# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Michael Hill' _publ_contact_author_email M.S.HILL@BATH.AC.UK _publ_section_title ; Catalytic 2,3,4-Hexatriene Formation by Terminal Alkyne Coupling at Calcium ; loop_ _publ_author_name 'Michael Hill' 'Anthony Barrett' 'Mark R Crimmin' 'Peter B Hitchcock' 'Sarah L. Lomas' ; P.Procopiou ; 'Kogularamanan Suntharalingam' data_jul1207 _database_code_depnum_ccdc_archive 'CCDC 706557' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C66 H92 Ca2 N4 O2, C7 H8' _chemical_formula_sum 'C73 H100 Ca2 N4 O2' _chemical_formula_weight 1145.73 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' Ca Ca 0.2262 0.3064 '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 triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.2296(2) _cell_length_b 14.3726(3) _cell_length_c 21.2865(4) _cell_angle_alpha 91.5190(10) _cell_angle_beta 104.5370(10) _cell_angle_gamma 115.6400(10) _cell_volume 3489.52(11) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 28675 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 26.022 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.090 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1244 _exptl_absorpt_coefficient_mu 0.208 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9018 _exptl_absorpt_correction_T_max 0.9531 _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54730 _diffrn_reflns_av_R_equivalents 0.0546 _diffrn_reflns_av_sigmaI/netI 0.0489 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 26.06 _reflns_number_total 13704 _reflns_number_gt 10031 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo & Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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. There are two independent molecules of the complex, each straddling an inversion centre. The disordered toluene solvate was included with anisotropic C atoms and H atoms omitted. Distance restraints were applied in the disordered solvent region, where the electron density was subject to considerable smearing. ; _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^)+(0.0554P)^2^+1.8004P] 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 13704 _refine_ls_number_parameters 751 _refine_ls_number_restraints 91 _refine_ls_R_factor_all 0.0777 _refine_ls_R_factor_gt 0.0497 _refine_ls_wR_factor_ref 0.1295 _refine_ls_wR_factor_gt 0.1154 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.138 _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 Ca1 Ca 0.61643(4) 0.61165(3) 0.57158(2) 0.02857(12) Uani 1 1 d . . . Ca1B Ca 0.53472(4) 0.14818(3) 0.99711(2) 0.02558(12) Uani 1 1 d . . . O1 O 0.74896(14) 0.56567(13) 0.65702(8) 0.0396(4) Uani 1 1 d . . . O1B O 0.57722(15) 0.25311(12) 1.10274(8) 0.0365(4) Uani 1 1 d . . . N1 N 0.77792(15) 0.76727(14) 0.56947(9) 0.0284(4) Uani 1 1 d . . . N2 N 0.60474(15) 0.71512(14) 0.65303(9) 0.0265(4) Uani 1 1 d . . . N1B N 0.67039(15) 0.29444(14) 0.96591(9) 0.0278(4) Uani 1 1 d . . . N2B N 0.40940(15) 0.21246(14) 0.93954(8) 0.0258(4) Uani 1 1 d . . . C1 C 0.84014(19) 0.84194(18) 0.62091(11) 0.0321(5) Uani 1 1 d . . . C2 C 0.8074(2) 0.84680(19) 0.67886(11) 0.0336(5) Uani 1 1 d . . . H2 H 0.8698 0.8932 0.7153 0.040 Uiso 1 1 calc R . . C3 C 0.69899(19) 0.79522(17) 0.69230(10) 0.0290(5) Uani 1 1 d . . . C4 C 0.9546(2) 0.9326(2) 0.62018(13) 0.0520(7) Uani 1 1 d . . . H4A H 0.9705 0.9233 0.5785 0.078 Uiso 0.50 1 calc PR . . H4B H 1.0184 0.9352 0.6567 0.078 Uiso 0.50 1 calc PR . . H4C H 0.9489 0.9981 0.6249 0.078 Uiso 0.50 1 calc PR . . H4D H 0.9880 0.9811 0.6615 0.078 Uiso 0.50 1 calc PR . . H4E H 0.9401 0.9692 0.5834 0.078 Uiso 0.50 1 calc PR . . H4F H 1.0096 0.9063 0.6152 0.078 Uiso 0.50 1 calc PR . . C5 C 0.6933(2) 0.8377(2) 0.75648(12) 0.0425(6) Uani 1 1 d . . . H5A H 0.6148 0.7971 0.7613 0.064 Uiso 0.50 1 calc PR . . H5B H 0.7097 0.9110 0.7566 0.064 Uiso 0.50 1 calc PR . . H5C H 0.7516 0.8324 0.7931 0.064 Uiso 0.50 1 calc PR . . H5D H 0.7693 0.8966 0.7794 0.064 Uiso 0.50 1 calc PR . . H5E H 0.6744 0.7826 0.7841 0.064 Uiso 0.50 1 calc PR . . H5F H 0.6325 0.8613 0.7476 0.064 Uiso 0.50 1 calc PR . . C6 C 0.81385(19) 0.77825(17) 0.51026(11) 0.0297(5) Uani 1 1 d . . . C7 C 0.7854(2) 0.83995(18) 0.46630(11) 0.0331(5) Uani 1 1 d . . . C8 C 0.8175(2) 0.8460(2) 0.40847(12) 0.0387(6) Uani 1 1 d . . . H8 H 0.7984 0.8876 0.3784 0.046 Uiso 1 1 calc R . . C9 C 0.8760(2) 0.7931(2) 0.39387(13) 0.0431(6) Uani 1 1 d . . . H9 H 0.8988 0.7995 0.3546 0.052 Uiso 1 1 calc R . . C10 C 0.9011(2) 0.7310(2) 0.43642(13) 0.0443(6) Uani 1 1 d . . . H10 H 0.9401 0.6935 0.4258 0.053 Uiso 1 1 calc R . . C11 C 0.8709(2) 0.7214(2) 0.49498(12) 0.0364(6) Uani 1 1 d . . . C12 C 0.7197(2) 0.8996(2) 0.47833(13) 0.0444(6) Uani 1 1 d . . . H12 H 0.7099 0.8924 0.5233 0.053 Uiso 1 1 calc R . . C13 C 0.5977(3) 0.8535(2) 0.42862(16) 0.0575(8) Uani 1 1 d . . . H13A H 0.6054 0.8629 0.3843 0.086 Uiso 1 1 calc R . . H13B H 0.5542 0.8893 0.4392 0.086 Uiso 1 1 calc R . . H13C H 0.5554 0.7788 0.4305 0.086 Uiso 1 1 calc R . . C14 C 0.7875(3) 1.0167(2) 0.47515(17) 0.0655(9) Uani 1 1 d . . . H14A H 0.8662 1.0453 0.5063 0.098 Uiso 1 1 calc R . . H14B H 0.7458 1.0536 0.4865 0.098 Uiso 1 1 calc R . . H14C H 0.7938 1.0257 0.4306 0.098 Uiso 1 1 calc R . . C15 C 0.9028(3) 0.6527(2) 0.54065(15) 0.0526(7) Uani 1 1 d . . . H15 H 0.8524 0.6362 0.5709 0.063 Uiso 1 1 calc R . . C16 C 1.0291(3) 0.7102(4) 0.5827(3) 0.1201(19) Uani 1 1 d . . . H16A H 1.0807 0.7315 0.5543 0.180 Uiso 1 1 calc R . . H16B H 1.0479 0.6641 0.6113 0.180 Uiso 1 1 calc R . . H16C H 1.0404 0.7723 0.6096 0.180 Uiso 1 1 calc R . . C17 C 0.8778(4) 0.5483(3) 0.5035(2) 0.0927(14) Uani 1 1 d . . . H17A H 0.7944 0.5105 0.4791 0.139 Uiso 1 1 calc R . . H17B H 0.8983 0.5062 0.5349 0.139 Uiso 1 1 calc R . . H17C H 0.9247 0.5618 0.4727 0.139 Uiso 1 1 calc R . . C18 C 0.49361(19) 0.68170(17) 0.66547(10) 0.0283(5) Uani 1 1 d . . . C19 C 0.4302(2) 0.7393(2) 0.64828(12) 0.0377(6) Uani 1 1 d . . . C20 C 0.3188(2) 0.7011(2) 0.65640(14) 0.0500(7) Uani 1 1 d . . . H20 H 0.2759 0.7400 0.6456 0.060 Uiso 1 1 calc R . . C21 C 0.2692(2) 0.6082(3) 0.67975(15) 0.0547(8) Uani 1 1 d . . . H21 H 0.1929 0.5833 0.6848 0.066 Uiso 1 1 calc R . . C22 C 0.3309(2) 0.5520(2) 0.69569(14) 0.0479(7) Uani 1 1 d . . . H22 H 0.2962 0.4877 0.7113 0.057 Uiso 1 1 calc R . . C23 C 0.4438(2) 0.58721(19) 0.68946(11) 0.0342(5) Uani 1 1 d . . . C24 C 0.4780(3) 0.8393(2) 0.61944(14) 0.0486(7) Uani 1 1 d . . . H24 H 0.5624 0.8606 0.6236 0.058 Uiso 1 1 calc R . . C25 C 0.4127(3) 0.8211(3) 0.54647(15) 0.0683(9) Uani 1 1 d . . . H25A H 0.4193 0.7651 0.5233 0.102 Uiso 1 1 calc R . . H25B H 0.4471 0.8855 0.5280 0.102 Uiso 1 1 calc R . . H25C H 0.3299 0.8012 0.5412 0.102 Uiso 1 1 calc R . . C26 C 0.4708(4) 0.9286(3) 0.65567(17) 0.0758(10) Uani 1 1 d . . . H26A H 0.3884 0.9120 0.6490 0.114 Uiso 1 1 calc R . . H26B H 0.5097 0.9933 0.6385 0.114 Uiso 1 1 calc R . . H26C H 0.5097 0.9378 0.7027 0.114 Uiso 1 1 calc R . . C27 C 0.5079(2) 0.52197(19) 0.70826(13) 0.0402(6) Uani 1 1 d . . . H27 H 0.5843 0.5568 0.6979 0.048 Uiso 1 1 calc R . . C28 C 0.5350(3) 0.5155(3) 0.78151(14) 0.0609(8) Uani 1 1 d . . . H28A H 0.5818 0.5861 0.8066 0.091 Uiso 1 1 calc R . . H28B H 0.5790 0.4751 0.7919 0.091 Uiso 1 1 calc R . . H28C H 0.4615 0.4811 0.7931 0.091 Uiso 1 1 calc R . . C29 C 0.4400(3) 0.4122(2) 0.66875(16) 0.0608(8) Uani 1 1 d . . . H29A H 0.3666 0.3746 0.6800 0.091 Uiso 1 1 calc R . . H29B H 0.4874 0.3747 0.6792 0.091 Uiso 1 1 calc R . . H29C H 0.4224 0.4168 0.6217 0.091 Uiso 1 1 calc R . . C30 C 0.5599(2) 0.41831(19) 0.52015(13) 0.0417(6) Uani 1 1 d . . . C31 C 0.6374(2) 0.43151(19) 0.56982(13) 0.0403(6) Uani 1 1 d . . . C32 C 0.7302(2) 0.4638(2) 0.63249(13) 0.0455(6) Uani 1 1 d . . . H32A H 0.7051 0.4145 0.6635 0.055 Uiso 1 1 calc R . . H32B H 0.8027 0.4666 0.6257 0.055 Uiso 1 1 calc R . . C33 C 0.8405(3) 0.6118(3) 0.71749(15) 0.0619(8) Uani 1 1 d . . . H33A H 0.8190 0.5691 0.7516 0.093 Uiso 1 1 calc R . . H33B H 0.8518 0.6823 0.7306 0.093 Uiso 1 1 calc R . . H33C H 0.9133 0.6156 0.7117 0.093 Uiso 1 1 calc R . . C1B C 0.6617(2) 0.38236(17) 0.95985(11) 0.0313(5) Uani 1 1 d . . . C2B C 0.5577(2) 0.39123(17) 0.95335(11) 0.0318(5) Uani 1 1 d . . . H2B H 0.5679 0.4608 0.9595 0.038 Uiso 1 1 calc R . . C3B C 0.44094(19) 0.31312(17) 0.93910(10) 0.0283(5) Uani 1 1 d . . . C4B C 0.7675(2) 0.4826(2) 0.95886(15) 0.0486(7) Uani 1 1 d . . . H4B1 H 0.8354 0.4691 0.9637 0.073 Uiso 0.50 1 calc PR . . H4B2 H 0.7845 0.5356 0.9952 0.073 Uiso 0.50 1 calc PR . . H4B3 H 0.7508 0.5079 0.9170 0.073 Uiso 0.50 1 calc PR . . H4B4 H 0.7451 0.5393 0.9536 0.073 Uiso 0.50 1 calc PR . . H4B5 H 0.7959 0.4728 0.9221 0.073 Uiso 0.50 1 calc PR . . H4B6 H 0.8297 0.5005 1.0003 0.073 Uiso 0.50 1 calc PR . . C5B C 0.3486(2) 0.3517(2) 0.92032(13) 0.0415(6) Uani 1 1 d . . . H5B1 H 0.2705 0.2924 0.9114 0.062 Uiso 0.50 1 calc PR . . H5B2 H 0.3551 0.3849 0.8809 0.062 Uiso 0.50 1 calc PR . . H5B3 H 0.3608 0.4025 0.9565 0.062 Uiso 0.50 1 calc PR . . H5B4 H 0.3871 0.4275 0.9212 0.062 Uiso 0.50 1 calc PR . . H5B5 H 0.3025 0.3350 0.9516 0.062 Uiso 0.50 1 calc PR . . H5B6 H 0.2968 0.3174 0.8760 0.062 Uiso 0.50 1 calc PR . . C6B C 0.77185(19) 0.28706(17) 0.95890(11) 0.0303(5) Uani 1 1 d . . . C7B C 0.7753(2) 0.26132(19) 0.89555(12) 0.0359(6) Uani 1 1 d . . . C8B C 0.8709(2) 0.2481(2) 0.88935(14) 0.0471(7) Uani 1 1 d . . . H8B H 0.8749 0.2317 0.8468 0.056 Uiso 1 1 calc R . . C9B C 0.9597(2) 0.2583(2) 0.94360(15) 0.0507(7) Uani 1 1 d . . . H9B H 1.0244 0.2493 0.9384 0.061 Uiso 1 1 calc R . . C10B C 0.9541(2) 0.2815(2) 1.00543(14) 0.0474(7) Uani 1 1 d . . . H10B H 1.0151 0.2876 1.0427 0.057 Uiso 1 1 calc R . . C11B C 0.8614(2) 0.2964(2) 1.01449(12) 0.0377(6) Uani 1 1 d . . . C12B C 0.6786(2) 0.2477(2) 0.83430(12) 0.0431(6) Uani 1 1 d . . . H12B H 0.6142 0.2521 0.8487 0.052 Uiso 1 1 calc R . . C13B C 0.7207(3) 0.3338(3) 0.79273(17) 0.0699(9) Uani 1 1 d . . . H13D H 0.7510 0.4020 0.8193 0.105 Uiso 1 1 calc R . . H13E H 0.6551 0.3241 0.7549 0.105 Uiso 1 1 calc R . . H13F H 0.7830 0.3304 0.7773 0.105 Uiso 1 1 calc R . . C14B C 0.6278(3) 0.1411(2) 0.79274(15) 0.0602(8) Uani 1 1 d . . . H14D H 0.6883 0.1360 0.7762 0.090 Uiso 1 1 calc R . . H14E H 0.5616 0.1325 0.7556 0.090 Uiso 1 1 calc R . . H14F H 0.6009 0.0862 0.8197 0.090 Uiso 1 1 calc R . . C15B C 0.8612(2) 0.3241(2) 1.08360(13) 0.0505(7) Uani 1 1 d . . . H15B H 0.7857 0.3263 1.0806 0.061 Uiso 1 1 calc R . . C16B C 0.9609(3) 0.4316(3) 1.11634(16) 0.0739(10) Uani 1 1 d . . . H16D H 1.0362 0.4305 1.1222 0.111 Uiso 1 1 calc R . . H16E H 0.9539 0.4495 1.1593 0.111 Uiso 1 1 calc R . . H16F H 0.9565 0.4839 1.0886 0.111 Uiso 1 1 calc R . . C17B C 0.8684(3) 0.2428(3) 1.12710(17) 0.0781(11) Uani 1 1 d . . . H17D H 0.8063 0.1734 1.1054 0.117 Uiso 1 1 calc R . . H17E H 0.8585 0.2594 1.1694 0.117 Uiso 1 1 calc R . . H17F H 0.9449 0.2437 1.1343 0.117 Uiso 1 1 calc R . . C18B C 0.28790(18) 0.13871(17) 0.91518(10) 0.0277(5) Uani 1 1 d . . . C19B C 0.2440(2) 0.08648(19) 0.84989(11) 0.0324(5) Uani 1 1 d . . . C20B C 0.1257(2) 0.0164(2) 0.82660(12) 0.0464(7) Uani 1 1 d . . . H20B H 0.0946 -0.0181 0.7825 0.056 Uiso 1 1 calc R . . C21B C 0.0522(2) -0.0045(3) 0.86578(13) 0.0576(8) Uani 1 1 d . . . H21B H -0.0289 -0.0510 0.8484 0.069 Uiso 1 1 calc R . . C22B C 0.0977(2) 0.0427(2) 0.93041(13) 0.0529(8) Uani 1 1 d . . . H22B H 0.0474 0.0270 0.9577 0.063 Uiso 1 1 calc R . . C23B C 0.2157(2) 0.1128(2) 0.95658(11) 0.0370(6) Uani 1 1 d . . . C24B C 0.3252(2) 0.10544(19) 0.80700(11) 0.0354(5) Uani 1 1 d . . . H24B H 0.4035 0.1187 0.8366 0.042 Uiso 1 1 calc R . . C25B C 0.2852(2) 0.0106(2) 0.75540(13) 0.0466(7) Uani 1 1 d . . . H25D H 0.2694 -0.0518 0.7767 0.070 Uiso 1 1 calc R . . H25E H 0.3469 0.0224 0.7345 0.070 Uiso 1 1 calc R . . H25F H 0.2136 0.0006 0.7221 0.070 Uiso 1 1 calc R . . C26B C 0.3432(3) 0.2017(2) 0.77422(13) 0.0514(7) Uani 1 1 d . . . H26D H 0.2670 0.1950 0.7486 0.077 Uiso 1 1 calc R . . H26E H 0.3918 0.2082 0.7450 0.077 Uiso 1 1 calc R . . H26F H 0.3823 0.2639 0.8079 0.077 Uiso 1 1 calc R . . C27B C 0.2635(2) 0.1530(2) 1.03000(12) 0.0418(6) Uani 1 1 d . . . H27B H 0.3486 0.2027 1.0397 0.050 Uiso 1 1 calc R . . C28B C 0.2038(3) 0.2114(2) 1.05350(14) 0.0526(7) Uani 1 1 d . . . H28D H 0.2111 0.2696 1.0289 0.079 Uiso 1 1 calc R . . H28E H 0.2413 0.2386 1.1005 0.079 Uiso 1 1 calc R . . H28F H 0.1207 0.1636 1.0462 0.079 Uiso 1 1 calc R . . C29B C 0.2536(3) 0.0627(3) 1.06820(13) 0.0544(8) Uani 1 1 d . . . H29D H 0.1708 0.0160 1.0629 0.082 Uiso 1 1 calc R . . H29E H 0.2947 0.0902 1.1149 0.082 Uiso 1 1 calc R . . H29F H 0.2890 0.0237 1.0514 0.082 Uiso 1 1 calc R . . C30B C 0.5239(2) 0.0100(2) 1.08160(12) 0.0397(6) Uani 1 1 d . . . C31B C 0.5505(2) 0.08762(19) 1.11882(11) 0.0373(6) Uani 1 1 d . . . C32B C 0.5796(2) 0.18990(19) 1.15350(12) 0.0409(6) Uani 1 1 d . . . H32C H 0.5212 0.1837 1.1766 0.049 Uiso 1 1 calc R . . H32D H 0.6583 0.2200 1.1859 0.049 Uiso 1 1 calc R . . C33B C 0.6043(3) 0.3575(2) 1.12670(15) 0.0633(9) Uani 1 1 d . . . H33D H 0.5498 0.3558 1.1510 0.095 Uiso 1 1 calc R . . H33E H 0.5968 0.3954 1.0896 0.095 Uiso 1 1 calc R . . H33F H 0.6847 0.3928 1.1559 0.095 Uiso 1 1 calc R . . C1S C 0.9803(3) 0.2698(3) 0.72663(15) 0.112(4) Uani 0.50 1 d PGD A 1 C2S C 0.9181(4) 0.1622(3) 0.72259(18) 0.133(3) Uani 1 1 d GD A 1 C3S C 0.8145(4) 0.1062(3) 0.6724(2) 0.099(3) Uani 0.50 1 d PGD A 1 C4S C 0.7732(3) 0.1577(4) 0.62623(18) 0.214(5) Uani 1 1 d GD A 1 C5S C 0.8354(4) 0.2653(4) 0.63027(18) 0.078(2) Uani 0.50 1 d PGD A 1 C6S C 0.9390(4) 0.3214(3) 0.6805(2) 0.119(2) Uani 1 1 d GD A 1 C7S C 1.0829(3) 0.3308(4) 0.7764(2) 0.127(2) Uani 1 1 d GD A 1 C8S C 0.8777(3) 0.2138(3) 0.67749(14) 0.133(6) Uani 0.50 1 d PGD A 1 C9S C 1.0408(4) 0.2294(5) 0.77932(17) 0.079(2) Uani 0.50 1 d PGD A 1 C10S C 1.0288(4) 0.3687(3) 0.7272(2) 0.179(8) Uani 0.50 1 d PGD A 1 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 Ca1 0.0315(2) 0.0257(2) 0.0279(2) 0.00174(19) 0.0090(2) 0.0125(2) Ca1B 0.0270(2) 0.0237(2) 0.0260(2) 0.00677(18) 0.00800(18) 0.01113(19) O1 0.0419(10) 0.0421(10) 0.0321(9) 0.0035(8) 0.0013(8) 0.0220(8) O1B 0.0512(10) 0.0305(9) 0.0295(9) 0.0025(7) 0.0120(8) 0.0201(8) N1 0.0274(9) 0.0325(11) 0.0262(10) 0.0065(8) 0.0097(8) 0.0133(8) N2 0.0273(9) 0.0271(10) 0.0255(9) 0.0050(8) 0.0077(8) 0.0126(8) N1B 0.0244(9) 0.0255(10) 0.0307(10) 0.0039(8) 0.0091(8) 0.0083(8) N2B 0.0252(9) 0.0275(10) 0.0236(9) 0.0028(8) 0.0075(8) 0.0110(8) C1 0.0259(11) 0.0353(13) 0.0296(12) 0.0073(10) 0.0055(10) 0.0103(10) C2 0.0272(12) 0.0387(14) 0.0240(12) 0.0012(10) 0.0023(10) 0.0084(10) C3 0.0326(12) 0.0295(12) 0.0221(11) 0.0046(9) 0.0054(10) 0.0129(10) C4 0.0336(14) 0.0583(18) 0.0360(14) 0.0011(13) 0.0078(12) -0.0023(13) C5 0.0408(14) 0.0492(16) 0.0262(12) -0.0029(11) 0.0089(11) 0.0115(12) C6 0.0257(11) 0.0316(13) 0.0290(12) 0.0054(10) 0.0101(10) 0.0092(10) C7 0.0361(13) 0.0328(13) 0.0291(12) 0.0058(10) 0.0112(10) 0.0135(11) C8 0.0454(14) 0.0384(14) 0.0293(13) 0.0082(11) 0.0128(11) 0.0150(12) C9 0.0448(15) 0.0477(16) 0.0354(14) 0.0044(12) 0.0210(12) 0.0149(13) C10 0.0419(14) 0.0506(16) 0.0485(16) 0.0044(13) 0.0235(13) 0.0229(13) C11 0.0315(12) 0.0421(14) 0.0407(14) 0.0095(11) 0.0161(11) 0.0180(11) C12 0.0641(18) 0.0535(17) 0.0346(14) 0.0175(12) 0.0209(13) 0.0394(15) C13 0.0527(17) 0.0586(19) 0.077(2) 0.0281(16) 0.0278(16) 0.0336(15) C14 0.078(2) 0.0497(19) 0.072(2) 0.0051(16) 0.0141(18) 0.0369(17) C15 0.0516(17) 0.067(2) 0.0657(19) 0.0306(16) 0.0310(15) 0.0414(16) C16 0.065(2) 0.142(4) 0.147(4) 0.079(4) 0.002(3) 0.054(3) C17 0.150(4) 0.087(3) 0.116(3) 0.051(2) 0.088(3) 0.092(3) C18 0.0273(11) 0.0317(12) 0.0234(11) 0.0003(9) 0.0063(9) 0.0119(10) C19 0.0376(13) 0.0440(15) 0.0328(13) 0.0016(11) 0.0066(11) 0.0220(12) C20 0.0391(15) 0.068(2) 0.0526(17) 0.0070(15) 0.0118(13) 0.0336(15) C21 0.0331(14) 0.077(2) 0.0572(18) 0.0110(16) 0.0187(13) 0.0244(15) C22 0.0389(14) 0.0514(17) 0.0494(16) 0.0101(13) 0.0192(13) 0.0134(13) C23 0.0320(12) 0.0377(14) 0.0309(12) 0.0040(10) 0.0119(10) 0.0126(11) C24 0.0525(16) 0.0495(17) 0.0574(17) 0.0153(14) 0.0169(14) 0.0343(14) C25 0.112(3) 0.072(2) 0.0513(19) 0.0209(16) 0.0359(19) 0.062(2) C26 0.111(3) 0.059(2) 0.064(2) 0.0047(17) 0.012(2) 0.053(2) C27 0.0437(14) 0.0366(14) 0.0484(15) 0.0162(12) 0.0244(12) 0.0189(12) C28 0.079(2) 0.064(2) 0.0495(18) 0.0127(15) 0.0126(16) 0.0447(18) C29 0.079(2) 0.0451(17) 0.062(2) 0.0055(15) 0.0279(17) 0.0271(16) C30 0.0461(15) 0.0305(14) 0.0453(16) -0.0037(11) 0.0070(13) 0.0183(12) C31 0.0480(15) 0.0309(14) 0.0436(15) 0.0051(11) 0.0097(13) 0.0214(12) C32 0.0555(16) 0.0389(15) 0.0447(15) 0.0101(12) 0.0077(13) 0.0273(13) C33 0.0618(19) 0.060(2) 0.0457(17) -0.0006(15) -0.0129(15) 0.0276(16) C1B 0.0323(12) 0.0245(12) 0.0309(12) 0.0030(10) 0.0108(10) 0.0068(10) C2B 0.0383(13) 0.0225(12) 0.0358(13) 0.0037(10) 0.0120(11) 0.0142(10) C3B 0.0348(12) 0.0298(13) 0.0252(11) 0.0059(9) 0.0096(10) 0.0184(10) C4B 0.0422(15) 0.0290(14) 0.0705(19) 0.0091(13) 0.0237(14) 0.0084(12) C5B 0.0430(14) 0.0388(14) 0.0501(16) 0.0102(12) 0.0120(12) 0.0257(12) C6B 0.0246(11) 0.0245(12) 0.0382(13) 0.0063(10) 0.0116(10) 0.0065(9) C7B 0.0307(12) 0.0357(14) 0.0395(14) 0.0039(11) 0.0140(11) 0.0116(11) C8B 0.0401(15) 0.0551(17) 0.0484(16) -0.0005(13) 0.0186(13) 0.0212(13) C9B 0.0340(14) 0.0608(19) 0.0632(19) 0.0050(15) 0.0175(14) 0.0252(14) C10B 0.0323(13) 0.0579(18) 0.0512(17) 0.0080(14) 0.0092(12) 0.0212(13) C11B 0.0276(12) 0.0399(14) 0.0415(14) 0.0062(11) 0.0104(11) 0.0115(11) C12B 0.0369(14) 0.0583(17) 0.0338(13) 0.0019(12) 0.0138(11) 0.0199(13) C13B 0.070(2) 0.072(2) 0.060(2) 0.0200(17) 0.0080(17) 0.0298(19) C14B 0.0539(18) 0.066(2) 0.0435(17) -0.0033(15) 0.0102(14) 0.0143(16) C15B 0.0300(13) 0.078(2) 0.0373(15) 0.0049(14) 0.0064(11) 0.0214(14) C16B 0.078(2) 0.079(2) 0.0491(19) -0.0088(17) 0.0104(17) 0.027(2) C17B 0.064(2) 0.100(3) 0.055(2) 0.030(2) 0.0161(17) 0.023(2) C18B 0.0240(11) 0.0333(13) 0.0252(11) 0.0065(9) 0.0055(9) 0.0133(10) C19B 0.0302(12) 0.0387(14) 0.0255(12) 0.0071(10) 0.0064(10) 0.0139(11) C20B 0.0343(14) 0.0606(18) 0.0267(13) 0.0004(12) 0.0034(11) 0.0091(13) C21B 0.0253(13) 0.080(2) 0.0372(15) -0.0003(15) 0.0032(12) 0.0010(14) C22B 0.0272(13) 0.080(2) 0.0367(15) 0.0053(14) 0.0129(12) 0.0098(14) C23B 0.0265(12) 0.0511(16) 0.0284(12) 0.0044(11) 0.0072(10) 0.0137(11) C24B 0.0348(13) 0.0422(14) 0.0254(12) 0.0041(10) 0.0084(10) 0.0144(11) C25B 0.0480(16) 0.0522(17) 0.0358(14) 0.0002(12) 0.0114(12) 0.0203(13) C26B 0.0711(19) 0.0530(18) 0.0347(14) 0.0151(13) 0.0252(14) 0.0264(15) C27B 0.0287(12) 0.0628(18) 0.0281(13) 0.0010(12) 0.0090(10) 0.0154(12) C28B 0.0563(17) 0.0590(19) 0.0440(16) 0.0030(14) 0.0177(14) 0.0262(15) C29B 0.0622(18) 0.087(2) 0.0326(14) 0.0085(14) 0.0134(13) 0.0510(18) C30B 0.0563(16) 0.0334(14) 0.0309(13) 0.0128(11) 0.0124(12) 0.0214(12) C31B 0.0509(15) 0.0357(14) 0.0263(12) 0.0102(11) 0.0122(11) 0.0196(12) C32B 0.0551(16) 0.0370(14) 0.0294(13) 0.0047(11) 0.0129(12) 0.0195(13) C33B 0.106(3) 0.0401(17) 0.0510(18) 0.0028(14) 0.0242(18) 0.0395(18) C1S 0.071(6) 0.237(15) 0.061(5) -0.008(7) 0.025(4) 0.099(8) C2S 0.151(5) 0.069(3) 0.194(6) -0.013(4) 0.145(5) 0.015(3) C3S 0.165(11) 0.074(6) 0.113(8) 0.046(6) 0.089(8) 0.076(7) C4S 0.128(5) 0.351(13) 0.122(5) -0.106(7) 0.017(5) 0.089(7) C5S 0.098(6) 0.053(4) 0.090(6) -0.006(4) 0.039(5) 0.036(4) C6S 0.128(5) 0.109(4) 0.148(6) 0.008(4) 0.080(5) 0.059(4) C7S 0.090(4) 0.179(7) 0.124(5) 0.018(4) 0.049(3) 0.063(4) C8S 0.088(7) 0.280(19) 0.051(5) -0.022(8) 0.010(5) 0.109(11) C9S 0.095(6) 0.098(6) 0.087(6) 0.031(5) 0.061(5) 0.063(5) C10S 0.177(16) 0.140(12) 0.26(2) 0.031(14) 0.164(16) 0.051(12) _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 Ca1 N2 2.3320(18) . ? Ca1 N1 2.3425(19) . ? Ca1 C30 2.498(3) 2_666 ? Ca1 O1 2.5068(16) . ? Ca1 C30 2.666(2) . ? Ca1 C31 2.721(2) . ? Ca1B N2B 2.3387(18) . ? Ca1B N1B 2.3428(18) . ? Ca1B O1B 2.4694(16) . ? Ca1B C30B 2.490(3) 2_657 ? Ca1B C30B 2.696(2) . ? Ca1B C31B 2.742(2) . ? O1 C33 1.428(3) . ? O1 C32 1.434(3) . ? O1B C33B 1.429(3) . ? O1B C32B 1.433(3) . ? N1 C1 1.322(3) . ? N1 C6 1.444(3) . ? N2 C3 1.327(3) . ? N2 C18 1.433(3) . ? N1B C1B 1.324(3) . ? N1B C6B 1.435(3) . ? N2B C3B 1.322(3) . ? N2B C18B 1.433(3) . ? C1 C2 1.416(3) . ? C1 C4 1.515(3) . ? C2 C3 1.409(3) . ? C3 C5 1.514(3) . ? C6 C7 1.400(3) . ? C6 C11 1.409(3) . ? C7 C8 1.392(3) . ? C7 C12 1.518(3) . ? C8 C9 1.375(4) . ? C9 C10 1.369(4) . ? C10 C11 1.394(3) . ? C11 C15 1.518(4) . ? C12 C13 1.531(4) . ? C12 C14 1.540(4) . ? C15 C16 1.514(5) . ? C15 C17 1.536(5) . ? C18 C23 1.404(3) . ? C18 C19 1.408(3) . ? C19 C20 1.392(4) . ? C19 C24 1.517(4) . ? C20 C21 1.379(4) . ? C21 C22 1.371(4) . ? C22 C23 1.397(3) . ? C23 C27 1.515(3) . ? C24 C25 1.529(4) . ? C24 C26 1.530(4) . ? C27 C28 1.525(4) . ? C27 C29 1.526(4) . ? C30 C31 1.218(4) . ? C30 Ca1 2.498(3) 2_666 ? C31 C32 1.468(4) . ? C1B C2B 1.409(3) . ? C1B C4B 1.519(3) . ? C2B C3B 1.409(3) . ? C3B C5B 1.520(3) . ? C6B C11B 1.405(3) . ? C6B C7B 1.406(3) . ? C7B C8B 1.394(3) . ? C7B C12B 1.519(4) . ? C8B C9B 1.377(4) . ? C9B C10B 1.377(4) . ? C10B C11B 1.389(3) . ? C11B C15B 1.515(4) . ? C12B C14B 1.523(4) . ? C12B C13B 1.528(4) . ? C15B C16B 1.526(4) . ? C15B C17B 1.530(5) . ? C18B C23B 1.400(3) . ? C18B C19B 1.412(3) . ? C19B C20B 1.390(3) . ? C19B C24B 1.521(3) . ? C20B C21B 1.378(4) . ? C21B C22B 1.377(4) . ? C22B C23B 1.391(3) . ? C23B C27B 1.522(3) . ? C24B C26B 1.519(4) . ? C24B C25B 1.532(3) . ? C27B C29B 1.525(4) . ? C27B C28B 1.527(4) . ? C30B C31B 1.212(3) . ? C30B Ca1B 2.490(3) 2_657 ? C31B C32B 1.471(3) . ? C1S C10S 1.2801 . ? C1S C8S 1.3721 . ? C1S C7S 1.3898 . ? C1S C2S 1.3900 . ? C1S C6S 1.3900 . ? C1S C9S 1.4907 . ? C2S C8S 1.3710 . ? C2S C3S 1.3900 . ? C2S C9S 1.6195 . ? C3S C8S 1.3891 . ? C3S C4S 1.3900 . ? C4S C5S 1.3900 . ? C4S C8S 1.4080 . ? C5S C6S 1.3900 . ? C5S C8S 1.4091 . ? C6S C10S 1.2385 . ? C6S C8S 1.3913 . ? C7S C9S 1.3259 . ? C7S C10S 1.3784 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ca1 N1 83.06(6) . . ? N2 Ca1 C30 101.46(7) . 2_666 ? N1 Ca1 C30 110.69(8) . 2_666 ? N2 Ca1 O1 90.07(6) . . ? N1 Ca1 O1 89.65(6) . . ? C30 Ca1 O1 157.53(7) 2_666 . ? N2 Ca1 C30 146.18(8) . . ? N1 Ca1 C30 127.84(8) . . ? C30 Ca1 C30 81.61(9) 2_666 . ? O1 Ca1 C30 78.21(7) . . ? N2 Ca1 C31 132.81(7) . . ? N1 Ca1 C31 118.58(7) . . ? C30 Ca1 C31 107.48(8) 2_666 . ? O1 Ca1 C31 52.14(7) . . ? C30 Ca1 C31 26.10(8) . . ? N2B Ca1B N1B 80.22(6) . . ? N2B Ca1B O1B 93.32(6) . . ? N1B Ca1B O1B 90.15(6) . . ? N2B Ca1B C30B 100.41(7) . 2_657 ? N1B Ca1B C30B 109.11(7) . 2_657 ? O1B Ca1B C30B 157.89(7) . 2_657 ? N2B Ca1B C30B 136.48(7) . . ? N1B Ca1B C30B 141.18(8) . . ? O1B Ca1B C30B 77.69(7) . . ? C30B Ca1B C30B 80.43(8) 2_657 . ? N2B Ca1B C31B 128.39(7) . . ? N1B Ca1B C31B 128.30(7) . . ? O1B Ca1B C31B 51.98(6) . . ? C30B Ca1B C31B 106.16(8) 2_657 . ? C30B Ca1B C31B 25.73(7) . . ? C33 O1 C32 113.2(2) . . ? C33 O1 Ca1 139.94(17) . . ? C32 O1 Ca1 106.59(13) . . ? C33B O1B C32B 113.37(19) . . ? C33B O1B Ca1B 138.14(16) . . ? C32B O1B Ca1B 108.42(13) . . ? C1 N1 C6 119.32(18) . . ? C1 N1 Ca1 122.83(14) . . ? C6 N1 Ca1 117.76(13) . . ? C3 N2 C18 119.79(18) . . ? C3 N2 Ca1 122.15(14) . . ? C18 N2 Ca1 117.59(13) . . ? C1B N1B C6B 120.50(18) . . ? C1B N1B Ca1B 123.84(14) . . ? C6B N1B Ca1B 115.45(13) . . ? C3B N2B C18B 119.45(18) . . ? C3B N2B Ca1B 123.34(14) . . ? C18B N2B Ca1B 116.04(13) . . ? N1 C1 C2 124.9(2) . . ? N1 C1 C4 120.3(2) . . ? C2 C1 C4 114.8(2) . . ? C3 C2 C1 131.7(2) . . ? N2 C3 C2 124.9(2) . . ? N2 C3 C5 119.6(2) . . ? C2 C3 C5 115.6(2) . . ? C7 C6 C11 120.2(2) . . ? C7 C6 N1 119.97(19) . . ? C11 C6 N1 119.7(2) . . ? C8 C7 C6 118.7(2) . . ? C8 C7 C12 118.3(2) . . ? C6 C7 C12 123.0(2) . . ? C9 C8 C7 121.6(2) . . ? C10 C9 C8 119.3(2) . . ? C9 C10 C11 121.8(2) . . ? C10 C11 C6 118.3(2) . . ? C10 C11 C15 119.3(2) . . ? C6 C11 C15 122.3(2) . . ? C7 C12 C13 110.5(2) . . ? C7 C12 C14 111.7(2) . . ? C13 C12 C14 109.9(2) . . ? C16 C15 C11 110.9(3) . . ? C16 C15 C17 111.2(3) . . ? C11 C15 C17 112.4(3) . . ? C23 C18 C19 120.1(2) . . ? C23 C18 N2 119.9(2) . . ? C19 C18 N2 119.7(2) . . ? C20 C19 C18 118.7(2) . . ? C20 C19 C24 119.2(2) . . ? C18 C19 C24 122.1(2) . . ? C21 C20 C19 121.5(3) . . ? C22 C21 C20 119.5(3) . . ? C21 C22 C23 121.5(3) . . ? C22 C23 C18 118.7(2) . . ? C22 C23 C27 119.1(2) . . ? C18 C23 C27 122.2(2) . . ? C19 C24 C25 110.4(2) . . ? C19 C24 C26 112.2(3) . . ? C25 C24 C26 109.8(2) . . ? C23 C27 C28 112.0(2) . . ? C23 C27 C29 111.9(2) . . ? C28 C27 C29 109.8(2) . . ? C31 C30 Ca1 172.1(2) . 2_666 ? C31 C30 Ca1 79.46(16) . . ? Ca1 C30 Ca1 98.39(9) 2_666 . ? C30 C31 C32 170.4(3) . . ? C30 C31 Ca1 74.44(16) . . ? C32 C31 Ca1 96.02(15) . . ? O1 C32 C31 105.19(19) . . ? N1B C1B C2B 124.3(2) . . ? N1B C1B C4B 120.5(2) . . ? C2B C1B C4B 115.2(2) . . ? C3B C2B C1B 130.1(2) . . ? N2B C3B C2B 124.6(2) . . ? N2B C3B C5B 120.3(2) . . ? C2B C3B C5B 115.1(2) . . ? C11B C6B C7B 120.4(2) . . ? C11B C6B N1B 120.6(2) . . ? C7B C6B N1B 118.7(2) . . ? C8B C7B C6B 118.5(2) . . ? C8B C7B C12B 119.5(2) . . ? C6B C7B C12B 122.0(2) . . ? C9B C8B C7B 121.4(2) . . ? C8B C9B C10B 119.6(2) . . ? C9B C10B C11B 121.5(3) . . ? C10B C11B C6B 118.7(2) . . ? C10B C11B C15B 119.2(2) . . ? C6B C11B C15B 122.1(2) . . ? C7B C12B C14B 111.4(2) . . ? C7B C12B C13B 111.9(2) . . ? C14B C12B C13B 109.9(2) . . ? C11B C15B C16B 111.8(2) . . ? C11B C15B C17B 112.3(3) . . ? C16B C15B C17B 109.3(3) . . ? C23B C18B C19B 120.2(2) . . ? C23B C18B N2B 120.79(19) . . ? C19B C18B N2B 118.79(19) . . ? C20B C19B C18B 118.2(2) . . ? C20B C19B C24B 121.2(2) . . ? C18B C19B C24B 120.6(2) . . ? C21B C20B C19B 121.8(2) . . ? C22B C21B C20B 119.3(2) . . ? C21B C22B C23B 121.4(2) . . ? C22B C23B C18B 118.8(2) . . ? C22B C23B C27B 118.9(2) . . ? C18B C23B C27B 122.2(2) . . ? C26B C24B C19B 112.4(2) . . ? C26B C24B C25B 110.1(2) . . ? C19B C24B C25B 112.9(2) . . ? C23B C27B C29B 109.9(2) . . ? C23B C27B C28B 113.4(2) . . ? C29B C27B C28B 110.1(2) . . ? C31B C30B Ca1B 178.4(2) . 2_657 ? C31B C30B Ca1B 79.25(16) . . ? Ca1B C30B Ca1B 99.57(8) 2_657 . ? C30B C31B C32B 170.0(2) . . ? C30B C31B Ca1B 75.02(15) . . ? C32B C31B Ca1B 95.01(14) . . ? O1B C32B C31B 104.54(18) . . ? C10S C1S C8S 115.5 . . ? C10S C1S C7S 62.0 . . ? C8S C1S C7S 177.1 . . ? C10S C1S C2S 174.7 . . ? C8S C1S C2S 59.5 . . ? C7S C1S C2S 122.9 . . ? C10S C1S C6S 55.1 . . ? C8S C1S C6S 60.5 . . ? C7S C1S C6S 117.1 . . ? C2S C1S C6S 120.0 . . ? C10S C1S C9S 116.7 . . ? C8S C1S C9S 127.8 . . ? C7S C1S C9S 54.7 . . ? C2S C1S C9S 68.3 . . ? C6S C1S C9S 171.6 . . ? C8S C2S C3S 60.4 . . ? C8S C2S C1S 59.6 . . ? C3S C2S C1S 120.0 . . ? C8S C2S C9S 118.4 . . ? C3S C2S C9S 178.1 . . ? C1S C2S C9S 58.8 . . ? C8S C3S C2S 59.1 . . ? C8S C3S C4S 60.9 . . ? C2S C3S C4S 120.0 . . ? C3S C4S C5S 120.0 . . ? C3S C4S C8S 59.5 . . ? C5S C4S C8S 60.5 . . ? C6S C5S C4S 120.0 . . ? C6S C5S C8S 59.6 . . ? C4S C5S C8S 60.4 . . ? C10S C6S C5S 177.1 . . ? C10S C6S C1S 57.9 . . ? C5S C6S C1S 120.0 . . ? C10S C6S C8S 117.0 . . ? C5S C6S C8S 60.9 . . ? C1S C6S C8S 59.1 . . ? C9S C7S C10S 121.6 . . ? C9S C7S C1S 66.5 . . ? C10S C7S C1S 55.1 . . ? C2S C8S C1S 60.9 . . ? C2S C8S C3S 60.5 . . ? C1S C8S C3S 121.4 . . ? C2S C8S C6S 121.3 . . ? C1S C8S C6S 60.4 . . ? C3S C8S C6S 178.1 . . ? C2S C8S C4S 120.1 . . ? C1S C8S C4S 178.9 . . ? C3S C8S C4S 59.6 . . ? C6S C8S C4S 118.6 . . ? C2S C8S C5S 179.0 . . ? C1S C8S C5S 119.9 . . ? C3S C8S C5S 118.7 . . ? C6S C8S C5S 59.5 . . ? C4S C8S C5S 59.1 . . ? C7S C9S C1S 58.8 . . ? C7S C9S C2S 111.6 . . ? C1S C9S C2S 52.9 . . ? C6S C10S C1S 67.0 . . ? C6S C10S C7S 129.9 . . ? C1S C10S C7S 62.9 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.06 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.661 _refine_diff_density_min -0.371 _refine_diff_density_rms 0.047 data_h08msh17 _database_code_depnum_ccdc_archive 'CCDC 706558' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58.40 H89.60 Ca N6 O2' _chemical_formula_weight 947.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c 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' '-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 44.3151(3) _cell_length_b 12.43580(10) _cell_length_c 24.4870(2) _cell_angle_alpha 90.00 _cell_angle_beta 121.19 _cell_angle_gamma 90.00 _cell_volume 11544.16(15) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 69907 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.091 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4144 _exptl_absorpt_coefficient_mu 0.152 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.81 _exptl_absorpt_correction_T_max 0.99 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 100189 _diffrn_reflns_av_R_equivalents 0.0867 _diffrn_reflns_av_sigmaI/netI 0.0430 _diffrn_reflns_limit_h_min -57 _diffrn_reflns_limit_h_max 57 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.68 _diffrn_reflns_theta_max 27.48 _reflns_number_total 13169 _reflns_number_gt 9551 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (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^)+(0.0758P)^2^+8.1209P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13169 _refine_ls_number_parameters 673 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0765 _refine_ls_R_factor_gt 0.0499 _refine_ls_wR_factor_ref 0.1533 _refine_ls_wR_factor_gt 0.1348 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.067 _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 Ca1 Ca 0.140879(9) 0.68554(3) 0.230285(16) 0.02658(10) Uani 1 1 d . . . O1 O 0.16995(3) 0.85313(10) 0.26359(6) 0.0332(3) Uani 1 1 d . J . O2 O 0.12502(4) 0.50523(10) 0.19326(7) 0.0424(3) Uani 1 1 d . D . N1 N 0.15181(3) 0.65393(11) 0.33905(6) 0.0267(3) Uani 1 1 d . . . N2 N 0.18271(4) 0.60823(11) 0.36431(6) 0.0261(3) Uani 1 1 d . . . N3 N 0.19335(4) 0.60346(11) 0.32269(7) 0.0276(3) Uani 1 1 d . . . N4 N 0.08258(4) 0.76192(12) 0.16676(7) 0.0284(3) Uani 1 1 d . . . N5 N 0.08334(4) 0.78648(12) 0.11517(7) 0.0298(3) Uani 1 1 d . . . N6 N 0.11292(4) 0.75677(12) 0.11926(7) 0.0280(3) Uani 1 1 d . . . C1 C 0.11562(5) 0.79304(15) 0.06672(8) 0.0319(4) Uani 1 1 d . . . C2 C 0.12909(5) 0.71897(17) 0.04074(9) 0.0370(4) Uani 1 1 d . . . C3 C 0.13388(6) 0.7523(2) -0.00850(10) 0.0495(5) Uani 1 1 d . . . H3 H 0.1431 0.7032 -0.0259 0.059 Uiso 1 1 calc R . . C4 C 0.12544(7) 0.8555(2) -0.03254(11) 0.0564(6) Uani 1 1 d . . . H4 H 0.1288 0.8769 -0.0662 0.068 Uiso 1 1 calc R . . C5 C 0.11219(6) 0.9266(2) -0.00782(10) 0.0509(5) Uani 1 1 d . . . H5 H 0.1061 0.9969 -0.0253 0.061 Uiso 1 1 calc R . . C6 C 0.10729(5) 0.89910(17) 0.04267(9) 0.0387(4) Uani 1 1 d . . . C7 C 0.09355(6) 0.98443(17) 0.06855(11) 0.0442(5) Uani 1 1 d . . . H7 H 0.0985 0.9591 0.1112 0.053 Uiso 1 1 calc R . . C8 C 0.11217(8) 1.09324(18) 0.07887(13) 0.0601(6) Uani 1 1 d . . . H8A H 0.1024 1.1453 0.0956 0.090 Uiso 1 1 calc R . . H8B H 0.1085 1.1193 0.0381 0.090 Uiso 1 1 calc R . . H8C H 0.1375 1.0846 0.1094 0.090 Uiso 1 1 calc R . . C9 C 0.05357(7) 0.9989(2) 0.02610(14) 0.0661(7) Uani 1 1 d . . . H9A H 0.0457 1.0543 0.0444 0.099 Uiso 1 1 calc R . . H9B H 0.0418 0.9308 0.0235 0.099 Uiso 1 1 calc R . . H9C H 0.0477 1.0209 -0.0168 0.099 Uiso 1 1 calc R . . C10 C 0.13442(5) 0.60209(17) 0.06128(10) 0.0422(5) Uani 1 1 d . . . H10 H 0.1415 0.5999 0.1072 0.051 Uiso 1 1 calc R . . C11 C 0.09905(7) 0.5432(2) 0.02279(12) 0.0570(6) Uani 1 1 d . . . H11A H 0.1021 0.4676 0.0359 0.086 Uiso 1 1 calc R . . H11B H 0.0908 0.5475 -0.0228 0.086 Uiso 1 1 calc R . . H11C H 0.0816 0.5769 0.0306 0.086 Uiso 1 1 calc R . . C12 C 0.16298(7) 0.5440(2) 0.05523(13) 0.0605(6) Uani 1 1 d . . . H12A H 0.1648 0.4693 0.0694 0.091 Uiso 1 1 calc R . . H12B H 0.1857 0.5803 0.0819 0.091 Uiso 1 1 calc R . . H12C H 0.1568 0.5452 0.0106 0.091 Uiso 1 1 calc R . . C13 C 0.05048(4) 0.79615(15) 0.16192(8) 0.0309(4) Uani 1 1 d . . . C14 C 0.01760(5) 0.75192(16) 0.11675(9) 0.0353(4) Uani 1 1 d . . . C15 C -0.01234(5) 0.78755(19) 0.11605(10) 0.0479(5) Uani 1 1 d . . . H15 H -0.0347 0.7593 0.0851 0.058 Uiso 1 1 calc R . . C16 C -0.01040(6) 0.8625(2) 0.15892(12) 0.0591(7) Uani 1 1 d . . . H16 H -0.0312 0.8851 0.1578 0.071 Uiso 1 1 calc R . . C17 C 0.02189(6) 0.9048(2) 0.20358(11) 0.0541(6) Uani 1 1 d . . . H17 H 0.0231 0.9564 0.2333 0.065 Uiso 1 1 calc R . . C18 C 0.05266(5) 0.87360(17) 0.20591(10) 0.0394(4) Uani 1 1 d . . . C19 C 0.01309(5) 0.66751(16) 0.06831(9) 0.0386(4) Uani 1 1 d . . . H19 H 0.0371 0.6441 0.0787 0.046 Uiso 1 1 calc R . . C20 C -0.00668(7) 0.5686(2) 0.07056(13) 0.0587(6) Uani 1 1 d . . . H20A H -0.0091 0.5163 0.0386 0.088 Uiso 1 1 calc R . . H20B H -0.0301 0.5900 0.0615 0.088 Uiso 1 1 calc R . . H20C H 0.0065 0.5360 0.1131 0.088 Uiso 1 1 calc R . . C21 C -0.00601(8) 0.7153(2) 0.00102(11) 0.0640(7) Uani 1 1 d . . . H21A H -0.0087 0.6599 -0.0297 0.096 Uiso 1 1 calc R . . H21B H 0.0078 0.7753 -0.0007 0.096 Uiso 1 1 calc R . . H21C H -0.0293 0.7412 -0.0096 0.096 Uiso 1 1 calc R . . C22 C 0.08710(5) 0.92960(19) 0.25250(11) 0.0491(5) Uani 1 1 d . . . H22 H 0.1068 0.8866 0.2547 0.059 Uiso 1 1 calc R . . C23 C 0.09365(6) 0.93714(19) 0.31992(11) 0.0515(5) Uani 1 1 d . . . H23A H 0.0932 0.8649 0.3354 0.077 Uiso 1 1 calc R . . H23B H 0.0752 0.9814 0.3195 0.077 Uiso 1 1 calc R . . H23C H 0.1168 0.9700 0.3482 0.077 Uiso 1 1 calc R . . C24 C 0.08803(9) 1.0412(3) 0.22750(15) 0.0785(9) Uani 1 1 d . . . H24A H 0.1103 1.0768 0.2578 0.118 Uiso 1 1 calc R . . H24B H 0.0682 1.0839 0.2227 0.118 Uiso 1 1 calc R . . H24C H 0.0862 1.0344 0.1860 0.118 Uiso 1 1 calc R . . C25 C 0.22554(4) 0.54727(14) 0.34520(8) 0.0279(4) Uani 1 1 d . . . C26 C 0.24957(4) 0.59232(15) 0.32957(8) 0.0321(4) Uani 1 1 d . . . C27 C 0.28154(5) 0.54055(18) 0.35039(9) 0.0400(4) Uani 1 1 d . . . H27 H 0.2979 0.5710 0.3407 0.048 Uiso 1 1 calc R . . C28 C 0.29011(5) 0.44593(18) 0.38484(9) 0.0442(5) Uani 1 1 d . . . H28 H 0.3123 0.4127 0.3996 0.053 Uiso 1 1 calc R . . C29 C 0.26619(5) 0.40034(17) 0.39759(9) 0.0403(5) Uani 1 1 d . . . H29 H 0.2720 0.3345 0.4206 0.048 Uiso 1 1 calc R . . C30 C 0.23345(5) 0.44788(15) 0.37775(8) 0.0330(4) Uani 1 1 d . . . C31 C 0.23978(5) 0.69308(16) 0.28868(9) 0.0354(4) Uani 1 1 d . . . H31 H 0.2255 0.7395 0.3003 0.043 Uiso 1 1 calc R . . C32 C 0.27078(6) 0.76081(18) 0.29750(11) 0.0466(5) Uani 1 1 d . . . H32A H 0.2618 0.8236 0.2693 0.070 Uiso 1 1 calc R . . H32B H 0.2855 0.7175 0.2869 0.070 Uiso 1 1 calc R . . H32C H 0.2849 0.7848 0.3420 0.070 Uiso 1 1 calc R . . C33 C 0.21602(6) 0.66282(19) 0.21823(10) 0.0462(5) Uani 1 1 d . . . H33A H 0.2096 0.7279 0.1919 0.069 Uiso 1 1 calc R . . H33B H 0.1946 0.6279 0.2118 0.069 Uiso 1 1 calc R . . H33C H 0.2286 0.6133 0.2058 0.069 Uiso 1 1 calc R . . C34 C 0.20773(5) 0.38808(15) 0.39046(10) 0.0405(4) Uani 1 1 d . . . H34 H 0.1840 0.4221 0.3635 0.049 Uiso 1 1 calc R . . C35 C 0.20427(7) 0.26891(18) 0.37124(13) 0.0594(6) Uani 1 1 d . . . H35A H 0.1976 0.2635 0.3264 0.089 Uiso 1 1 calc R . . H35B H 0.1861 0.2348 0.3769 0.089 Uiso 1 1 calc R . . H35C H 0.2269 0.2326 0.3982 0.089 Uiso 1 1 calc R . . C36 C 0.21765(7) 0.3972(2) 0.45984(12) 0.0560(6) Uani 1 1 d . . . H36A H 0.2003 0.3585 0.4658 0.084 Uiso 1 1 calc R . . H36B H 0.2180 0.4732 0.4708 0.084 Uiso 1 1 calc R . . H36C H 0.2411 0.3660 0.4876 0.084 Uiso 1 1 calc R . . C37 C 0.13902(4) 0.66796(13) 0.38160(8) 0.0270(3) Uani 1 1 d . . . C38 C 0.15776(4) 0.72354(14) 0.44000(8) 0.0294(4) Uani 1 1 d . . . C39 C 0.14110(5) 0.74172(16) 0.47446(9) 0.0363(4) Uani 1 1 d . . . H39 H 0.1534 0.7791 0.5140 0.044 Uiso 1 1 calc R . . C40 C 0.10718(5) 0.70670(18) 0.45247(10) 0.0419(5) Uani 1 1 d . . . H40 H 0.0963 0.7204 0.4765 0.050 Uiso 1 1 calc R . . C41 C 0.08913(5) 0.65173(17) 0.39543(9) 0.0395(4) Uani 1 1 d . . . H41 H 0.0658 0.6274 0.3805 0.047 Uiso 1 1 calc R . . C42 C 0.10442(5) 0.63134(15) 0.35947(8) 0.0318(4) Uani 1 1 d . . . C43 C 0.08509(5) 0.56240(17) 0.29979(10) 0.0408(5) Uani 1 1 d . . . H43 H 0.0924 0.5874 0.2695 0.049 Uiso 1 1 calc R . . C44 C 0.09683(7) 0.4465(2) 0.31671(13) 0.0612(6) Uani 1 1 d . . . H44A H 0.0844 0.4019 0.2782 0.092 Uiso 1 1 calc R . . H44B H 0.0913 0.4210 0.3484 0.092 Uiso 1 1 calc R . . H44C H 0.1223 0.4416 0.3344 0.092 Uiso 1 1 calc R . . C45 C 0.04501(6) 0.5710(2) 0.26551(11) 0.0555(6) Uani 1 1 d . . . H45A H 0.0380 0.6465 0.2549 0.083 Uiso 1 1 calc R . . H45B H 0.0369 0.5439 0.2934 0.083 Uiso 1 1 calc R . . H45C H 0.0344 0.5283 0.2262 0.083 Uiso 1 1 calc R . . C46 C 0.19504(5) 0.76618(16) 0.46860(8) 0.0355(4) Uani 1 1 d . . . H46 H 0.2028 0.7521 0.4374 0.043 Uiso 1 1 calc R . . C47 C 0.19696(6) 0.88787(19) 0.48028(11) 0.0501(5) Uani 1 1 d . . . H47A H 0.2213 0.9124 0.4986 0.075 Uiso 1 1 calc R . . H47B H 0.1890 0.9040 0.5100 0.075 Uiso 1 1 calc R . . H47C H 0.1817 0.9250 0.4397 0.075 Uiso 1 1 calc R . . C48 C 0.22029(5) 0.7069(2) 0.53045(9) 0.0508(6) Uani 1 1 d . . . H48A H 0.2442 0.7351 0.5480 0.076 Uiso 1 1 calc R . . H48B H 0.2200 0.6300 0.5216 0.076 Uiso 1 1 calc R . . H48C H 0.2128 0.7178 0.5614 0.076 Uiso 1 1 calc R . . C49 C 0.08907(6) 0.46475(19) 0.15626(11) 0.0481(5) Uani 1 1 d . . . H49A H 0.0758 0.4835 0.1773 0.058 Uiso 0.60 1 calc PR A 1 H49B H 0.0767 0.4963 0.1129 0.058 Uiso 0.60 1 calc PR A 1 H49C H 0.0822(17) 0.496(5) 0.116(3) 0.058 Uiso 0.40 1 d P B 2 H49D H 0.0751(17) 0.500(5) 0.171(3) 0.058 Uiso 0.40 1 d P C 2 C50 C 0.09163(18) 0.3512(9) 0.1530(5) 0.073(3) Uani 0.60 1 d PD D 1 H50A H 0.0900 0.3304 0.1125 0.088 Uiso 0.60 1 calc PR D 1 H50B H 0.0724 0.3153 0.1552 0.088 Uiso 0.60 1 calc PR D 1 C51 C 0.12771(13) 0.3188(4) 0.2105(2) 0.0451(11) Uani 0.60 1 d PD D 1 H51A H 0.1360 0.2485 0.2043 0.054 Uiso 0.60 1 calc PR D 1 H51B H 0.1279 0.3189 0.2511 0.054 Uiso 0.60 1 calc PR D 1 C52 C 0.14894(7) 0.41688(18) 0.20521(12) 0.0544(6) Uani 1 1 d . . . H52A H 0.1718 0.4274 0.2454 0.065 Uiso 0.60 1 calc PR D 1 H52B H 0.1531 0.4071 0.1695 0.065 Uiso 0.60 1 calc PR D 1 H52C H 0.1347(18) 0.346(6) 0.155(3) 0.065 Uiso 0.40 1 d P E 2 H52D H 0.1698(19) 0.436(5) 0.243(3) 0.065 Uiso 0.40 1 d P F 2 C53 C 0.18657(6) 0.88467(17) 0.33029(9) 0.0408(4) Uani 1 1 d . . . H53A H 0.2000 0.8241 0.3589 0.049 Uiso 0.53 1 calc PR G 1 H53B H 0.1688 0.9094 0.3403 0.049 Uiso 0.53 1 calc PR G 1 H53C H 0.2076(14) 0.831(4) 0.355(2) 0.049 Uiso 0.47 1 d P H 2 H53D H 0.1682(13) 0.860(4) 0.347(2) 0.049 Uiso 0.47 1 d P I 2 C54 C 0.21195(16) 0.9791(5) 0.3374(3) 0.0539(13) Uani 0.53 1 d PD J 1 H54A H 0.2157 1.0306 0.3712 0.065 Uiso 0.53 1 calc PR J 1 H54B H 0.2350 0.9525 0.3456 0.065 Uiso 0.53 1 calc PR J 1 C55 C 0.1894(3) 1.0274(11) 0.2700(4) 0.081(4) Uani 0.53 1 d PD J 1 H55A H 0.1697 1.0708 0.2666 0.097 Uiso 0.53 1 calc PR J 1 H55B H 0.2038 1.0732 0.2592 0.097 Uiso 0.53 1 calc PR J 1 C56 C 0.17637(7) 0.93539(19) 0.22941(11) 0.0553(6) Uani 1 1 d . . . H56A H 0.1939 0.9103 0.2188 0.066 Uiso 0.53 1 calc PR J 1 H56B H 0.1543 0.9533 0.1892 0.066 Uiso 0.53 1 calc PR J 1 H56C H 0.1477(16) 0.968(5) 0.205(3) 0.066 Uiso 0.47 1 d P K 2 H56D H 0.1697(15) 0.909(4) 0.184(3) 0.066 Uiso 0.47 1 d P L 2 C57 C 0.00301(13) 0.2431(6) 0.22621(19) 0.126(2) Uani 0.80 1 d PD . . H57A H 0.0200 0.1850 0.2335 0.152 Uiso 0.80 1 calc PR . . H57B H 0.0142 0.3122 0.2265 0.152 Uiso 0.80 1 calc PR . . C58 C -0.03013(13) 0.2274(6) 0.1605(2) 0.143(2) Uani 0.80 1 d PD . . H58A H -0.0390 0.1534 0.1582 0.172 Uiso 0.80 1 calc PR . . H58B H -0.0485 0.2775 0.1566 0.172 Uiso 0.80 1 calc PR . . C59 C -0.02545(18) 0.2447(8) 0.1037(3) 0.166(3) Uani 0.80 1 d PD . . H59A H -0.0479 0.2318 0.0640 0.248 Uiso 0.80 1 calc PR . . H59B H -0.0076 0.1947 0.1064 0.248 Uiso 0.80 1 calc PR . . H59C H -0.0178 0.3188 0.1041 0.248 Uiso 0.80 1 calc PR . . C50A C 0.0916(3) 0.3312(16) 0.1603(9) 0.075(4) Uani 0.40 1 d PD D 2 H50C H 0.0829 0.3010 0.1870 0.090 Uiso 0.40 1 calc PR D 2 H50D H 0.0791 0.2972 0.1176 0.090 Uiso 0.40 1 calc PR D 2 C51A C 0.1319(3) 0.3223(12) 0.1927(7) 0.098(5) Uani 0.40 1 d PDU D 2 H51C H 0.1412 0.2824 0.2333 0.117 Uiso 0.40 1 calc PR D 2 H51D H 0.1375 0.2795 0.1648 0.117 Uiso 0.40 1 calc PR D 2 C54A C 0.1943(2) 0.9997(5) 0.3342(3) 0.0574(16) Uani 0.47 1 d PD J 2 H54C H 0.2162 1.0180 0.3747 0.069 Uiso 0.47 1 calc PR J 2 H54D H 0.1746 1.0433 0.3302 0.069 Uiso 0.47 1 calc PR J 2 C55A C 0.1988(5) 1.0164(15) 0.2765(6) 0.116(7) Uani 0.47 1 d PD J 2 H55C H 0.1914 1.0897 0.2588 0.140 Uiso 0.47 1 calc PR J 2 H55D H 0.2238 1.0062 0.2891 0.140 Uiso 0.47 1 calc PR J 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 Ca1 0.02373(17) 0.02837(18) 0.02721(17) 0.00234(13) 0.01288(14) 0.00336(13) O1 0.0351(7) 0.0324(6) 0.0313(6) 0.0017(5) 0.0166(5) -0.0033(5) O2 0.0400(8) 0.0311(7) 0.0458(8) -0.0016(6) 0.0150(6) 0.0042(6) N1 0.0208(7) 0.0319(7) 0.0276(7) 0.0013(6) 0.0127(6) 0.0013(6) N2 0.0236(7) 0.0259(7) 0.0286(7) -0.0012(6) 0.0135(6) -0.0010(5) N3 0.0227(7) 0.0314(8) 0.0295(7) 0.0009(6) 0.0142(6) 0.0025(6) N4 0.0248(7) 0.0329(8) 0.0303(7) 0.0011(6) 0.0162(6) 0.0021(6) N5 0.0260(7) 0.0319(8) 0.0305(7) 0.0000(6) 0.0139(6) 0.0008(6) N6 0.0254(7) 0.0322(8) 0.0279(7) 0.0011(6) 0.0148(6) 0.0034(6) C1 0.0252(8) 0.0420(10) 0.0268(8) 0.0005(7) 0.0122(7) -0.0013(7) C2 0.0311(9) 0.0505(11) 0.0288(9) -0.0048(8) 0.0152(8) -0.0018(8) C3 0.0486(12) 0.0705(16) 0.0371(10) -0.0059(10) 0.0277(10) -0.0021(11) C4 0.0638(15) 0.0777(17) 0.0379(11) 0.0064(11) 0.0336(11) -0.0036(13) C5 0.0528(13) 0.0589(14) 0.0409(11) 0.0137(10) 0.0242(10) -0.0006(11) C6 0.0331(10) 0.0466(11) 0.0353(9) 0.0069(8) 0.0169(8) 0.0018(8) C7 0.0451(11) 0.0394(11) 0.0509(12) 0.0125(9) 0.0269(10) 0.0077(9) C8 0.0754(17) 0.0409(12) 0.0711(16) 0.0105(11) 0.0430(14) 0.0020(11) C9 0.0512(14) 0.0602(16) 0.0814(18) 0.0206(14) 0.0304(13) 0.0191(12) C10 0.0442(11) 0.0496(12) 0.0372(10) -0.0070(9) 0.0242(9) 0.0031(9) C11 0.0607(15) 0.0533(14) 0.0589(14) -0.0138(11) 0.0323(12) -0.0095(11) C12 0.0632(15) 0.0664(16) 0.0618(14) -0.0063(12) 0.0394(13) 0.0160(12) C13 0.0242(8) 0.0367(10) 0.0326(9) 0.0034(7) 0.0152(7) 0.0032(7) C14 0.0278(9) 0.0410(10) 0.0367(9) 0.0020(8) 0.0163(8) 0.0024(8) C15 0.0243(9) 0.0671(14) 0.0473(11) -0.0076(10) 0.0150(9) -0.0016(9) C16 0.0296(11) 0.0900(18) 0.0610(14) -0.0185(13) 0.0259(10) 0.0048(11) C17 0.0357(11) 0.0742(16) 0.0563(13) -0.0209(12) 0.0265(10) 0.0025(10) C18 0.0277(9) 0.0483(12) 0.0442(10) -0.0070(9) 0.0200(8) 0.0003(8) C19 0.0287(9) 0.0416(11) 0.0399(10) -0.0029(8) 0.0138(8) 0.0005(8) C20 0.0556(14) 0.0570(14) 0.0661(15) -0.0152(12) 0.0334(12) -0.0171(11) C21 0.0792(18) 0.0566(15) 0.0391(11) -0.0043(11) 0.0186(12) 0.0077(13) C22 0.0307(10) 0.0587(14) 0.0619(13) -0.0250(11) 0.0268(10) -0.0048(9) C23 0.0412(12) 0.0519(13) 0.0495(12) -0.0119(10) 0.0151(10) 0.0004(10) C24 0.088(2) 0.084(2) 0.0833(19) -0.0196(16) 0.0579(18) -0.0381(17) C25 0.0229(8) 0.0325(9) 0.0246(8) -0.0038(7) 0.0096(7) 0.0042(7) C26 0.0264(9) 0.0420(10) 0.0280(8) -0.0046(7) 0.0143(7) 0.0038(7) C27 0.0288(9) 0.0589(13) 0.0345(9) -0.0023(9) 0.0179(8) 0.0088(9) C28 0.0318(10) 0.0619(13) 0.0352(10) 0.0002(9) 0.0147(8) 0.0198(9) C29 0.0391(10) 0.0417(11) 0.0318(9) 0.0013(8) 0.0124(8) 0.0151(9) C30 0.0302(9) 0.0346(10) 0.0281(8) -0.0043(7) 0.0108(7) 0.0051(7) C31 0.0313(9) 0.0427(10) 0.0390(10) 0.0002(8) 0.0229(8) 0.0033(8) C32 0.0440(12) 0.0530(13) 0.0547(12) -0.0050(10) 0.0339(10) -0.0052(10) C33 0.0429(11) 0.0558(13) 0.0389(10) 0.0064(9) 0.0205(9) 0.0040(10) C34 0.0390(11) 0.0315(10) 0.0451(11) 0.0043(8) 0.0177(9) 0.0037(8) C35 0.0565(14) 0.0335(11) 0.0667(15) 0.0028(11) 0.0168(12) 0.0013(10) C36 0.0663(15) 0.0519(13) 0.0584(14) 0.0088(11) 0.0383(12) -0.0012(11) C37 0.0241(8) 0.0296(9) 0.0293(8) 0.0031(7) 0.0152(7) 0.0021(6) C38 0.0253(8) 0.0343(9) 0.0296(8) 0.0013(7) 0.0151(7) 0.0014(7) C39 0.0336(10) 0.0450(11) 0.0331(9) -0.0055(8) 0.0192(8) -0.0004(8) C40 0.0372(10) 0.0555(12) 0.0450(11) -0.0037(9) 0.0297(9) 0.0008(9) C41 0.0276(9) 0.0508(12) 0.0443(11) -0.0026(9) 0.0215(8) -0.0049(8) C42 0.0263(8) 0.0368(10) 0.0326(9) 0.0000(7) 0.0155(7) -0.0032(7) C43 0.0311(10) 0.0532(12) 0.0397(10) -0.0083(9) 0.0195(8) -0.0125(9) C44 0.0494(13) 0.0533(14) 0.0723(16) -0.0196(12) 0.0254(12) -0.0085(11) C45 0.0342(11) 0.0746(16) 0.0477(12) -0.0046(11) 0.0141(9) -0.0134(11) C46 0.0279(9) 0.0508(11) 0.0291(9) -0.0075(8) 0.0157(7) -0.0064(8) C47 0.0535(13) 0.0568(13) 0.0449(11) -0.0186(10) 0.0290(10) -0.0215(11) C48 0.0297(10) 0.0832(17) 0.0326(10) -0.0002(10) 0.0114(8) 0.0038(10) C49 0.0427(12) 0.0454(12) 0.0410(11) -0.0047(10) 0.0108(10) 0.0030(10) C50 0.045(3) 0.031(5) 0.076(4) -0.004(3) -0.016(3) -0.008(2) C51 0.044(2) 0.0235(18) 0.042(2) -0.0010(16) 0.0040(19) -0.0010(15) C52 0.0498(13) 0.0373(12) 0.0561(13) -0.0063(10) 0.0133(11) 0.0113(10) C53 0.0473(12) 0.0386(11) 0.0328(9) -0.0035(8) 0.0180(9) -0.0032(9) C54 0.063(4) 0.047(3) 0.045(3) -0.006(2) 0.023(3) -0.017(3) C55 0.167(10) 0.039(4) 0.082(7) -0.004(4) 0.097(7) -0.027(5) C56 0.0742(17) 0.0442(13) 0.0431(12) 0.0061(10) 0.0274(12) -0.0172(12) C57 0.120(4) 0.153(5) 0.081(3) -0.011(3) 0.034(3) -0.013(4) C58 0.110(4) 0.197(7) 0.099(4) -0.036(4) 0.038(3) -0.002(4) C59 0.115(5) 0.259(9) 0.098(4) -0.003(5) 0.037(4) -0.042(5) C50A 0.094(9) 0.021(5) 0.102(8) 0.004(4) 0.045(7) 0.007(4) C51A 0.082(6) 0.077(6) 0.106(7) -0.002(4) 0.029(4) 0.004(4) C54A 0.080(5) 0.042(3) 0.061(4) -0.013(3) 0.044(4) -0.019(3) C55A 0.171(10) 0.097(13) 0.091(8) -0.047(6) 0.075(7) -0.101(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ca1 O1 2.3623(13) . ? Ca1 O2 2.3841(14) . ? Ca1 N4 2.4154(14) . ? Ca1 N3 2.4738(14) . ? Ca1 N1 2.4791(14) . ? Ca1 N6 2.4944(14) . ? Ca1 N5 2.9290(15) . ? Ca1 N2 2.9717(14) . ? O1 C56 1.440(2) . ? O1 C53 1.455(2) . ? O2 C52 1.447(3) . ? O2 C49 1.455(3) . ? N1 N2 1.3052(19) . ? N1 C37 1.431(2) . ? N2 N3 1.3275(19) . ? N3 C25 1.419(2) . ? N4 N5 1.317(2) . ? N4 C13 1.430(2) . ? N5 N6 1.3148(19) . ? N6 C1 1.426(2) . ? C1 C6 1.413(3) . ? C1 C2 1.415(3) . ? C2 C3 1.391(3) . ? C2 C10 1.516(3) . ? C3 C4 1.380(4) . ? C3 H3 0.9500 . ? C4 C5 1.364(3) . ? C4 H4 0.9500 . ? C5 C6 1.404(3) . ? C5 H5 0.9500 . ? C6 C7 1.516(3) . ? C7 C9 1.531(3) . ? C7 C8 1.536(3) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C12 1.529(3) . ? C10 C11 1.533(3) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.407(3) . ? C13 C18 1.411(3) . ? C14 C15 1.390(3) . ? C14 C19 1.518(3) . ? C15 C16 1.373(3) . ? C15 H15 0.9500 . ? C16 C17 1.379(3) . ? C16 H16 0.9500 . ? C17 C18 1.390(3) . ? C17 H17 0.9500 . ? C18 C22 1.521(3) . ? C19 C20 1.527(3) . ? C19 C21 1.530(3) . ? C19 H19 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.524(3) . ? C22 C24 1.525(4) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C30 1.413(3) . ? C25 C26 1.420(2) . ? C26 C27 1.391(2) . ? C26 C31 1.520(3) . ? C27 C28 1.382(3) . ? C27 H27 0.9500 . ? C28 C29 1.373(3) . ? C28 H28 0.9500 . ? C29 C30 1.400(3) . ? C29 H29 0.9500 . ? C30 C34 1.522(3) . ? C31 C32 1.528(3) . ? C31 C33 1.531(3) . ? C31 H31 1.0000 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C36 1.523(3) . ? C34 C35 1.538(3) . ? C34 H34 1.0000 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.408(2) . ? C37 C42 1.411(2) . ? C38 C39 1.398(2) . ? C38 C46 1.517(2) . ? C39 C40 1.379(3) . ? C39 H39 0.9500 . ? C40 C41 1.379(3) . ? C40 H40 0.9500 . ? C41 C42 1.384(3) . ? C41 H41 0.9500 . ? C42 C43 1.519(3) . ? C43 C44 1.515(3) . ? C43 C45 1.525(3) . ? C43 H43 1.0000 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 C48 1.528(3) . ? C46 C47 1.534(3) . ? C46 H46 1.0000 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 C50 1.422(12) . ? C49 C50A 1.665(19) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C49 H49C 0.95(7) . ? C49 H49D 0.96(7) . ? C50 C51 1.539(2) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 C52 1.585(6) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C51 H52C 1.58(7) . ? C52 C51A 1.344(15) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C52 H52C 1.37(7) . ? C52 H52D 0.94(7) . ? C53 C54A 1.463(7) . ? C53 C54 1.572(6) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C53 H53C 1.04(5) . ? C53 H53D 1.13(5) . ? C54 C55 1.541(2) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.427(14) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C55A 1.465(17) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C56 H56C 1.16(6) . ? C56 H56D 1.04(6) . ? C57 C57 1.323(10) 2 ? C57 C58 1.529(2) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 C59 1.525(2) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C50A C51A 1.539(2) . ? C50A H50C 0.9900 . ? C50A H50D 0.9900 . ? C51A H52C 1.03(7) . ? C51A H51C 0.9900 . ? C51A H51D 0.9900 . ? C54A C55A 1.540(2) . ? C54A H54C 0.9900 . ? C54A H54D 0.9900 . ? C55A H55C 0.9900 . ? C55A H55D 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 Ca1 O2 164.10(5) . . ? O1 Ca1 N4 94.91(5) . . ? O2 Ca1 N4 96.81(5) . . ? O1 Ca1 N3 87.82(5) . . ? O2 Ca1 N3 84.95(5) . . ? N4 Ca1 N3 159.49(5) . . ? O1 Ca1 N1 90.05(4) . . ? O2 Ca1 N1 96.58(5) . . ? N4 Ca1 N1 107.64(5) . . ? N3 Ca1 N1 51.96(4) . . ? O1 Ca1 N6 86.40(5) . . ? O2 Ca1 N6 92.14(5) . . ? N4 Ca1 N6 52.88(5) . . ? N3 Ca1 N6 147.62(5) . . ? N1 Ca1 N6 159.65(5) . . ? O1 Ca1 N5 90.08(4) . . ? O2 Ca1 N5 95.67(4) . . ? N4 Ca1 N5 26.36(4) . . ? N3 Ca1 N5 174.05(4) . . ? N1 Ca1 N5 133.65(4) . . ? N6 Ca1 N5 26.54(4) . . ? O1 Ca1 N2 89.28(4) . . ? O2 Ca1 N2 90.47(4) . . ? N4 Ca1 N2 133.31(4) . . ? N3 Ca1 N2 26.23(4) . . ? N1 Ca1 N2 25.73(4) . . ? N6 Ca1 N2 172.87(4) . . ? N5 Ca1 N2 159.36(4) . . ? C56 O1 C53 108.86(15) . . ? C56 O1 Ca1 131.49(12) . . ? C53 O1 Ca1 119.59(11) . . ? C52 O2 C49 108.32(16) . . ? C52 O2 Ca1 126.61(13) . . ? C49 O2 Ca1 125.04(12) . . ? N2 N1 C37 114.95(13) . . ? N2 N1 Ca1 98.72(9) . . ? C37 N1 Ca1 146.29(10) . . ? N1 N2 N3 110.99(13) . . ? N1 N2 Ca1 55.55(8) . . ? N3 N2 Ca1 55.46(8) . . ? N2 N3 C25 114.15(13) . . ? N2 N3 Ca1 98.30(9) . . ? C25 N3 Ca1 146.97(11) . . ? N5 N4 C13 111.72(13) . . ? N5 N4 Ca1 99.13(9) . . ? C13 N4 Ca1 148.97(11) . . ? N6 N5 N4 112.43(13) . . ? N6 N5 Ca1 57.96(8) . . ? N4 N5 Ca1 54.51(8) . . ? N5 N6 C1 112.86(13) . . ? N5 N6 Ca1 95.50(9) . . ? C1 N6 Ca1 150.40(11) . . ? C6 C1 C2 120.00(17) . . ? C6 C1 N6 123.05(16) . . ? C2 C1 N6 116.86(16) . . ? C3 C2 C1 118.99(19) . . ? C3 C2 C10 120.39(18) . . ? C1 C2 C10 120.29(16) . . ? C4 C3 C2 121.2(2) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C5 C4 C3 119.81(19) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 122.1(2) . . ? C4 C5 H5 118.9 . . ? C6 C5 H5 118.9 . . ? C5 C6 C1 117.89(19) . . ? C5 C6 C7 118.48(19) . . ? C1 C6 C7 123.63(17) . . ? C6 C7 C9 111.9(2) . . ? C6 C7 C8 112.81(18) . . ? C9 C7 C8 110.01(19) . . ? C6 C7 H7 107.3 . . ? C9 C7 H7 107.3 . . ? C8 C7 H7 107.3 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C2 C10 C12 114.54(19) . . ? C2 C10 C11 108.65(18) . . ? C12 C10 C11 110.40(19) . . ? C2 C10 H10 107.7 . . ? C12 C10 H10 107.7 . . ? C11 C10 H10 107.7 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C18 120.04(16) . . ? C14 C13 N4 121.98(16) . . ? C18 C13 N4 117.93(15) . . ? C15 C14 C13 118.57(18) . . ? C15 C14 C19 118.17(17) . . ? C13 C14 C19 123.25(16) . . ? C16 C15 C14 121.70(19) . . ? C16 C15 H15 119.2 . . ? C14 C15 H15 119.1 . . ? C15 C16 C17 119.60(19) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? C16 C17 C18 121.3(2) . . ? C16 C17 H17 119.4 . . ? C18 C17 H17 119.4 . . ? C17 C18 C13 118.80(18) . . ? C17 C18 C22 119.01(18) . . ? C13 C18 C22 122.05(16) . . ? C14 C19 C20 112.00(18) . . ? C14 C19 C21 110.40(17) . . ? C20 C19 C21 110.11(19) . . ? C14 C19 H19 108.1 . . ? C20 C19 H19 108.1 . . ? C21 C19 H19 108.1 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C18 C22 C23 113.25(18) . . ? C18 C22 C24 109.9(2) . . ? C23 C22 C24 110.44(19) . . ? C18 C22 H22 107.7 . . ? C23 C22 H22 107.7 . . ? C24 C22 H22 107.7 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C30 C25 N3 123.78(15) . . ? C30 C25 C26 119.70(15) . . ? N3 C25 C26 116.39(15) . . ? C27 C26 C25 118.85(17) . . ? C27 C26 C31 120.80(17) . . ? C25 C26 C31 120.31(15) . . ? C28 C27 C26 121.57(19) . . ? C28 C27 H27 119.2 . . ? C26 C27 H27 119.2 . . ? C29 C28 C27 119.36(17) . . ? C29 C28 H28 120.3 . . ? C27 C28 H28 120.3 . . ? C28 C29 C30 122.00(19) . . ? C28 C29 H29 119.0 . . ? C30 C29 H29 119.0 . . ? C29 C30 C25 118.36(18) . . ? C29 C30 C34 118.29(17) . . ? C25 C30 C34 123.32(16) . . ? C26 C31 C32 115.60(16) . . ? C26 C31 C33 109.55(16) . . ? C32 C31 C33 109.76(16) . . ? C26 C31 H31 107.2 . . ? C32 C31 H31 107.2 . . ? C33 C31 H31 107.2 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C30 C34 C36 112.17(17) . . ? C30 C34 C35 112.00(18) . . ? C36 C34 C35 109.81(18) . . ? C30 C34 H34 107.5 . . ? C36 C34 H34 107.5 . . ? C35 C34 H34 107.5 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 C42 120.04(15) . . ? C38 C37 N1 123.46(15) . . ? C42 C37 N1 116.25(15) . . ? C39 C38 C37 118.31(16) . . ? C39 C38 C46 117.00(15) . . ? C37 C38 C46 124.68(15) . . ? C40 C39 C38 121.55(17) . . ? C40 C39 H39 119.2 . . ? C38 C39 H39 119.2 . . ? C41 C40 C39 119.69(17) . . ? C41 C40 H40 120.2 . . ? C39 C40 H40 120.2 . . ? C40 C41 C42 121.13(17) . . ? C40 C41 H41 119.4 . . ? C42 C41 H41 119.4 . . ? C41 C42 C37 119.27(16) . . ? C41 C42 C43 119.82(16) . . ? C37 C42 C43 120.71(15) . . ? C44 C43 C42 109.34(18) . . ? C44 C43 C45 110.78(18) . . ? C42 C43 C45 113.92(17) . . ? C44 C43 H43 107.5 . . ? C42 C43 H43 107.5 . . ? C45 C43 H43 107.5 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C38 C46 C48 110.64(16) . . ? C38 C46 C47 111.89(16) . . ? C48 C46 C47 110.45(17) . . ? C38 C46 H46 107.9 . . ? C48 C46 H46 107.9 . . ? C47 C46 H46 107.9 . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C46 C48 H48A 109.5 . . ? C46 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C46 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C50 C49 O2 106.6(3) . . ? C50 C49 C50A 7.0(12) . . ? O2 C49 C50A 106.9(5) . . ? C50 C49 H49A 110.4 . . ? O2 C49 H49A 110.4 . . ? C50A C49 H49A 104.1 . . ? C50 C49 H49B 110.4 . . ? O2 C49 H49B 110.4 . . ? C50A C49 H49B 116.2 . . ? H49A C49 H49B 108.6 . . ? C50 C49 H49C 110(4) . . ? O2 C49 H49C 99(4) . . ? C50A C49 H49C 117(4) . . ? H49A C49 H49C 118.7 . . ? H49B C49 H49C 12.2 . . ? C50 C49 H49D 124(4) . . ? O2 C49 H49D 109(4) . . ? C50A C49 H49D 118(4) . . ? H49A C49 H49D 15.0 . . ? H49B C49 H49D 96.3 . . ? H49C C49 H49D 105(5) . . ? C49 C50 C51 106.5(6) . . ? C49 C50 H50A 110.4 . . ? C51 C50 H50A 110.4 . . ? C49 C50 H50B 110.4 . . ? C51 C50 H50B 110.4 . . ? H50A C50 H50B 108.6 . . ? C50 C51 C52 96.0(5) . . ? C50 C51 H51A 112.6 . . ? C52 C51 H51A 112.6 . . ? C50 C51 H51B 112.6 . . ? C52 C51 H51B 112.6 . . ? H51A C51 H51B 110.1 . . ? C50 C51 H52C 74(2) . . ? C52 C51 H52C 51(2) . . ? H51A C51 H52C 78.8 . . ? H51B C51 H52C 163.7 . . ? C51A C52 O2 110.7(6) . . ? C51A C52 C51 19.8(7) . . ? O2 C52 C51 101.4(3) . . ? C51A C52 H52A 120.5 . . ? O2 C52 H52A 111.5 . . ? C51 C52 H52A 111.5 . . ? C51A C52 H52B 91.7 . . ? O2 C52 H52B 111.5 . . ? C51 C52 H52B 111.5 . . ? H52A C52 H52B 109.3 . . ? C51A C52 H52C 45(3) . . ? O2 C52 H52C 111(3) . . ? C51 C52 H52C 64(3) . . ? H52A C52 H52C 137.3 . . ? H52B C52 H52C 48.6 . . ? C51A C52 H52D 127(4) . . ? O2 C52 H52D 105(4) . . ? C51 C52 H52D 116(4) . . ? H52A C52 H52D 7.3 . . ? H52B C52 H52D 110.7 . . ? H52C C52 H52D 144(5) . . ? O1 C53 C54A 107.6(3) . . ? O1 C53 C54 104.1(2) . . ? C54A C53 C54 29.8(3) . . ? O1 C53 H53A 110.9 . . ? C54A C53 H53A 131.6 . . ? C54 C53 H53A 110.9 . . ? O1 C53 H53B 110.9 . . ? C54A C53 H53B 82.5 . . ? C54 C53 H53B 110.9 . . ? H53A C53 H53B 109.0 . . ? O1 C53 H53C 105(3) . . ? C54A C53 H53C 118(3) . . ? C54 C53 H53C 92(3) . . ? H53A C53 H53C 22.8 . . ? H53B C53 H53C 129.9 . . ? O1 C53 H53D 107(2) . . ? C54A C53 H53D 115(2) . . ? C54 C53 H53D 141(2) . . ? H53A C53 H53D 79.6 . . ? H53B C53 H53D 34.3 . . ? H53C C53 H53D 102(4) . . ? C55 C54 C53 98.1(5) . . ? C55 C54 H54A 112.1 . . ? C53 C54 H54A 112.1 . . ? C55 C54 H54B 112.1 . . ? C53 C54 H54B 112.1 . . ? H54A C54 H54B 109.8 . . ? C56 C55 C54 103.7(7) . . ? C56 C55 H55A 111.0 . . ? C54 C55 H55A 111.0 . . ? C56 C55 H55B 111.0 . . ? C54 C55 H55B 111.0 . . ? H55A C55 H55B 109.0 . . ? C55 C56 O1 107.1(3) . . ? C55 C56 C55A 15.4(9) . . ? O1 C56 C55A 106.8(4) . . ? C55 C56 H56A 110.3 . . ? O1 C56 H56A 110.3 . . ? C55A C56 H56A 96.7 . . ? C55 C56 H56B 110.3 . . ? O1 C56 H56B 110.3 . . ? C55A C56 H56B 123.2 . . ? H56A C56 H56B 108.5 . . ? C55 C56 H56C 91(3) . . ? O1 C56 H56C 93(3) . . ? C55A C56 H56C 106(3) . . ? H56A C56 H56C 140.8 . . ? H56B C56 H56C 32.3 . . ? C55 C56 H56D 142(3) . . ? O1 C56 H56D 111(3) . . ? C55A C56 H56D 139(3) . . ? H56A C56 H56D 56.7 . . ? H56B C56 H56D 54.8 . . ? H56C C56 H56D 86(4) . . ? C57 C57 C58 113.9(6) 2 . ? C57 C57 H57A 108.8 2 . ? C58 C57 H57A 108.8 . . ? C57 C57 H57B 108.8 2 . ? C58 C57 H57B 108.8 . . ? H57A C57 H57B 107.7 . . ? C59 C58 C57 115.6(5) . . ? C59 C58 H58A 108.4 . . ? C57 C58 H58A 108.4 . . ? C59 C58 H58B 108.4 . . ? C57 C58 H58B 108.4 . . ? H58A C58 H58B 107.4 . . ? C58 C59 H59A 109.5 . . ? C58 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C58 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C51A C50A C49 97.3(11) . . ? C51A C50A H50C 112.3 . . ? C49 C50A H50C 112.3 . . ? C51A C50A H50D 112.3 . . ? C49 C50A H50D 112.3 . . ? H50C C50A H50D 109.9 . . ? C52 C51A C50A 114.8(13) . . ? C52 C51A H52C 69(4) . . ? C50A C51A H52C 99(4) . . ? C52 C51A H51C 108.6 . . ? C50A C51A H51C 108.6 . . ? H52C C51A H51C 149.4 . . ? C52 C51A H51D 108.6 . . ? C50A C51A H51D 108.6 . . ? H52C C51A H51D 50.0 . . ? H51C C51A H51D 107.6 . . ? C53 C54A C55A 102.1(8) . . ? C53 C54A H54C 111.4 . . ? C55A C54A H54C 111.4 . . ? C53 C54A H54D 111.4 . . ? C55A C54A H54D 111.4 . . ? H54C C54A H54D 109.2 . . ? C56 C55A C54A 105.7(9) . . ? C56 C55A H55C 110.6 . . ? C54A C55A H55C 110.6 . . ? C56 C55A H55D 110.6 . . ? C54A C55A H55D 110.6 . . ? H55C C55A H55D 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 O2 Ca1 O1 C56 66.4(3) . . . . ? N4 Ca1 O1 C56 -70.99(19) . . . . ? N3 Ca1 O1 C56 129.37(19) . . . . ? N1 Ca1 O1 C56 -178.70(19) . . . . ? N6 Ca1 O1 C56 -18.75(19) . . . . ? N5 Ca1 O1 C56 -45.05(19) . . . . ? N2 Ca1 O1 C56 155.58(19) . . . . ? O2 Ca1 O1 C53 -110.5(2) . . . . ? N4 Ca1 O1 C53 112.06(13) . . . . ? N3 Ca1 O1 C53 -47.57(13) . . . . ? N1 Ca1 O1 C53 4.35(13) . . . . ? N6 Ca1 O1 C53 164.31(13) . . . . ? N5 Ca1 O1 C53 138.01(13) . . . . ? N2 Ca1 O1 C53 -21.36(13) . . . . ? O1 Ca1 O2 C52 32.8(3) . . . . ? N4 Ca1 O2 C52 170.01(17) . . . . ? N3 Ca1 O2 C52 -30.54(17) . . . . ? N1 Ca1 O2 C52 -81.27(17) . . . . ? N6 Ca1 O2 C52 117.15(17) . . . . ? N5 Ca1 O2 C52 143.52(17) . . . . ? N2 Ca1 O2 C52 -56.22(17) . . . . ? O1 Ca1 O2 C49 -149.58(18) . . . . ? N4 Ca1 O2 C49 -12.35(16) . . . . ? N3 Ca1 O2 C49 147.10(16) . . . . ? N1 Ca1 O2 C49 96.37(16) . . . . ? N6 Ca1 O2 C49 -65.22(16) . . . . ? N5 Ca1 O2 C49 -38.85(16) . . . . ? N2 Ca1 O2 C49 121.42(16) . . . . ? O1 Ca1 N1 N2 -88.24(10) . . . . ? O2 Ca1 N1 N2 77.27(10) . . . . ? N4 Ca1 N1 N2 176.59(9) . . . . ? N3 Ca1 N1 N2 -1.04(8) . . . . ? N6 Ca1 N1 N2 -167.96(12) . . . . ? N5 Ca1 N1 N2 -178.40(8) . . . . ? O1 Ca1 N1 C37 89.1(2) . . . . ? O2 Ca1 N1 C37 -105.4(2) . . . . ? N4 Ca1 N1 C37 -6.1(2) . . . . ? N3 Ca1 N1 C37 176.3(2) . . . . ? N6 Ca1 N1 C37 9.4(3) . . . . ? N5 Ca1 N1 C37 -1.1(2) . . . . ? N2 Ca1 N1 C37 177.3(3) . . . . ? C37 N1 N2 N3 -176.74(13) . . . . ? Ca1 N1 N2 N3 1.64(13) . . . . ? C37 N1 N2 Ca1 -178.37(16) . . . . ? O1 Ca1 N2 N1 91.60(10) . . . . ? O2 Ca1 N2 N1 -104.30(10) . . . . ? N4 Ca1 N2 N1 -4.47(12) . . . . ? N3 Ca1 N2 N1 178.14(15) . . . . ? N6 Ca1 N2 N1 144.2(3) . . . . ? N5 Ca1 N2 N1 3.28(17) . . . . ? O1 Ca1 N2 N3 -86.54(10) . . . . ? O2 Ca1 N2 N3 77.56(10) . . . . ? N4 Ca1 N2 N3 177.39(9) . . . . ? N1 Ca1 N2 N3 -178.14(15) . . . . ? N6 Ca1 N2 N3 -33.9(4) . . . . ? N5 Ca1 N2 N3 -174.86(12) . . . . ? N1 N2 N3 C25 -175.37(14) . . . . ? Ca1 N2 N3 C25 -173.73(16) . . . . ? N1 N2 N3 Ca1 -1.64(13) . . . . ? O1 Ca1 N3 N2 92.79(9) . . . . ? O2 Ca1 N3 N2 -101.40(10) . . . . ? N4 Ca1 N3 N2 -5.4(2) . . . . ? N1 Ca1 N3 N2 1.02(8) . . . . ? N6 Ca1 N3 N2 172.57(9) . . . . ? N5 Ca1 N3 N2 162.3(4) . . . . ? O1 Ca1 N3 C25 -97.7(2) . . . . ? O2 Ca1 N3 C25 68.1(2) . . . . ? N4 Ca1 N3 C25 164.04(18) . . . . ? N1 Ca1 N3 C25 170.5(2) . . . . ? N6 Ca1 N3 C25 -18.0(3) . . . . ? N5 Ca1 N3 C25 -28.2(6) . . . . ? N2 Ca1 N3 C25 169.5(3) . . . . ? O1 Ca1 N4 N5 80.21(10) . . . . ? O2 Ca1 N4 N5 -89.03(10) . . . . ? N3 Ca1 N4 N5 177.15(12) . . . . ? N1 Ca1 N4 N5 171.82(9) . . . . ? N6 Ca1 N4 N5 -1.51(9) . . . . ? N2 Ca1 N4 N5 173.85(8) . . . . ? O1 Ca1 N4 C13 -93.8(2) . . . . ? O2 Ca1 N4 C13 97.0(2) . . . . ? N3 Ca1 N4 C13 3.2(3) . . . . ? N1 Ca1 N4 C13 -2.2(2) . . . . ? N6 Ca1 N4 C13 -175.5(2) . . . . ? N5 Ca1 N4 C13 -174.0(3) . . . . ? N2 Ca1 N4 C13 -0.1(3) . . . . ? C13 N4 N5 N6 179.14(14) . . . . ? Ca1 N4 N5 N6 2.47(14) . . . . ? C13 N4 N5 Ca1 176.67(16) . . . . ? O1 Ca1 N5 N6 81.75(10) . . . . ? O2 Ca1 N5 N6 -83.40(10) . . . . ? N4 Ca1 N5 N6 -177.30(16) . . . . ? N3 Ca1 N5 N6 12.4(5) . . . . ? N1 Ca1 N5 N6 171.90(9) . . . . ? N2 Ca1 N5 N6 169.93(11) . . . . ? O1 Ca1 N5 N4 -100.95(10) . . . . ? O2 Ca1 N5 N4 93.90(10) . . . . ? N3 Ca1 N5 N4 -170.3(4) . . . . ? N1 Ca1 N5 N4 -10.80(12) . . . . ? N6 Ca1 N5 N4 177.30(16) . . . . ? N2 Ca1 N5 N4 -12.77(17) . . . . ? N4 N5 N6 C1 -173.71(14) . . . . ? Ca1 N5 N6 C1 -171.33(15) . . . . ? N4 N5 N6 Ca1 -2.38(14) . . . . ? O1 Ca1 N6 N5 -97.43(10) . . . . ? O2 Ca1 N6 N5 98.43(10) . . . . ? N4 Ca1 N6 N5 1.50(9) . . . . ? N3 Ca1 N6 N5 -177.62(9) . . . . ? N1 Ca1 N6 N5 -17.1(2) . . . . ? N2 Ca1 N6 N5 -150.2(3) . . . . ? O1 Ca1 N6 C1 66.2(2) . . . . ? O2 Ca1 N6 C1 -97.9(2) . . . . ? N4 Ca1 N6 C1 165.2(3) . . . . ? N3 Ca1 N6 C1 -14.0(3) . . . . ? N1 Ca1 N6 C1 146.6(2) . . . . ? N5 Ca1 N6 C1 163.7(3) . . . . ? N2 Ca1 N6 C1 13.5(5) . . . . ? N5 N6 C1 C6 45.6(2) . . . . ? Ca1 N6 C1 C6 -116.8(2) . . . . ? N5 N6 C1 C2 -137.80(16) . . . . ? Ca1 N6 C1 C2 59.9(3) . . . . ? C6 C1 C2 C3 -0.1(3) . . . . ? N6 C1 C2 C3 -176.81(17) . . . . ? C6 C1 C2 C10 -173.48(17) . . . . ? N6 C1 C2 C10 9.8(2) . . . . ? C1 C2 C3 C4 -0.6(3) . . . . ? C10 C2 C3 C4 172.8(2) . . . . ? C2 C3 C4 C5 0.1(4) . . . . ? C3 C4 C5 C6 1.1(4) . . . . ? C4 C5 C6 C1 -1.8(3) . . . . ? C4 C5 C6 C7 178.0(2) . . . . ? C2 C1 C6 C5 1.2(3) . . . . ? N6 C1 C6 C5 177.75(18) . . . . ? C2 C1 C6 C7 -178.56(18) . . . . ? N6 C1 C6 C7 -2.0(3) . . . . ? C5 C6 C7 C9 79.3(2) . . . . ? C1 C6 C7 C9 -101.0(2) . . . . ? C5 C6 C7 C8 -45.4(3) . . . . ? C1 C6 C7 C8 134.4(2) . . . . ? C3 C2 C10 C12 33.0(3) . . . . ? C1 C2 C10 C12 -153.70(19) . . . . ? C3 C2 C10 C11 -91.0(2) . . . . ? C1 C2 C10 C11 82.3(2) . . . . ? N5 N4 C13 C14 65.3(2) . . . . ? Ca1 N4 C13 C14 -121.1(2) . . . . ? N5 N4 C13 C18 -117.21(18) . . . . ? Ca1 N4 C13 C18 56.4(3) . . . . ? C18 C13 C14 C15 1.0(3) . . . . ? N4 C13 C14 C15 178.43(18) . . . . ? C18 C13 C14 C19 -179.36(18) . . . . ? N4 C13 C14 C19 -2.0(3) . . . . ? C13 C14 C15 C16 -1.4(3) . . . . ? C19 C14 C15 C16 179.0(2) . . . . ? C14 C15 C16 C17 0.7(4) . . . . ? C15 C16 C17 C18 0.4(4) . . . . ? C16 C17 C18 C13 -0.7(4) . . . . ? C16 C17 C18 C22 175.0(2) . . . . ? C14 C13 C18 C17 0.0(3) . . . . ? N4 C13 C18 C17 -177.53(19) . . . . ? C14 C13 C18 C22 -175.56(19) . . . . ? N4 C13 C18 C22 6.9(3) . . . . ? C15 C14 C19 C20 -53.9(3) . . . . ? C13 C14 C19 C20 126.5(2) . . . . ? C15 C14 C19 C21 69.2(3) . . . . ? C13 C14 C19 C21 -110.5(2) . . . . ? C17 C18 C22 C23 48.6(3) . . . . ? C13 C18 C22 C23 -135.9(2) . . . . ? C17 C18 C22 C24 -75.5(3) . . . . ? C13 C18 C22 C24 100.1(2) . . . . ? N2 N3 C25 C30 44.8(2) . . . . ? Ca1 N3 C25 C30 -123.79(19) . . . . ? N2 N3 C25 C26 -139.50(15) . . . . ? Ca1 N3 C25 C26 51.9(3) . . . . ? C30 C25 C26 C27 -4.1(2) . . . . ? N3 C25 C26 C27 -179.97(15) . . . . ? C30 C25 C26 C31 173.68(16) . . . . ? N3 C25 C26 C31 -2.2(2) . . . . ? C25 C26 C27 C28 1.0(3) . . . . ? C31 C26 C27 C28 -176.68(18) . . . . ? C26 C27 C28 C29 1.6(3) . . . . ? C27 C28 C29 C30 -1.2(3) . . . . ? C28 C29 C30 C25 -1.8(3) . . . . ? C28 C29 C30 C34 176.29(18) . . . . ? N3 C25 C30 C29 179.98(16) . . . . ? C26 C25 C30 C29 4.4(2) . . . . ? N3 C25 C30 C34 2.0(3) . . . . ? C26 C25 C30 C34 -173.56(16) . . . . ? C27 C26 C31 C32 -27.3(2) . . . . ? C25 C26 C31 C32 155.04(17) . . . . ? C27 C26 C31 C33 97.3(2) . . . . ? C25 C26 C31 C33 -80.4(2) . . . . ? C29 C30 C34 C36 77.0(2) . . . . ? C25 C30 C34 C36 -105.0(2) . . . . ? C29 C30 C34 C35 -47.0(2) . . . . ? C25 C30 C34 C35 130.98(19) . . . . ? N2 N1 C37 C38 56.0(2) . . . . ? Ca1 N1 C37 C38 -121.07(19) . . . . ? N2 N1 C37 C42 -129.71(16) . . . . ? Ca1 N1 C37 C42 53.2(3) . . . . ? C42 C37 C38 C39 -0.5(3) . . . . ? N1 C37 C38 C39 173.51(16) . . . . ? C42 C37 C38 C46 179.76(17) . . . . ? N1 C37 C38 C46 -6.2(3) . . . . ? C37 C38 C39 C40 0.0(3) . . . . ? C46 C38 C39 C40 179.69(18) . . . . ? C38 C39 C40 C41 0.5(3) . . . . ? C39 C40 C41 C42 -0.3(3) . . . . ? C40 C41 C42 C37 -0.3(3) . . . . ? C40 C41 C42 C43 174.76(19) . . . . ? C38 C37 C42 C41 0.7(3) . . . . ? N1 C37 C42 C41 -173.77(17) . . . . ? C38 C37 C42 C43 -174.29(17) . . . . ? N1 C37 C42 C43 11.2(2) . . . . ? C41 C42 C43 C44 -93.3(2) . . . . ? C37 C42 C43 C44 81.6(2) . . . . ? C41 C42 C43 C45 31.2(3) . . . . ? C37 C42 C43 C45 -153.85(18) . . . . ? C39 C38 C46 C48 66.2(2) . . . . ? C37 C38 C46 C48 -114.1(2) . . . . ? C39 C38 C46 C47 -57.4(2) . . . . ? C37 C38 C46 C47 122.32(19) . . . . ? C52 O2 C49 C50 7.0(6) . . . . ? Ca1 O2 C49 C50 -171.0(6) . . . . ? C52 O2 C49 C50A 14.3(8) . . . . ? Ca1 O2 C49 C50A -163.7(8) . . . . ? O2 C49 C50 C51 23.4(9) . . . . ? C50A C49 C50 C51 -70(5) . . . . ? C49 C50 C51 C52 -40.9(8) . . . . ? C49 O2 C52 C51A -14.6(8) . . . . ? Ca1 O2 C52 C51A 163.3(7) . . . . ? C49 O2 C52 C51 -32.9(3) . . . . ? Ca1 O2 C52 C51 145.1(2) . . . . ? C50 C51 C52 C51A -77(2) . . . . ? C50 C51 C52 O2 43.3(6) . . . . ? C56 O1 C53 C54A 16.6(4) . . . . ? Ca1 O1 C53 C54A -165.8(3) . . . . ? C56 O1 C53 C54 -14.2(3) . . . . ? Ca1 O1 C53 C54 163.4(3) . . . . ? O1 C53 C54 C55 33.4(6) . . . . ? C54A C53 C54 C55 -67.5(9) . . . . ? C53 C54 C55 C56 -41.8(7) . . . . ? C54 C55 C56 O1 35.6(7) . . . . ? C54 C55 C56 C55A -56(2) . . . . ? C53 O1 C56 C55 -13.2(5) . . . . ? Ca1 O1 C56 C55 169.6(4) . . . . ? C53 O1 C56 C55A 2.9(8) . . . . ? Ca1 O1 C56 C55A -174.3(7) . . . . ? C57 C57 C58 C59 170.6(5) 2 . . . ? C50 C49 C50A C51A 80(5) . . . . ? O2 C49 C50A C51A -8.9(12) . . . . ? O2 C52 C51A C50A 8.5(15) . . . . ? C51 C52 C51A C50A 73(2) . . . . ? C49 C50A C51A C52 0.4(16) . . . . ? O1 C53 C54A C55A -27.7(8) . . . . ? C54 C53 C54A C55A 60.0(10) . . . . ? C55 C56 C55A C54A 73.4(19) . . . . ? O1 C56 C55A C54A -20.1(12) . . . . ? C53 C54A C55A C56 29.3(12) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.566 _refine_diff_density_min -0.425 _refine_diff_density_rms 0.050