Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_address ; Freie Universitaet Berlin Fabeckstr. 34-36 14195 Berlin Bundesrepublik Deutschland ; ; Freie Universitaet Berlin Fabeckstr. 34-36 14195 Berlin Bundesrepublik Deutschland ; _publ_contact_author_name 'Peter Roesky' _publ_contact_author_address ; Fachbereich Biologie Chemie Pharmazie Freie Universitat Berlin Institut fur Chemie/Anorgoranische Fabeckstrasse, 34-36 Berlin D-14195 GERMANY ; _publ_contact_author_email ROESKY@CHEMIE.FU-BERLIN.DE _publ_section_title ; Aminotroponiminate Calcium and Strontium Complexes ; _publ_contact_author ; Prof. Dr. Peter Roesky Freie Universitaet Berlin Fabeckstr. 34-36 14195 Berlin Bundesrepublik Deutschland ; _publ_contact_author_fax +49/(0)3083852440 _publ_contact_author_phone +49/(0)3083854004 _publ_contact_letter ; ; _publ_requested_coeditor_name ? _publ_author_name 'Peter Roesky' data_1 _database_code_depnum_ccdc_archive 'CCDC 671208' _audit_creation_date 07-08-06 _audit_creation_method 'STOE X-RED' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H43 Ca I N2 O3' _chemical_formula_sum 'C25 H43 Ca I N2 O3' _chemical_formula_weight 586.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.4679(7) _cell_length_b 15.1307(10) _cell_length_c 19.5790(14) _cell_angle_alpha 69.776(5) _cell_angle_beta 81.096(5) _cell_angle_gamma 88.200(5) _cell_volume 2874.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 16235 _cell_measurement_theta_min 2.70 _cell_measurement_theta_max 29.50 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.471 _exptl_crystal_size_mid 0.324 _exptl_crystal_size_min 0.102 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.356 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1216 _exptl_absorpt_coefficient_mu 1.318 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.6965 _exptl_absorpt_correction_T_max 0.8546 _exptl_absorpt_process_details 'STOE X-RED & X-SHAPE' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'STOE IPDS 2T' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21744 _diffrn_reflns_av_R_equivalents 0.0470 _diffrn_reflns_av_sigmaI/netI 0.0559 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.70 _diffrn_reflns_theta_max 25.02 _reflns_number_total 10113 _reflns_number_gt 7248 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA, PLATON (A.L.Spek, 2005)' _computing_data_reduction 'STOE X-RED, PLATON (A.L.Spek, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e' _computing_publication_material 'X-STEP32, Microsoft Word' _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^+0.0000P] 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 10113 _refine_ls_number_parameters 581 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0647 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.0810 _refine_ls_wR_factor_gt 0.0744 _refine_ls_goodness_of_fit_ref 0.976 _refine_ls_restrained_S_all 0.976 _refine_ls_shift/su_max 0.002 _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 0.7569(3) -0.2751(2) 0.35643(19) 0.0319(7) Uani 1 1 d . . . C2 C 0.6573(4) -0.3160(3) 0.4185(2) 0.0418(9) Uani 1 1 d . . . H2 H 0.5877 -0.2754 0.4225 0.050 Uiso 1 1 calc R . . C3 C 0.6446(4) -0.4028(3) 0.4726(2) 0.0484(10) Uani 1 1 d . . . H3 H 0.5667 -0.4136 0.5068 0.058 Uiso 1 1 calc R . . C4 C 0.7285(5) -0.4773(3) 0.4850(2) 0.0538(11) Uani 1 1 d . . . H4 H 0.6964 -0.5367 0.5191 0.065 Uiso 1 1 calc R . . C5 C 0.8545(5) -0.4714(3) 0.4516(2) 0.0517(10) Uani 1 1 d . . . H5 H 0.8994 -0.5290 0.4643 0.062 Uiso 1 1 calc R . . C6 C 0.9267(4) -0.3940(3) 0.4018(2) 0.0477(10) Uani 1 1 d . . . H6 H 1.0159 -0.4065 0.3920 0.057 Uiso 1 1 calc R . . C7 C 0.8947(3) -0.3003(2) 0.36257(19) 0.0334(8) Uani 1 1 d . . . C8 C 0.6006(3) -0.1861(3) 0.2828(2) 0.0417(9) Uani 1 1 d . . . H8 H 0.5421 -0.2382 0.3183 0.050 Uiso 1 1 calc R . . C9 C 0.5613(4) -0.0948(3) 0.2958(3) 0.0567(12) Uani 1 1 d . . . H9A H 0.5631 -0.1026 0.3475 0.085 Uiso 1 1 calc R . . H9B H 0.4737 -0.0791 0.2844 0.085 Uiso 1 1 calc R . . H9C H 0.6219 -0.0439 0.2640 0.085 Uiso 1 1 calc R . . C10 C 0.5894(4) -0.1805(3) 0.2052(2) 0.0575(11) Uani 1 1 d . . . H10A H 0.6447 -0.1286 0.1697 0.086 Uiso 1 1 calc R . . H10B H 0.4994 -0.1695 0.1970 0.086 Uiso 1 1 calc R . . H10C H 0.6170 -0.2399 0.1985 0.086 Uiso 1 1 calc R . . C11 C 1.1151(4) -0.2452(3) 0.3389(2) 0.0554(11) Uani 1 1 d . . . H11 H 1.1158 -0.2929 0.3892 0.067 Uiso 1 1 calc R . . C12 C 1.1714(5) -0.1528(4) 0.3369(3) 0.0778(15) Uani 1 1 d . . . H12A H 1.1716 -0.1053 0.2878 0.117 Uiso 1 1 calc R . . H12B H 1.2602 -0.1621 0.3476 0.117 Uiso 1 1 calc R . . H12C H 1.1187 -0.1313 0.3738 0.117 Uiso 1 1 calc R . . C13 C 1.1961(5) -0.2805(4) 0.2836(3) 0.0810(16) Uani 1 1 d . . . H13A H 1.1526 -0.3352 0.2807 0.122 Uiso 1 1 calc R . . H13B H 1.2808 -0.2986 0.2988 0.122 Uiso 1 1 calc R . . H13C H 1.2076 -0.2305 0.2351 0.122 Uiso 1 1 calc R . . C14 C 0.8463(6) -0.0619(4) 0.3855(3) 0.0763(15) Uani 1 1 d . B . H14A H 0.7572 -0.0882 0.3953 0.092 Uiso 1 1 calc R . . H14B H 0.9048 -0.1139 0.4058 0.092 Uiso 1 1 calc R . . C15 C 0.8516(9) 0.0090(5) 0.4186(4) 0.125(3) Uani 1 1 d . . . H15A H 0.7673 0.0106 0.4490 0.150 Uiso 1 1 calc R A 1 H15B H 0.9185 -0.0071 0.4514 0.150 Uiso 1 1 calc R A 1 C16A C 0.8807(12) 0.0975(7) 0.3645(6) 0.065(3) Uiso 0.50 1 d P B 1 H16A H 0.9669 0.1207 0.3667 0.078 Uiso 0.50 1 calc PR B 1 H16B H 0.8153 0.1436 0.3715 0.078 Uiso 0.50 1 calc PR B 1 C16B C 0.8168(14) 0.1026(9) 0.3515(7) 0.083(4) Uiso 0.50 1 d P B 2 H16C H 0.7224 0.1076 0.3509 0.100 Uiso 0.50 1 calc PR B 2 H16D H 0.8510 0.1611 0.3546 0.100 Uiso 0.50 1 calc PR B 2 C17 C 0.8793(7) 0.0839(3) 0.2916(3) 0.0915(19) Uani 1 1 d . . . H17A H 0.7987 0.1082 0.2718 0.110 Uiso 1 1 calc R B 1 H17B H 0.9542 0.1172 0.2552 0.110 Uiso 1 1 calc R B 1 C18 C 0.9099(5) -0.1723(3) 0.0700(2) 0.0628(12) Uani 1 1 d . . . H18A H 0.9695 -0.1212 0.0356 0.075 Uiso 1 1 calc R . . H18B H 0.8201 -0.1502 0.0682 0.075 Uiso 1 1 calc R . . C19 C 0.9260(8) -0.2577(4) 0.0497(3) 0.098(2) Uani 1 1 d . . . H19A H 0.8504 -0.2675 0.0281 0.118 Uiso 1 1 calc R . . H19B H 1.0047 -0.2512 0.0129 0.118 Uiso 1 1 calc R . . C20 C 0.9372(7) -0.3370(4) 0.1165(3) 0.0852(17) Uani 1 1 d . . . H20A H 1.0128 -0.3749 0.1080 0.102 Uiso 1 1 calc R . . H20B H 0.8585 -0.3780 0.1315 0.102 Uiso 1 1 calc R . . C21 C 0.9530(6) -0.2985(3) 0.1741(3) 0.0698(14) Uani 1 1 d . . . H21A H 0.8864 -0.3263 0.2178 0.084 Uiso 1 1 calc R . . H21B H 1.0393 -0.3139 0.1892 0.084 Uiso 1 1 calc R . . C22 C 1.1694(5) 0.0591(4) 0.1508(3) 0.0759(15) Uani 1 1 d . . . H22A H 1.0968 0.1033 0.1436 0.091 Uiso 1 1 calc R C 1 H22B H 1.1990 0.0550 0.1974 0.091 Uiso 1 1 calc R C 1 C23A C 1.2730(9) 0.0962(7) 0.0913(5) 0.048(2) Uiso 0.50 1 d P D 1 H23A H 1.3454 0.1212 0.1070 0.058 Uiso 0.50 1 calc PR D 1 H23B H 1.2436 0.1460 0.0491 0.058 Uiso 0.50 1 calc PR D 1 C23B C 1.3089(12) 0.0607(10) 0.1006(7) 0.075(3) Uiso 0.50 1 d P D 2 H23C H 1.3249 0.1233 0.0616 0.090 Uiso 0.50 1 calc PR D 2 H23D H 1.3780 0.0502 0.1317 0.090 Uiso 0.50 1 calc PR D 2 C24 C 1.3131(5) -0.0009(5) 0.0719(4) 0.0908(19) Uani 1 1 d . . . H24A H 1.3447 0.0140 0.0187 0.109 Uiso 1 1 calc R D 1 H24B H 1.3797 -0.0362 0.1007 0.109 Uiso 1 1 calc R D 1 C25 C 1.1882(5) -0.0534(4) 0.0945(3) 0.0728(15) Uani 1 1 d . B . H25A H 1.1359 -0.0331 0.0540 0.087 Uiso 1 1 calc R . . H25B H 1.2024 -0.1218 0.1076 0.087 Uiso 1 1 calc R . . C26 C 1.5606(3) 0.3181(2) 0.37443(18) 0.0305(7) Uani 1 1 d . . . C27 C 1.6552(3) 0.3152(3) 0.4204(2) 0.0391(8) Uani 1 1 d . . . H27 H 1.7023 0.3729 0.4072 0.047 Uiso 1 1 calc R . . C28 C 1.6915(4) 0.2449(3) 0.4803(2) 0.0462(9) Uani 1 1 d . . . H28 H 1.7644 0.2602 0.4979 0.055 Uiso 1 1 calc R . . C29 C 1.6390(4) 0.1564(3) 0.5186(2) 0.0510(10) Uani 1 1 d . . . H29 H 1.6744 0.1198 0.5612 0.061 Uiso 1 1 calc R . . C30 C 1.5398(4) 0.1166(3) 0.5004(2) 0.0496(10) Uani 1 1 d . . . H30 H 1.5048 0.0592 0.5363 0.059 Uiso 1 1 calc R . . C31 C 1.4836(4) 0.1476(3) 0.4380(2) 0.0434(9) Uani 1 1 d . . . H31 H 1.4172 0.1063 0.4378 0.052 Uiso 1 1 calc R . . C32 C 1.5044(3) 0.2293(2) 0.37282(19) 0.0335(8) Uani 1 1 d . . . C33 C 1.5611(4) 0.4867(2) 0.3334(2) 0.0378(8) Uani 1 1 d . . . H33 H 1.5772 0.4744 0.3849 0.045 Uiso 1 1 calc R . . C34 C 1.6838(4) 0.5294(3) 0.2808(3) 0.0568(11) Uani 1 1 d . . . H34A H 1.7551 0.4860 0.2927 0.085 Uiso 1 1 calc R . . H34B H 1.7050 0.5894 0.2856 0.085 Uiso 1 1 calc R . . H34C H 1.6703 0.5404 0.2301 0.085 Uiso 1 1 calc R . . C35 C 1.4502(4) 0.5547(3) 0.3185(2) 0.0481(10) Uani 1 1 d . . . H35A H 1.4388 0.5724 0.2668 0.072 Uiso 1 1 calc R . . H35B H 1.4699 0.6112 0.3289 0.072 Uiso 1 1 calc R . . H35C H 1.3705 0.5242 0.3502 0.072 Uiso 1 1 calc R . . C36 C 1.4277(4) 0.1465(3) 0.3018(2) 0.0483(10) Uani 1 1 d . . . H36 H 1.4692 0.0926 0.3363 0.058 Uiso 1 1 calc R . . C37 C 1.4777(5) 0.1516(3) 0.2230(3) 0.0658(13) Uani 1 1 d . . . H37A H 1.4385 0.2046 0.1885 0.099 Uiso 1 1 calc R . . H37B H 1.4549 0.0928 0.2168 0.099 Uiso 1 1 calc R . . H37C H 1.5720 0.1605 0.2133 0.099 Uiso 1 1 calc R . . C38 C 1.2818(5) 0.1308(3) 0.3201(3) 0.0671(13) Uani 1 1 d . . . H38A H 1.2532 0.1255 0.3715 0.101 Uiso 1 1 calc R . . H38B H 1.2586 0.0726 0.3131 0.101 Uiso 1 1 calc R . . H38C H 1.2396 0.1841 0.2876 0.101 Uiso 1 1 calc R . . C39 C 1.7463(4) 0.3443(4) 0.1933(3) 0.0720(15) Uani 1 1 d . . . H39A H 1.7501 0.3705 0.2328 0.086 Uiso 1 1 calc R E 1 H39B H 1.7419 0.2747 0.2152 0.086 Uiso 1 1 calc R E 1 C40A C 1.8565(10) 0.3747(9) 0.1377(6) 0.069(3) Uiso 0.50 1 d P F 1 H40A H 1.9266 0.3287 0.1481 0.082 Uiso 0.50 1 calc PR F 1 H40B H 1.8893 0.4368 0.1348 0.082 Uiso 0.50 1 calc PR F 1 C40B C 1.8501(9) 0.3289(8) 0.1392(5) 0.060(3) Uiso 0.50 1 d P F 2 H40C H 1.8577 0.2610 0.1464 0.072 Uiso 0.50 1 calc PR F 2 H40D H 1.9341 0.3534 0.1434 0.072 Uiso 0.50 1 calc PR F 2 C41 C 1.8108(5) 0.3815(5) 0.0670(3) 0.093(2) Uani 1 1 d . . . H41A H 1.8415 0.4415 0.0276 0.111 Uiso 1 1 calc R F 1 H41B H 1.8436 0.3286 0.0510 0.111 Uiso 1 1 calc R F 1 C42 C 1.6671(4) 0.3773(4) 0.0830(2) 0.0668(13) Uani 1 1 d . F . H42A H 1.6301 0.4321 0.0478 0.080 Uiso 1 1 calc R . . H42B H 1.6329 0.3188 0.0798 0.080 Uiso 1 1 calc R . . C43 C 1.5338(5) 0.5979(4) 0.0849(3) 0.0753(15) Uani 1 1 d . . . H43A H 1.5316 0.5716 0.0453 0.090 Uiso 1 1 calc R . . H43B H 1.6207 0.5879 0.0999 0.090 Uiso 1 1 calc R . . C44 C 1.5052(5) 0.7008(3) 0.0584(3) 0.0675(13) Uani 1 1 d . . . H44A H 1.5176 0.7268 0.0039 0.081 Uiso 1 1 calc R . . H44B H 1.5623 0.7361 0.0763 0.081 Uiso 1 1 calc R . . C45 C 1.3666(5) 0.7067(3) 0.0898(3) 0.0750(15) Uani 1 1 d . . . H45A H 1.3146 0.7368 0.0500 0.090 Uiso 1 1 calc R . . H45B H 1.3591 0.7437 0.1232 0.090 Uiso 1 1 calc R . . C46 C 1.3213(4) 0.6060(3) 0.1317(3) 0.0592(12) Uani 1 1 d . . . H46A H 1.2650 0.6012 0.1784 0.071 Uiso 1 1 calc R . . H46B H 1.2724 0.5822 0.1020 0.071 Uiso 1 1 calc R . . C47 C 1.0953(4) 0.4204(4) 0.2786(3) 0.0738(15) Uani 1 1 d . . . H47A H 1.0988 0.4343 0.2251 0.089 Uiso 1 1 calc R G 1 H47B H 1.0617 0.4760 0.2908 0.089 Uiso 1 1 calc R G 1 C48A C 1.0136(10) 0.3375(7) 0.3207(6) 0.060(2) Uiso 0.50 1 d P H 1 H48A H 1.0277 0.2868 0.2993 0.073 Uiso 0.50 1 calc PR H 1 H48B H 0.9207 0.3526 0.3258 0.073 Uiso 0.50 1 calc PR H 1 C48B C 1.0015(12) 0.3659(9) 0.3443(7) 0.080(3) Uiso 0.50 1 d P H 2 H48C H 0.9455 0.4096 0.3624 0.097 Uiso 0.50 1 calc PR H 2 H48D H 0.9457 0.3249 0.3307 0.097 Uiso 0.50 1 calc PR H 2 C49 C 1.0707(5) 0.3105(4) 0.3998(3) 0.0882(18) Uani 1 1 d . . . H49A H 1.0147 0.3353 0.4343 0.106 Uiso 1 1 calc R H 1 H49B H 1.0765 0.2415 0.4233 0.106 Uiso 1 1 calc R H 1 C50 C 1.2019(5) 0.3567(4) 0.3789(3) 0.0694(14) Uani 1 1 d . F . H50A H 1.2058 0.4060 0.4011 0.083 Uiso 1 1 calc R . . H50B H 1.2688 0.3098 0.3956 0.083 Uiso 1 1 calc R . . Ca1 Ca 0.91468(7) -0.10338(5) 0.22343(4) 0.03316(16) Uani 1 1 d . . . Ca2 Ca 1.42666(6) 0.38763(5) 0.22530(4) 0.03251(16) Uani 1 1 d . . . N1 N 0.7353(3) -0.20839(19) 0.29597(16) 0.0325(6) Uani 1 1 d . B . N2 N 0.9803(3) -0.2312(2) 0.32548(16) 0.0379(7) Uani 1 1 d . B . N3 N 1.5233(3) 0.39707(19) 0.32741(15) 0.0307(6) Uani 1 1 d . F . N4 N 1.4664(3) 0.23457(19) 0.31066(16) 0.0351(7) Uani 1 1 d . F . O1 O 0.8867(3) -0.0164(2) 0.30756(16) 0.0593(8) Uani 1 1 d . B . O2 O 0.9399(3) -0.19862(18) 0.14491(14) 0.0453(6) Uani 1 1 d . B . O3 O 1.1232(3) -0.03295(19) 0.15723(15) 0.0494(7) Uani 1 1 d . B . O4 O 1.6357(2) 0.3788(2) 0.15728(14) 0.0524(7) Uani 1 1 d . F . O5 O 1.4373(2) 0.55311(18) 0.14602(14) 0.0456(6) Uani 1 1 d . F . O6 O 1.2211(2) 0.3976(2) 0.29947(15) 0.0526(7) Uani 1 1 d . F . I1 I 0.80353(3) 0.066741(19) 0.105622(15) 0.05264(9) Uani 1 1 d . B . I2 I 1.26472(3) 0.36297(2) 0.109740(15) 0.04991(9) Uani 1 1 d . F . 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 0.0366(19) 0.0312(18) 0.0298(18) -0.0129(15) -0.0049(15) 0.0009(15) C2 0.042(2) 0.045(2) 0.036(2) -0.0147(18) 0.0006(17) -0.0011(17) C3 0.056(2) 0.053(2) 0.030(2) -0.0111(18) 0.0070(18) -0.016(2) C4 0.078(3) 0.042(2) 0.035(2) -0.0054(18) -0.005(2) -0.013(2) C5 0.077(3) 0.035(2) 0.041(2) -0.0066(18) -0.019(2) 0.006(2) C6 0.050(2) 0.047(2) 0.045(2) -0.0108(19) -0.0172(19) 0.0130(19) C7 0.0372(19) 0.0367(19) 0.0278(18) -0.0115(15) -0.0090(15) 0.0033(16) C8 0.0293(19) 0.0344(19) 0.054(2) -0.0061(18) -0.0057(17) 0.0011(15) C9 0.045(2) 0.045(2) 0.069(3) -0.012(2) 0.006(2) 0.0091(19) C10 0.049(2) 0.065(3) 0.057(3) -0.013(2) -0.024(2) 0.003(2) C11 0.039(2) 0.067(3) 0.050(3) -0.003(2) -0.0176(19) 0.000(2) C12 0.055(3) 0.096(4) 0.077(4) -0.014(3) -0.027(3) -0.022(3) C13 0.041(3) 0.106(4) 0.090(4) -0.029(3) -0.008(3) 0.022(3) C14 0.108(4) 0.072(3) 0.053(3) -0.031(3) -0.004(3) 0.004(3) C15 0.214(8) 0.107(5) 0.072(4) -0.064(4) 0.002(5) -0.002(5) C17 0.158(6) 0.051(3) 0.080(4) -0.041(3) -0.019(4) 0.014(3) C18 0.091(4) 0.066(3) 0.033(2) -0.020(2) -0.007(2) 0.002(3) C19 0.171(7) 0.066(4) 0.072(4) -0.036(3) -0.034(4) 0.001(4) C20 0.138(5) 0.058(3) 0.065(3) -0.030(3) -0.008(3) -0.005(3) C21 0.116(4) 0.039(2) 0.057(3) -0.018(2) -0.017(3) 0.000(3) C22 0.078(3) 0.071(3) 0.081(4) -0.033(3) 0.004(3) -0.035(3) C24 0.054(3) 0.113(5) 0.086(4) -0.018(4) 0.014(3) -0.013(3) C25 0.069(3) 0.068(3) 0.075(4) -0.030(3) 0.023(3) -0.010(3) C26 0.0290(18) 0.0357(19) 0.0263(17) -0.0125(15) 0.0016(14) 0.0000(14) C27 0.035(2) 0.044(2) 0.038(2) -0.0135(18) -0.0048(16) -0.0028(16) C28 0.043(2) 0.059(3) 0.040(2) -0.018(2) -0.0144(18) 0.0045(19) C29 0.072(3) 0.050(2) 0.030(2) -0.0095(19) -0.019(2) 0.013(2) C30 0.077(3) 0.035(2) 0.036(2) -0.0092(18) -0.013(2) 0.002(2) C31 0.058(2) 0.0319(19) 0.040(2) -0.0109(17) -0.0076(18) -0.0044(17) C32 0.0367(19) 0.0299(18) 0.0326(19) -0.0097(15) -0.0047(15) 0.0048(15) C33 0.046(2) 0.0325(19) 0.036(2) -0.0112(16) -0.0078(16) -0.0068(16) C34 0.058(3) 0.050(2) 0.058(3) -0.015(2) -0.003(2) -0.017(2) C35 0.064(3) 0.036(2) 0.046(2) -0.0168(18) -0.009(2) 0.0004(19) C36 0.071(3) 0.033(2) 0.050(2) -0.0181(18) -0.030(2) 0.0086(19) C37 0.102(4) 0.053(3) 0.063(3) -0.035(2) -0.040(3) 0.023(3) C38 0.080(3) 0.050(3) 0.079(3) -0.023(3) -0.028(3) -0.012(2) C39 0.046(3) 0.122(4) 0.059(3) -0.044(3) -0.017(2) 0.029(3) C41 0.066(3) 0.135(5) 0.057(3) -0.017(3) 0.011(3) 0.032(3) C42 0.062(3) 0.098(4) 0.042(3) -0.030(3) -0.002(2) 0.018(3) C43 0.069(3) 0.073(3) 0.053(3) 0.008(2) 0.011(2) 0.005(3) C44 0.088(4) 0.053(3) 0.055(3) -0.015(2) 0.004(3) -0.014(3) C45 0.090(4) 0.053(3) 0.069(3) -0.007(3) -0.006(3) 0.014(3) C46 0.057(3) 0.050(3) 0.063(3) -0.012(2) -0.009(2) 0.014(2) C47 0.042(3) 0.102(4) 0.070(3) -0.024(3) 0.001(2) 0.008(3) C49 0.066(3) 0.080(4) 0.086(4) -0.003(3) 0.022(3) -0.001(3) C50 0.056(3) 0.101(4) 0.046(3) -0.025(3) 0.009(2) -0.012(3) Ca1 0.0357(4) 0.0326(4) 0.0289(4) -0.0089(3) -0.0018(3) -0.0025(3) Ca2 0.0317(4) 0.0361(4) 0.0287(4) -0.0097(3) -0.0058(3) 0.0044(3) N1 0.0289(15) 0.0318(15) 0.0362(17) -0.0115(13) -0.0036(12) 0.0005(12) N2 0.0342(16) 0.0433(18) 0.0356(17) -0.0115(14) -0.0089(13) 0.0010(14) N3 0.0328(15) 0.0297(15) 0.0292(15) -0.0106(13) -0.0016(12) -0.0025(12) N4 0.0433(17) 0.0275(15) 0.0375(17) -0.0124(13) -0.0127(13) 0.0044(13) O1 0.091(2) 0.0466(16) 0.0453(17) -0.0233(14) -0.0093(16) 0.0041(15) O2 0.0610(17) 0.0415(15) 0.0320(14) -0.0138(12) 0.0007(12) -0.0068(13) O3 0.0485(16) 0.0528(17) 0.0452(16) -0.0174(14) 0.0022(13) -0.0142(13) O4 0.0379(15) 0.083(2) 0.0374(15) -0.0237(15) -0.0051(12) 0.0194(14) O5 0.0443(15) 0.0452(15) 0.0395(15) -0.0073(12) -0.0016(12) 0.0045(12) O6 0.0328(14) 0.081(2) 0.0446(16) -0.0250(15) 0.0013(12) -0.0031(14) I1 0.06184(19) 0.04604(16) 0.03835(15) -0.00305(12) -0.00107(13) 0.00579(13) I2 0.04925(16) 0.06151(18) 0.04389(16) -0.02092(14) -0.01627(12) 0.00622(13) _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 N1 1.309(4) . ? C1 C2 1.441(5) . ? C1 C7 1.493(5) . ? C2 C3 1.368(5) . ? C3 C4 1.383(6) . ? C4 C5 1.370(6) . ? C5 C6 1.389(6) . ? C6 C7 1.417(5) . ? C7 N2 1.325(4) . ? C8 N1 1.480(5) . ? C8 C10 1.516(6) . ? C8 C9 1.522(5) . ? C11 N2 1.471(5) . ? C11 C13 1.505(7) . ? C11 C12 1.520(7) . ? C14 C15 1.439(7) . ? C14 O1 1.440(6) . ? C15 C16A 1.398(12) . ? C15 C16B 1.642(15) . ? C16A C17 1.513(12) . ? C16B C17 1.363(13) . ? C17 O1 1.442(5) . ? C18 O2 1.463(5) . ? C18 C19 1.476(7) . ? C19 C20 1.455(8) . ? C20 C21 1.467(6) . ? C21 O2 1.430(5) . ? C22 C23A 1.429(10) . ? C22 O3 1.447(5) . ? C22 C23B 1.625(13) . ? C23A C24 1.666(11) . ? C23B C24 1.239(12) . ? C24 C25 1.477(7) . ? C25 O3 1.433(5) . ? C26 N3 1.322(4) . ? C26 C27 1.429(5) . ? C26 C32 1.496(5) . ? C27 C28 1.379(5) . ? C28 C29 1.372(6) . ? C29 C30 1.368(6) . ? C30 C31 1.366(6) . ? C31 C32 1.430(5) . ? C32 N4 1.314(4) . ? C33 N3 1.473(4) . ? C33 C35 1.520(5) . ? C33 C34 1.520(5) . ? C36 N4 1.478(4) . ? C36 C38 1.520(6) . ? C36 C37 1.526(6) . ? C39 C40A 1.424(11) . ? C39 O4 1.439(5) . ? C39 C40B 1.468(10) . ? C40A C41 1.503(12) . ? C40B C41 1.478(12) . ? C41 C42 1.487(7) . ? C42 O4 1.448(5) . ? C43 O5 1.421(5) . ? C43 C44 1.498(7) . ? C44 C45 1.499(7) . ? C45 C46 1.510(6) . ? C46 O5 1.443(5) . ? C47 O6 1.436(5) . ? C47 C48A 1.456(11) . ? C47 C48B 1.491(12) . ? C48A C49 1.661(12) . ? C48B C49 1.409(13) . ? C49 C50 1.493(7) . ? C50 O6 1.445(5) . ? Ca1 O1 2.420(3) . ? Ca1 N1 2.423(3) . ? Ca1 N2 2.423(3) . ? Ca1 O2 2.427(2) . ? Ca1 O3 2.428(3) . ? Ca1 I1 3.1365(8) . ? Ca2 O4 2.404(2) . ? Ca2 N4 2.410(3) . ? Ca2 N3 2.424(3) . ? Ca2 O6 2.434(3) . ? Ca2 O5 2.443(3) . ? Ca2 I2 3.1533(8) . ? 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 C1 C2 123.1(3) . . ? N1 C1 C7 116.6(3) . . ? C2 C1 C7 119.9(3) . . ? C3 C2 C1 131.7(4) . . ? C2 C3 C4 129.5(4) . . ? C5 C4 C3 124.7(4) . . ? C4 C5 C6 129.9(4) . . ? C5 C6 C7 133.2(4) . . ? N2 C7 C6 124.6(3) . . ? N2 C7 C1 115.0(3) . . ? C6 C7 C1 120.2(3) . . ? N1 C8 C10 109.0(3) . . ? N1 C8 C9 110.3(3) . . ? C10 C8 C9 111.8(4) . . ? N2 C11 C13 111.9(4) . . ? N2 C11 C12 109.0(4) . . ? C13 C11 C12 110.4(4) . . ? C15 C14 O1 106.6(5) . . ? C16A C15 C14 110.6(6) . . ? C16A C15 C16B 26.9(6) . . ? C14 C15 C16B 100.2(6) . . ? C15 C16A C17 105.9(7) . . ? C17 C16B C15 100.9(8) . . ? C16B C17 O1 110.3(7) . . ? C16B C17 C16A 29.4(6) . . ? O1 C17 C16A 105.3(6) . . ? O2 C18 C19 106.4(4) . . ? C20 C19 C18 107.5(4) . . ? C19 C20 C21 107.5(4) . . ? O2 C21 C20 108.2(4) . . ? C23A C22 O3 113.2(5) . . ? C23A C22 C23B 22.9(5) . . ? O3 C22 C23B 98.6(6) . . ? C22 C23A C24 99.9(6) . . ? C24 C23B C22 111.2(9) . . ? C23B C24 C25 109.1(7) . . ? C23B C24 C23A 18.9(7) . . ? C25 C24 C23A 101.4(5) . . ? O3 C25 C24 106.7(4) . . ? N3 C26 C27 123.4(3) . . ? N3 C26 C32 115.5(3) . . ? C27 C26 C32 120.9(3) . . ? C28 C27 C26 132.4(4) . . ? C29 C28 C27 130.3(4) . . ? C30 C29 C28 125.2(4) . . ? C31 C30 C29 129.4(4) . . ? C30 C31 C32 133.1(4) . . ? N4 C32 C31 123.3(3) . . ? N4 C32 C26 115.9(3) . . ? C31 C32 C26 120.6(3) . . ? N3 C33 C35 109.1(3) . . ? N3 C33 C34 111.7(3) . . ? C35 C33 C34 110.6(3) . . ? N4 C36 C38 111.1(3) . . ? N4 C36 C37 108.6(3) . . ? C38 C36 C37 111.4(4) . . ? C40A C39 O4 106.0(6) . . ? C40A C39 C40B 27.5(5) . . ? O4 C39 C40B 108.5(5) . . ? C39 C40A C41 105.6(7) . . ? C39 C40B C41 104.6(7) . . ? C40B C41 C42 103.5(5) . . ? C40B C41 C40A 26.7(5) . . ? C42 C41 C40A 106.0(5) . . ? O4 C42 C41 105.2(4) . . ? O5 C43 C44 107.0(4) . . ? C43 C44 C45 105.2(4) . . ? C44 C45 C46 105.2(4) . . ? O5 C46 C45 105.7(4) . . ? O6 C47 C48A 105.6(6) . . ? O6 C47 C48B 105.6(6) . . ? C48A C47 C48B 28.6(5) . . ? C47 C48A C49 98.2(6) . . ? C49 C48B C47 108.9(8) . . ? C48B C49 C50 104.1(6) . . ? C48B C49 C48A 25.8(6) . . ? C50 C49 C48A 104.5(5) . . ? O6 C50 C49 105.3(4) . . ? O1 Ca1 N1 90.65(10) . . ? O1 Ca1 N2 85.28(10) . . ? N1 Ca1 N2 67.75(10) . . ? O1 Ca1 O2 176.81(10) . . ? N1 Ca1 O2 86.83(9) . . ? N2 Ca1 O2 91.95(10) . . ? O1 Ca1 O3 96.45(10) . . ? N1 Ca1 O3 166.21(10) . . ? N2 Ca1 O3 100.98(10) . . ? O2 Ca1 O3 85.62(9) . . ? O1 Ca1 I1 89.37(8) . . ? N1 Ca1 I1 107.85(7) . . ? N2 Ca1 I1 172.98(7) . . ? O2 Ca1 I1 93.25(7) . . ? O3 Ca1 I1 84.11(7) . . ? O4 Ca2 N4 87.01(10) . . ? O4 Ca2 N3 91.49(9) . . ? N4 Ca2 N3 67.53(9) . . ? O4 Ca2 O6 176.83(10) . . ? N4 Ca2 O6 91.94(10) . . ? N3 Ca2 O6 85.34(9) . . ? O4 Ca2 O5 84.93(10) . . ? N4 Ca2 O5 165.64(10) . . ? N3 Ca2 O5 100.78(9) . . ? O6 Ca2 O5 95.47(10) . . ? O4 Ca2 I2 96.09(7) . . ? N4 Ca2 I2 109.15(7) . . ? N3 Ca2 I2 171.59(7) . . ? O6 Ca2 I2 87.08(7) . . ? O5 Ca2 I2 83.56(7) . . ? C1 N1 C8 119.6(3) . . ? C1 N1 Ca1 117.6(2) . . ? C8 N1 Ca1 121.4(2) . . ? C7 N2 C11 118.1(3) . . ? C7 N2 Ca1 117.5(2) . . ? C11 N2 Ca1 123.3(2) . . ? C26 N3 C33 117.9(3) . . ? C26 N3 Ca2 118.2(2) . . ? C33 N3 Ca2 123.3(2) . . ? C32 N4 C36 118.4(3) . . ? C32 N4 Ca2 118.6(2) . . ? C36 N4 Ca2 122.1(2) . . ? C14 O1 C17 107.7(3) . . ? C14 O1 Ca1 121.9(3) . . ? C17 O1 Ca1 129.2(3) . . ? C21 O2 C18 109.0(3) . . ? C21 O2 Ca1 121.8(2) . . ? C18 O2 Ca1 127.3(2) . . ? C25 O3 C22 107.0(3) . . ? C25 O3 Ca1 122.7(2) . . ? C22 O3 Ca1 124.8(3) . . ? C39 O4 C42 106.9(3) . . ? C39 O4 Ca2 122.0(2) . . ? C42 O4 Ca2 128.6(2) . . ? C43 O5 C46 106.0(3) . . ? C43 O5 Ca2 126.9(3) . . ? C46 O5 Ca2 121.2(2) . . ? C47 O6 C50 106.6(3) . . ? C47 O6 Ca2 130.2(3) . . ? C50 O6 Ca2 121.6(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 C1 C2 C3 153.3(4) . . . . ? C7 C1 C2 C3 -34.0(6) . . . . ? C1 C2 C3 C4 2.4(7) . . . . ? C2 C3 C4 C5 12.7(7) . . . . ? C3 C4 C5 C6 2.0(7) . . . . ? C4 C5 C6 C7 -8.5(8) . . . . ? C5 C6 C7 N2 169.1(4) . . . . ? C5 C6 C7 C1 -15.3(6) . . . . ? N1 C1 C7 N2 27.9(4) . . . . ? C2 C1 C7 N2 -145.3(3) . . . . ? N1 C1 C7 C6 -148.1(3) . . . . ? C2 C1 C7 C6 38.7(5) . . . . ? O1 C14 C15 C16A 5.8(10) . . . . ? O1 C14 C15 C16B 31.6(8) . . . . ? C14 C15 C16A C17 6.5(12) . . . . ? C16B C15 C16A C17 -64.5(14) . . . . ? C16A C15 C16B C17 78.8(15) . . . . ? C14 C15 C16B C17 -37.1(10) . . . . ? C15 C16B C17 O1 28.7(11) . . . . ? C15 C16B C17 C16A -56.4(13) . . . . ? C15 C16A C17 C16B 88.0(16) . . . . ? C15 C16A C17 O1 -16.4(10) . . . . ? O2 C18 C19 C20 12.1(7) . . . . ? C18 C19 C20 C21 -10.6(8) . . . . ? C19 C20 C21 O2 5.1(7) . . . . ? O3 C22 C23A C24 -13.9(8) . . . . ? C23B C22 C23A C24 39.3(15) . . . . ? C23A C22 C23B C24 -116(2) . . . . ? O3 C22 C23B C24 16.1(11) . . . . ? C22 C23B C24 C25 -0.1(12) . . . . ? C22 C23B C24 C23A 68(2) . . . . ? C22 C23A C24 C23B -88(2) . . . . ? C22 C23A C24 C25 28.8(8) . . . . ? C23B C24 C25 O3 -16.6(10) . . . . ? C23A C24 C25 O3 -34.5(6) . . . . ? N3 C26 C27 C28 167.4(4) . . . . ? C32 C26 C27 C28 -17.4(6) . . . . ? C26 C27 C28 C29 -6.2(7) . . . . ? C27 C28 C29 C30 4.8(7) . . . . ? C28 C29 C30 C31 9.7(7) . . . . ? C29 C30 C31 C32 -1.5(8) . . . . ? C30 C31 C32 N4 160.5(4) . . . . ? C30 C31 C32 C26 -25.5(6) . . . . ? N3 C26 C32 N4 24.4(4) . . . . ? C27 C26 C32 N4 -151.1(3) . . . . ? N3 C26 C32 C31 -150.0(3) . . . . ? C27 C26 C32 C31 34.5(5) . . . . ? O4 C39 C40A C41 -28.6(9) . . . . ? C40B C39 C40A C41 70.8(14) . . . . ? C40A C39 C40B C41 -72.9(14) . . . . ? O4 C39 C40B C41 16.4(9) . . . . ? C39 C40B C41 C42 -30.2(9) . . . . ? C39 C40B C41 C40A 68.5(13) . . . . ? C39 C40A C41 C40B -74.6(14) . . . . ? C39 C40A C41 C42 13.8(10) . . . . ? C40B C41 C42 O4 33.5(7) . . . . ? C40A C41 C42 O4 6.0(8) . . . . ? O5 C43 C44 C45 -18.8(6) . . . . ? C43 C44 C45 C46 -1.2(6) . . . . ? C44 C45 C46 O5 20.4(5) . . . . ? O6 C47 C48A C49 40.0(7) . . . . ? C48B C47 C48A C49 -54.1(13) . . . . ? O6 C47 C48B C49 -2.4(10) . . . . ? C48A C47 C48B C49 91.5(16) . . . . ? C47 C48B C49 C50 20.0(10) . . . . ? C47 C48B C49 C48A -74.4(14) . . . . ? C47 C48A C49 C48B 70.5(14) . . . . ? C47 C48A C49 C50 -21.9(8) . . . . ? C48B C49 C50 O6 -30.3(8) . . . . ? C48A C49 C50 O6 -3.7(7) . . . . ? C2 C1 N1 C8 -13.0(5) . . . . ? C7 C1 N1 C8 174.1(3) . . . . ? C2 C1 N1 Ca1 153.6(3) . . . . ? C7 C1 N1 Ca1 -19.4(4) . . . . ? C10 C8 N1 C1 -132.2(3) . . . . ? C9 C8 N1 C1 104.7(4) . . . . ? C10 C8 N1 Ca1 61.7(4) . . . . ? C9 C8 N1 Ca1 -61.3(4) . . . . ? O1 Ca1 N1 C1 -78.6(2) . . . . ? N2 Ca1 N1 C1 6.1(2) . . . . ? O2 Ca1 N1 C1 99.5(2) . . . . ? O3 Ca1 N1 C1 42.6(5) . . . . ? I1 Ca1 N1 C1 -168.1(2) . . . . ? O1 Ca1 N1 C8 87.7(3) . . . . ? N2 Ca1 N1 C8 172.4(3) . . . . ? O2 Ca1 N1 C8 -94.2(3) . . . . ? O3 Ca1 N1 C8 -151.1(4) . . . . ? I1 Ca1 N1 C8 -1.8(3) . . . . ? C6 C7 N2 C11 -14.7(5) . . . . ? C1 C7 N2 C11 169.6(3) . . . . ? C6 C7 N2 Ca1 153.6(3) . . . . ? C1 C7 N2 Ca1 -22.1(4) . . . . ? C13 C11 N2 C7 95.2(4) . . . . ? C12 C11 N2 C7 -142.5(4) . . . . ? C13 C11 N2 Ca1 -72.4(4) . . . . ? C12 C11 N2 Ca1 50.0(4) . . . . ? O1 Ca1 N2 C7 102.1(3) . . . . ? N1 Ca1 N2 C7 9.5(2) . . . . ? O2 Ca1 N2 C7 -76.3(2) . . . . ? O3 Ca1 N2 C7 -162.2(2) . . . . ? I1 Ca1 N2 C7 61.6(7) . . . . ? O1 Ca1 N2 C11 -90.3(3) . . . . ? N1 Ca1 N2 C11 177.1(3) . . . . ? O2 Ca1 N2 C11 91.3(3) . . . . ? O3 Ca1 N2 C11 5.4(3) . . . . ? I1 Ca1 N2 C11 -130.8(6) . . . . ? C27 C26 N3 C33 -12.8(4) . . . . ? C32 C26 N3 C33 171.8(3) . . . . ? C27 C26 N3 Ca2 158.0(2) . . . . ? C32 C26 N3 Ca2 -17.5(3) . . . . ? C35 C33 N3 C26 -141.9(3) . . . . ? C34 C33 N3 C26 95.6(4) . . . . ? C35 C33 N3 Ca2 47.9(3) . . . . ? C34 C33 N3 Ca2 -74.6(4) . . . . ? O4 Ca2 N3 C26 -80.1(2) . . . . ? N4 Ca2 N3 C26 6.0(2) . . . . ? O6 Ca2 N3 C26 100.0(2) . . . . ? O5 Ca2 N3 C26 -165.3(2) . . . . ? I2 Ca2 N3 C26 74.3(6) . . . . ? O4 Ca2 N3 C33 90.1(2) . . . . ? N4 Ca2 N3 C33 176.2(3) . . . . ? O6 Ca2 N3 C33 -89.8(2) . . . . ? O5 Ca2 N3 C33 4.9(2) . . . . ? I2 Ca2 N3 C33 -115.5(5) . . . . ? C31 C32 N4 C36 -14.4(5) . . . . ? C26 C32 N4 C36 171.4(3) . . . . ? C31 C32 N4 Ca2 154.9(3) . . . . ? C26 C32 N4 Ca2 -19.3(4) . . . . ? C38 C36 N4 C32 96.5(4) . . . . ? C37 C36 N4 C32 -140.6(4) . . . . ? C38 C36 N4 Ca2 -72.4(4) . . . . ? C37 C36 N4 Ca2 50.5(4) . . . . ? O4 Ca2 N4 C32 100.7(3) . . . . ? N3 Ca2 N4 C32 7.9(2) . . . . ? O6 Ca2 N4 C32 -76.3(3) . . . . ? O5 Ca2 N4 C32 44.8(5) . . . . ? I2 Ca2 N4 C32 -163.9(2) . . . . ? O4 Ca2 N4 C36 -90.4(3) . . . . ? N3 Ca2 N4 C36 176.8(3) . . . . ? O6 Ca2 N4 C36 92.6(3) . . . . ? O5 Ca2 N4 C36 -146.3(4) . . . . ? I2 Ca2 N4 C36 5.0(3) . . . . ? C15 C14 O1 C17 -16.4(7) . . . . ? C15 C14 O1 Ca1 174.8(5) . . . . ? C16B C17 O1 C14 -10.4(9) . . . . ? C16A C17 O1 C14 20.1(8) . . . . ? C16B C17 O1 Ca1 157.3(7) . . . . ? C16A C17 O1 Ca1 -172.2(5) . . . . ? N1 Ca1 O1 C14 35.0(4) . . . . ? N2 Ca1 O1 C14 -32.6(4) . . . . ? O2 Ca1 O1 C14 -3(2) . . . . ? O3 Ca1 O1 C14 -133.1(4) . . . . ? I1 Ca1 O1 C14 142.9(4) . . . . ? N1 Ca1 O1 C17 -131.1(5) . . . . ? N2 Ca1 O1 C17 161.3(5) . . . . ? O2 Ca1 O1 C17 -168.8(18) . . . . ? O3 Ca1 O1 C17 60.7(5) . . . . ? I1 Ca1 O1 C17 -23.3(5) . . . . ? C20 C21 O2 C18 2.5(6) . . . . ? C20 C21 O2 Ca1 167.6(4) . . . . ? C19 C18 O2 C21 -9.0(6) . . . . ? C19 C18 O2 Ca1 -173.0(4) . . . . ? O1 Ca1 O2 C21 -16(2) . . . . ? N1 Ca1 O2 C21 -53.6(3) . . . . ? N2 Ca1 O2 C21 14.0(3) . . . . ? O3 Ca1 O2 C21 114.8(3) . . . . ? I1 Ca1 O2 C21 -161.3(3) . . . . ? O1 Ca1 O2 C18 146.3(19) . . . . ? N1 Ca1 O2 C18 108.5(3) . . . . ? N2 Ca1 O2 C18 176.1(3) . . . . ? O3 Ca1 O2 C18 -83.0(3) . . . . ? I1 Ca1 O2 C18 0.8(3) . . . . ? C24 C25 O3 C22 27.5(6) . . . . ? C24 C25 O3 Ca1 -177.6(3) . . . . ? C23A C22 O3 C25 -6.8(7) . . . . ? C23B C22 O3 C25 -25.2(7) . . . . ? C23A C22 O3 Ca1 -161.1(5) . . . . ? C23B C22 O3 Ca1 -179.4(5) . . . . ? O1 Ca1 O3 C25 -175.7(3) . . . . ? N1 Ca1 O3 C25 63.7(6) . . . . ? N2 Ca1 O3 C25 97.8(4) . . . . ? O2 Ca1 O3 C25 6.7(3) . . . . ? I1 Ca1 O3 C25 -87.0(3) . . . . ? O1 Ca1 O3 C22 -25.4(4) . . . . ? N1 Ca1 O3 C22 -145.9(5) . . . . ? N2 Ca1 O3 C22 -111.8(4) . . . . ? O2 Ca1 O3 C22 157.1(4) . . . . ? I1 Ca1 O3 C22 63.3(4) . . . . ? C40A C39 O4 C42 33.3(7) . . . . ? C40B C39 O4 C42 4.6(7) . . . . ? C40A C39 O4 Ca2 -163.2(6) . . . . ? C40B C39 O4 Ca2 168.1(5) . . . . ? C41 C42 O4 C39 -23.7(6) . . . . ? C41 C42 O4 Ca2 174.2(3) . . . . ? N4 Ca2 O4 C39 -42.7(4) . . . . ? N3 Ca2 O4 C39 24.7(4) . . . . ? O6 Ca2 O4 C39 28(2) . . . . ? O5 Ca2 O4 C39 125.4(4) . . . . ? I2 Ca2 O4 C39 -151.6(3) . . . . ? N4 Ca2 O4 C42 117.0(4) . . . . ? N3 Ca2 O4 C42 -175.6(4) . . . . ? O6 Ca2 O4 C42 -172.4(19) . . . . ? O5 Ca2 O4 C42 -74.9(4) . . . . ? I2 Ca2 O4 C42 8.0(4) . . . . ? C44 C43 O5 C46 32.3(5) . . . . ? C44 C43 O5 Ca2 -174.9(3) . . . . ? C45 C46 O5 C43 -32.7(5) . . . . ? C45 C46 O5 Ca2 172.6(3) . . . . ? O4 Ca2 O5 C43 6.4(4) . . . . ? N4 Ca2 O5 C43 62.5(6) . . . . ? N3 Ca2 O5 C43 96.9(4) . . . . ? O6 Ca2 O5 C43 -176.8(4) . . . . ? I2 Ca2 O5 C43 -90.4(4) . . . . ? O4 Ca2 O5 C46 155.4(3) . . . . ? N4 Ca2 O5 C46 -148.5(4) . . . . ? N3 Ca2 O5 C46 -114.0(3) . . . . ? O6 Ca2 O5 C46 -27.7(3) . . . . ? I2 Ca2 O5 C46 58.7(3) . . . . ? C48A C47 O6 C50 -46.7(6) . . . . ? C48B C47 O6 C50 -17.0(7) . . . . ? C48A C47 O6 Ca2 118.9(5) . . . . ? C48B C47 O6 Ca2 148.6(6) . . . . ? C49 C50 O6 C47 29.4(5) . . . . ? C49 C50 O6 Ca2 -137.7(3) . . . . ? O4 Ca2 O6 C47 159.6(19) . . . . ? N4 Ca2 O6 C47 -129.9(4) . . . . ? N3 Ca2 O6 C47 162.8(4) . . . . ? O5 Ca2 O6 C47 62.4(4) . . . . ? I2 Ca2 O6 C47 -20.8(4) . . . . ? O4 Ca2 O6 C50 -37(2) . . . . ? N4 Ca2 O6 C50 33.8(3) . . . . ? N3 Ca2 O6 C50 -33.5(3) . . . . ? O5 Ca2 O6 C50 -133.9(3) . . . . ? I2 Ca2 O6 C50 142.8(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.425 _refine_diff_density_min -0.450 _refine_diff_density_rms 0.062 #============================================================================== data_2 _database_code_depnum_ccdc_archive 'CCDC 671209' _audit_creation_date 07-05-11 _audit_creation_method 'STOE X-RED' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H70 I2 N4 O4 Sr2, C4 H8 O' _chemical_formula_sum 'C46 H78 I2 N4 O5 Sr2' _chemical_formula_weight 1196.16 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' I I -0.4742 1.8119 '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 monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.4224(9) _cell_length_b 17.5826(10) _cell_length_c 14.7213(11) _cell_angle_alpha 90.00 _cell_angle_beta 94.414(6) _cell_angle_gamma 90.00 _cell_volume 2689.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 13094 _cell_measurement_theta_min 2.70 _cell_measurement_theta_max 29.58 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.497 _exptl_crystal_size_mid 0.473 _exptl_crystal_size_min 0.441 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.477 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1208 _exptl_absorpt_coefficient_mu 3.173 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.3198 _exptl_absorpt_correction_T_max 0.3704 _exptl_absorpt_process_details 'STOE X-RED & X-SHAPE' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'STOE IPDS 2T' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12147 _diffrn_reflns_av_R_equivalents 0.0403 _diffrn_reflns_av_sigmaI/netI 0.0353 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.70 _diffrn_reflns_theta_max 25.02 _reflns_number_total 4708 _reflns_number_gt 3684 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA, PLATON (A.L.Spek, 2005)' _computing_data_reduction 'STOE X-RED, PLATON (A.L.Spek, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e' _computing_publication_material 'X-STEP32, Microsoft Word' _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^)+(0.0397P)^2^+2.9115P] 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 4708 _refine_ls_number_parameters 258 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0531 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_ref 0.0847 _refine_ls_wR_factor_gt 0.0794 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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 -0.2235(4) 0.1836(2) 0.2820(3) 0.0284(9) Uani 1 1 d . B . C2 C -0.3274(5) 0.2270(3) 0.3118(3) 0.0400(10) Uani 1 1 d . . . H2 H -0.3833 0.2467 0.2635 0.048 Uiso 1 1 calc R . . C3 C -0.3629(5) 0.2461(3) 0.3973(3) 0.0474(12) Uani 1 1 d . . . H3 H -0.4433 0.2714 0.3980 0.057 Uiso 1 1 calc R . . C4 C -0.2990(5) 0.2340(3) 0.4824(3) 0.0475(13) Uani 1 1 d . . . H4 H -0.3349 0.2559 0.5337 0.057 Uiso 1 1 calc R . . C5 C -0.1880(5) 0.1926(3) 0.4979(3) 0.0428(12) Uani 1 1 d . . . H5 H -0.1489 0.1958 0.5582 0.051 Uiso 1 1 calc R . . C6 C -0.1239(5) 0.1471(3) 0.4397(3) 0.0361(10) Uani 1 1 d . . . H6 H -0.0484 0.1238 0.4671 0.043 Uiso 1 1 calc R . . C7 C -0.1514(4) 0.1287(2) 0.3443(2) 0.0270(9) Uani 1 1 d . B . C8 C -0.2463(5) 0.2418(3) 0.1338(3) 0.0392(11) Uani 1 1 d . . . H8 H -0.2749 0.2860 0.1699 0.047 Uiso 1 1 calc R . . C9 C -0.3614(5) 0.2101(3) 0.0764(3) 0.0550(14) Uani 1 1 d . . . H9A H -0.3348 0.1656 0.0426 0.082 Uiso 1 1 calc R . . H9B H -0.3954 0.2491 0.0335 0.082 Uiso 1 1 calc R . . H9C H -0.4283 0.1952 0.1162 0.082 Uiso 1 1 calc R . . C10 C -0.1435(6) 0.2685(3) 0.0728(3) 0.0503(13) Uani 1 1 d . . . H10A H -0.0703 0.2893 0.1105 0.075 Uiso 1 1 calc R . . H10B H -0.1794 0.3078 0.0312 0.075 Uiso 1 1 calc R . . H10C H -0.1146 0.2253 0.0374 0.075 Uiso 1 1 calc R . . C11 C -0.0475(4) 0.0072(2) 0.3648(2) 0.0335(10) Uani 1 1 d . . . H11 H -0.0773 0.0128 0.4275 0.040 Uiso 1 1 calc R . . C12 C -0.0919(6) -0.0688(3) 0.3265(3) 0.0487(12) Uani 1 1 d . . . H12A H -0.1862 -0.0708 0.3219 0.073 Uiso 1 1 calc R . . H12B H -0.0577 -0.1095 0.3670 0.073 Uiso 1 1 calc R . . H12C H -0.0607 -0.0756 0.2660 0.073 Uiso 1 1 calc R . . C13 C 0.0979(5) 0.0127(3) 0.3705(3) 0.0467(12) Uani 1 1 d . . . H13A H 0.1278 0.0089 0.3091 0.070 Uiso 1 1 calc R . . H13B H 0.1351 -0.0288 0.4083 0.070 Uiso 1 1 calc R . . H13C H 0.1249 0.0616 0.3976 0.070 Uiso 1 1 calc R . . C14 C -0.3100(7) -0.0708(4) 0.0731(4) 0.0734(19) Uani 1 1 d . . . H14A H -0.2346 -0.1052 0.0777 0.088 Uiso 1 1 calc R . . H14B H -0.3289 -0.0568 0.0083 0.088 Uiso 1 1 calc R . . C15 C -0.4208(8) -0.1089(5) 0.1072(6) 0.098(3) Uani 1 1 d . . . H15A H -0.4938 -0.1089 0.0601 0.118 Uiso 1 1 calc R . . H15B H -0.3991 -0.1622 0.1235 0.118 Uiso 1 1 calc R . . C16 C -0.4544(8) -0.0676(5) 0.1865(6) 0.095(2) Uani 1 1 d . . . H16A H -0.4216 -0.0940 0.2430 0.114 Uiso 1 1 calc R . . H16B H -0.5489 -0.0622 0.1867 0.114 Uiso 1 1 calc R . . C17 C -0.3919(5) 0.0087(3) 0.1797(4) 0.0582(14) Uani 1 1 d . . . H17A H -0.4524 0.0456 0.1490 0.070 Uiso 1 1 calc R . . H17B H -0.3634 0.0284 0.2409 0.070 Uiso 1 1 calc R . . C18 C 0.1307(6) 0.2125(3) 0.2462(4) 0.0595(15) Uani 1 1 d . . . H18A H 0.0783 0.2012 0.2979 0.071 Uiso 1 1 calc R A 1 H18B H 0.0945 0.2578 0.2135 0.071 Uiso 1 1 calc R A 1 C19A C 0.271(2) 0.2257(12) 0.2796(14) 0.080(6) Uiso 0.40 1 d P B 1 H19A H 0.2786 0.2422 0.3441 0.096 Uiso 0.40 1 calc PR B 1 H19B H 0.3108 0.2646 0.2421 0.096 Uiso 0.40 1 calc PR B 1 C20A C 0.3369(14) 0.1445(9) 0.2684(9) 0.048(3) Uiso 0.40 1 d P B 1 H20A H 0.4309 0.1481 0.2637 0.058 Uiso 0.40 1 calc PR B 1 H20B H 0.3181 0.1085 0.3173 0.058 Uiso 0.40 1 calc PR B 1 C19B C 0.2491(10) 0.2061(7) 0.3095(7) 0.058(3) Uiso 0.60 1 d P B 2 H19C H 0.2741 0.2557 0.3374 0.070 Uiso 0.60 1 calc PR B 2 H19D H 0.2387 0.1681 0.3581 0.070 Uiso 0.60 1 calc PR B 2 C20B C 0.3416(12) 0.1806(8) 0.2456(8) 0.073(3) Uiso 0.60 1 d P B 2 H20C H 0.4150 0.1539 0.2782 0.087 Uiso 0.60 1 calc PR B 2 H20D H 0.3748 0.2243 0.2121 0.087 Uiso 0.60 1 calc PR B 2 C21 C 0.2654(5) 0.1264(3) 0.1803(4) 0.0528(13) Uani 1 1 d . . . H21A H 0.3028 0.1545 0.1304 0.063 Uiso 1 1 calc R B 1 H21B H 0.2711 0.0713 0.1675 0.063 Uiso 1 1 calc R B 1 N1 N -0.1907(3) 0.18380(19) 0.1965(2) 0.0282(7) Uani 1 1 d . B . N2 N -0.1062(3) 0.06797(19) 0.3062(2) 0.0285(7) Uani 1 1 d . B . O1 O -0.2832(3) -0.00408(19) 0.1266(2) 0.0424(8) Uani 1 1 d . B . O2 O 0.1334(3) 0.14815(19) 0.1857(2) 0.0412(8) Uani 1 1 d . B . I I 0.12110(3) -0.073299(17) 0.090970(16) 0.03619(10) Uani 1 1 d . . . Sr Sr -0.07244(3) 0.07012(2) 0.13653(2) 0.02612(11) Uani 1 1 d . . . C22 C -0.0828(14) 0.5234(9) 0.0388(10) 0.175(5) Uiso 1 1 d . . . H22A H -0.1413 0.5636 0.0581 0.210 Uiso 1 1 calc R . . H22B H -0.1284 0.4741 0.0404 0.210 Uiso 1 1 calc R . . C23 C 0.0470(17) 0.4604(10) 0.0596(11) 0.194(6) Uiso 1 1 d . . . H23A H -0.0275 0.4254 0.0584 0.233 Uiso 1 1 calc R . . H23B H 0.1204 0.4362 0.0952 0.233 Uiso 1 1 calc R . . O3 O 0.020(3) 0.521(2) 0.095(2) 0.297(14) Uiso 0.50 1 d P . . 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 0.027(2) 0.027(2) 0.032(2) -0.0055(16) 0.0044(16) -0.0016(18) C2 0.036(2) 0.044(3) 0.040(2) -0.007(2) 0.0041(18) 0.010(2) C3 0.037(3) 0.052(3) 0.055(3) -0.016(2) 0.019(2) 0.006(2) C4 0.055(3) 0.052(3) 0.039(2) -0.017(2) 0.021(2) -0.006(3) C5 0.053(3) 0.047(3) 0.029(2) -0.0106(19) 0.010(2) -0.008(2) C6 0.042(3) 0.038(3) 0.028(2) -0.0032(18) 0.0020(18) -0.003(2) C7 0.029(2) 0.029(2) 0.0229(18) -0.0035(16) 0.0047(15) -0.0047(18) C8 0.048(3) 0.034(3) 0.035(2) 0.0000(18) -0.0010(19) 0.015(2) C9 0.047(3) 0.066(4) 0.050(3) -0.002(3) -0.011(2) 0.017(3) C10 0.067(4) 0.043(3) 0.041(3) 0.014(2) 0.007(2) 0.005(3) C11 0.046(3) 0.032(2) 0.0223(19) 0.0043(17) 0.0038(17) 0.000(2) C12 0.066(3) 0.032(3) 0.047(3) 0.007(2) -0.004(2) -0.002(3) C13 0.048(3) 0.052(3) 0.040(2) 0.011(2) 0.002(2) 0.004(2) C14 0.081(5) 0.065(4) 0.077(4) -0.035(3) 0.028(3) -0.029(4) C15 0.077(5) 0.078(5) 0.143(7) -0.045(5) 0.032(5) -0.032(4) C16 0.080(5) 0.100(6) 0.107(6) -0.018(5) 0.029(4) -0.043(5) C17 0.043(3) 0.062(4) 0.072(3) -0.019(3) 0.018(3) -0.010(3) C18 0.059(4) 0.056(4) 0.063(3) -0.025(3) 0.003(3) -0.010(3) C21 0.041(3) 0.059(4) 0.058(3) -0.007(3) 0.006(2) -0.007(3) N1 0.035(2) 0.0245(17) 0.0253(16) -0.0002(13) 0.0009(14) 0.0050(15) N2 0.0354(19) 0.0278(18) 0.0224(15) 0.0013(13) 0.0031(13) 0.0007(16) O1 0.0404(18) 0.0455(19) 0.0419(16) -0.0131(15) 0.0072(14) -0.0082(16) O2 0.0352(18) 0.050(2) 0.0381(15) -0.0120(15) 0.0015(13) -0.0091(15) I 0.04635(19) 0.03553(17) 0.02657(14) -0.00120(11) 0.00190(11) 0.01098(14) Sr 0.0298(2) 0.0271(2) 0.02153(18) -0.00376(15) 0.00222(14) 0.00182(17) _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 N1 1.328(5) . ? C1 C2 1.422(6) . ? C1 C7 1.493(6) . ? C1 Sr 3.400(4) . ? C2 C3 1.379(6) . ? C3 C4 1.390(7) . ? C4 C5 1.370(7) . ? C5 C6 1.381(6) . ? C6 C7 1.447(5) . ? C7 N2 1.312(5) . ? C7 Sr 3.389(4) . ? C8 N1 1.465(5) . ? C8 C9 1.519(7) . ? C8 C10 1.524(7) . ? C11 N2 1.477(5) . ? C11 C12 1.509(6) . ? C11 C13 1.515(6) . ? C14 O1 1.429(6) . ? C14 C15 1.456(9) . ? C15 C16 1.441(10) . ? C16 C17 1.497(9) . ? C17 O1 1.443(6) . ? C18 O2 1.441(6) . ? C18 C19B 1.492(12) . ? C18 C19A 1.52(2) . ? C19A C20A 1.60(2) . ? C20A C21 1.481(14) . ? C19B C20B 1.468(16) . ? C20B C21 1.531(12) . ? C21 O2 1.435(6) . ? N1 Sr 2.542(3) . ? N2 Sr 2.549(3) . ? O1 Sr 2.549(3) . ? O2 Sr 2.602(3) . ? I Sr 3.3296(5) . ? I Sr 3.3489(5) 3 ? Sr I 3.3489(5) 3 ? C22 O3 1.30(3) . ? C22 C23 1.549(17) 3_565 ? C23 O3 1.23(3) . ? C23 C22 1.549(17) 3_565 ? 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 C1 C2 123.2(4) . . ? N1 C1 C7 115.5(4) . . ? C2 C1 C7 121.0(4) . . ? N1 C1 Sr 40.6(2) . . ? C2 C1 Sr 155.5(3) . . ? C7 C1 Sr 76.9(2) . . ? C3 C2 C1 132.5(4) . . ? C2 C3 C4 129.9(5) . . ? C5 C4 C3 124.8(4) . . ? C4 C5 C6 130.3(4) . . ? C5 C6 C7 131.4(4) . . ? N2 C7 C6 123.1(4) . . ? N2 C7 C1 116.3(3) . . ? C6 C7 C1 120.3(4) . . ? N2 C7 Sr 41.00(18) . . ? C6 C7 Sr 154.1(3) . . ? C1 C7 Sr 77.7(2) . . ? N1 C8 C9 110.7(4) . . ? N1 C8 C10 108.9(4) . . ? C9 C8 C10 110.3(4) . . ? N2 C11 C12 108.7(3) . . ? N2 C11 C13 110.7(4) . . ? C12 C11 C13 110.7(4) . . ? O1 C14 C15 108.3(5) . . ? C16 C15 C14 107.2(6) . . ? C15 C16 C17 105.2(6) . . ? O1 C17 C16 105.1(5) . . ? O2 C18 C19B 105.8(6) . . ? O2 C18 C19A 104.8(9) . . ? C19B C18 C19A 23.5(8) . . ? C18 C19A C20A 103.9(13) . . ? C21 C20A C19A 95.2(11) . . ? C20B C19B C18 100.1(8) . . ? C19B C20B C21 105.0(9) . . ? O2 C21 C20A 108.3(6) . . ? O2 C21 C20B 104.6(6) . . ? C20A C21 C20B 27.7(6) . . ? C1 N1 C8 118.8(4) . . ? C1 N1 Sr 119.6(3) . . ? C8 N1 Sr 120.5(2) . . ? C7 N2 C11 119.0(3) . . ? C7 N2 Sr 119.3(2) . . ? C11 N2 Sr 120.1(2) . . ? C14 O1 C17 107.3(4) . . ? C14 O1 Sr 125.7(3) . . ? C17 O1 Sr 126.8(3) . . ? C21 O2 C18 107.9(4) . . ? C21 O2 Sr 128.1(3) . . ? C18 O2 Sr 122.0(3) . . ? Sr I Sr 98.126(11) . 3 ? N1 Sr N2 64.16(10) . . ? N1 Sr O1 89.06(11) . . ? N2 Sr O1 82.25(10) . . ? N1 Sr O2 84.27(11) . . ? N2 Sr O2 84.74(10) . . ? O1 Sr O2 166.94(9) . . ? N1 Sr I 169.41(7) . . ? N2 Sr I 108.51(8) . . ? O1 Sr I 97.67(8) . . ? O2 Sr I 87.48(7) . . ? N1 Sr I 107.11(7) . 3 ? N2 Sr I 163.41(8) . 3 ? O1 Sr I 83.56(7) . 3 ? O2 Sr I 109.13(7) . 3 ? I Sr I 81.872(11) . 3 ? N1 Sr C7 44.71(10) . . ? N2 Sr C7 19.73(10) . . ? O1 Sr C7 86.51(9) . . ? O2 Sr C7 80.85(9) . . ? I Sr C7 127.23(7) . . ? I Sr C7 150.35(7) 3 . ? N1 Sr C1 19.87(10) . . ? N2 Sr C1 44.46(10) . . ? O1 Sr C1 84.12(10) . . ? O2 Sr C1 85.84(10) . . ? I Sr C1 152.65(7) . . ? I Sr C1 125.32(7) 3 . ? C7 Sr C1 25.42(9) . . ? O3 C22 C23 111(2) . 3_565 ? O3 C23 C22 108(2) . 3_565 ? C23 O3 C22 88(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 C1 C2 C3 -166.2(5) . . . . ? C7 C1 C2 C3 19.5(8) . . . . ? Sr C1 C2 C3 152.6(5) . . . . ? C1 C2 C3 C4 6.9(10) . . . . ? C2 C3 C4 C5 -6.3(9) . . . . ? C3 C4 C5 C6 -9.1(9) . . . . ? C4 C5 C6 C7 0.7(9) . . . . ? C5 C6 C7 N2 -158.2(5) . . . . ? C5 C6 C7 C1 28.1(7) . . . . ? C5 C6 C7 Sr 157.8(5) . . . . ? N1 C1 C7 N2 -27.1(5) . . . . ? C2 C1 C7 N2 147.6(4) . . . . ? Sr C1 C7 N2 -14.3(3) . . . . ? N1 C1 C7 C6 147.1(4) . . . . ? C2 C1 C7 C6 -38.2(6) . . . . ? Sr C1 C7 C6 159.9(4) . . . . ? N1 C1 C7 Sr -12.8(3) . . . . ? C2 C1 C7 Sr 161.9(4) . . . . ? O1 C14 C15 C16 -4.4(10) . . . . ? C14 C15 C16 C17 18.7(10) . . . . ? C15 C16 C17 O1 -26.2(8) . . . . ? O2 C18 C19A C20A -24.4(15) . . . . ? C19B C18 C19A C20A 71(2) . . . . ? C18 C19A C20A C21 39.8(15) . . . . ? O2 C18 C19B C20B 39.7(10) . . . . ? C19A C18 C19B C20B -51(2) . . . . ? C18 C19B C20B C21 -37.5(11) . . . . ? C19A C20A C21 O2 -42.9(12) . . . . ? C19A C20A C21 C20B 43.8(15) . . . . ? C19B C20B C21 O2 22.9(11) . . . . ? C19B C20B C21 C20A -78.7(17) . . . . ? C2 C1 N1 C8 12.3(6) . . . . ? C7 C1 N1 C8 -173.1(4) . . . . ? Sr C1 N1 C8 167.4(5) . . . . ? C2 C1 N1 Sr -155.2(3) . . . . ? C7 C1 N1 Sr 19.4(5) . . . . ? C9 C8 N1 C1 -97.4(5) . . . . ? C10 C8 N1 C1 141.2(4) . . . . ? C9 C8 N1 Sr 69.9(5) . . . . ? C10 C8 N1 Sr -51.4(5) . . . . ? C6 C7 N2 C11 13.2(6) . . . . ? C1 C7 N2 C11 -172.8(3) . . . . ? Sr C7 N2 C11 165.6(5) . . . . ? C6 C7 N2 Sr -152.4(3) . . . . ? C1 C7 N2 Sr 21.5(5) . . . . ? C12 C11 N2 C7 138.0(4) . . . . ? C13 C11 N2 C7 -100.1(4) . . . . ? C12 C11 N2 Sr -56.5(4) . . . . ? C13 C11 N2 Sr 65.4(4) . . . . ? C15 C14 O1 C17 -12.5(8) . . . . ? C15 C14 O1 Sr 162.2(5) . . . . ? C16 C17 O1 C14 23.7(7) . . . . ? C16 C17 O1 Sr -150.9(4) . . . . ? C20A C21 O2 C18 31.0(8) . . . . ? C20B C21 O2 C18 2.4(7) . . . . ? C20A C21 O2 Sr -133.3(7) . . . . ? C20B C21 O2 Sr -161.9(5) . . . . ? C19B C18 O2 C21 -26.6(7) . . . . ? C19A C18 O2 C21 -2.2(10) . . . . ? C19B C18 O2 Sr 138.9(6) . . . . ? C19A C18 O2 Sr 163.3(9) . . . . ? C1 N1 Sr N2 -6.7(3) . . . . ? C8 N1 Sr N2 -173.9(4) . . . . ? C1 N1 Sr O1 75.2(3) . . . . ? C8 N1 Sr O1 -92.1(3) . . . . ? C1 N1 Sr O2 -93.6(3) . . . . ? C8 N1 Sr O2 99.2(3) . . . . ? C1 N1 Sr I -54.6(6) . . . . ? C8 N1 Sr I 138.2(4) . . . . ? C1 N1 Sr I 158.1(3) . . . 3 ? C8 N1 Sr I -9.1(3) . . . 3 ? C1 N1 Sr C7 -10.8(3) . . . . ? C8 N1 Sr C7 -178.1(4) . . . . ? C8 N1 Sr C1 -167.2(5) . . . . ? C7 N2 Sr N1 -8.7(3) . . . . ? C11 N2 Sr N1 -174.1(3) . . . . ? C7 N2 Sr O1 -101.4(3) . . . . ? C11 N2 Sr O1 93.1(3) . . . . ? C7 N2 Sr O2 77.5(3) . . . . ? C11 N2 Sr O2 -88.0(3) . . . . ? C7 N2 Sr I 163.1(3) . . . . ? C11 N2 Sr I -2.4(3) . . . . ? C7 N2 Sr I -70.0(4) . . . 3 ? C11 N2 Sr I 124.6(3) . . . 3 ? C11 N2 Sr C7 -165.5(5) . . . . ? C7 N2 Sr C1 -11.9(3) . . . . ? C11 N2 Sr C1 -177.4(4) . . . . ? C14 O1 Sr N1 160.8(5) . . . . ? C17 O1 Sr N1 -25.5(4) . . . . ? C14 O1 Sr N2 -135.1(5) . . . . ? C17 O1 Sr N2 38.5(4) . . . . ? C14 O1 Sr O2 -140.0(5) . . . . ? C17 O1 Sr O2 33.7(7) . . . . ? C14 O1 Sr I -27.4(5) . . . . ? C17 O1 Sr I 146.3(4) . . . . ? C14 O1 Sr I 53.5(4) . . . 3 ? C17 O1 Sr I -132.9(4) . . . 3 ? C14 O1 Sr C7 -154.5(5) . . . . ? C17 O1 Sr C7 19.2(4) . . . . ? C14 O1 Sr C1 -179.9(5) . . . . ? C17 O1 Sr C1 -6.2(4) . . . . ? C21 O2 Sr N1 178.0(4) . . . . ? C18 O2 Sr N1 15.7(4) . . . . ? C21 O2 Sr N2 113.5(4) . . . . ? C18 O2 Sr N2 -48.8(4) . . . . ? C21 O2 Sr O1 118.3(5) . . . . ? C18 O2 Sr O1 -44.0(7) . . . . ? C21 O2 Sr I 4.6(4) . . . . ? C18 O2 Sr I -157.7(4) . . . . ? C21 O2 Sr I -75.9(4) . . . 3 ? C18 O2 Sr I 121.8(4) . . . 3 ? C21 O2 Sr C7 133.0(4) . . . . ? C18 O2 Sr C7 -29.3(4) . . . . ? C21 O2 Sr C1 158.1(4) . . . . ? C18 O2 Sr C1 -4.2(4) . . . . ? Sr I Sr N1 -148.6(4) 3 . . . ? Sr I Sr N2 166.68(8) 3 . . . ? Sr I Sr O1 82.33(7) 3 . . . ? Sr I Sr O2 -109.73(7) 3 . . . ? Sr I Sr I 0.0 3 . . 3 ? Sr I Sr C7 173.77(9) 3 . . . ? Sr I Sr C1 174.36(15) 3 . . . ? N2 C7 Sr N1 168.9(4) . . . . ? C6 C7 Sr N1 -128.6(7) . . . . ? C1 C7 Sr N1 8.6(2) . . . . ? C6 C7 Sr N2 62.5(7) . . . . ? C1 C7 Sr N2 -160.3(4) . . . . ? N2 C7 Sr O1 76.7(3) . . . . ? C6 C7 Sr O1 139.2(7) . . . . ? C1 C7 Sr O1 -83.6(2) . . . . ? N2 C7 Sr O2 -100.0(3) . . . . ? C6 C7 Sr O2 -37.5(7) . . . . ? C1 C7 Sr O2 99.7(2) . . . . ? N2 C7 Sr I -20.3(3) . . . . ? C6 C7 Sr I 42.2(7) . . . . ? C1 C7 Sr I 179.38(18) . . . . ? N2 C7 Sr I 147.2(3) . . . 3 ? C6 C7 Sr I -150.3(6) . . . 3 ? C1 C7 Sr I -13.2(3) . . . 3 ? N2 C7 Sr C1 160.3(4) . . . . ? C6 C7 Sr C1 -137.1(8) . . . . ? C2 C1 Sr N1 57.9(7) . . . . ? C7 C1 Sr N1 -162.1(4) . . . . ? N1 C1 Sr N2 171.4(4) . . . . ? C2 C1 Sr N2 -130.7(8) . . . . ? C7 C1 Sr N2 9.3(2) . . . . ? N1 C1 Sr O1 -103.7(3) . . . . ? C2 C1 Sr O1 -45.8(7) . . . . ? C7 C1 Sr O1 94.3(2) . . . . ? N1 C1 Sr O2 84.7(3) . . . . ? C2 C1 Sr O2 142.6(7) . . . . ? C7 C1 Sr O2 -77.4(2) . . . . ? N1 C1 Sr I 161.0(2) . . . . ? C2 C1 Sr I -141.1(7) . . . . ? C7 C1 Sr I -1.1(3) . . . . ? N1 C1 Sr I -25.9(3) . . . 3 ? C2 C1 Sr I 32.0(8) . . . 3 ? C7 C1 Sr I 172.06(18) . . . 3 ? N1 C1 Sr C7 162.1(4) . . . . ? C2 C1 Sr C7 -140.0(8) . . . . ? C22 C23 O3 C22 69(2) 3_565 . . . ? C23 C22 O3 C23 -71(3) 3_565 . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.879 _refine_diff_density_min -0.662 _refine_diff_density_rms 0.083 #============================================================================== data_3 _database_code_depnum_ccdc_archive 'CCDC 671210' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H31 Ca N3 O' _chemical_formula_sum 'C23 H31 Ca N3 O' _chemical_formula_weight 405.59 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' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2527(8) _cell_length_b 9.6709(10) _cell_length_c 13.0943(11) _cell_angle_alpha 85.627(8) _cell_angle_beta 77.814(7) _cell_angle_gamma 83.535(8) _cell_volume 1136.36(18) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.376 _exptl_crystal_size_mid 0.217 _exptl_crystal_size_min 0.061 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.185 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 436 _exptl_absorpt_coefficient_mu 0.293 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.9154 _exptl_absorpt_correction_T_max 0.9646 _exptl_absorpt_process_details 'STOE X-RED & X-SHAPE' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'STOE IPDS 2T' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8961 _diffrn_reflns_av_R_equivalents 0.0553 _diffrn_reflns_av_sigmaI/netI 0.0510 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 25.02 _reflns_number_total 3997 _reflns_number_gt 3131 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA, PLATON (A.L.Spek, 2005)' _computing_data_reduction 'STOE X-RED, PLATON (A.L.Spek, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e' _computing_publication_material 'X-STEP32, Microsoft Word' _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^)+(0.0877P)^2^+0.0315P] 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 3997 _refine_ls_number_parameters 258 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0665 _refine_ls_R_factor_gt 0.0497 _refine_ls_wR_factor_ref 0.1379 _refine_ls_wR_factor_gt 0.1289 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 0.6287(3) 0.6697(3) 0.78702(19) 0.0415(6) Uani 1 1 d . . . C2 C 0.6215(3) 0.5473(3) 0.8558(2) 0.0606(8) Uani 1 1 d . . . H2 H 0.5522 0.4874 0.8448 0.073 Uiso 1 1 calc R . . C3 C 0.6953(4) 0.4985(4) 0.9353(3) 0.0728(10) Uani 1 1 d . . . H3 H 0.6647 0.4138 0.9705 0.087 Uiso 1 1 calc R . . C4 C 0.8047(4) 0.5518(4) 0.9714(2) 0.0730(11) Uani 1 1 d . . . H4 H 0.8412 0.5008 1.0272 0.088 Uiso 1 1 calc R . . C5 C 0.8640(4) 0.6693(4) 0.9348(3) 0.0696(10) Uani 1 1 d . . . H5 H 0.9400 0.6904 0.9681 0.084 Uiso 1 1 calc R . . C6 C 0.8342(4) 0.7666(3) 0.8563(2) 0.0593(8) Uani 1 1 d . . . H6 H 0.8955 0.8410 0.8457 0.071 Uiso 1 1 calc R . . C7 C 0.7315(3) 0.7783(3) 0.78853(19) 0.0422(6) Uani 1 1 d . . . C8 C 0.4441(3) 0.5969(3) 0.7013(2) 0.0528(7) Uani 1 1 d . . . H8 H 0.3897 0.5610 0.7708 0.063 Uiso 1 1 calc R . . C9 C 0.5316(4) 0.4757(3) 0.6414(3) 0.0743(10) Uani 1 1 d . . . H9A H 0.5906 0.5112 0.5754 0.111 Uiso 1 1 calc R . . H9B H 0.4628 0.4135 0.6267 0.111 Uiso 1 1 calc R . . H9C H 0.5980 0.4242 0.6834 0.111 Uiso 1 1 calc R . . C10 C 0.3332(4) 0.6730(4) 0.6408(3) 0.0725(10) Uani 1 1 d . . . H10A H 0.2715 0.7454 0.6833 0.109 Uiso 1 1 calc R . . H10B H 0.2698 0.6066 0.6244 0.109 Uiso 1 1 calc R . . H10C H 0.3867 0.7161 0.5756 0.109 Uiso 1 1 calc R . . C11 C 0.8178(3) 0.9968(3) 0.7075(3) 0.0574(8) Uani 1 1 d . . . H11 H 0.8219 1.0306 0.7770 0.069 Uiso 1 1 calc R . . C12 C 0.9717(4) 0.9423(5) 0.6519(4) 0.0855(12) Uani 1 1 d . . . H12A H 1.0067 0.8591 0.6907 0.128 Uiso 1 1 calc R . . H12B H 1.0397 1.0142 0.6478 0.128 Uiso 1 1 calc R . . H12C H 0.9684 0.9185 0.5810 0.128 Uiso 1 1 calc R . . C13 C 0.7544(5) 1.1134(4) 0.6419(4) 0.0961(16) Uani 1 1 d . . . H13A H 0.7554 1.0808 0.5727 0.144 Uiso 1 1 calc R . . H13B H 0.8147 1.1921 0.6342 0.144 Uiso 1 1 calc R . . H13C H 0.6520 1.1432 0.6762 0.144 Uiso 1 1 calc R . . C14 C 0.2566(3) 1.1778(2) 0.70782(19) 0.0379(5) Uani 1 1 d . A . C15 C 0.1769(3) 1.2943(3) 0.7662(2) 0.0519(7) Uani 1 1 d . . . H15 H 0.2071 1.3050 0.8299 0.062 Uiso 1 1 calc R . . C16 C 0.0667(3) 1.3909(3) 0.7459(2) 0.0562(7) Uani 1 1 d . . . H16 H 0.0280 1.4545 0.7991 0.067 Uiso 1 1 calc R . . C17 C 0.0019(3) 1.4099(3) 0.6573(2) 0.0534(7) Uani 1 1 d . . . H17 H -0.0883 1.4692 0.6628 0.064 Uiso 1 1 calc R . . C18 C 0.0569(3) 1.3511(3) 0.5653(2) 0.0468(6) Uani 1 1 d . . . H18 H -0.0004 1.3746 0.5131 0.056 Uiso 1 1 calc R . . C19 C 0.1867(3) 1.2600(2) 0.5348(2) 0.0401(5) Uani 1 1 d . . . H19 H 0.2160 1.2502 0.4615 0.048 Uiso 1 1 calc R . . C20 C 0.2787(3) 1.1825(2) 0.59289(18) 0.0329(5) Uani 1 1 d . A . C21A C 0.3145(6) 1.0690(5) 0.8657(3) 0.0365(10) Uiso 0.60 1 d P A 1 H21A H 0.2185 1.1216 0.8981 0.044 Uiso 0.60 1 calc PR A 1 C22A C 0.4416(6) 1.1333(6) 0.8958(4) 0.0514(12) Uiso 0.60 1 d P A 1 H22A H 0.5360 1.0798 0.8673 0.077 Uiso 0.60 1 calc PR A 1 H22B H 0.4270 1.1316 0.9722 0.077 Uiso 0.60 1 calc PR A 1 H22C H 0.4434 1.2299 0.8673 0.077 Uiso 0.60 1 calc PR A 1 C23A C 0.3117(7) 0.9163(6) 0.9053(4) 0.0550(13) Uiso 0.60 1 d P A 1 H23A H 0.2370 0.8743 0.8781 0.083 Uiso 0.60 1 calc PR A 1 H23B H 0.2868 0.9107 0.9819 0.083 Uiso 0.60 1 calc PR A 1 H23C H 0.4097 0.8660 0.8812 0.083 Uiso 0.60 1 calc PR A 1 C21B C 0.2755(9) 1.0348(8) 0.8660(5) 0.0412(17) Uiso 0.40 1 d P A 2 H21B H 0.1791 1.0906 0.8932 0.049 Uiso 0.40 1 calc PR A 2 C22B C 0.3995(10) 1.0874(9) 0.9098(7) 0.056(2) Uiso 0.40 1 d P A 2 H22D H 0.4943 1.0340 0.8822 0.083 Uiso 0.40 1 calc PR A 2 H22E H 0.3770 1.0755 0.9864 0.083 Uiso 0.40 1 calc PR A 2 H22F H 0.4063 1.1864 0.8889 0.083 Uiso 0.40 1 calc PR A 2 C23B C 0.2608(11) 0.8840(9) 0.8964(7) 0.0574(19) Uiso 0.40 1 d P A 2 H23D H 0.1906 0.8502 0.8599 0.086 Uiso 0.40 1 calc PR A 2 H23E H 0.2243 0.8726 0.9721 0.086 Uiso 0.40 1 calc PR A 2 H23F H 0.3581 0.8305 0.8771 0.086 Uiso 0.40 1 calc PR A 2 N1 N 0.5439(2) 0.6974(2) 0.71733(16) 0.0394(5) Uani 1 1 d . . . N2 N 0.7169(2) 0.8861(2) 0.72159(16) 0.0409(5) Uani 1 1 d . . . N3 N 0.3235(2) 1.0688(2) 0.75080(16) 0.0451(5) Uani 1 1 d . . . O O 0.39059(18) 1.09951(16) 0.54471(12) 0.0387(4) Uani 1 1 d . . . Ca Ca 0.51546(5) 0.92314(5) 0.63379(4) 0.03433(17) 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 0.0388(13) 0.0462(14) 0.0342(13) 0.0007(10) -0.0042(10) 0.0110(10) C2 0.0550(17) 0.0671(19) 0.0506(17) 0.0205(14) -0.0049(14) 0.0059(14) C3 0.067(2) 0.085(2) 0.0473(18) 0.0268(17) 0.0035(16) 0.0242(18) C4 0.079(2) 0.090(3) 0.0383(16) -0.0059(16) -0.0148(16) 0.046(2) C5 0.080(2) 0.082(2) 0.0508(18) -0.0251(18) -0.0374(17) 0.0344(19) C6 0.0661(19) 0.0606(18) 0.0572(18) -0.0170(14) -0.0324(15) 0.0153(14) C7 0.0422(14) 0.0503(14) 0.0331(12) -0.0120(11) -0.0114(11) 0.0139(11) C8 0.0519(16) 0.0449(15) 0.0637(18) 0.0074(13) -0.0167(14) -0.0115(12) C9 0.084(2) 0.0457(16) 0.098(3) -0.0131(17) -0.021(2) -0.0157(16) C10 0.070(2) 0.064(2) 0.095(3) 0.0044(18) -0.041(2) -0.0163(17) C11 0.0516(17) 0.0576(17) 0.069(2) -0.0073(15) -0.0224(15) -0.0117(13) C12 0.062(2) 0.098(3) 0.100(3) 0.006(2) -0.020(2) -0.027(2) C13 0.085(3) 0.0474(19) 0.168(5) 0.029(2) -0.057(3) -0.0253(18) C14 0.0371(13) 0.0397(13) 0.0359(13) -0.0065(10) -0.0075(10) 0.0036(10) C15 0.0615(17) 0.0538(16) 0.0367(14) -0.0114(12) -0.0080(12) 0.0120(13) C16 0.0634(18) 0.0491(15) 0.0476(16) -0.0122(13) 0.0001(14) 0.0166(14) C17 0.0468(15) 0.0448(15) 0.0613(19) -0.0034(13) -0.0040(14) 0.0144(12) C18 0.0458(15) 0.0398(14) 0.0539(16) 0.0026(12) -0.0150(13) 0.0058(11) C19 0.0453(14) 0.0357(12) 0.0376(13) -0.0029(10) -0.0093(11) 0.0055(10) C20 0.0363(12) 0.0282(11) 0.0330(12) -0.0044(9) -0.0055(10) 0.0005(9) N1 0.0429(11) 0.0361(10) 0.0382(11) 0.0017(8) -0.0098(9) 0.0008(9) N2 0.0398(11) 0.0440(12) 0.0402(11) -0.0052(9) -0.0122(9) 0.0003(9) N3 0.0500(12) 0.0504(12) 0.0313(11) -0.0040(9) -0.0093(9) 0.0128(10) O 0.0448(10) 0.0368(9) 0.0315(8) -0.0042(7) -0.0081(7) 0.0113(7) Ca 0.0377(3) 0.0342(3) 0.0303(3) -0.00208(18) -0.00990(19) 0.00560(18) _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 N1 1.318(3) . ? C1 C2 1.431(4) . ? C1 C7 1.498(4) . ? C2 C3 1.388(4) . ? C3 C4 1.368(6) . ? C4 C5 1.330(6) . ? C5 C6 1.390(5) . ? C6 C7 1.421(4) . ? C7 N2 1.324(3) . ? C8 N1 1.469(3) . ? C8 C9 1.518(5) . ? C8 C10 1.519(4) . ? C11 N2 1.474(3) . ? C11 C13 1.506(5) . ? C11 C12 1.513(5) . ? C14 N3 1.311(3) . ? C14 C15 1.451(4) . ? C14 C20 1.473(3) . ? C15 C16 1.358(4) . ? C16 C17 1.406(4) . ? C17 C18 1.346(4) . ? C18 C19 1.412(4) . ? C19 C20 1.381(3) . ? C20 O 1.315(3) . ? C20 Ca 3.230(2) . ? C21A N3 1.489(5) . ? C21A C22A 1.525(7) . ? C21A C23A 1.528(7) . ? C21B C23B 1.495(12) . ? C21B N3 1.502(7) . ? C21B C22B 1.536(11) . ? N1 Ca 2.379(2) . ? N2 Ca 2.370(2) . ? N3 Ca 2.470(2) . ? O Ca 2.3295(16) . ? O Ca 2.3333(17) 2_676 ? Ca O 2.3333(17) 2_676 ? Ca Ca 3.7552(10) 2_676 ? 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 C1 C2 122.7(3) . . ? N1 C1 C7 114.1(2) . . ? C2 C1 C7 123.2(2) . . ? C3 C2 C1 133.0(3) . . ? C4 C3 C2 130.8(3) . . ? C5 C4 C3 125.3(3) . . ? C4 C5 C6 131.3(3) . . ? C5 C6 C7 133.6(3) . . ? N2 C7 C6 123.3(3) . . ? N2 C7 C1 113.8(2) . . ? C6 C7 C1 122.9(3) . . ? N1 C8 C9 110.6(2) . . ? N1 C8 C10 107.8(2) . . ? C9 C8 C10 110.5(3) . . ? N2 C11 C13 106.6(2) . . ? N2 C11 C12 110.0(3) . . ? C13 C11 C12 110.1(3) . . ? N3 C14 C15 123.4(2) . . ? N3 C14 C20 115.8(2) . . ? C15 C14 C20 120.5(2) . . ? C16 C15 C14 131.4(3) . . ? C15 C16 C17 129.1(3) . . ? C18 C17 C16 125.4(3) . . ? C17 C18 C19 129.8(3) . . ? C20 C19 C18 131.3(2) . . ? O C20 C19 119.0(2) . . ? O C20 C14 115.8(2) . . ? C19 C20 C14 125.0(2) . . ? O C20 Ca 37.54(10) . . ? C19 C20 Ca 153.67(17) . . ? C14 C20 Ca 79.05(13) . . ? N3 C21A C22A 114.1(4) . . ? N3 C21A C23A 105.5(4) . . ? C22A C21A C23A 111.0(4) . . ? C23B C21B N3 115.3(6) . . ? C23B C21B C22B 111.3(7) . . ? N3 C21B C22B 101.9(6) . . ? C1 N1 C8 120.8(2) . . ? C1 N1 Ca 121.68(17) . . ? C8 N1 Ca 116.80(16) . . ? C7 N2 C11 120.6(2) . . ? C7 N2 Ca 122.18(16) . . ? C11 N2 Ca 116.94(17) . . ? C14 N3 C21A 116.4(2) . . ? C14 N3 C21B 119.1(3) . . ? C21A N3 C21B 19.8(3) . . ? C14 N3 Ca 117.30(16) . . ? C21A N3 Ca 123.2(2) . . ? C21B N3 Ca 123.5(3) . . ? C20 O Ca 122.34(14) . . ? C20 O Ca 130.03(14) . 2_676 ? Ca O Ca 107.29(6) . 2_676 ? O Ca O 72.71(6) . 2_676 ? O Ca N2 140.49(7) . . ? O Ca N2 108.27(7) 2_676 . ? O Ca N1 153.62(7) . . ? O Ca N1 107.06(7) 2_676 . ? N2 Ca N1 65.53(7) . . ? O Ca N3 66.65(6) . . ? O Ca N3 139.32(6) 2_676 . ? N2 Ca N3 104.16(7) . . ? N1 Ca N3 108.36(7) . . ? O Ca C20 20.12(6) . . ? O Ca C20 92.72(6) 2_676 . ? N2 Ca C20 135.83(7) . . ? N1 Ca C20 144.61(7) . . ? N3 Ca C20 46.60(6) . . ? O Ca Ca 36.39(4) . 2_676 ? O Ca Ca 36.32(4) 2_676 2_676 ? N2 Ca Ca 132.32(6) . 2_676 ? N1 Ca Ca 137.56(6) . 2_676 ? N3 Ca Ca 103.02(5) . 2_676 ? C20 Ca Ca 56.43(4) . 2_676 ? 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 C1 C2 C3 -178.3(3) . . . . ? C7 C1 C2 C3 1.0(5) . . . . ? C1 C2 C3 C4 -2.4(7) . . . . ? C2 C3 C4 C5 0.5(6) . . . . ? C3 C4 C5 C6 1.0(6) . . . . ? C4 C5 C6 C7 0.9(6) . . . . ? C5 C6 C7 N2 176.4(3) . . . . ? C5 C6 C7 C1 -3.2(5) . . . . ? N1 C1 C7 N2 1.9(3) . . . . ? C2 C1 C7 N2 -177.5(2) . . . . ? N1 C1 C7 C6 -178.6(2) . . . . ? C2 C1 C7 C6 2.1(4) . . . . ? N3 C14 C15 C16 -156.7(3) . . . . ? C20 C14 C15 C16 29.2(5) . . . . ? C14 C15 C16 C17 -3.6(6) . . . . ? C15 C16 C17 C18 -13.6(5) . . . . ? C16 C17 C18 C19 0.0(5) . . . . ? C17 C18 C19 C20 14.8(5) . . . . ? C18 C19 C20 O 176.8(2) . . . . ? C18 C19 C20 C14 1.0(4) . . . . ? C18 C19 C20 Ca 154.2(3) . . . . ? N3 C14 C20 O -17.0(3) . . . . ? C15 C14 C20 O 157.5(2) . . . . ? N3 C14 C20 C19 158.9(2) . . . . ? C15 C14 C20 C19 -26.6(4) . . . . ? N3 C14 C20 Ca -9.32(19) . . . . ? C15 C14 C20 Ca 165.2(2) . . . . ? C2 C1 N1 C8 -4.7(4) . . . . ? C7 C1 N1 C8 176.0(2) . . . . ? C2 C1 N1 Ca 164.9(2) . . . . ? C7 C1 N1 Ca -14.4(3) . . . . ? C9 C8 N1 C1 -74.7(3) . . . . ? C10 C8 N1 C1 164.4(3) . . . . ? C9 C8 N1 Ca 115.2(2) . . . . ? C10 C8 N1 Ca -5.7(3) . . . . ? C6 C7 N2 C11 5.2(4) . . . . ? C1 C7 N2 C11 -175.2(2) . . . . ? C6 C7 N2 Ca -168.0(2) . . . . ? C1 C7 N2 Ca 11.5(3) . . . . ? C13 C11 N2 C7 -170.1(3) . . . . ? C12 C11 N2 C7 70.5(4) . . . . ? C13 C11 N2 Ca 3.4(4) . . . . ? C12 C11 N2 Ca -116.0(3) . . . . ? C15 C14 N3 C21A 0.0(4) . . . . ? C20 C14 N3 C21A 174.3(3) . . . . ? C15 C14 N3 C21B 22.3(5) . . . . ? C20 C14 N3 C21B -163.4(4) . . . . ? C15 C14 N3 Ca -160.8(2) . . . . ? C20 C14 N3 Ca 13.5(3) . . . . ? C22A C21A N3 C14 -90.7(4) . . . . ? C23A C21A N3 C14 147.2(3) . . . . ? C22A C21A N3 C21B 166.3(13) . . . . ? C23A C21A N3 C21B 44.2(10) . . . . ? C22A C21A N3 Ca 68.8(4) . . . . ? C23A C21A N3 Ca -53.3(5) . . . . ? C23B C21B N3 C14 136.6(6) . . . . ? C22B C21B N3 C14 -102.8(5) . . . . ? C23B C21B N3 C21A -136.0(15) . . . . ? C22B C21B N3 C21A -15.3(9) . . . . ? C23B C21B N3 Ca -40.2(8) . . . . ? C22B C21B N3 Ca 80.4(6) . . . . ? C19 C20 O Ca -163.79(16) . . . . ? C14 C20 O Ca 12.4(3) . . . . ? C19 C20 O Ca 8.6(3) . . . 2_676 ? C14 C20 O Ca -175.22(14) . . . 2_676 ? Ca C20 O Ca 172.4(2) . . . 2_676 ? C20 O Ca O 173.9(2) . . . 2_676 ? Ca O Ca O 0.0 2_676 . . 2_676 ? C20 O Ca N2 -88.15(19) . . . . ? Ca O Ca N2 97.96(11) 2_676 . . . ? C20 O Ca N1 80.2(2) . . . . ? Ca O Ca N1 -93.66(16) 2_676 . . . ? C20 O Ca N3 -4.15(16) . . . . ? Ca O Ca N3 -178.04(9) 2_676 . . . ? Ca O Ca C20 -173.9(2) 2_676 . . . ? C20 O Ca Ca 173.9(2) . . . 2_676 ? C7 N2 Ca O 160.81(16) . . . . ? C11 N2 Ca O -12.7(2) . . . . ? C7 N2 Ca O -114.45(19) . . . 2_676 ? C11 N2 Ca O 72.1(2) . . . 2_676 ? C7 N2 Ca N1 -13.55(18) . . . . ? C11 N2 Ca N1 173.0(2) . . . . ? C7 N2 Ca N3 90.5(2) . . . . ? C11 N2 Ca N3 -83.0(2) . . . . ? C7 N2 Ca C20 131.24(18) . . . . ? C11 N2 Ca C20 -42.2(2) . . . . ? C7 N2 Ca Ca -146.57(16) . . . 2_676 ? C11 N2 Ca Ca 40.0(2) . . . 2_676 ? C1 N1 Ca O -157.24(17) . . . . ? C8 N1 Ca O 12.8(3) . . . . ? C1 N1 Ca O 117.41(19) . . . 2_676 ? C8 N1 Ca O -72.6(2) . . . 2_676 ? C1 N1 Ca N2 14.66(18) . . . . ? C8 N1 Ca N2 -175.3(2) . . . . ? C1 N1 Ca N3 -82.9(2) . . . . ? C8 N1 Ca N3 87.1(2) . . . . ? C1 N1 Ca C20 -121.42(19) . . . . ? C8 N1 Ca C20 48.6(2) . . . . ? C1 N1 Ca Ca 141.43(16) . . . 2_676 ? C8 N1 Ca Ca -48.5(2) . . . 2_676 ? C14 N3 Ca O -5.64(17) . . . . ? C21A N3 Ca O -165.0(3) . . . . ? C21B N3 Ca O 171.2(4) . . . . ? C14 N3 Ca O -8.5(2) . . . 2_676 ? C21A N3 Ca O -167.9(3) . . . 2_676 ? C21B N3 Ca O 168.3(4) . . . 2_676 ? C14 N3 Ca N2 133.62(18) . . . . ? C21A N3 Ca N2 -25.7(3) . . . . ? C21B N3 Ca N2 -49.6(4) . . . . ? C14 N3 Ca N1 -157.87(18) . . . . ? C21A N3 Ca N1 42.8(3) . . . . ? C21B N3 Ca N1 19.0(4) . . . . ? C14 N3 Ca C20 -7.61(16) . . . . ? C21A N3 Ca C20 -167.0(3) . . . . ? C21B N3 Ca C20 169.2(4) . . . . ? C14 N3 Ca Ca -6.84(19) . . . 2_676 ? C21A N3 Ca Ca -166.2(3) . . . 2_676 ? C21B N3 Ca Ca 170.0(4) . . . 2_676 ? C19 C20 Ca O 33.4(3) . . . . ? C14 C20 Ca O -168.6(2) . . . . ? O C20 Ca O -5.84(19) . . . 2_676 ? C19 C20 Ca O 27.6(4) . . . 2_676 ? C14 C20 Ca O -174.48(13) . . . 2_676 ? O C20 Ca N2 114.11(18) . . . . ? C19 C20 Ca N2 147.5(4) . . . . ? C14 C20 Ca N2 -54.52(17) . . . . ? O C20 Ca N1 -130.87(17) . . . . ? C19 C20 Ca N1 -97.5(4) . . . . ? C14 C20 Ca N1 60.50(18) . . . . ? O C20 Ca N3 174.8(2) . . . . ? C19 C20 Ca N3 -151.8(4) . . . . ? C14 C20 Ca N3 6.12(13) . . . . ? O C20 Ca Ca -4.35(14) . . . 2_676 ? C19 C20 Ca Ca 29.1(4) . . . 2_676 ? C14 C20 Ca Ca -172.98(14) . . . 2_676 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.636 _refine_diff_density_min -0.283 _refine_diff_density_rms 0.052 #============================================================================== data_4 _database_code_depnum_ccdc_archive 'CCDC 671211' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H55 Ca N3 O2 P2' _chemical_formula_sum 'C45 H55 Ca N3 O2 P2' _chemical_formula_weight 771.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 11.2102(6) _cell_length_b 20.3384(11) _cell_length_c 19.1420(11) _cell_angle_alpha 90.00 _cell_angle_beta 102.373(4) _cell_angle_gamma 90.00 _cell_volume 4263.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 21217 _cell_measurement_theta_min 2.73 _cell_measurement_theta_max 29.45 _exptl_crystal_description rod _exptl_crystal_colour orange _exptl_crystal_size_max 0.480 _exptl_crystal_size_mid 0.462 _exptl_crystal_size_min 0.430 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.203 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1648 _exptl_absorpt_coefficient_mu 0.261 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.9359 _exptl_absorpt_correction_T_max 0.9727 _exptl_absorpt_process_details 'STOE X-RED & X-SHAPE' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'STOE IPDS 2T' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30286 _diffrn_reflns_av_R_equivalents 0.1480 _diffrn_reflns_av_sigmaI/netI 0.0879 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 25.02 _reflns_number_total 7512 _reflns_number_gt 5593 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA, PLATON (A.L.Spek, 2005)' _computing_data_reduction 'STOE X-RED, PLATON (A.L.Spek, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e' _computing_publication_material 'X-STEP32, Microsoft Word' _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^)+(0.0485P)^2^+3.5583P] 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 7512 _refine_ls_number_parameters 466 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0935 _refine_ls_R_factor_gt 0.0712 _refine_ls_wR_factor_ref 0.1578 _refine_ls_wR_factor_gt 0.1485 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 0.0691(3) 0.11437(16) 0.38972(18) 0.0315(7) Uani 1 1 d . . . C2 C 0.0479(3) 0.11303(17) 0.4607(2) 0.0395(8) Uani 1 1 d . . . H2 H 0.1022 0.0851 0.4923 0.047 Uiso 1 1 calc R . . C3 C -0.0354(4) 0.14416(19) 0.4921(2) 0.0480(10) Uani 1 1 d . . . H3 H -0.0255 0.1369 0.5420 0.058 Uiso 1 1 calc R . . C4 C -0.1319(4) 0.1846(2) 0.4619(2) 0.0562(11) Uani 1 1 d . . . H4 H -0.1859 0.1979 0.4913 0.067 Uiso 1 1 calc R . . C5 C -0.1556(4) 0.2072(2) 0.3921(3) 0.0544(11) Uani 1 1 d . . . H5 H -0.2320 0.2287 0.3767 0.065 Uiso 1 1 calc R . . C6 C -0.0851(3) 0.2030(2) 0.3420(2) 0.0484(10) Uani 1 1 d . . . H6 H -0.1196 0.2245 0.2982 0.058 Uiso 1 1 calc R . . C7 C 0.0300(3) 0.17276(17) 0.3426(2) 0.0374(8) Uani 1 1 d . A . C8 C 0.1548(4) 0.00633(17) 0.4031(2) 0.0432(9) Uani 1 1 d . . . H8 H 0.0914 0.0002 0.4321 0.052 Uiso 1 1 calc R . . C9 C 0.2804(4) 0.0060(2) 0.4536(3) 0.0655(13) Uani 1 1 d . . . H9A H 0.3439 0.0032 0.4256 0.098 Uiso 1 1 calc R . . H9B H 0.2868 -0.0321 0.4856 0.098 Uiso 1 1 calc R . . H9C H 0.2912 0.0465 0.4820 0.098 Uiso 1 1 calc R . . C10 C 0.1441(5) -0.04990(19) 0.3496(3) 0.0596(12) Uani 1 1 d . . . H10A H 0.0629 -0.0491 0.3179 0.089 Uiso 1 1 calc R . . H10B H 0.1558 -0.0919 0.3754 0.089 Uiso 1 1 calc R . . H10C H 0.2065 -0.0450 0.3212 0.089 Uiso 1 1 calc R . . C11A C 0.0937(7) 0.2562(4) 0.2695(4) 0.0353(15) Uiso 0.50 1 d P A 1 H11A H 0.0450 0.2845 0.2958 0.042 Uiso 0.50 1 calc PR A 1 C12A C 0.0205(8) 0.2455(4) 0.1902(5) 0.052(2) Uiso 0.50 1 d P A 1 H12A H 0.0688 0.2182 0.1644 0.078 Uiso 0.50 1 calc PR A 1 H12B H 0.0045 0.2882 0.1663 0.078 Uiso 0.50 1 calc PR A 1 H12C H -0.0571 0.2236 0.1907 0.078 Uiso 0.50 1 calc PR A 1 C13A C 0.2146(8) 0.2881(4) 0.2703(5) 0.054(2) Uiso 0.50 1 d P A 1 H13A H 0.2562 0.2972 0.3198 0.082 Uiso 0.50 1 calc PR A 1 H13B H 0.2015 0.3295 0.2434 0.082 Uiso 0.50 1 calc PR A 1 H13C H 0.2650 0.2586 0.2482 0.082 Uiso 0.50 1 calc PR A 1 C12B C 0.1274(10) 0.2335(5) 0.1814(6) 0.072(3) Uiso 0.50 1 d P A 2 H12D H 0.0967 0.2654 0.1433 0.108 Uiso 0.50 1 calc PR A 2 H12E H 0.1194 0.1890 0.1614 0.108 Uiso 0.50 1 calc PR A 2 H12F H 0.2135 0.2427 0.2021 0.108 Uiso 0.50 1 calc PR A 2 C13B C 0.0652(10) 0.3027(5) 0.2739(6) 0.073(3) Uiso 0.50 1 d P A 2 H13D H 0.0147 0.3040 0.3099 0.110 Uiso 0.50 1 calc PR A 2 H13E H 0.0380 0.3370 0.2381 0.110 Uiso 0.50 1 calc PR A 2 H13F H 0.1508 0.3103 0.2972 0.110 Uiso 0.50 1 calc PR A 2 C11B C 0.0533(8) 0.2390(4) 0.2395(5) 0.0438(18) Uiso 0.50 1 d P A 2 H11B H -0.0348 0.2300 0.2183 0.053 Uiso 0.50 1 calc PR A 2 C14 C 0.3763(3) -0.05479(16) 0.17350(19) 0.0360(8) Uani 1 1 d . . . C15 C 0.4606(4) -0.07619(19) 0.1350(2) 0.0476(10) Uani 1 1 d . . . H15 H 0.5423 -0.0604 0.1469 0.057 Uiso 1 1 calc R . . C16 C 0.4262(5) -0.1206(2) 0.0789(2) 0.0588(12) Uani 1 1 d . . . H16 H 0.4848 -0.1356 0.0533 0.071 Uiso 1 1 calc R . . C17 C 0.3072(5) -0.1430(2) 0.0604(2) 0.0592(12) Uani 1 1 d . . . H17 H 0.2836 -0.1726 0.0215 0.071 Uiso 1 1 calc R . . C18 C 0.2234(4) -0.1224(2) 0.0985(2) 0.0536(10) Uani 1 1 d . . . H18 H 0.1419 -0.1382 0.0861 0.064 Uiso 1 1 calc R . . C19 C 0.2573(3) -0.07845(18) 0.1551(2) 0.0422(9) Uani 1 1 d . . . H19 H 0.1987 -0.0645 0.1812 0.051 Uiso 1 1 calc R . . C20 C 0.5678(3) -0.01187(16) 0.28629(18) 0.0320(7) Uani 1 1 d . . . C21 C 0.6598(3) 0.03478(19) 0.2956(2) 0.0394(8) Uani 1 1 d . . . H21 H 0.6422 0.0775 0.2760 0.047 Uiso 1 1 calc R . . C22 C 0.7766(3) 0.0205(2) 0.3330(2) 0.0499(10) Uani 1 1 d . . . H22 H 0.8383 0.0533 0.3390 0.060 Uiso 1 1 calc R . . C23 C 0.8038(4) -0.0414(2) 0.3615(2) 0.0558(11) Uani 1 1 d . . . H23 H 0.8844 -0.0516 0.3864 0.067 Uiso 1 1 calc R . . C24 C 0.7135(4) -0.0882(2) 0.3536(3) 0.0598(12) Uani 1 1 d . . . H24 H 0.7313 -0.1307 0.3738 0.072 Uiso 1 1 calc R . . C25 C 0.5964(4) -0.07353(19) 0.3163(2) 0.0481(10) Uani 1 1 d . . . H25 H 0.5346 -0.1062 0.3111 0.058 Uiso 1 1 calc R . . C26 C 0.5466(3) 0.17730(16) 0.16941(19) 0.0327(7) Uani 1 1 d . . . C27 C 0.5341(3) 0.21326(17) 0.2290(2) 0.0393(8) Uani 1 1 d . . . H27 H 0.4827 0.1974 0.2588 0.047 Uiso 1 1 calc R . . C28 C 0.5961(4) 0.27232(17) 0.2456(2) 0.0457(9) Uani 1 1 d . . . H28 H 0.5858 0.2969 0.2861 0.055 Uiso 1 1 calc R . . C29 C 0.6720(3) 0.29517(18) 0.2036(2) 0.0459(10) Uani 1 1 d . . . H29 H 0.7150 0.3353 0.2154 0.055 Uiso 1 1 calc R . . C30 C 0.6858(3) 0.2602(2) 0.1450(2) 0.0459(9) Uani 1 1 d . . . H30 H 0.7375 0.2765 0.1155 0.055 Uiso 1 1 calc R . . C31 C 0.6251(3) 0.20136(19) 0.1283(2) 0.0400(8) Uani 1 1 d . . . H31 H 0.6372 0.1769 0.0881 0.048 Uiso 1 1 calc R . . C32A C 0.3388(7) 0.1398(4) 0.0760(4) 0.0290(18) Uiso 0.50 1 d P A 1 C33A C 0.2812(6) 0.1975(4) 0.0885(4) 0.0353(16) Uiso 0.50 1 d P A 1 H33A H 0.3074 0.2201 0.1325 0.042 Uiso 0.50 1 calc PR A 1 C34A C 0.1860(7) 0.2224(4) 0.0373(4) 0.0420(17) Uiso 0.50 1 d P A 1 H34A H 0.1466 0.2619 0.0463 0.050 Uiso 0.50 1 calc PR A 1 C35A C 0.1477(9) 0.1896(5) -0.0278(6) 0.050(2) Uiso 0.50 1 d P A 1 H35A H 0.0828 0.2078 -0.0626 0.060 Uiso 0.50 1 calc PR A 1 C36A C 0.2034(9) 0.1286(6) -0.0443(5) 0.047(2) Uiso 0.50 1 d P A 1 H36A H 0.1769 0.1050 -0.0876 0.056 Uiso 0.50 1 calc PR A 1 C37A C 0.3004(7) 0.1084(4) 0.0105(4) 0.0354(16) Uiso 0.50 1 d P A 1 H37A H 0.3435 0.0699 0.0023 0.043 Uiso 0.50 1 calc PR A 1 O1A O 0.3868(6) 0.1581(3) 0.3641(4) 0.0401(18) Uiso 0.50 1 d P A 1 C38A C 0.5086(9) 0.1196(5) 0.4114(5) 0.046(3) Uiso 0.50 1 d P A 1 H38A H 0.4978 0.0714 0.4059 0.055 Uiso 0.50 1 calc PR A 1 H38B H 0.5824 0.1323 0.3940 0.055 Uiso 0.50 1 calc PR A 1 C39A C 0.5226(9) 0.1380(5) 0.4870(5) 0.061(2) Uiso 0.50 1 d P A 1 H39A H 0.6094 0.1424 0.5117 0.073 Uiso 0.50 1 calc PR A 1 H39B H 0.4807 0.1069 0.5135 0.073 Uiso 0.50 1 calc PR A 1 C40A C 0.4521(13) 0.2102(7) 0.4740(8) 0.096(4) Uiso 0.50 1 d P A 1 H40A H 0.4119 0.2194 0.5142 0.116 Uiso 0.50 1 calc PR A 1 H40B H 0.5128 0.2453 0.4728 0.116 Uiso 0.50 1 calc PR A 1 C41A C 0.3617(9) 0.2103(5) 0.4075(6) 0.056(2) Uiso 0.50 1 d P A 1 H41A H 0.2790 0.2048 0.4173 0.067 Uiso 0.50 1 calc PR A 1 H41B H 0.3641 0.2527 0.3824 0.067 Uiso 0.50 1 calc PR A 1 O2A O 0.0785(5) 0.0537(3) 0.1836(3) 0.0354(14) Uiso 0.50 1 d P A 1 C43A C -0.0472(9) 0.0253(5) 0.0813(6) 0.066(2) Uiso 0.50 1 d P A 1 H43A H -0.0289 -0.0215 0.0740 0.079 Uiso 0.50 1 calc PR A 1 H43B H -0.0917 0.0439 0.0353 0.079 Uiso 0.50 1 calc PR A 1 C44A C -0.1247(15) 0.0323(10) 0.1401(9) 0.122(5) Uiso 0.50 1 d P A 1 H44A H -0.1793 0.0711 0.1312 0.146 Uiso 0.50 1 calc PR A 1 H44B H -0.1738 -0.0076 0.1431 0.146 Uiso 0.50 1 calc PR A 1 C45A C -0.0371(8) 0.0401(5) 0.1987(5) 0.048(2) Uiso 0.50 1 d P A 1 H45A H -0.0313 -0.0004 0.2279 0.057 Uiso 0.50 1 calc PR A 1 H45B H -0.0600 0.0767 0.2274 0.057 Uiso 0.50 1 calc PR A 1 C32B C 0.3531(8) 0.1203(5) 0.0662(5) 0.042(2) Uiso 0.50 1 d P A 2 C33B C 0.2913(8) 0.1772(5) 0.0631(5) 0.051(2) Uiso 0.50 1 d P A 2 H33B H 0.3148 0.2075 0.1013 0.061 Uiso 0.50 1 calc PR A 2 C34B C 0.1898(10) 0.1954(6) 0.0042(7) 0.066(3) Uiso 0.50 1 d P A 2 H34B H 0.1460 0.2355 0.0028 0.079 Uiso 0.50 1 calc PR A 2 C35B C 0.1663(11) 0.1526(7) -0.0441(6) 0.060(3) Uiso 0.50 1 d P A 2 H35B H 0.1009 0.1621 -0.0833 0.072 Uiso 0.50 1 calc PR A 2 C36B C 0.2274(13) 0.0908(9) -0.0468(8) 0.096(4) Uiso 0.50 1 d P A 2 H36B H 0.2038 0.0612 -0.0857 0.115 Uiso 0.50 1 calc PR A 2 C37B C 0.3219(9) 0.0770(6) 0.0099(5) 0.060(2) Uiso 0.50 1 d P A 2 H37B H 0.3662 0.0371 0.0103 0.072 Uiso 0.50 1 calc PR A 2 O1B O 0.3921(5) 0.1448(3) 0.3818(3) 0.0358(16) Uiso 0.50 1 d P A 2 C38B C 0.5098(9) 0.1353(5) 0.3974(6) 0.045(3) Uiso 0.50 1 d P A 2 H38C H 0.5498 0.1575 0.3625 0.054 Uiso 0.50 1 calc PR A 2 H38D H 0.5296 0.0879 0.3986 0.054 Uiso 0.50 1 calc PR A 2 C39B C 0.5481(11) 0.1656(7) 0.4703(7) 0.082(3) Uiso 0.50 1 d P A 2 H39C H 0.5931 0.2070 0.4671 0.098 Uiso 0.50 1 calc PR A 2 H39D H 0.6029 0.1352 0.5026 0.098 Uiso 0.50 1 calc PR A 2 C40B C 0.4352(10) 0.1796(6) 0.4998(6) 0.069(3) Uiso 0.50 1 d P A 2 H40C H 0.4109 0.1415 0.5259 0.083 Uiso 0.50 1 calc PR A 2 H40D H 0.4445 0.2192 0.5304 0.083 Uiso 0.50 1 calc PR A 2 C41B C 0.3580(9) 0.1895(5) 0.4352(6) 0.059(2) Uiso 0.50 1 d P A 2 H41C H 0.3634 0.2357 0.4200 0.071 Uiso 0.50 1 calc PR A 2 H41D H 0.2728 0.1807 0.4391 0.071 Uiso 0.50 1 calc PR A 2 O2B O 0.0695(5) 0.0775(3) 0.1830(3) 0.0380(15) Uiso 0.50 1 d P A 2 C43B C -0.0640(11) 0.0800(6) 0.0813(7) 0.082(3) Uiso 0.50 1 d P A 2 H43C H -0.0674 0.1253 0.0620 0.098 Uiso 0.50 1 calc PR A 2 H43D H -0.1024 0.0502 0.0419 0.098 Uiso 0.50 1 calc PR A 2 C44B C -0.1264(10) 0.0771(6) 0.1348(6) 0.069(3) Uiso 0.50 1 d P A 2 H44C H -0.1746 0.1178 0.1350 0.083 Uiso 0.50 1 calc PR A 2 H44D H -0.1838 0.0395 0.1266 0.083 Uiso 0.50 1 calc PR A 2 C45B C -0.0544(8) 0.0705(5) 0.1934(5) 0.050(2) Uiso 0.50 1 d P A 2 H45C H -0.0651 0.0267 0.2136 0.060 Uiso 0.50 1 calc PR A 2 H45D H -0.0710 0.1044 0.2272 0.060 Uiso 0.50 1 calc PR A 2 C42 C 0.0622(4) 0.0610(3) 0.1076(2) 0.0585(11) Uani 1 1 d . . . H42A H 0.0530 0.1078 0.0933 0.070 Uiso 1 1 calc R A 1 H42B H 0.1317 0.0419 0.0902 0.070 Uiso 1 1 calc R A 1 N1 N 0.1302(2) 0.06867(13) 0.36349(16) 0.0331(6) Uani 1 1 d . . . N2 N 0.1015(3) 0.18843(16) 0.2992(2) 0.0517(9) Uani 1 1 d . . . N3 N 0.3962(2) 0.08188(13) 0.20913(16) 0.0332(6) Uani 1 1 d . . . P1 P 0.40823(8) 0.00712(4) 0.24564(5) 0.0299(2) Uani 1 1 d . A . P2 P 0.47007(8) 0.09832(4) 0.14302(5) 0.0359(2) Uani 1 1 d . A . Ca Ca 0.24026(6) 0.10569(3) 0.27542(4) 0.03329(18) Uani 1 1 d . A . 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 0.0280(15) 0.0318(17) 0.0348(18) 0.0017(14) 0.0071(14) -0.0021(13) C2 0.045(2) 0.0372(19) 0.0365(19) 0.0038(15) 0.0099(16) 0.0048(16) C3 0.061(3) 0.047(2) 0.043(2) 0.0034(18) 0.027(2) 0.0024(19) C4 0.057(3) 0.063(3) 0.060(3) 0.007(2) 0.037(2) 0.014(2) C5 0.040(2) 0.058(2) 0.072(3) 0.007(2) 0.026(2) 0.0184(19) C6 0.041(2) 0.053(2) 0.053(2) 0.016(2) 0.0157(18) 0.0147(18) C7 0.0350(18) 0.0372(18) 0.042(2) 0.0080(15) 0.0117(16) 0.0054(14) C8 0.051(2) 0.0331(18) 0.052(2) 0.0110(17) 0.0254(18) 0.0071(16) C9 0.063(3) 0.058(3) 0.075(3) 0.028(2) 0.014(2) 0.021(2) C10 0.083(3) 0.0297(19) 0.081(3) 0.000(2) 0.053(3) -0.001(2) C14 0.0424(19) 0.0313(17) 0.0347(19) 0.0002(14) 0.0092(15) -0.0039(14) C15 0.055(2) 0.044(2) 0.051(2) -0.0120(18) 0.028(2) -0.0139(18) C16 0.081(3) 0.050(2) 0.054(3) -0.014(2) 0.035(2) -0.013(2) C17 0.084(3) 0.054(3) 0.038(2) -0.0107(19) 0.010(2) -0.020(2) C18 0.054(2) 0.054(2) 0.049(2) -0.006(2) 0.004(2) -0.013(2) C19 0.042(2) 0.0396(19) 0.044(2) -0.0018(16) 0.0062(17) -0.0052(16) C20 0.0350(17) 0.0317(16) 0.0312(17) -0.0007(14) 0.0114(14) 0.0017(14) C21 0.0350(18) 0.045(2) 0.039(2) -0.0005(16) 0.0110(16) -0.0045(16) C22 0.0337(19) 0.071(3) 0.046(2) 0.004(2) 0.0104(17) -0.0106(18) C23 0.039(2) 0.081(3) 0.047(2) 0.008(2) 0.0079(18) 0.008(2) C24 0.062(3) 0.051(2) 0.062(3) 0.009(2) 0.005(2) 0.017(2) C25 0.045(2) 0.0379(19) 0.060(3) 0.0018(18) 0.0071(19) -0.0019(17) C26 0.0288(16) 0.0338(17) 0.0360(18) 0.0067(14) 0.0081(14) 0.0032(13) C27 0.0420(19) 0.0341(18) 0.045(2) 0.0044(16) 0.0163(16) 0.0003(15) C28 0.054(2) 0.0299(18) 0.052(2) -0.0012(17) 0.0096(19) 0.0050(17) C29 0.046(2) 0.0334(18) 0.053(2) 0.0104(17) -0.0029(18) -0.0099(16) C30 0.039(2) 0.051(2) 0.047(2) 0.0145(19) 0.0079(17) -0.0083(17) C31 0.0385(19) 0.048(2) 0.0348(19) 0.0021(16) 0.0113(15) -0.0032(16) C42 0.059(3) 0.078(3) 0.037(2) 0.006(2) 0.008(2) 0.000(2) N1 0.0300(14) 0.0325(14) 0.0379(16) 0.0040(12) 0.0098(12) 0.0010(12) N2 0.0528(19) 0.0465(18) 0.065(2) 0.0248(17) 0.0338(18) 0.0207(16) N3 0.0338(14) 0.0303(14) 0.0373(16) 0.0015(12) 0.0118(12) -0.0012(11) P1 0.0300(4) 0.0281(4) 0.0335(5) -0.0009(3) 0.0115(3) -0.0023(3) P2 0.0399(5) 0.0358(5) 0.0351(5) -0.0011(4) 0.0148(4) -0.0065(4) Ca 0.0295(3) 0.0345(4) 0.0384(4) 0.0035(3) 0.0131(3) 0.0021(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 N1 1.316(4) . ? C1 C2 1.430(5) . ? C1 C7 1.499(5) . ? C1 Ca 3.209(3) . ? C2 C3 1.369(5) . ? C3 C4 1.383(6) . ? C4 C5 1.383(6) . ? C5 C6 1.371(6) . ? C6 C7 1.427(5) . ? C7 N2 1.312(5) . ? C7 Ca 3.221(4) . ? C8 N1 1.473(4) . ? C8 C10 1.522(6) . ? C8 C9 1.528(6) . ? C11A N2 1.486(8) . ? C11A C13A 1.500(11) . ? C11A C12A 1.578(11) . ? C12B C11B 1.528(13) . ? C13B C11B 1.448(13) . ? C11B N2 1.547(9) . ? C14 C15 1.388(5) . ? C14 C19 1.391(5) . ? C14 P1 1.846(4) . ? C15 C16 1.392(6) . ? C16 C17 1.382(6) . ? C17 C18 1.372(7) . ? C18 C19 1.393(6) . ? C20 C21 1.384(5) . ? C20 C25 1.388(5) . ? C20 P1 1.833(3) . ? C21 C22 1.382(5) . ? C22 C23 1.379(6) . ? C23 C24 1.375(7) . ? C24 C25 1.386(6) . ? C26 C27 1.387(5) . ? C26 C31 1.389(5) . ? C26 P2 1.840(3) . ? C27 C28 1.390(5) . ? C28 C29 1.370(6) . ? C29 C30 1.366(6) . ? C30 C31 1.380(5) . ? C32A C33A 1.384(13) . ? C32A C37A 1.391(11) . ? C32A P2 1.927(8) . ? C33A C34A 1.381(11) . ? C34A C35A 1.397(13) . ? C35A C36A 1.453(14) . ? C36A C37A 1.401(13) . ? O1A C41A 1.412(11) . ? O1A C38A 1.663(12) . ? O1A Ca 2.350(6) . ? C38A C39A 1.472(14) . ? C39A C40A 1.660(17) . ? C40A C41A 1.448(17) . ? O2A C45A 1.414(10) . ? O2A C42 1.436(7) . ? O2A Ca 2.475(5) . ? C43A C42 1.421(11) . ? C43A C44A 1.57(2) . ? C44A C45A 1.333(18) . ? C32B C33B 1.343(14) . ? C32B C37B 1.378(14) . ? C32B P2 1.804(9) . ? C33B C34B 1.466(15) . ? C34B C35B 1.257(17) . ? C35B C36B 1.436(18) . ? C36B C37B 1.374(17) . ? O1B C38B 1.303(11) . ? O1B C41B 1.477(11) . ? O1B Ca 2.488(6) . ? C38B C39B 1.500(16) . ? C39B C40B 1.519(16) . ? C40B C41B 1.364(15) . ? O2B C45B 1.452(10) . ? O2B C42 1.468(7) . ? O2B Ca 2.381(6) . ? C43B C44B 1.360(15) . ? C43B C42 1.449(12) . ? C44B C45B 1.241(13) . ? N1 Ca 2.413(3) . ? N2 Ca 2.400(3) . ? N3 P1 1.667(3) . ? N3 P2 1.688(3) . ? N3 Ca 2.418(3) . ? P1 Ca 2.8896(11) . ? 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 C1 C2 123.7(3) . . ? N1 C1 C7 116.0(3) . . ? C2 C1 C7 120.0(3) . . ? N1 C1 Ca 42.70(16) . . ? C2 C1 Ca 153.2(2) . . ? C7 C1 Ca 76.94(19) . . ? C3 C2 C1 132.5(4) . . ? C2 C3 C4 129.6(4) . . ? C5 C4 C3 124.9(4) . . ? C6 C5 C4 129.5(4) . . ? C5 C6 C7 132.5(4) . . ? N2 C7 C6 124.3(3) . . ? N2 C7 C1 115.7(3) . . ? C6 C7 C1 119.6(3) . . ? N2 C7 Ca 41.47(17) . . ? C6 C7 Ca 156.5(3) . . ? C1 C7 Ca 76.10(18) . . ? N1 C8 C10 108.8(3) . . ? N1 C8 C9 112.1(3) . . ? C10 C8 C9 110.6(4) . . ? N2 C11A C13A 114.8(6) . . ? N2 C11A C12A 102.5(6) . . ? C13A C11A C12A 110.6(7) . . ? C13B C11B C12B 112.7(8) . . ? C13B C11B N2 105.9(8) . . ? C12B C11B N2 109.3(7) . . ? C15 C14 C19 118.8(3) . . ? C15 C14 P1 124.5(3) . . ? C19 C14 P1 116.6(3) . . ? C14 C15 C16 120.3(4) . . ? C17 C16 C15 120.3(4) . . ? C18 C17 C16 119.7(4) . . ? C17 C18 C19 120.4(4) . . ? C14 C19 C18 120.4(4) . . ? C21 C20 C25 117.8(3) . . ? C21 C20 P1 122.9(3) . . ? C25 C20 P1 118.9(3) . . ? C22 C21 C20 121.3(4) . . ? C23 C22 C21 120.1(4) . . ? C24 C23 C22 119.6(4) . . ? C23 C24 C25 120.0(4) . . ? C24 C25 C20 121.2(4) . . ? C27 C26 C31 117.9(3) . . ? C27 C26 P2 124.3(3) . . ? C31 C26 P2 117.8(3) . . ? C26 C27 C28 120.7(3) . . ? C29 C28 C27 120.1(4) . . ? C30 C29 C28 120.0(3) . . ? C29 C30 C31 120.2(4) . . ? C30 C31 C26 121.1(4) . . ? C33A C32A C37A 118.6(8) . . ? C33A C32A P2 125.1(6) . . ? C37A C32A P2 116.3(7) . . ? C34A C33A C32A 120.4(8) . . ? C33A C34A C35A 120.1(8) . . ? C34A C35A C36A 122.5(9) . . ? C37A C36A C35A 112.9(8) . . ? C32A C37A C36A 125.5(9) . . ? C41A O1A C38A 106.2(6) . . ? C41A O1A Ca 124.6(5) . . ? C38A O1A Ca 123.0(5) . . ? C39A C38A O1A 108.5(7) . . ? C38A C39A C40A 97.5(9) . . ? C41A C40A C39A 110.8(10) . . ? O1A C41A C40A 109.0(9) . . ? C45A O2A C42 107.7(5) . . ? C45A O2A Ca 120.2(5) . . ? C42 O2A Ca 126.2(4) . . ? C42 C43A C44A 105.6(9) . . ? C45A C44A C43A 101.2(12) . . ? C44A C45A O2A 113.1(10) . . ? C33B C32B C37B 118.3(9) . . ? C33B C32B P2 121.8(8) . . ? C37B C32B P2 119.8(8) . . ? C32B C33B C34B 124.0(10) . . ? C35B C34B C33B 113.4(12) . . ? C34B C35B C36B 127.3(13) . . ? C37B C36B C35B 116.3(13) . . ? C36B C37B C32B 120.7(12) . . ? C38B O1B C41B 109.4(7) . . ? C38B O1B Ca 128.5(6) . . ? C41B O1B Ca 122.0(5) . . ? O1B C38B C39B 103.1(8) . . ? C38B C39B C40B 109.1(10) . . ? C41B C40B C39B 96.2(10) . . ? C40B C41B O1B 109.2(9) . . ? C45B O2B C42 105.0(5) . . ? C45B O2B Ca 124.3(5) . . ? C42 O2B Ca 130.7(4) . . ? C44B C43B C42 110.4(10) . . ? C45B C44B C43B 110.2(10) . . ? C44B C45B O2B 108.8(9) . . ? C43A C42 O2A 102.6(6) . . ? C43A C42 C43B 46.3(6) . . ? O2A C42 C43B 106.4(6) . . ? C43A C42 O2B 109.1(6) . . ? O2A C42 O2B 19.6(3) . . ? C43B C42 O2B 97.2(6) . . ? C1 N1 C8 117.8(3) . . ? C1 N1 Ca 115.6(2) . . ? C8 N1 Ca 124.1(2) . . ? C7 N2 C11A 118.3(4) . . ? C7 N2 C11B 117.7(4) . . ? C11A N2 C11B 28.1(3) . . ? C7 N2 Ca 117.3(2) . . ? C11A N2 Ca 124.4(3) . . ? C11B N2 Ca 117.6(4) . . ? P1 N3 P2 119.10(17) . . ? P1 N3 Ca 88.02(12) . . ? P2 N3 Ca 151.60(16) . . ? N3 P1 C20 110.76(15) . . ? N3 P1 C14 108.85(15) . . ? C20 P1 C14 100.88(16) . . ? N3 P1 Ca 56.77(10) . . ? C20 P1 Ca 132.89(11) . . ? C14 P1 Ca 126.21(12) . . ? N3 P2 C32B 105.8(3) . . ? N3 P2 C26 104.00(15) . . ? C32B P2 C26 102.8(3) . . ? N3 P2 C32A 99.1(3) . . ? C32B P2 C32A 14.3(3) . . ? C26 P2 C32A 92.6(3) . . ? O1A Ca O2B 166.4(2) . . ? O1A Ca N2 85.76(18) . . ? O2B Ca N2 81.90(18) . . ? O1A Ca N1 91.14(18) . . ? O2B Ca N1 89.64(15) . . ? N2 Ca N1 68.72(10) . . ? O1A Ca N3 89.88(17) . . ? O2B Ca N3 96.81(16) . . ? N2 Ca N3 144.13(10) . . ? N1 Ca N3 147.06(10) . . ? O1A Ca O2A 177.3(2) . . ? O2B Ca O2A 11.48(17) . . ? N2 Ca O2A 91.62(17) . . ? N1 Ca O2A 87.48(15) . . ? N3 Ca O2A 92.52(15) . . ? O1A Ca O1B 9.6(2) . . ? O2B Ca O1B 170.0(2) . . ? N2 Ca O1B 88.74(17) . . ? N1 Ca O1B 83.73(16) . . ? N3 Ca O1B 92.80(16) . . ? O2A Ca O1B 170.4(2) . . ? O1A Ca P1 94.18(16) . . ? O2B Ca P1 98.09(15) . . ? N2 Ca P1 179.34(9) . . ? N1 Ca P1 111.95(7) . . ? N3 Ca P1 35.21(7) . . ? O2A Ca P1 88.45(14) . . ? O1B Ca P1 91.31(14) . . ? O1A Ca C1 84.84(17) . . ? O2B Ca C1 90.96(15) . . ? N2 Ca C1 47.60(10) . . ? N1 Ca C1 21.71(9) . . ? N3 Ca C1 166.79(9) . . ? O2A Ca C1 93.06(14) . . ? O1B Ca C1 80.13(15) . . ? P1 Ca C1 133.06(6) . . ? O1A Ca C7 88.72(17) . . ? O2B Ca C7 81.82(16) . . ? N2 Ca C7 21.22(10) . . ? N1 Ca C7 47.58(9) . . ? N3 Ca C7 165.33(9) . . ? O2A Ca C7 88.67(15) . . ? O1B Ca C7 88.21(15) . . ? P1 Ca C7 159.45(7) . . ? C1 Ca C7 26.96(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 C1 C2 C3 -160.6(4) . . . . ? C7 C1 C2 C3 24.5(6) . . . . ? Ca C1 C2 C3 149.0(4) . . . . ? C1 C2 C3 C4 4.5(8) . . . . ? C2 C3 C4 C5 -6.9(8) . . . . ? C3 C4 C5 C6 -9.7(8) . . . . ? C4 C5 C6 C7 3.3(9) . . . . ? C5 C6 C7 N2 -159.5(5) . . . . ? C5 C6 C7 C1 27.3(7) . . . . ? C5 C6 C7 Ca 155.3(5) . . . . ? N1 C1 C7 N2 -30.3(5) . . . . ? C2 C1 C7 N2 145.0(4) . . . . ? Ca C1 C7 N2 -12.6(3) . . . . ? N1 C1 C7 C6 143.5(4) . . . . ? C2 C1 C7 C6 -41.3(5) . . . . ? Ca C1 C7 C6 161.1(4) . . . . ? N1 C1 C7 Ca -17.6(2) . . . . ? C2 C1 C7 Ca 157.6(3) . . . . ? C19 C14 C15 C16 -0.1(6) . . . . ? P1 C14 C15 C16 -176.6(3) . . . . ? C14 C15 C16 C17 1.0(7) . . . . ? C15 C16 C17 C18 -1.4(7) . . . . ? C16 C17 C18 C19 0.8(7) . . . . ? C15 C14 C19 C18 -0.5(6) . . . . ? P1 C14 C19 C18 176.3(3) . . . . ? C17 C18 C19 C14 0.2(6) . . . . ? C25 C20 C21 C22 0.6(6) . . . . ? P1 C20 C21 C22 173.3(3) . . . . ? C20 C21 C22 C23 0.3(6) . . . . ? C21 C22 C23 C24 -1.1(7) . . . . ? C22 C23 C24 C25 1.0(7) . . . . ? C23 C24 C25 C20 0.0(7) . . . . ? C21 C20 C25 C24 -0.8(6) . . . . ? P1 C20 C25 C24 -173.8(3) . . . . ? C31 C26 C27 C28 1.7(5) . . . . ? P2 C26 C27 C28 179.4(3) . . . . ? C26 C27 C28 C29 -1.0(6) . . . . ? C27 C28 C29 C30 0.7(6) . . . . ? C28 C29 C30 C31 -1.0(6) . . . . ? C29 C30 C31 C26 1.7(6) . . . . ? C27 C26 C31 C30 -2.0(5) . . . . ? P2 C26 C31 C30 -179.9(3) . . . . ? C37A C32A C33A C34A 1.3(11) . . . . ? P2 C32A C33A C34A -178.6(6) . . . . ? C32A C33A C34A C35A -0.4(11) . . . . ? C33A C34A C35A C36A 0.8(12) . . . . ? C34A C35A C36A C37A -1.9(12) . . . . ? C33A C32A C37A C36A -2.7(12) . . . . ? P2 C32A C37A C36A 177.2(6) . . . . ? C35A C36A C37A C32A 2.9(12) . . . . ? C41A O1A C38A C39A 18.1(10) . . . . ? Ca O1A C38A C39A -135.2(7) . . . . ? O1A C38A C39A C40A -25.5(10) . . . . ? C38A C39A C40A C41A 28.0(13) . . . . ? C38A O1A C41A C40A 1.2(12) . . . . ? Ca O1A C41A C40A 154.0(8) . . . . ? C39A C40A C41A O1A -18.2(14) . . . . ? C42 C43A C44A C45A -28.0(15) . . . . ? C43A C44A C45A O2A 13.4(16) . . . . ? C42 O2A C45A C44A 5.4(13) . . . . ? Ca O2A C45A C44A 159.8(10) . . . . ? C37B C32B C33B C34B 1.9(14) . . . . ? P2 C32B C33B C34B -175.5(7) . . . . ? C32B C33B C34B C35B -0.8(15) . . . . ? C33B C34B C35B C36B -0.3(17) . . . . ? C34B C35B C36B C37B 0.1(19) . . . . ? C35B C36B C37B C32B 1.1(17) . . . . ? C33B C32B C37B C36B -2.0(15) . . . . ? P2 C32B C37B C36B 175.5(9) . . . . ? C41B O1B C38B C39B 9.9(12) . . . . ? Ca O1B C38B C39B -175.3(7) . . . . ? O1B C38B C39B C40B 12.2(14) . . . . ? C38B C39B C40B C41B -29.6(13) . . . . ? C39B C40B C41B O1B 35.2(11) . . . . ? C38B O1B C41B C40B -32.3(12) . . . . ? Ca O1B C41B C40B 152.5(7) . . . . ? C42 C43B C44B C45B 11.9(15) . . . . ? C43B C44B C45B O2B 7.7(14) . . . . ? C42 O2B C45B C44B -23.8(11) . . . . ? Ca O2B C45B C44B 158.5(8) . . . . ? C44A C43A C42 O2A 30.9(10) . . . . ? C44A C43A C42 C43B -69.9(11) . . . . ? C44A C43A C42 O2B 11.6(11) . . . . ? C45A O2A C42 C43A -23.4(8) . . . . ? Ca O2A C42 C43A -175.9(5) . . . . ? C45A O2A C42 C43B 24.4(9) . . . . ? Ca O2A C42 C43B -128.2(6) . . . . ? C45A O2A C42 O2B 88.4(12) . . . . ? Ca O2A C42 O2B -64.1(10) . . . . ? C44B C43B C42 C43A 84.9(12) . . . . ? C44B C43B C42 O2A -7.0(12) . . . . ? C44B C43B C42 O2B -24.6(11) . . . . ? C45B O2B C42 C43A -18.7(8) . . . . ? Ca O2B C42 C43A 158.8(6) . . . . ? C45B O2B C42 O2A -92.2(12) . . . . ? Ca O2B C42 O2A 85.3(11) . . . . ? C45B O2B C42 C43B 27.4(8) . . . . ? Ca O2B C42 C43B -155.1(7) . . . . ? C2 C1 N1 C8 13.7(5) . . . . ? C7 C1 N1 C8 -171.3(3) . . . . ? Ca C1 N1 C8 162.9(4) . . . . ? C2 C1 N1 Ca -149.2(3) . . . . ? C7 C1 N1 Ca 25.8(4) . . . . ? C10 C8 N1 C1 142.5(3) . . . . ? C9 C8 N1 C1 -94.9(4) . . . . ? C10 C8 N1 Ca -56.1(4) . . . . ? C9 C8 N1 Ca 66.4(4) . . . . ? C6 C7 N2 C11A 26.7(7) . . . . ? C1 C7 N2 C11A -159.8(5) . . . . ? Ca C7 N2 C11A -178.6(6) . . . . ? C6 C7 N2 C11B -5.2(7) . . . . ? C1 C7 N2 C11B 168.2(5) . . . . ? Ca C7 N2 C11B 149.5(6) . . . . ? C6 C7 N2 Ca -154.7(3) . . . . ? C1 C7 N2 Ca 18.7(4) . . . . ? C13A C11A N2 C7 135.9(6) . . . . ? C12A C11A N2 C7 -104.2(6) . . . . ? C13A C11A N2 C11B -127.5(13) . . . . ? C12A C11A N2 C11B -7.6(8) . . . . ? C13A C11A N2 Ca -42.6(8) . . . . ? C12A C11A N2 Ca 77.4(6) . . . . ? C13B C11B N2 C7 77.1(8) . . . . ? C12B C11B N2 C7 -161.2(6) . . . . ? C13B C11B N2 C11A -21.6(8) . . . . ? C12B C11B N2 C11A 100.1(12) . . . . ? C13B C11B N2 Ca -133.5(6) . . . . ? C12B C11B N2 Ca -11.8(8) . . . . ? P2 N3 P1 C20 60.4(2) . . . . ? Ca N3 P1 C20 -128.45(13) . . . . ? P2 N3 P1 C14 -49.7(2) . . . . ? Ca N3 P1 C14 121.50(14) . . . . ? P2 N3 P1 Ca -171.2(2) . . . . ? C21 C20 P1 N3 10.6(4) . . . . ? C25 C20 P1 N3 -176.8(3) . . . . ? C21 C20 P1 C14 125.7(3) . . . . ? C25 C20 P1 C14 -61.7(3) . . . . ? C21 C20 P1 Ca -52.8(4) . . . . ? C25 C20 P1 Ca 119.8(3) . . . . ? C15 C14 P1 N3 81.4(4) . . . . ? C19 C14 P1 N3 -95.2(3) . . . . ? C15 C14 P1 C20 -35.2(4) . . . . ? C19 C14 P1 C20 148.2(3) . . . . ? C15 C14 P1 Ca 143.5(3) . . . . ? C19 C14 P1 Ca -33.1(3) . . . . ? P1 N3 P2 C32B 119.6(4) . . . . ? Ca N3 P2 C32B -41.6(5) . . . . ? P1 N3 P2 C26 -132.47(18) . . . . ? Ca N3 P2 C26 66.4(3) . . . . ? P1 N3 P2 C32A 132.6(3) . . . . ? Ca N3 P2 C32A -28.6(4) . . . . ? C33B C32B P2 N3 70.6(8) . . . . ? C37B C32B P2 N3 -106.8(8) . . . . ? C33B C32B P2 C26 -38.2(8) . . . . ? C37B C32B P2 C26 144.4(7) . . . . ? C33B C32B P2 C32A 7.0(13) . . . . ? C37B C32B P2 C32A -170(2) . . . . ? C27 C26 P2 N3 -3.5(3) . . . . ? C31 C26 P2 N3 174.2(3) . . . . ? C27 C26 P2 C32B 106.7(4) . . . . ? C31 C26 P2 C32B -75.6(4) . . . . ? C27 C26 P2 C32A 96.5(4) . . . . ? C31 C26 P2 C32A -85.7(4) . . . . ? C33A C32A P2 N3 62.4(6) . . . . ? C37A C32A P2 N3 -117.4(6) . . . . ? C33A C32A P2 C32B -178(2) . . . . ? C37A C32A P2 C32B 1.8(14) . . . . ? C33A C32A P2 C26 -42.2(6) . . . . ? C37A C32A P2 C26 138.0(6) . . . . ? C41A O1A Ca O2B 31.0(14) . . . . ? C38A O1A Ca O2B 179.4(8) . . . . ? C41A O1A Ca N2 6.4(7) . . . . ? C38A O1A Ca N2 154.8(6) . . . . ? C41A O1A Ca N1 -62.2(7) . . . . ? C38A O1A Ca N1 86.2(6) . . . . ? C41A O1A Ca N3 150.7(7) . . . . ? C38A O1A Ca N3 -60.8(6) . . . . ? C41A O1A Ca O2A -3(5) . . . . ? C38A O1A Ca O2A 145(5) . . . . ? C41A O1A Ca O1B -101.5(18) . . . . ? C38A O1A Ca O1B 47.0(15) . . . . ? C41A O1A Ca P1 -174.3(7) . . . . ? C38A O1A Ca P1 -25.9(6) . . . . ? C41A O1A Ca C1 -41.4(7) . . . . ? C38A O1A Ca C1 107.0(6) . . . . ? C41A O1A Ca C7 -14.7(7) . . . . ? C38A O1A Ca C7 133.8(6) . . . . ? C45B O2B Ca O1A -72.0(12) . . . . ? C42 O2B Ca O1A 110.9(10) . . . . ? C45B O2B Ca N2 -47.2(6) . . . . ? C42 O2B Ca N2 135.7(6) . . . . ? C45B O2B Ca N1 21.3(7) . . . . ? C42 O2B Ca N1 -155.7(5) . . . . ? C45B O2B Ca N3 169.0(6) . . . . ? C42 O2B Ca N3 -8.1(6) . . . . ? C45B O2B Ca O2A 100.4(14) . . . . ? C42 O2B Ca O2A -76.7(12) . . . . ? C45B O2B Ca O1B -26.9(16) . . . . ? C42 O2B Ca O1B 156.1(10) . . . . ? C45B O2B Ca P1 133.5(6) . . . . ? C42 O2B Ca P1 -43.6(5) . . . . ? C45B O2B Ca C1 -0.3(7) . . . . ? C42 O2B Ca C1 -177.4(5) . . . . ? C45B O2B Ca C7 -25.8(6) . . . . ? C42 O2B Ca C7 157.2(6) . . . . ? C7 N2 Ca O1A -97.4(4) . . . . ? C11A N2 Ca O1A 81.1(5) . . . . ? C11B N2 Ca O1A 113.1(5) . . . . ? C7 N2 Ca O2B 88.3(3) . . . . ? C11A N2 Ca O2B -93.3(5) . . . . ? C11B N2 Ca O2B -61.2(5) . . . . ? C7 N2 Ca N1 -4.5(3) . . . . ? C11A N2 Ca N1 173.9(5) . . . . ? C11B N2 Ca N1 -154.0(5) . . . . ? C7 N2 Ca N3 178.7(2) . . . . ? C11A N2 Ca N3 -2.9(6) . . . . ? C11B N2 Ca N3 29.2(5) . . . . ? C7 N2 Ca O2A 82.1(3) . . . . ? C11A N2 Ca O2A -99.4(5) . . . . ? C11B N2 Ca O2A -67.4(5) . . . . ? C7 N2 Ca O1B -88.3(3) . . . . ? C11A N2 Ca O1B 90.2(5) . . . . ? C11B N2 Ca O1B 122.2(5) . . . . ? C7 N2 Ca P1 178(100) . . . . ? C11A N2 Ca P1 -4(10) . . . . ? C11B N2 Ca P1 28(10) . . . . ? C7 N2 Ca C1 -10.5(3) . . . . ? C11A N2 Ca C1 167.9(5) . . . . ? C11B N2 Ca C1 -160.0(5) . . . . ? C11A N2 Ca C7 178.5(7) . . . . ? C11B N2 Ca C7 -149.5(6) . . . . ? C1 N1 Ca O1A 73.0(3) . . . . ? C8 N1 Ca O1A -88.8(3) . . . . ? C1 N1 Ca O2B -93.5(3) . . . . ? C8 N1 Ca O2B 104.8(3) . . . . ? C1 N1 Ca N2 -12.1(2) . . . . ? C8 N1 Ca N2 -173.8(3) . . . . ? C1 N1 Ca N3 164.5(2) . . . . ? C8 N1 Ca N3 2.7(4) . . . . ? C1 N1 Ca O2A -104.8(3) . . . . ? C8 N1 Ca O2A 93.5(3) . . . . ? C1 N1 Ca O1B 79.0(3) . . . . ? C8 N1 Ca O1B -82.7(3) . . . . ? C1 N1 Ca P1 167.9(2) . . . . ? C8 N1 Ca P1 6.2(3) . . . . ? C8 N1 Ca C1 -161.7(4) . . . . ? C1 N1 Ca C7 -14.3(2) . . . . ? C8 N1 Ca C7 -176.0(3) . . . . ? P1 N3 Ca O1A 97.44(19) . . . . ? P2 N3 Ca O1A -99.0(4) . . . . ? P1 N3 Ca O2B -94.41(18) . . . . ? P2 N3 Ca O2B 69.2(4) . . . . ? P1 N3 Ca N2 -179.98(17) . . . . ? P2 N3 Ca N2 -16.4(4) . . . . ? P1 N3 Ca N1 5.5(2) . . . . ? P2 N3 Ca N1 169.1(3) . . . . ? P1 N3 Ca O2A -83.72(17) . . . . ? P2 N3 Ca O2A 79.9(4) . . . . ? P1 N3 Ca O1B 88.30(18) . . . . ? P2 N3 Ca O1B -108.1(4) . . . . ? P2 N3 Ca P1 163.6(4) . . . . ? P1 N3 Ca C1 31.2(5) . . . . ? P2 N3 Ca C1 -165.2(3) . . . . ? P1 N3 Ca C7 -178.1(3) . . . . ? P2 N3 Ca C7 -14.5(6) . . . . ? C45A O2A Ca O1A -38(5) . . . . ? C42 O2A Ca O1A 111(5) . . . . ? C45A O2A Ca O2B -80.3(13) . . . . ? C42 O2A Ca O2B 69.1(11) . . . . ? C45A O2A Ca N2 -48.2(6) . . . . ? C42 O2A Ca N2 101.2(5) . . . . ? C45A O2A Ca N1 20.4(6) . . . . ? C42 O2A Ca N1 169.8(5) . . . . ? C45A O2A Ca N3 167.4(6) . . . . ? C42 O2A Ca N3 -43.2(5) . . . . ? C45A O2A Ca O1B 43.8(15) . . . . ? C42 O2A Ca O1B -166.8(10) . . . . ? C45A O2A Ca P1 132.4(6) . . . . ? C42 O2A Ca P1 -78.1(5) . . . . ? C45A O2A Ca C1 -0.6(6) . . . . ? C42 O2A Ca C1 148.8(5) . . . . ? C45A O2A Ca C7 -27.2(6) . . . . ? C42 O2A Ca C7 122.2(5) . . . . ? C38B O1B Ca O1A -89.1(18) . . . . ? C41B O1B Ca O1A 85.2(17) . . . . ? C38B O1B Ca O2B 179(49) . . . . ? C41B O1B Ca O2B -6.7(16) . . . . ? C38B O1B Ca N2 -160.8(8) . . . . ? C41B O1B Ca N2 13.5(7) . . . . ? C38B O1B Ca N1 130.5(8) . . . . ? C41B O1B Ca N1 -55.3(6) . . . . ? C38B O1B Ca N3 -16.6(8) . . . . ? C41B O1B Ca N3 157.6(7) . . . . ? C38B O1B Ca O2A 107.0(14) . . . . ? C41B O1B Ca O2A -78.8(14) . . . . ? C38B O1B Ca P1 18.6(8) . . . . ? C41B O1B Ca P1 -167.2(6) . . . . ? C38B O1B Ca C1 152.1(9) . . . . ? C41B O1B Ca C1 -33.6(6) . . . . ? C38B O1B Ca C7 178.0(8) . . . . ? C41B O1B Ca C7 -7.8(7) . . . . ? N3 P1 Ca O1A -83.8(2) . . . . ? C20 P1 Ca O1A 4.4(2) . . . . ? C14 P1 Ca O1A -173.8(2) . . . . ? N3 P1 Ca O2B 90.35(19) . . . . ? C20 P1 Ca O2B 178.6(2) . . . . ? C14 P1 Ca O2B 0.4(2) . . . . ? N3 P1 Ca N2 1(10) . . . . ? C20 P1 Ca N2 89(10) . . . . ? C14 P1 Ca N2 -89(10) . . . . ? N3 P1 Ca N1 -176.76(14) . . . . ? C20 P1 Ca N1 -88.50(17) . . . . ? C14 P1 Ca N1 93.29(16) . . . . ? C20 P1 Ca N3 88.26(19) . . . . ? C14 P1 Ca N3 -89.95(19) . . . . ? N3 P1 Ca O2A 96.59(18) . . . . ? C20 P1 Ca O2A -175.2(2) . . . . ? C14 P1 Ca O2A 6.63(19) . . . . ? N3 P1 Ca O1B -93.00(19) . . . . ? C20 P1 Ca O1B -4.7(2) . . . . ? C14 P1 Ca O1B 177.0(2) . . . . ? N3 P1 Ca C1 -170.68(15) . . . . ? C20 P1 Ca C1 -82.42(17) . . . . ? C14 P1 Ca C1 99.37(16) . . . . ? N3 P1 Ca C7 178.6(2) . . . . ? C20 P1 Ca C7 -93.1(3) . . . . ? C14 P1 Ca C7 88.7(2) . . . . ? N1 C1 Ca O1A -106.3(3) . . . . ? C2 C1 Ca O1A -35.5(5) . . . . ? C7 C1 Ca O1A 97.4(2) . . . . ? N1 C1 Ca O2B 86.6(3) . . . . ? C2 C1 Ca O2B 157.4(5) . . . . ? C7 C1 Ca O2B -69.7(2) . . . . ? N1 C1 Ca N2 164.7(3) . . . . ? C2 C1 Ca N2 -124.5(5) . . . . ? C7 C1 Ca N2 8.4(2) . . . . ? C2 C1 Ca N1 70.8(5) . . . . ? C7 C1 Ca N1 -156.3(3) . . . . ? N1 C1 Ca N3 -39.5(5) . . . . ? C2 C1 Ca N3 31.3(8) . . . . ? C7 C1 Ca N3 164.2(4) . . . . ? N1 C1 Ca O2A 75.3(3) . . . . ? C2 C1 Ca O2A 146.1(5) . . . . ? C7 C1 Ca O2A -81.0(2) . . . . ? N1 C1 Ca O1B -97.9(3) . . . . ? C2 C1 Ca O1B -27.1(5) . . . . ? C7 C1 Ca O1B 105.8(2) . . . . ? N1 C1 Ca P1 -15.4(3) . . . . ? C2 C1 Ca P1 55.4(5) . . . . ? C7 C1 Ca P1 -171.74(16) . . . . ? N1 C1 Ca C7 156.3(3) . . . . ? C2 C1 Ca C7 -132.9(6) . . . . ? N2 C7 Ca O1A 81.6(4) . . . . ? C6 C7 Ca O1A 143.8(7) . . . . ? C1 C7 Ca O1A -81.1(2) . . . . ? N2 C7 Ca O2B -88.7(4) . . . . ? C6 C7 Ca O2B -26.4(7) . . . . ? C1 C7 Ca O2B 108.7(2) . . . . ? C6 C7 Ca N2 62.2(7) . . . . ? C1 C7 Ca N2 -162.7(4) . . . . ? N2 C7 Ca N1 174.3(4) . . . . ? C6 C7 Ca N1 -123.5(7) . . . . ? C1 C7 Ca N1 11.60(17) . . . . ? N2 C7 Ca N3 -3.1(6) . . . . ? C6 C7 Ca N3 59.2(8) . . . . ? C1 C7 Ca N3 -165.7(3) . . . . ? N2 C7 Ca O2A -97.9(3) . . . . ? C6 C7 Ca O2A -35.7(7) . . . . ? C1 C7 Ca O2A 99.4(2) . . . . ? N2 C7 Ca O1B 91.1(3) . . . . ? C6 C7 Ca O1B 153.4(7) . . . . ? C1 C7 Ca O1B -71.5(2) . . . . ? N2 C7 Ca P1 -179.9(3) . . . . ? C6 C7 Ca P1 -117.7(6) . . . . ? C1 C7 Ca P1 17.4(3) . . . . ? N2 C7 Ca C1 162.7(4) . . . . ? C6 C7 Ca C1 -135.1(7) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.377 _refine_diff_density_min -0.318 _refine_diff_density_rms 0.055 _publ_section_abstract ; ; _publ_section_experimental ; ; _publ_section_comment ; ; _publ_section_references ; ; _publ_section_figure_captions ; ; #==============================================================================