.4495(11) 0.8087(6) 0.031(4) Uani 0.213(10) 1 d P A 2 H39C H 0.8781 0.4299 0.7764 0.037 Uiso 0.213(10) 1 calc PR A 2 H39D H 0.9363 0.4588 0.7774 0.037 Uiso 0.213(10) 1 calc PR A 2 C40 C 0.91045(10) 0.5682(2) 0.85155(14) 0.0318(5) Uani 1 1 d . . . H40B H 0.9246 0.5982 0.8113 0.038 Uiso 0.787(10) 1 calc PR A 1 H40A H 0.8855 0.6293 0.8599 0.038 Uiso 0.787(10) 1 calc PR A 1 H40D H 0.9174 0.6412 0.8241 0.038 Uiso 0.213(10) 1 calc PR A 2 H40C H 0.8769 0.5784 0.8623 0.038 Uiso 0.213(10) 1 calc PR A 2 O2 O 0.79546(7) 0.57834(18) 0.69467(11) 0.0371(4) Uani 1 1 d . . . C41 C 0.80577(11) 0.7007(3) 0.6742(2) 0.0471(7) Uani 1 1 d . . . H41A H 0.8200 0.6989 0.6309 0.057 Uiso 1 1 calc R . . H41B H 0.8307 0.7417 0.7156 0.057 Uiso 1 1 calc R . . C42 C 0.75514(10) 0.7690(2) 0.65566(16) 0.0347(5) Uani 1 1 d . . . H42A H 0.7513 0.8208 0.6111 0.042 Uiso 1 1 calc R . . H42B H 0.7523 0.8217 0.6974 0.042 Uiso 1 1 calc R . . C43 C 0.71504(9) 0.6659(2) 0.64155(14) 0.0292(5) Uani 1 1 d . . . H43B H 0.6956 0.6667 0.6793 0.035 Uiso 1 1 calc R . . H43A H 0.6909 0.6741 0.5920 0.035 Uiso 1 1 calc R . . C44 C 0.74673(9) 0.5490(2) 0.64695(14) 0.0304(5) Uani 1 1 d . . . H44A H 0.7307 0.4807 0.6677 0.037 Uiso 1 1 calc R . . H44B H 0.7499 0.5243 0.5976 0.037 Uiso 1 1 calc R . . O3 O 1.04070(6) 0.61908(17) 1.06626(9) 0.0307(4) Uani 1 1 d . B . C45 C 1.09213(8) 0.6674(2) 1.08124(15) 0.0292(5) Uani 1 1 d . B . H45B H 1.0969 0.7365 1.1168 0.035 Uiso 1 1 calc R . . H45A H 1.0993 0.6969 1.0351 0.035 Uiso 1 1 calc R . . C46 C 1.12673(10) 0.5612(3) 1.11359(19) 0.0427(7) Uani 1 1 d . . . H46C H 1.1471 0.5343 1.0798 0.051 Uiso 0.28(2) 1 calc PR B 4 H46D H 1.1502 0.5835 1.1619 0.051 Uiso 0.28(2) 1 calc PR B 4 H46B H 1.1599 0.5907 1.1451 0.051 Uiso 0.72(2) 1 calc PR B 3 H46A H 1.1330 0.5074 1.0743 0.051 Uiso 0.72(2) 1 calc PR B 3 C47 C 1.09610(17) 0.4940(5) 1.1594(4) 0.0331(14) Uani 0.72(2) 1 d P B 3 H47A H 1.1044 0.4051 1.1637 0.040 Uiso 0.72(2) 1 calc PR B 3 H47B H 1.1023 0.5299 1.2094 0.040 Uiso 0.72(2) 1 calc PR B 3 C47A C 1.0908(5) 0.4657(16) 1.1219(16) 0.050(5) Uani 0.28(2) 1 d P B 4 H47D H 1.0890 0.4012 1.0841 0.060 Uiso 0.28(2) 1 calc PR B 4 H47C H 1.1031 0.4270 1.1712 0.060 Uiso 0.28(2) 1 calc PR B 4 C48 C 1.04165(11) 0.5155(3) 1.11421(18) 0.0514(8) Uani 1 1 d . . . H48D H 1.0371 0.5418 1.1626 0.062 Uiso 0.28(2) 1 calc PR B 4 H48C H 1.0147 0.4552 1.0916 0.062 Uiso 0.28(2) 1 calc PR B 4 H48B H 1.0286 0.4414 1.0845 0.062 Uiso 0.72(2) 1 calc PR B 3 H48A H 1.0196 0.5319 1.1474 0.062 Uiso 0.72(2) 1 calc PR B 3 O4 O 1.02686(6) 0.87700(16) 1.16706(8) 0.0273(3) Uani 1 1 d . . . C49 C 1.07075(10) 0.9304(3) 1.21846(13) 0.0341(5) Uani 1 1 d . . . H49A H 1.0626 1.0135 1.2337 0.041 Uiso 1 1 calc R . . H49B H 1.0997 0.9369 1.1959 0.041 Uiso 1 1 calc R . . C50 C 1.08368(13) 0.8444(3) 1.28369(17) 0.0497(8) Uani 1 1 d . . . H50B H 1.0962 0.8908 1.3304 0.060 Uiso 1 1 calc R . . H50A H 1.1102 0.7845 1.2792 0.060 Uiso 1 1 calc R . . C51 C 1.03381(13) 0.7797(3) 1.28122(17) 0.0485(7) Uani 1 1 d . . . H51A H 1.0386 0.6893 1.2832 0.058 Uiso 1 1 calc R . . H51B H 1.0208 0.8054 1.3235 0.058 Uiso 1 1 calc R . . C52 C 0.99744(11) 0.8167(3) 1.20994(15) 0.0413(6) Uani 1 1 d . . . H52A H 0.9801 0.7433 1.1834 0.050 Uiso 1 1 calc R . . H52B H 0.9712 0.8732 1.2191 0.050 Uiso 1 1 calc R . . O5 O 0.69866(9) 0.8601(2) 0.80358(12) 0.0516(5) Uani 1 1 d . . . C53 C 0.71431(14) 0.9723(3) 0.8424(2) 0.0520(8) Uani 1 1 d . . . H53A H 0.6881 1.0368 0.8255 0.062 Uiso 1 1 calc R . . H53B H 0.7468 1.0014 0.8340 0.062 Uiso 1 1 calc R . . C54 C 0.72104(15) 0.9443(3) 0.92312(19) 0.0556(8) Uani 1 1 d . . . H54A H 0.6901 0.9666 0.9385 0.067 Uiso 1 1 calc R . . H54B H 0.7506 0.9894 0.9544 0.067 Uiso 1 1 calc R . . C55 C 0.73007(14) 0.8063(3) 0.92831(19) 0.0509(7) Uani 1 1 d . . . H55B H 0.7638 0.7868 0.9623 0.061 Uiso 1 1 calc R . . H55A H 0.7032 0.7641 0.9458 0.061 Uiso 1 1 calc R . . C56 C 0.72803(14) 0.7688(3) 0.84999(18) 0.0514(8) Uani 1 1 d . . . H56B H 0.7629 0.7649 0.8430 0.062 Uiso 1 1 calc R . . H56A H 0.7118 0.6870 0.8386 0.062 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 Li1 0.0229(17) 0.0192(17) 0.0329(19) 0.0003(15) 0.0089(15) -0.0001(14) Li2 0.0193(18) 0.056(3) 0.0184(17) 0.0002(17) 0.0035(14) -0.0081(17) N1 0.0154(8) 0.0192(8) 0.0213(8) 0.0027(7) 0.0070(6) 0.0009(6) N2 0.0161(8) 0.0193(8) 0.0181(8) 0.0004(6) 0.0050(6) -0.0003(6) C1 0.0205(9) 0.0151(9) 0.0196(9) -0.0027(7) 0.0048(8) 0.0003(7) C2 0.0191(9) 0.0216(10) 0.0240(10) -0.0016(8) 0.0051(8) 0.0000(7) C3 0.0211(10) 0.0285(11) 0.0228(10) -0.0024(8) -0.0005(8) 0.0040(8) C4 0.0282(11) 0.0309(11) 0.0173(9) 0.0004(8) 0.0035(8) 0.0027(9) C5 0.0238(10) 0.0251(10) 0.0199(9) -0.0008(8) 0.0076(8) -0.0002(8) C6 0.0209(9) 0.0148(9) 0.0183(9) -0.0025(7) 0.0051(7) 0.0003(7) C7 0.0137(8) 0.0210(9) 0.0180(9) 0.0012(7) 0.0026(7) 0.0003(7) C8 0.0186(9) 0.0176(9) 0.0256(10) 0.0022(8) 0.0077(8) 0.0014(7) C9 0.0195(9) 0.0193(9) 0.0252(10) 0.0034(8) 0.0070(8) -0.0008(7) C10 0.0128(8) 0.0237(10) 0.0192(9) 0.0001(8) 0.0043(7) 0.0002(7) C11 0.0192(9) 0.0178(9) 0.0195(9) -0.0008(7) 0.0037(7) 0.0017(7) C12 0.0164(9) 0.0182(9) 0.0200(9) 0.0024(7) 0.0039(7) -0.0010(7) C13 0.0263(11) 0.0168(10) 0.0465(13) 0.0007(9) 0.0232(10) 0.0010(8) C14 0.0337(13) 0.0243(12) 0.0569(17) 0.0089(11) 0.0177(12) 0.0083(10) C15 0.0460(15) 0.0258(12) 0.0447(14) -0.0099(11) 0.0175(12) -0.0032(11) C16 0.0203(10) 0.0214(10) 0.0252(10) -0.0017(8) 0.0100(8) 0.0004(7) C17 0.0344(12) 0.0282(11) 0.0241(10) 0.0032(9) 0.0137(9) 0.0022(9) C18 0.0186(10) 0.0342(12) 0.0377(12) -0.0010(10) 0.0094(9) 0.0013(9) C19 0.0235(10) 0.0171(9) 0.0228(9) 0.0012(8) 0.0088(8) -0.0005(7) C20 0.0307(11) 0.0207(10) 0.0303(11) 0.0068(9) 0.0089(9) 0.0016(8) C21 0.0273(11) 0.0225(10) 0.0288(11) -0.0022(9) 0.0092(9) -0.0045(8) C22 0.0171(9) 0.0186(9) 0.0181(9) 0.0022(7) 0.0048(7) 0.0013(7) C23 0.0199(9) 0.0209(10) 0.0205(9) 0.0005(8) 0.0065(8) -0.0001(8) C24 0.0232(10) 0.0223(10) 0.0230(10) -0.0020(8) 0.0093(8) 0.0021(8) C25 0.0179(9) 0.0233(10) 0.0227(9) 0.0039(8) 0.0069(8) 0.0031(8) C26 0.0174(9) 0.0198(9) 0.0202(9) 0.0015(8) 0.0031(7) -0.0010(7) C27 0.0199(9) 0.0183(9) 0.0169(9) 0.0022(7) 0.0058(7) 0.0011(7) C28 0.0214(10) 0.0253(11) 0.0317(11) -0.0099(9) 0.0106(9) -0.0034(8) C29 0.0318(12) 0.0407(14) 0.0309(12) -0.0141(11) 0.0080(10) -0.0065(10) C30 0.0341(13) 0.0234(11) 0.0506(15) -0.0072(11) 0.0167(12) -0.0030(9) C31 0.0183(9) 0.0242(10) 0.0289(11) 0.0000(9) 0.0097(8) -0.0005(8) C32 0.0255(11) 0.0443(15) 0.0320(12) 0.0064(10) 0.0150(10) 0.0012(10) C33 0.0205(10) 0.0318(12) 0.0367(12) 0.0018(10) 0.0082(9) 0.0055(9) C34 0.0211(9) 0.0203(10) 0.0204(9) -0.0015(8) 0.0076(8) -0.0007(8) C35 0.0262(11) 0.0320(12) 0.0302(11) -0.0108(10) 0.0066(9) -0.0060(9) C36 0.0279(11) 0.0239(11) 0.0292(11) -0.0025(9) 0.0087(9) 0.0051(8) O1 0.0245(8) 0.0199(7) 0.0277(8) 0.0002(6) 0.0020(6) 0.0004(6) C37 0.0291(11) 0.0198(10) 0.0345(12) 0.0023(9) 0.0030(9) 0.0010(8) C38 0.0521(17) 0.0293(14) 0.0430(15) -0.0079(11) -0.0015(13) -0.0031(12) C39 0.0275(17) 0.0283(16) 0.0291(16) -0.0050(12) 0.0052(13) -0.0055(11) C39A 0.031(7) 0.037(6) 0.026(6) -0.006(5) 0.009(5) -0.008(5) C40 0.0302(12) 0.0268(12) 0.0324(12) 0.0011(9) -0.0020(10) -0.0019(9) O2 0.0258(8) 0.0399(10) 0.0421(10) 0.0047(8) 0.0029(8) 0.0026(7) C41 0.0286(13) 0.0370(15) 0.073(2) -0.0081(14) 0.0090(13) -0.0028(11) C42 0.0334(13) 0.0287(12) 0.0427(14) -0.0057(11) 0.0112(11) -0.0023(10) C43 0.0238(11) 0.0293(12) 0.0339(12) -0.0036(10) 0.0068(9) 0.0013(9) C44 0.0269(11) 0.0289(12) 0.0354(12) -0.0002(10) 0.0081(10) 0.0014(9) O3 0.0190(7) 0.0407(10) 0.0305(8) 0.0092(7) 0.0030(6) -0.0035(7) C45 0.0174(10) 0.0277(11) 0.0410(13) 0.0044(10) 0.0049(9) 0.0013(8) C46 0.0251(12) 0.0410(15) 0.0624(18) 0.0208(13) 0.0122(12) 0.0076(11) C47 0.028(2) 0.035(2) 0.032(3) 0.011(2) 0.0009(19) -0.0026(15) C47A 0.040(6) 0.044(7) 0.057(12) 0.019(7) -0.002(7) -0.003(5) C48 0.0315(14) 0.068(2) 0.0475(16) 0.0307(15) -0.0011(12) -0.0139(13) O4 0.0268(8) 0.0358(9) 0.0187(7) -0.0002(6) 0.0050(6) -0.0040(7) C49 0.0361(13) 0.0388(14) 0.0235(11) -0.0019(10) 0.0011(10) -0.0079(11) C50 0.0487(17) 0.0560(19) 0.0334(14) 0.0113(13) -0.0085(13) -0.0123(14) C51 0.0563(18) 0.0506(17) 0.0339(14) 0.0162(13) 0.0036(13) -0.0070(14) C52 0.0408(15) 0.0557(17) 0.0272(12) 0.0044(12) 0.0088(11) -0.0121(13) O5 0.0569(13) 0.0495(13) 0.0424(12) 0.0021(9) 0.0030(10) 0.0036(10) C53 0.059(2) 0.0370(15) 0.0594(19) 0.0076(14) 0.0156(16) -0.0004(14) C54 0.062(2) 0.0497(19) 0.0475(17) -0.0054(15) 0.0013(15) 0.0045(15) C55 0.062(2) 0.0424(16) 0.0464(16) 0.0058(13) 0.0112(15) 0.0004(14) C56 0.0541(18) 0.0409(16) 0.0522(18) -0.0028(14) 0.0016(15) 0.0046(14) _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 Li1 O1 1.947(4) . ? Li1 O3 1.999(4) . ? Li1 N1 2.077(4) . ? Li1 N2 2.131(4) . ? Li1 Li2 2.441(6) . ? Li1 C1 2.462(4) . ? Li1 C6 2.492(4) . ? Li2 O4 1.899(4) . ? Li2 N1 1.942(4) . ? Li2 N2 1.982(4) . ? Li2 C1 2.684(4) . ? Li2 C6 2.706(4) . ? N1 C1 1.396(3) . ? N1 C7 1.411(2) . ? N2 C6 1.395(3) . ? N2 C22 1.412(2) . ? C1 C2 1.394(3) . ? C1 C6 1.442(3) . ? C2 C3 1.400(3) . ? C2 H2A 0.9500 . ? C3 C4 1.384(3) . ? C3 H3 0.9500 . ? C4 C5 1.401(3) . ? C4 H4 0.9500 . ? C5 C6 1.399(3) . ? C5 H5 0.9500 . ? C7 C8 1.417(3) . ? C7 C12 1.425(3) . ? C8 C9 1.392(3) . ? C8 C13 1.524(3) . ? C9 C10 1.385(3) . ? C9 H9 0.9500 . ? C10 C11 1.390(3) . ? C10 C16 1.523(3) . ? C11 C12 1.396(3) . ? C11 H11 0.9500 . ? C12 C19 1.527(3) . ? C13 C15 1.526(4) . ? C13 C14 1.531(4) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14C 0.9800 . ? C14 H14B 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C15 H15A 0.9800 . ? C16 C18 1.529(3) . ? C16 C17 1.535(3) . ? C16 H16 1.0000 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C17 H17A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C18 H18A 0.9800 . ? C19 C21 1.531(3) . ? C19 C20 1.533(3) . ? C19 H19 1.0000 . ? C20 H20A 0.9800 . ? C20 H20C 0.9800 . ? C20 H20B 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C21 H21A 0.9800 . ? C22 C23 1.415(3) . ? C22 C27 1.425(3) . ? C23 C24 1.394(3) . ? C23 C28 1.523(3) . ? C24 C25 1.390(3) . ? C24 H24 0.9500 . ? C25 C26 1.392(3) . ? C25 C31 1.523(3) . ? C26 C27 1.399(3) . ? C26 H26 0.9500 . ? C27 C34 1.524(3) . ? C28 C30 1.530(3) . ? C28 C29 1.534(3) . ? C28 H28 1.0000 . ? C29 H29C 0.9800 . ? C29 H29B 0.9800 . ? C29 H29A 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C33 1.526(3) . ? C31 C32 1.542(3) . ? C31 H31 1.0000 . ? C32 H32A 0.9800 . ? C32 H32C 0.9800 . ? C32 H32B 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C33 H33A 0.9800 . ? C34 C35 1.530(3) . ? C34 C36 1.532(3) . ? C34 H2 1.0000 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C35 H35A 0.9800 . ? C36 H36C 0.9800 . ? C36 H36B 0.9800 . ? C36 H36A 0.9800 . ? O1 C37 1.447(3) . ? O1 C40 1.452(3) . ? C37 C38 1.518(4) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39A 1.385(12) . ? C38 C39 1.492(4) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C38 H38C 0.9900 . ? C38 H38D 0.9900 . ? C39 C40 1.529(4) . ? C39 H39B 0.9900 . ? C39 H39A 0.9900 . ? C39A C40 1.529(12) . ? C39A H39C 0.9900 . ? C39A H39D 0.9900 . ? C40 H40B 0.9900 . ? C40 H40A 0.9900 . ? C40 H40D 0.9900 . ? C40 H40C 0.9900 . ? O2 C44 1.424(3) . ? O2 C41 1.432(4) . ? C41 C42 1.520(4) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.536(3) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.523(3) . ? C43 H43B 0.9900 . ? C43 H43A 0.9900 . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? O3 C48 1.437(3) . ? O3 C45 1.449(3) . ? C45 C46 1.510(3) . ? C45 H45B 0.9900 . ? C45 H45A 0.9900 . ? C46 C47A 1.461(13) . ? C46 C47 1.531(5) . ? C46 H46C 0.9900 . ? C46 H46D 0.9900 . ? C46 H46B 0.9900 . ? C46 H46A 0.9900 . ? C47 C48 1.515(6) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C47A C48 1.412(15) . ? C47A H47D 0.9900 . ? C47A H47C 0.9900 . ? C48 H48D 0.9900 . ? C48 H48C 0.9900 . ? C48 H48B 0.9900 . ? C48 H48A 0.9900 . ? O4 C52 1.434(3) . ? O4 C49 1.442(3) . ? C49 C50 1.505(4) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C51 1.516(4) . ? C50 H50B 0.9900 . ? C50 H50A 0.9900 . ? C51 C52 1.492(4) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? O5 C56 1.418(4) . ? O5 C53 1.426(4) . ? C53 C54 1.509(5) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C55 1.519(5) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.513(5) . ? C55 H55B 0.9900 . ? C55 H55A 0.9900 . ? C56 H56B 0.9900 . ? C56 H56A 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Li1 O3 111.33(19) . . ? O1 Li1 N1 116.85(19) . . ? O3 Li1 N1 116.5(2) . . ? O1 Li1 N2 131.0(2) . . ? O3 Li1 N2 99.78(18) . . ? N1 Li1 N2 77.78(14) . . ? O1 Li1 Li2 166.9(2) . . ? O3 Li1 Li2 79.14(18) . . ? N1 Li1 Li2 50.12(13) . . ? N2 Li1 Li2 50.84(13) . . ? O1 Li1 C1 102.26(17) . . ? O3 Li1 C1 145.2(2) . . ? N1 Li1 C1 34.53(9) . . ? N2 Li1 C1 62.34(12) . . ? Li2 Li1 C1 66.38(14) . . ? O1 Li1 C6 108.03(18) . . ? O3 Li1 C6 133.53(19) . . ? N1 Li1 C6 62.75(12) . . ? N2 Li1 C6 33.99(9) . . ? Li2 Li1 C6 66.54(14) . . ? C1 Li1 C6 33.84(8) . . ? O4 Li2 N1 122.1(2) . . ? O4 Li2 N2 152.0(2) . . ? N1 Li2 N2 84.64(16) . . ? O4 Li2 Li1 129.8(3) . . ? N1 Li2 Li1 55.17(15) . . ? N2 Li2 Li1 56.46(15) . . ? O4 Li2 C1 148.5(2) . . ? N1 Li2 C1 30.02(9) . . ? N2 Li2 C1 59.49(11) . . ? Li1 Li2 C1 57.19(13) . . ? O4 Li2 C6 172.5(3) . . ? N1 Li2 C6 59.65(12) . . ? N2 Li2 C6 29.82(9) . . ? Li1 Li2 C6 57.63(13) . . ? C1 Li2 C6 31.03(7) . . ? C1 N1 C7 116.17(16) . . ? C1 N1 Li2 105.88(18) . . ? C7 N1 Li2 118.77(18) . . ? C1 N1 Li1 88.00(16) . . ? C7 N1 Li1 144.04(17) . . ? Li2 N1 Li1 74.71(18) . . ? C6 N2 C22 118.40(16) . . ? C6 N2 Li2 105.21(17) . . ? C22 N2 Li2 130.24(17) . . ? C6 N2 Li1 87.34(16) . . ? C22 N2 Li1 128.83(16) . . ? Li2 N2 Li1 72.70(18) . . ? C2 C1 N1 125.58(19) . . ? C2 C1 C6 118.57(19) . . ? N1 C1 C6 115.84(17) . . ? C1 C2 C3 121.95(19) . . ? C1 C2 H2A 119.0 . . ? C3 C2 H2A 119.0 . . ? C4 C3 C2 119.6(2) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C3 C4 C5 119.8(2) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C6 C5 C4 121.8(2) . . ? C6 C5 H5 119.1 . . ? C4 C5 H5 119.1 . . ? N2 C6 C5 126.60(18) . . ? N2 C6 C1 115.10(17) . . ? C5 C6 C1 118.26(18) . . ? N1 C7 C8 121.18(18) . . ? N1 C7 C12 121.04(17) . . ? C8 C7 C12 117.62(17) . . ? C9 C8 C7 120.40(18) . . ? C9 C8 C13 118.78(18) . . ? C7 C8 C13 120.79(18) . . ? C10 C9 C8 122.26(19) . . ? C10 C9 H9 118.9 . . ? C8 C9 H9 118.9 . . ? C9 C10 C11 117.52(18) . . ? C9 C10 C16 121.79(18) . . ? C11 C10 C16 120.68(18) . . ? C10 C11 C12 122.61(18) . . ? C10 C11 H11 118.7 . . ? C12 C11 H11 118.7 . . ? C11 C12 C7 119.58(18) . . ? C11 C12 C19 118.61(18) . . ? C7 C12 C19 121.74(17) . . ? C8 C13 C15 110.06(19) . . ? C8 C13 C14 112.9(2) . . ? C15 C13 C14 110.5(2) . . ? C8 C13 H13 107.7 . . ? C15 C13 H13 107.7 . . ? C14 C13 H13 107.7 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? H14C C14 H14B 109.5 . . ? C13 C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C15 H15A 109.5 . . ? H15B C15 H15A 109.5 . . ? H15C C15 H15A 109.5 . . ? C10 C16 C18 111.03(17) . . ? C10 C16 C17 112.04(17) . . ? C18 C16 C17 110.25(19) . . ? C10 C16 H16 107.8 . . ? C18 C16 H16 107.8 . . ? C17 C16 H16 107.8 . . ? C16 C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C17 H17A 109.5 . . ? H17B C17 H17A 109.5 . . ? H17C C17 H17A 109.5 . . ? C16 C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C18 H18A 109.5 . . ? H18B C18 H18A 109.5 . . ? H18C C18 H18A 109.5 . . ? C12 C19 C21 111.27(17) . . ? C12 C19 C20 112.01(17) . . ? C21 C19 C20 110.50(17) . . ? C12 C19 H19 107.6 . . ? C21 C19 H19 107.6 . . ? C20 C19 H19 107.6 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? H20C C20 H20B 109.5 . . ? C19 C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C21 H21A 109.5 . . ? H21B C21 H21A 109.5 . . ? H21C C21 H21A 109.5 . . ? N2 C22 C23 122.80(18) . . ? N2 C22 C27 118.98(17) . . ? C23 C22 C27 117.95(18) . . ? C24 C23 C22 119.97(19) . . ? C24 C23 C28 118.46(18) . . ? C22 C23 C28 121.48(18) . . ? C25 C24 C23 122.60(19) . . ? C25 C24 H24 118.7 . . ? C23 C24 H24 118.7 . . ? C24 C25 C26 117.40(18) . . ? C24 C25 C31 121.30(18) . . ? C26 C25 C31 121.24(19) . . ? C25 C26 C27 122.32(19) . . ? C25 C26 H26 118.8 . . ? C27 C26 H26 118.8 . . ? C26 C27 C22 119.72(18) . . ? C26 C27 C34 120.94(18) . . ? C22 C27 C34 119.33(17) . . ? C23 C28 C30 111.40(19) . . ? C23 C28 C29 112.00(19) . . ? C30 C28 C29 110.4(2) . . ? C23 C28 H28 107.6 . . ? C30 C28 H28 107.6 . . ? C29 C28 H28 107.6 . . ? C28 C29 H29C 109.5 . . ? C28 C29 H29B 109.5 . . ? H29C C29 H29B 109.5 . . ? C28 C29 H29A 109.5 . . ? H29C C29 H29A 109.5 . . ? H29B C29 H29A 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C25 C31 C33 111.00(18) . . ? C25 C31 C32 112.19(18) . . ? C33 C31 C32 109.77(19) . . ? C25 C31 H31 107.9 . . ? C33 C31 H31 107.9 . . ? C32 C31 H31 107.9 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? H32C C32 H32B 109.5 . . ? C31 C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C33 H33A 109.5 . . ? H33B C33 H33A 109.5 . . ? H33C C33 H33A 109.5 . . ? C27 C34 C35 114.51(17) . . ? C27 C34 C36 110.88(17) . . ? C35 C34 C36 109.89(18) . . ? C27 C34 H2 107.1 . . ? C35 C34 H2 107.1 . . ? C36 C34 H2 107.1 . . ? C34 C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C35 H35A 109.5 . . ? H35B C35 H35A 109.5 . . ? H35C C35 H35A 109.5 . . ? C34 C36 H36C 109.5 . . ? C34 C36 H36B 109.5 . . ? H36C C36 H36B 109.5 . . ? C34 C36 H36A 109.5 . . ? H36C C36 H36A 109.5 . . ? H36B C36 H36A 109.5 . . ? C37 O1 C40 109.15(17) . . ? C37 O1 Li1 127.20(18) . . ? C40 O1 Li1 123.43(18) . . ? O1 C37 C38 105.81(19) . . ? O1 C37 H37A 110.6 . . ? C38 C37 H37A 110.6 . . ? O1 C37 H37B 110.6 . . ? C38 C37 H37B 110.6 . . ? H37A C37 H37B 108.7 . . ? C39A C38 C37 106.6(5) . . ? C39 C38 C37 103.1(2) . . ? C39 C38 H38A 111.1 . . ? C37 C38 H38A 111.1 . . ? C39A C38 H38B 137.1 . . ? C39 C38 H38B 111.1 . . ? C37 C38 H38B 111.1 . . ? H38A C38 H38B 109.1 . . ? C39A C38 H38C 110.4 . . ? C37 C38 H38C 110.4 . . ? C39A C38 H38D 110.4 . . ? C37 C38 H38D 110.4 . . ? H38C C38 H38D 108.6 . . ? C38 C39 C40 102.2(2) . . ? C38 C39 H39B 111.3 . . ? C40 C39 H39B 111.3 . . ? C38 C39 H39A 111.3 . . ? C40 C39 H39A 111.3 . . ? H39B C39 H39A 109.2 . . ? C38 C39A C40 107.5(7) . . ? C38 C39A H39C 110.2 . . ? C40 C39A H39C 110.2 . . ? C38 C39A H39D 110.2 . . ? C40 C39A H39D 110.2 . . ? H39C C39A H39D 108.5 . . ? O1 C40 C39A 102.1(5) . . ? O1 C40 C39 105.4(2) . . ? O1 C40 H40B 110.7 . . ? C39 C40 H40B 110.7 . . ? O1 C40 H40A 110.7 . . ? C39A C40 H40A 140.3 . . ? C39 C40 H40A 110.7 . . ? H40B C40 H40A 108.8 . . ? O1 C40 H40D 111.3 . . ? C39A C40 H40D 111.3 . . ? O1 C40 H40C 111.3 . . ? C39A C40 H40C 111.3 . . ? H40D C40 H40C 109.2 . . ? C44 O2 C41 104.8(2) . . ? O2 C41 C42 106.6(2) . . ? O2 C41 H41A 110.4 . . ? C42 C41 H41A 110.4 . . ? O2 C41 H41B 110.4 . . ? C42 C41 H41B 110.4 . . ? H41A C41 H41B 108.6 . . ? C41 C42 C43 104.0(2) . . ? C41 C42 H42A 111.0 . . ? C43 C42 H42A 111.0 . . ? C41 C42 H42B 111.0 . . ? C43 C42 H42B 111.0 . . ? H42A C42 H42B 109.0 . . ? C44 C43 C42 103.54(19) . . ? C44 C43 H43B 111.1 . . ? C42 C43 H43B 111.1 . . ? C44 C43 H43A 111.1 . . ? C42 C43 H43A 111.1 . . ? H43B C43 H43A 109.0 . . ? O2 C44 C43 105.7(2) . . ? O2 C44 H44A 110.6 . . ? C43 C44 H44A 110.6 . . ? O2 C44 H44B 110.6 . . ? C43 C44 H44B 110.6 . . ? H44A C44 H44B 108.7 . . ? C48 O3 C45 107.83(18) . . ? C48 O3 Li1 128.61(19) . . ? C45 O3 Li1 123.28(18) . . ? O3 C45 C46 105.5(2) . . ? O3 C45 H45B 110.6 . . ? C46 C45 H45B 110.6 . . ? O3 C45 H45A 110.6 . . ? C46 C45 H45A 110.6 . . ? H45B C45 H45A 108.8 . . ? C47A C46 C45 102.9(5) . . ? C45 C46 C47 102.5(2) . . ? C47A C46 H46C 111.2 . . ? C45 C46 H46C 111.2 . . ? C47A C46 H46D 111.2 . . ? C45 C46 H46D 111.2 . . ? H46C C46 H46D 109.1 . . ? C45 C46 H46B 111.3 . . ? C47 C46 H46B 111.3 . . ? C45 C46 H46A 111.3 . . ? C47 C46 H46A 111.3 . . ? H46B C46 H46A 109.2 . . ? C48 C47 C46 102.0(3) . . ? C48 C47 H47A 111.4 . . ? C46 C47 H47A 111.4 . . ? C48 C47 H47B 111.4 . . ? C46 C47 H47B 111.4 . . ? H47A C47 H47B 109.2 . . ? C48 C47A C46 111.0(10) . . ? C48 C47A H47D 109.4 . . ? C46 C47A H47D 109.4 . . ? C48 C47A H47C 109.4 . . ? C46 C47A H47C 109.4 . . ? H47D C47A H47C 108.0 . . ? C47A C48 O3 102.9(6) . . ? O3 C48 C47 108.9(2) . . ? C47A C48 H48D 111.2 . . ? O3 C48 H48D 111.2 . . ? C47A C48 H48C 111.2 . . ? O3 C48 H48C 111.2 . . ? C47 C48 H48C 129.7 . . ? H48D C48 H48C 109.1 . . ? O3 C48 H48B 109.9 . . ? C47 C48 H48B 109.9 . . ? O3 C48 H48A 109.9 . . ? C47 C48 H48A 109.9 . . ? H48B C48 H48A 108.3 . . ? C52 O4 C49 107.06(18) . . ? C52 O4 Li2 117.05(19) . . ? C49 O4 Li2 135.82(19) . . ? O4 C49 C50 105.5(2) . . ? O4 C49 H49A 110.6 . . ? C50 C49 H49A 110.6 . . ? O4 C49 H49B 110.6 . . ? C50 C49 H49B 110.6 . . ? H49A C49 H49B 108.8 . . ? C49 C50 C51 104.4(2) . . ? C49 C50 H50B 110.9 . . ? C51 C50 H50B 110.9 . . ? C49 C50 H50A 110.9 . . ? C51 C50 H50A 110.9 . . ? H50B C50 H50A 108.9 . . ? C52 C51 C50 106.0(2) . . ? C52 C51 H51A 110.5 . . ? C50 C51 H51A 110.5 . . ? C52 C51 H51B 110.5 . . ? C50 C51 H51B 110.5 . . ? H51A C51 H51B 108.7 . . ? O4 C52 C51 106.9(2) . . ? O4 C52 H52A 110.3 . . ? C51 C52 H52A 110.3 . . ? O4 C52 H52B 110.3 . . ? C51 C52 H52B 110.3 . . ? H52A C52 H52B 108.6 . . ? C56 O5 C53 104.0(2) . . ? O5 C53 C54 106.3(3) . . ? O5 C53 H53A 110.5 . . ? C54 C53 H53A 110.5 . . ? O5 C53 H53B 110.5 . . ? C54 C53 H53B 110.5 . . ? H53A C53 H53B 108.7 . . ? C53 C54 C55 103.8(3) . . ? C53 C54 H54A 111.0 . . ? C55 C54 H54A 111.0 . . ? C53 C54 H54B 111.0 . . ? C55 C54 H54B 111.0 . . ? H54A C54 H54B 109.0 . . ? C56 C55 C54 103.9(3) . . ? C56 C55 H55B 111.0 . . ? C54 C55 H55B 111.0 . . ? C56 C55 H55A 111.0 . . ? C54 C55 H55A 111.0 . . ? H55B C55 H55A 109.0 . . ? O5 C56 C55 106.1(3) . . ? O5 C56 H56B 110.5 . . ? C55 C56 H56B 110.5 . . ? O5 C56 H56A 110.5 . . ? C55 C56 H56A 110.5 . . ? H56B C56 H56A 108.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Li1 Li2 O4 110.7(10) . . . . ? O3 Li1 Li2 O4 -33.5(3) . . . . ? N1 Li1 Li2 O4 105.2(3) . . . . ? N2 Li1 Li2 O4 -145.8(3) . . . . ? C1 Li1 Li2 O4 141.5(3) . . . . ? C6 Li1 Li2 O4 178.5(3) . . . . ? O1 Li1 Li2 N1 5.4(10) . . . . ? O3 Li1 Li2 N1 -138.76(19) . . . . ? N2 Li1 Li2 N1 108.96(19) . . . . ? C1 Li1 Li2 N1 36.26(10) . . . . ? C6 Li1 Li2 N1 73.27(14) . . . . ? O1 Li1 Li2 N2 -103.5(10) . . . . ? O3 Li1 Li2 N2 112.29(17) . . . . ? N1 Li1 Li2 N2 -108.96(19) . . . . ? C1 Li1 Li2 N2 -72.70(13) . . . . ? C6 Li1 Li2 N2 -35.68(10) . . . . ? O1 Li1 Li2 C1 -30.8(10) . . . . ? O3 Li1 Li2 C1 -175.01(17) . . . . ? N1 Li1 Li2 C1 -36.26(11) . . . . ? N2 Li1 Li2 C1 72.70(13) . . . . ? C6 Li1 Li2 C1 37.02(9) . . . . ? O1 Li1 Li2 C6 -67.9(10) . . . . ? O3 Li1 Li2 C6 147.97(17) . . . . ? N1 Li1 Li2 C6 -73.27(14) . . . . ? N2 Li1 Li2 C6 35.68(10) . . . . ? C1 Li1 Li2 C6 -37.02(9) . . . . ? O4 Li2 N1 C1 157.7(3) . . . . ? N2 Li2 N1 C1 -31.0(2) . . . . ? Li1 Li2 N1 C1 -83.38(18) . . . . ? C6 Li2 N1 C1 -13.76(13) . . . . ? O4 Li2 N1 C7 24.9(4) . . . . ? N2 Li2 N1 C7 -163.82(16) . . . . ? Li1 Li2 N1 C7 143.8(2) . . . . ? C1 Li2 N1 C7 -132.8(2) . . . . ? C6 Li2 N1 C7 -146.56(18) . . . . ? O4 Li2 N1 Li1 -118.9(3) . . . . ? N2 Li2 N1 Li1 52.35(17) . . . . ? C1 Li2 N1 Li1 83.38(18) . . . . ? C6 Li2 N1 Li1 69.62(13) . . . . ? O1 Li1 N1 C1 -71.6(2) . . . . ? O3 Li1 N1 C1 153.4(2) . . . . ? N2 Li1 N1 C1 58.44(14) . . . . ? Li2 Li1 N1 C1 107.06(18) . . . . ? C6 Li1 N1 C1 25.87(12) . . . . ? O1 Li1 N1 C7 63.1(4) . . . . ? O3 Li1 N1 C7 -71.9(3) . . . . ? N2 Li1 N1 C7 -166.8(2) . . . . ? Li2 Li1 N1 C7 -118.2(3) . . . . ? C1 Li1 N1 C7 134.7(3) . . . . ? C6 Li1 N1 C7 160.6(3) . . . . ? O1 Li1 N1 Li2 -178.6(3) . . . . ? O3 Li1 N1 Li2 46.3(2) . . . . ? N2 Li1 N1 Li2 -48.62(15) . . . . ? C1 Li1 N1 Li2 -107.06(18) . . . . ? C6 Li1 N1 Li2 -81.19(15) . . . . ? O4 Li2 N2 C6 -164.9(6) . . . . ? N1 Li2 N2 C6 31.0(2) . . . . ? Li1 Li2 N2 C6 82.24(17) . . . . ? C1 Li2 N2 C6 13.58(13) . . . . ? O4 Li2 N2 C22 -13.8(7) . . . . ? N1 Li2 N2 C22 -177.87(18) . . . . ? Li1 Li2 N2 C22 -126.6(2) . . . . ? C1 Li2 N2 C22 164.7(2) . . . . ? C6 Li2 N2 C22 151.1(3) . . . . ? O4 Li2 N2 Li1 112.8(6) . . . . ? N1 Li2 N2 Li1 -51.23(16) . . . . ? C1 Li2 N2 Li1 -68.65(13) . . . . ? C6 Li2 N2 Li1 -82.24(17) . . . . ? O1 Li1 N2 C6 56.2(3) . . . . ? O3 Li1 N2 C6 -174.07(17) . . . . ? N1 Li1 N2 C6 -58.88(14) . . . . ? Li2 Li1 N2 C6 -106.83(17) . . . . ? C1 Li1 N2 C6 -25.84(11) . . . . ? O1 Li1 N2 C22 -68.8(3) . . . . ? O3 Li1 N2 C22 60.9(3) . . . . ? N1 Li1 N2 C22 176.11(18) . . . . ? Li2 Li1 N2 C22 128.2(2) . . . . ? C1 Li1 N2 C22 -150.85(19) . . . . ? C6 Li1 N2 C22 -125.0(2) . . . . ? O1 Li1 N2 Li2 163.1(3) . . . . ? O3 Li1 N2 Li2 -67.24(19) . . . . ? N1 Li1 N2 Li2 47.95(16) . . . . ? C1 Li1 N2 Li2 81.00(15) . . . . ? C6 Li1 N2 Li2 106.83(17) . . . . ? C7 N1 C1 C2 -20.8(3) . . . . ? Li2 N1 C1 C2 -155.0(2) . . . . ? Li1 N1 C1 C2 131.5(2) . . . . ? C7 N1 C1 C6 159.57(17) . . . . ? Li2 N1 C1 C6 25.3(2) . . . . ? Li1 N1 C1 C6 -48.14(19) . . . . ? C7 N1 C1 Li1 -152.3(2) . . . . ? Li2 N1 C1 Li1 73.49(19) . . . . ? C7 N1 C1 Li2 134.2(3) . . . . ? Li1 N1 C1 Li2 -73.49(19) . . . . ? O1 Li1 C1 C2 11.7(3) . . . . ? O3 Li1 C1 C2 -152.9(3) . . . . ? N1 Li1 C1 C2 -108.3(3) . . . . ? N2 Li1 C1 C2 141.8(3) . . . . ? Li2 Li1 C1 C2 -161.5(3) . . . . ? C6 Li1 C1 C2 115.9(3) . . . . ? O1 Li1 C1 N1 120.0(2) . . . . ? O3 Li1 C1 N1 -44.6(3) . . . . ? N2 Li1 C1 N1 -109.90(16) . . . . ? Li2 Li1 C1 N1 -53.20(15) . . . . ? C6 Li1 C1 N1 -135.85(19) . . . . ? O1 Li1 C1 C6 -104.17(18) . . . . ? O3 Li1 C1 C6 91.2(3) . . . . ? N1 Li1 C1 C6 135.85(19) . . . . ? N2 Li1 C1 C6 25.95(12) . . . . ? Li2 Li1 C1 C6 82.65(16) . . . . ? O1 Li1 C1 Li2 173.2(2) . . . . ? O3 Li1 C1 Li2 8.6(3) . . . . ? N1 Li1 C1 Li2 53.20(15) . . . . ? N2 Li1 C1 Li2 -56.70(13) . . . . ? C6 Li1 C1 Li2 -82.65(16) . . . . ? O4 Li2 C1 C2 32.2(8) . . . . ? N1 Li2 C1 C2 70.0(5) . . . . ? N2 Li2 C1 C2 -146.5(5) . . . . ? Li1 Li2 C1 C2 146.0(5) . . . . ? C6 Li2 C1 C2 -133.4(5) . . . . ? O4 Li2 C1 N1 -37.9(4) . . . . ? N2 Li2 C1 N1 143.4(2) . . . . ? Li1 Li2 C1 N1 76.0(2) . . . . ? C6 Li2 C1 N1 156.5(2) . . . . ? O4 Li2 C1 C6 165.6(5) . . . . ? N1 Li2 C1 C6 -156.5(2) . . . . ? N2 Li2 C1 C6 -13.09(13) . . . . ? Li1 Li2 C1 C6 -80.57(16) . . . . ? O4 Li2 C1 Li1 -113.8(5) . . . . ? N1 Li2 C1 Li1 -76.0(2) . . . . ? N2 Li2 C1 Li1 67.48(16) . . . . ? C6 Li2 C1 Li1 80.57(16) . . . . ? N1 C1 C2 C3 178.3(2) . . . . ? C6 C1 C2 C3 -2.1(3) . . . . ? Li1 C1 C2 C3 -101.8(3) . . . . ? Li2 C1 C2 C3 124.8(5) . . . . ? C1 C2 C3 C4 0.0(3) . . . . ? C2 C3 C4 C5 1.5(3) . . . . ? C3 C4 C5 C6 -0.9(3) . . . . ? C22 N2 C6 C5 -2.3(3) . . . . ? Li2 N2 C6 C5 152.9(2) . . . . ? Li1 N2 C6 C5 -135.8(2) . . . . ? C22 N2 C6 C1 -179.80(17) . . . . ? Li2 N2 C6 C1 -24.6(2) . . . . ? Li1 N2 C6 C1 46.70(19) . . . . ? C22 N2 C6 Li1 133.5(2) . . . . ? Li2 N2 C6 Li1 -71.27(19) . . . . ? C22 N2 C6 Li2 -155.2(3) . . . . ? Li1 N2 C6 Li2 71.27(19) . . . . ? C4 C5 C6 N2 -178.5(2) . . . . ? C4 C5 C6 C1 -1.1(3) . . . . ? C4 C5 C6 Li1 96.5(3) . . . . ? C4 C5 C6 Li2 -119.5(4) . . . . ? C2 C1 C6 N2 -179.73(18) . . . . ? N1 C1 C6 N2 -0.1(2) . . . . ? Li1 C1 C6 N2 -40.83(17) . . . . ? Li2 C1 C6 N2 17.84(18) . . . . ? C2 C1 C6 C5 2.6(3) . . . . ? N1 C1 C6 C5 -177.80(19) . . . . ? Li1 C1 C6 C5 141.5(2) . . . . ? Li2 C1 C6 C5 -159.9(2) . . . . ? C2 C1 C6 Li1 -138.9(2) . . . . ? N1 C1 C6 Li1 40.73(17) . . . . ? Li2 C1 C6 Li1 58.67(15) . . . . ? C2 C1 C6 Li2 162.4(2) . . . . ? N1 C1 C6 Li2 -17.93(18) . . . . ? Li1 C1 C6 Li2 -58.67(15) . . . . ? O1 Li1 C6 N2 -138.7(2) . . . . ? O3 Li1 C6 N2 8.1(2) . . . . ? N1 Li1 C6 N2 109.75(16) . . . . ? Li2 Li1 C6 N2 54.00(15) . . . . ? C1 Li1 C6 N2 136.12(19) . . . . ? O1 Li1 C6 C5 -28.2(4) . . . . ? O3 Li1 C6 C5 118.6(3) . . . . ? N1 Li1 C6 C5 -139.7(3) . . . . ? N2 Li1 C6 C5 110.6(3) . . . . ? Li2 Li1 C6 C5 164.6(3) . . . . ? C1 Li1 C6 C5 -113.3(3) . . . . ? O1 Li1 C6 C1 85.15(18) . . . . ? O3 Li1 C6 C1 -128.0(3) . . . . ? N1 Li1 C6 C1 -26.37(12) . . . . ? N2 Li1 C6 C1 -136.12(19) . . . . ? Li2 Li1 C6 C1 -82.12(16) . . . . ? O1 Li1 C6 Li2 167.3(2) . . . . ? O3 Li1 C6 Li2 -45.9(2) . . . . ? N1 Li1 C6 Li2 55.76(13) . . . . ? N2 Li1 C6 Li2 -54.00(15) . . . . ? C1 Li1 C6 Li2 82.12(16) . . . . ? O4 Li2 C6 N2 110.9(16) . . . . ? N1 Li2 C6 N2 -143.5(2) . . . . ? Li1 Li2 C6 N2 -77.90(19) . . . . ? C1 Li2 C6 N2 -156.9(2) . . . . ? O4 Li2 C6 C5 33.8(18) . . . . ? N1 Li2 C6 C5 139.4(4) . . . . ? N2 Li2 C6 C5 -77.0(5) . . . . ? Li1 Li2 C6 C5 -154.9(5) . . . . ? C1 Li2 C6 C5 126.1(5) . . . . ? O4 Li2 C6 C1 -92.3(16) . . . . ? N1 Li2 C6 C1 13.35(13) . . . . ? N2 Li2 C6 C1 156.9(2) . . . . ? Li1 Li2 C6 C1 78.99(16) . . . . ? O4 Li2 C6 Li1 -171.2(16) . . . . ? N1 Li2 C6 Li1 -65.64(16) . . . . ? N2 Li2 C6 Li1 77.9(2) . . . . ? C1 Li2 C6 Li1 -78.99(16) . . . . ? C1 N1 C7 C8 121.5(2) . . . . ? Li2 N1 C7 C8 -110.3(2) . . . . ? Li1 N1 C7 C8 -6.2(4) . . . . ? C1 N1 C7 C12 -63.3(2) . . . . ? Li2 N1 C7 C12 64.9(3) . . . . ? Li1 N1 C7 C12 169.0(3) . . . . ? N1 C7 C8 C9 175.20(18) . . . . ? C12 C7 C8 C9 -0.2(3) . . . . ? N1 C7 C8 C13 -6.7(3) . . . . ? C12 C7 C8 C13 177.9(2) . . . . ? C7 C8 C9 C10 0.6(3) . . . . ? C13 C8 C9 C10 -177.5(2) . . . . ? C8 C9 C10 C11 -0.2(3) . . . . ? C8 C9 C10 C16 178.64(19) . . . . ? C9 C10 C11 C12 -0.7(3) . . . . ? C16 C10 C11 C12 -179.49(18) . . . . ? C10 C11 C12 C7 1.1(3) . . . . ? C10 C11 C12 C19 -175.82(19) . . . . ? N1 C7 C12 C11 -176.00(18) . . . . ? C8 C7 C12 C11 -0.6(3) . . . . ? N1 C7 C12 C19 0.8(3) . . . . ? C8 C7 C12 C19 176.16(19) . . . . ? C9 C8 C13 C15 71.0(3) . . . . ? C7 C8 C13 C15 -107.1(2) . . . . ? C9 C8 C13 C14 -53.0(3) . . . . ? C7 C8 C13 C14 129.0(2) . . . . ? C9 C10 C16 C18 -72.9(3) . . . . ? C11 C10 C16 C18 105.9(2) . . . . ? C9 C10 C16 C17 50.9(3) . . . . ? C11 C10 C16 C17 -130.4(2) . . . . ? C11 C12 C19 C21 64.8(2) . . . . ? C7 C12 C19 C21 -112.0(2) . . . . ? C11 C12 C19 C20 -59.5(2) . . . . ? C7 C12 C19 C20 123.7(2) . . . . ? C6 N2 C22 C23 -72.7(3) . . . . ? Li2 N2 C22 C23 139.3(3) . . . . ? Li1 N2 C22 C23 38.9(3) . . . . ? C6 N2 C22 C27 113.4(2) . . . . ? Li2 N2 C22 C27 -34.6(3) . . . . ? Li1 N2 C22 C27 -135.0(2) . . . . ? N2 C22 C23 C24 -172.23(19) . . . . ? C27 C22 C23 C24 1.8(3) . . . . ? N2 C22 C23 C28 4.4(3) . . . . ? C27 C22 C23 C28 178.36(19) . . . . ? C22 C23 C24 C25 -0.2(3) . . . . ? C28 C23 C24 C25 -176.9(2) . . . . ? C23 C24 C25 C26 -0.8(3) . . . . ? C23 C24 C25 C31 176.5(2) . . . . ? C24 C25 C26 C27 0.2(3) . . . . ? C31 C25 C26 C27 -177.13(19) . . . . ? C25 C26 C27 C22 1.4(3) . . . . ? C25 C26 C27 C34 -178.19(19) . . . . ? N2 C22 C27 C26 171.88(18) . . . . ? C23 C22 C27 C26 -2.3(3) . . . . ? N2 C22 C27 C34 -8.5(3) . . . . ? C23 C22 C27 C34 177.26(18) . . . . ? C24 C23 C28 C30 64.4(3) . . . . ? C22 C23 C28 C30 -112.2(2) . . . . ? C24 C23 C28 C29 -59.7(3) . . . . ? C22 C23 C28 C29 123.6(2) . . . . ? C24 C25 C31 C33 -69.8(3) . . . . ? C26 C25 C31 C33 107.4(2) . . . . ? C24 C25 C31 C32 53.4(3) . . . . ? C26 C25 C31 C32 -129.4(2) . . . . ? C26 C27 C34 C35 -17.7(3) . . . . ? C22 C27 C34 C35 162.74(19) . . . . ? C26 C27 C34 C36 107.4(2) . . . . ? C22 C27 C34 C36 -72.2(2) . . . . ? O3 Li1 O1 C37 11.0(3) . . . . ? N1 Li1 O1 C37 -126.3(2) . . . . ? N2 Li1 O1 C37 136.5(2) . . . . ? Li2 Li1 O1 C37 -130.9(10) . . . . ? C1 Li1 O1 C37 -159.65(18) . . . . ? C6 Li1 O1 C37 165.76(18) . . . . ? O3 Li1 O1 C40 -175.10(19) . . . . ? N1 Li1 O1 C40 47.7(3) . . . . ? N2 Li1 O1 C40 -49.6(3) . . . . ? Li2 Li1 O1 C40 43.0(11) . . . . ? C1 Li1 O1 C40 14.3(3) . . . . ? C6 Li1 O1 C40 -20.3(3) . . . . ? C40 O1 C37 C38 10.2(3) . . . . ? Li1 O1 C37 C38 -175.1(2) . . . . ? O1 C37 C38 C39A 9.7(6) . . . . ? O1 C37 C38 C39 -30.3(3) . . . . ? C39A C38 C39 C40 -62.7(7) . . . . ? C37 C38 C39 C40 37.4(3) . . . . ? C39 C38 C39A C40 65.7(7) . . . . ? C37 C38 C39A C40 -24.8(9) . . . . ? C37 O1 C40 C39A -24.0(5) . . . . ? Li1 O1 C40 C39A 161.1(5) . . . . ? C37 O1 C40 C39 13.5(3) . . . . ? Li1 O1 C40 C39 -161.4(2) . . . . ? C38 C39A C40 O1 30.5(8) . . . . ? C38 C39A C40 C39 -69.0(8) . . . . ? C38 C39 C40 O1 -31.9(3) . . . . ? C38 C39 C40 C39A 57.7(8) . . . . ? C44 O2 C41 C42 36.9(3) . . . . ? O2 C41 C42 C43 -18.9(3) . . . . ? C41 C42 C43 C44 -4.7(3) . . . . ? C41 O2 C44 C43 -40.0(3) . . . . ? C42 C43 C44 O2 27.1(3) . . . . ? O1 Li1 O3 C48 -49.1(4) . . . . ? N1 Li1 O3 C48 88.4(3) . . . . ? N2 Li1 O3 C48 169.5(3) . . . . ? Li2 Li1 O3 C48 122.8(3) . . . . ? C1 Li1 O3 C48 114.8(4) . . . . ? C6 Li1 O3 C48 164.9(3) . . . . ? O1 Li1 O3 C45 124.0(2) . . . . ? N1 Li1 O3 C45 -98.6(3) . . . . ? N2 Li1 O3 C45 -17.5(3) . . . . ? Li2 Li1 O3 C45 -64.2(2) . . . . ? C1 Li1 O3 C45 -72.2(4) . . . . ? C6 Li1 O3 C45 -22.0(4) . . . . ? C48 O3 C45 C46 24.1(3) . . . . ? Li1 O3 C45 C46 -150.2(2) . . . . ? O3 C45 C46 C47A -6.5(13) . . . . ? O3 C45 C46 C47 -35.9(4) . . . . ? C47A C46 C47 C48 -60.8(12) . . . . ? C45 C46 C47 C48 33.2(5) . . . . ? C45 C46 C47A C48 -14(2) . . . . ? C47 C46 C47A C48 79(2) . . . . ? C46 C47A C48 O3 28(2) . . . . ? C46 C47A C48 C47 -77.4(18) . . . . ? C45 O3 C48 C47A -32.0(13) . . . . ? Li1 O3 C48 C47A 141.9(12) . . . . ? C45 O3 C48 C47 -2.2(5) . . . . ? Li1 O3 C48 C47 171.7(4) . . . . ? C46 C47 C48 C47A 62.8(11) . . . . ? C46 C47 C48 O3 -19.9(6) . . . . ? N1 Li2 O4 C52 14.4(4) . . . . ? N2 Li2 O4 C52 -146.7(5) . . . . ? Li1 Li2 O4 C52 -54.8(4) . . . . ? C1 Li2 O4 C52 35.7(6) . . . . ? C6 Li2 O4 C52 115.6(16) . . . . ? N1 Li2 O4 C49 -169.0(2) . . . . ? N2 Li2 O4 C49 29.9(8) . . . . ? Li1 Li2 O4 C49 121.9(3) . . . . ? C1 Li2 O4 C49 -147.7(4) . . . . ? C6 Li2 O4 C49 -67.8(17) . . . . ? C52 O4 C49 C50 32.8(3) . . . . ? Li2 O4 C49 C50 -144.0(3) . . . . ? O4 C49 C50 C51 -24.7(3) . . . . ? C49 C50 C51 C52 8.2(4) . . . . ? C49 O4 C52 C51 -27.6(3) . . . . ? Li2 O4 C52 C51 150.0(3) . . . . ? C50 C51 C52 O4 11.3(4) . . . . ? C56 O5 C53 C54 -38.9(4) . . . . ? O5 C53 C54 C55 23.1(4) . . . . ? C53 C54 C55 C56 0.4(4) . . . . ? C53 O5 C56 C55 39.1(3) . . . . ? C54 C55 C56 O5 -24.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.36 _refine_diff_density_min -0.20 _refine_diff_density_rms 0.04 _database_code_depnum_ccdc_archive 'CCDC 961088' ####################################################################### # # 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_3 _refine_special_details ; Disordered components were modelled on parts with geometric restraints. Selected oxygen atoms were modelled with approximate isotropy. Thermal parameters along bonds were equalised and a rigid bond restraint was applied. ; _audit_creation_method 'enCIFer editing of SHELXL-97 created file' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C88 H132 N4 Na4 O4' _chemical_formula_sum 'C88 H132 N4 Na4 O4' _chemical_formula_weight 1401.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.6580(3) _cell_length_b 24.4174(5) _cell_length_c 16.7902(4) _cell_angle_alpha 90.00 _cell_angle_beta 106.983(3) _cell_angle_gamma 90.00 _cell_volume 4178.93(18) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 7897 _cell_measurement_theta_min 3.62 _cell_measurement_theta_max 74.27 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_min 0.0919 _exptl_crystal_size_mid 0.2331 _exptl_crystal_size_max 0.2572 _exptl_crystal_density_diffrn 1.114 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1528 _exptl_absorpt_coefficient_mu 0.692 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.922 _exptl_absorpt_correction_T_max 1.143 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) Numerical absorption correction based on gaussian integration over a multifaceted crystal model ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Single source at offset), Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3613 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_%s 0 _diffrn_reflns_number 19821 _diffrn_reflns_av_R_equivalents 0.0357 _diffrn_reflns_av_sigmaI/netI 0.0407 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.62 _diffrn_reflns_theta_max 74.44 _reflns_number_total 8310 _reflns_number_gt 6204 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material 'enCIFer(Allen et al.,2004);PLATON(Spek,2003)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0569P)^2^+1.8456P] 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 8310 _refine_ls_number_parameters 781 _refine_ls_number_restraints 1955 _refine_ls_R_factor_all 0.0725 _refine_ls_R_factor_gt 0.0497 _refine_ls_wR_factor_ref 0.1311 _refine_ls_wR_factor_gt 0.1172 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.027 _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 Na1 Na 0.70954(6) 0.42369(3) 0.27867(4) 0.03099(17) Uani 1 1 d U . . Na2 Na 0.82047(7) 0.48305(3) 0.46072(4) 0.02924(16) Uani 1 1 d U . . O1 O 0.4978(5) 0.4541(4) 0.2167(4) 0.0419(8) Uani 0.459(19) 1 d PDU A 1 O1A O 0.5052(4) 0.4664(3) 0.2304(4) 0.0428(8) Uani 0.541(19) 1 d PDU A 2 O2 O 0.6009(8) 0.3474(2) 0.2396(5) 0.0445(10) Uani 0.399(5) 1 d PDU A 1 O2A O 0.6085(5) 0.33371(15) 0.2481(3) 0.0409(7) Uani 0.601(5) 1 d PDU A 2 N1 N 0.82624(14) 0.50698(6) 0.31982(9) 0.0266(2) Uani 1 1 d DU A . N2 N 0.90068(13) 0.40883(6) 0.39391(9) 0.0232(2) Uani 1 1 d DU A . C1 C 0.95853(16) 0.49677(7) 0.34774(10) 0.0216(2) Uani 1 1 d U A . C2 C 0.99887(15) 0.44418(7) 0.38905(10) 0.0203(2) Uani 1 1 d U . . C3 C 1.13426(16) 0.43363(7) 0.42035(10) 0.0237(3) Uani 1 1 d U . . H3 H 1.1622 0.4005 0.4498 0.028 Uiso 1 1 calc R . . C4 C 1.22973(17) 0.47036(8) 0.40965(11) 0.0275(3) Uani 1 1 d U . . H4 H 1.3203 0.4616 0.4305 0.033 Uiso 1 1 calc R A . C5 C 1.19092(18) 0.51928(8) 0.36864(11) 0.0292(3) Uani 1 1 d U . . H5 H 1.2548 0.5442 0.3609 0.035 Uiso 1 1 calc R . . C6 C 1.05735(18) 0.53204(7) 0.33843(10) 0.0256(3) Uani 1 1 d U . . H6 H 1.0325 0.5659 0.3105 0.031 Uiso 1 1 calc R A . C7 C 0.7851(10) 0.5496(3) 0.2609(4) 0.0279(5) Uani 0.690(7) 1 d PDU A 1 C7A C 0.779(2) 0.5490(7) 0.2594(10) 0.0286(6) Uani 0.310(7) 1 d PDU A 2 C8 C 0.7793(7) 0.5414(2) 0.1770(4) 0.0228(4) Uani 0.690(7) 1 d PDU A 1 C8A C 0.7799(16) 0.5428(5) 0.1751(10) 0.0241(7) Uani 0.310(7) 1 d PDU A 2 C9 C 0.7220(9) 0.5802(3) 0.1158(5) 0.0233(7) Uani 0.690(7) 1 d PDU A 1 H9 H 0.7203 0.5733 0.0598 0.028 Uiso 0.690(7) 1 calc PR A 1 C9A C 0.710(2) 0.5831(7) 0.1192(11) 0.0237(10) Uani 0.310(7) 1 d PDU A 2 H9A H 0.7064 0.5800 0.0623 0.028 Uiso 0.310(7) 1 calc PR A 2 C10 C 0.6679(5) 0.6283(2) 0.1345(3) 0.0259(7) Uani 0.690(7) 1 d PDU A 1 C10A C 0.6456(12) 0.6268(5) 0.1427(6) 0.0259(10) Uani 0.310(7) 1 d PDU A 2 C11 C 0.6795(4) 0.63849(16) 0.2180(2) 0.0286(7) Uani 0.690(7) 1 d PDU A 1 H11 H 0.6459 0.6718 0.2327 0.034 Uiso 0.690(7) 1 calc PR A 1 C11A C 0.6439(9) 0.6292(4) 0.2248(5) 0.0267(10) Uani 0.310(7) 1 d PDU A 2 H11A H 0.5965 0.6580 0.2409 0.032 Uiso 0.310(7) 1 calc PR A 2 C12 C 0.7392(4) 0.60121(16) 0.2806(2) 0.0296(6) Uani 0.690(7) 1 d PDU A 1 C12A C 0.7083(9) 0.5915(4) 0.2847(5) 0.0293(9) Uani 0.310(7) 1 d PDU A 2 C13 C 0.83447(17) 0.49061(7) 0.14750(11) 0.0254(3) Uani 1 1 d DU . . H13 H 0.8780 0.4681 0.1977 0.030 Uiso 0.690(7) 1 calc PR A 1 H13A H 0.8776 0.4686 0.1983 0.030 Uiso 0.310(7) 1 calc PR A 2 C14 C 0.72542(19) 0.45552(8) 0.08994(12) 0.0307(4) Uani 1 1 d DU A . H14A H 0.6610 0.4458 0.1189 0.046 Uiso 1 1 calc R . . H14B H 0.7637 0.4221 0.0747 0.046 Uiso 1 1 calc R . . H14C H 0.6821 0.4763 0.0395 0.046 Uiso 1 1 calc R . . C15 C 0.9377(2) 0.50408(10) 0.10346(14) 0.0416(5) Uani 1 1 d DU A . H15A H 0.8972 0.5254 0.0530 0.062 Uiso 1 1 calc R . . H15B H 0.9736 0.4700 0.0883 0.062 Uiso 1 1 calc R . . H15C H 1.0086 0.5255 0.1408 0.062 Uiso 1 1 calc R . . C16 C 0.5916(5) 0.6680(3) 0.0673(3) 0.0289(8) Uani 0.690(7) 1 d PDU A 1 H16 H 0.6091 0.6591 0.0134 0.035 Uiso 0.690(7) 1 calc PR A 1 C16A C 0.5699(11) 0.6670(6) 0.0773(8) 0.0272(12) Uani 0.310(7) 1 d PDU A 2 H16A H 0.5745 0.6512 0.0232 0.033 Uiso 0.310(7) 1 calc PR A 2 C17 C 0.4446(5) 0.6624(3) 0.0566(4) 0.0339(13) Uani 0.690(7) 1 d PDU A 1 H17A H 0.4177 0.6243 0.0433 0.051 Uiso 0.690(7) 1 calc PR A 1 H17B H 0.3956 0.6863 0.0113 0.051 Uiso 0.690(7) 1 calc PR A 1 H17C H 0.4264 0.6730 0.1084 0.051 Uiso 0.690(7) 1 calc PR A 1 C17A C 0.4224(11) 0.6666(7) 0.0707(10) 0.033(2) Uani 0.310(7) 1 d PDU A 2 H17D H 0.3879 0.6294 0.0585 0.050 Uiso 0.310(7) 1 calc PR A 2 H17E H 0.3754 0.6913 0.0258 0.050 Uiso 0.310(7) 1 calc PR A 2 H17F H 0.4104 0.6790 0.1235 0.050 Uiso 0.310(7) 1 calc PR A 2 C18 C 0.6295(14) 0.7282(3) 0.0903(8) 0.0386(16) Uani 0.690(7) 1 d PDU A 1 H18A H 0.6182 0.7364 0.1449 0.058 Uiso 0.690(7) 1 calc PR A 1 H18B H 0.5730 0.7524 0.0483 0.058 Uiso 0.690(7) 1 calc PR A 1 H18C H 0.7213 0.7341 0.0922 0.058 Uiso 0.690(7) 1 calc PR A 1 C18A C 0.638(3) 0.7231(6) 0.0830(17) 0.034(2) Uani 0.310(7) 1 d PDU A 2 H18D H 0.6350 0.7417 0.1342 0.052 Uiso 0.310(7) 1 calc PR A 2 H18E H 0.5923 0.7454 0.0348 0.052 Uiso 0.310(7) 1 calc PR A 2 H18F H 0.7293 0.7178 0.0838 0.052 Uiso 0.310(7) 1 calc PR A 2 C19 C 0.7421(4) 0.61352(16) 0.3697(2) 0.0361(7) Uani 0.690(7) 1 d PDU A 1 H19 H 0.8132 0.5906 0.4068 0.043 Uiso 0.690(7) 1 calc PR A 1 C19A C 0.6962(10) 0.5962(3) 0.3729(5) 0.0355(11) Uani 0.310(7) 1 d PDU A 2 H19A H 0.7745 0.5772 0.4103 0.043 Uiso 0.310(7) 1 calc PR A 2 C20 C 0.6132(4) 0.5960(2) 0.3842(2) 0.0489(9) Uani 0.690(7) 1 d PDU A 1 H20A H 0.5405 0.6162 0.3464 0.073 Uiso 0.690(7) 1 calc PR A 1 H20B H 0.6161 0.6038 0.4420 0.073 Uiso 0.690(7) 1 calc PR A 1 H20C H 0.6001 0.5566 0.3736 0.073 Uiso 0.690(7) 1 calc PR A 1 C20A C 0.5762(9) 0.5647(5) 0.3797(5) 0.0494(17) Uani 0.310(7) 1 d PDU A 2 H20D H 0.5743 0.5649 0.4377 0.074 Uiso 0.310(7) 1 calc PR A 2 H20E H 0.5807 0.5269 0.3614 0.074 Uiso 0.310(7) 1 calc PR A 2 H20F H 0.4965 0.5822 0.3444 0.074 Uiso 0.310(7) 1 calc PR A 2 C21 C 0.7741(5) 0.67376(17) 0.3947(2) 0.0523(11) Uani 0.690(7) 1 d PDU A 1 H21A H 0.8541 0.6846 0.3812 0.079 Uiso 0.690(7) 1 calc PR A 1 H21B H 0.7875 0.6779 0.4546 0.079 Uiso 0.690(7) 1 calc PR A 1 H21C H 0.7011 0.6971 0.3641 0.079 Uiso 0.690(7) 1 calc PR A 1 C21A C 0.7033(12) 0.6556(4) 0.4025(5) 0.055(2) Uani 0.310(7) 1 d PDU A 2 H21D H 0.6215 0.6745 0.3736 0.082 Uiso 0.310(7) 1 calc PR A 2 H21E H 0.7772 0.6740 0.3902 0.082 Uiso 0.310(7) 1 calc PR A 2 H21F H 0.7156 0.6564 0.4627 0.082 Uiso 0.310(7) 1 calc PR A 2 C22 C 0.928(3) 0.3525(5) 0.4077(14) 0.0267(6) Uani 0.436(4) 1 d PDU A 1 C22A C 0.933(2) 0.3528(4) 0.4061(11) 0.0262(5) Uani 0.564(4) 1 d PDU A 2 C23 C 0.9755(10) 0.3210(5) 0.3506(5) 0.0278(6) Uani 0.436(4) 1 d PDU A 1 C23A C 0.9862(8) 0.3214(4) 0.3533(4) 0.0281(5) Uani 0.564(4) 1 d PDU A 2 C24 C 0.9760(6) 0.2638(3) 0.3645(4) 0.0275(8) Uani 0.436(4) 1 d PDU A 1 H24 H 1.0099 0.2411 0.3298 0.033 Uiso 0.436(4) 1 calc PR A 1 C24A C 1.0130(4) 0.2654(2) 0.3634(3) 0.0266(7) Uani 0.564(4) 1 d PDU A 2 H24A H 1.0491 0.2468 0.3254 0.032 Uiso 0.564(4) 1 calc PR A 2 C25 C 0.9306(5) 0.23812(18) 0.4253(3) 0.0273(7) Uani 0.436(4) 1 d PDU A 1 C25A C 0.9876(4) 0.23681(14) 0.4281(2) 0.0244(6) Uani 0.564(4) 1 d PDU A 2 C26 C 0.8800(5) 0.2713(2) 0.4749(3) 0.0253(7) Uani 0.436(4) 1 d PDU A 1 H26 H 0.8482 0.2544 0.5162 0.030 Uiso 0.436(4) 1 calc PR A 1 C26A C 0.9355(4) 0.26617(15) 0.4821(2) 0.0252(6) Uani 0.564(4) 1 d PDU A 2 H26A H 0.9180 0.2475 0.5274 0.030 Uiso 0.564(4) 1 calc PR A 2 C27 C 0.8729(6) 0.3283(2) 0.4678(4) 0.0270(7) Uani 0.436(4) 1 d PDU A 1 C27A C 0.9081(4) 0.32222(18) 0.4722(3) 0.0253(6) Uani 0.564(4) 1 d PDU A 2 C28 C 1.01121(18) 0.34581(8) 0.27615(11) 0.0281(3) Uani 1 1 d DU . . H28 H 1.0030 0.3865 0.2792 0.034 Uiso 0.436(4) 1 calc PR A 1 H28A H 1.0030 0.3865 0.2792 0.034 Uiso 0.564(4) 1 calc PR A 2 C29 C 0.91160(19) 0.32630(8) 0.19555(11) 0.0323(4) Uani 1 1 d DU A . H29A H 0.9203 0.2867 0.1898 0.048 Uiso 1 1 calc R . . H29B H 0.9281 0.3450 0.1479 0.048 Uiso 1 1 calc R . . H29C H 0.8226 0.3348 0.1974 0.048 Uiso 1 1 calc R . . C30 C 1.1509(2) 0.33292(10) 0.27370(14) 0.0419(5) Uani 1 1 d DU A . H30A H 1.1605 0.2933 0.2684 0.063 Uiso 1 1 calc R . . H30B H 1.2141 0.3458 0.3252 0.063 Uiso 1 1 calc R . . H30C H 1.1672 0.3514 0.2259 0.063 Uiso 1 1 calc R . . C31 C 0.9382(5) 0.17635(18) 0.4378(3) 0.0296(8) Uani 0.436(4) 1 d PDU A 1 H31 H 0.8684 0.1662 0.4641 0.036 Uiso 0.436(4) 1 calc PR A 1 C31A C 1.0182(4) 0.17585(13) 0.4418(2) 0.0256(6) Uani 0.564(4) 1 d PDU A 2 H31A H 1.0514 0.1626 0.3953 0.031 Uiso 0.564(4) 1 calc PR A 2 C32 C 0.9101(6) 0.14471(19) 0.3568(3) 0.0463(12) Uani 0.436(4) 1 d PDU A 1 H32A H 0.8282 0.1580 0.3179 0.069 Uiso 0.436(4) 1 calc PR A 1 H32B H 0.9017 0.1057 0.3677 0.069 Uiso 0.436(4) 1 calc PR A 1 H32C H 0.9823 0.1500 0.3325 0.069 Uiso 0.436(4) 1 calc PR A 1 C32A C 0.8947(3) 0.14298(14) 0.4393(3) 0.0362(8) Uani 0.564(4) 1 d PDU A 2 H32D H 0.8581 0.1562 0.4830 0.054 Uiso 0.564(4) 1 calc PR A 2 H32E H 0.9174 0.1041 0.4486 0.054 Uiso 0.564(4) 1 calc PR A 2 H32F H 0.8297 0.1475 0.3848 0.054 Uiso 0.564(4) 1 calc PR A 2 C33 C 1.0689(5) 0.1597(2) 0.4986(4) 0.0328(10) Uani 0.436(4) 1 d PDU A 1 H33A H 1.1397 0.1673 0.4738 0.049 Uiso 0.436(4) 1 calc PR A 1 H33B H 1.0674 0.1205 0.5107 0.049 Uiso 0.436(4) 1 calc PR A 1 H33C H 1.0837 0.1806 0.5503 0.049 Uiso 0.436(4) 1 calc PR A 1 C33A C 1.1257(4) 0.16610(17) 0.5234(3) 0.0323(8) Uani 0.564(4) 1 d PDU A 2 H33D H 1.2038 0.1873 0.5234 0.048 Uiso 0.564(4) 1 calc PR A 2 H33E H 1.1478 0.1270 0.5289 0.048 Uiso 0.564(4) 1 calc PR A 2 H33F H 1.0946 0.1777 0.5702 0.048 Uiso 0.564(4) 1 calc PR A 2 C34 C 0.8080(6) 0.3608(3) 0.5219(4) 0.0268(9) Uani 0.436(4) 1 d PDU A 1 H34 H 0.8563 0.3964 0.5347 0.032 Uiso 0.436(4) 1 calc PR A 1 C34A C 0.8470(5) 0.35240(19) 0.5307(3) 0.0263(8) Uani 0.564(4) 1 d PDU A 2 H34A H 0.8854 0.3901 0.5389 0.032 Uiso 0.564(4) 1 calc PR A 2 C35 C 0.6654(6) 0.3748(3) 0.4754(4) 0.0322(12) Uani 0.436(4) 1 d PDU A 1 H35A H 0.6617 0.3929 0.4226 0.048 Uiso 0.436(4) 1 calc PR A 1 H35B H 0.6299 0.3994 0.5096 0.048 Uiso 0.436(4) 1 calc PR A 1 H35C H 0.6133 0.3411 0.4641 0.048 Uiso 0.436(4) 1 calc PR A 1 C35A C 0.6985(5) 0.3585(2) 0.4900(3) 0.0324(10) Uani 0.564(4) 1 d PDU A 2 H35D H 0.6826 0.3761 0.4354 0.049 Uiso 0.564(4) 1 calc PR A 2 H35E H 0.6611 0.3811 0.5256 0.049 Uiso 0.564(4) 1 calc PR A 2 H35F H 0.6573 0.3223 0.4830 0.049 Uiso 0.564(4) 1 calc PR A 2 C36 C 0.8152(7) 0.3343(3) 0.6051(3) 0.0342(12) Uani 0.436(4) 1 d PDU A 1 H36A H 0.7638 0.3003 0.5955 0.051 Uiso 0.436(4) 1 calc PR A 1 H36B H 0.7796 0.3595 0.6384 0.051 Uiso 0.436(4) 1 calc PR A 1 H36C H 0.9068 0.3259 0.6349 0.051 Uiso 0.436(4) 1 calc PR A 1 C36A C 0.8729(6) 0.3263(2) 0.6170(3) 0.0377(11) Uani 0.564(4) 1 d PDU A 2 H36D H 0.8283 0.2908 0.6116 0.056 Uiso 0.564(4) 1 calc PR A 2 H36E H 0.8395 0.3503 0.6528 0.056 Uiso 0.564(4) 1 calc PR A 2 H36F H 0.9674 0.3210 0.6416 0.056 Uiso 0.564(4) 1 calc PR A 2 C37 C 0.4457(8) 0.4956(5) 0.1559(6) 0.0449(11) Uani 0.459(19) 1 d PDU A 1 H37A H 0.4404 0.4818 0.0996 0.054 Uiso 0.459(19) 1 calc PR A 1 H37B H 0.5036 0.5282 0.1672 0.054 Uiso 0.459(19) 1 calc PR A 1 C37A C 0.4526(6) 0.5108(4) 0.1723(5) 0.0446(10) Uani 0.541(19) 1 d PDU A 2 H37C H 0.4561 0.5014 0.1156 0.053 Uiso 0.541(19) 1 calc PR A 2 H37D H 0.5024 0.5451 0.1904 0.053 Uiso 0.541(19) 1 calc PR A 2 C38 C 0.3100(9) 0.5110(5) 0.1603(7) 0.0470(12) Uani 0.459(19) 1 d PDU A 1 H38A H 0.2485 0.5167 0.1040 0.056 Uiso 0.459(19) 1 calc PR A 1 H38B H 0.3126 0.5446 0.1938 0.056 Uiso 0.459(19) 1 calc PR A 1 C38A C 0.3112(8) 0.5168(4) 0.1741(6) 0.0471(11) Uani 0.541(19) 1 d PDU A 2 H38C H 0.2541 0.5303 0.1200 0.056 Uiso 0.541(19) 1 calc PR A 2 H38D H 0.3050 0.5422 0.2187 0.056 Uiso 0.541(19) 1 calc PR A 2 C39 C 0.2714(8) 0.4611(6) 0.2026(8) 0.0454(11) Uani 0.459(19) 1 d PDU A 1 H39A H 0.2406 0.4305 0.1631 0.055 Uiso 0.459(19) 1 calc PR A 1 H39B H 0.2034 0.4701 0.2301 0.055 Uiso 0.459(19) 1 calc PR A 1 C39A C 0.2736(7) 0.4585(5) 0.1914(7) 0.0472(12) Uani 0.541(19) 1 d PDU A 2 H39C H 0.2005 0.4588 0.2166 0.057 Uiso 0.541(19) 1 calc PR A 2 H39D H 0.2472 0.4366 0.1394 0.057 Uiso 0.541(19) 1 calc PR A 2 C40 C 0.4040(8) 0.4486(5) 0.2660(5) 0.0449(10) Uani 0.459(19) 1 d PDU A 1 H40A H 0.4238 0.4751 0.3126 0.054 Uiso 0.459(19) 1 calc PR A 1 H40B H 0.4056 0.4111 0.2886 0.054 Uiso 0.459(19) 1 calc PR A 1 C40A C 0.3974(6) 0.4355(4) 0.2517(5) 0.0446(10) Uani 0.541(19) 1 d PDU A 2 H40C H 0.3989 0.4423 0.3101 0.054 Uiso 0.541(19) 1 calc PR A 2 H40D H 0.4050 0.3957 0.2433 0.054 Uiso 0.541(19) 1 calc PR A 2 C41 C 0.5087(8) 0.3409(3) 0.1577(4) 0.0515(11) Uani 0.399(5) 1 d PDU A 1 H41A H 0.5502 0.3507 0.1140 0.062 Uiso 0.399(5) 1 calc PR A 1 H41B H 0.4311 0.3646 0.1515 0.062 Uiso 0.399(5) 1 calc PR A 1 C41A C 0.5192(5) 0.3180(2) 0.1693(3) 0.0557(9) Uani 0.601(5) 1 d PDU A 2 H41C H 0.5195 0.3457 0.1262 0.067 Uiso 0.601(5) 1 calc PR A 2 H41D H 0.4289 0.3148 0.1737 0.067 Uiso 0.601(5) 1 calc PR A 2 C42 C 0.4701(7) 0.2826(3) 0.1511(4) 0.0589(13) Uani 0.399(5) 1 d PDU A 1 H42A H 0.4584 0.2688 0.0939 0.071 Uiso 0.399(5) 1 calc PR A 1 H42B H 0.3872 0.2773 0.1655 0.071 Uiso 0.399(5) 1 calc PR A 1 C42A C 0.5652(4) 0.26395(18) 0.1468(2) 0.0517(9) Uani 0.601(5) 1 d PDU A 2 H42C H 0.6272 0.2688 0.1134 0.062 Uiso 0.601(5) 1 calc PR A 2 H42D H 0.4904 0.2413 0.1148 0.062 Uiso 0.601(5) 1 calc PR A 2 C43 C 0.5823(7) 0.2534(3) 0.2129(4) 0.0447(10) Uani 0.399(5) 1 d PDU A 1 H43A H 0.6564 0.2466 0.1897 0.054 Uiso 0.399(5) 1 calc PR A 1 H43B H 0.5538 0.2183 0.2315 0.054 Uiso 0.399(5) 1 calc PR A 1 C43A C 0.6341(5) 0.23764(19) 0.2318(3) 0.0488(8) Uani 0.601(5) 1 d PDU A 2 H43C H 0.5842 0.2056 0.2422 0.059 Uiso 0.601(5) 1 calc PR A 2 H43D H 0.7242 0.2259 0.2347 0.059 Uiso 0.601(5) 1 calc PR A 2 C44 C 0.6173(11) 0.2957(3) 0.2829(5) 0.0423(10) Uani 0.399(5) 1 d PDU A 1 H44A H 0.5578 0.2929 0.3182 0.051 Uiso 0.399(5) 1 calc PR A 1 H44B H 0.7089 0.2910 0.3182 0.051 Uiso 0.399(5) 1 calc PR A 1 C44A C 0.6362(7) 0.28321(19) 0.2941(3) 0.0421(8) Uani 0.601(5) 1 d PDU A 2 H44C H 0.5693 0.2763 0.3232 0.050 Uiso 0.601(5) 1 calc PR A 2 H44D H 0.7234 0.2851 0.3361 0.050 Uiso 0.601(5) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Na1 0.0198(3) 0.0463(4) 0.0237(3) 0.0005(3) 0.0015(2) -0.0033(3) Na2 0.0271(3) 0.0366(4) 0.0251(3) -0.0009(3) 0.0094(2) 0.0009(3) O1 0.0185(6) 0.0804(19) 0.0264(13) 0.0125(14) 0.0057(7) 0.0022(9) O1A 0.0196(6) 0.0780(17) 0.0301(14) 0.0139(13) 0.0059(7) 0.0046(8) O2 0.0414(16) 0.0574(11) 0.0290(17) -0.0043(13) 0.0012(13) -0.0202(12) O2A 0.0373(12) 0.0588(10) 0.0256(13) -0.0088(11) 0.0077(10) -0.0217(11) N1 0.0239(5) 0.0316(5) 0.0229(5) 0.0043(5) 0.0046(5) 0.0071(4) N2 0.0216(5) 0.0269(5) 0.0197(6) 0.0028(4) 0.0039(4) -0.0020(4) C1 0.0227(4) 0.0232(6) 0.0172(7) 0.0016(5) 0.0032(4) 0.0029(4) C2 0.0198(5) 0.0226(6) 0.0167(7) 0.0013(5) 0.0026(4) -0.0002(4) C3 0.0206(6) 0.0287(8) 0.0194(7) 0.0018(6) 0.0019(5) 0.0026(5) C4 0.0178(6) 0.0411(9) 0.0222(8) -0.0016(7) 0.0036(6) -0.0023(6) C5 0.0278(6) 0.0373(8) 0.0219(8) -0.0019(7) 0.0065(6) -0.0115(7) C6 0.0320(6) 0.0235(7) 0.0199(7) 0.0015(6) 0.0054(6) -0.0038(5) C7 0.0249(13) 0.0331(7) 0.0216(7) 0.0019(6) 0.0001(9) 0.0086(8) C7A 0.0258(18) 0.0348(9) 0.0213(10) 0.0016(9) 0.0005(13) 0.0099(10) C8 0.0190(10) 0.0243(9) 0.0231(7) 0.0029(6) 0.0032(8) -0.0011(8) C8A 0.0212(16) 0.0263(13) 0.0222(10) 0.0022(9) 0.0025(13) 0.0015(12) C9 0.0206(19) 0.0252(11) 0.0223(9) 0.0025(8) 0.0035(11) 0.0000(9) C9A 0.021(2) 0.0262(16) 0.0214(13) 0.0013(13) 0.0025(17) 0.0016(15) C10 0.0257(17) 0.0260(9) 0.0222(9) 0.0024(8) 0.0011(10) 0.0022(11) C10A 0.025(2) 0.0269(15) 0.0223(13) 0.0006(13) 0.0016(15) 0.0040(14) C11 0.0304(17) 0.0271(13) 0.0234(8) 0.0002(8) 0.0002(11) 0.0066(12) C11A 0.026(2) 0.029(2) 0.0226(13) 0.0008(14) 0.0028(17) 0.0065(17) C12 0.0311(16) 0.0314(11) 0.0222(8) 0.0021(7) 0.0015(9) 0.0082(11) C12A 0.030(2) 0.0329(17) 0.0223(11) 0.0016(12) 0.0023(14) 0.0099(14) C13 0.0238(8) 0.0288(8) 0.0231(7) 0.0046(6) 0.0060(6) 0.0042(6) C14 0.0345(9) 0.0296(9) 0.0263(9) -0.0022(6) 0.0059(7) 0.0033(7) C15 0.0282(9) 0.0619(14) 0.0389(11) 0.0068(10) 0.0164(8) 0.0067(8) C16 0.0291(16) 0.0250(10) 0.0260(13) 0.0027(11) -0.0024(12) 0.0022(13) C16A 0.029(2) 0.0263(16) 0.0226(18) 0.0001(17) 0.002(2) 0.0050(16) C17 0.0291(15) 0.036(2) 0.028(2) 0.0043(18) -0.0047(15) 0.0028(14) C17A 0.027(2) 0.034(4) 0.033(5) -0.003(4) -0.002(3) 0.007(2) C18 0.037(2) 0.0238(11) 0.045(3) -0.0018(16) -0.005(2) 0.0044(16) C18A 0.035(4) 0.026(3) 0.034(4) 0.003(3) -0.002(4) 0.004(3) C19 0.0415(17) 0.0395(14) 0.0224(8) 0.0015(10) 0.0016(12) 0.0164(13) C19A 0.041(3) 0.041(2) 0.0209(14) 0.0013(18) 0.002(2) 0.018(2) C20 0.0450(19) 0.075(3) 0.0267(14) 0.0110(18) 0.0102(13) 0.0218(17) C20A 0.042(4) 0.079(5) 0.029(3) 0.011(4) 0.013(2) 0.016(3) C21 0.076(3) 0.0407(16) 0.0274(15) -0.0048(12) -0.0055(18) 0.0206(16) C21A 0.081(5) 0.045(3) 0.024(3) -0.004(2) -0.005(3) 0.033(3) C22 0.0315(19) 0.0249(7) 0.0208(13) 0.0012(9) 0.0032(10) -0.0057(9) C22A 0.0307(18) 0.0245(7) 0.0208(12) 0.0015(8) 0.0035(9) -0.0054(8) C23 0.0319(17) 0.0251(9) 0.0227(9) 0.0031(11) 0.0021(10) 0.0000(14) C23A 0.0323(15) 0.0259(9) 0.0228(8) 0.0027(9) 0.0029(9) 0.0002(12) C24 0.029(2) 0.0259(9) 0.0258(15) 0.0029(10) 0.0053(14) 0.0004(16) C24A 0.0274(19) 0.0267(9) 0.0255(12) 0.0030(9) 0.0075(12) -0.0010(13) C25 0.0262(19) 0.0263(10) 0.0272(14) 0.0044(9) 0.0043(14) -0.0002(12) C25A 0.0240(16) 0.0237(9) 0.0254(12) 0.0011(8) 0.0070(12) -0.0013(10) C26 0.027(2) 0.0258(10) 0.0187(15) 0.0044(11) 0.0005(15) -0.0017(15) C26A 0.0296(18) 0.0229(9) 0.0218(12) 0.0024(9) 0.0057(13) 0.0010(12) C27 0.032(2) 0.0245(10) 0.0220(13) 0.0036(10) 0.0030(12) -0.0029(13) C27A 0.0307(18) 0.0218(9) 0.0213(11) 0.0003(8) 0.0043(12) -0.0021(11) C28 0.0331(8) 0.0245(8) 0.0262(7) 0.0023(6) 0.0082(6) 0.0050(7) C29 0.0382(9) 0.0353(10) 0.0236(6) 0.0027(7) 0.0095(6) 0.0021(8) C30 0.0350(8) 0.0502(13) 0.0416(11) 0.0018(10) 0.0128(7) 0.0099(9) C31 0.0262(18) 0.0267(11) 0.0355(16) 0.0058(11) 0.0085(15) 0.0001(14) C31A 0.0241(15) 0.0246(9) 0.0301(13) 0.0025(10) 0.0110(11) 0.0018(11) C32 0.060(3) 0.0275(17) 0.042(2) -0.0002(15) 0.0000(19) 0.001(2) C32A 0.0327(15) 0.0245(14) 0.054(2) -0.0015(15) 0.0178(14) -0.0041(12) C33 0.030(2) 0.033(2) 0.035(2) 0.0080(18) 0.0099(15) 0.0075(18) C33A 0.0319(18) 0.0337(18) 0.0319(18) 0.0079(14) 0.0103(12) 0.0066(15) C34 0.034(2) 0.0245(17) 0.0188(16) 0.0040(14) 0.0039(15) -0.0040(17) C34A 0.0365(19) 0.0190(14) 0.0234(13) 0.0008(11) 0.0085(13) -0.0039(13) C35 0.031(2) 0.039(4) 0.027(2) 0.006(2) 0.0093(18) -0.0029(18) C35A 0.0350(19) 0.033(3) 0.032(2) -0.0049(18) 0.0145(15) -0.0045(16) C36 0.050(3) 0.028(3) 0.0230(18) 0.0062(16) 0.0092(19) -0.005(3) C36A 0.062(3) 0.028(2) 0.0272(15) 0.0049(15) 0.0189(18) 0.004(2) C37 0.0224(13) 0.084(2) 0.027(2) 0.0148(17) 0.0060(14) 0.0068(16) C37A 0.0221(12) 0.081(2) 0.029(2) 0.0152(17) 0.0049(14) 0.0072(13) C38 0.0243(14) 0.089(2) 0.027(2) 0.0116(18) 0.0070(16) 0.0088(14) C38A 0.0235(12) 0.0880(18) 0.029(2) 0.0129(18) 0.0073(15) 0.0099(12) C39 0.0224(10) 0.089(2) 0.027(2) 0.0088(19) 0.0104(13) 0.0082(15) C39A 0.0209(9) 0.0908(19) 0.032(2) 0.0114(19) 0.0105(13) 0.0062(13) C40 0.0229(11) 0.085(2) 0.028(2) 0.0116(17) 0.0089(12) 0.0033(17) C40A 0.0232(9) 0.086(2) 0.028(2) 0.0125(17) 0.0115(14) 0.0048(14) C41 0.052(2) 0.0573(17) 0.0337(18) -0.0075(17) -0.0048(16) -0.0167(19) C41A 0.0526(17) 0.0710(16) 0.0343(14) -0.0147(14) -0.0017(12) -0.0234(14) C42 0.062(2) 0.0572(19) 0.0416(19) -0.0071(17) -0.0102(17) -0.0181(18) C42A 0.0544(19) 0.0703(18) 0.0321(12) -0.0190(12) 0.0154(13) -0.0338(15) C43 0.044(2) 0.0559(13) 0.0306(18) -0.0068(15) 0.0045(17) -0.0196(18) C43A 0.055(2) 0.0594(13) 0.0354(16) -0.0181(12) 0.0181(15) -0.0271(15) C44 0.043(2) 0.0560(14) 0.0275(16) -0.0062(14) 0.0090(15) -0.0220(19) C44A 0.046(2) 0.0525(12) 0.0304(13) -0.0115(11) 0.0154(14) -0.0214(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 Na1 O2 2.190(5) . ? Na1 O1 2.314(5) . ? Na1 O1A 2.336(5) . ? Na1 N1 2.3788(18) . ? Na1 N2 2.3923(15) . ? Na1 O2A 2.434(3) . ? Na1 C1 3.1263(18) . ? Na1 Na2 3.2758(10) . ? Na2 N2 2.4153(16) . ? Na2 N1 2.4549(16) . ? Na2 C4 2.6453(19) 3_766 ? Na2 C2 2.7020(18) . ? Na2 C1 2.7398(18) . ? Na2 C3 2.7922(19) 3_766 ? Na2 C5 2.9035(19) 3_766 ? O1 C37 1.432(7) . ? O1 C40 1.478(9) . ? O1A C37A 1.456(7) . ? O1A C40A 1.503(8) . ? O2 C44 1.441(7) . ? O2 C41 1.447(7) . ? O2A C41A 1.438(5) . ? O2A C44A 1.439(5) . ? N1 C1 1.372(2) . ? N1 C7 1.414(6) . ? N1 C7A 1.426(12) . ? N2 C2 1.377(2) . ? N2 C22 1.411(10) . ? N2 C22A 1.411(8) . ? C1 C6 1.404(2) . ? C1 C2 1.463(2) . ? C2 C3 1.408(2) . ? C3 C4 1.407(3) . ? C3 Na2 2.7922(19) 3_766 ? C3 H3 0.9500 . ? C4 C5 1.380(3) . ? C4 Na2 2.6453(19) 3_766 ? C4 H4 0.9500 . ? C5 C6 1.400(3) . ? C5 Na2 2.9034(19) 3_766 ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.407(6) . ? C7 C12 1.426(6) . ? C7A C12A 1.420(13) . ? C7A C8A 1.425(12) . ? C8 C9 1.399(6) . ? C8 C13 1.517(5) . ? C8A C9A 1.414(13) . ? C8A C13 1.527(9) . ? C9 C10 1.383(5) . ? C9 H9 0.9500 . ? C9A C10A 1.385(10) . ? C9A H9A 0.9500 . ? C10 C11 1.393(4) . ? C10 C16 1.529(5) . ? C10A C11A 1.385(9) . ? C10A C16A 1.517(10) . ? C11 C12 1.396(4) . ? C11 H11 0.9500 . ? C11A C12A 1.388(9) . ? C11A H11A 0.9500 . ? C12 C19 1.516(4) . ? C12A C19A 1.529(8) . ? C13 C15 1.530(2) . ? C13 C14 1.537(3) . ? C13 H13 1.0000 . ? C13 H13A 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.530(5) . ? C16 C18 1.544(7) . ? C16 H16 1.0000 . ? C16A C18A 1.539(12) . ? C16A C17A 1.543(9) . ? C16A H16A 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C17A H17D 0.9800 . ? C17A H17E 0.9800 . ? C17A H17F 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C18A H18D 0.9800 . ? C18A H18E 0.9800 . ? C18A H18F 0.9800 . ? C19 C20 1.526(5) . ? C19 C21 1.540(5) . ? C19 H19 1.0000 . ? C19A C20A 1.524(9) . ? C19A C21A 1.527(9) . ? C19A H19A 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C20A H20D 0.9800 . ? C20A H20E 0.9800 . ? C20A H20F 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C21A H21D 0.9800 . ? C21A H21E 0.9800 . ? C21A H21F 0.9800 . ? C22 C27 1.432(10) . ? C22 C23 1.434(10) . ? C22A C23A 1.410(8) . ? C22A C27A 1.426(8) . ? C23 C24 1.414(10) . ? C23 C28 1.534(7) . ? C23A C24A 1.396(8) . ? C23A C28 1.519(6) . ? C24 C25 1.399(7) . ? C24 H24 0.9500 . ? C24A C25A 1.384(5) . ? C24A H24A 0.9500 . ? C25 C26 1.379(6) . ? C25 C31 1.522(6) . ? C25A C26A 1.393(5) . ? C25A C31A 1.527(4) . ? C26 C27 1.399(6) . ? C26 H26 0.9500 . ? C26A C27A 1.399(5) . ? C26A H26A 0.9500 . ? C27 C34 1.517(6) . ? C27A C34A 1.518(5) . ? C28 C29 1.532(3) . ? C28 C30 1.533(3) . ? C28 H28 1.0000 . ? C28 H28A 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.516(6) . ? C31 C33 1.522(6) . ? C31 H31 1.0000 . ? C31A C33A 1.526(5) . ? C31A C32A 1.532(5) . ? C31A H31A 1.0000 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C32A H32D 0.9800 . ? C32A H32E 0.9800 . ? C32A H32F 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C33A H33D 0.9800 . ? C33A H33E 0.9800 . ? C33A H33F 0.9800 . ? C34 C36 1.521(6) . ? C34 C35 1.531(6) . ? C34 H34 1.0000 . ? C34A C36A 1.533(5) . ? C34A C35A 1.536(5) . ? C34A H34A 1.0000 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C35A H35D 0.9800 . ? C35A H35E 0.9800 . ? C35A H35F 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C36A H36D 0.9800 . ? C36A H36E 0.9800 . ? C36A H36F 0.9800 . ? C37 C38 1.517(8) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C37A C38A 1.524(7) . ? C37A H37C 0.9900 . ? C37A H37D 0.9900 . ? C38 C39 1.527(10) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C38A C39A 1.531(10) . ? C38A H38C 0.9900 . ? C38A H38D 0.9900 . ? C39 C40 1.531(9) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C39A C40A 1.517(8) . ? C39A H39C 0.9900 . ? C39A H39D 0.9900 . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C40A H40C 0.9900 . ? C40A H40D 0.9900 . ? C41 C42 1.477(8) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C41A C42A 1.495(7) . ? C41A H41C 0.9900 . ? C41A H41D 0.9900 . ? C42 C43 1.513(8) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C42A C43A 1.542(6) . ? C42A H42C 0.9900 . ? C42A H42D 0.9900 . ? C43 C44 1.528(8) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C43A C44A 1.522(6) . ? C43A H43C 0.9900 . ? C43A H43D 0.9900 . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C44A H44C 0.9900 . ? C44A H44D 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Na1 O1 77.1(3) . . ? O2 Na1 O1A 85.3(3) . . ? O1 Na1 O1A 9.2(2) . . ? O2 Na1 N1 179.4(2) . . ? O1 Na1 N1 102.4(2) . . ? O1A Na1 N1 94.3(2) . . ? O2 Na1 N2 111.35(19) . . ? O1 Na1 N2 154.2(2) . . ? O1A Na1 N2 146.7(2) . . ? N1 Na1 N2 69.22(5) . . ? O2 Na1 O2A 6.7(3) . . ? O1 Na1 O2A 83.2(2) . . ? O1A Na1 O2A 91.1(2) . . ? N1 Na1 O2A 173.89(12) . . ? N2 Na1 O2A 104.68(12) . . ? O2 Na1 C1 156.0(2) . . ? O1 Na1 C1 126.5(2) . . ? O1A Na1 C1 118.56(19) . . ? N1 Na1 C1 24.37(5) . . ? N2 Na1 C1 49.94(5) . . ? O2A Na1 C1 150.29(13) . . ? O2 Na1 Na2 132.1(2) . . ? O1 Na1 Na2 108.4(2) . . ? O1A Na1 Na2 99.9(2) . . ? N1 Na1 Na2 48.32(4) . . ? N2 Na1 Na2 47.34(4) . . ? O2A Na1 Na2 127.79(12) . . ? C1 Na1 Na2 50.61(3) . . ? N2 Na2 N1 67.61(5) . . ? N2 Na2 C4 152.73(6) . 3_766 ? N1 Na2 C4 139.33(6) . 3_766 ? N2 Na2 C2 30.57(5) . . ? N1 Na2 C2 55.63(5) . . ? C4 Na2 C2 148.79(6) 3_766 . ? N2 Na2 C1 55.64(5) . . ? N1 Na2 C1 30.00(5) . . ? C4 Na2 C1 142.72(6) 3_766 . ? C2 Na2 C1 31.18(5) . . ? N2 Na2 C3 150.25(6) . 3_766 ? N1 Na2 C3 117.91(6) . 3_766 ? C4 Na2 C3 29.83(5) 3_766 3_766 ? C2 Na2 C3 125.27(6) . 3_766 ? C1 Na2 C3 112.99(6) . 3_766 ? N2 Na2 C5 124.48(6) . 3_766 ? N1 Na2 C5 167.32(6) . 3_766 ? C4 Na2 C5 28.32(6) 3_766 3_766 ? C2 Na2 C5 132.09(6) . 3_766 ? C1 Na2 C5 150.61(6) . 3_766 ? C3 Na2 C5 49.97(5) 3_766 3_766 ? N2 Na2 Na1 46.75(4) . . ? N1 Na2 Na1 46.36(4) . . ? C4 Na2 Na1 148.58(5) 3_766 . ? C2 Na2 Na1 62.49(4) . . ? C1 Na2 Na1 61.87(4) . . ? C3 Na2 Na1 158.37(5) 3_766 . ? C5 Na2 Na1 143.55(5) 3_766 . ? N2 Na2 Na2 82.30(4) . 3_766 ? N1 Na2 Na2 88.64(4) . 3_766 ? C4 Na2 Na2 92.66(5) 3_766 3_766 ? C2 Na2 Na2 57.10(4) . 3_766 ? C1 Na2 Na2 61.20(4) . 3_766 ? C3 Na2 Na2 69.08(4) 3_766 3_766 ? C5 Na2 Na2 89.41(4) 3_766 3_766 ? Na1 Na2 Na2 118.55(3) . 3_766 ? C37 O1 C40 106.2(5) . . ? C37 O1 Na1 132.2(4) . . ? C40 O1 Na1 116.7(4) . . ? C37A O1A C40A 111.2(4) . . ? C37A O1A Na1 134.6(4) . . ? C40A O1A Na1 113.1(4) . . ? C44 O2 C41 109.3(5) . . ? C44 O2 Na1 128.2(4) . . ? C41 O2 Na1 122.1(4) . . ? C41A O2A C44A 104.0(3) . . ? C41A O2A Na1 124.6(3) . . ? C44A O2A Na1 130.6(3) . . ? C1 N1 C7 116.8(5) . . ? C1 N1 C7A 119.1(10) . . ? C1 N1 Na1 109.98(11) . . ? C7 N1 Na1 113.4(5) . . ? C7A N1 Na1 111.3(10) . . ? C1 N1 Na2 86.56(10) . . ? C7 N1 Na2 139.4(3) . . ? C7A N1 Na2 138.9(6) . . ? Na1 N1 Na2 85.31(6) . . ? C2 N2 C22 119.9(11) . . ? C2 N2 C22A 117.3(8) . . ? C2 N2 Na1 109.83(10) . . ? C22 N2 Na1 111.4(14) . . ? C22A N2 Na1 112.2(10) . . ? C2 N2 Na2 86.30(10) . . ? C22 N2 Na2 137.6(5) . . ? C22A N2 Na2 139.9(4) . . ? Na1 N2 Na2 85.90(5) . . ? N1 C1 C6 125.43(16) . . ? N1 C1 C2 116.85(15) . . ? C6 C1 C2 117.71(15) . . ? N1 C1 Na2 63.43(9) . . ? C6 C1 Na2 136.39(12) . . ? C2 C1 Na2 72.98(9) . . ? N1 C1 Na1 45.65(9) . . ? C6 C1 Na1 153.11(11) . . ? C2 C1 Na1 77.00(9) . . ? Na2 C1 Na1 67.52(4) . . ? N2 C2 C3 125.24(15) . . ? N2 C2 C1 117.07(14) . . ? C3 C2 C1 117.69(15) . . ? N2 C2 Na2 63.13(9) . . ? C3 C2 Na2 132.52(12) . . ? C1 C2 Na2 75.84(9) . . ? C4 C3 C2 122.44(16) . . ? C4 C3 Na2 69.29(10) . 3_766 ? C2 C3 Na2 94.46(11) . 3_766 ? C4 C3 H3 118.8 . . ? C2 C3 H3 118.8 . . ? Na2 C3 H3 106.6 3_766 . ? C5 C4 C3 119.53(16) . . ? C5 C4 Na2 86.28(11) . 3_766 ? C3 C4 Na2 80.88(10) . 3_766 ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? Na2 C4 H4 102.8 3_766 . ? C4 C5 C6 119.88(16) . . ? C4 C5 Na2 65.39(10) . 3_766 ? C6 C5 Na2 91.76(11) . 3_766 ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? Na2 C5 H5 112.6 3_766 . ? C5 C6 C1 122.66(17) . . ? C5 C6 H6 118.7 . . ? C1 C6 H6 118.7 . . ? C8 C7 N1 120.7(6) . . ? C8 C7 C12 116.1(4) . . ? N1 C7 C12 123.1(5) . . ? C12A C7A C8A 122.1(10) . . ? C12A C7A N1 114.8(11) . . ? C8A C7A N1 121.8(12) . . ? C9 C8 C7 121.4(5) . . ? C9 C8 C13 116.2(5) . . ? C7 C8 C13 122.4(6) . . ? C9A C8A C7A 115.5(11) . . ? C9A C8A C13 123.6(10) . . ? C7A C8A C13 120.2(12) . . ? C10 C9 C8 122.0(5) . . ? C10 C9 H9 119.0 . . ? C8 C9 H9 119.0 . . ? C10A C9A C8A 123.8(13) . . ? C10A C9A H9A 118.1 . . ? C8A C9A H9A 118.1 . . ? C9 C10 C11 117.3(4) . . ? C9 C10 C16 122.6(4) . . ? C11 C10 C16 120.0(4) . . ? C9A C10A C11A 117.8(10) . . ? C9A C10A C16A 119.6(10) . . ? C11A C10A C16A 122.3(8) . . ? C10 C11 C12 121.9(3) . . ? C10 C11 H11 119.0 . . ? C12 C11 H11 119.0 . . ? C10A C11A C12A 123.0(8) . . ? C10A C11A H11A 118.5 . . ? C12A C11A H11A 118.5 . . ? C11 C12 C7 120.9(4) . . ? C11 C12 C19 119.2(3) . . ? C7 C12 C19 119.6(4) . . ? C11A C12A C7A 117.6(8) . . ? C11A C12A C19A 119.2(7) . . ? C7A C12A C19A 123.2(8) . . ? C8 C13 C15 112.6(3) . . ? C8A C13 C15 111.0(6) . . ? C8 C13 C14 111.5(3) . . ? C8A C13 C14 111.8(6) . . ? C15 C13 C14 109.53(16) . . ? C8 C13 H13 107.7 . . ? C8A C13 H13 109.1 . . ? C15 C13 H13 107.7 . . ? C14 C13 H13 107.7 . . ? C8 C13 H13A 106.7 . . ? C8A C13 H13A 108.1 . . ? C15 C13 H13A 108.1 . . ? C14 C13 H13A 108.1 . . ? 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 . . ? C10 C16 C17 109.6(3) . . ? C10 C16 C18 112.1(5) . . ? C17 C16 C18 107.4(8) . . ? C10 C16 H16 109.2 . . ? C17 C16 H16 109.2 . . ? C18 C16 H16 109.2 . . ? C10A C16A C18A 112.9(10) . . ? C10A C16A C17A 111.3(8) . . ? C18A C16A C17A 117.4(18) . . ? C10A C16A H16A 104.6 . . ? C18A C16A H16A 104.6 . . ? C17A C16A H16A 104.6 . . ? C16A C17A H17D 109.5 . . ? C16A C17A H17E 109.5 . . ? H17D C17A H17E 109.5 . . ? C16A C17A H17F 109.5 . . ? H17D C17A H17F 109.5 . . ? H17E C17A H17F 109.5 . . ? C16A C18A H18D 109.5 . . ? C16A C18A H18E 109.5 . . ? H18D C18A H18E 109.5 . . ? C16A C18A H18F 109.5 . . ? H18D C18A H18F 109.5 . . ? H18E C18A H18F 109.5 . . ? C12 C19 C20 110.0(3) . . ? C12 C19 C21 113.4(3) . . ? C20 C19 C21 111.3(3) . . ? C12 C19 H19 107.3 . . ? C20 C19 H19 107.3 . . ? C21 C19 H19 107.3 . . ? C20A C19A C21A 114.6(8) . . ? C20A C19A C12A 110.2(6) . . ? C21A C19A C12A 112.2(6) . . ? C20A C19A H19A 106.4 . . ? C21A C19A H19A 106.4 . . ? C12A C19A H19A 106.4 . . ? C19A C20A H20D 109.5 . . ? C19A C20A H20E 109.5 . . ? H20D C20A H20E 109.5 . . ? C19A C20A H20F 109.5 . . ? H20D C20A H20F 109.5 . . ? H20E C20A H20F 109.5 . . ? C19A C21A H21D 109.5 . . ? C19A C21A H21E 109.5 . . ? H21D C21A H21E 109.5 . . ? C19A C21A H21F 109.5 . . ? H21D C21A H21F 109.5 . . ? H21E C21A H21F 109.5 . . ? N2 C22 C27 114.3(8) . . ? N2 C22 C23 120.6(9) . . ? C27 C22 C23 123.2(9) . . ? C23A C22A N2 124.2(7) . . ? C23A C22A C27A 113.9(6) . . ? N2 C22A C27A 121.8(6) . . ? C24 C23 C22 113.8(7) . . ? C24 C23 C28 122.3(7) . . ? C22 C23 C28 123.6(9) . . ? C24A C23A C22A 124.2(6) . . ? C24A C23A C28 114.0(5) . . ? C22A C23A C28 121.7(7) . . ? C25 C24 C23 125.3(6) . . ? C25 C24 H24 117.3 . . ? C23 C24 H24 117.3 . . ? C25A C24A C23A 120.6(4) . . ? C25A C24A H24A 119.7 . . ? C23A C24A H24A 119.7 . . ? C26 C25 C24 117.2(5) . . ? C26 C25 C31 120.8(4) . . ? C24 C25 C31 122.0(5) . . ? C24A C25A C26A 117.3(3) . . ? C24A C25A C31A 121.9(3) . . ? C26A C25A C31A 120.8(3) . . ? C25 C26 C27 123.6(5) . . ? C25 C26 H26 118.2 . . ? C27 C26 H26 118.2 . . ? C25A C26A C27A 122.4(3) . . ? C25A C26A H26A 118.8 . . ? C27A C26A H26A 118.8 . . ? C26 C27 C22 116.6(6) . . ? C26 C27 C34 119.5(5) . . ? C22 C27 C34 123.9(6) . . ? C26A C27A C22A 121.6(4) . . ? C26A C27A C34A 120.8(4) . . ? C22A C27A C34A 117.5(5) . . ? C23A C28 C29 112.5(4) . . ? C23A C28 C30 110.8(3) . . ? C29 C28 C30 109.89(16) . . ? C29 C28 C23 108.9(4) . . ? C30 C28 C23 114.5(4) . . ? C23A C28 H28 107.9 . . ? C29 C28 H28 107.8 . . ? C30 C28 H28 107.8 . . ? C23 C28 H28 107.8 . . ? C23A C28 H28A 107.8 . . ? C29 C28 H28A 107.8 . . ? C30 C28 H28A 107.8 . . ? C23 C28 H28A 107.7 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 C25 113.1(4) . . ? C32 C31 C33 111.5(4) . . ? C25 C31 C33 111.1(4) . . ? C32 C31 H31 106.9 . . ? C25 C31 H31 106.9 . . ? C33 C31 H31 106.9 . . ? C33A C31A C25A 111.0(3) . . ? C33A C31A C32A 110.9(3) . . ? C25A C31A C32A 111.3(3) . . ? C33A C31A H31A 107.8 . . ? C25A C31A H31A 107.8 . . ? C32A C31A H31A 107.8 . . ? C31A C32A H32D 109.5 . . ? C31A C32A H32E 109.5 . . ? H32D C32A H32E 109.5 . . ? C31A C32A H32F 109.5 . . ? H32D C32A H32F 109.5 . . ? H32E C32A H32F 109.5 . . ? C31A C33A H33D 109.5 . . ? C31A C33A H33E 109.5 . . ? H33D C33A H33E 109.5 . . ? C31A C33A H33F 109.5 . . ? H33D C33A H33F 109.5 . . ? H33E C33A H33F 109.5 . . ? C27 C34 C36 114.7(5) . . ? C27 C34 C35 111.7(4) . . ? C36 C34 C35 109.8(5) . . ? C27 C34 H34 106.7 . . ? C36 C34 H34 106.7 . . ? C35 C34 H34 106.7 . . ? C27A C34A C36A 114.6(3) . . ? C27A C34A C35A 109.9(3) . . ? C36A C34A C35A 109.8(4) . . ? C27A C34A H34A 107.4 . . ? C36A C34A H34A 107.4 . . ? C35A C34A H34A 107.4 . . ? C34A C35A H35D 109.5 . . ? C34A C35A H35E 109.5 . . ? H35D C35A H35E 109.5 . . ? C34A C35A H35F 109.5 . . ? H35D C35A H35F 109.5 . . ? H35E C35A H35F 109.5 . . ? C34A C36A H36D 109.5 . . ? C34A C36A H36E 109.5 . . ? H36D C36A H36E 109.5 . . ? C34A C36A H36F 109.5 . . ? H36D C36A H36F 109.5 . . ? H36E C36A H36F 109.5 . . ? O1 C37 C38 108.5(5) . . ? O1 C37 H37A 110.0 . . ? C38 C37 H37A 110.0 . . ? O1 C37 H37B 110.0 . . ? C38 C37 H37B 110.0 . . ? H37A C37 H37B 108.4 . . ? O1A C37A C38A 104.3(4) . . ? O1A C37A H37C 110.9 . . ? C38A C37A H37C 110.9 . . ? O1A C37A H37D 110.9 . . ? C38A C37A H37D 110.9 . . ? H37C C37A H37D 108.9 . . ? C37 C38 C39 102.4(6) . . ? C37 C38 H38A 111.3 . . ? C39 C38 H38A 111.3 . . ? C37 C38 H38B 111.3 . . ? C39 C38 H38B 111.3 . . ? H38A C38 H38B 109.2 . . ? C37A C38A C39A 103.3(5) . . ? C37A C38A H38C 111.1 . . ? C39A C38A H38C 111.1 . . ? C37A C38A H38D 111.1 . . ? C39A C38A H38D 111.1 . . ? H38C C38A H38D 109.1 . . ? C38 C39 C40 99.4(6) . . ? C38 C39 H39A 111.9 . . ? C40 C39 H39A 111.9 . . ? C38 C39 H39B 111.9 . . ? C40 C39 H39B 111.9 . . ? H39A C39 H39B 109.6 . . ? C40A C39A C38A 104.2(6) . . ? C40A C39A H39C 110.9 . . ? C38A C39A H39C 110.9 . . ? C40A C39A H39D 110.9 . . ? C38A C39A H39D 110.9 . . ? H39C C39A H39D 108.9 . . ? O1 C40 C39 103.4(5) . . ? O1 C40 H40A 111.1 . . ? C39 C40 H40A 111.1 . . ? O1 C40 H40B 111.1 . . ? C39 C40 H40B 111.1 . . ? H40A C40 H40B 109.1 . . ? O1A C40A C39A 103.4(5) . . ? O1A C40A H40C 111.1 . . ? C39A C40A H40C 111.1 . . ? O1A C40A H40D 111.1 . . ? C39A C40A H40D 111.1 . . ? H40C C40A H40D 109.0 . . ? O2 C41 C42 105.9(5) . . ? O2 C41 H41A 110.5 . . ? C42 C41 H41A 110.5 . . ? O2 C41 H41B 110.5 . . ? C42 C41 H41B 110.5 . . ? H41A C41 H41B 108.7 . . ? O2A C41A C42A 106.9(4) . . ? O2A C41A H41C 110.3 . . ? C42A C41A H41C 110.3 . . ? O2A C41A H41D 110.3 . . ? C42A C41A H41D 110.3 . . ? H41C C41A H41D 108.6 . . ? C41 C42 C43 104.8(5) . . ? C41 C42 H42A 110.8 . . ? C43 C42 H42A 110.8 . . ? C41 C42 H42B 110.8 . . ? C43 C42 H42B 110.8 . . ? H42A C42 H42B 108.9 . . ? C41A C42A C43A 103.7(3) . . ? C41A C42A H42C 111.0 . . ? C43A C42A H42C 111.0 . . ? C41A C42A H42D 111.0 . . ? C43A C42A H42D 111.0 . . ? H42C C42A H42D 109.0 . . ? C42 C43 C44 100.1(5) . . ? C42 C43 H43A 111.8 . . ? C44 C43 H43A 111.8 . . ? C42 C43 H43B 111.8 . . ? C44 C43 H43B 111.8 . . ? H43A C43 H43B 109.5 . . ? C44A C43A C42A 103.8(4) . . ? C44A C43A H43C 111.0 . . ? C42A C43A H43C 111.0 . . ? C44A C43A H43D 111.0 . . ? C42A C43A H43D 111.0 . . ? H43C C43A H43D 109.0 . . ? O2 C44 C43 103.8(5) . . ? O2 C44 H44A 111.0 . . ? C43 C44 H44A 111.0 . . ? O2 C44 H44B 111.0 . . ? C43 C44 H44B 111.0 . . ? H44A C44 H44B 109.0 . . ? O2A C44A C43A 107.4(4) . . ? O2A C44A H44C 110.2 . . ? C43A C44A H44C 110.2 . . ? O2A C44A H44D 110.2 . . ? C43A C44A H44D 110.2 . . ? H44C C44A H44D 108.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Na1 Na2 N2 80.4(3) . . . . ? O1 Na1 Na2 N2 169.6(2) . . . . ? O1A Na1 Na2 N2 173.08(15) . . . . ? N1 Na1 Na2 N2 -100.04(7) . . . . ? O2A Na1 Na2 N2 73.82(17) . . . . ? C1 Na1 Na2 N2 -67.93(6) . . . . ? O2 Na1 Na2 N1 -179.5(3) . . . . ? O1 Na1 Na2 N1 -90.4(2) . . . . ? O1A Na1 Na2 N1 -86.87(15) . . . . ? N2 Na1 Na2 N1 100.04(7) . . . . ? O2A Na1 Na2 N1 173.87(18) . . . . ? C1 Na1 Na2 N1 32.11(6) . . . . ? O2 Na1 Na2 C4 -62.8(3) . . . 3_766 ? O1 Na1 Na2 C4 26.4(2) . . . 3_766 ? O1A Na1 Na2 C4 29.85(18) . . . 3_766 ? N1 Na1 Na2 C4 116.72(11) . . . 3_766 ? N2 Na1 Na2 C4 -143.24(11) . . . 3_766 ? O2A Na1 Na2 C4 -69.4(2) . . . 3_766 ? C1 Na1 Na2 C4 148.83(11) . . . 3_766 ? O2 Na1 Na2 C2 113.0(3) . . . . ? O1 Na1 Na2 C2 -157.9(2) . . . . ? O1A Na1 Na2 C2 -154.36(15) . . . . ? N1 Na1 Na2 C2 -67.48(6) . . . . ? N2 Na1 Na2 C2 32.56(6) . . . . ? O2A Na1 Na2 C2 106.38(17) . . . . ? C1 Na1 Na2 C2 -35.38(5) . . . . ? O2 Na1 Na2 C1 148.4(3) . . . . ? O1 Na1 Na2 C1 -122.5(2) . . . . ? O1A Na1 Na2 C1 -118.98(15) . . . . ? N1 Na1 Na2 C1 -32.11(6) . . . . ? N2 Na1 Na2 C1 67.93(6) . . . . ? O2A Na1 Na2 C1 141.76(17) . . . . ? O2 Na1 Na2 C3 -130.1(3) . . . 3_766 ? O1 Na1 Na2 C3 -40.9(2) . . . 3_766 ? O1A Na1 Na2 C3 -37.43(19) . . . 3_766 ? N1 Na1 Na2 C3 49.44(13) . . . 3_766 ? N2 Na1 Na2 C3 149.48(13) . . . 3_766 ? O2A Na1 Na2 C3 -136.7(2) . . . 3_766 ? C1 Na1 Na2 C3 81.55(13) . . . 3_766 ? O2 Na1 Na2 C5 -11.5(3) . . . 3_766 ? O1 Na1 Na2 C5 77.6(2) . . . 3_766 ? O1A Na1 Na2 C5 81.10(16) . . . 3_766 ? N1 Na1 Na2 C5 167.97(10) . . . 3_766 ? N2 Na1 Na2 C5 -91.98(9) . . . 3_766 ? O2A Na1 Na2 C5 -18.16(19) . . . 3_766 ? C1 Na1 Na2 C5 -159.92(9) . . . 3_766 ? O2 Na1 Na2 Na2 124.3(3) . . . 3_766 ? O1 Na1 Na2 Na2 -146.6(2) . . . 3_766 ? O1A Na1 Na2 Na2 -143.07(14) . . . 3_766 ? N1 Na1 Na2 Na2 -56.20(6) . . . 3_766 ? N2 Na1 Na2 Na2 43.84(6) . . . 3_766 ? O2A Na1 Na2 Na2 117.66(17) . . . 3_766 ? C1 Na1 Na2 Na2 -24.09(5) . . . 3_766 ? O2 Na1 O1 C37 -131.4(7) . . . . ? O1A Na1 O1 C37 76.0(18) . . . . ? N1 Na1 O1 C37 48.2(6) . . . . ? N2 Na1 O1 C37 115.9(6) . . . . ? O2A Na1 O1 C37 -134.3(6) . . . . ? C1 Na1 O1 C37 43.9(6) . . . . ? Na2 Na1 O1 C37 98.1(6) . . . . ? O2 Na1 O1 C40 77.1(10) . . . . ? O1A Na1 O1 C40 -75.5(19) . . . . ? N1 Na1 O1 C40 -103.2(10) . . . . ? N2 Na1 O1 C40 -35.6(14) . . . . ? O2A Na1 O1 C40 74.3(10) . . . . ? C1 Na1 O1 C40 -107.5(9) . . . . ? Na2 Na1 O1 C40 -53.4(10) . . . . ? O2 Na1 O1A C37A -126.6(5) . . . . ? O1 Na1 O1A C37A -100(2) . . . . ? N1 Na1 O1A C37A 53.0(5) . . . . ? N2 Na1 O1A C37A 110.7(5) . . . . ? O2A Na1 O1A C37A -129.9(5) . . . . ? C1 Na1 O1A C37A 51.0(5) . . . . ? Na2 Na1 O1A C37A 101.4(5) . . . . ? O2 Na1 O1A C40A 40.4(8) . . . . ? O1 Na1 O1A C40A 67.1(17) . . . . ? N1 Na1 O1A C40A -140.0(8) . . . . ? N2 Na1 O1A C40A -82.3(9) . . . . ? O2A Na1 O1A C40A 37.2(8) . . . . ? C1 Na1 O1A C40A -141.9(7) . . . . ? Na2 Na1 O1A C40A -91.6(8) . . . . ? O1 Na1 O2 C44 -142.0(9) . . . . ? O1A Na1 O2 C44 -137.8(9) . . . . ? N2 Na1 O2 C44 12.4(9) . . . . ? O2A Na1 O2 C44 13(3) . . . . ? C1 Na1 O2 C44 47.2(13) . . . . ? Na2 Na1 O2 C44 -38.7(10) . . . . ? O1 Na1 O2 C41 45.8(7) . . . . ? O1A Na1 O2 C41 50.0(7) . . . . ? N2 Na1 O2 C41 -159.8(7) . . . . ? O2A Na1 O2 C41 -159(4) . . . . ? C1 Na1 O2 C41 -125.0(6) . . . . ? Na2 Na1 O2 C41 149.1(6) . . . . ? O2 Na1 O2A C41A 23(3) . . . . ? O1 Na1 O2A C41A 47.1(5) . . . . ? O1A Na1 O2A C41A 51.7(5) . . . . ? N2 Na1 O2A C41A -158.0(4) . . . . ? C1 Na1 O2A C41A -130.0(4) . . . . ? Na2 Na1 O2A C41A 155.2(4) . . . . ? O2 Na1 O2A C44A -169(4) . . . . ? O1 Na1 O2A C44A -144.5(5) . . . . ? O1A Na1 O2A C44A -139.9(5) . . . . ? N2 Na1 O2A C44A 10.4(5) . . . . ? C1 Na1 O2A C44A 38.4(7) . . . . ? Na2 Na1 O2A C44A -36.5(6) . . . . ? O1 Na1 N1 C1 -171.6(2) . . . . ? O1A Na1 N1 C1 -175.9(2) . . . . ? N2 Na1 N1 C1 33.85(11) . . . . ? Na2 Na1 N1 C1 84.62(11) . . . . ? O1 Na1 N1 C7 -38.9(4) . . . . ? O1A Na1 N1 C7 -43.1(4) . . . . ? N2 Na1 N1 C7 166.6(4) . . . . ? C1 Na1 N1 C7 132.8(4) . . . . ? Na2 Na1 N1 C7 -142.6(4) . . . . ? O1 Na1 N1 C7A -37.5(8) . . . . ? O1A Na1 N1 C7A -41.8(8) . . . . ? N2 Na1 N1 C7A 168.0(8) . . . . ? C1 Na1 N1 C7A 134.1(8) . . . . ? Na2 Na1 N1 C7A -141.3(8) . . . . ? O1 Na1 N1 Na2 103.75(18) . . . . ? O1A Na1 N1 Na2 99.48(17) . . . . ? N2 Na1 N1 Na2 -50.76(5) . . . . ? C1 Na1 N1 Na2 -84.62(11) . . . . ? N2 Na2 N1 C1 -59.52(10) . . . . ? C4 Na2 N1 C1 115.21(11) 3_766 . . . ? C2 Na2 N1 C1 -27.34(9) . . . . ? C3 Na2 N1 C1 88.09(11) 3_766 . . . ? C5 Na2 N1 C1 103.9(3) 3_766 . . . ? Na1 Na2 N1 C1 -110.39(11) . . . . ? Na2 Na2 N1 C1 22.72(10) 3_766 . . . ? N2 Na2 N1 C7 171.9(7) . . . . ? C4 Na2 N1 C7 -13.3(8) 3_766 . . . ? C2 Na2 N1 C7 -155.9(7) . . . . ? C1 Na2 N1 C7 -128.5(8) . . . . ? C3 Na2 N1 C7 -40.5(7) 3_766 . . . ? C5 Na2 N1 C7 -24.6(8) 3_766 . . . ? Na1 Na2 N1 C7 121.1(7) . . . . ? Na2 Na2 N1 C7 -105.8(7) 3_766 . . . ? N2 Na2 N1 C7A 168.3(17) . . . . ? C4 Na2 N1 C7A -17.0(17) 3_766 . . . ? C2 Na2 N1 C7A -159.6(17) . . . . ? C1 Na2 N1 C7A -132.2(17) . . . . ? C3 Na2 N1 C7A -44.1(17) 3_766 . . . ? C5 Na2 N1 C7A -28.3(17) 3_766 . . . ? Na1 Na2 N1 C7A 117.4(17) . . . . ? Na2 Na2 N1 C7A -109.5(17) 3_766 . . . ? N2 Na2 N1 Na1 50.87(5) . . . . ? C4 Na2 N1 Na1 -134.40(8) 3_766 . . . ? C2 Na2 N1 Na1 83.05(6) . . . . ? C1 Na2 N1 Na1 110.39(11) . . . . ? C3 Na2 N1 Na1 -161.53(5) 3_766 . . . ? C5 Na2 N1 Na1 -145.7(2) 3_766 . . . ? Na2 Na2 N1 Na1 133.10(4) 3_766 . . . ? O2 Na1 N2 C2 147.2(3) . . . . ? O1 Na1 N2 C2 -107.8(5) . . . . ? O1A Na1 N2 C2 -97.0(3) . . . . ? N1 Na1 N2 C2 -32.70(11) . . . . ? O2A Na1 N2 C2 147.11(18) . . . . ? C1 Na1 N2 C2 -15.22(10) . . . . ? Na2 Na1 N2 C2 -84.57(11) . . . . ? O2 Na1 N2 C22 11.9(6) . . . . ? O1 Na1 N2 C22 116.9(7) . . . . ? O1A Na1 N2 C22 127.6(6) . . . . ? N1 Na1 N2 C22 -168.0(6) . . . . ? O2A Na1 N2 C22 11.8(6) . . . . ? C1 Na1 N2 C22 -150.5(6) . . . . ? Na2 Na1 N2 C22 140.1(6) . . . . ? O2 Na1 N2 C22A 14.8(5) . . . . ? O1 Na1 N2 C22A 119.8(7) . . . . ? O1A Na1 N2 C22A 130.5(5) . . . . ? N1 Na1 N2 C22A -165.1(4) . . . . ? O2A Na1 N2 C22A 14.7(5) . . . . ? C1 Na1 N2 C22A -147.6(4) . . . . ? Na2 Na1 N2 C22A 143.0(4) . . . . ? O2 Na1 N2 Na2 -128.3(3) . . . . ? O1 Na1 N2 Na2 -23.2(5) . . . . ? O1A Na1 N2 Na2 -12.5(3) . . . . ? N1 Na1 N2 Na2 51.87(5) . . . . ? O2A Na1 N2 Na2 -128.32(15) . . . . ? C1 Na1 N2 Na2 69.35(6) . . . . ? N1 Na2 N2 C2 59.79(9) . . . . ? C4 Na2 N2 C2 -112.70(14) 3_766 . . . ? C1 Na2 N2 C2 28.32(8) . . . . ? C3 Na2 N2 C2 -47.63(15) 3_766 . . . ? C5 Na2 N2 C2 -115.86(10) 3_766 . . . ? Na1 Na2 N2 C2 110.21(10) . . . . ? Na2 Na2 N2 C2 -31.91(8) 3_766 . . . ? N1 Na2 N2 C22 -168(2) . . . . ? C4 Na2 N2 C22 19(2) 3_766 . . . ? C2 Na2 N2 C22 132(2) . . . . ? C1 Na2 N2 C22 160(2) . . . . ? C3 Na2 N2 C22 84(2) 3_766 . . . ? C5 Na2 N2 C22 16(2) 3_766 . . . ? Na1 Na2 N2 C22 -118(2) . . . . ? Na2 Na2 N2 C22 100(2) 3_766 . . . ? N1 Na2 N2 C22A -170.6(16) . . . . ? C4 Na2 N2 C22A 16.9(16) 3_766 . . . ? C2 Na2 N2 C22A 129.6(16) . . . . ? C1 Na2 N2 C22A 157.9(16) . . . . ? C3 Na2 N2 C22A 82.0(16) 3_766 . . . ? C5 Na2 N2 C22A 13.7(16) 3_766 . . . ? Na1 Na2 N2 C22A -120.2(16) . . . . ? Na2 Na2 N2 C22A 97.7(16) 3_766 . . . ? N1 Na2 N2 Na1 -50.42(5) . . . . ? C4 Na2 N2 Na1 137.09(12) 3_766 . . . ? C2 Na2 N2 Na1 -110.21(10) . . . . ? C1 Na2 N2 Na1 -81.89(6) . . . . ? C3 Na2 N2 Na1 -157.84(10) 3_766 . . . ? C5 Na2 N2 Na1 133.93(6) 3_766 . . . ? Na2 Na2 N2 Na1 -142.13(4) 3_766 . . . ? C7 N1 C1 C6 15.6(4) . . . . ? C7A N1 C1 C6 16.6(8) . . . . ? Na1 N1 C1 C6 146.63(15) . . . . ? Na2 N1 C1 C6 -129.62(16) . . . . ? C7 N1 C1 C2 -163.1(4) . . . . ? C7A N1 C1 C2 -162.1(8) . . . . ? Na1 N1 C1 C2 -32.05(17) . . . . ? Na2 N1 C1 C2 51.69(14) . . . . ? C7 N1 C1 Na2 145.2(4) . . . . ? C7A N1 C1 Na2 146.2(8) . . . . ? Na1 N1 C1 Na2 -83.75(8) . . . . ? C7 N1 C1 Na1 -131.0(4) . . . . ? C7A N1 C1 Na1 -130.1(8) . . . . ? Na2 N1 C1 Na1 83.75(8) . . . . ? N2 Na2 C1 N1 105.15(11) . . . . ? C4 Na2 C1 N1 -103.26(13) 3_766 . . . ? C2 Na2 C1 N1 132.93(15) . . . . ? C3 Na2 C1 N1 -106.38(11) 3_766 . . . ? C5 Na2 C1 N1 -154.27(13) 3_766 . . . ? Na1 Na2 C1 N1 50.29(9) . . . . ? Na2 Na2 C1 N1 -153.86(11) 3_766 . . . ? N2 Na2 C1 C6 -140.35(19) . . . . ? N1 Na2 C1 C6 114.5(2) . . . . ? C4 Na2 C1 C6 11.2(2) 3_766 . . . ? C2 Na2 C1 C6 -112.6(2) . . . . ? C3 Na2 C1 C6 8.12(19) 3_766 . . . ? C5 Na2 C1 C6 -39.8(2) 3_766 . . . ? Na1 Na2 C1 C6 164.79(18) . . . . ? Na2 Na2 C1 C6 -39.36(16) 3_766 . . . ? N2 Na2 C1 C2 -27.78(9) . . . . ? N1 Na2 C1 C2 -132.93(15) . . . . ? C4 Na2 C1 C2 123.81(12) 3_766 . . . ? C3 Na2 C1 C2 120.69(9) 3_766 . . . ? C5 Na2 C1 C2 72.79(15) 3_766 . . . ? Na1 Na2 C1 C2 -82.64(9) . . . . ? Na2 Na2 C1 C2 73.20(9) 3_766 . . . ? N2 Na2 C1 Na1 54.86(5) . . . . ? N1 Na2 C1 Na1 -50.29(9) . . . . ? C4 Na2 C1 Na1 -153.55(9) 3_766 . . . ? C2 Na2 C1 Na1 82.64(9) . . . . ? C3 Na2 C1 Na1 -156.67(5) 3_766 . . . ? C5 Na2 C1 Na1 155.44(12) 3_766 . . . ? Na2 Na2 C1 Na1 155.85(5) 3_766 . . . ? O2 Na1 C1 N1 179.0(6) . . . . ? O1 Na1 C1 N1 10.2(3) . . . . ? O1A Na1 C1 N1 4.7(2) . . . . ? N2 Na1 C1 N1 -137.12(13) . . . . ? O2A Na1 C1 N1 -173.4(3) . . . . ? Na2 Na1 C1 N1 -74.19(11) . . . . ? O2 Na1 C1 C6 96.7(7) . . . . ? O1 Na1 C1 C6 -72.1(4) . . . . ? O1A Na1 C1 C6 -77.6(3) . . . . ? N1 Na1 C1 C6 -82.2(3) . . . . ? N2 Na1 C1 C6 140.6(3) . . . . ? O2A Na1 C1 C6 104.3(4) . . . . ? Na2 Na1 C1 C6 -156.4(3) . . . . ? O2 Na1 C1 C2 -30.1(6) . . . . ? O1 Na1 C1 C2 161.1(2) . . . . ? O1A Na1 C1 C2 155.6(2) . . . . ? N1 Na1 C1 C2 150.92(16) . . . . ? N2 Na1 C1 C2 13.80(9) . . . . ? O2A Na1 C1 C2 -22.5(3) . . . . ? Na2 Na1 C1 C2 76.73(9) . . . . ? O2 Na1 C1 Na2 -106.9(6) . . . . ? O1 Na1 C1 Na2 84.4(2) . . . . ? O1A Na1 C1 Na2 78.8(2) . . . . ? N1 Na1 C1 Na2 74.19(11) . . . . ? N2 Na1 C1 Na2 -62.93(6) . . . . ? O2A Na1 C1 Na2 -99.3(3) . . . . ? C22 N2 C2 C3 -20.0(11) . . . . ? C22A N2 C2 C3 -21.3(8) . . . . ? Na1 N2 C2 C3 -150.97(14) . . . . ? Na2 N2 C2 C3 124.74(16) . . . . ? C22 N2 C2 C1 159.8(11) . . . . ? C22A N2 C2 C1 158.5(8) . . . . ? Na1 N2 C2 C1 28.83(17) . . . . ? Na2 N2 C2 C1 -55.46(14) . . . . ? C22 N2 C2 Na2 -144.8(11) . . . . ? C22A N2 C2 Na2 -146.0(8) . . . . ? Na1 N2 C2 Na2 84.29(7) . . . . ? N1 C1 C2 N2 2.1(2) . . . . ? C6 C1 C2 N2 -176.74(15) . . . . ? Na2 C1 C2 N2 49.27(13) . . . . ? Na1 C1 C2 N2 -20.87(12) . . . . ? N1 C1 C2 C3 -178.13(15) . . . . ? C6 C1 C2 C3 3.1(2) . . . . ? Na2 C1 C2 C3 -130.91(15) . . . . ? Na1 C1 C2 C3 158.95(15) . . . . ? N1 C1 C2 Na2 -47.22(13) . . . . ? C6 C1 C2 Na2 133.99(15) . . . . ? Na1 C1 C2 Na2 -70.15(3) . . . . ? N1 Na2 C2 N2 -104.51(10) . . . . ? C4 Na2 C2 N2 125.36(13) 3_766 . . . ? C1 Na2 C2 N2 -130.84(14) . . . . ? C3 Na2 C2 N2 153.32(9) 3_766 . . . ? C5 Na2 C2 N2 88.33(11) 3_766 . . . ? Na1 Na2 C2 N2 -50.42(8) . . . . ? Na2 Na2 C2 N2 141.39(10) 3_766 . . . ? N2 Na2 C2 C3 -114.4(2) . . . . ? N1 Na2 C2 C3 141.10(18) . . . . ? C4 Na2 C2 C3 11.0(2) 3_766 . . . ? C1 Na2 C2 C3 114.8(2) . . . . ? C3 Na2 C2 C3 38.9(2) 3_766 . . . ? C5 Na2 C2 C3 -26.1(2) 3_766 . . . ? Na1 Na2 C2 C3 -164.81(18) . . . . ? Na2 Na2 C2 C3 27.00(15) 3_766 . . . ? N2 Na2 C2 C1 130.84(14) . . . . ? N1 Na2 C2 C1 26.33(9) . . . . ? C4 Na2 C2 C1 -103.80(14) 3_766 . . . ? C3 Na2 C2 C1 -75.84(11) 3_766 . . . ? C5 Na2 C2 C1 -140.83(10) 3_766 . . . ? Na1 Na2 C2 C1 80.43(9) . . . . ? Na2 Na2 C2 C1 -87.76(9) 3_766 . . . ? N2 C2 C3 C4 176.69(16) . . . . ? C1 C2 C3 C4 -3.1(2) . . . . ? Na2 C2 C3 C4 -99.22(19) . . . . ? N2 C2 C3 Na2 -115.06(16) . . . 3_766 ? C1 C2 C3 Na2 65.14(15) . . . 3_766 ? Na2 C2 C3 Na2 -30.97(16) . . . 3_766 ? C2 C3 C4 C5 1.4(3) . . . . ? Na2 C3 C4 C5 -80.42(16) 3_766 . . . ? C2 C3 C4 Na2 81.85(16) . . . 3_766 ? C3 C4 C5 C6 0.3(3) . . . . ? Na2 C4 C5 C6 -77.04(16) 3_766 . . . ? C3 C4 C5 Na2 77.33(15) . . . 3_766 ? C4 C5 C6 C1 -0.2(3) . . . . ? Na2 C5 C6 C1 -62.60(17) 3_766 . . . ? N1 C1 C6 C5 179.78(17) . . . . ? C2 C1 C6 C5 -1.5(3) . . . . ? Na2 C1 C6 C5 92.6(2) . . . . ? Na1 C1 C6 C5 -119.8(2) . . . . ? C1 N1 C7 C8 77.0(8) . . . . ? C7A N1 C7 C8 -83(20) . . . . ? Na1 N1 C7 C8 -52.4(8) . . . . ? Na2 N1 C7 C8 -164.0(4) . . . . ? C1 N1 C7 C12 -107.4(8) . . . . ? C7A N1 C7 C12 92(20) . . . . ? Na1 N1 C7 C12 123.2(8) . . . . ? Na2 N1 C7 C12 11.6(14) . . . . ? C1 N1 C7A C12A -121.1(15) . . . . ? C7 N1 C7A C12A -101(21) . . . . ? Na1 N1 C7A C12A 109.4(16) . . . . ? Na2 N1 C7A C12A 1(3) . . . . ? C1 N1 C7A C8A 71(2) . . . . ? C7 N1 C7A C8A 91(20) . . . . ? Na1 N1 C7A C8A -58(2) . . . . ? Na2 N1 C7A C8A -166.5(8) . . . . ? N1 C7 C8 C9 171.1(9) . . . . ? C12 C7 C8 C9 -4.8(9) . . . . ? N1 C7 C8 C13 -9.2(10) . . . . ? C12 C7 C8 C13 175.0(7) . . . . ? C12A C7A C8A C9A 2(2) . . . . ? N1 C7A C8A C9A 169(2) . . . . ? C12A C7A C8A C13 -168.0(18) . . . . ? N1 C7A C8A C13 -1(2) . . . . ? C7 C8 C9 C10 -0.3(9) . . . . ? C13 C8 C9 C10 179.9(7) . . . . ? C7A C8A C9A C10A 1(2) . . . . ? C13 C8A C9A C10A 171.3(16) . . . . ? C8 C9 C10 C11 3.9(9) . . . . ? C8 C9 C10 C16 -173.0(6) . . . . ? C8A C9A C10A C11A -4(2) . . . . ? C8A C9A C10A C16A -178.3(15) . . . . ? C9 C10 C11 C12 -2.2(7) . . . . ? C16 C10 C11 C12 174.8(3) . . . . ? C9A C10A C11A C12A 3.1(17) . . . . ? C16A C10A C11A C12A 177.3(9) . . . . ? C10 C11 C12 C7 -3.1(7) . . . . ? C10 C11 C12 C19 -176.8(3) . . . . ? C8 C7 C12 C11 6.5(10) . . . . ? N1 C7 C12 C11 -169.3(6) . . . . ? C8 C7 C12 C19 -179.9(5) . . . . ? N1 C7 C12 C19 4.3(12) . . . . ? C10A C11A C12A C7A 0.3(17) . . . . ? C10A C11A C12A C19A -177.6(9) . . . . ? C8A C7A C12A C11A -3(2) . . . . ? N1 C7A C12A C11A -170.8(13) . . . . ? C8A C7A C12A C19A 174.6(13) . . . . ? N1 C7A C12A C19A 7(3) . . . . ? C9 C8 C13 C8A 32(31) . . . . ? C7 C8 C13 C8A -148(31) . . . . ? C9 C8 C13 C15 57.2(6) . . . . ? C7 C8 C13 C15 -122.6(6) . . . . ? C9 C8 C13 C14 -66.4(6) . . . . ? C7 C8 C13 C14 113.8(6) . . . . ? C9A C8A C13 C8 -142(32) . . . . ? C7A C8A C13 C8 28(31) . . . . ? C9A C8A C13 C15 63.0(16) . . . . ? C7A C8A C13 C15 -127.4(13) . . . . ? C9A C8A C13 C14 -59.7(15) . . . . ? C7A C8A C13 C14 110.0(13) . . . . ? C9 C10 C16 C17 104.4(7) . . . . ? C11 C10 C16 C17 -72.4(6) . . . . ? C9 C10 C16 C18 -136.5(9) . . . . ? C11 C10 C16 C18 46.7(8) . . . . ? C9A C10A C16A C18A -108(2) . . . . ? C11A C10A C16A C18A 77.7(19) . . . . ? C9A C10A C16A C17A 117.4(16) . . . . ? C11A C10A C16A C17A -56.8(15) . . . . ? C11 C12 C19 C20 83.3(4) . . . . ? C7 C12 C19 C20 -90.4(6) . . . . ? C11 C12 C19 C21 -42.0(4) . . . . ? C7 C12 C19 C21 144.3(6) . . . . ? C11A C12A C19A C20A 88.1(9) . . . . ? C7A C12A C19A C20A -89.7(15) . . . . ? C11A C12A C19A C21A -40.9(10) . . . . ? C7A C12A C19A C21A 141.3(15) . . . . ? C2 N2 C22 C27 136.0(16) . . . . ? C22A N2 C22 C27 159(48) . . . . ? Na1 N2 C22 C27 -94(2) . . . . ? Na2 N2 C22 C27 15(4) . . . . ? C2 N2 C22 C23 -59(3) . . . . ? C22A N2 C22 C23 -36(44) . . . . ? Na1 N2 C22 C23 71(2) . . . . ? Na2 N2 C22 C23 179.4(9) . . . . ? C2 N2 C22A C23A -56(2) . . . . ? C22 N2 C22A C23A 147(48) . . . . ? Na1 N2 C22A C23A 72(2) . . . . ? Na2 N2 C22A C23A -176.4(8) . . . . ? C2 N2 C22A C27A 126.5(15) . . . . ? C22 N2 C22A C27A -31(44) . . . . ? Na1 N2 C22A C27A -104.9(18) . . . . ? Na2 N2 C22A C27A 6(3) . . . . ? N2 C22 C23 C24 -169.5(19) . . . . ? C27 C22 C23 C24 -6(3) . . . . ? N2 C22 C23 C28 5(3) . . . . ? C27 C22 C23 C28 168.6(17) . . . . ? N2 C22A C23A C24A -177.2(14) . . . . ? C27A C22A C23A C24A 0(2) . . . . ? N2 C22A C23A C28 -1(3) . . . . ? C27A C22A C23A C28 176.1(11) . . . . ? C22 C23 C24 C25 2.4(16) . . . . ? C28 C23 C24 C25 -172.4(7) . . . . ? C22A C23A C24A C25A 0.1(15) . . . . ? C28 C23A C24A C25A -176.2(5) . . . . ? C23 C24 C25 C26 0.7(7) . . . . ? C23 C24 C25 C31 -178.2(6) . . . . ? C23A C24A C25A C26A -0.4(6) . . . . ? C23A C24A C25A C31A -178.8(4) . . . . ? C24 C25 C26 C27 -0.4(7) . . . . ? C31 C25 C26 C27 178.5(5) . . . . ? C24A C25A C26A C27A 0.6(5) . . . . ? C31A C25A C26A C27A 179.0(3) . . . . ? C25 C26 C27 C22 -3.0(16) . . . . ? C25 C26 C27 C34 176.4(5) . . . . ? N2 C22 C27 C26 170.9(15) . . . . ? C23 C22 C27 C26 7(3) . . . . ? N2 C22 C27 C34 -8(3) . . . . ? C23 C22 C27 C34 -172.8(16) . . . . ? C25A C26A C27A C22A -0.4(13) . . . . ? C25A C26A C27A C34A 177.8(3) . . . . ? C23A C22A C27A C26A 0(2) . . . . ? N2 C22A C27A C26A 177.5(13) . . . . ? C23A C22A C27A C34A -178.2(11) . . . . ? N2 C22A C27A C34A -1(2) . . . . ? C24A C23A C28 C29 70.0(6) . . . . ? C22A C23A C28 C29 -106.4(13) . . . . ? C24A C23A C28 C30 -53.4(6) . . . . ? C22A C23A C28 C30 130.2(13) . . . . ? C24A C23A C28 C23 100(11) . . . . ? C22A C23A C28 C23 -76(11) . . . . ? C24 C23 C28 C23A -88(11) . . . . ? C22 C23 C28 C23A 98(11) . . . . ? C24 C23 C28 C29 62.8(7) . . . . ? C22 C23 C28 C29 -111.5(17) . . . . ? C24 C23 C28 C30 -60.7(8) . . . . ? C22 C23 C28 C30 125.1(17) . . . . ? C26 C25 C31 C32 142.9(5) . . . . ? C24 C25 C31 C32 -38.1(6) . . . . ? C26 C25 C31 C33 -90.8(5) . . . . ? C24 C25 C31 C33 88.1(5) . . . . ? C24A C25A C31A C33A 114.3(4) . . . . ? C26A C25A C31A C33A -64.1(4) . . . . ? C24A C25A C31A C32A -121.7(4) . . . . ? C26A C25A C31A C32A 59.9(4) . . . . ? C26 C27 C34 C36 28.4(7) . . . . ? C22 C27 C34 C36 -152.3(16) . . . . ? C26 C27 C34 C35 -97.4(6) . . . . ? C22 C27 C34 C35 81.9(17) . . . . ? C26A C27A C34A C36A 25.2(5) . . . . ? C22A C27A C34A C36A -156.4(12) . . . . ? C26A C27A C34A C35A -98.9(4) . . . . ? C22A C27A C34A C35A 79.4(12) . . . . ? C40 O1 C37 C38 -7.1(9) . . . . ? Na1 O1 C37 C38 -160.8(7) . . . . ? C40A O1A C37A C38A 14.1(8) . . . . ? Na1 O1A C37A C38A -178.6(6) . . . . ? O1 C37 C38 C39 -20.9(10) . . . . ? O1A C37A C38A C39A -31.3(8) . . . . ? C37 C38 C39 C40 38.8(10) . . . . ? C37A C38A C39A C40A 37.2(9) . . . . ? C37 O1 C40 C39 32.5(9) . . . . ? Na1 O1 C40 C39 -169.2(6) . . . . ? C38 C39 C40 O1 -44.1(11) . . . . ? C37A O1A C40A C39A 9.0(8) . . . . ? Na1 O1A C40A C39A -161.2(5) . . . . ? C38A C39A C40A O1A -28.3(9) . . . . ? C44 O2 C41 C42 -1.1(10) . . . . ? Na1 O2 C41 C42 172.5(7) . . . . ? C44A O2A C41A C42A -38.9(6) . . . . ? Na1 O2A C41A C42A 132.1(4) . . . . ? O2 C41 C42 C43 -23.7(9) . . . . ? O2A C41A C42A C43A 28.4(5) . . . . ? C41 C42 C43 C44 37.5(8) . . . . ? C41A C42A C43A C44A -7.5(5) . . . . ? C41 O2 C44 C43 25.0(10) . . . . ? Na1 O2 C44 C43 -148.0(7) . . . . ? C42 C43 C44 O2 -37.8(8) . . . . ? C41A O2A C44A C43A 33.5(6) . . . . ? Na1 O2A C44A C43A -136.7(4) . . . . ? C42A C43A C44A O2A -15.6(5) . . . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 67.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.398 _refine_diff_density_min -0.302 _refine_diff_density_rms 0.043 _database_code_depnum_ccdc_archive 'CCDC 961089' ####################################################################### # # 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_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C96 H148 K4 N4 O6' _chemical_formula_sum 'C96 H148 K4 N4 O6' _chemical_formula_weight 1610.58 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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.850(3) _cell_length_b 12.896(4) _cell_length_c 28.251(8) _cell_angle_alpha 90.00 _cell_angle_beta 100.892(5) _cell_angle_gamma 90.00 _cell_volume 4597(2) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 2855 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 26.28 _exptl_crystal_description BLOCK _exptl_crystal_colour GREEN _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.163 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1752 _exptl_absorpt_coefficient_mu 0.247 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.570 _exptl_absorpt_correction_T_max 0.746 _exptl_absorpt_process_details 'SADABS 2007/2' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% 0 _diffrn_reflns_number 23072 _diffrn_reflns_av_R_equivalents 0.1201 _diffrn_reflns_av_sigmaI/netI 0.1553 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8070 _reflns_number_gt 4714 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36A (Bruker, 2002)' _computing_data_reduction 'Bruker SAINT; SHELXTL (Sheldrick, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'enCIFer(Allen et al.,2004);PLATON(Spek,2003)' _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^)+(0.1134P)^2^+9.1364P] 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 8070 _refine_ls_number_parameters 508 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1720 _refine_ls_R_factor_gt 0.1070 _refine_ls_wR_factor_ref 0.2695 _refine_ls_wR_factor_gt 0.2402 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _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 K1 K 0.39176(12) 0.60976(11) 0.49691(5) 0.0223(4) Uani 1 1 d . . . K2 K 0.27263(12) 0.68699(11) 0.37640(5) 0.0238(4) Uani 1 1 d . . . N1 N 0.3182(4) 0.4909(4) 0.41775(17) 0.0176(11) Uani 1 1 d . . . N2 N 0.4796(4) 0.6356(4) 0.41582(17) 0.0185(12) Uani 1 1 d . . . C1 C 0.4179(5) 0.4573(4) 0.41192(19) 0.0153(13) Uani 1 1 d . . . C2 C 0.4417(5) 0.3525(5) 0.4061(2) 0.0213(15) Uani 1 1 d . . . H2 H 0.3879 0.3024 0.4069 0.026 Uiso 1 1 calc R . . C3 C 0.5411(5) 0.3182(5) 0.3991(2) 0.0186(14) Uani 1 1 d . . . H3 H 0.5532 0.2465 0.3947 0.022 Uiso 1 1 calc R . . C4 C 0.6198(5) 0.3876(5) 0.3987(2) 0.0196(14) Uani 1 1 d . . . H4 H 0.6870 0.3653 0.3931 0.024 Uiso 1 1 calc R . . C5 C 0.6011(5) 0.4924(5) 0.4064(2) 0.0182(14) Uani 1 1 d . . . H5 H 0.6583 0.5399 0.4081 0.022 Uiso 1 1 calc R . . C6 C 0.5025(5) 0.5305(5) 0.4117(2) 0.0166(13) Uani 1 1 d . . . C7 C 0.2330(5) 0.4263(4) 0.4006(2) 0.0174(13) Uani 1 1 d . . . C8 C 0.2005(5) 0.4044(5) 0.3505(2) 0.0187(14) Uani 1 1 d . . . C9 C 0.1108(5) 0.3467(5) 0.3348(2) 0.0193(14) Uani 1 1 d . . . H9 H 0.0918 0.3324 0.3013 0.023 Uiso 1 1 calc R . . C10 C 0.0460(5) 0.3079(5) 0.3649(2) 0.0270(16) Uani 1 1 d . . . C11 C 0.0779(5) 0.3298(5) 0.4134(2) 0.0217(15) Uani 1 1 d . . . H11 H 0.0357 0.3049 0.4352 0.026 Uiso 1 1 calc R . . C12 C 0.1687(5) 0.3867(5) 0.4318(2) 0.0203(14) Uani 1 1 d . . . C13 C 0.2617(5) 0.4470(5) 0.3136(2) 0.0197(14) Uani 1 1 d . . . H13 H 0.3204 0.4910 0.3314 0.024 Uiso 1 1 calc R . . C14 C 0.3125(6) 0.3603(5) 0.2883(2) 0.0271(16) Uani 1 1 d . . . H14B H 0.2567 0.3165 0.2699 0.041 Uiso 1 1 calc R . . H14C H 0.3585 0.3181 0.3124 0.041 Uiso 1 1 calc R . . H14A H 0.3545 0.3911 0.2663 0.041 Uiso 1 1 calc R . . C15 C 0.1918(5) 0.5165(5) 0.2766(2) 0.0234(15) Uani 1 1 d . . . H15A H 0.2353 0.5494 0.2559 0.035 Uiso 1 1 calc R . . H15C H 0.1588 0.5701 0.2934 0.035 Uiso 1 1 calc R . . H15B H 0.1365 0.4745 0.2568 0.035 Uiso 1 1 calc R . . C16 C -0.0500(5) 0.2426(5) 0.3461(2) 0.0255(15) Uani 1 1 d . . . H16 H -0.0836 0.2241 0.3741 0.031 Uiso 1 1 calc R . . C17 C -0.1328(6) 0.2990(6) 0.3094(2) 0.0309(17) Uani 1 1 d . . . H17B H -0.1529 0.3637 0.3235 0.046 Uiso 1 1 calc R . . H17C H -0.1955 0.2548 0.3004 0.046 Uiso 1 1 calc R . . H17A H -0.1034 0.3146 0.2806 0.046 Uiso 1 1 calc R . . C18 C -0.0164(6) 0.1420(5) 0.3251(2) 0.0269(16) Uani 1 1 d . . . H18B H -0.0792 0.0994 0.3134 0.040 Uiso 1 1 calc R . . H18C H 0.0320 0.1039 0.3501 0.040 Uiso 1 1 calc R . . H18A H 0.0195 0.1577 0.2983 0.040 Uiso 1 1 calc R . . C19 C 0.1989(5) 0.4101(5) 0.4855(2) 0.0189(14) Uani 1 1 d . . . H19 H 0.2780 0.4093 0.4949 0.023 Uiso 1 1 calc R . . C20 C 0.1536(6) 0.3334(5) 0.5177(2) 0.0262(16) Uani 1 1 d . . . H20A H 0.0770 0.3443 0.5142 0.039 Uiso 1 1 calc R . . H20C H 0.1875 0.3445 0.5515 0.039 Uiso 1 1 calc R . . H20B H 0.1672 0.2623 0.5082 0.039 Uiso 1 1 calc R . . C21 C 0.1594(5) 0.5186(5) 0.4948(2) 0.0228(15) Uani 1 1 d . . . H21A H 0.1871 0.5688 0.4743 0.034 Uiso 1 1 calc R . . H21C H 0.1840 0.5370 0.5288 0.034 Uiso 1 1 calc R . . H21B H 0.0818 0.5196 0.4874 0.034 Uiso 1 1 calc R . . C22 C 0.5488(5) 0.7054(5) 0.4009(2) 0.0190(14) Uani 1 1 d . . . C23 C 0.5704(5) 0.7079(5) 0.3538(2) 0.0224(15) Uani 1 1 d . . . C24 C 0.6397(5) 0.7827(5) 0.3408(2) 0.0223(15) Uani 1 1 d . . . H24 H 0.6560 0.7806 0.3094 0.027 Uiso 1 1 calc R . . C25 C 0.6843(5) 0.8585(5) 0.3723(2) 0.0209(14) Uani 1 1 d . . . C26 C 0.6584(5) 0.8606(5) 0.4173(2) 0.0220(15) Uani 1 1 d . . . H26 H 0.6860 0.9149 0.4388 0.026 Uiso 1 1 calc R . . C27 C 0.5939(5) 0.7870(5) 0.4328(2) 0.0182(14) Uani 1 1 d . . . C28 C 0.5166(5) 0.6333(5) 0.3142(2) 0.0225(15) Uani 1 1 d . . . H28 H 0.4743 0.5824 0.3295 0.027 Uiso 1 1 calc R . . C29 C 0.4399(6) 0.6913(5) 0.2751(2) 0.0303(17) Uani 1 1 d . . . H29B H 0.4776 0.7478 0.2624 0.045 Uiso 1 1 calc R . . H29C H 0.3816 0.7200 0.2889 0.045 Uiso 1 1 calc R . . H29A H 0.4114 0.6433 0.2490 0.045 Uiso 1 1 calc R . . C30 C 0.5953(6) 0.5724(5) 0.2912(2) 0.0327(17) Uani 1 1 d . . . H30A H 0.5568 0.5270 0.2660 0.049 Uiso 1 1 calc R . . H30C H 0.6403 0.5302 0.3158 0.049 Uiso 1 1 calc R . . H30B H 0.6396 0.6206 0.2769 0.049 Uiso 1 1 calc R . . C31 C 0.7604(6) 0.9389(5) 0.3590(2) 0.0270(16) Uani 1 1 d . . . H31 H 0.7681 0.9244 0.3250 0.032 Uiso 1 1 calc R . . C32 C 0.8687(5) 0.9275(5) 0.3901(2) 0.0265(16) Uani 1 1 d . . . H32B H 0.9148 0.9834 0.3827 0.040 Uiso 1 1 calc R . . H32A H 0.8989 0.8604 0.3837 0.040 Uiso 1 1 calc R . . H32C H 0.8627 0.9314 0.4241 0.040 Uiso 1 1 calc R . . C33 C 0.7148(6) 1.0476(5) 0.3598(3) 0.0360(18) Uani 1 1 d . . . H33A H 0.6472 1.0515 0.3370 0.054 Uiso 1 1 calc R . . H33B H 0.7646 1.0979 0.3505 0.054 Uiso 1 1 calc R . . H33C H 0.7033 1.0635 0.3923 0.054 Uiso 1 1 calc R . . C34 C 0.5655(5) 0.7941(5) 0.4824(2) 0.0206(14) Uani 1 1 d . . . H34 H 0.5614 0.7217 0.4946 0.025 Uiso 1 1 calc R . . C35 C 0.4579(5) 0.8424(5) 0.4792(2) 0.0277(16) Uani 1 1 d . . . H35B H 0.4595 0.9140 0.4677 0.041 Uiso 1 1 calc R . . H35C H 0.4386 0.8422 0.5112 0.041 Uiso 1 1 calc R . . H35A H 0.4055 0.8026 0.4567 0.041 Uiso 1 1 calc R . . C36 C 0.6464(5) 0.8534(5) 0.5199(2) 0.0239(15) Uani 1 1 d . . . H36B H 0.7175 0.8251 0.5205 0.036 Uiso 1 1 calc R . . H36C H 0.6279 0.8459 0.5518 0.036 Uiso 1 1 calc R . . H36A H 0.6454 0.9270 0.5112 0.036 Uiso 1 1 calc R . . O1 O 0.2965(4) 0.8834(4) 0.33996(16) 0.0332(12) Uani 1 1 d . . . C37 C 0.2208(6) 0.9606(6) 0.3205(3) 0.0333(17) Uani 1 1 d . . . H37B H 0.1520 0.9476 0.3303 0.040 Uiso 1 1 calc R . . H37A H 0.2098 0.9612 0.2848 0.040 Uiso 1 1 calc R . . C38 C 0.2682(6) 1.0622(6) 0.3411(3) 0.0369(18) Uani 1 1 d . . . H38B H 0.2448 1.0790 0.3717 0.044 Uiso 1 1 calc R . . H38A H 0.2479 1.1198 0.3180 0.044 Uiso 1 1 calc R . . C39 C 0.3876(6) 1.0433(5) 0.3498(3) 0.0370(19) Uani 1 1 d . . . H39A H 0.4217 1.0875 0.3284 0.044 Uiso 1 1 calc R . . H39B H 0.4205 1.0578 0.3837 0.044 Uiso 1 1 calc R . . C40 C 0.3980(6) 0.9294(5) 0.3380(3) 0.0325(17) Uani 1 1 d . . . H40A H 0.4149 0.9211 0.3054 0.039 Uiso 1 1 calc R . . H40B H 0.4547 0.8963 0.3617 0.039 Uiso 1 1 calc R . . O2 O 0.2005(4) 0.7776(4) 0.46416(18) 0.0351(12) Uani 1 1 d . . . C41 C 0.1684(7) 0.7807(6) 0.5101(3) 0.045(2) Uani 1 1 d . . . H41B H 0.2297 0.7959 0.5361 0.054 Uiso 1 1 calc R . . H41A H 0.1370 0.7136 0.5171 0.054 Uiso 1 1 calc R . . C42 C 0.0864(6) 0.8671(6) 0.5059(3) 0.0354(18) Uani 1 1 d . . . H42A H 0.0153 0.8427 0.4901 0.043 Uiso 1 1 calc R . . H42B H 0.0823 0.8968 0.5378 0.043 Uiso 1 1 calc R . . C43 C 0.1310(6) 0.9436(6) 0.4750(3) 0.0386(19) Uani 1 1 d . . . H43B H 0.1888 0.9850 0.4943 0.046 Uiso 1 1 calc R . . H43A H 0.0754 0.9910 0.4583 0.046 Uiso 1 1 calc R . . C44 C 0.1725(6) 0.8735(5) 0.4394(3) 0.0348(18) Uani 1 1 d . . . H44A H 0.1172 0.8621 0.4104 0.042 Uiso 1 1 calc R . . H44B H 0.2352 0.9051 0.4294 0.042 Uiso 1 1 calc R . . O3 O 0.0565(4) 0.6981(4) 0.35129(15) 0.0291(11) Uani 1 1 d . . . C45 C 0.0041(6) 0.6275(6) 0.3788(2) 0.0337(18) Uani 1 1 d . . . H45B H 0.0012 0.6574 0.4108 0.040 Uiso 1 1 calc R . . H45A H 0.0430 0.5609 0.3836 0.040 Uiso 1 1 calc R . . C46 C -0.1038(6) 0.6109(6) 0.3511(3) 0.0352(18) Uani 1 1 d . . . H46A H -0.1549 0.6588 0.3618 0.042 Uiso 1 1 calc R . . H46B H -0.1272 0.5386 0.3545 0.042 Uiso 1 1 calc R . . C47 C -0.0934(6) 0.6332(6) 0.3000(2) 0.0364(19) Uani 1 1 d . . . H47A H -0.1617 0.6555 0.2802 0.044 Uiso 1 1 calc R . . H47B H -0.0662 0.5724 0.2848 0.044 Uiso 1 1 calc R . . C48 C -0.0139(6) 0.7205(6) 0.3076(2) 0.0324(17) Uani 1 1 d . . . H48A H 0.0250 0.7239 0.2805 0.039 Uiso 1 1 calc R . . H48B H -0.0498 0.7877 0.3099 0.039 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 K1 0.0313(9) 0.0164(7) 0.0198(7) -0.0023(5) 0.0064(6) -0.0061(6) K2 0.0289(9) 0.0126(7) 0.0293(7) 0.0012(6) 0.0042(6) 0.0007(6) N1 0.024(3) 0.009(3) 0.022(3) -0.004(2) 0.009(2) 0.001(2) N2 0.028(3) 0.006(3) 0.023(3) -0.002(2) 0.009(2) -0.005(2) C1 0.023(4) 0.008(3) 0.015(3) 0.001(2) 0.002(3) 0.001(3) C2 0.035(4) 0.012(3) 0.015(3) 0.000(2) -0.001(3) -0.004(3) C3 0.023(4) 0.012(3) 0.020(3) -0.005(2) 0.002(3) 0.001(3) C4 0.018(4) 0.020(3) 0.020(3) -0.002(3) 0.001(3) 0.004(3) C5 0.025(4) 0.012(3) 0.017(3) -0.001(2) 0.004(3) -0.003(3) C6 0.022(4) 0.014(3) 0.014(3) -0.004(2) 0.006(3) -0.001(3) C7 0.023(4) 0.007(3) 0.024(3) 0.000(2) 0.008(3) 0.004(3) C8 0.031(4) 0.009(3) 0.019(3) 0.001(2) 0.012(3) -0.001(3) C9 0.026(4) 0.016(3) 0.016(3) -0.003(2) 0.005(3) -0.007(3) C10 0.026(4) 0.019(4) 0.038(4) -0.004(3) 0.011(3) -0.003(3) C11 0.026(4) 0.017(4) 0.023(3) 0.001(3) 0.007(3) -0.002(3) C12 0.028(4) 0.004(3) 0.030(3) 0.000(2) 0.008(3) 0.001(3) C13 0.026(4) 0.010(3) 0.024(3) -0.004(2) 0.007(3) -0.003(3) C14 0.044(5) 0.021(4) 0.019(3) -0.001(3) 0.011(3) 0.000(3) C15 0.027(4) 0.023(4) 0.021(3) 0.002(3) 0.006(3) -0.004(3) C16 0.031(4) 0.024(4) 0.022(3) -0.005(3) 0.006(3) -0.008(3) C17 0.031(4) 0.024(4) 0.038(4) -0.002(3) 0.005(3) -0.001(3) C18 0.031(4) 0.016(4) 0.032(4) -0.003(3) 0.002(3) -0.010(3) C19 0.026(4) 0.014(3) 0.019(3) -0.001(2) 0.008(3) -0.006(3) C20 0.037(4) 0.019(4) 0.023(3) 0.002(3) 0.007(3) -0.002(3) C21 0.032(4) 0.013(3) 0.024(3) -0.005(3) 0.006(3) 0.000(3) C22 0.022(4) 0.012(3) 0.023(3) -0.001(2) 0.004(3) -0.004(3) C23 0.028(4) 0.014(3) 0.026(3) 0.001(3) 0.006(3) -0.003(3) C24 0.032(4) 0.018(4) 0.017(3) 0.002(2) 0.006(3) -0.001(3) C25 0.030(4) 0.011(3) 0.023(3) 0.004(2) 0.006(3) -0.004(3) C26 0.022(4) 0.015(3) 0.027(3) -0.002(3) 0.001(3) -0.003(3) C27 0.018(4) 0.016(3) 0.019(3) 0.004(2) 0.003(3) -0.004(3) C28 0.030(4) 0.021(4) 0.015(3) 0.001(2) 0.001(3) -0.008(3) C29 0.040(5) 0.023(4) 0.027(4) -0.001(3) 0.005(3) -0.015(3) C30 0.049(5) 0.021(4) 0.029(4) -0.003(3) 0.012(3) -0.010(3) C31 0.040(5) 0.015(3) 0.029(3) 0.001(3) 0.014(3) -0.009(3) C32 0.030(4) 0.016(3) 0.035(4) -0.002(3) 0.012(3) -0.014(3) C33 0.045(5) 0.016(4) 0.050(5) 0.012(3) 0.017(4) -0.005(3) C34 0.034(4) 0.007(3) 0.022(3) 0.000(2) 0.008(3) 0.000(3) C35 0.031(4) 0.018(4) 0.037(4) -0.002(3) 0.013(3) -0.001(3) C36 0.035(4) 0.014(3) 0.024(3) 0.000(3) 0.010(3) -0.003(3) O1 0.045(3) 0.018(3) 0.037(3) 0.006(2) 0.009(2) 0.005(2) C37 0.033(4) 0.025(4) 0.040(4) 0.003(3) 0.003(3) 0.004(3) C38 0.039(5) 0.022(4) 0.046(4) -0.002(3) -0.001(4) 0.009(3) C39 0.050(5) 0.021(4) 0.039(4) -0.007(3) 0.007(4) -0.003(4) C40 0.034(5) 0.021(4) 0.045(4) 0.006(3) 0.013(3) 0.005(3) O2 0.043(3) 0.013(3) 0.051(3) -0.007(2) 0.014(2) 0.002(2) C41 0.072(6) 0.023(4) 0.046(5) 0.002(3) 0.024(4) 0.013(4) C42 0.037(5) 0.028(4) 0.043(4) -0.007(3) 0.011(4) -0.007(3) C43 0.043(5) 0.019(4) 0.057(5) -0.006(3) 0.020(4) 0.005(4) C44 0.042(5) 0.022(4) 0.041(4) -0.003(3) 0.012(4) 0.000(3) O3 0.033(3) 0.029(3) 0.025(2) 0.000(2) 0.005(2) -0.005(2) C45 0.037(5) 0.035(5) 0.031(4) 0.005(3) 0.011(3) 0.004(4) C46 0.033(5) 0.023(4) 0.046(4) 0.003(3) 0.000(4) 0.001(3) C47 0.028(4) 0.051(5) 0.031(4) -0.008(3) 0.006(3) -0.008(4) C48 0.033(4) 0.037(5) 0.029(4) 0.002(3) 0.010(3) 0.004(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag K1 N1 2.729(5) . ? K1 N2 2.759(5) . ? K1 C4 2.982(6) 3_666 ? K1 C5 3.018(6) 3_666 ? K1 C3 3.046(6) 3_666 ? K1 C1 3.170(6) . ? K1 C2 3.180(6) 3_666 ? K1 C6 3.188(6) . ? K1 C6 3.234(6) 3_666 ? K1 O2 3.274(5) . ? K1 C1 3.314(6) 3_666 ? K1 C34 3.339(6) . ? K2 O3 2.737(5) . ? K2 N2 2.763(6) . ? K2 O1 2.773(5) . ? K2 N1 2.801(5) . ? K2 O2 3.040(5) . ? K2 C44 3.388(7) . ? K2 C7 3.487(6) . ? K2 C22 3.493(7) . ? N1 C7 1.388(8) . ? N1 C1 1.391(8) . ? N2 C22 1.386(8) . ? N2 C6 1.397(8) . ? C1 C2 1.403(8) . ? C1 C6 1.441(8) . ? C1 K1 3.314(6) 3_666 ? C2 C3 1.400(9) . ? C2 K1 3.180(6) 3_666 ? C2 H2 0.9500 . ? C3 C4 1.353(9) . ? C3 K1 3.046(6) 3_666 ? C3 H3 0.9500 . ? C4 C5 1.397(8) . ? C4 K1 2.982(6) 3_666 ? C4 H4 0.9500 . ? C5 C6 1.393(9) . ? C5 K1 3.018(6) 3_666 ? C5 H5 0.9500 . ? C6 K1 3.234(6) 3_666 ? C7 C12 1.414(9) . ? C7 C8 1.427(8) . ? C8 C9 1.373(9) . ? C8 C13 1.520(8) . ? C9 C10 1.391(9) . ? C9 H9 0.9500 . ? C10 C11 1.384(9) . ? C10 C16 1.504(9) . ? C11 C12 1.394(9) . ? C11 H11 0.9500 . ? C12 C19 1.523(8) . ? C13 C15 1.533(9) . ? C13 C14 1.537(8) . ? C13 H13 1.0000 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C14 H14A 0.9800 . ? C15 H15A 0.9800 . ? C15 H15C 0.9800 . ? C15 H15B 0.9800 . ? C16 C18 1.523(9) . ? C16 C17 1.524(9) . ? C16 H16 1.0000 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C17 H17A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C18 H18A 0.9800 . ? C19 C21 1.528(8) . ? C19 C20 1.532(8) . ? C19 H19 1.0000 . ? C20 H20A 0.9800 . ? C20 H20C 0.9800 . ? C20 H20B 0.9800 . ? C21 H21A 0.9800 . ? C21 H21C 0.9800 . ? C21 H21B 0.9800 . ? C22 C23 1.409(8) . ? C22 C27 1.435(8) . ? C23 C24 1.407(9) . ? C23 C28 1.537(8) . ? C24 C25 1.371(9) . ? C24 H24 0.9500 . ? C25 C26 1.375(8) . ? C25 C31 1.521(9) . ? C26 C27 1.383(9) . ? C26 H26 0.9500 . ? C27 C34 1.518(8) . ? C28 C30 1.522(10) . ? C28 C29 1.530(9) . ? C28 H28 1.0000 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C29 H29A 0.9800 . ? C30 H30A 0.9800 . ? C30 H30C 0.9800 . ? C30 H30B 0.9800 . ? C31 C32 1.506(10) . ? C31 C33 1.522(10) . ? C31 H31 1.0000 . ? C32 H32B 0.9800 . ? C32 H32A 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.504(9) . ? C34 C36 1.540(9) . ? C34 H34 1.0000 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C35 H35A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C36 H36A 0.9800 . ? O1 C37 1.427(8) . ? O1 C40 1.443(9) . ? C37 C38 1.515(10) . ? C37 H37B 0.9900 . ? C37 H37A 0.9900 . ? C38 C39 1.527(11) . ? C38 H38B 0.9900 . ? C38 H38A 0.9900 . ? C39 C40 1.518(10) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? O2 C44 1.433(8) . ? O2 C41 1.435(8) . ? C41 C42 1.524(10) . ? C41 H41B 0.9900 . ? C41 H41A 0.9900 . ? C42 C43 1.501(10) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.521(10) . ? C43 H43B 0.9900 . ? C43 H43A 0.9900 . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? O3 C48 1.414(8) . ? O3 C45 1.443(8) . ? C45 C46 1.473(10) . ? C45 H45B 0.9900 . ? C45 H45A 0.9900 . ? C46 C47 1.500(10) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.508(10) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 K1 N2 61.31(15) . . ? N1 K1 C4 137.98(17) . 3_666 ? N2 K1 C4 157.65(17) . 3_666 ? N1 K1 C5 116.30(16) . 3_666 ? N2 K1 C5 148.98(17) . 3_666 ? C4 K1 C5 26.92(16) 3_666 3_666 ? N1 K1 C3 162.33(16) . 3_666 ? N2 K1 C3 132.70(17) . 3_666 ? C4 K1 C3 25.91(17) 3_666 3_666 ? C5 K1 C3 46.04(17) 3_666 3_666 ? N1 K1 C1 25.92(15) . . ? N2 K1 C1 47.74(14) . . ? C4 K1 C1 142.06(16) 3_666 . ? C5 K1 C1 115.16(16) 3_666 . ? C3 K1 C1 150.27(17) 3_666 . ? N1 K1 C2 149.88(17) . 3_666 ? N2 K1 C2 112.51(17) . 3_666 ? C4 K1 C2 45.32(17) 3_666 3_666 ? C5 K1 C2 52.16(17) 3_666 3_666 ? C3 K1 C2 25.87(16) 3_666 3_666 ? C1 K1 C2 126.70(17) . 3_666 ? N1 K1 C6 48.37(15) . . ? N2 K1 C6 25.91(14) . . ? C4 K1 C6 149.73(17) 3_666 . ? C5 K1 C6 127.01(16) 3_666 . ? C3 K1 C6 137.78(17) 3_666 . ? C1 K1 C6 26.19(15) . . ? C2 K1 C6 112.11(17) 3_666 . ? N1 K1 C6 111.62(15) . 3_666 ? N2 K1 C6 123.66(16) . 3_666 ? C4 K1 C6 46.25(16) 3_666 3_666 ? C5 K1 C6 25.46(16) 3_666 3_666 ? C3 K1 C6 53.19(16) 3_666 3_666 ? C1 K1 C6 99.74(15) . 3_666 ? C2 K1 C6 44.33(15) 3_666 3_666 ? C6 K1 C6 104.09(13) . 3_666 ? N1 K1 O2 90.83(14) . . ? N2 K1 O2 95.08(14) . . ? C4 K1 O2 95.56(15) 3_666 . ? C5 K1 O2 115.91(15) 3_666 . ? C3 K1 O2 97.57(15) 3_666 . ? C1 K1 O2 112.16(14) . . ? C2 K1 O2 119.29(15) 3_666 . ? C6 K1 O2 114.64(14) . . ? C6 K1 O2 140.81(14) 3_666 . ? N1 K1 C1 125.51(15) . 3_666 ? N2 K1 C1 108.60(16) . 3_666 ? C4 K1 C1 53.26(16) 3_666 3_666 ? C5 K1 C1 44.87(16) 3_666 3_666 ? C3 K1 C1 45.34(15) 3_666 3_666 ? C1 K1 C1 104.98(13) . 3_666 ? C2 K1 C1 24.84(15) 3_666 3_666 ? C6 K1 C1 97.69(15) . 3_666 ? C6 K1 C1 25.38(15) 3_666 3_666 ? O2 K1 C1 142.80(13) . 3_666 ? N1 K1 C34 115.82(15) . . ? N2 K1 C34 54.85(14) . . ? C4 K1 C34 105.82(16) 3_666 . ? C5 K1 C34 121.00(16) 3_666 . ? C3 K1 C34 80.03(16) 3_666 . ? C1 K1 C34 100.36(15) . . ? C2 K1 C34 68.89(16) 3_666 . ? C6 K1 C34 74.43(15) . . ? C6 K1 C34 107.82(16) 3_666 . ? O2 K1 C34 88.76(14) . . ? C1 K1 C34 82.44(15) 3_666 . ? O3 K2 N2 165.78(15) . . ? O3 K2 O1 91.94(15) . . ? N2 K2 O1 101.71(15) . . ? O3 K2 N1 106.12(15) . . ? N2 K2 N1 60.38(15) . . ? O1 K2 N1 161.90(16) . . ? O3 K2 O2 74.95(14) . . ? N2 K2 O2 100.49(14) . . ? O1 K2 O2 91.37(14) . . ? N1 K2 O2 94.52(14) . . ? O3 K2 C44 68.37(17) . . ? N2 K2 C44 113.00(17) . . ? O1 K2 C44 68.05(16) . . ? N1 K2 C44 119.48(16) . . ? O2 K2 C44 25.02(15) . . ? O3 K2 C7 85.59(15) . . ? N2 K2 C7 81.65(15) . . ? O1 K2 C7 169.70(14) . . ? N1 K2 C7 22.26(15) . . ? O2 K2 C7 97.61(13) . . ? C44 K2 C7 119.84(16) . . ? O3 K2 C22 172.24(15) . . ? N2 K2 C22 21.86(14) . . ? O1 K2 C22 80.31(15) . . ? N1 K2 C22 81.62(15) . . ? O2 K2 C22 105.51(14) . . ? C44 K2 C22 108.68(17) . . ? C7 K2 C22 101.96(15) . . ? O3 K2 K1 119.27(10) . . ? N2 K2 K1 49.27(10) . . ? O1 K2 K1 123.14(11) . . ? N1 K2 K1 48.52(10) . . ? O2 K2 K1 58.37(10) . . ? C44 K2 K1 80.52(13) . . ? C7 K2 K1 66.40(10) . . ? C22 K2 K1 66.23(10) . . ? C7 N1 C1 117.0(5) . . ? C7 N1 K1 138.7(4) . . ? C1 N1 K1 95.1(3) . . ? C7 N1 K2 107.9(4) . . ? C1 N1 K2 110.9(3) . . ? K1 N1 K2 81.22(14) . . ? C22 N2 C6 116.6(5) . . ? C22 N2 K1 135.9(4) . . ? C6 N2 K1 94.4(3) . . ? C22 N2 K2 110.2(4) . . ? C6 N2 K2 113.6(4) . . ? K1 N2 K2 81.36(14) . . ? N1 C1 C2 122.7(6) . . ? N1 C1 C6 120.6(5) . . ? C2 C1 C6 116.7(6) . . ? N1 C1 K1 59.0(3) . . ? C2 C1 K1 138.1(4) . . ? C6 C1 K1 77.6(3) . . ? N1 C1 K1 123.4(3) . 3_666 ? C2 C1 K1 72.2(3) . 3_666 ? C6 C1 K1 74.2(3) . 3_666 ? K1 C1 K1 75.02(13) . 3_666 ? C3 C2 C1 123.1(6) . . ? C3 C2 K1 71.7(3) . 3_666 ? C1 C2 K1 82.9(3) . 3_666 ? C3 C2 H2 118.5 . . ? C1 C2 H2 118.5 . . ? K1 C2 H2 117.3 3_666 . ? C4 C3 C2 119.8(6) . . ? C4 C3 K1 74.4(3) . 3_666 ? C2 C3 K1 82.4(3) . 3_666 ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? K1 C3 H3 113.5 3_666 . ? C3 C4 C5 119.2(6) . . ? C3 C4 K1 79.7(3) . 3_666 ? C5 C4 K1 78.0(3) . 3_666 ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? K1 C4 H4 112.5 3_666 . ? C6 C5 C4 123.0(6) . . ? C6 C5 K1 85.9(3) . 3_666 ? C4 C5 K1 75.1(3) . 3_666 ? C6 C5 H5 118.5 . . ? C4 C5 H5 118.5 . . ? K1 C5 H5 110.1 3_666 . ? C5 C6 N2 124.1(5) . . ? C5 C6 C1 118.2(5) . . ? N2 C6 C1 117.7(5) . . ? C5 C6 K1 137.6(4) . . ? N2 C6 K1 59.7(3) . . ? C1 C6 K1 76.2(3) . . ? C5 C6 K1 68.6(3) . 3_666 ? N2 C6 K1 122.7(4) . 3_666 ? C1 C6 K1 80.4(3) . 3_666 ? K1 C6 K1 75.92(13) . 3_666 ? N1 C7 C12 120.9(5) . . ? N1 C7 C8 122.0(5) . . ? C12 C7 C8 116.9(6) . . ? N1 C7 K2 49.9(3) . . ? C12 C7 K2 126.5(4) . . ? C8 C7 K2 91.3(3) . . ? C9 C8 C7 119.8(5) . . ? C9 C8 C13 119.1(5) . . ? C7 C8 C13 121.1(6) . . ? C8 C9 C10 124.2(6) . . ? C8 C9 H9 117.9 . . ? C10 C9 H9 117.9 . . ? C11 C10 C9 115.6(6) . . ? C11 C10 C16 122.2(6) . . ? C9 C10 C16 122.2(6) . . ? C10 C11 C12 123.3(6) . . ? C10 C11 H11 118.4 . . ? C12 C11 H11 118.4 . . ? C11 C12 C7 120.3(6) . . ? C11 C12 C19 121.0(5) . . ? C7 C12 C19 118.7(5) . . ? C8 C13 C15 111.5(5) . . ? C8 C13 C14 112.1(5) . . ? C15 C13 C14 110.7(5) . . ? C8 C13 H13 107.4 . . ? C15 C13 H13 107.4 . . ? C14 C13 H13 107.4 . . ? C13 C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C14 H14A 109.5 . . ? H14B C14 H14A 109.5 . . ? H14C C14 H14A 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? H15C C15 H15B 109.5 . . ? C10 C16 C18 109.9(6) . . ? C10 C16 C17 113.2(6) . . ? C18 C16 C17 110.7(5) . . ? C10 C16 H16 107.6 . . ? C18 C16 H16 107.6 . . ? C17 C16 H16 107.6 . . ? C16 C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C17 H17A 109.5 . . ? H17B C17 H17A 109.5 . . ? H17C C17 H17A 109.5 . . ? C16 C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C18 H18A 109.5 . . ? H18B C18 H18A 109.5 . . ? H18C C18 H18A 109.5 . . ? C12 C19 C21 108.8(5) . . ? C12 C19 C20 114.2(5) . . ? C21 C19 C20 108.2(5) . . ? C12 C19 H19 108.5 . . ? C21 C19 H19 108.5 . . ? C20 C19 H19 108.5 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? H20C C20 H20B 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? H21C C21 H21B 109.5 . . ? N2 C22 C23 123.7(5) . . ? N2 C22 C27 119.5(5) . . ? C23 C22 C27 116.6(5) . . ? N2 C22 K2 47.9(3) . . ? C23 C22 K2 100.9(4) . . ? C27 C22 K2 116.7(4) . . ? C24 C23 C22 120.6(6) . . ? C24 C23 C28 117.4(5) . . ? C22 C23 C28 122.0(5) . . ? C25 C24 C23 121.8(6) . . ? C25 C24 H24 119.1 . . ? C23 C24 H24 119.1 . . ? C24 C25 C26 118.0(6) . . ? C24 C25 C31 122.4(6) . . ? C26 C25 C31 119.6(6) . . ? C25 C26 C27 122.8(6) . . ? C25 C26 H26 118.6 . . ? C27 C26 H26 118.6 . . ? C26 C27 C22 120.0(5) . . ? C26 C27 C34 120.9(5) . . ? C22 C27 C34 119.0(5) . . ? C30 C28 C29 109.4(5) . . ? C30 C28 C23 113.0(6) . . ? C29 C28 C23 111.0(5) . . ? C30 C28 H28 107.7 . . ? C29 C28 H28 107.7 . . ? C23 C28 H28 107.7 . . ? C28 C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C29 H29A 109.5 . . ? H29B C29 H29A 109.5 . . ? H29C C29 H29A 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? H30C C30 H30B 109.5 . . ? C32 C31 C25 110.8(5) . . ? C32 C31 C33 113.4(6) . . ? C25 C31 C33 110.9(6) . . ? C32 C31 H31 107.1 . . ? C25 C31 H31 107.1 . . ? C33 C31 H31 107.1 . . ? C31 C32 H32B 109.5 . . ? C31 C32 H32A 109.5 . . ? H32B C32 H32A 109.5 . . ? C31 C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C35 C34 C27 110.4(5) . . ? C35 C34 C36 109.2(5) . . ? C27 C34 C36 114.6(5) . . ? C35 C34 K1 71.0(3) . . ? C27 C34 K1 110.7(4) . . ? C36 C34 K1 130.5(4) . . ? C35 C34 H34 107.5 . . ? C27 C34 H34 107.5 . . ? C36 C34 H34 107.5 . . ? K1 C34 H34 38.1 . . ? C34 C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C35 H35A 109.5 . . ? H35B C35 H35A 109.5 . . ? H35C C35 H35A 109.5 . . ? C34 C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C34 C36 H36A 109.5 . . ? H36B C36 H36A 109.5 . . ? H36C C36 H36A 109.5 . . ? C37 O1 C40 104.7(5) . . ? C37 O1 K2 131.7(4) . . ? C40 O1 K2 123.6(4) . . ? O1 C37 C38 105.0(6) . . ? O1 C37 H37B 110.7 . . ? C38 C37 H37B 110.7 . . ? O1 C37 H37A 110.7 . . ? C38 C37 H37A 110.7 . . ? H37B C37 H37A 108.8 . . ? C37 C38 C39 104.0(6) . . ? C37 C38 H38B 111.0 . . ? C39 C38 H38B 111.0 . . ? C37 C38 H38A 111.0 . . ? C39 C38 H38A 111.0 . . ? H38B C38 H38A 109.0 . . ? C40 C39 C38 104.3(6) . . ? C40 C39 H39A 110.9 . . ? C38 C39 H39A 110.9 . . ? C40 C39 H39B 110.9 . . ? C38 C39 H39B 110.9 . . ? H39A C39 H39B 108.9 . . ? O1 C40 C39 105.8(6) . . ? O1 C40 H40A 110.6 . . ? C39 C40 H40A 110.6 . . ? O1 C40 H40B 110.6 . . ? C39 C40 H40B 110.6 . . ? H40A C40 H40B 108.7 . . ? C44 O2 C41 109.2(5) . . ? C44 O2 K2 91.2(4) . . ? C41 O2 K2 158.8(4) . . ? C44 O2 K1 144.5(4) . . ? C41 O2 K1 95.2(4) . . ? K2 O2 K1 69.40(10) . . ? O2 C41 C42 105.2(6) . . ? O2 C41 H41B 110.7 . . ? C42 C41 H41B 110.7 . . ? O2 C41 H41A 110.7 . . ? C42 C41 H41A 110.7 . . ? H41B C41 H41A 108.8 . . ? C43 C42 C41 101.0(6) . . ? C43 C42 H42A 111.6 . . ? C41 C42 H42A 111.6 . . ? C43 C42 H42B 111.6 . . ? C41 C42 H42B 111.6 . . ? H42A C42 H42B 109.4 . . ? C42 C43 C44 102.4(6) . . ? C42 C43 H43B 111.3 . . ? C44 C43 H43B 111.3 . . ? C42 C43 H43A 111.3 . . ? C44 C43 H43A 111.3 . . ? H43B C43 H43A 109.2 . . ? O2 C44 C43 106.1(6) . . ? O2 C44 K2 63.7(3) . . ? C43 C44 K2 169.9(5) . . ? O2 C44 H44A 110.5 . . ? C43 C44 H44A 110.5 . . ? K2 C44 H44A 75.1 . . ? O2 C44 H44B 110.5 . . ? C43 C44 H44B 110.5 . . ? K2 C44 H44B 74.4 . . ? H44A C44 H44B 108.7 . . ? C48 O3 C45 108.2(5) . . ? C48 O3 K2 133.4(4) . . ? C45 O3 K2 112.4(4) . . ? O3 C45 C46 107.1(6) . . ? O3 C45 H45B 110.3 . . ? C46 C45 H45B 110.3 . . ? O3 C45 H45A 110.3 . . ? C46 C45 H45A 110.3 . . ? H45B C45 H45A 108.6 . . ? C45 C46 C47 103.7(6) . . ? C45 C46 H46A 111.0 . . ? C47 C46 H46A 111.0 . . ? C45 C46 H46B 111.0 . . ? C47 C46 H46B 111.0 . . ? H46A C46 H46B 109.0 . . ? C46 C47 C48 100.8(6) . . ? C46 C47 H47A 111.6 . . ? C48 C47 H47A 111.6 . . ? C46 C47 H47B 111.6 . . ? C48 C47 H47B 111.6 . . ? H47A C47 H47B 109.4 . . ? O3 C48 C47 106.0(6) . . ? O3 C48 H48A 110.5 . . ? C47 C48 H48A 110.5 . . ? O3 C48 H48B 110.5 . . ? C47 C48 H48B 110.5 . . ? H48A C48 H48B 108.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 K1 K2 O3 85.93(18) . . . . ? N2 K1 K2 O3 169.67(18) . . . . ? C4 K1 K2 O3 -33.6(3) 3_666 . . . ? C5 K1 K2 O3 22.1(3) 3_666 . . . ? C3 K1 K2 O3 -81.0(3) 3_666 . . . ? C1 K1 K2 O3 113.37(18) . . . . ? C2 K1 K2 O3 -129.6(3) 3_666 . . . ? C6 K1 K2 O3 142.87(17) . . . . ? C6 K1 K2 O3 95.2(4) 3_666 . . . ? O2 K1 K2 O3 -45.99(16) . . . . ? C1 K1 K2 O3 173.6(3) 3_666 . . . ? C34 K1 K2 O3 -140.60(16) . . . . ? N1 K1 K2 N2 -83.73(19) . . . . ? C4 K1 K2 N2 156.7(3) 3_666 . . . ? C5 K1 K2 N2 -147.5(3) 3_666 . . . ? C3 K1 K2 N2 109.4(3) 3_666 . . . ? C1 K1 K2 N2 -56.30(18) . . . . ? C2 K1 K2 N2 60.7(3) 3_666 . . . ? C6 K1 K2 N2 -26.79(18) . . . . ? C6 K1 K2 N2 -74.5(4) 3_666 . . . ? O2 K1 K2 N2 144.35(17) . . . . ? C1 K1 K2 N2 3.9(3) 3_666 . . . ? C34 K1 K2 N2 49.73(17) . . . . ? N1 K1 K2 O1 -159.71(19) . . . . ? N2 K1 K2 O1 -75.98(18) . . . . ? C4 K1 K2 O1 80.7(3) 3_666 . . . ? C5 K1 K2 O1 136.5(3) 3_666 . . . ? C3 K1 K2 O1 33.4(3) 3_666 . . . ? C1 K1 K2 O1 -132.28(18) . . . . ? C2 K1 K2 O1 -15.3(3) 3_666 . . . ? C6 K1 K2 O1 -102.77(18) . . . . ? C6 K1 K2 O1 -150.5(4) 3_666 . . . ? O2 K1 K2 O1 68.37(17) . . . . ? C1 K1 K2 O1 -72.0(3) 3_666 . . . ? C34 K1 K2 O1 -26.25(17) . . . . ? N2 K1 K2 N1 83.73(19) . . . . ? C4 K1 K2 N1 -119.6(3) 3_666 . . . ? C5 K1 K2 N1 -63.8(3) 3_666 . . . ? C3 K1 K2 N1 -166.9(3) 3_666 . . . ? C1 K1 K2 N1 27.43(18) . . . . ? C2 K1 K2 N1 144.5(3) 3_666 . . . ? C6 K1 K2 N1 56.94(19) . . . . ? C6 K1 K2 N1 9.3(4) 3_666 . . . ? O2 K1 K2 N1 -131.92(18) . . . . ? C1 K1 K2 N1 87.7(3) 3_666 . . . ? C34 K1 K2 N1 133.46(18) . . . . ? N1 K1 K2 O2 131.92(18) . . . . ? N2 K1 K2 O2 -144.35(17) . . . . ? C4 K1 K2 O2 12.4(3) 3_666 . . . ? C5 K1 K2 O2 68.1(3) 3_666 . . . ? C3 K1 K2 O2 -35.0(2) 3_666 . . . ? C1 K1 K2 O2 159.36(17) . . . . ? C2 K1 K2 O2 -83.6(3) 3_666 . . . ? C6 K1 K2 O2 -171.14(17) . . . . ? C6 K1 K2 O2 141.2(4) 3_666 . . . ? C1 K1 K2 O2 -140.4(3) 3_666 . . . ? C34 K1 K2 O2 -94.62(15) . . . . ? N1 K1 K2 C44 144.5(2) . . . . ? N2 K1 K2 C44 -131.81(19) . . . . ? C4 K1 K2 C44 24.9(3) 3_666 . . . ? C5 K1 K2 C44 80.7(3) 3_666 . . . ? C3 K1 K2 C44 -22.4(3) 3_666 . . . ? C1 K1 K2 C44 171.90(19) . . . . ? C2 K1 K2 C44 -71.1(3) 3_666 . . . ? C6 K1 K2 C44 -158.60(18) . . . . ? C6 K1 K2 C44 153.7(4) 3_666 . . . ? O2 K1 K2 C44 12.54(17) . . . . ? C1 K1 K2 C44 -127.9(3) 3_666 . . . ? C34 K1 K2 C44 -82.08(17) . . . . ? N1 K1 K2 C7 15.89(17) . . . . ? N2 K1 K2 C7 99.62(17) . . . . ? C4 K1 K2 C7 -103.7(3) 3_666 . . . ? C5 K1 K2 C7 -47.9(3) 3_666 . . . ? C3 K1 K2 C7 -151.0(2) 3_666 . . . ? C1 K1 K2 C7 43.32(16) . . . . ? C2 K1 K2 C7 160.3(3) 3_666 . . . ? C6 K1 K2 C7 72.83(16) . . . . ? C6 K1 K2 C7 25.1(4) 3_666 . . . ? O2 K1 K2 C7 -116.04(16) . . . . ? C1 K1 K2 C7 103.6(3) 3_666 . . . ? C34 K1 K2 C7 149.35(15) . . . . ? N1 K1 K2 C22 -100.18(18) . . . . ? N2 K1 K2 C22 -16.45(17) . . . . ? C4 K1 K2 C22 140.3(3) 3_666 . . . ? C5 K1 K2 C22 -164.0(3) 3_666 . . . ? C3 K1 K2 C22 92.9(2) 3_666 . . . ? C1 K1 K2 C22 -72.74(16) . . . . ? C2 K1 K2 C22 44.3(3) 3_666 . . . ? C6 K1 K2 C22 -43.24(16) . . . . ? C6 K1 K2 C22 -90.9(4) 3_666 . . . ? O2 K1 K2 C22 127.90(16) . . . . ? C1 K1 K2 C22 -12.5(3) 3_666 . . . ? C34 K1 K2 C22 33.28(15) . . . . ? N2 K1 N1 C7 -166.5(6) . . . . ? C4 K1 N1 C7 28.1(7) 3_666 . . . ? C5 K1 N1 C7 48.5(6) 3_666 . . . ? C3 K1 N1 C7 47.5(9) 3_666 . . . ? C1 K1 N1 C7 142.4(8) . . . . ? C2 K1 N1 C7 107.7(6) 3_666 . . . ? C6 K1 N1 C7 165.8(7) . . . . ? C6 K1 N1 C7 75.9(6) 3_666 . . . ? O2 K1 N1 C7 -71.1(6) . . . . ? C1 K1 N1 C7 100.3(6) 3_666 . . . ? C34 K1 N1 C7 -160.2(5) . . . . ? N2 K1 N1 C1 51.1(3) . . . . ? C4 K1 N1 C1 -114.3(4) 3_666 . . . ? C5 K1 N1 C1 -93.9(3) 3_666 . . . ? C3 K1 N1 C1 -94.9(6) 3_666 . . . ? C2 K1 N1 C1 -34.7(5) 3_666 . . . ? C6 K1 N1 C1 23.4(3) . . . . ? C6 K1 N1 C1 -66.5(3) 3_666 . . . ? O2 K1 N1 C1 146.4(3) . . . . ? C1 K1 N1 C1 -42.1(4) 3_666 . . . ? C34 K1 N1 C1 57.4(4) . . . . ? N2 K1 N1 K2 -59.31(15) . . . . ? C4 K1 N1 K2 135.3(2) 3_666 . . . ? C5 K1 N1 K2 155.68(16) 3_666 . . . ? C3 K1 N1 K2 154.7(5) 3_666 . . . ? C1 K1 N1 K2 -110.4(3) . . . . ? C2 K1 N1 K2 -145.1(3) 3_666 . . . ? C6 K1 N1 K2 -87.00(19) . . . . ? C6 K1 N1 K2 -176.88(13) 3_666 . . . ? O2 K1 N1 K2 36.03(13) . . . . ? C1 K1 N1 K2 -152.54(15) 3_666 . . . ? C34 K1 N1 K2 -53.00(18) . . . . ? O3 K2 N1 C7 23.5(4) . . . . ? N2 K2 N1 C7 -161.4(4) . . . . ? O1 K2 N1 C7 -152.3(5) . . . . ? O2 K2 N1 C7 99.1(4) . . . . ? C44 K2 N1 C7 97.3(4) . . . . ? C22 K2 N1 C7 -155.9(4) . . . . ? K1 K2 N1 C7 138.5(4) . . . . ? O3 K2 N1 C1 152.8(3) . . . . ? N2 K2 N1 C1 -32.0(3) . . . . ? O1 K2 N1 C1 -22.9(7) . . . . ? O2 K2 N1 C1 -131.5(4) . . . . ? C44 K2 N1 C1 -133.3(4) . . . . ? C7 K2 N1 C1 129.4(5) . . . . ? C22 K2 N1 C1 -26.5(4) . . . . ? K1 K2 N1 C1 -92.1(4) . . . . ? O3 K2 N1 K1 -115.09(13) . . . . ? N2 K2 N1 K1 60.05(14) . . . . ? O1 K2 N1 K1 69.1(5) . . . . ? O2 K2 N1 K1 -39.46(14) . . . . ? C44 K2 N1 K1 -41.2(2) . . . . ? C7 K2 N1 K1 -138.5(4) . . . . ? C22 K2 N1 K1 65.58(13) . . . . ? N1 K1 N2 C22 170.8(6) . . . . ? C4 K1 N2 C22 -35.5(8) 3_666 . . . ? C5 K1 N2 C22 -95.2(6) 3_666 . . . ? C3 K1 N2 C22 -22.6(7) 3_666 . . . ? C1 K1 N2 C22 -161.9(7) . . . . ? C2 K1 N2 C22 -42.0(6) 3_666 . . . ? C6 K1 N2 C22 -136.6(8) . . . . ? C6 K1 N2 C22 -91.2(6) 3_666 . . . ? O2 K1 N2 C22 82.6(6) . . . . ? C1 K1 N2 C22 -68.3(6) 3_666 . . . ? C34 K1 N2 C22 -2.3(5) . . . . ? N1 K1 N2 C6 -52.6(3) . . . . ? C4 K1 N2 C6 101.0(5) 3_666 . . . ? C5 K1 N2 C6 41.4(5) 3_666 . . . ? C3 K1 N2 C6 114.0(4) 3_666 . . . ? C1 K1 N2 C6 -25.3(3) . . . . ? C2 K1 N2 C6 94.6(4) 3_666 . . . ? C6 K1 N2 C6 45.4(5) 3_666 . . . ? O2 K1 N2 C6 -140.8(3) . . . . ? C1 K1 N2 C6 68.3(4) 3_666 . . . ? C34 K1 N2 C6 134.3(4) . . . . ? N1 K1 N2 K2 60.61(15) . . . . ? C4 K1 N2 K2 -145.7(4) 3_666 . . . ? C5 K1 N2 K2 154.6(3) 3_666 . . . ? C3 K1 N2 K2 -132.75(19) 3_666 . . . ? C1 K1 N2 K2 88.0(2) . . . . ? C2 K1 N2 K2 -152.20(14) 3_666 . . . ? C6 K1 N2 K2 113.2(4) . . . . ? C6 K1 N2 K2 158.67(14) 3_666 . . . ? O2 K1 N2 K2 -27.55(13) . . . . ? C1 K1 N2 K2 -178.44(13) 3_666 . . . ? C34 K1 N2 K2 -112.44(19) . . . . ? O3 K2 N2 C22 -175.5(5) . . . . ? O1 K2 N2 C22 -12.0(4) . . . . ? N1 K2 N2 C22 165.2(4) . . . . ? O2 K2 N2 C22 -105.6(4) . . . . ? C44 K2 N2 C22 -82.9(4) . . . . ? C7 K2 N2 C22 158.2(4) . . . . ? K1 K2 N2 C22 -135.9(4) . . . . ? O3 K2 N2 C6 51.5(8) . . . . ? O1 K2 N2 C6 -145.0(4) . . . . ? N1 K2 N2 C6 32.2(3) . . . . ? O2 K2 N2 C6 121.4(4) . . . . ? C44 K2 N2 C6 144.1(4) . . . . ? C7 K2 N2 C6 25.1(4) . . . . ? C22 K2 N2 C6 -133.0(6) . . . . ? K1 K2 N2 C6 91.1(4) . . . . ? O3 K2 N2 K1 -39.6(6) . . . . ? O1 K2 N2 K1 123.94(13) . . . . ? N1 K2 N2 K1 -58.94(13) . . . . ? O2 K2 N2 K1 30.31(14) . . . . ? C44 K2 N2 K1 53.01(18) . . . . ? C7 K2 N2 K1 -65.94(13) . . . . ? C22 K2 N2 K1 135.9(4) . . . . ? C7 N1 C1 C2 -23.0(8) . . . . ? K1 N1 C1 C2 130.2(5) . . . . ? K2 N1 C1 C2 -147.3(4) . . . . ? C7 N1 C1 C6 157.1(5) . . . . ? K1 N1 C1 C6 -49.8(5) . . . . ? K2 N1 C1 C6 32.8(6) . . . . ? C7 N1 C1 K1 -153.2(5) . . . . ? K2 N1 C1 K1 82.5(2) . . . . ? C7 N1 C1 K1 -112.3(5) . . . 3_666 ? K1 N1 C1 K1 40.8(4) . . . 3_666 ? K2 N1 C1 K1 123.4(3) . . . 3_666 ? N2 K1 C1 N1 -112.7(4) . . . . ? C4 K1 C1 N1 97.2(4) 3_666 . . . ? C5 K1 C1 N1 98.8(3) 3_666 . . . ? C3 K1 C1 N1 142.4(4) 3_666 . . . ? C2 K1 C1 N1 159.1(3) 3_666 . . . ? C6 K1 C1 N1 -137.7(5) . . . . ? C6 K1 C1 N1 120.1(3) 3_666 . . . ? O2 K1 C1 N1 -36.6(3) . . . . ? C1 K1 C1 N1 145.6(4) 3_666 . . . ? C34 K1 C1 N1 -129.6(3) . . . . ? N1 K1 C1 C2 -106.0(8) . . . . ? N2 K1 C1 C2 141.3(7) . . . . ? C4 K1 C1 C2 -8.8(8) 3_666 . . . ? C5 K1 C1 C2 -7.2(7) 3_666 . . . ? C3 K1 C1 C2 36.4(8) 3_666 . . . ? C2 K1 C1 C2 53.1(8) 3_666 . . . ? C6 K1 C1 C2 116.3(8) . . . . ? C6 K1 C1 C2 14.1(7) 3_666 . . . ? O2 K1 C1 C2 -142.6(6) . . . . ? C1 K1 C1 C2 39.6(6) 3_666 . . . ? C34 K1 C1 C2 124.4(7) . . . . ? N1 K1 C1 C6 137.7(5) . . . . ? N2 K1 C1 C6 25.0(3) . . . . ? C4 K1 C1 C6 -125.1(4) 3_666 . . . ? C5 K1 C1 C6 -123.5(3) 3_666 . . . ? C3 K1 C1 C6 -79.9(5) 3_666 . . . ? C2 K1 C1 C6 -63.1(4) 3_666 . . . ? C6 K1 C1 C6 -102.1(3) 3_666 . . . ? O2 K1 C1 C6 101.1(3) . . . . ? C1 K1 C1 C6 -76.7(3) 3_666 . . . ? C34 K1 C1 C6 8.2(4) . . . . ? N1 K1 C1 K1 -145.6(4) . . . 3_666 ? N2 K1 C1 K1 101.7(2) . . . 3_666 ? C4 K1 C1 K1 -48.4(3) 3_666 . . 3_666 ? C5 K1 C1 K1 -46.77(18) 3_666 . . 3_666 ? C3 K1 C1 K1 -3.1(4) 3_666 . . 3_666 ? C2 K1 C1 K1 13.6(2) 3_666 . . 3_666 ? C6 K1 C1 K1 76.7(3) . . . 3_666 ? C6 K1 C1 K1 -25.44(14) 3_666 . . 3_666 ? O2 K1 C1 K1 177.78(12) . . . 3_666 ? C1 K1 C1 K1 0.0 3_666 . . 3_666 ? C34 K1 C1 K1 84.86(14) . . . 3_666 ? N1 C1 C2 C3 178.5(5) . . . . ? C6 C1 C2 C3 -1.5(8) . . . . ? K1 C1 C2 C3 -103.0(7) . . . . ? K1 C1 C2 C3 -62.7(5) 3_666 . . . ? N1 C1 C2 K1 -118.7(5) . . . 3_666 ? C6 C1 C2 K1 61.2(4) . . . 3_666 ? K1 C1 C2 K1 -40.3(6) . . . 3_666 ? C1 C2 C3 C4 1.1(9) . . . . ? K1 C2 C3 C4 -67.1(5) 3_666 . . . ? C1 C2 C3 K1 68.3(5) . . . 3_666 ? C2 C3 C4 C5 1.6(8) . . . . ? K1 C3 C4 C5 -69.9(5) 3_666 . . . ? C2 C3 C4 K1 71.5(5) . . . 3_666 ? C3 C4 C5 C6 -4.1(9) . . . . ? K1 C4 C5 C6 -74.9(5) 3_666 . . . ? C3 C4 C5 K1 70.8(5) . . . 3_666 ? C4 C5 C6 N2 -174.9(5) . . . . ? K1 C5 C6 N2 115.8(5) 3_666 . . . ? C4 C5 C6 C1 3.7(8) . . . . ? K1 C5 C6 C1 -65.6(5) 3_666 . . . ? C4 C5 C6 K1 104.4(7) . . . . ? K1 C5 C6 K1 35.1(6) 3_666 . . . ? C4 C5 C6 K1 69.3(5) . . . 3_666 ? C22 N2 C6 C5 18.0(8) . . . . ? K1 N2 C6 C5 -129.6(5) . . . . ? K2 N2 C6 C5 147.9(5) . . . . ? C22 N2 C6 C1 -160.6(5) . . . . ? K1 N2 C6 C1 51.8(5) . . . . ? K2 N2 C6 C1 -30.7(6) . . . . ? C22 N2 C6 K1 147.6(5) . . . . ? K2 N2 C6 K1 -82.5(2) . . . . ? C22 N2 C6 K1 102.9(5) . . . 3_666 ? K1 N2 C6 K1 -44.8(4) . . . 3_666 ? K2 N2 C6 K1 -127.3(3) . . . 3_666 ? N1 C1 C6 C5 179.1(5) . . . . ? C2 C1 C6 C5 -0.8(8) . . . . ? K1 C1 C6 C5 137.0(5) . . . . ? K1 C1 C6 C5 59.3(5) 3_666 . . . ? N1 C1 C6 N2 -2.2(8) . . . . ? C2 C1 C6 N2 177.9(5) . . . . ? K1 C1 C6 N2 -44.3(4) . . . . ? K1 C1 C6 N2 -122.0(5) 3_666 . . . ? N1 C1 C6 K1 42.1(4) . . . . ? C2 C1 C6 K1 -137.9(5) . . . . ? K1 C1 C6 K1 -77.72(10) 3_666 . . . ? N1 C1 C6 K1 119.8(5) . . . 3_666 ? C2 C1 C6 K1 -60.2(4) . . . 3_666 ? K1 C1 C6 K1 77.72(10) . . . 3_666 ? N1 K1 C6 C5 -140.1(7) . . . . ? N2 K1 C6 C5 108.8(7) . . . . ? C4 K1 C6 C5 -23.4(8) 3_666 . . . ? C5 K1 C6 C5 -46.0(7) 3_666 . . . ? C3 K1 C6 C5 16.5(7) 3_666 . . . ? C1 K1 C6 C5 -116.9(8) . . . . ? C2 K1 C6 C5 12.5(7) 3_666 . . . ? C6 K1 C6 C5 -33.5(6) 3_666 . . . ? O2 K1 C6 C5 152.6(6) . . . . ? C1 K1 C6 C5 -8.5(6) 3_666 . . . ? C34 K1 C6 C5 71.4(6) . . . . ? N1 K1 C6 N2 111.1(4) . . . . ? C4 K1 C6 N2 -132.2(4) 3_666 . . . ? C5 K1 C6 N2 -154.8(3) 3_666 . . . ? C3 K1 C6 N2 -92.3(4) 3_666 . . . ? C1 K1 C6 N2 134.3(5) . . . . ? C2 K1 C6 N2 -96.3(4) 3_666 . . . ? C6 K1 C6 N2 -142.3(4) 3_666 . . . ? O2 K1 C6 N2 43.8(4) . . . . ? C1 K1 C6 N2 -117.3(4) 3_666 . . . ? C34 K1 C6 N2 -37.4(3) . . . . ? N1 K1 C6 C1 -23.2(3) . . . . ? N2 K1 C6 C1 -134.3(5) . . . . ? C4 K1 C6 C1 93.5(5) 3_666 . . . ? C5 K1 C6 C1 71.0(4) 3_666 . . . ? C3 K1 C6 C1 133.4(3) 3_666 . . . ? C2 K1 C6 C1 129.5(3) 3_666 . . . ? C6 K1 C6 C1 83.4(3) 3_666 . . . ? O2 K1 C6 C1 -90.4(3) . . . . ? C1 K1 C6 C1 108.4(3) 3_666 . . . ? C34 K1 C6 C1 -171.7(4) . . . . ? N1 K1 C6 K1 -106.6(2) . . . 3_666 ? N2 K1 C6 K1 142.3(4) . . . 3_666 ? C4 K1 C6 K1 10.1(4) 3_666 . . 3_666 ? C5 K1 C6 K1 -12.4(2) 3_666 . . 3_666 ? C3 K1 C6 K1 50.0(3) 3_666 . . 3_666 ? C1 K1 C6 K1 -83.4(3) . . . 3_666 ? C2 K1 C6 K1 46.05(17) 3_666 . . 3_666 ? C6 K1 C6 K1 0.0 3_666 . . 3_666 ? O2 K1 C6 K1 -173.84(12) . . . 3_666 ? C1 K1 C6 K1 25.04(14) 3_666 . . 3_666 ? C34 K1 C6 K1 104.93(15) . . . 3_666 ? C1 N1 C7 C12 120.5(6) . . . . ? K1 N1 C7 C12 -16.5(9) . . . . ? K2 N1 C7 C12 -113.7(5) . . . . ? C1 N1 C7 C8 -65.3(7) . . . . ? K1 N1 C7 C8 157.7(4) . . . . ? K2 N1 C7 C8 60.6(6) . . . . ? C1 N1 C7 K2 -125.8(5) . . . . ? K1 N1 C7 K2 97.2(5) . . . . ? O3 K2 C7 N1 -157.5(4) . . . . ? N2 K2 C7 N1 16.3(3) . . . . ? O1 K2 C7 N1 126.1(8) . . . . ? O2 K2 C7 N1 -83.3(4) . . . . ? C44 K2 C7 N1 -95.5(4) . . . . ? C22 K2 C7 N1 24.4(4) . . . . ? K1 K2 C7 N1 -32.8(3) . . . . ? O3 K2 C7 C12 -55.2(5) . . . . ? N2 K2 C7 C12 118.5(5) . . . . ? O1 K2 C7 C12 -131.6(8) . . . . ? N1 K2 C7 C12 102.3(6) . . . . ? O2 K2 C7 C12 19.0(5) . . . . ? C44 K2 C7 C12 6.8(6) . . . . ? C22 K2 C7 C12 126.7(5) . . . . ? K1 K2 C7 C12 69.5(5) . . . . ? O3 K2 C7 C8 70.2(4) . . . . ? N2 K2 C7 C8 -116.1(4) . . . . ? O1 K2 C7 C8 -6.2(11) . . . . ? N1 K2 C7 C8 -132.3(6) . . . . ? O2 K2 C7 C8 144.4(4) . . . . ? C44 K2 C7 C8 132.1(4) . . . . ? C22 K2 C7 C8 -107.9(4) . . . . ? K1 K2 C7 C8 -165.1(4) . . . . ? N1 C7 C8 C9 -174.9(6) . . . . ? C12 C7 C8 C9 -0.4(9) . . . . ? K2 C7 C8 C9 -133.1(5) . . . . ? N1 C7 C8 C13 3.1(9) . . . . ? C12 C7 C8 C13 177.6(5) . . . . ? K2 C7 C8 C13 44.9(5) . . . . ? C7 C8 C9 C10 1.1(10) . . . . ? C13 C8 C9 C10 -177.0(6) . . . . ? C8 C9 C10 C11 -0.8(10) . . . . ? C8 C9 C10 C16 -178.4(6) . . . . ? C9 C10 C11 C12 -0.1(10) . . . . ? C16 C10 C11 C12 177.4(6) . . . . ? C10 C11 C12 C7 0.7(10) . . . . ? C10 C11 C12 C19 179.0(6) . . . . ? N1 C7 C12 C11 174.1(6) . . . . ? C8 C7 C12 C11 -0.4(9) . . . . ? K2 C7 C12 C11 113.5(6) . . . . ? N1 C7 C12 C19 -4.2(9) . . . . ? C8 C7 C12 C19 -178.7(5) . . . . ? K2 C7 C12 C19 -64.7(7) . . . . ? C9 C8 C13 C15 58.2(7) . . . . ? C7 C8 C13 C15 -119.8(6) . . . . ? C9 C8 C13 C14 -66.5(8) . . . . ? C7 C8 C13 C14 115.5(6) . . . . ? C11 C10 C16 C18 -114.2(7) . . . . ? C9 C10 C16 C18 63.2(8) . . . . ? C11 C10 C16 C17 121.4(7) . . . . ? C9 C10 C16 C17 -61.2(9) . . . . ? C11 C12 C19 C21 -97.0(7) . . . . ? C7 C12 C19 C21 81.3(7) . . . . ? C11 C12 C19 C20 24.0(8) . . . . ? C7 C12 C19 C20 -157.7(6) . . . . ? C6 N2 C22 C23 58.7(8) . . . . ? K1 N2 C22 C23 -171.4(5) . . . . ? K2 N2 C22 C23 -72.8(7) . . . . ? C6 N2 C22 C27 -127.9(6) . . . . ? K1 N2 C22 C27 2.1(9) . . . . ? K2 N2 C22 C27 100.7(6) . . . . ? C6 N2 C22 K2 131.5(6) . . . . ? K1 N2 C22 K2 -98.6(5) . . . . ? O1 K2 C22 N2 168.1(4) . . . . ? N1 K2 C22 N2 -13.0(4) . . . . ? O2 K2 C22 N2 79.4(4) . . . . ? C44 K2 C22 N2 105.4(4) . . . . ? C7 K2 C22 N2 -22.1(4) . . . . ? K1 K2 C22 N2 35.2(3) . . . . ? N2 K2 C22 C23 126.0(6) . . . . ? O1 K2 C22 C23 -65.9(4) . . . . ? N1 K2 C22 C23 113.0(4) . . . . ? O2 K2 C22 C23 -154.6(4) . . . . ? C44 K2 C22 C23 -128.7(4) . . . . ? C7 K2 C22 C23 103.9(4) . . . . ? K1 K2 C22 C23 161.2(4) . . . . ? N2 K2 C22 C27 -106.7(6) . . . . ? O1 K2 C22 C27 61.4(4) . . . . ? N1 K2 C22 C27 -119.7(4) . . . . ? O2 K2 C22 C27 -27.3(4) . . . . ? C44 K2 C22 C27 -1.3(5) . . . . ? C7 K2 C22 C27 -128.8(4) . . . . ? K1 K2 C22 C27 -71.5(4) . . . . ? N2 C22 C23 C24 178.5(6) . . . . ? C27 C22 C23 C24 4.8(9) . . . . ? K2 C22 C23 C24 132.2(6) . . . . ? N2 C22 C23 C28 1.1(10) . . . . ? C27 C22 C23 C28 -172.6(6) . . . . ? K2 C22 C23 C28 -45.2(6) . . . . ? C22 C23 C24 C25 -3.3(10) . . . . ? C28 C23 C24 C25 174.2(6) . . . . ? C23 C24 C25 C26 -0.8(10) . . . . ? C23 C24 C25 C31 179.2(6) . . . . ? C24 C25 C26 C27 3.2(10) . . . . ? C31 C25 C26 C27 -176.7(6) . . . . ? C25 C26 C27 C22 -1.5(10) . . . . ? C25 C26 C27 C34 -178.6(6) . . . . ? N2 C22 C27 C26 -176.4(6) . . . . ? C23 C22 C27 C26 -2.5(9) . . . . ? K2 C22 C27 C26 -121.7(5) . . . . ? N2 C22 C27 C34 0.7(9) . . . . ? C23 C22 C27 C34 174.6(6) . . . . ? K2 C22 C27 C34 55.4(7) . . . . ? C24 C23 C28 C30 57.3(8) . . . . ? C22 C23 C28 C30 -125.2(7) . . . . ? C24 C23 C28 C29 -66.1(8) . . . . ? C22 C23 C28 C29 111.3(7) . . . . ? C24 C25 C31 C32 -116.0(7) . . . . ? C26 C25 C31 C32 64.0(8) . . . . ? C24 C25 C31 C33 117.2(7) . . . . ? C26 C25 C31 C33 -62.9(8) . . . . ? C26 C27 C34 C35 98.4(7) . . . . ? C22 C27 C34 C35 -78.7(7) . . . . ? C26 C27 C34 C36 -25.4(8) . . . . ? C22 C27 C34 C36 157.5(6) . . . . ? C26 C27 C34 K1 175.0(5) . . . . ? C22 C27 C34 K1 -2.1(7) . . . . ? N1 K1 C34 C35 100.4(4) . . . . ? N2 K1 C34 C35 107.2(4) . . . . ? C4 K1 C34 C35 -85.4(4) 3_666 . . . ? C5 K1 C34 C35 -109.7(4) 3_666 . . . ? C3 K1 C34 C35 -87.8(4) 3_666 . . . ? C1 K1 C34 C35 122.4(3) . . . . ? C2 K1 C34 C35 -112.1(4) 3_666 . . . ? C6 K1 C34 C35 126.1(4) . . . . ? C6 K1 C34 C35 -133.8(3) 3_666 . . . ? O2 K1 C34 C35 10.1(3) . . . . ? C1 K1 C34 C35 -133.7(4) 3_666 . . . ? N1 K1 C34 C27 -4.9(5) . . . . ? N2 K1 C34 C27 1.9(4) . . . . ? C4 K1 C34 C27 169.4(4) 3_666 . . . ? C5 K1 C34 C27 145.0(4) 3_666 . . . ? C3 K1 C34 C27 166.9(4) 3_666 . . . ? C1 K1 C34 C27 17.1(4) . . . . ? C2 K1 C34 C27 142.6(4) 3_666 . . . ? C6 K1 C34 C27 20.8(4) . . . . ? C6 K1 C34 C27 121.0(4) 3_666 . . . ? O2 K1 C34 C27 -95.2(4) . . . . ? C1 K1 C34 C27 121.1(4) 3_666 . . . ? N1 K1 C34 C36 -160.2(5) . . . . ? N2 K1 C34 C36 -153.4(6) . . . . ? C4 K1 C34 C36 14.0(6) 3_666 . . . ? C5 K1 C34 C36 -10.3(6) 3_666 . . . ? C3 K1 C34 C36 11.5(5) 3_666 . . . ? C1 K1 C34 C36 -138.2(5) . . . . ? C2 K1 C34 C36 -12.7(5) 3_666 . . . ? C6 K1 C34 C36 -134.5(5) . . . . ? C6 K1 C34 C36 -34.4(6) 3_666 . . . ? O2 K1 C34 C36 109.5(5) . . . . ? C1 K1 C34 C36 -34.3(5) 3_666 . . . ? O3 K2 O1 C37 5.4(5) . . . . ? N2 K2 O1 C37 -170.6(5) . . . . ? N1 K2 O1 C37 -178.7(5) . . . . ? O2 K2 O1 C37 -69.6(5) . . . . ? C44 K2 O1 C37 -60.4(5) . . . . ? C7 K2 O1 C37 81.2(10) . . . . ? C22 K2 O1 C37 -175.1(5) . . . . ? K1 K2 O1 C37 -122.0(5) . . . . ? O3 K2 O1 C40 -175.5(5) . . . . ? N2 K2 O1 C40 8.5(5) . . . . ? N1 K2 O1 C40 0.4(8) . . . . ? O2 K2 O1 C40 109.5(5) . . . . ? C44 K2 O1 C40 118.8(5) . . . . ? C7 K2 O1 C40 -99.7(9) . . . . ? C22 K2 O1 C40 4.0(4) . . . . ? K1 K2 O1 C40 57.2(5) . . . . ? C40 O1 C37 C38 -40.8(7) . . . . ? K2 O1 C37 C38 138.4(5) . . . . ? O1 C37 C38 C39 28.0(7) . . . . ? C37 C38 C39 C40 -5.4(8) . . . . ? C37 O1 C40 C39 37.3(7) . . . . ? K2 O1 C40 C39 -142.0(4) . . . . ? C38 C39 C40 O1 -18.8(7) . . . . ? O3 K2 O2 C44 -70.9(4) . . . . ? N2 K2 O2 C44 122.9(4) . . . . ? O1 K2 O2 C44 20.7(4) . . . . ? N1 K2 O2 C44 -176.4(4) . . . . ? C7 K2 O2 C44 -154.3(4) . . . . ? C22 K2 O2 C44 101.0(4) . . . . ? K1 K2 O2 C44 149.6(4) . . . . ? O3 K2 O2 C41 94.0(13) . . . . ? N2 K2 O2 C41 -72.2(13) . . . . ? O1 K2 O2 C41 -174.4(13) . . . . ? N1 K2 O2 C41 -11.5(14) . . . . ? C44 K2 O2 C41 164.9(15) . . . . ? C7 K2 O2 C41 10.6(13) . . . . ? C22 K2 O2 C41 -94.1(13) . . . . ? K1 K2 O2 C41 -45.5(13) . . . . ? O3 K2 O2 K1 139.49(13) . . . . ? N2 K2 O2 K1 -26.69(13) . . . . ? O1 K2 O2 K1 -128.87(12) . . . . ? N1 K2 O2 K1 34.00(13) . . . . ? C44 K2 O2 K1 -149.6(4) . . . . ? C7 K2 O2 K1 56.17(13) . . . . ? C22 K2 O2 K1 -48.54(13) . . . . ? N1 K1 O2 C44 -95.7(7) . . . . ? N2 K1 O2 C44 -34.4(7) . . . . ? C4 K1 O2 C44 125.9(7) 3_666 . . . ? C5 K1 O2 C44 144.3(7) 3_666 . . . ? C3 K1 O2 C44 99.9(7) 3_666 . . . ? C1 K1 O2 C44 -80.6(7) . . . . ? C2 K1 O2 C44 85.0(7) 3_666 . . . ? C6 K1 O2 C44 -52.1(7) . . . . ? C6 K1 O2 C44 137.4(7) 3_666 . . . ? C1 K1 O2 C44 95.9(7) 3_666 . . . ? C34 K1 O2 C44 20.1(7) . . . . ? N1 K1 O2 C41 130.1(4) . . . . ? N2 K1 O2 C41 -168.6(4) . . . . ? C4 K1 O2 C41 -8.3(4) 3_666 . . . ? C5 K1 O2 C41 10.1(5) 3_666 . . . ? C3 K1 O2 C41 -34.3(4) 3_666 . . . ? C1 K1 O2 C41 145.2(4) . . . . ? C2 K1 O2 C41 -49.2(5) 3_666 . . . ? C6 K1 O2 C41 173.7(4) . . . . ? C6 K1 O2 C41 3.2(5) 3_666 . . . ? C1 K1 O2 C41 -38.3(5) 3_666 . . . ? C34 K1 O2 C41 -114.1(4) . . . . ? N1 K1 O2 K2 -34.90(13) . . . . ? N2 K1 O2 K2 26.37(13) . . . . ? C4 K1 O2 K2 -173.32(14) 3_666 . . . ? C5 K1 O2 K2 -154.88(15) 3_666 . . . ? C3 K1 O2 K2 160.68(14) 3_666 . . . ? C1 K1 O2 K2 -19.78(16) . . . . ? C2 K1 O2 K2 145.74(15) 3_666 . . . ? C6 K1 O2 K2 8.68(16) . . . . ? C6 K1 O2 K2 -161.83(19) 3_666 . . . ? C1 K1 O2 K2 156.7(2) 3_666 . . . ? C34 K1 O2 K2 80.91(12) . . . . ? C44 O2 C41 C42 18.8(8) . . . . ? K2 O2 C41 C42 -145.2(10) . . . . ? K1 O2 C41 C42 172.7(5) . . . . ? O2 C41 C42 C43 -36.1(8) . . . . ? C41 C42 C43 C44 38.7(8) . . . . ? C41 O2 C44 C43 6.2(8) . . . . ? K2 O2 C44 C43 -179.6(5) . . . . ? K1 O2 C44 C43 -124.7(6) . . . . ? C41 O2 C44 K2 -174.3(6) . . . . ? K1 O2 C44 K2 54.8(6) . . . . ? C42 C43 C44 O2 -28.8(8) . . . . ? C42 C43 C44 K2 -31(3) . . . . ? O3 K2 C44 O2 100.9(4) . . . . ? N2 K2 C44 O2 -63.8(4) . . . . ? O1 K2 C44 O2 -157.6(4) . . . . ? N1 K2 C44 O2 4.1(5) . . . . ? C7 K2 C44 O2 29.8(4) . . . . ? C22 K2 C44 O2 -86.7(4) . . . . ? K1 K2 C44 O2 -25.9(4) . . . . ? O3 K2 C44 C43 103(3) . . . . ? N2 K2 C44 C43 -61(3) . . . . ? O1 K2 C44 C43 -155(3) . . . . ? N1 K2 C44 C43 7(3) . . . . ? O2 K2 C44 C43 2(3) . . . . ? C7 K2 C44 C43 32(3) . . . . ? C22 K2 C44 C43 -84(3) . . . . ? K1 K2 C44 C43 -24(3) . . . . ? N2 K2 O3 C48 -143.0(7) . . . . ? O1 K2 O3 C48 53.1(6) . . . . ? N1 K2 O3 C48 -125.5(6) . . . . ? O2 K2 O3 C48 144.0(6) . . . . ? C44 K2 O3 C48 118.6(6) . . . . ? C7 K2 O3 C48 -116.8(6) . . . . ? K1 K2 O3 C48 -176.6(5) . . . . ? N2 K2 O3 C45 5.5(8) . . . . ? O1 K2 O3 C45 -158.4(4) . . . . ? N1 K2 O3 C45 22.9(4) . . . . ? O2 K2 O3 C45 -67.5(4) . . . . ? C44 K2 O3 C45 -92.9(4) . . . . ? C7 K2 O3 C45 31.6(4) . . . . ? K1 K2 O3 C45 -28.1(4) . . . . ? C48 O3 C45 C46 -2.5(7) . . . . ? K2 O3 C45 C46 -159.0(4) . . . . ? O3 C45 C46 C47 24.9(8) . . . . ? C45 C46 C47 C48 -35.9(7) . . . . ? C45 O3 C48 C47 -20.9(7) . . . . ? K2 O3 C48 C47 128.5(5) . . . . ? C46 C47 C48 O3 35.3(7) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.724 _refine_diff_density_min -0.761 _refine_diff_density_rms 0.104 _database_code_depnum_ccdc_archive 'CCDC 961090' ####################################################################### # # 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_6 _refine_special_details ; Both methyl groups of one of the isopropyl groups are disordered over two positions; the occupancies of the two components were refined competitively, converging at a ration of 0.61(7):0.39(7). Chemically equivalent 1,2- and 1,3-distances of the isopropyl group were restrained to be approximately equal. The disordered atoms could not be sensibly refined with anisotropic thermal parameters, and so these atoms were refined isotropically. Global rigid bond restraints were also applied to the whole molecule. ; _audit_creation_method ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H50 Cs N2' _chemical_formula_sum 'C36 H50 Cs N2' _chemical_formula_weight 643.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' Cs Cs -0.7457 7.9052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n m a' _symmetry_space_group_name_Hall '-P 2ac 2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 11.3436(9) _cell_length_b 26.935(4) _cell_length_c 11.4129(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3487.1(7) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 1477 _cell_measurement_theta_min 3.28 _cell_measurement_theta_max 74.26 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.1219 _exptl_crystal_size_mid 0.0765 _exptl_crystal_size_min 0.0274 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.226 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1340 _exptl_absorpt_coefficient_mu 8.444 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.259 _exptl_absorpt_correction_T_max 0.697 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Single source at offset), Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3613 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 7519 _diffrn_reflns_av_R_equivalents 0.1719 _diffrn_reflns_av_sigmaI/netI 0.2141 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.28 _diffrn_reflns_theta_max 66.59 _reflns_number_total 2880 _reflns_number_gt 1517 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'enCIFer (Allen et al., 2004); PLATON (Spek, 2009)' _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^)+(0.0851P)^2^+7.5509P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom, Me from difmap' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2880 _refine_ls_number_parameters 180 _refine_ls_number_restraints 50 _refine_ls_R_factor_all 0.1828 _refine_ls_R_factor_gt 0.0993 _refine_ls_wR_factor_ref 0.2640 _refine_ls_wR_factor_gt 0.2117 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.056 _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 Cs1 Cs 0.18133(9) 0.2500 0.70575(12) 0.0411(4) Uani 1 2 d SU . . C10 C 0.4473(11) 0.1341(5) 0.7987(15) 0.042(3) Uani 1 1 d U . . H10 H 0.4360 0.1709 0.8002 0.050 Uiso 1 1 calc R . . C16 C 0.3118(11) 0.1658(5) 0.3813(12) 0.045(3) Uani 1 1 d DU . . H16 H 0.3239 0.2001 0.4121 0.054 Uiso 0.61(7) 1 calc PR A 1 H16A H 0.3604 0.1957 0.3998 0.054 Uiso 0.39(7) 1 calc PR A 2 C5 C 0.3956(10) 0.1154(4) 0.6844(13) 0.034(3) Uani 1 1 d U A . C9 C 0.3321(11) 0.1304(4) 0.4843(11) 0.034(3) Uani 1 1 d DU A . C12 C 0.5794(13) 0.1245(6) 0.8003(16) 0.056(4) Uani 1 1 d U . . H12A H 0.6142 0.1361 0.7266 0.084 Uiso 1 1 calc R . . H12B H 0.5939 0.0888 0.8092 0.084 Uiso 1 1 calc R . . H12C H 0.6152 0.1424 0.8660 0.084 Uiso 1 1 calc R . . C6 C 0.3652(11) 0.0655(4) 0.6708(13) 0.036(3) Uani 1 1 d U . . H6 H 0.3761 0.0435 0.7350 0.043 Uiso 1 1 calc R . . C8 C 0.3046(12) 0.0810(5) 0.4755(13) 0.041(3) Uani 1 1 d U . . H8 H 0.2736 0.0692 0.4033 0.050 Uiso 1 1 calc R A . C4 C 0.3787(8) 0.1488(4) 0.5891(11) 0.025(2) Uani 1 1 d U . . C11 C 0.3888(16) 0.1135(7) 0.9069(15) 0.062(4) Uani 1 1 d U . . H11A H 0.3031 0.1169 0.8997 0.092 Uiso 1 1 calc R . . H11B H 0.4161 0.1318 0.9759 0.092 Uiso 1 1 calc R . . H11C H 0.4092 0.0783 0.9153 0.092 Uiso 1 1 calc R . . C15 C 0.1620(17) -0.0140(6) 0.6245(17) 0.065(5) Uani 1 1 d U A . H15A H 0.1737 -0.0046 0.7066 0.097 Uiso 1 1 calc R . . H15B H 0.1385 -0.0490 0.6202 0.097 Uiso 1 1 calc R . . H15C H 0.1001 0.0067 0.5900 0.097 Uiso 1 1 calc R . . C7 C 0.3197(14) 0.0468(5) 0.5669(14) 0.042(3) Uani 1 1 d U A . C13 C 0.2791(16) -0.0064(5) 0.5555(17) 0.056(4) Uani 1 1 d U . . H13 H 0.2622 -0.0128 0.4708 0.067 Uiso 1 1 calc R A . C17 C 0.399(3) 0.1589(14) 0.283(2) 0.067(10) Uiso 0.61(7) 1 d PDU A 1 H17A H 0.4768 0.1700 0.3085 0.100 Uiso 0.61(7) 1 calc PR A 1 H17B H 0.3735 0.1786 0.2152 0.100 Uiso 0.61(7) 1 calc PR A 1 H17C H 0.4020 0.1238 0.2611 0.100 Uiso 0.61(7) 1 calc PR A 1 C14 C 0.374(2) -0.0435(5) 0.594(2) 0.075(6) Uani 1 1 d U A . H14A H 0.3935 -0.0379 0.6771 0.113 Uiso 1 1 calc R . . H14B H 0.4452 -0.0389 0.5466 0.113 Uiso 1 1 calc R . . H14C H 0.3449 -0.0775 0.5845 0.113 Uiso 1 1 calc R . . C18 C 0.1841(17) 0.1631(13) 0.337(3) 0.052(9) Uiso 0.61(7) 1 d PDU A 1 H18A H 0.1663 0.1291 0.3124 0.078 Uiso 0.61(7) 1 calc PR A 1 H18B H 0.1740 0.1858 0.2712 0.078 Uiso 0.61(7) 1 calc PR A 1 H18C H 0.1305 0.1727 0.4009 0.078 Uiso 0.61(7) 1 calc PR A 1 N1 N 0.3939(8) 0.2003(3) 0.6057(9) 0.023(2) Uiso 1 1 d U A . C3 C 0.6905(11) 0.2237(5) 0.4867(11) 0.034(3) Uani 1 1 d U . . H3 H 0.7587 0.2062 0.4617 0.041 Uiso 1 1 calc R . . C2 C 0.5930(10) 0.1981(4) 0.5223(10) 0.026(2) Uani 1 1 d U . . H2 H 0.5933 0.1628 0.5180 0.031 Uiso 1 1 calc R . . C1 C 0.4899(10) 0.2230(4) 0.5664(10) 0.022(2) Uani 1 1 d U . . C17A C 0.363(5) 0.1455(16) 0.268(2) 0.054(15) Uiso 0.39(7) 1 d PDU A 2 H17D H 0.4431 0.1331 0.2825 0.082 Uiso 0.39(7) 1 calc PR A 2 H17E H 0.3662 0.1721 0.2093 0.082 Uiso 0.39(7) 1 calc PR A 2 H17F H 0.3136 0.1184 0.2390 0.082 Uiso 0.39(7) 1 calc PR A 2 C18A C 0.189(3) 0.185(2) 0.370(4) 0.061(16) Uiso 0.39(7) 1 d PDU A 2 H18D H 0.1363 0.1573 0.3486 0.091 Uiso 0.39(7) 1 calc PR A 2 H18E H 0.1861 0.2102 0.3085 0.091 Uiso 0.39(7) 1 calc PR A 2 H18F H 0.1635 0.1991 0.4444 0.091 Uiso 0.39(7) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cs1 0.0294(5) 0.0554(7) 0.0386(8) 0.000 0.0114(6) 0.000 C10 0.042(6) 0.037(6) 0.045(7) 0.013(6) -0.015(6) -0.012(6) C16 0.070(9) 0.044(6) 0.022(7) -0.005(5) -0.007(7) 0.006(8) C5 0.026(5) 0.037(5) 0.039(6) 0.010(5) -0.009(5) 0.003(5) C9 0.044(7) 0.040(5) 0.019(6) 0.000(5) 0.006(5) 0.010(6) C12 0.044(6) 0.080(10) 0.044(9) 0.005(10) -0.009(6) -0.007(7) C6 0.036(6) 0.032(5) 0.038(7) 0.013(5) -0.004(5) -0.007(5) C8 0.045(7) 0.046(5) 0.033(7) -0.003(5) -0.002(6) -0.008(6) C4 0.013(4) 0.034(5) 0.028(6) 0.004(4) 0.009(4) 0.001(4) C11 0.064(9) 0.086(11) 0.035(7) -0.006(9) 0.006(7) -0.013(9) C15 0.078(9) 0.052(8) 0.065(12) -0.006(9) 0.020(9) -0.026(8) C7 0.048(7) 0.037(5) 0.040(8) 0.002(5) 0.002(7) -0.004(6) C13 0.075(9) 0.047(6) 0.046(10) -0.010(7) 0.016(8) -0.014(6) C14 0.089(10) 0.041(7) 0.096(17) -0.008(10) 0.017(11) -0.008(7) C3 0.030(5) 0.041(6) 0.032(8) -0.004(6) 0.002(5) 0.008(5) C2 0.034(5) 0.036(6) 0.008(6) -0.005(5) -0.002(5) 0.007(5) C1 0.028(5) 0.029(5) 0.008(6) 0.004(5) -0.001(4) 0.004(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cs1 N1 2.985(9) 8_565 ? Cs1 N1 2.985(9) . ? Cs1 C1 3.465(11) 6_557 ? Cs1 C1 3.465(11) 3_456 ? C10 C11 1.51(2) . ? C10 C5 1.52(2) . ? C10 C12 1.52(2) . ? C10 H10 1.0000 . ? C16 C18A 1.49(2) . ? C16 C17 1.504(19) . ? C16 C17A 1.52(2) . ? C16 C9 1.531(19) . ? C16 C18 1.535(19) . ? C16 H16 1.0000 . ? C16 H16A 1.0000 . ? C5 C6 1.397(18) . ? C5 C4 1.426(18) . ? C9 C8 1.371(19) . ? C9 C4 1.399(18) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C6 C7 1.39(2) . ? C6 H6 0.9500 . ? C8 C7 1.40(2) . ? C8 H8 0.9500 . ? C4 N1 1.409(15) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C15 C13 1.56(2) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C7 C13 1.51(2) . ? C13 C14 1.54(3) . ? C13 H13 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? N1 C1 1.328(15) . ? C3 C2 1.366(18) . ? C3 C3 1.42(2) 8_565 ? C3 H3 0.9500 . ? C2 C1 1.439(16) . ? C2 H2 0.9500 . ? C1 C1 1.45(2) 8_565 ? C1 Cs1 3.465(11) 6_657 ? C17A H17D 0.9800 . ? C17A H17E 0.9800 . ? C17A H17F 0.9800 . ? C18A H18D 0.9800 . ? C18A H18E 0.9800 . ? C18A H18F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cs1 N1 53.3(3) 8_565 . ? N1 Cs1 C1 152.5(3) 8_565 6_557 ? N1 Cs1 C1 134.4(3) . 6_557 ? N1 Cs1 C1 134.4(3) 8_565 3_456 ? N1 Cs1 C1 152.5(3) . 3_456 ? C1 Cs1 C1 24.2(4) 6_557 3_456 ? N1 Cs1 C12 132.7(3) 8_565 6_557 ? N1 Cs1 C12 80.2(3) . 6_557 ? C1 Cs1 C12 67.2(3) 6_557 6_557 ? C1 Cs1 C12 90.6(3) 3_456 6_557 ? N1 Cs1 C4 20.1(2) 8_565 8_565 ? N1 Cs1 C4 73.1(2) . 8_565 ? C1 Cs1 C4 142.1(3) 6_557 8_565 ? C1 Cs1 C4 119.0(2) 3_456 8_565 ? C12 Cs1 C4 150.4(3) 6_557 8_565 ? N1 Cs1 C1 16.0(2) 8_565 8_565 ? N1 Cs1 C1 37.4(2) . 8_565 ? C1 Cs1 C1 154.8(2) 6_557 8_565 ? C1 Cs1 C1 145.8(3) 3_456 8_565 ? C12 Cs1 C1 117.2(3) 6_557 8_565 ? C4 Cs1 C1 36.0(2) 8_565 8_565 ? C11 C10 C5 114.3(11) . . ? C11 C10 C12 111.2(14) . . ? C5 C10 C12 109.5(13) . . ? C11 C10 H10 107.1 . . ? C5 C10 H10 107.1 . . ? C12 C10 H10 107.1 . . ? C18A C16 C17 126(2) . . ? C18A C16 C17A 114(2) . . ? C17 C16 C17A 21.6(19) . . ? C18A C16 C9 114.9(13) . . ? C17 C16 C9 113.5(12) . . ? C17A C16 C9 111.9(12) . . ? C18A C16 C18 26.3(19) . . ? C17 C16 C18 111.7(18) . . ? C17A C16 C18 94(2) . . ? C9 C16 C18 111.3(12) . . ? C18A C16 H16 80.9 . . ? C17 C16 H16 106.6 . . ? C17A C16 H16 125.4 . . ? C9 C16 H16 106.6 . . ? C18 C16 H16 106.6 . . ? C18A C16 H16A 104.9 . . ? C17 C16 H16A 84.0 . . ? C17A C16 H16A 104.9 . . ? C9 C16 H16A 104.9 . . ? C18 C16 H16A 128.8 . . ? H16 C16 H16A 26.2 . . ? C6 C5 C4 119.4(12) . . ? C6 C5 C10 120.7(12) . . ? C4 C5 C10 119.9(10) . . ? C8 C9 C4 119.6(13) . . ? C8 C9 C16 120.9(13) . . ? C4 C9 C16 119.4(11) . . ? 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 . . ? C7 C6 C5 122.4(13) . . ? C7 C6 H6 118.8 . . ? C5 C6 H6 118.8 . . ? C9 C8 C7 123.6(14) . . ? C9 C8 H8 118.2 . . ? C7 C8 H8 118.2 . . ? C9 C4 N1 120.7(11) . . ? C9 C4 C5 118.6(11) . . ? N1 C4 C5 120.2(11) . . ? 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 . . ? 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 . . ? C6 C7 C8 116.4(11) . . ? C6 C7 C13 122.1(14) . . ? C8 C7 C13 121.3(14) . . ? C7 C13 C14 112.1(15) . . ? C7 C13 C15 109.9(14) . . ? C14 C13 C15 111.6(15) . . ? C7 C13 H13 107.7 . . ? C14 C13 H13 107.7 . . ? C15 C13 H13 107.7 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? 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 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? C1 N1 C4 120.5(9) . . ? C1 N1 Cs1 125.9(7) . . ? C4 N1 Cs1 113.2(6) . . ? C2 C3 C3 120.4(7) . 8_565 ? C2 C3 Cs1 77.5(7) . 6_657 ? C3 C3 Cs1 78.6(2) 8_565 6_657 ? C2 C3 H3 119.8 . . ? C3 C3 H3 119.8 8_565 . ? Cs1 C3 H3 114.6 6_657 . ? C3 C2 C1 121.7(11) . . ? C3 C2 Cs1 80.4(7) . 6_657 ? C1 C2 Cs1 74.9(6) . 6_657 ? C3 C2 H2 119.1 . . ? C1 C2 H2 119.1 . . ? Cs1 C2 H2 116.0 6_657 . ? N1 C1 C2 124.8(10) . . ? N1 C1 C1 117.4(6) . 8_565 ? C2 C1 C1 117.8(7) . 8_565 ? N1 C1 Cs1 110.9(7) . 6_657 ? C2 C1 Cs1 81.4(7) . 6_657 ? C1 C1 Cs1 77.88(18) 8_565 6_657 ? C16 C17A H17D 109.5 . . ? C16 C17A H17E 109.5 . . ? H17D C17A H17E 109.5 . . ? C16 C17A H17F 109.5 . . ? H17D C17A H17F 109.5 . . ? H17E C17A H17F 109.5 . . ? C16 C18A H18D 109.5 . . ? C16 C18A H18E 109.5 . . ? H18D C18A H18E 109.5 . . ? C16 C18A H18F 109.5 . . ? H18D C18A H18F 109.5 . . ? H18E C18A H18F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 C10 C5 C6 -41.9(18) . . . . ? C12 C10 C5 C6 83.6(16) . . . . ? C11 C10 C5 C4 138.7(14) . . . . ? C12 C10 C5 C4 -95.8(14) . . . . ? C18A C16 C9 C8 82(3) . . . . ? C17 C16 C9 C8 -73(3) . . . . ? C17A C16 C9 C8 -50(3) . . . . ? C18 C16 C9 C8 54(2) . . . . ? C18A C16 C9 C4 -97(3) . . . . ? C17 C16 C9 C4 107(2) . . . . ? C17A C16 C9 C4 131(3) . . . . ? C18 C16 C9 C4 -126(2) . . . . ? C4 C5 C6 C7 0.6(19) . . . . ? C10 C5 C6 C7 -178.8(12) . . . . ? C4 C9 C8 C7 0(2) . . . . ? C16 C9 C8 C7 -179.2(12) . . . . ? C8 C9 C4 N1 -172.0(11) . . . . ? C16 C9 C4 N1 7.6(15) . . . . ? C8 C9 C4 C5 -0.4(17) . . . . ? C16 C9 C4 C5 179.3(10) . . . . ? C6 C5 C4 C9 -0.1(17) . . . . ? C10 C5 C4 C9 179.3(11) . . . . ? C6 C5 C4 N1 171.6(10) . . . . ? C10 C5 C4 N1 -9.0(16) . . . . ? C5 C6 C7 C8 -1(2) . . . . ? C5 C6 C7 C13 -175.6(14) . . . . ? C9 C8 C7 C6 0(2) . . . . ? C9 C8 C7 C13 175.2(14) . . . . ? C6 C7 C13 C14 -53(2) . . . . ? C8 C7 C13 C14 132.2(17) . . . . ? C6 C7 C13 C15 72(2) . . . . ? C8 C7 C13 C15 -103.0(19) . . . . ? C9 C4 N1 C1 -84.2(13) . . . . ? C5 C4 N1 C1 104.3(13) . . . . ? C9 C4 N1 Cs1 88.6(11) . . . . ? C5 C4 N1 Cs1 -83.0(10) . . . . ? N1 Cs1 N1 C1 3.2(10) 8_565 . . . ? C1 Cs1 N1 C1 -141.8(8) 6_557 . . . ? C1 Cs1 N1 C1 -114.0(9) 3_456 . . . ? C12 Cs1 N1 C1 174.1(10) 6_557 . . . ? C4 Cs1 N1 C1 7.1(9) 8_565 . . . ? C1 Cs1 N1 C1 1.8(5) 8_565 . . . ? Cs1 Cs1 N1 C1 -54.6(8) 6_657 . . . ? Cs1 Cs1 N1 C1 151.9(7) 6_557 . . . ? N1 Cs1 N1 C4 -169.1(7) 8_565 . . . ? C1 Cs1 N1 C4 45.9(9) 6_557 . . . ? C1 Cs1 N1 C4 73.7(10) 3_456 . . . ? C12 Cs1 N1 C4 1.8(8) 6_557 . . . ? C4 Cs1 N1 C4 -165.2(10) 8_565 . . . ? C1 Cs1 N1 C4 -170.5(10) 8_565 . . . ? Cs1 Cs1 N1 C4 133.1(9) 6_657 . . . ? Cs1 Cs1 N1 C4 -20.4(10) 6_557 . . . ? C3 C3 C2 C1 -3.1(14) 8_565 . . . ? Cs1 C3 C2 C1 65.5(11) 6_657 . . . ? C3 C3 C2 Cs1 -68.6(5) 8_565 . . 6_657 ? C4 N1 C1 C2 -10.6(18) . . . . ? Cs1 N1 C1 C2 177.7(8) . . . . ? C4 N1 C1 C1 168.6(8) . . . 8_565 ? Cs1 N1 C1 C1 -3.2(10) . . . 8_565 ? C4 N1 C1 Cs1 -104.6(10) . . . 6_657 ? Cs1 N1 C1 Cs1 83.6(8) . . . 6_657 ? C3 C2 C1 N1 -177.8(12) . . . . ? Cs1 C2 C1 N1 -109.5(11) 6_657 . . . ? C3 C2 C1 C1 3.1(14) . . . 8_565 ? Cs1 C2 C1 C1 71.4(4) 6_657 . . 8_565 ? C3 C2 C1 Cs1 -68.3(11) . . . 6_657 ? _diffrn_measured_fraction_theta_max 0.915 _diffrn_reflns_theta_full 66.59 _diffrn_measured_fraction_theta_full 0.915 _refine_diff_density_max 1.175 _refine_diff_density_min -1.707 _refine_diff_density_rms 0.163 _vrf_PLAT029_I ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.915 RESPONSE: ...completeness is low due to instrument error. ; _vrf_PLAT973_I ; PROBLEM: Large Calcd. Positive Residual Density on Cs1 2.36 eA-3 RESPONSE: ...large Q peak close to Cs1 of no chemical significance. ; #=== End of CIF _database_code_depnum_ccdc_archive 'CCDC 961091'