# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 #===END #============================================================================== # Attachment 'web_deposit_cif_file_1_chuanjianghu_1319705833.shelxl.cif' data_general2 _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 #TrackingRef 'web_deposit_cif_file_1_chuanjianghu_1319705833.shelxl.cif' _audit_creation_date 2011-10-27 _audit_creation_method 'SHELXL 97' _audit_update_record ? #============================================================================== # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_coeditor_code ? #============================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'Chuan-Jiang Hu' _publ_contact_author_email cjhu@suda.edu.cn _publ_contact_author_fax '0086 (0)512 65880903' _publ_contact_author_phone '0086 (0)512 65880903' _publ_contact_author_address ; College of Chemistry, Chemical Engineering and Materials Science Suzhou University, Suzhou 215123, Jiangsu, P. R. China ; _publ_requested_category ? _publ_requested_coeditor_name ? #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; ENTER SECTION TITLE ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Xiaoxu Kai' ; FIRST AUTHORS FOOTNOTES ; ; FIRST AUTHORS ADDRESS ; 'Jiaxun Jiang' '' '' _publ_section_synopsis ; ENTER SYNOPSIS ; #============================================================================== # TEXT _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Rigaku/MSC and Rigaku Corporation. (2001). CrystalStructure. Single Crystal Structure Analysis Software. Version 3.00. Rigaku/MSC, 9009 New Trails Drive, The Woodlands, TX, USA 77381-5209. Rigaku, 3-9-12 Akishima, Tokyo 196-8666, Japan. Watkin, D.J., Prout, C.K. Carruthers, J.R. & Betteridge, P.W., CRYSTALS Issue 10, Chemical Crystallography Laboratory, Oxford, UK. ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; #============================================================================== data_final _database_code_depnum_ccdc_archive 'CCDC 851199' #TrackingRef '8392_web_deposit_cif_file_0_chuanjianghu_1322533151.final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common bisporphyrin _chemical_melting_point 'not measured' _chemical_formula_moiety '2(C93 H60 N8 O), 3(C H2 Cl2)' _chemical_formula_sum 'C189 H126 Cl6 N16 O2' _chemical_formula_weight 2865.78 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' 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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.992(3) _cell_length_b 14.142(3) _cell_length_c 38.237(8) _cell_angle_alpha 90.46(3) _cell_angle_beta 95.22(3) _cell_angle_gamma 96.13(3) _cell_volume 7490(3) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 33148 _cell_measurement_theta_min 3.0196 _cell_measurement_theta_max 27.5204 _exptl_crystal_description Prism _exptl_crystal_colour black _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.158 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2728 _exptl_absorpt_coefficient_mu 0.069 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9695 _exptl_absorpt_correction_T_max 0.9897 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 62410 _diffrn_reflns_av_R_equivalents 0.0794 _diffrn_reflns_av_sigmaI/netI 0.1136 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 25.00 _reflns_number_total 26252 _reflns_number_gt 15545 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0720P)^2^+1.0950P] 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 26252 _refine_ls_number_parameters 1825 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.1331 _refine_ls_R_factor_gt 0.0875 _refine_ls_wR_factor_ref 0.2267 _refine_ls_wR_factor_gt 0.2013 _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_restrained_S_all 1.115 _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 N11 N 0.1094(2) 0.1746(2) 0.86189(7) 0.0345(7) Uani 1 1 d . . . N12 N 0.1525(2) 0.0486(2) 0.80545(8) 0.0369(7) Uani 1 1 d . . . H12 H 0.1188 0.0415 0.8235 0.044 Uiso 1 1 calc R . . N13 N 0.0118(2) -0.0960(2) 0.83047(8) 0.0382(7) Uani 1 1 d . . . N14 N -0.0320(2) 0.0263(2) 0.88631(8) 0.0368(7) Uani 1 1 d . . . H14 H 0.0099 0.0289 0.8708 0.044 Uiso 1 1 calc R . . C1A1 C 0.0735(3) 0.2250(2) 0.88733(9) 0.0333(8) Uani 1 1 d . . . C1A2 C 0.1859(3) 0.2280(2) 0.85023(9) 0.0339(8) Uani 1 1 d . . . C1A3 C 0.2182(3) 0.1245(3) 0.80054(9) 0.0368(9) Uani 1 1 d . . . C1A4 C 0.1469(3) -0.0160(3) 0.77748(9) 0.0385(9) Uani 1 1 d . . . C1A5 C 0.0303(3) -0.1407(3) 0.80033(9) 0.0364(9) Uani 1 1 d . . . C1A6 C -0.0496(3) -0.1599(3) 0.84660(10) 0.0371(9) Uani 1 1 d . . . C1A7 C -0.0874(3) -0.0548(3) 0.89480(10) 0.0410(9) Uani 1 1 d . . . C1A8 C -0.0521(3) 0.1032(3) 0.90582(9) 0.0368(9) Uani 1 1 d . . . C1B1 C 0.1370(3) 0.3179(3) 0.89676(9) 0.0346(8) Uani 1 1 d . . . H1B1 H 0.0983 0.3723 0.8978 0.042 Uiso 1 1 calc R . . C1B2 C 0.2012(3) 0.3267(2) 0.86679(9) 0.0328(8) Uani 1 1 d . . . H1B2 H 0.2697 0.3456 0.8751 0.039 Uiso 1 1 calc R . . C1B3 C 0.2549(3) 0.1082(3) 0.76759(10) 0.0453(10) Uani 1 1 d . . . H1B3 H 0.3014 0.1490 0.7572 0.054 Uiso 1 1 calc R . . C1B4 C 0.2115(3) 0.0245(3) 0.75382(10) 0.0438(10) Uani 1 1 d . . . H1B4 H 0.2224 -0.0025 0.7322 0.053 Uiso 1 1 calc R . . C1B5 C -0.0223(3) -0.2354(3) 0.79731(11) 0.0442(10) Uani 1 1 d . . . H1B5 H -0.0231 -0.2795 0.7787 0.053 Uiso 1 1 calc R . . C1B6 C -0.0693(3) -0.2473(3) 0.82611(10) 0.0425(10) Uani 1 1 d . . . H1B6 H -0.1079 -0.3024 0.8320 0.051 Uiso 1 1 calc R . . C1B7 C -0.1455(3) -0.0282(3) 0.92097(10) 0.0452(10) Uani 1 1 d . . . H1B7 H -0.1908 -0.0693 0.9318 0.054 Uiso 1 1 calc R . . C1B8 C -0.1246(3) 0.0673(3) 0.92778(10) 0.0475(10) Uani 1 1 d . . . H1B8 H -0.1529 0.1030 0.9441 0.057 Uiso 1 1 calc R . . C1M1 C 0.2391(3) 0.2068(3) 0.82301(9) 0.0345(8) Uani 1 1 d . . . C1M2 C 0.0910(3) -0.1033(3) 0.77530(9) 0.0382(9) Uani 1 1 d . . . C1M3 C -0.0927(3) -0.1424(3) 0.87786(10) 0.0396(9) Uani 1 1 d . . . C1M4 C -0.0044(3) 0.1955(3) 0.90598(9) 0.0354(9) Uani 1 1 d . . . C110 C 0.3249(3) 0.2733(3) 0.81502(9) 0.0374(9) Uani 1 1 d . . . C111 C 0.4102(3) 0.2359(3) 0.81177(10) 0.0445(10) Uani 1 1 d . . . H111 H 0.4141 0.1717 0.8174 0.053 Uiso 1 1 calc R . . C112 C 0.4924(3) 0.2892(3) 0.80038(11) 0.0551(12) Uani 1 1 d . . . H112 H 0.5506 0.2620 0.7995 0.066 Uiso 1 1 calc R . . C113 C 0.4855(3) 0.3810(3) 0.79068(12) 0.0562(12) Uani 1 1 d . . . H113 H 0.5388 0.4162 0.7820 0.067 Uiso 1 1 calc R . . C114 C 0.4005(3) 0.4241(3) 0.79340(10) 0.0475(11) Uani 1 1 d . . . C115 C 0.3932(4) 0.5186(3) 0.78209(11) 0.0547(12) Uani 1 1 d . . . H115 H 0.4464 0.5526 0.7728 0.066 Uiso 1 1 calc R . . C116 C 0.3117(4) 0.5610(3) 0.78430(10) 0.0560(12) Uani 1 1 d . . . H116 H 0.3065 0.6218 0.7751 0.067 Uiso 1 1 calc R . . C117 C 0.2347(3) 0.5130(3) 0.80058(10) 0.0483(11) Uani 1 1 d . . . H117 H 0.1793 0.5437 0.8031 0.058 Uiso 1 1 calc R . . C118 C 0.2385(3) 0.4223(3) 0.81286(9) 0.0376(9) Uani 1 1 d . . . C119 C 0.3199(3) 0.3726(3) 0.80780(9) 0.0401(9) Uani 1 1 d . . . C120 C 0.1653(3) 0.3892(3) 0.83715(9) 0.0386(9) Uani 1 1 d . . . O1 O 0.0825(2) 0.4086(2) 0.83383(7) 0.0511(7) Uani 1 1 d . . . C121 C 0.1004(3) -0.1659(3) 0.74409(10) 0.0423(10) Uani 1 1 d . . . C122 C 0.1421(3) -0.2515(3) 0.74835(12) 0.0520(11) Uani 1 1 d . . . H122 H 0.1668 -0.2686 0.7708 0.062 Uiso 1 1 calc R . . C123 C 0.1475(4) -0.3104(3) 0.72016(12) 0.0634(13) Uani 1 1 d . . . H123 H 0.1748 -0.3679 0.7236 0.076 Uiso 1 1 calc R . . C124 C 0.1131(4) -0.2862(4) 0.68669(12) 0.0724(15) Uani 1 1 d . . . H124 H 0.1172 -0.3267 0.6674 0.087 Uiso 1 1 calc R . . C125 C 0.0732(5) -0.2023(4) 0.68202(12) 0.0781(17) Uani 1 1 d . . . H125 H 0.0507 -0.1845 0.6594 0.094 Uiso 1 1 calc R . . C126 C 0.0658(4) -0.1433(3) 0.71080(11) 0.0628(13) Uani 1 1 d . . . H126 H 0.0366 -0.0869 0.7073 0.075 Uiso 1 1 calc R . . C131 C -0.1473(3) -0.2230(3) 0.89530(11) 0.0448(10) Uani 1 1 d . . . C132 C -0.2279(3) -0.2768(3) 0.87860(12) 0.0521(11) Uani 1 1 d . . . H132 H -0.2519 -0.2619 0.8558 0.063 Uiso 1 1 calc R . . C133 C -0.2729(3) -0.3531(3) 0.89597(13) 0.0555(12) Uani 1 1 d . . . H133 H -0.3263 -0.3907 0.8846 0.067 Uiso 1 1 calc R . . C134 C -0.2394(3) -0.3735(3) 0.92971(13) 0.0528(12) Uani 1 1 d . . . H134 H -0.2702 -0.4252 0.9411 0.063 Uiso 1 1 calc R . . C135 C -0.1627(3) -0.3201(3) 0.94669(12) 0.0527(11) Uani 1 1 d . . . H135 H -0.1413 -0.3343 0.9699 0.063 Uiso 1 1 calc R . . C136 C -0.1158(3) -0.2450(3) 0.92998(11) 0.0486(10) Uani 1 1 d . . . H136 H -0.0625 -0.2083 0.9418 0.058 Uiso 1 1 calc R . . C141 C -0.0441(3) 0.2669(3) 0.92841(10) 0.0383(9) Uani 1 1 d . . . C142 C -0.1022(3) 0.3309(3) 0.91243(11) 0.0483(10) Uani 1 1 d . . . H142 H -0.1134 0.3307 0.8878 0.058 Uiso 1 1 calc R . . C143 C -0.1437(3) 0.3949(3) 0.93217(14) 0.0588(12) Uani 1 1 d . . . H143 H -0.1836 0.4370 0.9209 0.071 Uiso 1 1 calc R . . C144 C -0.1269(4) 0.3976(3) 0.96834(14) 0.0637(13) Uani 1 1 d . . . H144 H -0.1542 0.4420 0.9817 0.076 Uiso 1 1 calc R . . C145 C -0.0695(4) 0.3340(3) 0.98457(12) 0.0604(13) Uani 1 1 d . . . H145 H -0.0592 0.3341 1.0092 0.072 Uiso 1 1 calc R . . C146 C -0.0270(3) 0.2700(3) 0.96487(10) 0.0489(11) Uani 1 1 d . . . H146 H 0.0135 0.2285 0.9762 0.059 Uiso 1 1 calc R . . N21 N 0.2977(2) 0.3248(2) 0.98182(7) 0.0352(7) Uani 1 1 d . . . H21 H 0.3359 0.3505 0.9993 0.042 Uiso 1 1 calc R . . N22 N 0.4149(2) 0.2476(2) 1.04148(8) 0.0374(7) Uani 1 1 d . . . N23 N 0.4764(2) 0.4373(2) 1.07011(8) 0.0378(7) Uani 1 1 d . . . H23 H 0.4535 0.4138 1.0496 0.045 Uiso 1 1 calc R . . N24 N 0.3677(2) 0.5123(2) 1.00830(7) 0.0353(7) Uani 1 1 d . . . C2A1 C 0.2505(3) 0.3742(3) 0.95608(9) 0.0320(8) Uani 1 1 d . . . C2A2 C 0.2758(3) 0.2297(3) 0.97586(9) 0.0343(8) Uani 1 1 d . . . C2A3 C 0.3737(3) 0.1635(3) 1.02606(10) 0.0387(9) Uani 1 1 d . . . C2A4 C 0.4666(3) 0.2235(3) 1.07196(10) 0.0427(10) Uani 1 1 d . . . C2A5 C 0.5118(3) 0.3865(3) 1.09719(10) 0.0397(9) Uani 1 1 d . . . C2A6 C 0.4817(3) 0.5316(3) 1.07988(10) 0.0390(9) Uani 1 1 d . . . C2A7 C 0.4028(3) 0.5971(3) 1.02521(10) 0.0384(9) Uani 1 1 d . . . C2A8 C 0.3158(3) 0.5368(3) 0.97812(9) 0.0354(9) Uani 1 1 d . . . C2B1 C 0.1946(3) 0.3044(2) 0.93168(9) 0.0321(8) Uani 1 1 d . . . C2B2 C 0.2121(3) 0.2178(3) 0.94431(9) 0.0354(9) Uani 1 1 d . . . H2B2 H 0.1864 0.1590 0.9339 0.042 Uiso 1 1 calc R . . C2B3 C 0.4017(3) 0.0851(3) 1.04742(10) 0.0496(11) Uani 1 1 d . . . H2B3 H 0.3832 0.0201 1.0425 0.059 Uiso 1 1 calc R . . C2B4 C 0.4584(3) 0.1215(3) 1.07523(10) 0.0483(11) Uani 1 1 d . . . H2B4 H 0.4875 0.0873 1.0935 0.058 Uiso 1 1 calc R . . C2B5 C 0.5423(3) 0.4507(3) 1.12599(10) 0.0440(10) Uani 1 1 d . . . H2B5 H 0.5705 0.4348 1.1481 0.053 Uiso 1 1 calc R . . C2B6 C 0.5233(3) 0.5390(3) 1.11562(10) 0.0421(10) Uani 1 1 d . . . H2B6 H 0.5353 0.5950 1.1294 0.051 Uiso 1 1 calc R . . C2B7 C 0.3772(3) 0.6752(3) 1.00415(10) 0.0402(9) Uani 1 1 d . . . H2B7 H 0.3947 0.7401 1.0094 0.048 Uiso 1 1 calc R . . C2B8 C 0.3231(3) 0.6381(3) 0.97527(10) 0.0400(9) Uani 1 1 d . . . H2B8 H 0.2954 0.6725 0.9567 0.048 Uiso 1 1 calc R . . C2M1 C 0.3089(3) 0.1549(3) 0.99542(9) 0.0375(9) Uani 1 1 d . . . C2M2 C 0.5130(3) 0.2881(3) 1.09811(10) 0.0416(9) Uani 1 1 d . . . C2M3 C 0.4507(3) 0.6059(3) 1.05914(10) 0.0362(9) Uani 1 1 d . . . C2M4 C 0.2568(3) 0.4738(3) 0.95444(9) 0.0368(9) Uani 1 1 d . . . C211 C 0.2710(3) 0.0561(3) 0.98364(10) 0.0414(10) Uani 1 1 d . . . C212 C 0.1731(3) 0.0260(3) 0.98334(11) 0.0524(11) Uani 1 1 d . . . H212 H 0.1312 0.0678 0.9911 0.063 Uiso 1 1 calc R . . C213 C 0.1363(4) -0.0653(4) 0.97166(15) 0.0729(15) Uani 1 1 d . . . H213 H 0.0700 -0.0852 0.9716 0.087 Uiso 1 1 calc R . . C214 C 0.1980(5) -0.1261(3) 0.96027(14) 0.0773(17) Uani 1 1 d . . . H214 H 0.1734 -0.1876 0.9521 0.093 Uiso 1 1 calc R . . C215 C 0.2940(4) -0.0982(3) 0.96065(13) 0.0678(14) Uani 1 1 d . . . H215 H 0.3356 -0.1407 0.9532 0.081 Uiso 1 1 calc R . . C216 C 0.3310(4) -0.0072(3) 0.97195(11) 0.0545(11) Uani 1 1 d . . . H216 H 0.3974 0.0119 0.9717 0.065 Uiso 1 1 calc R . . C221 C 0.5597(3) 0.2446(3) 1.13048(11) 0.0473(10) Uani 1 1 d . . . C222 C 0.6441(4) 0.2038(4) 1.12889(13) 0.0675(14) Uani 1 1 d . . . H222 H 0.6735 0.2053 1.1077 0.081 Uiso 1 1 calc R . . C223 C 0.6867(4) 0.1606(4) 1.15781(15) 0.0803(17) Uani 1 1 d . . . H223 H 0.7447 0.1334 1.1564 0.096 Uiso 1 1 calc R . . C224 C 0.6431(5) 0.1581(4) 1.18874(15) 0.0770(17) Uani 1 1 d . . . H224 H 0.6711 0.1284 1.2084 0.092 Uiso 1 1 calc R . . C225 C 0.5588(4) 0.1987(4) 1.19091(13) 0.0739(16) Uani 1 1 d . . . H225 H 0.5296 0.1971 1.2121 0.089 Uiso 1 1 calc R . . C226 C 0.5168(4) 0.2420(4) 1.16181(12) 0.0639(13) Uani 1 1 d . . . H226 H 0.4591 0.2697 1.1633 0.077 Uiso 1 1 calc R . . C231 C 0.4672(3) 0.7037(3) 1.07609(10) 0.0418(10) Uani 1 1 d . . . C232 C 0.5588(3) 0.7476(3) 1.08398(10) 0.0452(10) Uani 1 1 d . . . H232 H 0.6120 0.7167 1.0786 0.054 Uiso 1 1 calc R . . C233 C 0.5739(4) 0.8369(3) 1.09987(12) 0.0570(12) Uani 1 1 d . . . H233 H 0.6371 0.8666 1.1050 0.068 Uiso 1 1 calc R . . C234 C 0.4972(4) 0.8818(3) 1.10808(13) 0.0684(14) Uani 1 1 d U . . H234 H 0.5076 0.9414 1.1196 0.082 Uiso 1 1 calc R . . C235 C 0.4050(4) 0.8403(4) 1.09959(14) 0.0759(15) Uani 1 1 d U . . H235 H 0.3522 0.8722 1.1047 0.091 Uiso 1 1 calc R . . C236 C 0.3900(3) 0.7517(3) 1.08352(13) 0.0598(12) Uani 1 1 d . . . H236 H 0.3266 0.7235 1.0775 0.072 Uiso 1 1 calc R . . C241 C 0.1911(3) 0.5204(2) 0.92830(9) 0.0330(8) Uani 1 1 d . . . C242 C 0.2241(3) 0.5680(3) 0.89963(10) 0.0470(10) Uani 1 1 d . . . H242 H 0.2883 0.5656 0.8946 0.056 Uiso 1 1 calc R . . C243 C 0.1636(5) 0.6195(3) 0.87813(12) 0.0671(15) Uani 1 1 d . . . H243 H 0.1868 0.6523 0.8588 0.081 Uiso 1 1 calc R . . C244 C 0.0689(4) 0.6217(4) 0.88562(15) 0.0713(15) Uani 1 1 d . . . H244 H 0.0276 0.6573 0.8716 0.086 Uiso 1 1 calc R . . C245 C 0.0355(4) 0.5724(3) 0.91330(15) 0.0640(13) Uani 1 1 d . . . H245 H -0.0294 0.5724 0.9178 0.077 Uiso 1 1 calc R . . C246 C 0.0960(3) 0.5223(3) 0.93489(11) 0.0445(10) Uani 1 1 d . . . H246 H 0.0723 0.4895 0.9541 0.053 Uiso 1 1 calc R . . N31 N 0.7803(2) 0.8564(2) 0.35812(7) 0.0356(7) Uani 1 1 d . . . N32 N 0.8927(2) 0.7871(2) 0.30471(8) 0.0363(7) Uani 1 1 d . . . H32 H 0.9022 0.8308 0.3212 0.044 Uiso 1 1 calc R . . N33 N 1.0466(2) 0.9407(2) 0.32728(8) 0.0395(8) Uani 1 1 d . . . N34 N 0.9379(2) 1.0065(2) 0.38080(8) 0.0392(8) Uani 1 1 d . . . H34 H 0.9306 0.9601 0.3654 0.047 Uiso 1 1 calc R . . C3A1 C 0.7351(3) 0.9019(3) 0.38293(9) 0.0344(8) Uani 1 1 d . . . C3A2 C 0.7231(3) 0.7750(3) 0.34830(9) 0.0316(8) Uani 1 1 d . . . C3A3 C 0.8173(3) 0.7188(3) 0.30160(9) 0.0355(9) Uani 1 1 d . . . C3A4 C 0.9534(3) 0.7787(3) 0.27820(9) 0.0376(9) Uani 1 1 d . . . C3A5 C 1.0831(3) 0.9093(3) 0.29797(9) 0.0384(9) Uani 1 1 d . . . C3A6 C 1.1157(3) 1.0072(3) 0.34247(10) 0.0396(9) Uani 1 1 d . . . C3A7 C 1.0228(3) 1.0636(3) 0.38921(10) 0.0424(10) Uani 1 1 d . . . C3A8 C 0.8662(3) 1.0326(3) 0.39989(10) 0.0406(9) Uani 1 1 d . . . C3B1 C 0.6472(3) 0.8433(3) 0.39377(9) 0.0350(8) Uani 1 1 d . . . H3B1 H 0.5921 0.8814 0.3948 0.042 Uiso 1 1 calc R . . C3B2 C 0.6283(3) 0.7674(3) 0.36472(9) 0.0328(8) Uani 1 1 d . . . H3B2 H 0.6124 0.7033 0.3742 0.039 Uiso 1 1 calc R . . C3B3 C 0.8285(3) 0.6635(3) 0.27089(9) 0.0383(9) Uani 1 1 d U . . H3B3 H 0.7869 0.6105 0.2620 0.046 Uiso 1 1 calc R . . C3B4 C 0.9097(3) 0.7011(3) 0.25696(10) 0.0425(10) Uani 1 1 d U . . H3B4 H 0.9331 0.6791 0.2365 0.051 Uiso 1 1 calc R . . C3B5 C 1.1778(3) 0.9585(3) 0.29429(11) 0.0456(10) Uani 1 1 d . . . H3B5 H 1.2176 0.9500 0.2762 0.055 Uiso 1 1 calc R . . C3B6 C 1.1972(3) 1.0187(3) 0.32187(10) 0.0452(10) Uani 1 1 d . . . H3B6 H 1.2537 1.0606 0.3269 0.054 Uiso 1 1 calc R . . C3B7 C 1.0018(3) 1.1291(3) 0.41545(11) 0.0484(11) Uani 1 1 d . . . H3B7 H 1.0463 1.1768 0.4266 0.058 Uiso 1 1 calc R . . C3B8 C 0.9085(3) 1.1119(3) 0.42165(11) 0.0473(10) Uani 1 1 d . . . H3B8 H 0.8766 1.1459 0.4375 0.057 Uiso 1 1 calc R . . C3M1 C 0.7388(3) 0.7082(3) 0.32275(9) 0.0355(9) Uani 1 1 d . . . C3M2 C 1.0396(3) 0.8351(3) 0.27481(9) 0.0391(9) Uani 1 1 d . . . C3M3 C 1.1066(3) 1.0612(3) 0.37334(10) 0.0426(10) Uani 1 1 d . . . C3M4 C 0.7729(3) 0.9862(3) 0.40071(10) 0.0397(9) Uani 1 1 d . . . C310 C 0.6700(3) 0.6200(3) 0.31765(9) 0.0370(9) Uani 1 1 d . . . C311 C 0.7076(3) 0.5338(3) 0.31855(9) 0.0420(10) Uani 1 1 d . . . H311 H 0.7746 0.5332 0.3235 0.050 Uiso 1 1 calc R . . C312 C 0.6496(3) 0.4464(3) 0.31230(10) 0.0483(11) Uani 1 1 d . . . H312 H 0.6770 0.3888 0.3152 0.058 Uiso 1 1 calc R . . C313 C 0.5541(3) 0.4459(3) 0.30216(11) 0.0504(11) Uani 1 1 d . . . H313 H 0.5168 0.3877 0.2964 0.060 Uiso 1 1 calc R . . C314 C 0.5093(3) 0.5313(3) 0.30012(10) 0.0456(10) Uani 1 1 d . . . C315 C 0.4108(3) 0.5312(3) 0.28892(11) 0.0532(12) Uani 1 1 d . . . H316 H 0.3740 0.4733 0.2822 0.064 Uiso 1 1 calc R . . C316 C 0.3685(3) 0.6116(4) 0.28757(11) 0.0585(13) Uani 1 1 d . . . H317 H 0.3037 0.6100 0.2784 0.070 Uiso 1 1 calc R . . C317 C 0.4198(3) 0.6991(3) 0.29979(10) 0.0490(11) Uani 1 1 d . . . H318 H 0.3885 0.7548 0.2995 0.059 Uiso 1 1 calc R . . C318 C 0.5152(3) 0.7022(3) 0.31207(10) 0.0412(9) Uani 1 1 d . . . C319 C 0.5665(3) 0.6200(3) 0.31038(9) 0.0396(9) Uani 1 1 d . . . C320 C 0.5565(3) 0.7879(3) 0.33373(10) 0.0393(9) Uani 1 1 d . . . O2 O 0.5343(2) 0.8676(2) 0.32828(7) 0.0532(8) Uani 1 1 d . . . C321 C 1.09519(19) 0.8103(2) 0.24459(6) 0.0448(10) Uani 1 1 d GU . . C322 C 1.0696(2) 0.8426(3) 0.21116(7) 0.0827(16) Uani 1 1 d GU . . H322 H 1.0157 0.8767 0.2072 0.099 Uiso 1 1 calc R . . C323 C 1.1239(2) 0.8246(3) 0.18363(5) 0.0892(17) Uani 1 1 d GU . . H323 H 1.1066 0.8465 0.1610 0.107 Uiso 1 1 calc R . . C324 C 1.2037(2) 0.7742(3) 0.18952(6) 0.0650(13) Uani 1 1 d GU . . H324 H 1.2403 0.7620 0.1709 0.078 Uiso 1 1 calc R . . C325 C 1.2292(2) 0.7418(2) 0.22294(8) 0.0687(13) Uani 1 1 d GU . . H325 H 1.2832 0.7077 0.2269 0.082 Uiso 1 1 calc R . . C326 C 1.1750(2) 0.7598(2) 0.25048(6) 0.0616(12) Uani 1 1 d GU . . H326 H 1.1923 0.7380 0.2731 0.074 Uiso 1 1 calc R . . C331 C 1.1934(3) 1.1217(3) 0.39031(11) 0.0442(10) Uani 1 1 d . . . C332 C 1.2420(3) 1.1946(3) 0.37386(13) 0.0598(12) Uani 1 1 d . . . H332 H 1.2210 1.2100 0.3508 0.072 Uiso 1 1 calc R . . C333 C 1.3238(4) 1.2468(3) 0.39154(17) 0.0707(15) Uani 1 1 d . . . H333 H 1.3589 1.2955 0.3799 0.085 Uiso 1 1 calc R . . C334 C 1.3522(4) 1.2270(4) 0.42545(18) 0.0743(16) Uani 1 1 d . . . H334 H 1.4059 1.2630 0.4373 0.089 Uiso 1 1 calc R . . C335 C 1.3034(4) 1.1556(4) 0.44224(14) 0.0681(14) Uani 1 1 d . . . H335 H 1.3237 1.1419 0.4656 0.082 Uiso 1 1 calc R . . C336 C 1.2252(3) 1.1038(3) 0.42521(12) 0.0536(11) Uani 1 1 d . . . H336 H 1.1916 1.0547 0.4371 0.064 Uiso 1 1 calc R . . C341 C 0.7094(3) 1.0313(3) 0.42391(11) 0.0434(10) Uani 1 1 d . . . C342 C 0.7176(3) 1.0203(4) 0.46036(12) 0.0594(12) Uani 1 1 d . . . H342 H 0.7611 0.9804 0.4709 0.071 Uiso 1 1 calc R . . C343 C 0.6609(4) 1.0689(4) 0.48106(14) 0.0706(15) Uani 1 1 d . . . H343 H 0.6678 1.0626 0.5056 0.085 Uiso 1 1 calc R . . C344 C 0.5953(4) 1.1257(4) 0.46609(16) 0.0745(16) Uani 1 1 d . . . H344 H 0.5568 1.1573 0.4802 0.089 Uiso 1 1 calc R . . C345 C 0.5865(4) 1.1362(4) 0.43032(16) 0.0726(15) Uani 1 1 d . . . H345 H 0.5421 1.1754 0.4199 0.087 Uiso 1 1 calc R . . C346 C 0.6430(3) 1.0888(3) 0.40951(14) 0.0584(12) Uani 1 1 d . . . H346 H 0.6358 1.0961 0.3850 0.070 Uiso 1 1 calc R . . N41 N 0.6724(2) 0.7117(2) 0.47902(8) 0.0356(7) Uani 1 1 d . . . H41 H 0.6535 0.6788 0.4968 0.043 Uiso 1 1 calc R . . N42 N 0.7706(2) 0.6082(2) 0.53583(8) 0.0385(7) Uani 1 1 d . . . N43 N 0.5881(2) 0.5419(2) 0.56356(8) 0.0378(7) Uani 1 1 d . . . H43 H 0.6035 0.5604 0.5430 0.045 Uiso 1 1 calc R . . N44 N 0.4916(2) 0.6387(2) 0.50509(7) 0.0353(7) Uani 1 1 d . . . C4A1 C 0.6119(3) 0.7494(2) 0.45361(9) 0.0331(8) Uani 1 1 d . . . C4A2 C 0.7662(3) 0.7333(3) 0.47229(9) 0.0361(9) Uani 1 1 d . . . C4A3 C 0.8505(3) 0.6468(3) 0.52043(10) 0.0402(9) Uani 1 1 d . . . C4A4 C 0.8061(3) 0.5624(3) 0.56519(10) 0.0427(10) Uani 1 1 d . . . C4A5 C 0.6513(3) 0.5150(3) 0.59046(9) 0.0377(9) Uani 1 1 d . . . C4A6 C 0.4971(3) 0.5348(3) 0.57440(10) 0.0379(9) Uani 1 1 d . . . C4A7 C 0.4119(3) 0.6038(3) 0.52164(9) 0.0348(9) Uani 1 1 d . . . C4A8 C 0.4569(3) 0.6848(3) 0.47576(9) 0.0351(9) Uani 1 1 d . . . C4B1 C 0.6732(3) 0.7980(2) 0.42884(9) 0.0332(8) Uani 1 1 d . . . C4B2 C 0.7656(3) 0.7860(3) 0.44068(9) 0.0382(9) Uani 1 1 d . . . H4B2 H 0.8207 0.8090 0.4297 0.046 Uiso 1 1 calc R . . C4B3 C 0.9373(3) 0.6213(3) 0.53972(11) 0.0523(11) Uani 1 1 d . . . H4B3 H 1.0009 0.6383 0.5342 0.063 Uiso 1 1 calc R . . C4B4 C 0.9103(3) 0.5687(3) 0.56705(11) 0.0532(11) Uani 1 1 d . . . H4B4 H 0.9512 0.5413 0.5840 0.064 Uiso 1 1 calc R . . C4B5 C 0.5953(3) 0.4884(3) 0.61932(10) 0.0435(10) Uani 1 1 d . . . H4B5 H 0.6192 0.4663 0.6412 0.052 Uiso 1 1 calc R . . C4B6 C 0.5021(3) 0.5010(3) 0.60939(10) 0.0430(10) Uani 1 1 d . . . H4B6 H 0.4499 0.4895 0.6232 0.052 Uiso 1 1 calc R . . C4B7 C 0.3249(3) 0.6240(3) 0.50125(10) 0.0397(9) Uani 1 1 d . . . H4B7 H 0.2611 0.6057 0.5064 0.048 Uiso 1 1 calc R . . C4B8 C 0.3528(3) 0.6741(3) 0.47338(10) 0.0421(10) Uani 1 1 d . . . H4B8 H 0.3116 0.6978 0.4555 0.051 Uiso 1 1 calc R . . C4M1 C 0.8490(3) 0.7050(3) 0.49102(10) 0.0407(9) Uani 1 1 d . . . C4M2 C 0.7518(3) 0.5203(3) 0.59092(10) 0.0397(9) Uani 1 1 d . . . C4M3 C 0.4141(3) 0.5608(3) 0.55472(9) 0.0350(8) Uani 1 1 d . . . C4M4 C 0.5119(3) 0.7393(3) 0.45252(9) 0.0357(9) Uani 1 1 d . . . C411 C 0.9436(3) 0.7429(3) 0.47828(10) 0.0422(10) Uani 1 1 d . . . C412 C 0.9756(3) 0.8373(4) 0.48028(12) 0.0592(12) Uani 1 1 d . . . H412 H 0.9378 0.8794 0.4903 0.071 Uiso 1 1 calc R . . C413 C 1.0620(4) 0.8734(5) 0.46801(18) 0.0898(19) Uani 1 1 d . . . H413 H 1.0821 0.9390 0.4696 0.108 Uiso 1 1 calc R . . C414 C 1.1182(4) 0.8124(6) 0.45346(17) 0.094(2) Uani 1 1 d . . . H414 H 1.1764 0.8364 0.4447 0.112 Uiso 1 1 calc R . . C415 C 1.0894(4) 0.7159(5) 0.45171(15) 0.0838(18) Uani 1 1 d . . . H415 H 1.1286 0.6743 0.4421 0.101 Uiso 1 1 calc R . . C416 C 1.0022(3) 0.6799(4) 0.46414(12) 0.0601(12) Uani 1 1 d . . . H416 H 0.9828 0.6141 0.4631 0.072 Uiso 1 1 calc R . . C421 C 0.8075(3) 0.4860(3) 0.62265(10) 0.0474(10) Uani 1 1 d . . . C422 C 0.8181(3) 0.3895(3) 0.62681(11) 0.0548(11) Uani 1 1 d . . . H422 H 0.7859 0.3448 0.6103 0.066 Uiso 1 1 calc R . . C423 C 0.8755(4) 0.3589(4) 0.65500(13) 0.0690(14) Uani 1 1 d . . . H423 H 0.8834 0.2940 0.6571 0.083 Uiso 1 1 calc R . . C424 C 0.9209(4) 0.4229(4) 0.67981(13) 0.0768(16) Uani 1 1 d . . . H424 H 0.9588 0.4019 0.6992 0.092 Uiso 1 1 calc R . . C425 C 0.9106(4) 0.5184(4) 0.67630(14) 0.0834(18) Uani 1 1 d . . . H425 H 0.9422 0.5626 0.6931 0.100 Uiso 1 1 calc R . . C426 C 0.8533(4) 0.5495(4) 0.64767(12) 0.0701(15) Uani 1 1 d . . . H426 H 0.8460 0.6146 0.6456 0.084 Uiso 1 1 calc R . . C431 C 0.3207(3) 0.5461(3) 0.57186(9) 0.0387(9) Uani 1 1 d . . . C432 C 0.2832(3) 0.4572(3) 0.58074(10) 0.0429(10) Uani 1 1 d . . . H432 H 0.3155 0.4044 0.5757 0.052 Uiso 1 1 calc R . . C433 C 0.1978(3) 0.4434(3) 0.59711(11) 0.0511(11) Uani 1 1 d . . . H433 H 0.1732 0.3817 0.6030 0.061 Uiso 1 1 calc R . . C434 C 0.1491(3) 0.5204(4) 0.60467(11) 0.0581(13) Uani 1 1 d . . . H434 H 0.0919 0.5117 0.6159 0.070 Uiso 1 1 calc R . . C435 C 0.1864(3) 0.6101(4) 0.59533(12) 0.0607(12) Uani 1 1 d . . . H435 H 0.1541 0.6630 0.6001 0.073 Uiso 1 1 calc R . . C436 C 0.2710(3) 0.6228(3) 0.57894(12) 0.0528(11) Uani 1 1 d . . . H436 H 0.2950 0.6842 0.5725 0.063 Uiso 1 1 calc R . . C441 C 0.4561(3) 0.7978(3) 0.42757(9) 0.0352(9) Uani 1 1 d . . . C442 C 0.4017(3) 0.7616(3) 0.39774(10) 0.0460(10) Uani 1 1 d . . . H442 H 0.4014 0.6972 0.3915 0.055 Uiso 1 1 calc R . . C443 C 0.3475(3) 0.8191(4) 0.37676(12) 0.0581(12) Uani 1 1 d . . . H443 H 0.3094 0.7933 0.3567 0.070 Uiso 1 1 calc R . . C444 C 0.3493(4) 0.9129(4) 0.38504(15) 0.0719(15) Uani 1 1 d . . . H444 H 0.3128 0.9518 0.3706 0.086 Uiso 1 1 calc R . . C445 C 0.4037(4) 0.9512(3) 0.41425(15) 0.0677(14) Uani 1 1 d . . . H445 H 0.4044 1.0162 0.4198 0.081 Uiso 1 1 calc R . . C446 C 0.4571(3) 0.8954(3) 0.43545(12) 0.0497(11) Uani 1 1 d . . . H446 H 0.4948 0.9223 0.4554 0.060 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 N11 0.0330(18) 0.0371(17) 0.0332(16) -0.0046(14) -0.0009(13) 0.0068(14) N12 0.041(2) 0.0354(17) 0.0360(17) -0.0010(14) 0.0093(14) 0.0087(15) N13 0.0395(19) 0.0362(17) 0.0405(17) -0.0028(15) 0.0084(14) 0.0074(15) N14 0.0393(19) 0.0368(17) 0.0355(16) -0.0047(14) 0.0112(14) 0.0034(14) C1A1 0.033(2) 0.0334(19) 0.0327(19) -0.0001(16) -0.0037(16) 0.0066(16) C1A2 0.039(2) 0.0308(19) 0.0313(19) -0.0017(16) -0.0008(16) 0.0048(17) C1A3 0.036(2) 0.042(2) 0.0336(19) 0.0018(17) 0.0026(16) 0.0088(18) C1A4 0.052(3) 0.034(2) 0.0308(19) -0.0030(17) 0.0055(17) 0.0103(18) C1A5 0.044(2) 0.0310(19) 0.035(2) -0.0038(16) 0.0046(17) 0.0072(17) C1A6 0.039(2) 0.0299(19) 0.042(2) -0.0005(17) -0.0011(17) 0.0056(17) C1A7 0.043(2) 0.039(2) 0.042(2) -0.0012(18) 0.0122(18) 0.0034(18) C1A8 0.038(2) 0.036(2) 0.036(2) -0.0023(17) 0.0059(16) 0.0002(17) C1B1 0.040(2) 0.0303(19) 0.0326(19) -0.0001(16) -0.0047(16) 0.0067(16) C1B2 0.034(2) 0.0310(19) 0.0336(19) 0.0003(16) -0.0014(15) 0.0063(16) C1B3 0.054(3) 0.045(2) 0.038(2) -0.0029(19) 0.0087(19) 0.005(2) C1B4 0.055(3) 0.038(2) 0.041(2) -0.0040(18) 0.0121(19) 0.0102(19) C1B5 0.050(3) 0.036(2) 0.046(2) -0.0078(18) 0.0026(19) 0.0073(19) C1B6 0.050(3) 0.034(2) 0.044(2) -0.0028(18) 0.0042(19) 0.0060(18) C1B7 0.049(3) 0.038(2) 0.050(2) -0.0027(19) 0.0182(19) -0.0009(19) C1B8 0.051(3) 0.047(2) 0.046(2) -0.005(2) 0.014(2) 0.003(2) C1M1 0.041(2) 0.037(2) 0.0268(18) 0.0011(16) 0.0009(16) 0.0084(17) C1M2 0.046(2) 0.037(2) 0.0315(19) -0.0024(17) -0.0012(17) 0.0108(18) C1M3 0.046(2) 0.0287(19) 0.043(2) 0.0017(17) -0.0010(18) 0.0032(17) C1M4 0.035(2) 0.035(2) 0.037(2) -0.0011(16) 0.0022(16) 0.0062(17) C110 0.037(2) 0.041(2) 0.0321(19) 0.0050(17) -0.0023(16) 0.0004(18) C111 0.042(3) 0.049(2) 0.043(2) 0.0032(19) 0.0072(18) 0.005(2) C112 0.041(3) 0.072(3) 0.055(3) 0.003(2) 0.015(2) 0.010(2) C113 0.046(3) 0.065(3) 0.056(3) 0.000(2) 0.013(2) -0.010(2) C114 0.054(3) 0.051(3) 0.034(2) -0.0030(19) 0.0020(19) -0.010(2) C115 0.070(3) 0.050(3) 0.040(2) -0.001(2) 0.006(2) -0.011(2) C116 0.085(4) 0.043(2) 0.038(2) 0.011(2) 0.002(2) -0.002(3) C117 0.072(3) 0.042(2) 0.031(2) 0.0037(18) -0.003(2) 0.011(2) C118 0.047(2) 0.038(2) 0.0274(18) 0.0020(16) -0.0024(16) 0.0058(18) C119 0.043(2) 0.045(2) 0.0301(19) -0.0041(17) -0.0031(17) -0.0009(19) C120 0.047(3) 0.032(2) 0.035(2) -0.0030(16) -0.0038(18) 0.0017(18) O1 0.052(2) 0.0555(18) 0.0466(16) 0.0028(14) -0.0027(14) 0.0151(15) C121 0.045(3) 0.041(2) 0.041(2) -0.0059(18) 0.0069(18) 0.0050(19) C122 0.061(3) 0.045(2) 0.051(2) -0.009(2) -0.001(2) 0.016(2) C123 0.080(4) 0.054(3) 0.058(3) -0.015(2) 0.005(2) 0.020(3) C124 0.109(5) 0.065(3) 0.044(3) -0.017(3) 0.017(3) 0.010(3) C125 0.127(5) 0.071(3) 0.037(2) -0.009(2) -0.004(3) 0.025(3) C126 0.098(4) 0.051(3) 0.042(2) -0.007(2) -0.004(2) 0.025(3) C131 0.048(3) 0.036(2) 0.052(2) -0.0007(19) 0.012(2) 0.0066(19) C132 0.050(3) 0.047(2) 0.061(3) -0.006(2) 0.011(2) 0.006(2) C133 0.054(3) 0.038(2) 0.074(3) -0.006(2) 0.019(2) -0.007(2) C134 0.054(3) 0.036(2) 0.074(3) 0.008(2) 0.031(2) 0.009(2) C135 0.054(3) 0.048(3) 0.060(3) 0.015(2) 0.020(2) 0.010(2) C136 0.050(3) 0.050(2) 0.046(2) -0.002(2) 0.006(2) 0.005(2) C141 0.038(2) 0.033(2) 0.045(2) -0.0067(18) 0.0096(17) 0.0014(17) C142 0.046(3) 0.052(3) 0.048(2) -0.005(2) 0.0013(19) 0.011(2) C143 0.048(3) 0.045(3) 0.084(4) -0.013(2) 0.007(2) 0.013(2) C144 0.065(3) 0.054(3) 0.075(3) -0.017(3) 0.028(3) 0.007(3) C145 0.079(4) 0.059(3) 0.045(2) -0.015(2) 0.020(2) 0.001(3) C146 0.056(3) 0.050(2) 0.041(2) -0.007(2) 0.009(2) 0.007(2) N21 0.043(2) 0.0277(16) 0.0327(16) -0.0013(13) -0.0047(14) 0.0032(14) N22 0.041(2) 0.0318(16) 0.0386(17) 0.0014(14) -0.0038(14) 0.0078(14) N23 0.041(2) 0.0345(17) 0.0364(17) -0.0013(14) -0.0051(14) 0.0062(14) N24 0.0381(19) 0.0323(16) 0.0350(16) -0.0007(14) 0.0001(14) 0.0040(14) C2A1 0.032(2) 0.0344(19) 0.0298(18) -0.0033(16) 0.0041(15) 0.0042(16) C2A2 0.037(2) 0.034(2) 0.0317(19) 0.0025(16) 0.0050(16) 0.0037(17) C2A3 0.046(2) 0.0300(19) 0.040(2) -0.0037(17) -0.0041(18) 0.0120(17) C2A4 0.048(3) 0.037(2) 0.043(2) 0.0029(18) -0.0010(19) 0.0074(19) C2A5 0.040(2) 0.040(2) 0.038(2) 0.0007(18) -0.0051(17) 0.0060(18) C2A6 0.034(2) 0.042(2) 0.040(2) -0.0087(18) 0.0005(17) 0.0002(18) C2A7 0.037(2) 0.038(2) 0.039(2) -0.0022(17) -0.0003(17) 0.0039(17) C2A8 0.035(2) 0.0315(19) 0.039(2) 0.0021(16) 0.0013(17) 0.0024(16) C2B1 0.031(2) 0.0324(19) 0.0330(18) -0.0031(16) 0.0052(15) 0.0014(16) C2B2 0.037(2) 0.034(2) 0.0336(19) -0.0039(16) 0.0013(16) 0.0014(17) C2B3 0.063(3) 0.038(2) 0.046(2) 0.0035(19) -0.012(2) 0.009(2) C2B4 0.059(3) 0.040(2) 0.043(2) 0.0060(19) -0.011(2) 0.009(2) C2B5 0.048(3) 0.050(2) 0.032(2) 0.0057(18) -0.0047(17) 0.003(2) C2B6 0.052(3) 0.033(2) 0.040(2) -0.0057(17) -0.0037(18) 0.0008(18) C2B7 0.042(2) 0.0287(19) 0.048(2) 0.0043(17) -0.0032(18) 0.0020(17) C2B8 0.046(3) 0.034(2) 0.038(2) 0.0064(17) -0.0050(18) 0.0035(18) C2M1 0.043(2) 0.033(2) 0.037(2) 0.0013(17) 0.0047(17) 0.0057(17) C2M2 0.036(2) 0.046(2) 0.043(2) 0.0010(18) -0.0035(17) 0.0122(18) C2M3 0.029(2) 0.037(2) 0.041(2) -0.0028(17) -0.0004(16) -0.0015(17) C2M4 0.040(2) 0.035(2) 0.036(2) -0.0005(17) 0.0057(17) 0.0029(17) C211 0.051(3) 0.033(2) 0.039(2) 0.0086(17) -0.0045(18) 0.0023(19) C212 0.058(3) 0.040(2) 0.058(3) 0.005(2) -0.001(2) -0.001(2) C213 0.073(4) 0.049(3) 0.091(4) 0.001(3) 0.005(3) -0.016(3) C214 0.109(5) 0.036(3) 0.080(4) -0.011(3) -0.008(3) -0.008(3) C215 0.095(4) 0.040(3) 0.068(3) -0.009(2) -0.002(3) 0.012(3) C216 0.067(3) 0.039(2) 0.057(3) -0.002(2) 0.000(2) 0.011(2) C221 0.052(3) 0.041(2) 0.047(2) 0.0002(19) -0.012(2) 0.010(2) C222 0.078(4) 0.067(3) 0.057(3) -0.003(3) -0.013(3) 0.022(3) C223 0.089(4) 0.078(4) 0.072(4) 0.002(3) -0.025(3) 0.028(3) C224 0.089(4) 0.061(3) 0.074(4) 0.015(3) -0.035(3) 0.009(3) C225 0.084(4) 0.082(4) 0.052(3) 0.029(3) -0.007(3) 0.005(3) C226 0.068(3) 0.071(3) 0.052(3) 0.016(2) 0.003(2) 0.009(3) C231 0.050(3) 0.034(2) 0.040(2) 0.0001(17) -0.0054(18) 0.0079(19) C232 0.051(3) 0.038(2) 0.045(2) -0.0012(18) 0.0019(19) -0.002(2) C233 0.066(3) 0.039(2) 0.059(3) -0.002(2) -0.008(2) -0.011(2) C234 0.094(4) 0.042(3) 0.064(3) -0.009(2) -0.021(3) 0.008(3) C235 0.095(4) 0.056(3) 0.080(3) -0.017(3) -0.008(3) 0.037(3) C236 0.048(3) 0.051(3) 0.079(3) -0.014(2) -0.003(2) 0.008(2) C241 0.035(2) 0.0259(18) 0.037(2) -0.0015(16) -0.0012(16) 0.0062(16) C242 0.055(3) 0.044(2) 0.042(2) 0.0006(19) 0.002(2) 0.005(2) C243 0.106(5) 0.049(3) 0.041(2) 0.007(2) -0.015(3) 0.005(3) C244 0.076(4) 0.051(3) 0.082(4) -0.001(3) -0.030(3) 0.018(3) C245 0.050(3) 0.050(3) 0.092(4) -0.010(3) -0.010(3) 0.020(2) C246 0.042(3) 0.038(2) 0.052(2) -0.0054(19) -0.0027(19) 0.0061(19) N31 0.0376(19) 0.0380(17) 0.0317(16) -0.0006(14) 0.0010(13) 0.0086(14) N32 0.0322(18) 0.0389(17) 0.0375(17) -0.0085(14) 0.0041(13) 0.0021(14) N33 0.0343(19) 0.0409(18) 0.0430(18) -0.0027(15) 0.0000(14) 0.0063(15) N34 0.039(2) 0.0373(17) 0.0411(17) -0.0107(15) 0.0032(14) 0.0042(15) C3A1 0.038(2) 0.0324(19) 0.0340(19) 0.0054(16) 0.0029(16) 0.0109(17) C3A2 0.029(2) 0.037(2) 0.0291(18) 0.0041(16) 0.0012(15) 0.0058(16) C3A3 0.035(2) 0.036(2) 0.0344(19) -0.0038(16) -0.0011(16) 0.0056(17) C3A4 0.039(2) 0.045(2) 0.0302(19) -0.0018(17) 0.0013(16) 0.0121(18) C3A5 0.033(2) 0.047(2) 0.035(2) 0.0008(18) 0.0007(16) 0.0068(18) C3A6 0.036(2) 0.040(2) 0.043(2) -0.0016(18) 0.0019(17) 0.0085(18) C3A7 0.039(2) 0.040(2) 0.046(2) -0.0026(19) -0.0009(18) -0.0005(19) C3A8 0.044(3) 0.035(2) 0.043(2) -0.0073(18) 0.0063(18) 0.0082(18) C3B1 0.036(2) 0.0332(19) 0.038(2) -0.0026(16) 0.0040(16) 0.0113(16) C3B2 0.033(2) 0.038(2) 0.0278(18) 0.0009(16) 0.0021(15) 0.0066(16) C3B3 0.042(2) 0.040(2) 0.0326(19) -0.0035(17) 0.0035(17) 0.0033(18) C3B4 0.043(2) 0.048(2) 0.035(2) -0.0089(18) -0.0049(17) 0.0122(19) C3B5 0.038(2) 0.052(2) 0.047(2) 0.002(2) 0.0093(18) 0.002(2) C3B6 0.039(2) 0.053(2) 0.043(2) -0.001(2) 0.0055(18) -0.001(2) C3B7 0.042(3) 0.045(2) 0.057(3) -0.018(2) 0.004(2) 0.000(2) C3B8 0.047(3) 0.047(2) 0.049(2) -0.017(2) 0.0092(19) 0.005(2) C3M1 0.031(2) 0.040(2) 0.0344(19) -0.0022(17) -0.0006(16) 0.0037(17) C3M2 0.035(2) 0.049(2) 0.0336(19) 0.0013(18) -0.0015(16) 0.0119(19) C3M3 0.046(3) 0.035(2) 0.046(2) 0.0015(18) 0.0035(19) 0.0030(18) C3M4 0.040(2) 0.040(2) 0.041(2) -0.0015(18) 0.0036(17) 0.0124(18) C310 0.038(2) 0.038(2) 0.0347(19) -0.0008(17) 0.0063(16) 0.0033(17) C311 0.049(3) 0.044(2) 0.033(2) -0.0039(18) 0.0039(17) 0.0064(19) C312 0.066(3) 0.036(2) 0.043(2) -0.0028(18) 0.005(2) 0.007(2) C313 0.057(3) 0.047(2) 0.047(2) -0.011(2) 0.015(2) -0.008(2) C314 0.048(3) 0.054(3) 0.035(2) -0.0039(19) 0.0148(18) -0.004(2) C315 0.053(3) 0.059(3) 0.044(2) -0.008(2) 0.004(2) -0.009(2) C316 0.046(3) 0.078(3) 0.047(3) -0.002(2) -0.006(2) -0.004(3) C317 0.036(2) 0.065(3) 0.046(2) -0.006(2) -0.0025(18) 0.007(2) C318 0.039(2) 0.051(2) 0.034(2) -0.0027(18) 0.0004(17) 0.0082(19) C319 0.043(3) 0.046(2) 0.0300(19) 0.0035(17) 0.0063(17) 0.0024(19) C320 0.036(2) 0.046(2) 0.036(2) -0.0018(18) 0.0027(17) 0.0042(19) O2 0.064(2) 0.0456(17) 0.0504(17) 0.0027(14) -0.0039(14) 0.0165(15) C321 0.039(2) 0.057(2) 0.038(2) -0.0038(19) 0.0022(17) 0.0088(19) C322 0.068(3) 0.146(4) 0.043(2) 0.012(3) 0.005(2) 0.054(3) C323 0.084(4) 0.155(5) 0.038(2) 0.005(3) 0.009(2) 0.052(3) C324 0.063(3) 0.086(3) 0.049(2) -0.012(2) 0.015(2) 0.015(3) C325 0.079(3) 0.075(3) 0.062(3) 0.012(3) 0.029(2) 0.031(3) C326 0.067(3) 0.071(3) 0.054(2) 0.017(2) 0.022(2) 0.027(2) C331 0.041(2) 0.035(2) 0.058(3) -0.008(2) 0.006(2) 0.0119(19) C332 0.057(3) 0.046(3) 0.075(3) -0.008(2) 0.009(2) -0.001(2) C333 0.070(4) 0.041(3) 0.104(4) -0.014(3) 0.031(3) -0.004(2) C334 0.048(3) 0.062(3) 0.111(5) -0.033(3) 0.002(3) 0.009(3) C335 0.053(3) 0.069(3) 0.080(3) -0.026(3) -0.012(3) 0.014(3) C336 0.048(3) 0.054(3) 0.059(3) -0.021(2) -0.005(2) 0.013(2) C341 0.038(2) 0.040(2) 0.053(2) -0.0115(19) 0.0099(19) 0.0041(19) C342 0.055(3) 0.071(3) 0.055(3) -0.010(2) 0.011(2) 0.012(2) C343 0.066(4) 0.082(4) 0.062(3) -0.033(3) 0.017(3) -0.003(3) C344 0.063(4) 0.067(3) 0.097(4) -0.038(3) 0.026(3) 0.007(3) C345 0.059(3) 0.059(3) 0.103(4) -0.015(3) 0.014(3) 0.020(3) C346 0.056(3) 0.044(2) 0.077(3) -0.005(2) 0.004(2) 0.015(2) N41 0.0316(18) 0.0433(18) 0.0320(16) 0.0020(14) 0.0013(13) 0.0061(14) N42 0.0363(19) 0.0466(19) 0.0329(16) 0.0021(15) 0.0000(14) 0.0095(15) N43 0.039(2) 0.0407(18) 0.0346(16) 0.0009(14) 0.0045(14) 0.0064(15) N44 0.0368(19) 0.0361(17) 0.0319(16) 0.0002(14) 0.0017(13) 0.0010(14) C4A1 0.034(2) 0.0310(19) 0.0337(19) -0.0027(16) 0.0015(16) 0.0053(16) C4A2 0.032(2) 0.041(2) 0.035(2) 0.0004(17) -0.0020(16) 0.0055(17) C4A3 0.032(2) 0.046(2) 0.043(2) 0.0042(19) -0.0008(17) 0.0092(18) C4A4 0.044(3) 0.046(2) 0.040(2) 0.0068(19) 0.0041(18) 0.0141(19) C4A5 0.045(3) 0.034(2) 0.034(2) 0.0013(16) -0.0021(17) 0.0077(18) C4A6 0.037(2) 0.036(2) 0.041(2) 0.0003(17) 0.0024(17) 0.0045(17) C4A7 0.036(2) 0.035(2) 0.0335(19) -0.0006(16) 0.0018(16) 0.0068(17) C4A8 0.035(2) 0.036(2) 0.0340(19) -0.0027(17) -0.0022(16) 0.0084(17) C4B1 0.035(2) 0.0286(18) 0.0358(19) -0.0044(16) 0.0025(16) 0.0054(16) C4B2 0.042(2) 0.039(2) 0.035(2) -0.0036(17) 0.0054(17) 0.0094(18) C4B3 0.028(2) 0.076(3) 0.054(3) 0.012(2) -0.0026(19) 0.013(2) C4B4 0.038(3) 0.072(3) 0.052(3) 0.017(2) 0.000(2) 0.016(2) C4B5 0.045(3) 0.048(2) 0.037(2) 0.0078(18) 0.0007(18) 0.007(2) C4B6 0.041(3) 0.047(2) 0.041(2) 0.0030(19) 0.0066(18) 0.0070(19) C4B7 0.033(2) 0.046(2) 0.039(2) -0.0011(18) 0.0048(17) 0.0012(18) C4B8 0.034(2) 0.053(2) 0.039(2) -0.0032(19) -0.0015(17) 0.0071(19) C4M1 0.040(2) 0.043(2) 0.038(2) -0.0055(18) -0.0016(18) 0.0048(18) C4M2 0.043(3) 0.036(2) 0.040(2) 0.0020(17) -0.0017(18) 0.0083(18) C4M3 0.032(2) 0.035(2) 0.038(2) 0.0004(17) 0.0047(16) 0.0034(16) C4M4 0.035(2) 0.038(2) 0.0350(19) -0.0030(17) 0.0041(16) 0.0045(17) C411 0.037(2) 0.053(3) 0.035(2) 0.0025(19) -0.0054(17) 0.001(2) C412 0.041(3) 0.067(3) 0.069(3) 0.003(3) 0.003(2) 0.005(2) C413 0.066(4) 0.076(4) 0.125(5) 0.015(4) 0.016(4) -0.014(3) C414 0.054(4) 0.119(6) 0.106(5) 0.013(4) 0.024(3) -0.016(4) C415 0.045(3) 0.118(5) 0.091(4) -0.011(4) 0.025(3) 0.007(3) C416 0.043(3) 0.073(3) 0.065(3) -0.005(3) 0.002(2) 0.011(2) C421 0.043(3) 0.062(3) 0.037(2) 0.010(2) -0.0015(18) 0.013(2) C422 0.062(3) 0.058(3) 0.046(2) 0.005(2) -0.002(2) 0.017(2) C423 0.079(4) 0.063(3) 0.067(3) 0.021(3) -0.002(3) 0.025(3) C424 0.071(4) 0.102(5) 0.056(3) 0.031(3) -0.015(3) 0.024(3) C425 0.105(5) 0.076(4) 0.059(3) 0.012(3) -0.034(3) -0.004(3) C426 0.086(4) 0.059(3) 0.058(3) 0.004(2) -0.030(3) 0.005(3) C431 0.037(2) 0.045(2) 0.0331(19) 0.0012(17) 0.0013(16) 0.0037(18) C432 0.041(2) 0.045(2) 0.042(2) -0.0017(19) 0.0071(18) 0.0009(19) C433 0.043(3) 0.061(3) 0.047(2) 0.008(2) 0.002(2) -0.004(2) C434 0.038(3) 0.095(4) 0.043(2) 0.012(3) 0.0068(19) 0.013(3) C435 0.061(3) 0.069(3) 0.059(3) 0.011(2) 0.018(2) 0.025(3) C436 0.047(3) 0.054(3) 0.062(3) 0.010(2) 0.014(2) 0.014(2) C441 0.028(2) 0.039(2) 0.039(2) 0.0029(17) 0.0084(16) 0.0059(17) C442 0.041(3) 0.051(2) 0.045(2) -0.002(2) -0.0047(19) 0.008(2) C443 0.043(3) 0.080(4) 0.050(3) 0.011(2) -0.011(2) 0.011(2) C444 0.062(3) 0.071(4) 0.086(4) 0.028(3) -0.005(3) 0.031(3) C445 0.055(3) 0.047(3) 0.105(4) 0.002(3) 0.010(3) 0.020(2) C446 0.046(3) 0.045(2) 0.062(3) 0.001(2) 0.007(2) 0.017(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N11 C1A2 1.355(5) . ? N11 C1A1 1.363(5) . ? N12 C1A3 1.364(5) . ? N12 C1A4 1.392(5) . ? N12 H12 0.8700 . ? N13 C1A5 1.368(5) . ? N13 C1A6 1.369(5) . ? N14 C1A7 1.372(5) . ? N14 C1A8 1.380(5) . ? N14 H14 0.8700 . ? C1A1 C1M4 1.387(5) . ? C1A1 C1B1 1.527(5) . ? C1A2 C1M1 1.383(5) . ? C1A2 C1B2 1.514(5) . ? C1A3 C1B3 1.429(5) . ? C1A3 C1M1 1.429(5) . ? C1A4 C1M2 1.387(5) . ? C1A4 C1B4 1.418(5) . ? C1A5 C1M2 1.405(5) . ? C1A5 C1B5 1.457(5) . ? C1A6 C1M3 1.418(5) . ? C1A6 C1B6 1.446(5) . ? C1A7 C1M3 1.385(5) . ? C1A7 C1B7 1.418(5) . ? C1A8 C1M4 1.401(5) . ? C1A8 C1B8 1.430(5) . ? C1B1 C1B2 1.517(5) . ? C1B1 C2B1 1.520(5) . ? C1B1 H1B1 0.9900 . ? C1B2 C120 1.525(5) . ? C1B2 H1B2 0.9900 . ? C1B3 C1B4 1.351(5) . ? C1B3 H1B3 0.9400 . ? C1B4 H1B4 0.9400 . ? C1B5 C1B6 1.336(5) . ? C1B5 H1B5 0.9400 . ? C1B6 H1B6 0.9400 . ? C1B7 C1B8 1.368(5) . ? C1B7 H1B7 0.9400 . ? C1B8 H1B8 0.9400 . ? C1M1 C110 1.500(5) . ? C1M2 C121 1.503(5) . ? C1M3 C131 1.499(5) . ? C1M4 C141 1.502(5) . ? C110 C111 1.372(6) . ? C110 C119 1.441(5) . ? C111 C112 1.411(6) . ? C111 H111 0.9400 . ? C112 C113 1.364(7) . ? C112 H112 0.9400 . ? C113 C114 1.404(7) . ? C113 H113 0.9400 . ? C114 C115 1.420(6) . ? C114 C119 1.432(6) . ? C115 C116 1.353(7) . ? C115 H115 0.9400 . ? C116 C117 1.408(6) . ? C116 H116 0.9400 . ? C117 C118 1.373(5) . ? C117 H117 0.9400 . ? C118 C119 1.427(6) . ? C118 C120 1.486(5) . ? C120 O1 1.216(5) . ? C121 C126 1.372(6) . ? C121 C122 1.404(6) . ? C122 C123 1.370(6) . ? C122 H122 0.9400 . ? C123 C124 1.385(7) . ? C123 H123 0.9400 . ? C124 C125 1.371(7) . ? C124 H124 0.9400 . ? C125 C126 1.393(6) . ? C125 H125 0.9400 . ? C126 H126 0.9400 . ? C131 C132 1.392(6) . ? C131 C136 1.407(6) . ? C132 C133 1.393(6) . ? C132 H132 0.9400 . ? C133 C134 1.375(6) . ? C133 H133 0.9400 . ? C134 C135 1.355(6) . ? C134 H134 0.9400 . ? C135 C136 1.380(6) . ? C135 H135 0.9400 . ? C136 H136 0.9400 . ? C141 C142 1.389(6) . ? C141 C146 1.392(5) . ? C142 C143 1.381(6) . ? C142 H142 0.9400 . ? C143 C144 1.381(7) . ? C143 H143 0.9400 . ? C144 C145 1.382(7) . ? C144 H144 0.9400 . ? C145 C146 1.388(6) . ? C145 H145 0.9400 . ? C146 H146 0.9400 . ? N21 C2A2 1.360(4) . ? N21 C2A1 1.372(5) . ? N21 H21 0.8700 . ? N22 C2A3 1.369(5) . ? N22 C2A4 1.379(5) . ? N23 C2A5 1.353(5) . ? N23 C2A6 1.374(5) . ? N23 H23 0.8700 . ? N24 C2A8 1.373(5) . ? N24 C2A7 1.379(5) . ? C2A1 C2M4 1.404(5) . ? C2A1 C2B1 1.464(5) . ? C2A2 C2M1 1.395(5) . ? C2A2 C2B2 1.430(5) . ? C2A3 C2M1 1.411(5) . ? C2A3 C2B3 1.449(5) . ? C2A4 C2M2 1.413(5) . ? C2A4 C2B4 1.442(5) . ? C2A5 C2M2 1.394(5) . ? C2A5 C2B5 1.427(5) . ? C2A6 C2M3 1.403(5) . ? C2A6 C2B6 1.434(5) . ? C2A7 C2M3 1.404(5) . ? C2A7 C2B7 1.429(5) . ? C2A8 C2M4 1.411(5) . ? C2A8 C2B8 1.431(5) . ? C2B1 C2B2 1.358(5) . ? C2B2 H2B2 0.9400 . ? C2B3 C2B4 1.333(5) . ? C2B3 H2B3 0.9400 . ? C2B4 H2B4 0.9400 . ? C2B5 C2B6 1.360(6) . ? C2B5 H2B5 0.9400 . ? C2B6 H2B6 0.9400 . ? C2B7 C2B8 1.349(5) . ? C2B7 H2B7 0.9400 . ? C2B8 H2B8 0.9400 . ? C2M1 C211 1.492(5) . ? C2M2 C221 1.513(5) . ? C2M3 C231 1.509(5) . ? C2M4 C241 1.500(5) . ? C211 C216 1.388(6) . ? C211 C212 1.390(6) . ? C212 C213 1.392(6) . ? C212 H212 0.9400 . ? C213 C214 1.378(8) . ? C213 H213 0.9400 . ? C214 C215 1.358(8) . ? C214 H214 0.9400 . ? C215 C216 1.385(6) . ? C215 H215 0.9400 . ? C216 H216 0.9400 . ? C221 C222 1.374(7) . ? C221 C226 1.387(6) . ? C222 C223 1.386(7) . ? C222 H222 0.9400 . ? C223 C224 1.378(8) . ? C223 H223 0.9400 . ? C224 C225 1.375(8) . ? C224 H224 0.9400 . ? C225 C226 1.389(6) . ? C225 H225 0.9400 . ? C226 H226 0.9400 . ? C231 C232 1.369(6) . ? C231 C236 1.384(6) . ? C232 C233 1.384(6) . ? C232 H232 0.9400 . ? C233 C234 1.363(7) . ? C233 H233 0.9400 . ? C234 C235 1.368(7) . ? C234 H234 0.9400 . ? C235 C236 1.379(6) . ? C235 H235 0.9400 . ? C236 H236 0.9400 . ? C241 C246 1.380(6) . ? C241 C242 1.381(5) . ? C242 C243 1.392(6) . ? C242 H242 0.9400 . ? C243 C244 1.385(8) . ? C243 H243 0.9400 . ? C244 C245 1.363(7) . ? C244 H244 0.9400 . ? C245 C246 1.381(6) . ? C245 H245 0.9400 . ? C246 H246 0.9400 . ? N31 C3A2 1.360(4) . ? N31 C3A1 1.378(5) . ? N32 C3A3 1.347(5) . ? N32 C3A4 1.392(5) . ? N32 H32 0.8700 . ? N33 C3A6 1.361(5) . ? N33 C3A5 1.363(5) . ? N34 C3A7 1.373(5) . ? N34 C3A8 1.373(5) . ? N34 H34 0.8700 . ? C3A1 C3M4 1.397(5) . ? C3A1 C3B1 1.500(5) . ? C3A2 C3M1 1.401(5) . ? C3A2 C3B2 1.512(5) . ? C3A3 C3M1 1.419(5) . ? C3A3 C3B3 1.435(5) . ? C3A4 C3M2 1.391(5) . ? C3A4 C3B4 1.410(5) . ? C3A5 C3M2 1.416(5) . ? C3A5 C3B5 1.450(5) . ? C3A6 C3M3 1.423(5) . ? C3A6 C3B6 1.441(5) . ? C3A7 C3M3 1.372(6) . ? C3A7 C3B7 1.431(6) . ? C3A8 C3M4 1.399(5) . ? C3A8 C3B8 1.434(5) . ? C3B1 C4B1 1.522(5) . ? C3B1 C3B2 1.524(5) . ? C3B1 H3B1 0.9900 . ? C3B2 C320 1.533(5) . ? C3B2 H3B2 0.9900 . ? C3B3 C3B4 1.359(5) . ? C3B3 H3B3 0.9400 . ? C3B4 H3B4 0.9400 . ? C3B5 C3B6 1.339(5) . ? C3B5 H3B5 0.9400 . ? C3B6 H3B6 0.9400 . ? C3B7 C3B8 1.345(6) . ? C3B7 H3B7 0.9400 . ? C3B8 H3B8 0.9400 . ? C3M1 C310 1.492(5) . ? C3M2 C321 1.509(4) . ? C3M3 C331 1.501(6) . ? C3M4 C341 1.496(5) . ? C310 C311 1.379(5) . ? C310 C319 1.450(6) . ? C311 C312 1.410(5) . ? C311 H311 0.9400 . ? C312 C313 1.356(6) . ? C312 H312 0.9400 . ? C313 C314 1.418(6) . ? C313 H313 0.9400 . ? C314 C315 1.405(6) . ? C314 C319 1.445(5) . ? C315 C316 1.337(7) . ? C315 H316 0.9400 . ? C316 C317 1.416(6) . ? C316 H317 0.9400 . ? C317 C318 1.371(6) . ? C317 H318 0.9400 . ? C318 C319 1.433(6) . ? C318 C320 1.495(5) . ? C320 O2 1.215(5) . ? C321 C322 1.3900 . ? C321 C326 1.3900 . ? C322 C323 1.3900 . ? C322 H322 0.9400 . ? C323 C324 1.3900 . ? C323 H323 0.9400 . ? C324 C325 1.3900 . ? C324 H324 0.9400 . ? C325 C326 1.3900 . ? C325 H325 0.9400 . ? C326 H326 0.9400 . ? C331 C332 1.364(6) . ? C331 C336 1.402(6) . ? C332 C333 1.408(7) . ? C332 H332 0.9400 . ? C333 C334 1.362(8) . ? C333 H333 0.9400 . ? C334 C335 1.356(7) . ? C334 H334 0.9400 . ? C335 C336 1.360(6) . ? C335 H335 0.9400 . ? C336 H336 0.9400 . ? C341 C346 1.380(6) . ? C341 C342 1.399(6) . ? C342 C343 1.396(6) . ? C342 H342 0.9400 . ? C343 C344 1.373(8) . ? C343 H343 0.9400 . ? C344 C345 1.372(8) . ? C344 H344 0.9400 . ? C345 C346 1.388(7) . ? C345 H345 0.9400 . ? C346 H346 0.9400 . ? N41 C4A2 1.364(5) . ? N41 C4A1 1.379(5) . ? N41 H41 0.8700 . ? N42 C4A3 1.374(5) . ? N42 C4A4 1.380(5) . ? N43 C4A6 1.368(5) . ? N43 C4A5 1.377(5) . ? N43 H43 0.8700 . ? N44 C4A8 1.378(5) . ? N44 C4A7 1.379(5) . ? C4A1 C4M4 1.388(5) . ? C4A1 C4B1 1.462(5) . ? C4A2 C4M1 1.403(5) . ? C4A2 C4B2 1.425(5) . ? C4A3 C4M1 1.399(5) . ? C4A3 C4B3 1.444(6) . ? C4A4 C4M2 1.396(5) . ? C4A4 C4B4 1.446(6) . ? C4A5 C4M2 1.399(6) . ? C4A5 C4B5 1.440(5) . ? C4A6 C4M3 1.409(5) . ? C4A6 C4B6 1.422(5) . ? C4A7 C4M3 1.408(5) . ? C4A7 C4B7 1.441(5) . ? C4A8 C4M4 1.408(5) . ? C4A8 C4B8 1.443(5) . ? C4B1 C4B2 1.358(5) . ? C4B2 H4B2 0.9400 . ? C4B3 C4B4 1.346(6) . ? C4B3 H4B3 0.9400 . ? C4B4 H4B4 0.9400 . ? C4B5 C4B6 1.356(6) . ? C4B5 H4B5 0.9400 . ? C4B6 H4B6 0.9400 . ? C4B7 C4B8 1.349(5) . ? C4B7 H4B7 0.9400 . ? C4B8 H4B8 0.9400 . ? C4M1 C411 1.499(6) . ? C4M2 C421 1.495(5) . ? C4M3 C431 1.510(5) . ? C4M4 C441 1.491(5) . ? C411 C412 1.361(6) . ? C411 C416 1.410(6) . ? C412 C413 1.384(7) . ? C412 H412 0.9400 . ? C413 C414 1.374(9) . ? C413 H413 0.9400 . ? C414 C415 1.380(9) . ? C414 H414 0.9400 . ? C415 C416 1.397(7) . ? C415 H415 0.9400 . ? C416 H416 0.9400 . ? C421 C426 1.373(6) . ? C421 C422 1.397(6) . ? C422 C423 1.385(6) . ? C422 H422 0.9400 . ? C423 C424 1.370(7) . ? C423 H423 0.9400 . ? C424 C425 1.379(8) . ? C424 H424 0.9400 . ? C425 C426 1.399(7) . ? C425 H425 0.9400 . ? C426 H426 0.9400 . ? C431 C432 1.369(5) . ? C431 C436 1.387(6) . ? C432 C433 1.394(6) . ? C432 H432 0.9400 . ? C433 C434 1.387(6) . ? C433 H433 0.9400 . ? C434 C435 1.382(7) . ? C434 H434 0.9400 . ? C435 C436 1.384(6) . ? C435 H435 0.9400 . ? C436 H436 0.9400 . ? C441 C442 1.375(5) . ? C441 C446 1.409(5) . ? C442 C443 1.382(6) . ? C442 H442 0.9400 . ? C443 C444 1.357(7) . ? C443 H443 0.9400 . ? C444 C445 1.367(7) . ? C444 H444 0.9400 . ? C445 C446 1.365(6) . ? C445 H445 0.9400 . ? C446 H446 0.9400 . ? 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 C1A2 N11 C1A1 108.7(3) . . ? C1A3 N12 C1A4 110.3(3) . . ? C1A3 N12 H12 124.9 . . ? C1A4 N12 H12 124.9 . . ? C1A5 N13 C1A6 105.7(3) . . ? C1A7 N14 C1A8 110.6(3) . . ? C1A7 N14 H14 124.7 . . ? C1A8 N14 H14 124.7 . . ? N11 C1A1 C1M4 126.8(3) . . ? N11 C1A1 C1B1 111.7(3) . . ? C1M4 C1A1 C1B1 121.2(3) . . ? N11 C1A2 C1M1 127.7(3) . . ? N11 C1A2 C1B2 112.1(3) . . ? C1M1 C1A2 C1B2 119.5(3) . . ? N12 C1A3 C1B3 106.4(3) . . ? N12 C1A3 C1M1 125.7(3) . . ? C1B3 C1A3 C1M1 127.8(3) . . ? C1M2 C1A4 N12 124.9(3) . . ? C1M2 C1A4 C1B4 129.0(3) . . ? N12 C1A4 C1B4 106.1(3) . . ? N13 C1A5 C1M2 126.5(3) . . ? N13 C1A5 C1B5 110.2(3) . . ? C1M2 C1A5 C1B5 123.3(3) . . ? N13 C1A6 C1M3 125.6(3) . . ? N13 C1A6 C1B6 110.3(3) . . ? C1M3 C1A6 C1B6 124.1(3) . . ? N14 C1A7 C1M3 125.8(3) . . ? N14 C1A7 C1B7 106.7(3) . . ? C1M3 C1A7 C1B7 127.2(4) . . ? N14 C1A8 C1M4 126.3(3) . . ? N14 C1A8 C1B8 106.1(3) . . ? C1M4 C1A8 C1B8 127.3(4) . . ? C1B2 C1B1 C2B1 111.7(3) . . ? C1B2 C1B1 C1A1 102.1(3) . . ? C2B1 C1B1 C1A1 107.6(3) . . ? C1B2 C1B1 H1B1 111.7 . . ? C2B1 C1B1 H1B1 111.7 . . ? C1A1 C1B1 H1B1 111.7 . . ? C1A2 C1B2 C1B1 102.9(3) . . ? C1A2 C1B2 C120 103.1(3) . . ? C1B1 C1B2 C120 113.7(3) . . ? C1A2 C1B2 H1B2 112.1 . . ? C1B1 C1B2 H1B2 112.1 . . ? C120 C1B2 H1B2 112.1 . . ? C1B4 C1B3 C1A3 108.7(4) . . ? C1B4 C1B3 H1B3 125.7 . . ? C1A3 C1B3 H1B3 125.7 . . ? C1B3 C1B4 C1A4 108.6(3) . . ? C1B3 C1B4 H1B4 125.7 . . ? C1A4 C1B4 H1B4 125.7 . . ? C1B6 C1B5 C1A5 106.5(3) . . ? C1B6 C1B5 H1B5 126.7 . . ? C1A5 C1B5 H1B5 126.7 . . ? C1B5 C1B6 C1A6 107.3(4) . . ? C1B5 C1B6 H1B6 126.3 . . ? C1A6 C1B6 H1B6 126.3 . . ? C1B8 C1B7 C1A7 108.5(4) . . ? C1B8 C1B7 H1B7 125.7 . . ? C1A7 C1B7 H1B7 125.7 . . ? C1B7 C1B8 C1A8 108.1(4) . . ? C1B7 C1B8 H1B8 126.0 . . ? C1A8 C1B8 H1B8 126.0 . . ? C1A2 C1M1 C1A3 124.8(3) . . ? C1A2 C1M1 C110 119.9(3) . . ? C1A3 C1M1 C110 115.3(3) . . ? C1A4 C1M2 C1A5 126.2(3) . . ? C1A4 C1M2 C121 116.7(3) . . ? C1A5 C1M2 C121 117.1(3) . . ? C1A7 C1M3 C1A6 125.0(3) . . ? C1A7 C1M3 C131 115.3(3) . . ? C1A6 C1M3 C131 119.7(3) . . ? C1A1 C1M4 C1A8 125.8(4) . . ? C1A1 C1M4 C141 118.9(3) . . ? C1A8 C1M4 C141 115.3(3) . . ? C111 C110 C119 118.6(4) . . ? C111 C110 C1M1 118.0(3) . . ? C119 C110 C1M1 123.1(4) . . ? C110 C111 C112 123.0(4) . . ? C110 C111 H111 118.5 . . ? C112 C111 H111 118.5 . . ? C113 C112 C111 118.5(4) . . ? C113 C112 H112 120.7 . . ? C111 C112 H112 120.7 . . ? C112 C113 C114 121.5(4) . . ? C112 C113 H113 119.3 . . ? C114 C113 H113 119.3 . . ? C113 C114 C115 120.9(4) . . ? C113 C114 C119 120.0(4) . . ? C115 C114 C119 119.2(4) . . ? C116 C115 C114 121.6(4) . . ? C116 C115 H115 119.2 . . ? C114 C115 H115 119.2 . . ? C115 C116 C117 119.3(4) . . ? C115 C116 H116 120.4 . . ? C117 C116 H116 120.4 . . ? C118 C117 C116 121.6(4) . . ? C118 C117 H117 119.2 . . ? C116 C117 H117 119.2 . . ? C117 C118 C119 120.2(4) . . ? C117 C118 C120 116.0(4) . . ? C119 C118 C120 122.7(3) . . ? C118 C119 C114 117.7(4) . . ? C118 C119 C110 124.4(4) . . ? C114 C119 C110 117.8(4) . . ? O1 C120 C118 123.5(4) . . ? O1 C120 C1B2 121.6(4) . . ? C118 C120 C1B2 115.0(4) . . ? C126 C121 C122 117.7(4) . . ? C126 C121 C1M2 121.6(4) . . ? C122 C121 C1M2 120.7(4) . . ? C123 C122 C121 120.8(4) . . ? C123 C122 H122 119.6 . . ? C121 C122 H122 119.6 . . ? C122 C123 C124 120.7(5) . . ? C122 C123 H123 119.7 . . ? C124 C123 H123 119.7 . . ? C125 C124 C123 119.2(5) . . ? C125 C124 H124 120.4 . . ? C123 C124 H124 120.4 . . ? C124 C125 C126 120.1(5) . . ? C124 C125 H125 119.9 . . ? C126 C125 H125 119.9 . . ? C121 C126 C125 121.4(5) . . ? C121 C126 H126 119.3 . . ? C125 C126 H126 119.3 . . ? C132 C131 C136 118.7(4) . . ? C132 C131 C1M3 122.7(4) . . ? C136 C131 C1M3 118.6(4) . . ? C131 C132 C133 119.5(4) . . ? C131 C132 H132 120.3 . . ? C133 C132 H132 120.3 . . ? C134 C133 C132 120.3(4) . . ? C134 C133 H133 119.8 . . ? C132 C133 H133 119.8 . . ? C135 C134 C133 120.9(4) . . ? C135 C134 H134 119.5 . . ? C133 C134 H134 119.5 . . ? C134 C135 C136 120.1(4) . . ? C134 C135 H135 119.9 . . ? C136 C135 H135 119.9 . . ? C135 C136 C131 120.4(4) . . ? C135 C136 H136 119.8 . . ? C131 C136 H136 119.8 . . ? C142 C141 C146 118.4(4) . . ? C142 C141 C1M4 119.1(4) . . ? C146 C141 C1M4 122.5(4) . . ? C143 C142 C141 121.0(4) . . ? C143 C142 H142 119.5 . . ? C141 C142 H142 119.5 . . ? C142 C143 C144 120.5(5) . . ? C142 C143 H143 119.8 . . ? C144 C143 H143 119.8 . . ? C143 C144 C145 119.1(4) . . ? C143 C144 H144 120.5 . . ? C145 C144 H144 120.5 . . ? C144 C145 C146 120.7(4) . . ? C144 C145 H145 119.7 . . ? C146 C145 H145 119.7 . . ? C145 C146 C141 120.4(4) . . ? C145 C146 H146 119.8 . . ? C141 C146 H146 119.8 . . ? C2A2 N21 C2A1 109.9(3) . . ? C2A2 N21 H21 125.0 . . ? C2A1 N21 H21 125.0 . . ? C2A3 N22 C2A4 106.0(3) . . ? C2A5 N23 C2A6 109.9(3) . . ? C2A5 N23 H23 125.1 . . ? C2A6 N23 H23 125.1 . . ? C2A8 N24 C2A7 105.6(3) . . ? N21 C2A1 C2M4 124.7(3) . . ? N21 C2A1 C2B1 107.5(3) . . ? C2M4 C2A1 C2B1 127.8(3) . . ? N21 C2A2 C2M1 128.4(3) . . ? N21 C2A2 C2B2 107.2(3) . . ? C2M1 C2A2 C2B2 124.4(3) . . ? N22 C2A3 C2M1 125.2(3) . . ? N22 C2A3 C2B3 109.4(3) . . ? C2M1 C2A3 C2B3 125.3(3) . . ? N22 C2A4 C2M2 125.7(3) . . ? N22 C2A4 C2B4 110.0(3) . . ? C2M2 C2A4 C2B4 124.1(4) . . ? N23 C2A5 C2M2 126.8(3) . . ? N23 C2A5 C2B5 107.9(3) . . ? C2M2 C2A5 C2B5 125.2(4) . . ? N23 C2A6 C2M3 126.6(3) . . ? N23 C2A6 C2B6 106.7(3) . . ? C2M3 C2A6 C2B6 126.7(3) . . ? N24 C2A7 C2M3 125.1(3) . . ? N24 C2A7 C2B7 110.0(3) . . ? C2M3 C2A7 C2B7 124.7(3) . . ? N24 C2A8 C2M4 126.2(3) . . ? N24 C2A8 C2B8 110.0(3) . . ? C2M4 C2A8 C2B8 123.6(3) . . ? C2B2 C2B1 C2A1 105.8(3) . . ? C2B2 C2B1 C1B1 123.4(3) . . ? C2A1 C2B1 C1B1 130.5(3) . . ? C2B1 C2B2 C2A2 109.6(3) . . ? C2B1 C2B2 H2B2 125.2 . . ? C2A2 C2B2 H2B2 125.2 . . ? C2B4 C2B3 C2A3 107.8(4) . . ? C2B4 C2B3 H2B3 126.1 . . ? C2A3 C2B3 H2B3 126.1 . . ? C2B3 C2B4 C2A4 106.9(4) . . ? C2B3 C2B4 H2B4 126.6 . . ? C2A4 C2B4 H2B4 126.6 . . ? C2B6 C2B5 C2A5 107.6(3) . . ? C2B6 C2B5 H2B5 126.2 . . ? C2A5 C2B5 H2B5 126.2 . . ? C2B5 C2B6 C2A6 107.9(3) . . ? C2B5 C2B6 H2B6 126.0 . . ? C2A6 C2B6 H2B6 126.0 . . ? C2B8 C2B7 C2A7 107.1(3) . . ? C2B8 C2B7 H2B7 126.5 . . ? C2A7 C2B7 H2B7 126.5 . . ? C2B7 C2B8 C2A8 107.2(3) . . ? C2B7 C2B8 H2B8 126.4 . . ? C2A8 C2B8 H2B8 126.4 . . ? C2A2 C2M1 C2A3 126.2(3) . . ? C2A2 C2M1 C211 117.6(3) . . ? C2A3 C2M1 C211 116.2(3) . . ? C2A5 C2M2 C2A4 124.7(4) . . ? C2A5 C2M2 C221 118.9(3) . . ? C2A4 C2M2 C221 116.2(3) . . ? C2A6 C2M3 C2A7 126.5(3) . . ? C2A6 C2M3 C231 115.9(3) . . ? C2A7 C2M3 C231 117.6(3) . . ? C2A1 C2M4 C2A8 124.6(3) . . ? C2A1 C2M4 C241 120.1(3) . . ? C2A8 C2M4 C241 115.0(3) . . ? C216 C211 C212 118.3(4) . . ? C216 C211 C2M1 121.6(4) . . ? C212 C211 C2M1 120.1(4) . . ? C211 C212 C213 120.8(5) . . ? C211 C212 H212 119.6 . . ? C213 C212 H212 119.6 . . ? C214 C213 C212 119.4(5) . . ? C214 C213 H213 120.3 . . ? C212 C213 H213 120.3 . . ? C215 C214 C213 120.7(4) . . ? C215 C214 H214 119.7 . . ? C213 C214 H214 119.7 . . ? C214 C215 C216 120.3(5) . . ? C214 C215 H215 119.9 . . ? C216 C215 H215 119.9 . . ? C215 C216 C211 120.6(5) . . ? C215 C216 H216 119.7 . . ? C211 C216 H216 119.7 . . ? C222 C221 C226 118.9(4) . . ? C222 C221 C2M2 120.2(4) . . ? C226 C221 C2M2 120.9(4) . . ? C221 C222 C223 121.4(5) . . ? C221 C222 H222 119.3 . . ? C223 C222 H222 119.3 . . ? C224 C223 C222 119.2(6) . . ? C224 C223 H223 120.4 . . ? C222 C223 H223 120.4 . . ? C225 C224 C223 120.3(5) . . ? C225 C224 H224 119.9 . . ? C223 C224 H224 119.9 . . ? C224 C225 C226 120.1(5) . . ? C224 C225 H225 120.0 . . ? C226 C225 H225 120.0 . . ? C221 C226 C225 120.2(5) . . ? C221 C226 H226 119.9 . . ? C225 C226 H226 119.9 . . ? C232 C231 C236 118.5(4) . . ? C232 C231 C2M3 120.7(4) . . ? C236 C231 C2M3 120.7(4) . . ? C231 C232 C233 120.7(4) . . ? C231 C232 H232 119.6 . . ? C233 C232 H232 119.6 . . ? C234 C233 C232 120.0(4) . . ? C234 C233 H233 120.0 . . ? C232 C233 H233 120.0 . . ? C233 C234 C235 120.2(4) . . ? C233 C234 H234 119.9 . . ? C235 C234 H234 119.9 . . ? C234 C235 C236 119.7(5) . . ? C234 C235 H235 120.1 . . ? C236 C235 H235 120.1 . . ? C235 C236 C231 120.7(5) . . ? C235 C236 H236 119.6 . . ? C231 C236 H236 119.6 . . ? C246 C241 C242 118.9(4) . . ? C246 C241 C2M4 118.4(3) . . ? C242 C241 C2M4 122.4(4) . . ? C241 C242 C243 120.9(5) . . ? C241 C242 H242 119.6 . . ? C243 C242 H242 119.6 . . ? C244 C243 C242 119.1(5) . . ? C244 C243 H243 120.5 . . ? C242 C243 H243 120.5 . . ? C245 C244 C243 120.0(5) . . ? C245 C244 H244 120.0 . . ? C243 C244 H244 120.0 . . ? C244 C245 C246 120.8(5) . . ? C244 C245 H245 119.6 . . ? C246 C245 H245 119.6 . . ? C241 C246 C245 120.2(4) . . ? C241 C246 H246 119.9 . . ? C245 C246 H246 119.9 . . ? C3A2 N31 C3A1 107.2(3) . . ? C3A3 N32 C3A4 111.3(3) . . ? C3A3 N32 H32 124.3 . . ? C3A4 N32 H32 124.3 . . ? C3A6 N33 C3A5 105.6(3) . . ? C3A7 N34 C3A8 111.0(3) . . ? C3A7 N34 H34 124.5 . . ? C3A8 N34 H34 124.5 . . ? N31 C3A1 C3M4 124.9(3) . . ? N31 C3A1 C3B1 112.8(3) . . ? C3M4 C3A1 C3B1 121.6(3) . . ? N31 C3A2 C3M1 127.1(3) . . ? N31 C3A2 C3B2 112.4(3) . . ? C3M1 C3A2 C3B2 120.0(3) . . ? N32 C3A3 C3M1 126.9(3) . . ? N32 C3A3 C3B3 106.2(3) . . ? C3M1 C3A3 C3B3 126.8(3) . . ? C3M2 C3A4 N32 125.8(3) . . ? C3M2 C3A4 C3B4 128.7(4) . . ? N32 C3A4 C3B4 105.5(3) . . ? N33 C3A5 C3M2 126.3(3) . . ? N33 C3A5 C3B5 110.7(3) . . ? C3M2 C3A5 C3B5 122.9(4) . . ? N33 C3A6 C3M3 124.8(4) . . ? N33 C3A6 C3B6 110.3(3) . . ? C3M3 C3A6 C3B6 124.8(4) . . ? C3M3 C3A7 N34 126.0(4) . . ? C3M3 C3A7 C3B7 128.4(4) . . ? N34 C3A7 C3B7 105.4(4) . . ? N34 C3A8 C3M4 127.4(3) . . ? N34 C3A8 C3B8 106.2(3) . . ? C3M4 C3A8 C3B8 126.1(4) . . ? C3A1 C3B1 C4B1 108.8(3) . . ? C3A1 C3B1 C3B2 101.9(3) . . ? C4B1 C3B1 C3B2 110.1(3) . . ? C3A1 C3B1 H3B1 111.9 . . ? C4B1 C3B1 H3B1 111.9 . . ? C3B2 C3B1 H3B1 111.9 . . ? C3A2 C3B2 C3B1 102.5(3) . . ? C3A2 C3B2 C320 102.4(3) . . ? C3B1 C3B2 C320 116.0(3) . . ? C3A2 C3B2 H3B2 111.7 . . ? C3B1 C3B2 H3B2 111.7 . . ? C320 C3B2 H3B2 111.7 . . ? C3B4 C3B3 C3A3 108.0(3) . . ? C3B4 C3B3 H3B3 126.0 . . ? C3A3 C3B3 H3B3 126.0 . . ? C3B3 C3B4 C3A4 109.0(3) . . ? C3B3 C3B4 H3B4 125.5 . . ? C3A4 C3B4 H3B4 125.5 . . ? C3B6 C3B5 C3A5 106.0(4) . . ? C3B6 C3B5 H3B5 127.0 . . ? C3A5 C3B5 H3B5 127.0 . . ? C3B5 C3B6 C3A6 107.4(4) . . ? C3B5 C3B6 H3B6 126.3 . . ? C3A6 C3B6 H3B6 126.3 . . ? C3B8 C3B7 C3A7 109.5(4) . . ? C3B8 C3B7 H3B7 125.2 . . ? C3A7 C3B7 H3B7 125.2 . . ? C3B7 C3B8 C3A8 107.8(4) . . ? C3B7 C3B8 H3B8 126.1 . . ? C3A8 C3B8 H3B8 126.1 . . ? C3A2 C3M1 C3A3 123.8(3) . . ? C3A2 C3M1 C310 118.5(3) . . ? C3A3 C3M1 C310 117.7(3) . . ? C3A4 C3M2 C3A5 126.6(3) . . ? C3A4 C3M2 C321 116.3(3) . . ? C3A5 C3M2 C321 117.0(3) . . ? C3A7 C3M3 C3A6 124.8(4) . . ? C3A7 C3M3 C331 116.0(4) . . ? C3A6 C3M3 C331 119.2(4) . . ? C3A1 C3M4 C3A8 126.6(4) . . ? C3A1 C3M4 C341 117.7(3) . . ? C3A8 C3M4 C341 115.7(3) . . ? C311 C310 C319 118.3(3) . . ? C311 C310 C3M1 117.9(3) . . ? C319 C310 C3M1 123.8(3) . . ? C310 C311 C312 122.5(4) . . ? C310 C311 H311 118.7 . . ? C312 C311 H311 118.7 . . ? C313 C312 C311 119.7(4) . . ? C313 C312 H312 120.1 . . ? C311 C312 H312 120.1 . . ? C312 C313 C314 121.4(4) . . ? C312 C313 H313 119.3 . . ? C314 C313 H313 119.3 . . ? C315 C314 C313 121.6(4) . . ? C315 C314 C319 119.6(4) . . ? C313 C314 C319 118.9(4) . . ? C316 C315 C314 121.4(4) . . ? C316 C315 H316 119.3 . . ? C314 C315 H316 119.3 . . ? C315 C316 C317 120.9(4) . . ? C315 C316 H317 119.5 . . ? C317 C316 H317 119.5 . . ? C318 C317 C316 119.7(4) . . ? C318 C317 H318 120.2 . . ? C316 C317 H318 120.2 . . ? C317 C318 C319 121.3(4) . . ? C317 C318 C320 116.3(4) . . ? C319 C318 C320 121.3(3) . . ? C318 C319 C314 116.5(4) . . ? C318 C319 C310 125.0(3) . . ? C314 C319 C310 118.5(4) . . ? O2 C320 C318 123.9(4) . . ? O2 C320 C3B2 121.6(3) . . ? C318 C320 C3B2 114.5(3) . . ? C322 C321 C326 120.0 . . ? C322 C321 C3M2 119.7(2) . . ? C326 C321 C3M2 120.2(2) . . ? C321 C322 C323 120.0 . . ? C321 C322 H322 120.0 . . ? C323 C322 H322 120.0 . . ? C324 C323 C322 120.0 . . ? C324 C323 H323 120.0 . . ? C322 C323 H323 120.0 . . ? C323 C324 C325 120.0 . . ? C323 C324 H324 120.0 . . ? C325 C324 H324 120.0 . . ? C326 C325 C324 120.0 . . ? C326 C325 H325 120.0 . . ? C324 C325 H325 120.0 . . ? C325 C326 C321 120.0 . . ? C325 C326 H326 120.0 . . ? C321 C326 H326 120.0 . . ? C332 C331 C336 118.0(4) . . ? C332 C331 C3M3 123.6(4) . . ? C336 C331 C3M3 118.4(4) . . ? C331 C332 C333 119.9(5) . . ? C331 C332 H332 120.1 . . ? C333 C332 H332 120.1 . . ? C334 C333 C332 120.0(5) . . ? C334 C333 H333 120.0 . . ? C332 C333 H333 120.0 . . ? C335 C334 C333 120.5(5) . . ? C335 C334 H334 119.7 . . ? C333 C334 H334 119.7 . . ? C334 C335 C336 119.9(5) . . ? C334 C335 H335 120.1 . . ? C336 C335 H335 120.1 . . ? C335 C336 C331 121.6(5) . . ? C335 C336 H336 119.2 . . ? C331 C336 H336 119.2 . . ? C346 C341 C342 118.2(4) . . ? C346 C341 C3M4 119.7(4) . . ? C342 C341 C3M4 122.0(4) . . ? C343 C342 C341 119.8(5) . . ? C343 C342 H342 120.1 . . ? C341 C342 H342 120.1 . . ? C344 C343 C342 120.9(5) . . ? C344 C343 H343 119.5 . . ? C342 C343 H343 119.5 . . ? C345 C344 C343 119.5(5) . . ? C345 C344 H344 120.2 . . ? C343 C344 H344 120.2 . . ? C344 C345 C346 120.0(5) . . ? C344 C345 H345 120.0 . . ? C346 C345 H345 120.0 . . ? C341 C346 C345 121.5(5) . . ? C341 C346 H346 119.2 . . ? C345 C346 H346 119.2 . . ? C4A2 N41 C4A1 110.1(3) . . ? C4A2 N41 H41 125.0 . . ? C4A1 N41 H41 125.0 . . ? C4A3 N42 C4A4 105.5(3) . . ? C4A6 N43 C4A5 109.0(3) . . ? C4A6 N43 H43 125.5 . . ? C4A5 N43 H43 125.5 . . ? C4A8 N44 C4A7 106.2(3) . . ? N41 C4A1 C4M4 124.6(3) . . ? N41 C4A1 C4B1 106.9(3) . . ? C4M4 C4A1 C4B1 128.5(3) . . ? N41 C4A2 C4M1 127.8(4) . . ? N41 C4A2 C4B2 107.1(3) . . ? C4M1 C4A2 C4B2 125.0(4) . . ? N42 C4A3 C4M1 125.4(4) . . ? N42 C4A3 C4B3 110.2(3) . . ? C4M1 C4A3 C4B3 124.4(4) . . ? N42 C4A4 C4M2 126.1(4) . . ? N42 C4A4 C4B4 110.2(3) . . ? C4M2 C4A4 C4B4 123.6(4) . . ? N43 C4A5 C4M2 126.6(3) . . ? N43 C4A5 C4B5 107.0(3) . . ? C4M2 C4A5 C4B5 126.1(3) . . ? N43 C4A6 C4M3 125.6(3) . . ? N43 C4A6 C4B6 108.1(3) . . ? C4M3 C4A6 C4B6 126.2(4) . . ? N44 C4A7 C4M3 125.6(3) . . ? N44 C4A7 C4B7 110.0(3) . . ? C4M3 C4A7 C4B7 124.2(3) . . ? N44 C4A8 C4M4 126.8(3) . . ? N44 C4A8 C4B8 109.1(3) . . ? C4M4 C4A8 C4B8 124.0(3) . . ? C4B2 C4B1 C4A1 106.3(3) . . ? C4B2 C4B1 C3B1 122.6(3) . . ? C4A1 C4B1 C3B1 130.7(3) . . ? C4B1 C4B2 C4A2 109.6(3) . . ? C4B1 C4B2 H4B2 125.2 . . ? C4A2 C4B2 H4B2 125.2 . . ? C4B4 C4B3 C4A3 107.3(4) . . ? C4B4 C4B3 H4B3 126.3 . . ? C4A3 C4B3 H4B3 126.3 . . ? C4B3 C4B4 C4A4 106.7(4) . . ? C4B3 C4B4 H4B4 126.7 . . ? C4A4 C4B4 H4B4 126.7 . . ? C4B6 C4B5 C4A5 107.9(3) . . ? C4B6 C4B5 H4B5 126.1 . . ? C4A5 C4B5 H4B5 126.1 . . ? C4B5 C4B6 C4A6 107.9(4) . . ? C4B5 C4B6 H4B6 126.0 . . ? C4A6 C4B6 H4B6 126.0 . . ? C4B8 C4B7 C4A7 106.5(3) . . ? C4B8 C4B7 H4B7 126.7 . . ? C4A7 C4B7 H4B7 126.7 . . ? C4B7 C4B8 C4A8 108.0(4) . . ? C4B7 C4B8 H4B8 126.0 . . ? C4A8 C4B8 H4B8 126.0 . . ? C4A3 C4M1 C4A2 125.8(4) . . ? C4A3 C4M1 C411 118.2(3) . . ? C4A2 C4M1 C411 116.0(3) . . ? C4A4 C4M2 C4A5 125.2(4) . . ? C4A4 C4M2 C421 116.3(4) . . ? C4A5 C4M2 C421 118.3(3) . . ? C4A7 C4M3 C4A6 125.8(3) . . ? C4A7 C4M3 C431 117.6(3) . . ? C4A6 C4M3 C431 116.6(3) . . ? C4A1 C4M4 C4A8 125.5(3) . . ? C4A1 C4M4 C441 118.9(3) . . ? C4A8 C4M4 C441 115.2(3) . . ? C412 C411 C416 118.5(4) . . ? C412 C411 C4M1 121.7(4) . . ? C416 C411 C4M1 119.8(4) . . ? C411 C412 C413 122.2(5) . . ? C411 C412 H412 118.9 . . ? C413 C412 H412 118.9 . . ? C414 C413 C412 119.4(6) . . ? C414 C413 H413 120.3 . . ? C412 C413 H413 120.3 . . ? C413 C414 C415 120.1(5) . . ? C413 C414 H414 119.9 . . ? C415 C414 H414 119.9 . . ? C414 C415 C416 120.2(6) . . ? C414 C415 H415 119.9 . . ? C416 C415 H415 119.9 . . ? C415 C416 C411 119.5(5) . . ? C415 C416 H416 120.3 . . ? C411 C416 H416 120.3 . . ? C426 C421 C422 118.4(4) . . ? C426 C421 C4M2 120.4(4) . . ? C422 C421 C4M2 121.1(4) . . ? C423 C422 C421 120.8(4) . . ? C423 C422 H422 119.6 . . ? C421 C422 H422 119.6 . . ? C424 C423 C422 120.2(5) . . ? C424 C423 H423 119.9 . . ? C422 C423 H423 119.9 . . ? C423 C424 C425 119.7(5) . . ? C423 C424 H424 120.1 . . ? C425 C424 H424 120.1 . . ? C424 C425 C426 120.1(5) . . ? C424 C425 H425 120.0 . . ? C426 C425 H425 120.0 . . ? C421 C426 C425 120.7(5) . . ? C421 C426 H426 119.6 . . ? C425 C426 H426 119.6 . . ? C432 C431 C436 118.5(4) . . ? C432 C431 C4M3 120.9(4) . . ? C436 C431 C4M3 120.6(4) . . ? C431 C432 C433 121.2(4) . . ? C431 C432 H432 119.4 . . ? C433 C432 H432 119.4 . . ? C434 C433 C432 120.2(4) . . ? C434 C433 H433 119.9 . . ? C432 C433 H433 119.9 . . ? C435 C434 C433 118.7(4) . . ? C435 C434 H434 120.7 . . ? C433 C434 H434 120.7 . . ? C434 C435 C436 120.6(5) . . ? C434 C435 H435 119.7 . . ? C436 C435 H435 119.7 . . ? C435 C436 C431 120.9(4) . . ? C435 C436 H436 119.6 . . ? C431 C436 H436 119.6 . . ? C442 C441 C446 118.1(4) . . ? C442 C441 C4M4 123.8(3) . . ? C446 C441 C4M4 118.1(3) . . ? C441 C442 C443 120.7(4) . . ? C441 C442 H442 119.7 . . ? C443 C442 H442 119.7 . . ? C444 C443 C442 120.1(4) . . ? C444 C443 H443 120.0 . . ? C442 C443 H443 120.0 . . ? C443 C444 C445 120.6(5) . . ? C443 C444 H444 119.7 . . ? C445 C444 H444 119.7 . . ? C446 C445 C444 120.2(5) . . ? C446 C445 H445 119.9 . . ? C444 C445 H445 119.9 . . ? C445 C446 C441 120.3(4) . . ? C445 C446 H446 119.8 . . ? C441 C446 H446 119.8 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.377 _refine_diff_density_min -0.413 _refine_diff_density_rms 0.063 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.146 0.272 0.256 607 102 ' ' 2 -0.146 0.728 0.744 607 100 ' ' 3 0.033 0.618 0.476 14 1 ' ' 4 0.293 0.506 0.612 30 2 ' ' 5 0.264 0.694 0.469 7 1 ' ' 6 0.334 0.750 0.971 13 1 ' ' 7 0.367 0.687 0.615 5 0 ' ' 8 0.384 0.963 0.981 14 2 ' ' 9 0.463 0.265 0.883 29 4 ' ' 10 0.537 0.735 0.117 29 4 ' ' 11 0.616 0.037 0.019 14 2 ' ' 12 0.666 0.250 0.029 13 1 ' ' 13 0.639 0.333 0.385 6 0 ' ' 14 0.712 0.503 0.388 29 4 ' ' 15 0.736 0.306 0.531 7 1 ' ' 16 0.967 0.382 0.524 14 2 ' ' _platon_squeeze_details ; ; #===END #============================================================================== #============================================================================== data_shelxl _database_code_depnum_ccdc_archive 'CCDC 851200' #TrackingRef 'web_deposit_cif_file_1_chuanjianghu_1319705833.shelxl.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C49 H30 N4 O' _chemical_formula_sum 'C49 H30 N4 O' _chemical_formula_weight 690.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.166(3) _cell_length_b 13.222(3) _cell_length_c 19.062(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.98(3) _cell_angle_gamma 90.00 _cell_volume 3526.6(12) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 14968 _cell_measurement_theta_min 3.0814 _cell_measurement_theta_max 27.5398 _exptl_crystal_description Prism _exptl_crystal_colour Green _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.45 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.301 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1440 _exptl_absorpt_coefficient_mu 0.079 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9543 _exptl_absorpt_correction_T_max 0.9655 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite __diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19714 _diffrn_reflns_av_R_equivalents 0.0412 _diffrn_reflns_av_sigmaI/netI 0.0515 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 27.49 _reflns_number_total 8022 _reflns_number_gt 6327 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0748P)^2^+0.5966P] 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 SHELXL _refine_ls_extinction_coef 0.0281(19) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8022 _refine_ls_number_parameters 488 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0849 _refine_ls_R_factor_gt 0.0666 _refine_ls_wR_factor_ref 0.1680 _refine_ls_wR_factor_gt 0.1555 _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_restrained_S_all 1.114 _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 N1 N 0.04591(11) 0.36338(11) 0.44118(8) 0.0379(4) Uani 1 1 d . . . H1 H 0.0394 0.3921 0.3997 0.045 Uiso 1 1 calc R . . N2 N -0.02086(11) 0.29714(12) 0.29827(8) 0.0402(4) Uani 1 1 d . . . N3 N 0.05197(11) 0.47558(12) 0.23905(8) 0.0402(4) Uani 1 1 d . . . H3 H 0.0482 0.4532 0.2814 0.048 Uiso 1 1 calc R . . N4 N 0.11536(10) 0.54464(11) 0.38242(7) 0.0369(3) Uani 1 1 d . . . C(A1 C 0.10393(13) 0.39700(14) 0.50111(9) 0.0375(4) Uani 1 1 d . . . C(A2 C 0.00013(13) 0.27785(14) 0.45711(9) 0.0368(4) Uani 1 1 d . . . C(A3 C -0.06404(14) 0.22596(14) 0.33443(10) 0.0412(4) Uani 1 1 d . . . C(A4 C -0.03282(14) 0.26718(15) 0.22859(10) 0.0428(4) Uani 1 1 d . . . C(A5 C 0.02958(13) 0.42194(15) 0.17753(9) 0.0400(4) Uani 1 1 d . . . C(A6 C 0.08134(13) 0.57014(15) 0.22329(9) 0.0396(4) Uani 1 1 d . . . C(A7 C 0.13295(13) 0.63095(14) 0.34664(9) 0.0372(4) Uani 1 1 d . . . C(A8 C 0.15582(12) 0.55863(14) 0.45204(9) 0.0373(4) Uani 1 1 d . . . C(B1 C 0.09990(14) 0.32486(15) 0.55521(10) 0.0418(4) Uani 1 1 d . . . H(B1 H 0.1356 0.3266 0.6011 0.050 Uiso 1 1 calc R . . C(B2 C 0.03475(13) 0.25166(15) 0.52913(9) 0.0412(4) Uani 1 1 d . . . C(B3 C -0.10185(16) 0.14649(15) 0.28555(11) 0.0493(5) Uani 1 1 d . . . H(B3 H -0.1353 0.0887 0.2967 0.059 Uiso 1 1 calc R . . C(B4 C -0.08042(17) 0.17048(15) 0.22161(11) 0.0505(5) Uani 1 1 d . . . H(B4 H -0.0939 0.1316 0.1800 0.061 Uiso 1 1 calc R . . C(B5 C 0.04545(14) 0.48604(16) 0.11986(10) 0.0449(5) Uani 1 1 d . . . H(B5 H 0.0364 0.4682 0.0715 0.054 Uiso 1 1 calc R . . C(B6 C 0.07577(14) 0.57691(16) 0.14755(10) 0.0449(5) Uani 1 1 d . . . H(B6 H 0.0905 0.6340 0.1219 0.054 Uiso 1 1 calc R . . C(B7 C 0.18323(13) 0.70270(14) 0.39582(10) 0.0410(4) Uani 1 1 d . . . H(B7 H 0.2022 0.7683 0.3851 0.049 Uiso 1 1 calc R . . C(B8 C 0.19784(14) 0.65795(14) 0.45988(10) 0.0421(4) Uani 1 1 d . . . H(B8 H 0.2298 0.6864 0.5022 0.051 Uiso 1 1 calc R . . C(M1 C -0.06518(13) 0.22235(14) 0.40816(10) 0.0388(4) Uani 1 1 d . . . C(M2 C -0.00870(14) 0.32380(15) 0.17169(9) 0.0412(4) Uani 1 1 d . . . C(M3 C 0.11557(13) 0.64487(14) 0.27251(9) 0.0377(4) Uani 1 1 d . . . C(M4 C 0.15498(13) 0.48849(14) 0.50747(9) 0.0381(4) Uani 1 1 d . . . C10 C -0.14202(14) 0.16028(15) 0.43122(10) 0.0434(4) Uani 1 1 d . . . C11 C -0.23028(15) 0.17021(17) 0.38797(12) 0.0523(5) Uani 1 1 d . . . H11 H -0.2370 0.2198 0.3522 0.063 Uiso 1 1 calc R . . C12 C -0.30918(17) 0.1101(2) 0.39506(14) 0.0649(6) Uani 1 1 d . . . H12 H -0.3680 0.1202 0.3654 0.078 Uiso 1 1 calc R . . C13 C -0.29958(17) 0.0373(2) 0.44524(14) 0.0661(7) Uani 1 1 d . . . H13 H -0.3507 -0.0073 0.4477 0.079 Uiso 1 1 calc R . . C14 C -0.21483(16) 0.02669(17) 0.49389(12) 0.0538(5) Uani 1 1 d . . . C15 C -0.20904(19) -0.05020(19) 0.54541(13) 0.0621(6) Uani 1 1 d . . . H15 H -0.2613 -0.0940 0.5455 0.075 Uiso 1 1 calc R . . C16 C -0.13023(18) -0.06273(18) 0.59479(13) 0.0606(6) Uani 1 1 d . . . H16 H -0.1257 -0.1171 0.6269 0.073 Uiso 1 1 calc R . . C17 C -0.05564(17) 0.00701(17) 0.59694(11) 0.0522(5) Uani 1 1 d . . . H17 H -0.0027 0.0010 0.6331 0.063 Uiso 1 1 calc R . . C18 C -0.05649(14) 0.08428(15) 0.54814(10) 0.0437(4) Uani 1 1 d . . . C19 C -0.13428(14) 0.09345(15) 0.49097(10) 0.0430(4) Uani 1 1 d . . . C20 C 0.02347(16) 0.15779(17) 0.56798(11) 0.0500(5) Uani 1 1 d . . . O1 O 0.08138(15) 0.14223(15) 0.62137(10) 0.0863(7) Uani 1 1 d . . . C21 C -0.02843(15) 0.27815(15) 0.09916(10) 0.0437(4) Uani 1 1 d . . . C22 C 0.04614(18) 0.2568(2) 0.06223(12) 0.0636(6) Uani 1 1 d . . . H22 H 0.1092 0.2717 0.0830 0.076 Uiso 1 1 calc R . . C23 C 0.0291(2) 0.2140(2) -0.00469(13) 0.0707(7) Uani 1 1 d . . . H23 H 0.0803 0.2008 -0.0293 0.085 Uiso 1 1 calc R . . C24 C -0.0632(2) 0.19050(19) -0.03537(12) 0.0637(6) Uani 1 1 d . . . H24 H -0.0749 0.1598 -0.0804 0.076 Uiso 1 1 calc R . . C25 C -0.13737(18) 0.21213(18) 0.00006(11) 0.0573(6) Uani 1 1 d . . . H25 H -0.2002 0.1962 -0.0207 0.069 Uiso 1 1 calc R . . C26 C -0.12073(16) 0.25744(17) 0.06662(10) 0.0502(5) Uani 1 1 d . . . H26 H -0.1726 0.2742 0.0897 0.060 Uiso 1 1 calc R . . C31 C 0.14344(13) 0.74435(14) 0.24500(9) 0.0400(4) Uani 1 1 d . . . C32 C 0.22387(15) 0.75225(18) 0.21150(11) 0.0510(5) Uani 1 1 d . . . H32 H 0.2599 0.6942 0.2054 0.061 Uiso 1 1 calc R . . C33 C 0.25121(17) 0.8450(2) 0.18713(13) 0.0610(6) Uani 1 1 d . . . H33 H 0.3052 0.8493 0.1642 0.073 Uiso 1 1 calc R . . C34 C 0.19920(18) 0.93107(19) 0.19654(12) 0.0611(6) Uani 1 1 d . . . H34 H 0.2179 0.9940 0.1803 0.073 Uiso 1 1 calc R . . C35 C 0.11981(17) 0.92414(16) 0.22974(11) 0.0536(5) Uani 1 1 d . . . H35 H 0.0843 0.9826 0.2361 0.064 Uiso 1 1 calc R . . C36 C 0.09192(15) 0.83147(15) 0.25384(10) 0.0453(5) Uani 1 1 d . . . H36 H 0.0376 0.8277 0.2764 0.054 Uiso 1 1 calc R . . C41 C 0.20963(14) 0.51568(14) 0.57810(10) 0.0429(4) Uani 1 1 d . . . C42 C 0.30685(15) 0.53813(15) 0.58467(12) 0.0514(5) Uani 1 1 d . . . H42 H 0.3388 0.5310 0.5453 0.062 Uiso 1 1 calc R . . C43 C 0.35680(18) 0.57111(17) 0.64939(13) 0.0620(7) Uani 1 1 d . . . H43 H 0.4220 0.5872 0.6533 0.074 Uiso 1 1 calc R . . C44 C 0.3110(2) 0.58025(17) 0.70769(13) 0.0666(7) Uani 1 1 d . . . H44 H 0.3448 0.6037 0.7510 0.080 Uiso 1 1 calc R . . C45 C 0.2156(2) 0.55513(18) 0.70280(12) 0.0631(7) Uani 1 1 d . . . H45 H 0.1850 0.5597 0.7430 0.076 Uiso 1 1 calc R . . C46 C 0.16499(17) 0.52304(17) 0.63824(10) 0.0519(5) Uani 1 1 d . . . H46 H 0.1000 0.5061 0.6350 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 N1 0.0404(8) 0.0412(8) 0.0302(7) -0.0006(6) -0.0004(6) -0.0027(7) N2 0.0444(8) 0.0412(8) 0.0331(8) -0.0016(6) 0.0003(6) -0.0020(7) N3 0.0449(9) 0.0425(9) 0.0313(8) -0.0003(6) 0.0001(6) -0.0016(7) N4 0.0373(8) 0.0403(8) 0.0316(7) -0.0010(6) 0.0007(6) 0.0007(6) C(A1 0.0350(9) 0.0427(10) 0.0333(9) -0.0019(7) 0.0003(7) 0.0017(8) C(A2 0.0374(9) 0.0381(9) 0.0337(9) -0.0014(7) 0.0019(7) 0.0000(8) C(A3 0.0447(10) 0.0375(10) 0.0377(9) -0.0024(7) -0.0048(8) 0.0001(8) C(A4 0.0487(11) 0.0416(10) 0.0350(9) -0.0043(8) -0.0029(8) 0.0008(8) C(A5 0.0385(9) 0.0455(10) 0.0342(9) -0.0039(7) 0.0006(7) -0.0010(8) C(A6 0.0387(9) 0.0429(10) 0.0356(9) -0.0003(7) 0.0005(7) -0.0001(8) C(A7 0.0345(9) 0.0390(10) 0.0372(9) -0.0038(7) 0.0024(7) 0.0025(8) C(A8 0.0356(9) 0.0393(9) 0.0351(9) -0.0042(7) -0.0006(7) 0.0016(7) C(B1 0.0414(10) 0.0472(11) 0.0339(9) -0.0002(8) -0.0034(7) -0.0008(8) C(B2 0.0423(10) 0.0434(10) 0.0360(9) 0.0013(8) 0.0005(8) -0.0012(8) C(B3 0.0646(13) 0.0371(10) 0.0414(11) -0.0014(8) -0.0064(9) -0.0089(9) C(B4 0.0709(14) 0.0399(10) 0.0361(10) -0.0049(8) -0.0056(9) -0.0046(10) C(B5 0.0463(11) 0.0553(12) 0.0317(9) -0.0035(8) 0.0019(8) -0.0046(9) C(B6 0.0464(11) 0.0492(11) 0.0385(10) 0.0020(8) 0.0050(8) -0.0054(9) C(B7 0.0421(10) 0.0381(10) 0.0405(10) -0.0025(7) -0.0006(8) -0.0021(8) C(B8 0.0452(10) 0.0397(10) 0.0387(10) -0.0057(8) -0.0024(8) -0.0022(8) C(M1 0.0401(9) 0.0356(9) 0.0384(9) -0.0011(7) -0.0004(7) 0.0005(8) C(M2 0.0433(10) 0.0441(10) 0.0339(9) -0.0039(7) -0.0014(7) 0.0015(8) C(M3 0.0359(9) 0.0386(10) 0.0374(9) -0.0012(7) 0.0021(7) -0.0001(8) C(M4 0.0357(9) 0.0430(10) 0.0332(9) -0.0059(7) -0.0017(7) 0.0009(8) C10 0.0464(10) 0.0386(10) 0.0440(10) -0.0041(8) 0.0030(8) -0.0043(8) C11 0.0458(11) 0.0490(12) 0.0583(13) -0.0001(9) -0.0035(9) -0.0050(9) C12 0.0468(12) 0.0655(15) 0.0775(17) 0.0037(13) -0.0057(11) -0.0076(11) C13 0.0503(13) 0.0679(16) 0.0788(17) 0.0068(13) 0.0064(12) -0.0156(12) C14 0.0543(12) 0.0494(12) 0.0584(13) -0.0032(10) 0.0115(10) -0.0071(10) C15 0.0651(15) 0.0574(14) 0.0663(15) 0.0023(11) 0.0176(12) -0.0141(12) C16 0.0724(16) 0.0510(13) 0.0606(14) 0.0100(10) 0.0176(12) -0.0053(12) C17 0.0593(13) 0.0493(12) 0.0489(12) 0.0051(9) 0.0109(10) 0.0034(10) C18 0.0498(11) 0.0398(10) 0.0426(10) 0.0009(8) 0.0110(8) 0.0021(9) C19 0.0470(11) 0.0392(10) 0.0435(10) -0.0057(8) 0.0091(8) -0.0011(8) C20 0.0547(12) 0.0537(12) 0.0392(10) 0.0076(9) 0.0000(9) -0.0018(10) O1 0.0923(14) 0.0867(13) 0.0653(11) 0.0339(10) -0.0333(10) -0.0286(11) C21 0.0522(11) 0.0425(10) 0.0341(9) -0.0041(8) -0.0004(8) -0.0007(9) C22 0.0537(13) 0.0804(17) 0.0537(13) -0.0221(12) -0.0011(10) 0.0070(12) C23 0.0720(16) 0.0838(18) 0.0570(14) -0.0248(13) 0.0121(12) 0.0094(14) C24 0.0850(18) 0.0618(14) 0.0409(12) -0.0141(10) -0.0005(11) -0.0043(13) C25 0.0674(14) 0.0598(13) 0.0393(11) -0.0004(9) -0.0083(10) -0.0164(11) C26 0.0548(12) 0.0573(12) 0.0365(10) 0.0006(9) 0.0008(9) -0.0073(10) C31 0.0408(9) 0.0433(10) 0.0336(9) -0.0008(7) -0.0011(7) -0.0052(8) C32 0.0441(11) 0.0559(13) 0.0531(12) -0.0041(10) 0.0082(9) -0.0065(10) C33 0.0538(13) 0.0733(17) 0.0568(13) -0.0024(11) 0.0112(10) -0.0248(12) C34 0.0729(16) 0.0570(14) 0.0505(13) 0.0023(10) 0.0010(11) -0.0289(13) C35 0.0664(14) 0.0429(11) 0.0483(12) 0.0015(9) -0.0013(10) -0.0056(10) C36 0.0480(11) 0.0463(11) 0.0410(10) 0.0007(8) 0.0051(8) -0.0027(9) C41 0.0490(11) 0.0386(10) 0.0366(10) -0.0002(7) -0.0075(8) -0.0006(8) C42 0.0510(12) 0.0446(11) 0.0518(12) 0.0068(9) -0.0135(9) -0.0053(9) C43 0.0660(14) 0.0491(12) 0.0596(14) 0.0116(10) -0.0251(11) -0.0101(11) C44 0.0895(19) 0.0434(12) 0.0527(14) 0.0010(10) -0.0340(13) 0.0012(12) C45 0.0865(18) 0.0567(14) 0.0399(11) -0.0041(10) -0.0092(11) 0.0169(13) C46 0.0571(12) 0.0559(13) 0.0386(10) -0.0040(9) -0.0053(9) 0.0096(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C(A2 1.361(2) . ? N1 C(A1 1.373(2) . ? N1 H1 0.8700 . ? N2 C(A3 1.366(2) . ? N2 C(A4 1.371(2) . ? N3 C(A5 1.365(2) . ? N3 C(A6 1.366(2) . ? N3 H3 0.8700 . ? N4 C(A7 1.372(2) . ? N4 C(A8 1.374(2) . ? C(A1 C(M4 1.405(3) . ? C(A1 C(B1 1.412(3) . ? C(A2 C(M1 1.413(2) . ? C(A2 C(B2 1.427(2) . ? C(A3 C(M1 1.409(3) . ? C(A3 C(B3 1.450(3) . ? C(A4 C(M2 1.403(3) . ? C(A4 C(B4 1.442(3) . ? C(A5 C(M2 1.404(3) . ? C(A5 C(B5 1.433(3) . ? C(A6 C(M3 1.396(3) . ? C(A6 C(B6 1.436(3) . ? C(A7 C(M3 1.408(3) . ? C(A7 C(B7 1.441(2) . ? C(A8 C(M4 1.407(3) . ? C(A8 C(B8 1.440(3) . ? C(B1 C(B2 1.376(3) . ? C(B1 H(B1 0.9400 . ? C(B2 C20 1.467(3) . ? C(B3 C(B4 1.339(3) . ? C(B3 H(B3 0.9400 . ? C(B4 H(B4 0.9400 . ? C(B5 C(B6 1.355(3) . ? C(B5 H(B5 0.9400 . ? C(B6 H(B6 0.9400 . ? C(B7 C(B8 1.344(3) . ? C(B7 H(B7 0.9400 . ? C(B8 H(B8 0.9400 . ? C(M1 C10 1.484(3) . ? C(M2 C21 1.495(3) . ? C(M3 C31 1.492(3) . ? C(M4 C41 1.489(2) . ? C10 C11 1.392(3) . ? C10 C19 1.432(3) . ? C11 C12 1.395(3) . ? C11 H11 0.9400 . ? C12 C13 1.349(3) . ? C12 H12 0.9400 . ? C13 C14 1.405(3) . ? C13 H13 0.9400 . ? C14 C15 1.407(3) . ? C14 C19 1.451(3) . ? C15 C16 1.353(3) . ? C15 H15 0.9400 . ? C16 C17 1.398(3) . ? C16 H16 0.9400 . ? C17 C18 1.381(3) . ? C17 H17 0.9400 . ? C18 C19 1.429(3) . ? C18 C20 1.496(3) . ? C20 O1 1.221(2) . ? C21 C26 1.384(3) . ? C21 C22 1.387(3) . ? C22 C23 1.382(3) . ? C22 H22 0.9400 . ? C23 C24 1.382(4) . ? C23 H23 0.9400 . ? C24 C25 1.365(4) . ? C24 H24 0.9400 . ? C25 C26 1.390(3) . ? C25 H25 0.9400 . ? C26 H26 0.9400 . ? C31 C36 1.388(3) . ? C31 C32 1.394(3) . ? C32 C33 1.388(3) . ? C32 H32 0.9400 . ? C33 C34 1.382(4) . ? C33 H33 0.9400 . ? C34 C35 1.377(3) . ? C34 H34 0.9400 . ? C35 C36 1.388(3) . ? C35 H35 0.9400 . ? C36 H36 0.9400 . ? C41 C42 1.395(3) . ? C41 C46 1.396(3) . ? C42 C43 1.393(3) . ? C42 H42 0.9400 . ? C43 C44 1.377(4) . ? C43 H43 0.9400 . ? C44 C45 1.380(4) . ? C44 H44 0.9400 . ? C45 C46 1.391(3) . ? C45 H45 0.9400 . ? C46 H46 0.9400 . ? 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 C(A2 N1 C(A1 109.11(15) . . ? C(A2 N1 H1 125.4 . . ? C(A1 N1 H1 125.4 . . ? C(A3 N2 C(A4 107.00(15) . . ? C(A5 N3 C(A6 108.93(15) . . ? C(A5 N3 H3 125.5 . . ? C(A6 N3 H3 125.5 . . ? C(A7 N4 C(A8 106.71(15) . . ? N1 C(A1 C(M4 125.71(16) . . ? N1 C(A1 C(B1 107.56(16) . . ? C(M4 C(A1 C(B1 126.69(16) . . ? N1 C(A2 C(M1 124.74(16) . . ? N1 C(A2 C(B2 108.19(15) . . ? C(M1 C(A2 C(B2 126.93(17) . . ? N2 C(A3 C(M1 127.04(16) . . ? N2 C(A3 C(B3 108.94(17) . . ? C(M1 C(A3 C(B3 123.76(18) . . ? N2 C(A4 C(M2 125.90(17) . . ? N2 C(A4 C(B4 109.33(17) . . ? C(M2 C(A4 C(B4 124.65(17) . . ? N3 C(A5 C(M2 125.69(17) . . ? N3 C(A5 C(B5 107.97(17) . . ? C(M2 C(A5 C(B5 126.19(17) . . ? N3 C(A6 C(M3 125.84(17) . . ? N3 C(A6 C(B6 107.90(16) . . ? C(M3 C(A6 C(B6 126.17(18) . . ? N4 C(A7 C(M3 126.21(16) . . ? N4 C(A7 C(B7 109.50(15) . . ? C(M3 C(A7 C(B7 123.91(17) . . ? N4 C(A8 C(M4 125.84(16) . . ? N4 C(A8 C(B8 109.06(16) . . ? C(M4 C(A8 C(B8 125.09(16) . . ? C(B2 C(B1 C(A1 108.21(16) . . ? C(B2 C(B1 H(B1 125.9 . . ? C(A1 C(B1 H(B1 125.9 . . ? C(B1 C(B2 C(A2 106.71(16) . . ? C(B1 C(B2 C20 122.19(17) . . ? C(A2 C(B2 C20 130.02(17) . . ? C(B4 C(B3 C(A3 107.43(18) . . ? C(B4 C(B3 H(B3 126.3 . . ? C(A3 C(B3 H(B3 126.3 . . ? C(B3 C(B4 C(A4 107.17(17) . . ? C(B3 C(B4 H(B4 126.4 . . ? C(A4 C(B4 H(B4 126.4 . . ? C(B6 C(B5 C(A5 107.68(17) . . ? C(B6 C(B5 H(B5 126.2 . . ? C(A5 C(B5 H(B5 126.2 . . ? C(B5 C(B6 C(A6 107.50(17) . . ? C(B5 C(B6 H(B6 126.3 . . ? C(A6 C(B6 H(B6 126.3 . . ? C(B8 C(B7 C(A7 106.95(17) . . ? C(B8 C(B7 H(B7 126.5 . . ? C(A7 C(B7 H(B7 126.5 . . ? C(B7 C(B8 C(A8 107.74(16) . . ? C(B7 C(B8 H(B8 126.1 . . ? C(A8 C(B8 H(B8 126.1 . . ? C(A3 C(M1 C(A2 122.21(17) . . ? C(A3 C(M1 C10 115.94(16) . . ? C(A2 C(M1 C10 121.80(17) . . ? C(A4 C(M2 C(A5 124.71(17) . . ? C(A4 C(M2 C21 117.82(17) . . ? C(A5 C(M2 C21 117.43(17) . . ? C(A6 C(M3 C(A7 124.74(17) . . ? C(A6 C(M3 C31 118.09(16) . . ? C(A7 C(M3 C31 116.98(16) . . ? C(A1 C(M4 C(A8 124.56(16) . . ? C(A1 C(M4 C41 118.29(16) . . ? C(A8 C(M4 C41 117.11(16) . . ? C11 C10 C19 118.64(19) . . ? C11 C10 C(M1 113.90(18) . . ? C19 C10 C(M1 127.46(18) . . ? C10 C11 C12 123.2(2) . . ? C10 C11 H11 118.4 . . ? C12 C11 H11 118.4 . . ? C13 C12 C11 118.8(2) . . ? C13 C12 H12 120.6 . . ? C11 C12 H12 120.6 . . ? C12 C13 C14 121.4(2) . . ? C12 C13 H13 119.3 . . ? C14 C13 H13 119.3 . . ? C13 C14 C15 118.9(2) . . ? C13 C14 C19 120.7(2) . . ? C15 C14 C19 120.4(2) . . ? C16 C15 C14 121.7(2) . . ? C16 C15 H15 119.1 . . ? C14 C15 H15 119.1 . . ? C15 C16 C17 118.5(2) . . ? C15 C16 H16 120.7 . . ? C17 C16 H16 120.7 . . ? C18 C17 C16 122.8(2) . . ? C18 C17 H17 118.6 . . ? C16 C17 H17 118.6 . . ? C17 C18 C19 120.09(19) . . ? C17 C18 C20 112.57(18) . . ? C19 C18 C20 126.96(18) . . ? C18 C19 C10 127.81(18) . . ? C18 C19 C14 115.89(18) . . ? C10 C19 C14 116.30(18) . . ? O1 C20 C(B2 116.84(19) . . ? O1 C20 C18 119.02(19) . . ? C(B2 C20 C18 124.06(17) . . ? C26 C21 C22 118.26(18) . . ? C26 C21 C(M2 121.44(19) . . ? C22 C21 C(M2 120.30(19) . . ? C23 C22 C21 121.0(2) . . ? C23 C22 H22 119.5 . . ? C21 C22 H22 119.5 . . ? C24 C23 C22 120.0(2) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C25 C24 C23 119.6(2) . . ? C25 C24 H24 120.2 . . ? C23 C24 H24 120.2 . . ? C24 C25 C26 120.5(2) . . ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? C21 C26 C25 120.5(2) . . ? C21 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? C36 C31 C32 118.43(19) . . ? C36 C31 C(M3 121.08(18) . . ? C32 C31 C(M3 120.47(18) . . ? C33 C32 C31 120.7(2) . . ? C33 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? C34 C33 C32 120.1(2) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? C35 C34 C33 119.7(2) . . ? C35 C34 H34 120.2 . . ? C33 C34 H34 120.2 . . ? C34 C35 C36 120.4(2) . . ? C34 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C35 C36 C31 120.7(2) . . ? C35 C36 H36 119.7 . . ? C31 C36 H36 119.7 . . ? C42 C41 C46 118.59(18) . . ? C42 C41 C(M4 119.96(19) . . ? C46 C41 C(M4 121.41(18) . . ? C43 C42 C41 120.3(2) . . ? C43 C42 H42 119.9 . . ? C41 C42 H42 119.9 . . ? C44 C43 C42 120.3(2) . . ? C44 C43 H43 119.9 . . ? C42 C43 H43 119.9 . . ? C43 C44 C45 120.3(2) . . ? C43 C44 H44 119.9 . . ? C45 C44 H44 119.9 . . ? C44 C45 C46 119.8(2) . . ? C44 C45 H45 120.1 . . ? C46 C45 H45 120.1 . . ? C45 C46 C41 120.7(2) . . ? C45 C46 H46 119.6 . . ? C41 C46 H46 119.6 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.302 _refine_diff_density_min -0.271 _refine_diff_density_rms 0.071 #===END #==============================================================================