# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Michael Hill' _publ_contact_author_email M.S.HILL@BATH.AC.UK _publ_section_title ; Beta-Diketiminate C-H Activation With Heavier Group 2 Alkyls ; loop_ _publ_author_name 'Michael Hill' 'Anthony G. M. Barrett' 'Mark R Crimmin' 'Dugald J. MacDougall' 'Mary Mahon' ; P.Procopiou ; # Attachment 'Compound_9.cif' data_c:\x-ray\helix\h08msh23\maxus_~1\h08msh23 _database_code_depnum_ccdc_archive 'CCDC 727087' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H48 N2 O Sr' _chemical_formula_weight 576.35 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' Sr Sr -1.5307 3.2498 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pcab loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z+1/2' 'x+1/2, -y, -z+1/2' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z-1/2' '-x-1/2, y, z-1/2' 'x-1/2, -y-1/2, z' _cell_length_a 13.4819(1) _cell_length_b 21.4266(2) _cell_length_c 21.6732(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6260.77(11) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 57609 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.223 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2448 _exptl_absorpt_coefficient_mu 1.748 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.70 _exptl_absorpt_correction_T_max 0.85 _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 91870 _diffrn_reflns_av_R_equivalents 0.1270 _diffrn_reflns_av_sigmaI/netI 0.0553 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 4.51 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7146 _reflns_number_gt 4933 _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^)+(0.0370P)^2^+4.2061P] 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 7146 _refine_ls_number_parameters 388 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0774 _refine_ls_R_factor_gt 0.0402 _refine_ls_wR_factor_ref 0.0965 _refine_ls_wR_factor_gt 0.0827 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _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 Sr1 Sr 0.488119(16) -0.054786(10) 0.427954(10) 0.02347(8) Uani 1 1 d . . . O1 O 0.60789(14) -0.14547(9) 0.41086(8) 0.0366(5) Uani 1 1 d D . . N1 N 0.62904(14) 0.09641(9) 0.49197(9) 0.0232(4) Uani 1 1 d . . . N2 N 0.50927(14) 0.00128(10) 0.32411(9) 0.0235(4) Uani 1 1 d . . . C1 C 0.47409(18) 0.07243(12) 0.44552(11) 0.0248(5) Uani 1 1 d D . . C2 C 0.57927(18) 0.07111(11) 0.44313(11) 0.0224(5) Uani 1 1 d . . . C3 C 0.63472(18) 0.03914(11) 0.39480(11) 0.0230(5) Uani 1 1 d D . . H3 H 0.7068(4) 0.0420(11) 0.4000(12) 0.028(7) Uiso 1 1 d D . . C4 C 0.60230(17) 0.01872(11) 0.33627(11) 0.0232(5) Uani 1 1 d . . . C5 C 0.68042(18) 0.01545(13) 0.28607(11) 0.0285(6) Uani 1 1 d . . . H5A H 0.6712 -0.0228 0.2620 0.043 Uiso 1 1 calc R D . H5B H 0.7465 0.0153 0.3049 0.043 Uiso 1 1 calc R . . H5C H 0.6740 0.0518 0.2589 0.043 Uiso 1 1 calc R . . C6 C 0.73212(17) 0.10847(11) 0.48706(11) 0.0236(5) Uani 1 1 d . . . C7 C 0.80110(18) 0.07248(12) 0.52097(11) 0.0273(6) Uani 1 1 d . . . C8 C 0.90087(19) 0.08993(13) 0.52107(12) 0.0334(6) Uani 1 1 d . . . H8 H 0.9470 0.0665 0.5448 0.040 Uiso 1 1 calc R . . C9 C 0.93349(19) 0.14026(13) 0.48755(13) 0.0354(7) Uani 1 1 d . . . H9 H 1.0015 0.1518 0.4886 0.042 Uiso 1 1 calc R . . C10 C 0.8668(2) 0.17413(13) 0.45224(12) 0.0328(6) Uani 1 1 d . . . H10 H 0.8903 0.2082 0.4282 0.039 Uiso 1 1 calc R . . C11 C 0.76650(18) 0.15943(12) 0.45120(11) 0.0276(6) Uani 1 1 d . . . C12 C 0.7673(2) 0.01546(13) 0.55644(13) 0.0352(7) Uani 1 1 d . . . H12 H 0.6987 0.0053 0.5421 0.042 Uiso 1 1 calc R . . C13 C 0.7610(4) 0.0291(2) 0.62461(16) 0.0900(16) Uani 1 1 d . . . H13A H 0.8280 0.0347 0.6413 0.135 Uiso 1 1 calc R . . H13B H 0.7286 -0.0058 0.6457 0.135 Uiso 1 1 calc R . . H13C H 0.7225 0.0673 0.6312 0.135 Uiso 1 1 calc R . . C14 C 0.8318(3) -0.04212(16) 0.5442(2) 0.0700(12) Uani 1 1 d . . . H14A H 0.8395 -0.0480 0.4996 0.105 Uiso 1 1 calc R . . H14B H 0.8000 -0.0791 0.5621 0.105 Uiso 1 1 calc R . . H14C H 0.8972 -0.0362 0.5631 0.105 Uiso 1 1 calc R . . C15 C 0.6950(2) 0.19743(13) 0.41222(13) 0.0363(7) Uani 1 1 d . . . H15 H 0.6286 0.1767 0.4143 0.044 Uiso 1 1 calc R . . C16 C 0.6832(3) 0.26398(19) 0.43622(19) 0.0858(14) Uani 1 1 d . . . H16A H 0.6583 0.2629 0.4787 0.129 Uiso 1 1 calc R . . H16B H 0.6360 0.2866 0.4101 0.129 Uiso 1 1 calc R . . H16C H 0.7476 0.2852 0.4353 0.129 Uiso 1 1 calc R . . C17 C 0.7263(3) 0.19977(18) 0.34450(16) 0.0665(10) Uani 1 1 d . . . H17A H 0.7882 0.2234 0.3407 0.100 Uiso 1 1 calc R . . H17B H 0.6743 0.2202 0.3202 0.100 Uiso 1 1 calc R . . H17C H 0.7363 0.1572 0.3292 0.100 Uiso 1 1 calc R . . C18 C 0.48085(16) -0.00392(12) 0.26097(11) 0.0232(5) Uani 1 1 d . . . C19 C 0.45959(18) 0.05061(12) 0.22752(12) 0.0295(6) Uani 1 1 d . . . C20 C 0.42971(19) 0.04471(14) 0.16572(13) 0.0361(7) Uani 1 1 d . . . H20 H 0.4156 0.0812 0.1425 0.043 Uiso 1 1 calc R . . C21 C 0.42045(19) -0.01277(15) 0.13812(12) 0.0380(7) Uani 1 1 d . . . H21 H 0.3994 -0.0158 0.0964 0.046 Uiso 1 1 calc R D . C22 C 0.4418(2) -0.06596(14) 0.17132(12) 0.0349(7) Uani 1 1 d . . . H22 H 0.4355 -0.1056 0.1521 0.042 Uiso 1 1 calc R . . C23 C 0.47254(18) -0.06258(12) 0.23256(12) 0.0287(6) Uani 1 1 d . . . C24 C 0.4679(2) 0.11466(13) 0.25703(14) 0.0416(7) Uani 1 1 d . . . H24 H 0.5105 0.1102 0.2945 0.050 Uiso 1 1 calc R . . C25 C 0.3661(3) 0.13706(16) 0.27844(17) 0.0616(10) Uani 1 1 d . . . H25A H 0.3232 0.1434 0.2425 0.092 Uiso 1 1 calc R D . H25B H 0.3733 0.1765 0.3009 0.092 Uiso 1 1 calc R . . H25C H 0.3365 0.1056 0.3057 0.092 Uiso 1 1 calc R . . C26 C 0.5178(3) 0.16194(16) 0.21466(19) 0.0687(11) Uani 1 1 d . . . H26A H 0.5825 0.1459 0.2016 0.103 Uiso 1 1 calc R D . H26B H 0.5269 0.2014 0.2368 0.103 Uiso 1 1 calc R . . H26C H 0.4760 0.1690 0.1783 0.103 Uiso 1 1 calc R . . C27 C 0.5020(2) -0.12153(13) 0.26644(13) 0.0374(7) Uani 1 1 d . . . H27 H 0.5412 -0.1081 0.3033 0.045 Uiso 1 1 calc R . . C28 C 0.5694(3) -0.16361(16) 0.22841(18) 0.0626(10) Uani 1 1 d . . . H28A H 0.5298 -0.1858 0.1974 0.094 Uiso 1 1 calc R D . H28B H 0.6018 -0.1939 0.2556 0.094 Uiso 1 1 calc R . . H28C H 0.6198 -0.1382 0.2077 0.094 Uiso 1 1 calc R . . C29 C 0.4137(3) -0.15720(18) 0.2905(2) 0.0755(12) Uani 1 1 d . . . H29A H 0.3742 -0.1300 0.3173 0.113 Uiso 1 1 calc R D . H29B H 0.4367 -0.1935 0.3141 0.113 Uiso 1 1 calc R . . H29C H 0.3730 -0.1713 0.2557 0.113 Uiso 1 1 calc R . . C30 C 0.5981(3) -0.20879(15) 0.4328(2) 0.0551(9) Uani 1 1 d D D . H30A H 0.5288 -0.2232 0.4274 0.066 Uiso 0.55 1 calc PR A 1 H30B H 0.6146 -0.2107 0.4773 0.066 Uiso 0.55 1 calc PR A 1 H30C H 0.542(6) -0.219(4) 0.405(4) 0.066 Uiso 0.45 1 d P B 2 H30D H 0.542(6) -0.219(4) 0.451(4) 0.066 Uiso 0.45 1 d P C 2 C31 C 0.6675(10) -0.2504(10) 0.3968(8) 0.049(3) Uani 0.55 1 d PD D 1 H31A H 0.6363 -0.2671 0.3589 0.059 Uiso 0.55 1 calc PR D 1 H31B H 0.6937 -0.2852 0.4221 0.059 Uiso 0.55 1 calc PR D 1 C31A C 0.6871(10) -0.2390(10) 0.4072(9) 0.039(4) Uani 0.45 1 d PD D 2 H31C H 0.6697 -0.2593 0.3677 0.047 Uiso 0.45 1 calc PR D 2 H31D H 0.7098 -0.2719 0.4361 0.047 Uiso 0.45 1 calc PR D 2 C32 C 0.7460(11) -0.2015(6) 0.3829(8) 0.077(6) Uani 0.55 1 d PD D 1 H32A H 0.8033 -0.2081 0.4106 0.092 Uiso 0.55 1 calc PR D 1 H32B H 0.7694 -0.2071 0.3399 0.092 Uiso 0.55 1 calc PR D 1 C32A C 0.7687(15) -0.1945(7) 0.3968(11) 0.073(6) Uani 0.45 1 d PD D 2 H32C H 0.8171 -0.1942 0.4311 0.087 Uiso 0.45 1 calc PR D 2 H32D H 0.8034 -0.2020 0.3572 0.087 Uiso 0.45 1 calc PR D 2 C33 C 0.7088(6) -0.1356(6) 0.3907(5) 0.059(5) Uani 0.55 1 d PD D 1 H33A H 0.7478 -0.1128 0.4222 0.071 Uiso 0.55 1 calc PR D 1 H33B H 0.7111 -0.1123 0.3513 0.071 Uiso 0.55 1 calc PR D 1 C33A C 0.7090(8) -0.1386(6) 0.3953(10) 0.103(9) Uani 0.45 1 d PD D 2 H33C H 0.7388 -0.1078 0.4239 0.123 Uiso 0.45 1 calc PR D 2 H33D H 0.7129 -0.1207 0.3532 0.123 Uiso 0.45 1 calc PR D 2 H1A H 0.4399(16) 0.0623(10) 0.4069(6) 0.021(6) Uiso 1 1 d D . . H1B H 0.4472(17) 0.1090(7) 0.4669(10) 0.029(7) Uiso 1 1 d D . . 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 Sr1 0.02741(12) 0.02496(13) 0.01804(12) -0.00111(10) 0.00201(9) -0.00113(10) O1 0.0398(11) 0.0348(11) 0.0351(11) 0.0057(9) 0.0058(8) 0.0058(9) N1 0.0236(10) 0.0270(12) 0.0190(10) -0.0041(9) -0.0014(8) 0.0000(9) N2 0.0252(10) 0.0278(11) 0.0175(10) -0.0006(9) -0.0011(8) -0.0013(9) C1 0.0271(13) 0.0268(13) 0.0204(12) -0.0037(10) 0.0002(10) 0.0024(11) C2 0.0280(12) 0.0217(13) 0.0173(12) 0.0013(10) -0.0002(9) -0.0016(10) C3 0.0234(12) 0.0284(14) 0.0170(12) -0.0018(10) 0.0000(10) 0.0000(10) C4 0.0273(13) 0.0210(13) 0.0213(13) 0.0001(10) 0.0021(10) 0.0003(10) C5 0.0279(13) 0.0350(15) 0.0227(13) -0.0030(11) 0.0022(10) -0.0014(11) C6 0.0258(12) 0.0287(14) 0.0162(12) -0.0061(10) 0.0026(9) -0.0019(10) C7 0.0265(13) 0.0329(15) 0.0226(13) -0.0033(11) -0.0024(10) -0.0018(11) C8 0.0271(13) 0.0406(17) 0.0326(15) -0.0049(13) -0.0051(11) -0.0001(12) C9 0.0264(14) 0.0407(17) 0.0391(16) -0.0113(13) 0.0020(12) -0.0062(12) C10 0.0381(15) 0.0295(15) 0.0309(15) -0.0061(12) 0.0075(12) -0.0081(12) C11 0.0319(13) 0.0281(14) 0.0229(13) -0.0050(11) 0.0020(11) -0.0026(11) C12 0.0287(14) 0.0418(17) 0.0350(16) 0.0070(13) -0.0060(11) -0.0048(12) C13 0.121(4) 0.119(4) 0.030(2) 0.006(2) 0.005(2) -0.066(3) C14 0.051(2) 0.047(2) 0.111(3) 0.027(2) 0.006(2) 0.0037(17) C15 0.0391(15) 0.0338(16) 0.0361(16) 0.0057(13) -0.0002(12) -0.0041(13) C16 0.109(3) 0.074(3) 0.074(3) -0.020(2) -0.031(3) 0.053(3) C17 0.086(3) 0.069(3) 0.045(2) 0.0135(19) -0.0030(18) 0.013(2) C18 0.0201(11) 0.0304(13) 0.0189(12) -0.0017(10) 0.0003(9) -0.0021(10) C19 0.0241(12) 0.0349(15) 0.0296(14) 0.0020(12) -0.0028(10) -0.0007(11) C20 0.0272(14) 0.0508(19) 0.0302(15) 0.0112(14) -0.0033(11) -0.0009(13) C21 0.0263(13) 0.069(2) 0.0191(14) -0.0017(14) -0.0033(11) -0.0033(14) C22 0.0309(14) 0.0470(18) 0.0268(14) -0.0106(13) -0.0030(11) -0.0042(13) C23 0.0275(13) 0.0332(15) 0.0252(13) -0.0043(11) -0.0010(10) -0.0023(11) C24 0.0519(18) 0.0313(16) 0.0417(17) 0.0037(13) -0.0128(14) 0.0029(14) C25 0.073(2) 0.050(2) 0.062(2) -0.0091(18) -0.0049(19) 0.0220(18) C26 0.085(3) 0.0388(19) 0.082(3) 0.015(2) -0.007(2) -0.0104(19) C27 0.0491(17) 0.0317(15) 0.0315(15) -0.0077(12) -0.0055(13) 0.0022(13) C28 0.071(2) 0.047(2) 0.069(2) -0.0030(19) 0.0080(19) 0.0159(18) C29 0.064(2) 0.064(2) 0.099(3) 0.034(2) 0.018(2) 0.001(2) C30 0.055(2) 0.0371(18) 0.073(3) 0.0141(19) 0.0132(19) 0.0033(16) C31 0.091(8) 0.030(6) 0.027(6) -0.017(4) -0.007(5) 0.003(5) C31A 0.064(7) 0.029(9) 0.025(7) -0.011(5) -0.010(5) 0.009(6) C32 0.054(8) 0.097(9) 0.078(8) 0.031(6) 0.036(8) 0.053(7) C32A 0.045(8) 0.080(9) 0.093(11) 0.068(8) 0.002(6) 0.004(5) C33 0.027(7) 0.102(11) 0.049(5) -0.010(5) 0.008(4) 0.006(6) C33A 0.044(11) 0.013(6) 0.25(2) 0.002(8) 0.033(10) -0.006(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sr1 N1 2.5104(19) 5_656 ? Sr1 O1 2.5535(18) . ? Sr1 N2 2.567(2) . ? Sr1 C1 2.759(3) . ? Sr1 C1 2.815(3) 5_656 ? Sr1 C3 2.911(2) . ? Sr1 C2 2.959(2) 5_656 ? Sr1 C2 2.982(2) . ? Sr1 H1A 2.63(2) . ? O1 C33A 1.413(10) . ? O1 C33 1.444(8) . ? O1 C30 1.444(4) . ? N1 C2 1.366(3) . ? N1 C6 1.418(3) . ? N1 Sr1 2.5104(19) 5_656 ? N2 C4 1.335(3) . ? N2 C18 1.425(3) . ? C1 C2 1.419(3) . ? C1 Sr1 2.815(3) 5_656 ? C1 H1A 0.980(3) . ? C1 H1B 0.980(3) . ? C2 C3 1.458(3) . ? C2 Sr1 2.959(2) 5_656 ? C3 C4 1.411(3) . ? C3 H3 0.980(3) . ? C4 C5 1.516(3) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.414(3) . ? C6 C11 1.418(3) . ? C7 C8 1.396(3) . ? C7 C12 1.514(4) . ? C8 C9 1.373(4) . ? C8 H8 0.9500 . ? C9 C10 1.385(4) . ? C9 H9 0.9500 . ? C10 C11 1.389(4) . ? C10 H10 0.9500 . ? C11 C15 1.518(4) . ? C12 C13 1.509(4) . ? C12 C14 1.533(4) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.526(5) . ? C15 C17 1.528(4) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C23 1.404(3) . ? C18 C19 1.404(4) . ? C19 C20 1.404(4) . ? C19 C24 1.518(4) . ? C20 C21 1.375(4) . ? C20 H20 0.9500 . ? C21 C22 1.378(4) . ? C21 H21 0.9500 . ? C22 C23 1.392(4) . ? C22 H22 0.9500 . ? C23 C27 1.514(4) . ? C24 C26 1.524(5) . ? C24 C25 1.526(4) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C29 1.507(4) . ? C27 C28 1.523(4) . ? C27 H27 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31A 1.472(15) . ? C30 C31 1.510(14) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C30 H30C 0.99(8) . ? C30 H30D 0.87(8) . ? C31 C32 1.520(14) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C31A C32A 1.475(17) . ? C31A H31C 0.9900 . ? C31A H31D 0.9900 . ? C32 C33 1.508(13) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C32A C33A 1.443(17) . ? C32A H32C 0.9900 . ? C32A H32D 0.9900 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C33A H33C 0.9900 . ? C33A H33D 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Sr1 O1 103.17(6) 5_656 . ? N1 Sr1 N2 147.38(6) 5_656 . ? O1 Sr1 N2 99.13(6) . . ? N1 Sr1 C1 102.27(7) 5_656 . ? O1 Sr1 C1 144.61(7) . . ? N2 Sr1 C1 70.50(7) . . ? N1 Sr1 C1 52.60(7) 5_656 5_656 ? O1 Sr1 C1 85.68(7) . 5_656 ? N2 Sr1 C1 153.75(7) . 5_656 ? C1 Sr1 C1 90.61(7) . 5_656 ? N1 Sr1 C3 147.51(6) 5_656 . ? O1 Sr1 C3 93.49(6) . . ? N2 Sr1 C3 52.02(6) . . ? C1 Sr1 C3 52.95(7) . . ? C1 Sr1 C3 102.15(7) 5_656 . ? N1 Sr1 C2 27.38(6) 5_656 5_656 ? O1 Sr1 C2 103.96(6) . 5_656 ? N2 Sr1 C2 156.54(6) . 5_656 ? C1 Sr1 C2 88.02(7) . 5_656 ? C1 Sr1 C2 28.32(7) 5_656 5_656 ? C3 Sr1 C2 121.55(6) . 5_656 ? N1 Sr1 C2 120.29(6) 5_656 . ? O1 Sr1 C2 116.34(6) . . ? N2 Sr1 C2 68.14(6) . . ? C1 Sr1 C2 28.28(7) . . ? C1 Sr1 C2 86.53(7) 5_656 . ? C3 Sr1 C2 28.61(7) . . ? C2 Sr1 C2 97.43(6) 5_656 . ? N1 Sr1 H1A 107.6(5) 5_656 . ? O1 Sr1 H1A 148.9(5) . . ? N2 Sr1 H1A 55.2(4) . . ? C1 Sr1 H1A 20.78(7) . . ? C1 Sr1 H1A 110.0(2) 5_656 . ? C3 Sr1 H1A 57.7(5) . . ? C2 Sr1 H1A 101.6(4) 5_656 . ? C2 Sr1 H1A 42.2(3) . . ? C33A O1 C33 4.5(12) . . ? C33A O1 C30 105.4(6) . . ? C33 O1 C30 108.8(5) . . ? C33A O1 Sr1 124.4(5) . . ? C33 O1 Sr1 121.9(5) . . ? C30 O1 Sr1 127.55(17) . . ? C2 N1 C6 119.72(19) . . ? C2 N1 Sr1 94.92(14) . 5_656 ? C6 N1 Sr1 137.19(15) . 5_656 ? C4 N2 C18 117.64(19) . . ? C4 N2 Sr1 93.57(14) . . ? C18 N2 Sr1 140.83(15) . . ? C2 C1 Sr1 84.65(15) . . ? C2 C1 Sr1 81.50(14) . 5_656 ? Sr1 C1 Sr1 89.39(7) . 5_656 ? C2 C1 H1A 115.8(14) . . ? Sr1 C1 H1A 72.3(14) . . ? Sr1 C1 H1A 152.6(14) 5_656 . ? C2 C1 H1B 113.7(15) . . ? Sr1 C1 H1B 151.8(15) . . ? Sr1 C1 H1B 73.4(15) 5_656 . ? H1A C1 H1B 114(2) . . ? N1 C2 C1 117.0(2) . . ? N1 C2 C3 119.4(2) . . ? C1 C2 C3 123.2(2) . . ? N1 C2 Sr1 57.71(12) . 5_656 ? C1 C2 Sr1 70.18(14) . 5_656 ? C3 C2 Sr1 141.29(16) . 5_656 ? N1 C2 Sr1 130.32(16) . . ? C1 C2 Sr1 67.07(14) . . ? C3 C2 Sr1 72.96(13) . . ? Sr1 C2 Sr1 82.57(6) 5_656 . ? C4 C3 C2 129.2(2) . . ? C4 C3 Sr1 78.30(14) . . ? C2 C3 Sr1 78.43(13) . . ? C4 C3 H3 115.5(15) . . ? C2 C3 H3 113.3(15) . . ? Sr1 C3 H3 133.5(15) . . ? N2 C4 C3 123.7(2) . . ? N2 C4 C5 119.9(2) . . ? C3 C4 C5 116.4(2) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 N1 120.4(2) . . ? C7 C6 C11 119.3(2) . . ? N1 C6 C11 120.1(2) . . ? C8 C7 C6 119.2(2) . . ? C8 C7 C12 120.4(2) . . ? C6 C7 C12 120.4(2) . . ? C9 C8 C7 121.2(3) . . ? C9 C8 H8 119.4 . . ? C7 C8 H8 119.4 . . ? C8 C9 C10 119.7(2) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? C9 C10 C11 121.4(3) . . ? C9 C10 H10 119.3 . . ? C11 C10 H10 119.3 . . ? C10 C11 C6 119.0(2) . . ? C10 C11 C15 120.3(2) . . ? C6 C11 C15 120.7(2) . . ? C13 C12 C7 111.0(3) . . ? C13 C12 C14 110.9(3) . . ? C7 C12 C14 113.0(2) . . ? C13 C12 H12 107.2 . . ? C7 C12 H12 107.2 . . ? C14 C12 H12 107.2 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 C16 112.2(2) . . ? C11 C15 C17 112.2(3) . . ? C16 C15 C17 109.0(3) . . ? C11 C15 H15 107.8 . . ? C16 C15 H15 107.8 . . ? C17 C15 H15 107.8 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C23 C18 C19 120.1(2) . . ? C23 C18 N2 120.8(2) . . ? C19 C18 N2 119.0(2) . . ? C20 C19 C18 118.4(2) . . ? C20 C19 C24 120.3(2) . . ? C18 C19 C24 121.3(2) . . ? C21 C20 C19 121.4(3) . . ? C21 C20 H20 119.3 . . ? C19 C20 H20 119.3 . . ? C20 C21 C22 119.6(2) . . ? C20 C21 H21 120.2 . . ? C22 C21 H21 120.2 . . ? C21 C22 C23 121.1(3) . . ? C21 C22 H22 119.4 . . ? C23 C22 H22 119.4 . . ? C22 C23 C18 119.2(2) . . ? C22 C23 C27 119.8(2) . . ? C18 C23 C27 120.9(2) . . ? C19 C24 C26 112.3(3) . . ? C19 C24 C25 110.2(3) . . ? C26 C24 C25 111.8(3) . . ? C19 C24 H24 107.4 . . ? C26 C24 H24 107.4 . . ? C25 C24 H24 107.4 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C29 C27 C23 112.6(2) . . ? C29 C27 C28 111.0(3) . . ? C23 C27 C28 112.8(2) . . ? C29 C27 H27 106.7 . . ? C23 C27 H27 106.7 . . ? C28 C27 H27 106.7 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O1 C30 C31A 102.4(9) . . ? O1 C30 C31 109.2(9) . . ? C31A C30 C31 16.3(8) . . ? O1 C30 H30A 109.8 . . ? C31A C30 H30A 126.0 . . ? C31 C30 H30A 109.8 . . ? O1 C30 H30B 109.8 . . ? C31A C30 H30B 99.5 . . ? C31 C30 H30B 109.8 . . ? H30A C30 H30B 108.3 . . ? O1 C30 H30C 94(5) . . ? C31A C30 H30C 107(5) . . ? C31 C30 H30C 92(5) . . ? H30A C30 H30C 31.3 . . ? H30B C30 H30C 139.5 . . ? O1 C30 H30D 118(5) . . ? C31A C30 H30D 139(5) . . ? C31 C30 H30D 127(5) . . ? H30A C30 H30D 32.9 . . ? H30B C30 H30D 75.7 . . ? H30C C30 H30D 64(6) . . ? C30 C31 C32 97.3(10) . . ? C30 C31 H31A 112.3 . . ? C32 C31 H31A 112.3 . . ? C30 C31 H31B 112.3 . . ? C32 C31 H31B 112.3 . . ? H31A C31 H31B 109.9 . . ? C30 C31A C32A 112.4(13) . . ? C30 C31A H31C 109.1 . . ? C32A C31A H31C 109.1 . . ? C30 C31A H31D 109.1 . . ? C32A C31A H31D 109.1 . . ? H31C C31A H31D 107.8 . . ? C33 C32 C31 113.1(10) . . ? C33 C32 H32A 109.0 . . ? C31 C32 H32A 109.0 . . ? C33 C32 H32B 109.0 . . ? C31 C32 H32B 109.0 . . ? H32A C32 H32B 107.8 . . ? C33A C32A C31A 97.2(13) . . ? C33A C32A H32C 112.3 . . ? C31A C32A H32C 112.3 . . ? C33A C32A H32D 112.3 . . ? C31A C32A H32D 112.3 . . ? H32C C32A H32D 109.9 . . ? O1 C33 C32 102.1(8) . . ? O1 C33 H33A 111.3 . . ? C32 C33 H33A 111.3 . . ? O1 C33 H33B 111.3 . . ? C32 C33 H33B 111.3 . . ? H33A C33 H33B 109.2 . . ? O1 C33A C32A 116.5(10) . . ? O1 C33A H33C 108.2 . . ? C32A C33A H33C 108.2 . . ? O1 C33A H33D 108.2 . . ? C32A C33A H33D 108.2 . . ? H33C C33A H33D 107.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Sr1 O1 C33A -148.0(11) 5_656 . . . ? N2 Sr1 O1 C33A 56.0(11) . . . . ? C1 Sr1 O1 C33A -13.1(11) . . . . ? C1 Sr1 O1 C33A -98.0(11) 5_656 . . . ? C3 Sr1 O1 C33A 3.9(11) . . . . ? C2 Sr1 O1 C33A -119.9(11) 5_656 . . . ? C2 Sr1 O1 C33A -14.1(11) . . . . ? N1 Sr1 O1 C33 -152.5(5) 5_656 . . . ? N2 Sr1 O1 C33 51.5(5) . . . . ? C1 Sr1 O1 C33 -17.5(5) . . . . ? C1 Sr1 O1 C33 -102.5(5) 5_656 . . . ? C3 Sr1 O1 C33 -0.6(5) . . . . ? C2 Sr1 O1 C33 -124.3(5) 5_656 . . . ? C2 Sr1 O1 C33 -18.5(5) . . . . ? N1 Sr1 O1 C30 10.9(3) 5_656 . . . ? N2 Sr1 O1 C30 -145.1(3) . . . . ? C1 Sr1 O1 C30 145.8(3) . . . . ? C1 Sr1 O1 C30 60.9(3) 5_656 . . . ? C3 Sr1 O1 C30 162.8(3) . . . . ? C2 Sr1 O1 C30 39.1(3) 5_656 . . . ? C2 Sr1 O1 C30 144.8(3) . . . . ? N1 Sr1 N2 C4 158.80(14) 5_656 . . . ? O1 Sr1 N2 C4 -68.42(14) . . . . ? C1 Sr1 N2 C4 76.56(15) . . . . ? C1 Sr1 N2 C4 30.4(2) 5_656 . . . ? C3 Sr1 N2 C4 18.87(13) . . . . ? C2 Sr1 N2 C4 101.32(19) 5_656 . . . ? C2 Sr1 N2 C4 46.39(14) . . . . ? N1 Sr1 N2 C18 -56.9(3) 5_656 . . . ? O1 Sr1 N2 C18 75.9(2) . . . . ? C1 Sr1 N2 C18 -139.1(2) . . . . ? C1 Sr1 N2 C18 174.7(2) 5_656 . . . ? C3 Sr1 N2 C18 163.2(3) . . . . ? C2 Sr1 N2 C18 -114.3(3) 5_656 . . . ? C2 Sr1 N2 C18 -169.3(3) . . . . ? N1 Sr1 C1 C2 133.25(14) 5_656 . . . ? O1 Sr1 C1 C2 -1.9(2) . . . . ? N2 Sr1 C1 C2 -79.88(14) . . . . ? C1 Sr1 C1 C2 81.52(14) 5_656 . . . ? C3 Sr1 C1 C2 -23.30(13) . . . . ? C2 Sr1 C1 C2 109.72(13) 5_656 . . . ? N1 Sr1 C1 Sr1 51.74(7) 5_656 . . 5_656 ? O1 Sr1 C1 Sr1 -83.39(12) . . . 5_656 ? N2 Sr1 C1 Sr1 -161.40(8) . . . 5_656 ? C1 Sr1 C1 Sr1 0.0 5_656 . . 5_656 ? C3 Sr1 C1 Sr1 -104.81(9) . . . 5_656 ? C2 Sr1 C1 Sr1 28.21(7) 5_656 . . 5_656 ? C2 Sr1 C1 Sr1 -81.52(14) . . . 5_656 ? C6 N1 C2 C1 -166.9(2) . . . . ? Sr1 N1 C2 C1 39.4(2) 5_656 . . . ? C6 N1 C2 C3 19.1(3) . . . . ? Sr1 N1 C2 C3 -134.7(2) 5_656 . . . ? C6 N1 C2 Sr1 153.8(2) . . . 5_656 ? C6 N1 C2 Sr1 111.2(2) . . . . ? Sr1 N1 C2 Sr1 -42.53(19) 5_656 . . . ? Sr1 C1 C2 N1 -124.9(2) . . . . ? Sr1 C1 C2 N1 -34.8(2) 5_656 . . . ? Sr1 C1 C2 C3 48.9(2) . . . . ? Sr1 C1 C2 C3 139.1(2) 5_656 . . . ? Sr1 C1 C2 Sr1 -90.18(6) . . . 5_656 ? Sr1 C1 C2 Sr1 90.18(6) 5_656 . . . ? N1 Sr1 C2 N1 51.3(2) 5_656 . . . ? O1 Sr1 C2 N1 -74.4(2) . . . . ? N2 Sr1 C2 N1 -164.0(2) . . . . ? C1 Sr1 C2 N1 106.8(3) . . . . ? C1 Sr1 C2 N1 9.0(2) 5_656 . . . ? C3 Sr1 C2 N1 -114.5(3) . . . . ? C2 Sr1 C2 N1 35.19(17) 5_656 . . . ? N1 Sr1 C2 C1 -55.51(16) 5_656 . . . ? O1 Sr1 C2 C1 178.79(13) . . . . ? N2 Sr1 C2 C1 89.24(15) . . . . ? C1 Sr1 C2 C1 -97.77(14) 5_656 . . . ? C3 Sr1 C2 C1 138.8(2) . . . . ? C2 Sr1 C2 C1 -71.58(14) 5_656 . . . ? N1 Sr1 C2 C3 165.73(12) 5_656 . . . ? O1 Sr1 C2 C3 40.03(15) . . . . ? N2 Sr1 C2 C3 -49.52(13) . . . . ? C1 Sr1 C2 C3 -138.8(2) . . . . ? C1 Sr1 C2 C3 123.47(14) 5_656 . . . ? C2 Sr1 C2 C3 149.66(16) 5_656 . . . ? N1 Sr1 C2 Sr1 16.07(8) 5_656 . . 5_656 ? O1 Sr1 C2 Sr1 -109.63(6) . . . 5_656 ? N2 Sr1 C2 Sr1 160.82(8) . . . 5_656 ? C1 Sr1 C2 Sr1 71.58(14) . . . 5_656 ? C1 Sr1 C2 Sr1 -26.19(6) 5_656 . . 5_656 ? C3 Sr1 C2 Sr1 -149.66(16) . . . 5_656 ? C2 Sr1 C2 Sr1 0.0 5_656 . . 5_656 ? N1 C2 C3 C4 -168.6(2) . . . . ? C1 C2 C3 C4 17.7(4) . . . . ? Sr1 C2 C3 C4 117.5(3) 5_656 . . . ? Sr1 C2 C3 C4 64.2(2) . . . . ? N1 C2 C3 Sr1 127.2(2) . . . . ? C1 C2 C3 Sr1 -46.5(2) . . . . ? Sr1 C2 C3 Sr1 53.2(2) 5_656 . . . ? N1 Sr1 C3 C4 -157.93(13) 5_656 . . . ? O1 Sr1 C3 C4 80.69(14) . . . . ? N2 Sr1 C3 C4 -18.17(13) . . . . ? C1 Sr1 C3 C4 -111.54(16) . . . . ? C1 Sr1 C3 C4 167.02(14) 5_656 . . . ? C2 Sr1 C3 C4 -170.58(13) 5_656 . . . ? C2 Sr1 C3 C4 -134.6(2) . . . . ? N1 Sr1 C3 C2 -23.3(2) 5_656 . . . ? O1 Sr1 C3 C2 -144.73(13) . . . . ? N2 Sr1 C3 C2 116.41(16) . . . . ? C1 Sr1 C3 C2 23.04(13) . . . . ? C1 Sr1 C3 C2 -58.40(14) 5_656 . . . ? C2 Sr1 C3 C2 -36.00(18) 5_656 . . . ? C18 N2 C4 C3 165.4(2) . . . . ? Sr1 N2 C4 C3 -39.2(2) . . . . ? C18 N2 C4 C5 -16.4(3) . . . . ? Sr1 N2 C4 C5 139.1(2) . . . . ? C2 C3 C4 N2 -29.7(4) . . . . ? Sr1 C3 C4 N2 34.6(2) . . . . ? C2 C3 C4 C5 152.0(2) . . . . ? Sr1 C3 C4 C5 -143.7(2) . . . . ? C2 N1 C6 C7 -110.2(3) . . . . ? Sr1 N1 C6 C7 29.4(3) 5_656 . . . ? C2 N1 C6 C11 74.0(3) . . . . ? Sr1 N1 C6 C11 -146.44(19) 5_656 . . . ? N1 C6 C7 C8 -172.4(2) . . . . ? C11 C6 C7 C8 3.4(4) . . . . ? N1 C6 C7 C12 7.9(4) . . . . ? C11 C6 C7 C12 -176.2(2) . . . . ? C6 C7 C8 C9 -1.8(4) . . . . ? C12 C7 C8 C9 177.8(2) . . . . ? C7 C8 C9 C10 -0.8(4) . . . . ? C8 C9 C10 C11 1.8(4) . . . . ? C9 C10 C11 C6 -0.2(4) . . . . ? C9 C10 C11 C15 179.8(2) . . . . ? C7 C6 C11 C10 -2.5(4) . . . . ? N1 C6 C11 C10 173.4(2) . . . . ? C7 C6 C11 C15 177.5(2) . . . . ? N1 C6 C11 C15 -6.6(4) . . . . ? C8 C7 C12 C13 77.0(4) . . . . ? C6 C7 C12 C13 -103.3(3) . . . . ? C8 C7 C12 C14 -48.3(4) . . . . ? C6 C7 C12 C14 131.4(3) . . . . ? C10 C11 C15 C16 -67.5(4) . . . . ? C6 C11 C15 C16 112.6(3) . . . . ? C10 C11 C15 C17 55.7(4) . . . . ? C6 C11 C15 C17 -124.3(3) . . . . ? C4 N2 C18 C23 103.2(3) . . . . ? Sr1 N2 C18 C23 -35.7(4) . . . . ? C4 N2 C18 C19 -77.7(3) . . . . ? Sr1 N2 C18 C19 143.3(2) . . . . ? C23 C18 C19 C20 0.3(4) . . . . ? N2 C18 C19 C20 -178.7(2) . . . . ? C23 C18 C19 C24 180.0(2) . . . . ? N2 C18 C19 C24 1.0(4) . . . . ? C18 C19 C20 C21 0.5(4) . . . . ? C24 C19 C20 C21 -179.2(3) . . . . ? C19 C20 C21 C22 -0.7(4) . . . . ? C20 C21 C22 C23 0.1(4) . . . . ? C21 C22 C23 C18 0.6(4) . . . . ? C21 C22 C23 C27 -175.9(2) . . . . ? C19 C18 C23 C22 -0.8(4) . . . . ? N2 C18 C23 C22 178.2(2) . . . . ? C19 C18 C23 C27 175.7(2) . . . . ? N2 C18 C23 C27 -5.3(4) . . . . ? C20 C19 C24 C26 -43.5(4) . . . . ? C18 C19 C24 C26 136.9(3) . . . . ? C20 C19 C24 C25 81.9(3) . . . . ? C18 C19 C24 C25 -97.8(3) . . . . ? C22 C23 C27 C29 -81.2(3) . . . . ? C18 C23 C27 C29 102.3(3) . . . . ? C22 C23 C27 C28 45.3(4) . . . . ? C18 C23 C27 C28 -131.2(3) . . . . ? C33A O1 C30 C31A -19.4(12) . . . . ? C33 O1 C30 C31A -16.4(8) . . . . ? Sr1 O1 C30 C31A 178.5(7) . . . . ? C33A O1 C30 C31 -34.9(11) . . . . ? C33 O1 C30 C31 -31.9(8) . . . . ? Sr1 O1 C30 C31 163.0(6) . . . . ? O1 C30 C31 C32 29.1(12) . . . . ? C31A C30 C31 C32 -39(6) . . . . ? O1 C30 C31A C32A 26.3(17) . . . . ? C31 C30 C31A C32A 143(8) . . . . ? C30 C31 C32 C33 -18.2(16) . . . . ? C30 C31A C32A C33A -21(2) . . . . ? C33A O1 C33 C32 59(14) . . . . ? C30 O1 C33 C32 17.9(10) . . . . ? Sr1 O1 C33 C32 -175.9(8) . . . . ? C31 C32 C33 O1 1.3(16) . . . . ? C33 O1 C33A C32A -132(15) . . . . ? C30 O1 C33A C32A 8(2) . . . . ? Sr1 O1 C33A C32A 170.7(13) . . . . ? C31A C32A C33A O1 7(2) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.393 _refine_diff_density_min -0.474 _refine_diff_density_rms 0.064 # Attachment 'Compound_10.cif' data_c:\x-ray\kappa\k08msh68\maxus2\k08msh68 _database_code_depnum_ccdc_archive 'CCDC 727088' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H108 Ba2 N4 O2' _chemical_formula_weight 1408.36 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' Ba Ba -0.3244 2.2819 '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/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.7330(2) _cell_length_b 24.2770(3) _cell_length_c 13.0420(2) _cell_angle_alpha 90.00 _cell_angle_beta 114.635(1) _cell_angle_gamma 90.00 _cell_volume 3664.59(9) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 156903 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 30.034 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.276 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1464 _exptl_absorpt_coefficient_mu 1.114 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.66 _exptl_absorpt_correction_T_max 0.72 _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 62937 _diffrn_reflns_av_R_equivalents 0.0454 _diffrn_reflns_av_sigmaI/netI 0.0380 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.76 _diffrn_reflns_theta_max 30.06 _reflns_number_total 10568 _reflns_number_gt 8426 _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^)+(0.0192P)^2^+3.2370P] 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 10568 _refine_ls_number_parameters 416 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0498 _refine_ls_R_factor_gt 0.0326 _refine_ls_wR_factor_ref 0.0723 _refine_ls_wR_factor_gt 0.0660 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.003 _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 Ba1 Ba 0.663322(10) 0.462878(5) 0.594556(10) 0.02377(4) Uani 1 1 d . . . O1 O 0.74749(18) 0.39689(7) 0.47594(15) 0.0488(5) Uani 1 1 d . . . N1 N 0.31251(15) 0.43038(7) 0.43918(14) 0.0245(3) Uani 1 1 d . . . N2 N 0.63612(14) 0.38680(7) 0.73862(13) 0.0232(3) Uani 1 1 d . . . C1 C 0.44003(19) 0.46808(8) 0.61491(17) 0.0256(4) Uani 1 1 d D . . C2 C 0.41016(17) 0.42428(8) 0.53675(16) 0.0234(4) Uani 1 1 d . . . C3 C 0.48212(18) 0.37557(8) 0.55211(17) 0.0245(4) Uani 1 1 d . . . H3 H 0.4684 0.3550 0.4858 0.029 Uiso 1 1 calc R . . C4 C 0.56912(18) 0.35508(8) 0.65220(17) 0.0241(4) Uani 1 1 d . . . C5 C 0.5879(2) 0.29298(8) 0.65778(19) 0.0312(5) Uani 1 1 d . . . H5A H 0.6709 0.2851 0.6923 0.047 Uiso 1 1 calc R . . H5B H 0.5534 0.2776 0.5814 0.047 Uiso 1 1 calc R . . H5C H 0.5514 0.2763 0.7032 0.047 Uiso 1 1 calc R . . C6 C 0.26411(18) 0.38472(8) 0.36801(17) 0.0278(4) Uani 1 1 d . . . C7 C 0.2029(2) 0.34421(9) 0.39914(19) 0.0341(5) Uani 1 1 d . . . C8 C 0.1478(2) 0.30177(9) 0.3233(2) 0.0393(6) Uani 1 1 d . . . H8 H 0.1067 0.2744 0.3439 0.047 Uiso 1 1 calc R . . C9 C 0.1514(2) 0.29859(9) 0.2195(2) 0.0396(6) Uani 1 1 d . . . H9 H 0.1129 0.2695 0.1690 0.047 Uiso 1 1 calc R . . C10 C 0.2116(2) 0.33804(10) 0.1892(2) 0.0379(5) Uani 1 1 d . . . H10 H 0.2142 0.3357 0.1176 0.045 Uiso 1 1 calc R . . C11 C 0.26844(18) 0.38111(9) 0.26182(18) 0.0300(5) Uani 1 1 d . . . C12 C 0.1978(3) 0.34486(12) 0.5128(2) 0.0540(8) Uani 1 1 d . . . H12 H 0.2356 0.3795 0.5528 0.065 Uiso 1 1 calc R . . C13 C 0.2645(3) 0.29577(18) 0.5844(3) 0.0853(14) Uani 1 1 d . . . H13A H 0.2290 0.2614 0.5465 0.128 Uiso 1 1 calc R . . H13B H 0.2620 0.2973 0.6585 0.128 Uiso 1 1 calc R . . H13C H 0.3450 0.2973 0.5941 0.128 Uiso 1 1 calc R . . C14 C 0.0735(3) 0.34404(13) 0.5025(3) 0.0602(8) Uani 1 1 d . . . H14A H 0.0300 0.3746 0.4543 0.090 Uiso 1 1 calc R . . H14B H 0.0741 0.3480 0.5776 0.090 Uiso 1 1 calc R . . H14C H 0.0369 0.3090 0.4691 0.090 Uiso 1 1 calc R . . C15 C 0.3312(2) 0.42506(10) 0.2263(2) 0.0372(5) Uani 1 1 d . . . H15 H 0.3908 0.4416 0.2967 0.045 Uiso 1 1 calc R . . C16 C 0.2479(3) 0.47103(12) 0.1621(2) 0.0471(7) Uani 1 1 d D . . C17 C 0.3942(3) 0.40365(15) 0.1569(3) 0.0670(9) Uani 1 1 d . . . H17A H 0.4430 0.3723 0.1958 0.100 Uiso 1 1 calc R . . H17B H 0.4425 0.4330 0.1479 0.100 Uiso 1 1 calc R . . H17C H 0.3375 0.3919 0.0825 0.100 Uiso 1 1 calc R . . C18 C 0.69765(18) 0.36095(8) 0.84554(16) 0.0247(4) Uani 1 1 d . . . C19 C 0.63665(19) 0.34579(9) 0.90988(18) 0.0293(4) Uani 1 1 d . . . C20 C 0.6973(2) 0.32146(10) 1.01548(19) 0.0351(5) Uani 1 1 d . . . H20 H 0.6565 0.3106 1.0588 0.042 Uiso 1 1 calc R . . C21 C 0.8148(2) 0.31283(10) 1.05822(19) 0.0386(6) Uani 1 1 d . . . H21 H 0.8543 0.2958 1.1298 0.046 Uiso 1 1 calc R . . C22 C 0.8743(2) 0.32903(9) 0.99640(19) 0.0350(5) Uani 1 1 d . . . H22 H 0.9556 0.3238 1.0267 0.042 Uiso 1 1 calc R . . C23 C 0.81770(19) 0.35310(9) 0.88965(17) 0.0280(4) Uani 1 1 d . . . C24 C 0.5099(2) 0.36009(11) 0.8714(2) 0.0399(6) Uani 1 1 d . . . H24 H 0.4749 0.3626 0.7872 0.048 Uiso 1 1 calc R . . C25 C 0.4407(3) 0.31741(14) 0.9042(3) 0.0572(8) Uani 1 1 d . . . H25A H 0.4508 0.2810 0.8773 0.086 Uiso 1 1 calc R . . H25B H 0.3587 0.3274 0.8700 0.086 Uiso 1 1 calc R . . H25C H 0.4685 0.3166 0.9865 0.086 Uiso 1 1 calc R . . C26 C 0.5007(3) 0.41709(13) 0.9175(3) 0.0572(8) Uani 1 1 d . . . H26A H 0.5346 0.4159 1.0001 0.086 Uiso 1 1 calc R . . H26B H 0.4193 0.4278 0.8892 0.086 Uiso 1 1 calc R . . H26C H 0.5425 0.4441 0.8926 0.086 Uiso 1 1 calc R . . C27 C 0.8895(2) 0.37103(10) 0.8277(2) 0.0372(5) Uani 1 1 d . . . H27 H 0.8364 0.3871 0.7536 0.045 Uiso 1 1 calc R . . C28 C 0.9542(3) 0.32225(14) 0.8049(3) 0.0568(8) Uani 1 1 d . . . H28A H 1.0098 0.3072 0.8768 0.085 Uiso 1 1 calc R . . H28B H 0.9953 0.3350 0.7603 0.085 Uiso 1 1 calc R . . H28C H 0.8987 0.2936 0.7631 0.085 Uiso 1 1 calc R . . C29 C 0.9770(3) 0.41560(12) 0.8950(3) 0.0534(7) Uani 1 1 d . . . H29A H 0.9361 0.4463 0.9111 0.080 Uiso 1 1 calc R . . H29B H 1.0178 0.4290 0.8507 0.080 Uiso 1 1 calc R . . H29C H 1.0328 0.3999 0.9661 0.080 Uiso 1 1 calc R . . C30 C 0.7576(3) 0.33902(12) 0.4954(3) 0.0606(8) Uani 1 1 d . . . H30A H 0.7174 0.3278 0.5426 0.073 Uiso 1 1 calc R . . H30B H 0.8399 0.3282 0.5342 0.073 Uiso 1 1 calc R . . C31 C 0.7046(5) 0.31334(15) 0.3852(3) 0.0908(14) Uani 1 1 d . . . H31A H 0.6199 0.3102 0.3597 0.109 Uiso 1 1 calc R . . H31B H 0.7372 0.2762 0.3862 0.109 Uiso 1 1 calc R . . C32 C 0.7333(4) 0.35130(16) 0.3109(3) 0.0771(11) Uani 1 1 d . . . H32A H 0.6701 0.3522 0.2341 0.092 Uiso 1 1 calc R . . H32B H 0.8055 0.3398 0.3058 0.092 Uiso 1 1 calc R . . C33 C 0.7476(4) 0.40660(13) 0.3674(3) 0.0692(10) Uani 1 1 d . . . H33A H 0.8213 0.4238 0.3760 0.083 Uiso 1 1 calc R . . H33B H 0.6833 0.4314 0.3220 0.083 Uiso 1 1 calc R . . C34 C 1.0307(2) 0.55484(11) 0.7714(2) 0.0460(6) Uani 1 1 d . . . H34 H 0.9885 0.5842 0.7845 0.055 Uiso 1 1 calc R . . C35 C 1.1413(2) 0.54261(11) 0.8501(2) 0.0434(6) Uani 1 1 d . . . H35 H 1.1752 0.5639 0.9172 0.052 Uiso 1 1 calc R . . C36 C 1.2022(2) 0.49979(11) 0.8317(2) 0.0468(6) Uani 1 1 d . . . H36 H 1.2779 0.4916 0.8862 0.056 Uiso 1 1 calc R . . C37 C 1.1539(3) 0.46877(12) 0.7343(3) 0.0498(7) Uani 1 1 d . . . H37 H 1.1962 0.4393 0.7216 0.060 Uiso 1 1 calc R . . C38 C 1.0432(3) 0.48083(12) 0.6552(2) 0.0512(7) Uani 1 1 d . . . H38 H 1.0092 0.4596 0.5882 0.061 Uiso 1 1 calc R . . C39 C 0.9824(2) 0.52402(11) 0.6742(2) 0.0452(6) Uani 1 1 d . . . H39 H 0.9068 0.5324 0.6197 0.054 Uiso 1 1 calc R . . H1A H 0.3799(13) 0.4875(8) 0.6154(19) 0.026(6) Uiso 1 1 d D . . H1B H 0.4971(15) 0.4617(9) 0.6836(9) 0.031(6) Uiso 1 1 d D . . H16A H 0.203(3) 0.4588(13) 0.0923(12) 0.070(10) Uiso 1 1 d D . . H16B H 0.200(2) 0.4807(12) 0.194(2) 0.048(9) Uiso 1 1 d D . . H16C H 0.279(3) 0.5031(7) 0.154(3) 0.062(9) Uiso 1 1 d D . . 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 Ba1 0.02703(7) 0.02104(6) 0.02122(6) 0.00261(5) 0.00806(5) 0.00013(5) O1 0.0758(14) 0.0385(10) 0.0435(10) -0.0060(8) 0.0361(10) 0.0045(9) N1 0.0264(9) 0.0209(8) 0.0227(8) 0.0004(6) 0.0067(7) -0.0023(6) N2 0.0277(9) 0.0222(8) 0.0170(8) 0.0037(6) 0.0067(7) 0.0015(7) C1 0.0275(11) 0.0262(10) 0.0213(10) 0.0009(8) 0.0083(8) 0.0029(8) C2 0.0251(10) 0.0232(9) 0.0214(9) 0.0032(7) 0.0091(8) -0.0024(7) C3 0.0276(10) 0.0237(9) 0.0194(9) 0.0008(7) 0.0069(8) -0.0001(8) C4 0.0263(10) 0.0247(9) 0.0216(10) 0.0014(7) 0.0103(8) -0.0002(8) C5 0.0365(12) 0.0231(10) 0.0280(11) 0.0017(8) 0.0076(9) 0.0026(8) C6 0.0267(11) 0.0237(10) 0.0254(10) 0.0016(8) 0.0035(8) 0.0020(8) C7 0.0318(12) 0.0299(11) 0.0314(12) 0.0044(9) 0.0040(9) -0.0066(9) C8 0.0349(13) 0.0266(11) 0.0437(14) 0.0024(10) 0.0039(10) -0.0066(9) C9 0.0334(13) 0.0263(11) 0.0439(14) -0.0082(10) 0.0011(10) -0.0019(9) C10 0.0339(13) 0.0372(12) 0.0349(13) -0.0083(10) 0.0069(10) 0.0015(10) C11 0.0252(11) 0.0291(11) 0.0296(11) -0.0033(8) 0.0053(9) 0.0007(8) C12 0.0657(19) 0.0537(17) 0.0394(15) 0.0013(12) 0.0188(13) -0.0325(14) C13 0.0473(19) 0.130(3) 0.062(2) 0.054(2) 0.0064(16) -0.021(2) C14 0.084(2) 0.0473(17) 0.0608(19) 0.0021(14) 0.0411(18) -0.0055(15) C15 0.0375(13) 0.0440(13) 0.0307(12) -0.0097(10) 0.0148(10) -0.0097(10) C16 0.0559(18) 0.0447(16) 0.0299(13) -0.0003(11) 0.0072(12) -0.0149(13) C17 0.074(2) 0.077(2) 0.070(2) -0.0236(18) 0.0504(19) -0.0191(18) C18 0.0308(11) 0.0209(9) 0.0179(9) 0.0012(7) 0.0057(8) 0.0016(8) C19 0.0339(12) 0.0287(10) 0.0240(10) 0.0037(8) 0.0110(9) 0.0004(8) C20 0.0443(14) 0.0363(12) 0.0242(11) 0.0066(9) 0.0139(10) -0.0004(10) C21 0.0460(14) 0.0380(13) 0.0220(11) 0.0088(9) 0.0043(10) 0.0027(10) C22 0.0325(12) 0.0344(12) 0.0276(11) 0.0061(9) 0.0022(9) 0.0045(9) C23 0.0316(12) 0.0263(10) 0.0228(10) 0.0017(8) 0.0081(9) 0.0037(8) C24 0.0362(13) 0.0533(15) 0.0334(13) 0.0130(11) 0.0178(10) 0.0059(11) C25 0.0430(16) 0.081(2) 0.0521(17) 0.0217(16) 0.0244(13) 0.0001(15) C26 0.0592(19) 0.065(2) 0.0551(18) 0.0090(15) 0.0314(15) 0.0234(15) C27 0.0310(12) 0.0465(14) 0.0338(12) 0.0103(10) 0.0131(10) 0.0095(10) C28 0.0535(18) 0.068(2) 0.0539(18) -0.0043(15) 0.0276(15) 0.0142(15) C29 0.0472(17) 0.0471(16) 0.0678(19) 0.0091(14) 0.0257(15) -0.0065(12) C30 0.098(3) 0.0451(16) 0.0556(18) 0.0046(14) 0.0483(18) 0.0076(16) C31 0.151(4) 0.0462(19) 0.055(2) -0.0109(16) 0.024(2) -0.013(2) C32 0.109(3) 0.086(3) 0.0407(17) -0.0034(17) 0.0352(19) 0.028(2) C33 0.112(3) 0.0499(18) 0.077(2) 0.0120(16) 0.069(2) 0.0124(18) C34 0.0496(16) 0.0412(14) 0.0502(16) 0.0048(12) 0.0238(13) 0.0146(12) C35 0.0480(15) 0.0392(14) 0.0421(14) -0.0008(11) 0.0177(12) 0.0023(11) C36 0.0399(15) 0.0467(15) 0.0514(16) 0.0046(12) 0.0165(12) 0.0080(11) C37 0.0594(18) 0.0436(15) 0.0536(17) 0.0009(13) 0.0305(15) 0.0105(13) C38 0.066(2) 0.0480(15) 0.0390(15) -0.0006(12) 0.0207(14) -0.0028(14) C39 0.0417(15) 0.0459(15) 0.0441(15) 0.0097(12) 0.0139(12) 0.0001(11) _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 Ba1 N1 2.6677(16) 3_666 ? Ba1 O1 2.7369(17) . ? Ba1 N2 2.7576(16) . ? Ba1 H1B 2.81(3) . ? Ba1 C1 2.966(2) . ? Ba1 C1 3.001(2) 3_666 ? Ba1 C2 3.1587(19) 3_666 ? Ba1 C16 3.307(3) 3_666 ? Ba1 H16C 5.87(3) . ? Ba1 H16B 6.05(3) . ? Ba1 H1B 2.81(3) . ? O1 C30 1.424(3) . ? O1 C33 1.436(3) . ? N1 C2 1.367(2) . ? N1 C6 1.412(3) . ? N1 Ba1 2.6677(16) 3_666 ? N2 C4 1.338(3) . ? N2 C18 1.429(2) . ? C1 C2 1.411(3) . ? C1 Ba1 3.001(2) 3_666 ? C1 H1A 0.901(3) . ? C1 H1B 0.901(3) . ? C2 C3 1.458(3) . ? C3 C4 1.405(3) . ? C3 H3 0.9500 . ? C4 C5 1.523(3) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C11 1.411(3) . ? C6 C7 1.415(3) . ? C7 C8 1.398(3) . ? C7 C12 1.511(4) . ? C8 C9 1.376(4) . ? C8 H8 0.9500 . ? C9 C10 1.383(4) . ? C9 H9 0.9500 . ? C10 C11 1.394(3) . ? C10 H10 0.9500 . ? C11 C15 1.517(3) . ? C12 C14 1.532(4) . ? C12 C13 1.534(5) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.527(4) . ? C15 C17 1.529(4) . ? C15 H15 1.0000 . ? C16 Ba1 3.307(3) 3_666 ? C16 H16A 0.901(3) . ? C16 H16B 0.902(3) . ? C16 H16C 0.901(3) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C23 1.404(3) . ? C18 C19 1.409(3) . ? C19 C20 1.398(3) . ? C19 C24 1.517(3) . ? C20 C21 1.377(3) . ? C20 H20 0.9500 . ? C21 C22 1.375(4) . ? C21 H21 0.9500 . ? C22 C23 1.401(3) . ? C22 H22 0.9500 . ? C23 C27 1.514(3) . ? C24 C25 1.532(4) . ? C24 C26 1.533(4) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C29 1.539(4) . ? C27 C28 1.541(4) . ? C27 H27 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.450(4) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.488(5) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.505(5) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C39 1.377(4) . ? C34 C35 1.386(4) . ? C34 H34 0.9500 . ? C35 C36 1.377(4) . ? C35 H35 0.9500 . ? C36 C37 1.381(4) . ? C36 H36 0.9500 . ? C37 C38 1.388(4) . ? C37 H37 0.9500 . ? C38 C39 1.386(4) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ba1 O1 112.09(6) 3_666 . ? N1 Ba1 N2 144.98(5) 3_666 . ? O1 Ba1 N2 100.55(5) . . ? N1 Ba1 H1B 103.7(5) 3_666 . ? O1 Ba1 H1B 140.2(5) . . ? N2 Ba1 H1B 51.7(4) . . ? N1 Ba1 C1 98.87(6) 3_666 . ? O1 Ba1 C1 133.73(6) . . ? N2 Ba1 C1 64.55(5) . . ? H1B Ba1 C1 17.68(7) . . ? N1 Ba1 C1 49.03(5) 3_666 3_666 ? O1 Ba1 C1 86.49(6) . 3_666 ? N2 Ba1 C1 149.58(5) . 3_666 ? H1B Ba1 C1 105.2(2) . 3_666 ? C1 Ba1 C1 89.12(6) . 3_666 ? N1 Ba1 C2 25.38(5) 3_666 3_666 ? O1 Ba1 C2 107.37(5) . 3_666 ? N2 Ba1 C2 149.02(5) . 3_666 ? H1B Ba1 C2 97.4(4) . 3_666 ? C1 Ba1 C2 86.17(5) . 3_666 ? C1 Ba1 C2 26.33(5) 3_666 3_666 ? N1 Ba1 C16 70.74(6) 3_666 3_666 ? O1 Ba1 C16 140.24(8) . 3_666 ? N2 Ba1 C16 76.16(6) . 3_666 ? H1B Ba1 C16 67.9(3) . 3_666 ? C1 Ba1 C16 81.40(7) . 3_666 ? C1 Ba1 C16 116.58(6) 3_666 3_666 ? C2 Ba1 C16 90.29(6) 3_666 3_666 ? N1 Ba1 H16C 77.49(10) 3_666 . ? O1 Ba1 H16C 84.6(3) . . ? N2 Ba1 H16C 119.24(11) . . ? H1B Ba1 H16C 86.7(3) . . ? C1 Ba1 H16C 69.0(3) . . ? C1 Ba1 H16C 31.33(7) 3_666 . ? C2 Ba1 H16C 52.23(11) 3_666 . ? C16 Ba1 H16C 132.2(3) 3_666 . ? N1 Ba1 H16B 85.8(3) 3_666 . ? O1 Ba1 H16B 91.41(13) . . ? N2 Ba1 H16B 106.4(2) . . ? H1B Ba1 H16B 74.08(14) . . ? C1 Ba1 H16B 56.49(11) . . ? C1 Ba1 H16B 43.5(3) 3_666 . ? C2 Ba1 H16B 60.5(3) 3_666 . ? C16 Ba1 H16B 127.90(15) 3_666 . ? H16C Ba1 H16B 13.6(3) . . ? N1 Ba1 H1B 103.7(5) 3_666 . ? O1 Ba1 H1B 140.2(5) . . ? N2 Ba1 H1B 51.7(4) . . ? H1B Ba1 H1B 0.0(10) . . ? C1 Ba1 H1B 17.68(7) . . ? C1 Ba1 H1B 105.2(2) 3_666 . ? C2 Ba1 H1B 97.4(4) 3_666 . ? C16 Ba1 H1B 67.9(3) 3_666 . ? H16C Ba1 H1B 86.7(3) . . ? H16B Ba1 H1B 74.08(14) . . ? C30 O1 C33 107.5(2) . . ? C30 O1 Ba1 120.33(16) . . ? C33 O1 Ba1 128.53(17) . . ? C2 N1 C6 120.36(17) . . ? C2 N1 Ba1 97.82(11) . 3_666 ? C6 N1 Ba1 134.67(13) . 3_666 ? C4 N2 C18 117.85(16) . . ? C4 N2 Ba1 91.64(11) . . ? C18 N2 Ba1 141.78(13) . . ? C2 C1 Ba1 83.28(12) . . ? C2 C1 Ba1 83.08(12) . 3_666 ? Ba1 C1 Ba1 90.88(6) . 3_666 ? C2 C1 H1A 115.1(15) . . ? Ba1 C1 H1A 150.7(15) . . ? Ba1 C1 H1A 70.4(15) 3_666 . ? C2 C1 H1B 116.8(15) . . ? Ba1 C1 H1B 71.1(16) . . ? Ba1 C1 H1B 150.2(16) 3_666 . ? H1A C1 H1B 115(2) . . ? N1 C2 C1 117.23(18) . . ? N1 C2 C3 119.44(18) . . ? C1 C2 C3 123.18(18) . . ? C4 C3 C2 128.46(19) . . ? C4 C3 H3 115.8 . . ? C2 C3 H3 115.8 . . ? N2 C4 C3 123.93(18) . . ? N2 C4 C5 119.81(18) . . ? C3 C4 C5 116.24(18) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C11 C6 N1 120.59(19) . . ? C11 C6 C7 119.3(2) . . ? N1 C6 C7 119.9(2) . . ? C8 C7 C6 118.9(2) . . ? C8 C7 C12 119.2(2) . . ? C6 C7 C12 121.9(2) . . ? C9 C8 C7 121.7(2) . . ? C9 C8 H8 119.2 . . ? C7 C8 H8 119.2 . . ? C8 C9 C10 119.5(2) . . ? C8 C9 H9 120.3 . . ? C10 C9 H9 120.3 . . ? C9 C10 C11 121.2(2) . . ? C9 C10 H10 119.4 . . ? C11 C10 H10 119.4 . . ? C10 C11 C6 119.4(2) . . ? C10 C11 C15 120.7(2) . . ? C6 C11 C15 119.84(19) . . ? C7 C12 C14 112.3(2) . . ? C7 C12 C13 110.5(3) . . ? C14 C12 C13 109.4(2) . . ? C7 C12 H12 108.2 . . ? C14 C12 H12 108.2 . . ? C13 C12 H12 108.2 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 C16 110.3(2) . . ? C11 C15 C17 114.5(2) . . ? C16 C15 C17 109.9(2) . . ? C11 C15 H15 107.3 . . ? C16 C15 H15 107.3 . . ? C17 C15 H15 107.3 . . ? C15 C16 Ba1 86.98(14) . 3_666 ? C15 C16 H16A 108(2) . . ? Ba1 C16 H16A 162(2) 3_666 . ? C15 C16 H16B 112.8(19) . . ? Ba1 C16 H16B 57.1(19) 3_666 . ? H16A C16 H16B 107(3) . . ? C15 C16 H16C 117(2) . . ? Ba1 C16 H16C 73(2) 3_666 . ? H16A C16 H16C 107(3) . . ? H16B C16 H16C 105(3) . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C23 C18 C19 119.79(18) . . ? C23 C18 N2 121.33(19) . . ? C19 C18 N2 118.80(19) . . ? C20 C19 C18 118.8(2) . . ? C20 C19 C24 119.8(2) . . ? C18 C19 C24 121.17(19) . . ? C21 C20 C19 121.6(2) . . ? C21 C20 H20 119.2 . . ? C19 C20 H20 119.2 . . ? C22 C21 C20 119.4(2) . . ? C22 C21 H21 120.3 . . ? C20 C21 H21 120.3 . . ? C21 C22 C23 121.4(2) . . ? C21 C22 H22 119.3 . . ? C23 C22 H22 119.3 . . ? C22 C23 C18 119.0(2) . . ? C22 C23 C27 118.4(2) . . ? C18 C23 C27 122.60(18) . . ? C19 C24 C25 114.1(2) . . ? C19 C24 C26 108.8(2) . . ? C25 C24 C26 110.7(2) . . ? C19 C24 H24 107.6 . . ? C25 C24 H24 107.6 . . ? C26 C24 H24 107.6 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 C29 110.7(2) . . ? C23 C27 C28 111.9(2) . . ? C29 C27 C28 109.4(2) . . ? C23 C27 H27 108.3 . . ? C29 C27 H27 108.3 . . ? C28 C27 H27 108.3 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O1 C30 C31 106.1(3) . . ? O1 C30 H30A 110.5 . . ? C31 C30 H30A 110.5 . . ? O1 C30 H30B 110.5 . . ? C31 C30 H30B 110.5 . . ? H30A C30 H30B 108.7 . . ? C30 C31 C32 103.9(3) . . ? C30 C31 H31A 111.0 . . ? C32 C31 H31A 111.0 . . ? C30 C31 H31B 111.0 . . ? C32 C31 H31B 111.0 . . ? H31A C31 H31B 109.0 . . ? C31 C32 C33 104.3(3) . . ? C31 C32 H32A 110.9 . . ? C33 C32 H32A 110.9 . . ? C31 C32 H32B 110.9 . . ? C33 C32 H32B 110.9 . . ? H32A C32 H32B 108.9 . . ? O1 C33 C32 106.6(3) . . ? O1 C33 H33A 110.4 . . ? C32 C33 H33A 110.4 . . ? O1 C33 H33B 110.4 . . ? C32 C33 H33B 110.4 . . ? H33A C33 H33B 108.6 . . ? C39 C34 C35 119.5(2) . . ? C39 C34 H34 120.3 . . ? C35 C34 H34 120.3 . . ? C36 C35 C34 120.3(3) . . ? C36 C35 H35 119.8 . . ? C34 C35 H35 119.8 . . ? C35 C36 C37 120.4(3) . . ? C35 C36 H36 119.8 . . ? C37 C36 H36 119.8 . . ? C36 C37 C38 119.6(3) . . ? C36 C37 H37 120.2 . . ? C38 C37 H37 120.2 . . ? C39 C38 C37 119.8(3) . . ? C39 C38 H38 120.1 . . ? C37 C38 H38 120.1 . . ? C34 C39 C38 120.5(3) . . ? C34 C39 H39 119.8 . . ? C38 C39 H39 119.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Ba1 O1 C30 170.9(2) 3_666 . . . ? N2 Ba1 O1 C30 3.9(2) . . . . ? H1B Ba1 O1 C30 -36.6(3) . . . . ? C1 Ba1 O1 C30 -60.9(2) . . . . ? C1 Ba1 O1 C30 -146.3(2) 3_666 . . . ? C2 Ba1 O1 C30 -162.6(2) 3_666 . . . ? C16 Ba1 O1 C30 84.9(2) 3_666 . . . ? H16C Ba1 O1 C30 -114.9(2) . . . . ? H16B Ba1 O1 C30 -103.1(3) . . . . ? N1 Ba1 O1 C33 -33.6(3) 3_666 . . . ? N2 Ba1 O1 C33 159.4(3) . . . . ? H1B Ba1 O1 C33 118.9(3) . . . . ? C1 Ba1 O1 C33 94.6(3) . . . . ? C1 Ba1 O1 C33 9.2(3) 3_666 . . . ? C2 Ba1 O1 C33 -7.0(3) 3_666 . . . ? C16 Ba1 O1 C33 -119.6(3) 3_666 . . . ? H16C Ba1 O1 C33 40.6(3) . . . . ? H16B Ba1 O1 C33 52.4(4) . . . . ? N1 Ba1 N2 C4 145.66(12) 3_666 . . . ? O1 Ba1 N2 C4 -55.55(13) . . . . ? H1B Ba1 N2 C4 92.5(4) . . . . ? C1 Ba1 N2 C4 78.09(12) . . . . ? C1 Ba1 N2 C4 45.65(17) 3_666 . . . ? C2 Ba1 N2 C4 98.62(14) 3_666 . . . ? C16 Ba1 N2 C4 165.04(14) 3_666 . . . ? H16C Ba1 N2 C4 34.2(4) . . . . ? H16B Ba1 N2 C4 39.1(2) . . . . ? N1 Ba1 N2 C18 -72.0(2) 3_666 . . . ? O1 Ba1 N2 C18 86.8(2) . . . . ? H1B Ba1 N2 C18 -125.1(5) . . . . ? C1 Ba1 N2 C18 -139.6(2) . . . . ? C1 Ba1 N2 C18 -171.99(18) 3_666 . . . ? C2 Ba1 N2 C18 -119.0(2) 3_666 . . . ? C16 Ba1 N2 C18 -52.6(2) 3_666 . . . ? H16C Ba1 N2 C18 176.5(4) . . . . ? H16B Ba1 N2 C18 -178.6(3) . . . . ? N1 Ba1 C1 C2 131.16(11) 3_666 . . . ? O1 Ba1 C1 C2 -1.38(15) . . . . ? N2 Ba1 C1 C2 -81.32(12) . . . . ? H1B Ba1 C1 C2 -121.3(16) . . . . ? C1 Ba1 C1 C2 82.92(12) 3_666 . . . ? C2 Ba1 C1 C2 109.11(11) 3_666 . . . ? C16 Ba1 C1 C2 -160.02(13) 3_666 . . . ? H16C Ba1 C1 C2 58.3(2) . . . . ? H16B Ba1 C1 C2 52.3(3) . . . . ? N1 Ba1 C1 Ba1 48.23(6) 3_666 . . 3_666 ? O1 Ba1 C1 Ba1 -84.30(8) . . . 3_666 ? N2 Ba1 C1 Ba1 -164.24(7) . . . 3_666 ? H1B Ba1 C1 Ba1 155.7(16) . . . 3_666 ? C1 Ba1 C1 Ba1 0.0 3_666 . . 3_666 ? C2 Ba1 C1 Ba1 26.19(5) 3_666 . . 3_666 ? C16 Ba1 C1 Ba1 117.06(7) 3_666 . . 3_666 ? H16C Ba1 C1 Ba1 -24.64(18) . . . 3_666 ? H16B Ba1 C1 Ba1 -30.6(3) . . . 3_666 ? C6 N1 C2 C1 -167.03(19) . . . . ? Ba1 N1 C2 C1 38.44(19) 3_666 . . . ? C6 N1 C2 C3 17.2(3) . . . . ? Ba1 N1 C2 C3 -137.36(16) 3_666 . . . ? Ba1 C1 C2 N1 -125.18(17) . . . . ? Ba1 C1 C2 N1 -33.47(17) 3_666 . . . ? Ba1 C1 C2 C3 50.45(19) . . . . ? Ba1 C1 C2 C3 142.16(18) 3_666 . . . ? N1 C2 C3 C4 -164.4(2) . . . . ? C1 C2 C3 C4 20.1(3) . . . . ? C18 N2 C4 C3 162.8(2) . . . . ? Ba1 N2 C4 C3 -42.4(2) . . . . ? C18 N2 C4 C5 -19.1(3) . . . . ? Ba1 N2 C4 C5 135.57(18) . . . . ? C2 C3 C4 N2 -31.4(3) . . . . ? C2 C3 C4 C5 150.5(2) . . . . ? C2 N1 C6 C11 -110.2(2) . . . . ? Ba1 N1 C6 C11 33.0(3) 3_666 . . . ? C2 N1 C6 C7 74.6(3) . . . . ? Ba1 N1 C6 C7 -142.17(17) 3_666 . . . ? C11 C6 C7 C8 -0.3(3) . . . . ? N1 C6 C7 C8 174.9(2) . . . . ? C11 C6 C7 C12 178.3(2) . . . . ? N1 C6 C7 C12 -6.6(3) . . . . ? C6 C7 C8 C9 -0.2(4) . . . . ? C12 C7 C8 C9 -178.8(2) . . . . ? C7 C8 C9 C10 0.4(4) . . . . ? C8 C9 C10 C11 -0.2(4) . . . . ? C9 C10 C11 C6 -0.3(3) . . . . ? C9 C10 C11 C15 -178.2(2) . . . . ? N1 C6 C11 C10 -174.6(2) . . . . ? C7 C6 C11 C10 0.6(3) . . . . ? N1 C6 C11 C15 3.3(3) . . . . ? C7 C6 C11 C15 178.5(2) . . . . ? C8 C7 C12 C14 -55.9(3) . . . . ? C6 C7 C12 C14 125.5(3) . . . . ? C8 C7 C12 C13 66.5(3) . . . . ? C6 C7 C12 C13 -112.0(3) . . . . ? C10 C11 C15 C16 86.7(3) . . . . ? C6 C11 C15 C16 -91.2(3) . . . . ? C10 C11 C15 C17 -37.9(3) . . . . ? C6 C11 C15 C17 144.2(2) . . . . ? C11 C15 C16 Ba1 94.84(16) . . . 3_666 ? C17 C15 C16 Ba1 -137.94(19) . . . 3_666 ? C4 N2 C18 C23 107.5(2) . . . . ? Ba1 N2 C18 C23 -28.8(3) . . . . ? C4 N2 C18 C19 -75.8(2) . . . . ? Ba1 N2 C18 C19 147.85(17) . . . . ? C23 C18 C19 C20 -2.1(3) . . . . ? N2 C18 C19 C20 -178.78(19) . . . . ? C23 C18 C19 C24 172.3(2) . . . . ? N2 C18 C19 C24 -4.4(3) . . . . ? C18 C19 C20 C21 1.0(3) . . . . ? C24 C19 C20 C21 -173.5(2) . . . . ? C19 C20 C21 C22 0.7(4) . . . . ? C20 C21 C22 C23 -1.4(4) . . . . ? C21 C22 C23 C18 0.3(3) . . . . ? C21 C22 C23 C27 178.7(2) . . . . ? C19 C18 C23 C22 1.5(3) . . . . ? N2 C18 C23 C22 178.09(19) . . . . ? C19 C18 C23 C27 -176.9(2) . . . . ? N2 C18 C23 C27 -0.2(3) . . . . ? C20 C19 C24 C25 -38.6(3) . . . . ? C18 C19 C24 C25 147.0(2) . . . . ? C20 C19 C24 C26 85.6(3) . . . . ? C18 C19 C24 C26 -88.8(3) . . . . ? C22 C23 C27 C29 -61.6(3) . . . . ? C18 C23 C27 C29 116.7(2) . . . . ? C22 C23 C27 C28 60.6(3) . . . . ? C18 C23 C27 C28 -121.0(2) . . . . ? C33 O1 C30 C31 -29.4(4) . . . . ? Ba1 O1 C30 C31 130.8(3) . . . . ? O1 C30 C31 C32 34.9(4) . . . . ? C30 C31 C32 C33 -26.9(5) . . . . ? C30 O1 C33 C32 11.6(4) . . . . ? Ba1 O1 C33 C32 -146.3(2) . . . . ? C31 C32 C33 O1 9.7(4) . . . . ? C39 C34 C35 C36 -0.4(4) . . . . ? C34 C35 C36 C37 0.3(4) . . . . ? C35 C36 C37 C38 -0.3(4) . . . . ? C36 C37 C38 C39 0.4(4) . . . . ? C35 C34 C39 C38 0.5(4) . . . . ? C37 C38 C39 C34 -0.5(4) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 30.06 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.139 _refine_diff_density_min -0.632 _refine_diff_density_rms 0.074 # Attachment 'Compound_11.cif' data_c:\x-ray\kappa\old_ka~1\k08msh~1\maxus2\k08msh57 _database_code_depnum_ccdc_archive 'CCDC 727089' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H61 Ca N3 O' _chemical_formula_weight 664.02 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.2139(2) _cell_length_b 17.7982(4) _cell_length_c 18.2010(5) _cell_angle_alpha 90.125(1) _cell_angle_beta 91.025(1) _cell_angle_gamma 97.899(1) _cell_volume 3918.42(15) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 54565 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 25.028 _exptl_crystal_description Block _exptl_crystal_colour Colourless _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 1.126 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1448 _exptl_absorpt_coefficient_mu 0.194 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.88 _exptl_absorpt_correction_T_max 1.00 _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 65141 _diffrn_reflns_av_R_equivalents 0.1176 _diffrn_reflns_av_sigmaI/netI 0.0878 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.84 _diffrn_reflns_theta_max 25.07 _reflns_number_total 13817 _reflns_number_gt 8509 _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^)+(0.0346P)^2^+5.2857P] 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 13817 _refine_ls_number_parameters 844 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1253 _refine_ls_R_factor_gt 0.0654 _refine_ls_wR_factor_ref 0.1575 _refine_ls_wR_factor_gt 0.1286 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _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 C1 C -0.2898(4) -0.7890(2) 0.7365(3) 0.0534(12) Uani 1 1 d . . . H1A H -0.3601 -0.7931 0.7634 0.064 Uiso 1 1 calc R . . H1B H -0.2362 -0.7463 0.7556 0.064 Uiso 1 1 calc R . . C2 C -0.3037(3) -0.7892(2) 0.6588(2) 0.0422(10) Uani 1 1 d . . . C3 C -0.2163(3) -0.7968(2) 0.6100(2) 0.0355(9) Uani 1 1 d . . . C4 C -0.2336(4) -0.7990(2) 0.5338(2) 0.0483(11) Uani 1 1 d . . . H4 H -0.1727 -0.8019 0.5027 0.058 Uiso 1 1 calc R . . C5 C -0.3366(5) -0.7972(3) 0.5029(3) 0.0663(15) Uani 1 1 d . . . H5 H -0.3474 -0.7994 0.4510 0.080 Uiso 1 1 calc R . . C6 C -0.4241(5) -0.7922(3) 0.5489(4) 0.0715(17) Uani 1 1 d . . . H6 H -0.4959 -0.7913 0.5283 0.086 Uiso 1 1 calc R . . C7 C -0.4094(4) -0.7883(2) 0.6237(3) 0.0600(14) Uani 1 1 d . . . H7 H -0.4717 -0.7849 0.6534 0.072 Uiso 1 1 calc R . . C8 C -0.0341(3) -0.8372(3) 0.5949(2) 0.0526(12) Uani 1 1 d . . . H8A H 0.0365 -0.8390 0.6207 0.079 Uiso 1 1 calc R . . H8B H -0.0216 -0.8069 0.5501 0.079 Uiso 1 1 calc R . . H8C H -0.0676 -0.8888 0.5818 0.079 Uiso 1 1 calc R . . C9 C -0.0526(3) -0.7274(2) 0.6653(3) 0.0554(12) Uani 1 1 d . . . H9A H 0.0197 -0.7326 0.6874 0.083 Uiso 1 1 calc R . . H9B H -0.0976 -0.7051 0.7014 0.083 Uiso 1 1 calc R . . H9C H -0.0427 -0.6944 0.6223 0.083 Uiso 1 1 calc R . . C10 C -0.2810(3) -1.0416(2) 0.8606(2) 0.0351(9) Uani 1 1 d . . . C11 C -0.1829(3) -1.0734(2) 0.8529(2) 0.0361(9) Uani 1 1 d . . . H11 H -0.1840 -1.1229 0.8725 0.043 Uiso 1 1 calc R . . C12 C -0.0834(3) -1.0429(2) 0.8206(2) 0.0311(8) Uani 1 1 d . . . C13 C 0.0149(3) -1.0837(2) 0.8392(2) 0.0417(10) Uani 1 1 d . . . H13A H 0.0806 -1.0587 0.8144 0.063 Uiso 1 1 calc R . . H13B H -0.0008 -1.1366 0.8227 0.063 Uiso 1 1 calc R . . H13C H 0.0283 -1.0822 0.8925 0.063 Uiso 1 1 calc R . . C14 C -0.3639(3) -1.0826(2) 0.9132(2) 0.0513(11) Uani 1 1 d . . . H14A H -0.3805 -1.0473 0.9515 0.077 Uiso 1 1 calc R . . H14B H -0.3327 -1.1250 0.9359 0.077 Uiso 1 1 calc R . . H14C H -0.4321 -1.1020 0.8861 0.077 Uiso 1 1 calc R . . C15 C 0.0340(3) -0.9509(2) 0.7513(2) 0.0304(8) Uani 1 1 d . . . C16 C 0.0828(3) -0.9843(2) 0.6924(2) 0.0320(8) Uani 1 1 d . . . C17 C 0.1774(3) -0.9445(2) 0.6619(2) 0.0395(9) Uani 1 1 d . . . H17 H 0.2110 -0.9663 0.6219 0.047 Uiso 1 1 calc R . . C18 C 0.2234(3) -0.8745(2) 0.6883(2) 0.0436(10) Uani 1 1 d . . . H18 H 0.2862 -0.8476 0.6653 0.052 Uiso 1 1 calc R . . C19 C 0.1781(3) -0.8434(2) 0.7482(2) 0.0404(10) Uani 1 1 d . . . H19 H 0.2119 -0.7960 0.7675 0.049 Uiso 1 1 calc R . . C20 C 0.0836(3) -0.8804(2) 0.7807(2) 0.0335(9) Uani 1 1 d . . . C21 C 0.0355(3) -1.0611(2) 0.6595(2) 0.0347(9) Uani 1 1 d . . . H21 H -0.0299 -1.0821 0.6889 0.042 Uiso 1 1 calc R . . C22 C 0.1186(3) -1.1182(2) 0.6620(2) 0.0464(10) Uani 1 1 d . . . H22A H 0.0844 -1.1665 0.6405 0.070 Uiso 1 1 calc R . . H22B H 0.1405 -1.1261 0.7131 0.070 Uiso 1 1 calc R . . H22C H 0.1840 -1.0985 0.6339 0.070 Uiso 1 1 calc R . . C23 C -0.0041(3) -1.0526(2) 0.5802(2) 0.0431(10) Uani 1 1 d . . . H23A H -0.0344 -1.1025 0.5604 0.065 Uiso 1 1 calc R . . H23B H 0.0583 -1.0307 0.5504 0.065 Uiso 1 1 calc R . . H23C H -0.0615 -1.0192 0.5789 0.065 Uiso 1 1 calc R . . C24 C 0.0371(3) -0.8475(2) 0.8496(2) 0.0420(10) Uani 1 1 d . . . H24 H -0.0453 -0.8550 0.8439 0.050 Uiso 1 1 calc R . . C25 C 0.0653(4) -0.8904(3) 0.9179(2) 0.0575(12) Uani 1 1 d . . . H25A H 0.0408 -0.9447 0.9106 0.086 Uiso 1 1 calc R . . H25B H 0.0277 -0.8722 0.9602 0.086 Uiso 1 1 calc R . . H25C H 0.1454 -0.8818 0.9268 0.086 Uiso 1 1 calc R . . C26 C 0.0737(4) -0.7631(2) 0.8606(3) 0.0607(13) Uani 1 1 d . . . H26A H 0.0547 -0.7357 0.8165 0.091 Uiso 1 1 calc R . . H26B H 0.1538 -0.7540 0.8693 0.091 Uiso 1 1 calc R . . H26C H 0.0361 -0.7452 0.9030 0.091 Uiso 1 1 calc R . . C27 C -0.3964(3) -0.9452(2) 0.8517(2) 0.0317(8) Uani 1 1 d . . . C28 C -0.3826(3) -0.8923(2) 0.9100(2) 0.0350(9) Uani 1 1 d . . . C29 C -0.4707(3) -0.8546(2) 0.9282(2) 0.0421(10) Uani 1 1 d . . . H29 H -0.4616 -0.8183 0.9669 0.050 Uiso 1 1 calc R . . C30 C -0.5715(3) -0.8687(2) 0.8912(2) 0.0448(10) Uani 1 1 d . . . H30 H -0.6306 -0.8420 0.9039 0.054 Uiso 1 1 calc R . . C31 C -0.5848(3) -0.9219(2) 0.8357(2) 0.0452(10) Uani 1 1 d . . . H31 H -0.6543 -0.9323 0.8108 0.054 Uiso 1 1 calc R . . C32 C -0.4992(3) -0.9608(2) 0.8152(2) 0.0382(9) Uani 1 1 d . . . C33 C -0.5170(3) -1.0175(2) 0.7515(2) 0.0449(10) Uani 1 1 d . . . H33 H -0.4487 -1.0424 0.7476 0.054 Uiso 1 1 calc R . . C34 C -0.5342(4) -0.9783(3) 0.6791(2) 0.0556(12) Uani 1 1 d . . . H34A H -0.5446 -1.0160 0.6394 0.083 Uiso 1 1 calc R . . H34B H -0.4693 -0.9411 0.6693 0.083 Uiso 1 1 calc R . . H34C H -0.5999 -0.9524 0.6820 0.083 Uiso 1 1 calc R . . C35 C -0.6139(4) -1.0794(3) 0.7657(3) 0.0656(14) Uani 1 1 d . . . H35A H -0.6228 -1.1152 0.7244 0.098 Uiso 1 1 calc R . . H35B H -0.6817 -1.0563 0.7710 0.098 Uiso 1 1 calc R . . H35C H -0.5993 -1.1064 0.8109 0.098 Uiso 1 1 calc R . . C36 C -0.2742(3) -0.8761(2) 0.9533(2) 0.0438(10) Uani 1 1 d . . . H36 H -0.2214 -0.9086 0.9328 0.053 Uiso 1 1 calc R . . C37 C -0.2905(5) -0.8962(4) 1.0350(3) 0.0842(18) Uani 1 1 d . . . H37A H -0.3234 -0.9494 1.0393 0.126 Uiso 1 1 calc R . . H37B H -0.3398 -0.8635 1.0568 0.126 Uiso 1 1 calc R . . H37C H -0.2188 -0.8885 1.0609 0.126 Uiso 1 1 calc R . . C38 C -0.2230(4) -0.7942(3) 0.9473(3) 0.0587(12) Uani 1 1 d . . . H38A H -0.1533 -0.7863 0.9756 0.088 Uiso 1 1 calc R . . H38B H -0.2739 -0.7614 0.9669 0.088 Uiso 1 1 calc R . . H38C H -0.2087 -0.7819 0.8956 0.088 Uiso 1 1 calc R . . C39 C -0.2783(3) -1.0794(2) 0.6450(2) 0.0395(9) Uani 1 1 d . . . H39A H -0.2977 -1.0888 0.6971 0.047 Uiso 1 1 calc R . . H39B H -0.2100 -1.1015 0.6348 0.047 Uiso 1 1 calc R . . C40 C -0.3031(3) -0.9867(2) 0.5556(2) 0.0399(9) Uani 1 1 d . . . H40A H -0.2418 -0.9639 0.5243 0.048 Uiso 1 1 calc R . . H40B H -0.3608 -0.9527 0.5561 0.048 Uiso 1 1 calc R . . C41 C -0.3504(4) -1.0648(3) 0.5272(2) 0.0625(14) Uani 1 1 d . . . H41A H -0.2977 -1.0853 0.4945 0.075 Uiso 1 1 calc R . . H41B H -0.4208 -1.0630 0.4998 0.075 Uiso 1 1 calc R . . C42 C -0.3694(4) -1.1128(2) 0.5959(3) 0.0547(12) Uani 1 1 d . . . H42A H -0.4423 -1.1084 0.6173 0.066 Uiso 1 1 calc R . . H42B H -0.3647 -1.1668 0.5854 0.066 Uiso 1 1 calc R . . C43 C -0.1836(4) -0.2732(2) 0.7210(2) 0.0507(11) Uani 1 1 d . . . H43A H -0.2136 -0.2387 0.7557 0.061 Uiso 1 1 calc R . . H43B H -0.1019 -0.2637 0.7200 0.061 Uiso 1 1 calc R . . C44 C -0.2360(3) -0.2783(2) 0.6506(2) 0.0373(9) Uani 1 1 d . . . C45 C -0.3505(3) -0.3052(2) 0.6382(2) 0.0311(8) Uani 1 1 d . . . C46 C -0.3963(3) -0.3129(2) 0.5678(2) 0.0357(9) Uani 1 1 d . . . H46 H -0.4734 -0.3289 0.5618 0.043 Uiso 1 1 calc R . . C47 C -0.3321(4) -0.2978(2) 0.5062(2) 0.0480(11) Uani 1 1 d . . . H47 H -0.3642 -0.3039 0.4583 0.058 Uiso 1 1 calc R . . C48 C -0.2214(4) -0.2741(3) 0.5158(3) 0.0524(12) Uani 1 1 d . . . H48 H -0.1763 -0.2642 0.4740 0.063 Uiso 1 1 calc R . . C49 C -0.1743(3) -0.2645(2) 0.5846(3) 0.0502(11) Uani 1 1 d . . . H49 H -0.0972 -0.2479 0.5888 0.060 Uiso 1 1 calc R . . C50 C -0.5219(3) -0.3728(3) 0.6880(3) 0.0567(12) Uani 1 1 d . . . H50A H -0.5614 -0.3832 0.7341 0.085 Uiso 1 1 calc R . . H50B H -0.5074 -0.4207 0.6660 0.085 Uiso 1 1 calc R . . H50C H -0.5671 -0.3470 0.6539 0.085 Uiso 1 1 calc R . . C51 C -0.4408(4) -0.2558(3) 0.7420(2) 0.0617(14) Uani 1 1 d . . . H51A H -0.4852 -0.2709 0.7852 0.093 Uiso 1 1 calc R . . H51B H -0.4820 -0.2260 0.7090 0.093 Uiso 1 1 calc R . . H51C H -0.3714 -0.2252 0.7576 0.093 Uiso 1 1 calc R . . C52 C -0.0970(3) -0.5231(2) 0.81553(19) 0.0306(8) Uani 1 1 d . . . C53 C -0.1875(3) -0.5702(2) 0.8426(2) 0.0339(9) Uani 1 1 d . . . H53 H -0.1733 -0.6195 0.8559 0.041 Uiso 1 1 calc R . . C54 C -0.2975(3) -0.5563(2) 0.8534(2) 0.0321(8) Uani 1 1 d . . . C55 C -0.3635(3) -0.6131(2) 0.9043(2) 0.0435(10) Uani 1 1 d . . . H55A H -0.4384 -0.6000 0.9092 0.065 Uiso 1 1 calc R . . H55B H -0.3270 -0.6114 0.9528 0.065 Uiso 1 1 calc R . . H55C H -0.3676 -0.6643 0.8836 0.065 Uiso 1 1 calc R . . C56 C 0.0147(3) -0.5508(2) 0.8275(2) 0.0410(10) Uani 1 1 d . . . H56A H 0.0543 -0.5485 0.7810 0.062 Uiso 1 1 calc R . . H56B H 0.0033 -0.6032 0.8451 0.062 Uiso 1 1 calc R . . H56C H 0.0583 -0.5184 0.8641 0.062 Uiso 1 1 calc R . . C57 C -0.0007(3) -0.4056(2) 0.7755(2) 0.0332(9) Uani 1 1 d . . . C58 C 0.0613(3) -0.4032(2) 0.7107(2) 0.0402(10) Uani 1 1 d . . . C59 C 0.1543(3) -0.3489(3) 0.7055(3) 0.0555(12) Uani 1 1 d . . . H59 H 0.1961 -0.3463 0.6618 0.067 Uiso 1 1 calc R . . C60 C 0.1874(3) -0.2987(3) 0.7619(3) 0.0555(12) Uani 1 1 d . . . H60 H 0.2510 -0.2620 0.7571 0.067 Uiso 1 1 calc R . . C61 C 0.1276(3) -0.3024(2) 0.8251(2) 0.0469(11) Uani 1 1 d . . . H61 H 0.1518 -0.2684 0.8643 0.056 Uiso 1 1 calc R . . C62 C 0.0329(3) -0.3543(2) 0.8337(2) 0.0371(9) Uani 1 1 d . . . C63 C 0.0286(3) -0.4584(3) 0.6477(2) 0.0524(12) Uani 1 1 d . . . H63 H -0.0386 -0.4931 0.6626 0.063 Uiso 1 1 calc R . . C64 C 0.1186(4) -0.5073(3) 0.6302(3) 0.0713(15) Uani 1 1 d . . . H64A H 0.0932 -0.5421 0.5898 0.107 Uiso 1 1 calc R . . H64B H 0.1345 -0.5364 0.6738 0.107 Uiso 1 1 calc R . . H64C H 0.1859 -0.4745 0.6158 0.107 Uiso 1 1 calc R . . C65 C -0.0020(5) -0.4162(3) 0.5796(3) 0.0762(16) Uani 1 1 d . . . H65A H -0.0234 -0.4525 0.5397 0.114 Uiso 1 1 calc R . . H65B H 0.0616 -0.3801 0.5648 0.114 Uiso 1 1 calc R . . H65C H -0.0641 -0.3886 0.5905 0.114 Uiso 1 1 calc R . . C66 C -0.0315(4) -0.3566(2) 0.9043(2) 0.0452(10) Uani 1 1 d . . . H66 H -0.1005 -0.3933 0.8972 0.054 Uiso 1 1 calc R . . C67 C 0.0341(5) -0.3840(3) 0.9692(3) 0.0724(15) Uani 1 1 d . . . H67A H -0.0101 -0.3850 1.0137 0.109 Uiso 1 1 calc R . . H67B H 0.1030 -0.3493 0.9766 0.109 Uiso 1 1 calc R . . H67C H 0.0512 -0.4351 0.9587 0.109 Uiso 1 1 calc R . . C68 C -0.0650(4) -0.2788(2) 0.9213(2) 0.0510(11) Uani 1 1 d . . . H68A H -0.1065 -0.2814 0.9670 0.077 Uiso 1 1 calc R . . H68B H -0.1113 -0.2636 0.8810 0.077 Uiso 1 1 calc R . . H68C H 0.0015 -0.2413 0.9269 0.077 Uiso 1 1 calc R . . C69 C -0.4518(3) -0.4866(2) 0.8416(2) 0.0327(8) Uani 1 1 d . . . C70 C -0.4652(3) -0.4225(2) 0.8847(2) 0.0357(9) Uani 1 1 d . . . C71 C -0.5718(3) -0.4040(2) 0.8934(2) 0.0439(10) Uani 1 1 d . . . H71 H -0.5818 -0.3609 0.9222 0.053 Uiso 1 1 calc R . . C72 C -0.6628(3) -0.4468(2) 0.8612(2) 0.0459(11) Uani 1 1 d . . . H72 H -0.7344 -0.4327 0.8668 0.055 Uiso 1 1 calc R . . C73 C -0.6493(3) -0.5100(2) 0.8212(2) 0.0432(10) Uani 1 1 d . . . H73 H -0.7127 -0.5398 0.8002 0.052 Uiso 1 1 calc R . . C74 C -0.5447(3) -0.5322(2) 0.8099(2) 0.0373(9) Uani 1 1 d . . . C75 C -0.3660(3) -0.3770(2) 0.9238(2) 0.0417(10) Uani 1 1 d . . . H75 H -0.3047 -0.3686 0.8877 0.050 Uiso 1 1 calc R . . C76 C -0.3867(4) -0.2989(2) 0.9516(3) 0.0575(12) Uani 1 1 d . . . H76A H -0.3194 -0.2732 0.9757 0.086 Uiso 1 1 calc R . . H76B H -0.4470 -0.3052 0.9868 0.086 Uiso 1 1 calc R . . H76C H -0.4071 -0.2684 0.9100 0.086 Uiso 1 1 calc R . . C77 C -0.3255(4) -0.4218(2) 0.9883(2) 0.0486(11) Uani 1 1 d . . . H77A H -0.2617 -0.3917 1.0124 0.073 Uiso 1 1 calc R . . H77B H -0.3039 -0.4694 0.9700 0.073 Uiso 1 1 calc R . . H77C H -0.3850 -0.4331 1.0236 0.073 Uiso 1 1 calc R . . C78 C -0.5363(3) -0.6025(2) 0.7649(2) 0.0424(10) Uani 1 1 d . . . H78 H -0.4573 -0.6115 0.7663 0.051 Uiso 1 1 calc R . . C79 C -0.5695(4) -0.5930(3) 0.6843(2) 0.0605(13) Uani 1 1 d . . . H79A H -0.5626 -0.6396 0.6571 0.091 Uiso 1 1 calc R . . H79B H -0.5209 -0.5505 0.6630 0.091 Uiso 1 1 calc R . . H79C H -0.6463 -0.5827 0.6813 0.091 Uiso 1 1 calc R . . C80 C -0.6055(4) -0.6726(3) 0.7969(3) 0.0641(14) Uani 1 1 d . . . H80A H -0.5978 -0.7170 0.7664 0.096 Uiso 1 1 calc R . . H80B H -0.6833 -0.6648 0.7976 0.096 Uiso 1 1 calc R . . H80C H -0.5795 -0.6809 0.8471 0.096 Uiso 1 1 calc R . . C81 C -0.2710(3) -0.5754(2) 0.6466(2) 0.0407(10) Uani 1 1 d . . . H81A H -0.3332 -0.6096 0.6676 0.049 Uiso 1 1 calc R . . H81B H -0.2054 -0.5745 0.6795 0.049 Uiso 1 1 calc R . . C82 C -0.3314(4) -0.4899(2) 0.5600(2) 0.0475(11) Uani 1 1 d . . . H82A H -0.2776 -0.4513 0.5360 0.057 Uiso 1 1 calc R . . H82B H -0.4057 -0.4739 0.5560 0.057 Uiso 1 1 calc R . . C83 C -0.2464(4) -0.6004(2) 0.5709(2) 0.0503(11) Uani 1 1 d . . . H83A H -0.2567 -0.6564 0.5666 0.060 Uiso 1 1 calc R . . H83B H -0.1702 -0.5800 0.5567 0.060 Uiso 1 1 calc R . . C84 C -0.3311(4) -0.5664(2) 0.5251(2) 0.0511(11) Uani 1 1 d . . . H84A H -0.3091 -0.5617 0.4731 0.061 Uiso 1 1 calc R . . H84B H -0.4047 -0.5974 0.5279 0.061 Uiso 1 1 calc R . . N1 N -0.3024(2) -0.97893(17) 0.82749(16) 0.0302(7) Uani 1 1 d . . . N2 N -0.0720(2) -0.98205(16) 0.77815(16) 0.0296(7) Uani 1 1 d . . . N3 N -0.1087(2) -0.80248(17) 0.64285(17) 0.0358(7) Uani 1 1 d . . . N4 N -0.3410(2) -0.49887(16) 0.82503(16) 0.0310(7) Uani 1 1 d . . . N5 N -0.4165(3) -0.32419(18) 0.70309(17) 0.0385(8) Uani 1 1 d . . . N6 N -0.1017(2) -0.45647(16) 0.78269(15) 0.0286(7) Uani 1 1 d . . . O1 O -0.2630(2) -0.99883(13) 0.62977(13) 0.0357(6) Uani 1 1 d . . . O2 O -0.2999(2) -0.49943(15) 0.63688(14) 0.0417(7) Uiso 1 1 d . . . Ca1 Ca -0.21078(6) -0.91304(4) 0.72694(4) 0.02923(18) Uani 1 1 d . . . Ca2 Ca -0.26321(6) -0.41187(4) 0.73390(4) 0.02917(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.067(3) 0.039(3) 0.059(3) 0.007(2) 0.022(2) 0.020(2) C2 0.041(2) 0.026(2) 0.062(3) 0.0085(19) 0.000(2) 0.0123(17) C3 0.040(2) 0.023(2) 0.044(2) 0.0018(17) -0.0019(17) 0.0044(16) C4 0.069(3) 0.031(2) 0.046(3) 0.0010(19) -0.012(2) 0.010(2) C5 0.094(4) 0.039(3) 0.065(3) -0.002(2) -0.045(3) 0.013(3) C6 0.067(4) 0.033(3) 0.113(5) 0.003(3) -0.049(3) 0.008(2) C7 0.038(3) 0.035(3) 0.108(5) 0.008(3) -0.003(3) 0.0085(19) C8 0.044(3) 0.059(3) 0.058(3) 0.017(2) 0.015(2) 0.014(2) C9 0.043(3) 0.044(3) 0.076(3) 0.008(2) -0.015(2) -0.004(2) C10 0.033(2) 0.037(2) 0.035(2) 0.0034(18) 0.0054(16) 0.0034(17) C11 0.040(2) 0.026(2) 0.043(2) 0.0050(17) 0.0059(17) 0.0061(16) C12 0.030(2) 0.031(2) 0.033(2) -0.0002(17) -0.0008(15) 0.0084(16) C13 0.036(2) 0.045(2) 0.047(2) 0.013(2) -0.0011(18) 0.0151(18) C14 0.045(2) 0.046(3) 0.065(3) 0.020(2) 0.020(2) 0.009(2) C15 0.0249(18) 0.032(2) 0.035(2) 0.0054(17) -0.0018(15) 0.0061(15) C16 0.0267(19) 0.035(2) 0.034(2) 0.0003(17) -0.0019(15) 0.0060(16) C17 0.031(2) 0.044(2) 0.045(2) -0.0011(19) 0.0061(17) 0.0091(18) C18 0.025(2) 0.044(3) 0.060(3) 0.005(2) 0.0096(18) -0.0010(17) C19 0.031(2) 0.033(2) 0.056(3) -0.0007(19) -0.0020(18) -0.0003(17) C20 0.0282(19) 0.033(2) 0.039(2) -0.0002(17) -0.0011(16) 0.0044(16) C21 0.030(2) 0.038(2) 0.036(2) 0.0009(17) 0.0012(16) 0.0054(16) C22 0.042(2) 0.042(2) 0.058(3) -0.006(2) -0.001(2) 0.0121(19) C23 0.043(2) 0.047(3) 0.039(2) -0.0033(19) 0.0002(18) 0.0052(19) C24 0.039(2) 0.044(2) 0.043(2) -0.0063(19) -0.0008(18) 0.0046(18) C25 0.071(3) 0.058(3) 0.041(3) -0.002(2) -0.005(2) 0.005(2) C26 0.086(4) 0.044(3) 0.051(3) -0.012(2) 0.003(2) 0.003(2) C27 0.0296(19) 0.033(2) 0.033(2) 0.0069(17) 0.0033(15) 0.0054(16) C28 0.033(2) 0.038(2) 0.036(2) 0.0031(18) 0.0015(16) 0.0074(17) C29 0.044(2) 0.045(2) 0.039(2) -0.0029(19) 0.0039(18) 0.0097(19) C30 0.036(2) 0.054(3) 0.047(3) 0.003(2) 0.0068(19) 0.019(2) C31 0.030(2) 0.058(3) 0.048(3) 0.002(2) 0.0002(18) 0.0091(19) C32 0.031(2) 0.046(2) 0.037(2) 0.0004(19) 0.0001(16) 0.0052(17) C33 0.030(2) 0.057(3) 0.048(3) -0.001(2) -0.0016(18) 0.0078(19) C34 0.050(3) 0.074(3) 0.046(3) -0.001(2) -0.002(2) 0.022(2) C35 0.055(3) 0.065(3) 0.071(3) -0.017(3) 0.000(2) -0.014(2) C36 0.039(2) 0.051(3) 0.043(2) -0.008(2) -0.0036(18) 0.0101(19) C37 0.074(4) 0.109(5) 0.066(4) 0.023(3) -0.027(3) 0.005(3) C38 0.051(3) 0.057(3) 0.065(3) -0.008(2) -0.013(2) -0.002(2) C39 0.044(2) 0.030(2) 0.045(2) 0.0061(18) 0.0010(18) 0.0050(17) C40 0.045(2) 0.041(2) 0.032(2) 0.0035(18) -0.0047(17) 0.0013(18) C41 0.092(4) 0.048(3) 0.040(3) 0.000(2) -0.011(2) -0.019(3) C42 0.057(3) 0.038(3) 0.067(3) 0.002(2) -0.012(2) 0.002(2) C43 0.054(3) 0.030(2) 0.066(3) 0.007(2) -0.024(2) -0.0024(19) C44 0.043(2) 0.023(2) 0.045(2) 0.0069(17) -0.0084(18) 0.0022(16) C45 0.033(2) 0.0253(19) 0.036(2) 0.0039(16) 0.0001(16) 0.0088(15) C46 0.036(2) 0.032(2) 0.039(2) 0.0019(17) -0.0040(17) 0.0058(17) C47 0.068(3) 0.045(3) 0.033(2) 0.0011(19) -0.002(2) 0.016(2) C48 0.054(3) 0.054(3) 0.052(3) 0.014(2) 0.019(2) 0.013(2) C49 0.032(2) 0.043(3) 0.075(3) 0.018(2) 0.007(2) 0.0028(18) C50 0.039(2) 0.066(3) 0.067(3) 0.027(3) 0.010(2) 0.011(2) C51 0.091(4) 0.055(3) 0.047(3) 0.012(2) 0.025(3) 0.037(3) C52 0.033(2) 0.032(2) 0.0264(19) -0.0036(16) -0.0030(15) 0.0061(16) C53 0.040(2) 0.028(2) 0.035(2) 0.0039(17) 0.0010(17) 0.0060(16) C54 0.037(2) 0.027(2) 0.031(2) 0.0004(16) 0.0045(16) 0.0019(16) C55 0.047(2) 0.037(2) 0.047(3) 0.0126(19) 0.0098(19) 0.0051(18) C56 0.034(2) 0.043(2) 0.048(3) 0.008(2) -0.0010(18) 0.0114(18) C57 0.0271(19) 0.036(2) 0.036(2) 0.0071(17) -0.0001(16) 0.0030(16) C58 0.030(2) 0.051(3) 0.039(2) 0.0018(19) 0.0012(17) 0.0037(18) C59 0.038(2) 0.067(3) 0.060(3) 0.011(3) 0.012(2) 0.001(2) C60 0.033(2) 0.047(3) 0.082(4) 0.011(3) -0.002(2) -0.0099(19) C61 0.044(2) 0.038(2) 0.055(3) 0.002(2) -0.010(2) -0.0045(19) C62 0.037(2) 0.035(2) 0.038(2) 0.0031(18) -0.0086(17) -0.0013(17) C63 0.042(2) 0.075(3) 0.039(3) -0.002(2) 0.0094(19) 0.001(2) C64 0.090(4) 0.073(4) 0.057(3) 0.004(3) 0.009(3) 0.029(3) C65 0.083(4) 0.100(4) 0.054(3) -0.013(3) -0.009(3) 0.045(3) C66 0.056(3) 0.040(2) 0.036(2) -0.0038(19) -0.0024(19) -0.0089(19) C67 0.124(5) 0.049(3) 0.045(3) 0.007(2) -0.011(3) 0.018(3) C68 0.057(3) 0.052(3) 0.042(3) -0.007(2) -0.007(2) 0.002(2) C69 0.033(2) 0.031(2) 0.034(2) 0.0049(17) 0.0087(16) 0.0051(16) C70 0.038(2) 0.030(2) 0.039(2) 0.0077(18) 0.0097(17) 0.0044(16) C71 0.052(3) 0.035(2) 0.047(3) 0.0076(19) 0.018(2) 0.013(2) C72 0.035(2) 0.053(3) 0.053(3) 0.013(2) 0.0128(19) 0.013(2) C73 0.029(2) 0.049(3) 0.050(3) 0.012(2) 0.0059(18) 0.0013(18) C74 0.032(2) 0.039(2) 0.041(2) 0.0065(18) 0.0062(17) 0.0013(17) C75 0.053(3) 0.032(2) 0.041(2) 0.0023(18) 0.0110(19) 0.0052(18) C76 0.079(3) 0.038(3) 0.055(3) -0.007(2) 0.002(2) 0.007(2) C77 0.060(3) 0.046(3) 0.040(2) -0.002(2) 0.004(2) 0.007(2) C78 0.035(2) 0.043(2) 0.047(3) -0.008(2) 0.0036(18) -0.0014(18) C79 0.053(3) 0.073(3) 0.054(3) -0.018(3) -0.008(2) 0.005(2) C80 0.057(3) 0.046(3) 0.085(4) -0.005(3) 0.013(3) -0.008(2) C81 0.048(2) 0.029(2) 0.047(2) -0.0019(18) -0.0036(19) 0.0092(18) C82 0.059(3) 0.052(3) 0.034(2) 0.002(2) -0.0073(19) 0.016(2) C83 0.066(3) 0.035(2) 0.051(3) -0.001(2) 0.015(2) 0.007(2) C84 0.062(3) 0.051(3) 0.038(2) -0.012(2) -0.002(2) 0.001(2) N1 0.0268(16) 0.0325(17) 0.0315(17) 0.0017(14) 0.0005(12) 0.0054(13) N2 0.0240(15) 0.0307(17) 0.0340(17) 0.0018(14) 0.0004(12) 0.0032(12) N3 0.0327(17) 0.0295(17) 0.045(2) 0.0014(15) -0.0007(14) 0.0034(13) N4 0.0323(16) 0.0294(17) 0.0308(17) 0.0014(14) 0.0046(13) 0.0016(13) N5 0.0443(19) 0.0363(19) 0.0365(19) 0.0085(15) 0.0076(15) 0.0102(15) N6 0.0288(16) 0.0259(16) 0.0306(17) -0.0014(13) 0.0010(12) 0.0017(12) O1 0.0451(15) 0.0278(14) 0.0339(15) 0.0000(11) -0.0050(11) 0.0044(11) Ca1 0.0283(4) 0.0294(4) 0.0305(4) 0.0020(3) -0.0014(3) 0.0058(3) Ca2 0.0301(4) 0.0273(4) 0.0298(4) 0.0017(3) -0.0004(3) 0.0031(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.421(6) . ? C1 Ca1 2.535(4) . ? C2 C3 1.422(5) . ? C2 C7 1.432(6) . ? C2 Ca1 2.886(4) . ? C3 C4 1.398(5) . ? C3 N3 1.450(5) . ? C3 Ca1 2.979(4) . ? C4 C5 1.373(6) . ? C5 C6 1.382(7) . ? C6 C7 1.370(7) . ? C8 N3 1.468(5) . ? C9 N3 1.470(5) . ? C10 N1 1.324(5) . ? C10 C11 1.403(5) . ? C10 C14 1.520(5) . ? C11 C12 1.402(5) . ? C12 N2 1.324(4) . ? C12 C13 1.521(5) . ? C15 C16 1.405(5) . ? C15 C20 1.416(5) . ? C15 N2 1.432(4) . ? C15 Ca1 3.177(3) . ? C16 C17 1.395(5) . ? C16 C21 1.526(5) . ? C17 C18 1.377(5) . ? C18 C19 1.380(6) . ? C19 C20 1.391(5) . ? C20 C24 1.534(5) . ? C21 C23 1.527(5) . ? C21 C22 1.533(5) . ? C24 C25 1.518(6) . ? C24 C26 1.519(6) . ? C27 C32 1.403(5) . ? C27 C28 1.409(5) . ? C27 N1 1.443(4) . ? C27 Ca1 3.234(3) . ? C28 C29 1.387(5) . ? C28 C36 1.522(5) . ? C29 C30 1.384(5) . ? C30 C31 1.375(6) . ? C31 C32 1.386(5) . ? C32 C33 1.528(6) . ? C33 C34 1.517(6) . ? C33 C35 1.528(6) . ? C36 C38 1.510(6) . ? C36 C37 1.539(6) . ? C39 O1 1.448(4) . ? C39 C42 1.473(5) . ? C40 O1 1.455(4) . ? C40 C41 1.515(6) . ? C41 C42 1.518(6) . ? C43 C44 1.419(5) . ? C43 Ca2 2.538(4) . ? C44 C45 1.428(5) . ? C44 C49 1.432(6) . ? C44 Ca2 2.807(4) . ? C45 C46 1.387(5) . ? C45 N5 1.456(5) . ? C45 Ca2 2.878(3) . ? C46 C47 1.385(5) . ? C47 C48 1.368(6) . ? C48 C49 1.369(6) . ? C50 N5 1.471(5) . ? C51 N5 1.474(5) . ? C52 N6 1.338(4) . ? C52 C53 1.389(5) . ? C52 C56 1.526(5) . ? C53 C54 1.416(5) . ? C54 N4 1.316(4) . ? C54 C55 1.529(5) . ? C57 C58 1.410(5) . ? C57 C62 1.416(5) . ? C57 N6 1.435(4) . ? C58 C59 1.392(6) . ? C58 C63 1.521(6) . ? C59 C60 1.377(6) . ? C60 C61 1.370(6) . ? C61 C62 1.389(5) . ? C62 C66 1.516(5) . ? C63 C65 1.517(6) . ? C63 C64 1.531(6) . ? C66 C68 1.530(6) . ? C66 C67 1.532(6) . ? C69 C70 1.413(5) . ? C69 C74 1.414(5) . ? C69 N4 1.438(4) . ? C69 Ca2 3.202(3) . ? C70 C71 1.399(5) . ? C70 C75 1.526(5) . ? C71 C72 1.379(6) . ? C72 C73 1.368(6) . ? C73 C74 1.407(5) . ? C74 C78 1.510(5) . ? C75 C76 1.532(6) . ? C75 C77 1.533(6) . ? C78 C79 1.530(6) . ? C78 C80 1.530(6) . ? C81 02 1.454(4) . ? C81 C83 1.495(5) . ? C82 02 1.462(4) . ? C82 C84 1.502(6) . ? C83 C84 1.507(6) . ? N1 Ca1 2.387(3) . ? N2 Ca1 2.402(3) . ? N3 Ca1 2.679(3) . ? N4 Ca2 2.390(3) . ? N5 Ca2 2.650(3) . ? N6 Ca2 2.383(3) . ? O1 Ca1 2.355(3) . ? 02 Ca2 2.349(3) . ? 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 C2 C1 Ca1 89.1(2) . . ? C1 C2 C3 122.9(4) . . ? C1 C2 C7 122.3(4) . . ? C3 C2 C7 114.6(4) . . ? C1 C2 Ca1 61.4(2) . . ? C3 C2 Ca1 79.6(2) . . ? C7 C2 Ca1 129.8(3) . . ? C4 C3 C2 121.4(4) . . ? C4 C3 N3 121.7(4) . . ? C2 C3 N3 116.9(3) . . ? C4 C3 Ca1 134.9(3) . . ? C2 C3 Ca1 72.4(2) . . ? N3 C3 Ca1 63.91(18) . . ? C5 C4 C3 121.6(5) . . ? C4 C5 C6 118.4(5) . . ? C7 C6 C5 121.4(4) . . ? C6 C7 C2 122.6(5) . . ? N1 C10 C11 124.5(3) . . ? N1 C10 C14 120.0(3) . . ? C11 C10 C14 115.4(3) . . ? C12 C11 C10 129.5(3) . . ? N2 C12 C11 124.1(3) . . ? N2 C12 C13 120.9(3) . . ? C11 C12 C13 115.0(3) . . ? C16 C15 C20 120.3(3) . . ? C16 C15 N2 121.7(3) . . ? C20 C15 N2 117.7(3) . . ? C16 C15 Ca1 117.5(2) . . ? C20 C15 Ca1 99.1(2) . . ? N2 C15 Ca1 45.52(15) . . ? C17 C16 C15 118.3(3) . . ? C17 C16 C21 118.7(3) . . ? C15 C16 C21 122.9(3) . . ? C18 C17 C16 121.7(4) . . ? C17 C18 C19 119.8(4) . . ? C18 C19 C20 120.9(4) . . ? C19 C20 C15 118.9(3) . . ? C19 C20 C24 120.6(3) . . ? C15 C20 C24 120.4(3) . . ? C16 C21 C23 111.0(3) . . ? C16 C21 C22 112.5(3) . . ? C23 C21 C22 109.3(3) . . ? C25 C24 C26 109.9(4) . . ? C25 C24 C20 111.0(3) . . ? C26 C24 C20 113.9(3) . . ? C32 C27 C28 119.8(3) . . ? C32 C27 N1 120.9(3) . . ? C28 C27 N1 119.2(3) . . ? C32 C27 Ca1 107.1(2) . . ? C28 C27 Ca1 113.7(2) . . ? N1 C27 Ca1 42.84(15) . . ? C29 C28 C27 118.8(3) . . ? C29 C28 C36 119.6(4) . . ? C27 C28 C36 121.6(3) . . ? C30 C29 C28 121.5(4) . . ? C31 C30 C29 119.1(4) . . ? C30 C31 C32 121.6(4) . . ? C31 C32 C27 119.2(4) . . ? C31 C32 C33 119.6(3) . . ? C27 C32 C33 121.2(3) . . ? C34 C33 C35 110.4(4) . . ? C34 C33 C32 111.4(4) . . ? C35 C33 C32 111.3(3) . . ? C38 C36 C28 112.0(3) . . ? C38 C36 C37 109.1(4) . . ? C28 C36 C37 111.2(3) . . ? O1 C39 C42 105.7(3) . . ? O1 C40 C41 105.3(3) . . ? C40 C41 C42 104.5(3) . . ? C39 C42 C41 102.4(3) . . ? C44 C43 Ca2 85.4(2) . . ? C43 C44 C45 123.9(4) . . ? C43 C44 C49 121.7(4) . . ? C45 C44 C49 114.0(4) . . ? C43 C44 Ca2 64.3(2) . . ? C45 C44 Ca2 78.2(2) . . ? C49 C44 Ca2 127.2(3) . . ? C46 C45 C44 121.6(3) . . ? C46 C45 N5 121.8(3) . . ? C44 C45 N5 116.6(3) . . ? C46 C45 Ca2 131.7(3) . . ? C44 C45 Ca2 72.72(19) . . ? N5 C45 Ca2 66.21(17) . . ? C47 C46 C45 121.5(4) . . ? C48 C47 C46 118.6(4) . . ? C47 C48 C49 121.2(4) . . ? C48 C49 C44 123.1(4) . . ? N6 C52 C53 124.9(3) . . ? N6 C52 C56 119.5(3) . . ? C53 C52 C56 115.5(3) . . ? C52 C53 C54 130.3(3) . . ? N4 C54 C53 124.6(3) . . ? N4 C54 C55 121.3(3) . . ? C53 C54 C55 114.0(3) . . ? C58 C57 C62 120.1(3) . . ? C58 C57 N6 121.5(3) . . ? C62 C57 N6 118.3(3) . . ? C59 C58 C57 118.4(4) . . ? C59 C58 C63 120.2(4) . . ? C57 C58 C63 121.4(3) . . ? C60 C59 C58 121.8(4) . . ? C61 C60 C59 119.3(4) . . ? C60 C61 C62 122.1(4) . . ? C61 C62 C57 118.3(4) . . ? C61 C62 C66 120.7(4) . . ? C57 C62 C66 121.0(3) . . ? C65 C63 C58 110.5(4) . . ? C65 C63 C64 110.4(4) . . ? C58 C63 C64 112.7(4) . . ? C62 C66 C68 110.7(3) . . ? C62 C66 C67 111.7(4) . . ? C68 C66 C67 110.4(3) . . ? C70 C69 C74 120.6(3) . . ? C70 C69 N4 117.6(3) . . ? C74 C69 N4 121.4(3) . . ? C70 C69 Ca2 99.7(2) . . ? C74 C69 Ca2 117.9(2) . . ? N4 C69 Ca2 44.17(15) . . ? C71 C70 C69 118.5(4) . . ? C71 C70 C75 120.9(4) . . ? C69 C70 C75 120.6(3) . . ? C72 C71 C70 121.4(4) . . ? C73 C72 C71 119.6(4) . . ? C72 C73 C74 122.3(4) . . ? C73 C74 C69 117.5(4) . . ? C73 C74 C78 119.2(3) . . ? C69 C74 C78 123.2(3) . . ? C70 C75 C76 114.3(3) . . ? C70 C75 C77 110.9(3) . . ? C76 C75 C77 109.0(3) . . ? C74 C78 C79 112.1(4) . . ? C74 C78 C80 111.7(3) . . ? C79 C78 C80 109.9(4) . . ? 02 C81 C83 104.5(3) . . ? 02 C82 C84 105.1(3) . . ? C81 C83 C84 101.8(3) . . ? C82 C84 C83 102.9(3) . . ? C10 N1 C27 117.8(3) . . ? C10 N1 Ca1 129.2(2) . . ? C27 N1 Ca1 112.9(2) . . ? C12 N2 C15 121.0(3) . . ? C12 N2 Ca1 129.6(2) . . ? C15 N2 Ca1 109.3(2) . . ? C3 N3 C8 114.2(3) . . ? C3 N3 C9 110.9(3) . . ? C8 N3 C9 107.8(3) . . ? C3 N3 Ca1 87.0(2) . . ? C8 N3 Ca1 107.2(2) . . ? C9 N3 Ca1 128.6(3) . . ? C54 N4 C69 121.2(3) . . ? C54 N4 Ca2 127.4(2) . . ? C69 N4 Ca2 111.0(2) . . ? C45 N5 C50 114.2(3) . . ? C45 N5 C51 111.8(3) . . ? C50 N5 C51 107.9(3) . . ? C45 N5 Ca2 83.61(19) . . ? C50 N5 Ca2 108.6(2) . . ? C51 N5 Ca2 128.9(3) . . ? C52 N6 C57 118.1(3) . . ? C52 N6 Ca2 126.5(2) . . ? C57 N6 Ca2 115.5(2) . . ? C39 O1 C40 109.1(3) . . ? C39 O1 Ca1 118.9(2) . . ? C40 O1 Ca1 131.1(2) . . ? C81 02 C82 108.9(3) . . ? C81 02 Ca2 118.6(2) . . ? C82 02 Ca2 131.6(2) . . ? O1 Ca1 N1 101.11(10) . . ? O1 Ca1 N2 95.50(9) . . ? N1 Ca1 N2 76.84(10) . . ? O1 Ca1 C1 121.20(13) . . ? N1 Ca1 C1 99.33(12) . . ? N2 Ca1 C1 142.88(14) . . ? O1 Ca1 N3 95.77(9) . . ? N1 Ca1 N3 162.05(10) . . ? N2 Ca1 N3 107.75(9) . . ? C1 Ca1 N3 66.25(12) . . ? O1 Ca1 C2 94.54(11) . . ? N1 Ca1 C2 119.83(11) . . ? N2 Ca1 C2 158.31(11) . . ? C1 Ca1 C2 29.49(13) . . ? N3 Ca1 C2 52.02(10) . . ? O1 Ca1 C3 83.53(10) . . ? N1 Ca1 C3 147.47(10) . . ? N2 Ca1 C3 135.21(10) . . ? C1 Ca1 C3 53.12(12) . . ? N3 Ca1 C3 29.09(9) . . ? C2 Ca1 C3 28.00(11) . . ? O1 Ca1 C15 97.62(9) . . ? N1 Ca1 C15 101.04(9) . . ? N2 Ca1 C15 25.17(9) . . ? C1 Ca1 C15 131.11(13) . . ? N3 Ca1 C15 82.59(9) . . ? C2 Ca1 C15 133.96(10) . . ? C3 Ca1 C15 110.31(10) . . ? O1 Ca1 C27 107.30(9) . . ? N1 Ca1 C27 24.27(9) . . ? N2 Ca1 C27 99.61(9) . . ? C1 Ca1 C27 76.11(12) . . ? N3 Ca1 C27 142.15(9) . . ? C2 Ca1 C27 95.67(10) . . ? C3 Ca1 C27 123.54(10) . . ? C15 Ca1 C27 122.12(9) . . ? 02 Ca2 N6 97.93(10) . . ? 02 Ca2 N4 94.15(10) . . ? N6 Ca2 N4 78.79(10) . . ? 02 Ca2 C43 125.57(13) . . ? N6 Ca2 C43 97.84(12) . . ? N4 Ca2 C43 140.02(13) . . ? 02 Ca2 N5 98.94(10) . . ? N6 Ca2 N5 162.11(10) . . ? N4 Ca2 N5 105.81(10) . . ? C43 Ca2 N5 67.30(12) . . ? 02 Ca2 C44 98.33(10) . . ? N6 Ca2 C44 118.05(10) . . ? N4 Ca2 C44 157.10(11) . . ? C43 Ca2 C44 30.26(12) . . ? N5 Ca2 C44 53.35(10) . . ? 02 Ca2 C45 86.30(10) . . ? N6 Ca2 C45 146.45(10) . . ? N4 Ca2 C45 134.33(10) . . ? C43 Ca2 C45 54.85(11) . . ? N5 Ca2 C45 30.18(9) . . ? C44 Ca2 C45 29.06(10) . . ? 02 Ca2 C69 97.53(10) . . ? N6 Ca2 C69 102.61(10) . . ? N4 Ca2 C69 24.78(9) . . ? C43 Ca2 C69 128.71(13) . . ? N5 Ca2 C69 81.03(9) . . ? C44 Ca2 C69 133.42(10) . . ? C45 Ca2 C69 109.83(10) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.07 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.474 _refine_diff_density_min -0.324 _refine_diff_density_rms 0.056