Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Peter Junk' _publ_contact_author_address ; School of Chemistry Monash University Box 23 Clayton Victoria 3800 AUSTRALIA ; _publ_contact_author_email PETER.JUNK@SCI.MONASH.EDU.AU _publ_section_title ; Synthesis and Structural Characterisation of Heavy Alkaline Earth N,N'-Bis(aryl)formamidinate Complexes ; loop_ _publ_author_name 'Peter Junk' 'Marcus L. Cole' 'Glen B. Deacon' 'Craig M. Forsyth' 'Kristina Konstas' # Attachment 'revised combined CIF.txt' data_COMPOUND_1 _database_code_depnum_ccdc_archive 'CCDC 298094' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point 439-443 _chemical_formula_moiety 'C38 H46 Ca N4 O2' _chemical_formula_sum 'C38 H46 Ca N4 O2' _chemical_formula_weight 630.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _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 11.2249(3) _cell_length_b 16.7282(9) _cell_length_c 19.6462(10) _cell_angle_alpha 90.00 _cell_angle_beta 105.930(3) _cell_angle_gamma 90.00 _cell_volume 3547.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'rectangular block' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.181 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1352 _exptl_absorpt_coefficient_mu 0.214 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9385 _exptl_absorpt_correction_T_max 0.9894 _exptl_absorpt_process_details 'performed as part of the DENZO-SMN package' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'psi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23008 _diffrn_reflns_av_R_equivalents 0.0665 _diffrn_reflns_av_sigmaI/netI 0.1092 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 27.88 _reflns_number_total 8358 _reflns_number_gt 4683 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction X-Seed _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed / POV-Ray' _computing_publication_material 'Microsoft Office 2000' _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^)+(0.1373P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8358 _refine_ls_number_parameters 411 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1229 _refine_ls_R_factor_gt 0.0510 _refine_ls_wR_factor_ref 0.1810 _refine_ls_wR_factor_gt 0.1357 _refine_ls_goodness_of_fit_ref 0.777 _refine_ls_restrained_S_all 0.777 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ca1 Ca 0.28026(4) 0.01301(3) 0.77356(2) 0.02077(15) Uani 1 1 d . . . O1 O 0.20721(15) 0.05329(10) 0.87038(8) 0.0281(4) Uani 1 1 d . . . O2 O 0.35667(15) -0.04064(11) 0.68216(9) 0.0299(4) Uani 1 1 d . . . N1 N 0.25600(16) 0.14304(12) 0.71807(10) 0.0228(5) Uani 1 1 d . . . N2 N 0.43788(16) 0.11759(12) 0.80313(9) 0.0218(5) Uani 1 1 d . . . N3 N 0.09817(16) -0.07132(12) 0.73704(10) 0.0226(5) Uani 1 1 d . . . N4 N 0.27408(16) -0.12470(12) 0.81098(10) 0.0214(4) Uani 1 1 d . . . C1 C 0.17839(19) 0.20060(15) 0.67591(12) 0.0206(5) Uani 1 1 d . . . C2 C 0.0968(2) 0.17607(16) 0.61056(12) 0.0239(5) Uani 1 1 d . . . C3 C 0.0210(2) 0.23347(17) 0.56922(13) 0.0277(6) Uani 1 1 d . . . H3 H -0.0336 0.2178 0.5251 0.033 Uiso 1 1 calc R . . C4 C 0.0219(2) 0.31249(17) 0.58974(13) 0.0300(6) Uani 1 1 d . . . H4 H -0.0304 0.3503 0.5597 0.036 Uiso 1 1 calc R . . C5 C 0.0993(2) 0.33629(17) 0.65426(13) 0.0305(6) Uani 1 1 d . . . H5 H 0.1004 0.3904 0.6691 0.037 Uiso 1 1 calc R . . C6 C 0.1757(2) 0.27986(16) 0.69723(13) 0.0257(6) Uani 1 1 d . . . H6 H 0.2272 0.2958 0.7421 0.031 Uiso 1 1 calc R . . C7 C 0.0940(2) 0.09092(17) 0.58617(13) 0.0344(7) Uani 1 1 d . . . H7A H 0.0333 0.0855 0.5399 0.052 Uiso 1 1 calc R . . H7B H 0.0706 0.0560 0.6204 0.052 Uiso 1 1 calc R . . H7C H 0.1762 0.0757 0.5823 0.052 Uiso 1 1 calc R . . C8 C 0.56293(19) 0.13904(14) 0.83314(12) 0.0200(5) Uani 1 1 d . . . C9 C 0.6102(2) 0.13775(16) 0.90740(12) 0.0233(5) Uani 1 1 d . . . C10 C 0.7340(2) 0.15891(16) 0.93692(13) 0.0272(6) Uani 1 1 d . . . H10 H 0.7663 0.1593 0.9870 0.033 Uiso 1 1 calc R . . C11 C 0.8109(2) 0.17933(15) 0.89553(13) 0.0252(6) Uani 1 1 d . . . H11 H 0.8951 0.1926 0.9170 0.030 Uiso 1 1 calc R . . C12 C 0.7644(2) 0.18031(15) 0.82269(13) 0.0247(6) Uani 1 1 d . . . H12 H 0.8166 0.1945 0.7938 0.030 Uiso 1 1 calc R . . C13 C 0.6409(2) 0.16041(15) 0.79177(12) 0.0230(5) Uani 1 1 d . . . H13 H 0.6093 0.1614 0.7417 0.028 Uiso 1 1 calc R . . C14 C 0.5287(2) 0.1173(2) 0.95381(13) 0.0412(8) Uani 1 1 d . . . H14A H 0.5787 0.1151 1.0033 0.062 Uiso 1 1 calc R . . H14B H 0.4899 0.0651 0.9399 0.062 Uiso 1 1 calc R . . H14C H 0.4644 0.1582 0.9486 0.062 Uiso 1 1 calc R . . C15 C 0.3695(2) 0.16525(14) 0.75447(12) 0.0205(5) Uani 1 1 d . . . H15 H 0.4013 0.2156 0.7453 0.025 Uiso 1 1 calc R . . C16 C -0.0159(2) -0.08383(15) 0.68614(12) 0.0212(5) Uani 1 1 d . . . C17 C -0.1097(2) -0.02605(16) 0.68055(13) 0.0261(6) Uani 1 1 d . . . C18 C -0.2229(2) -0.03804(18) 0.63054(14) 0.0361(7) Uani 1 1 d . . . H18 H -0.2875 -0.0004 0.6272 0.043 Uiso 1 1 calc R . . C19 C -0.2440(2) -0.10336(19) 0.58544(15) 0.0411(7) Uani 1 1 d . . . H19 H -0.3227 -0.1105 0.5522 0.049 Uiso 1 1 calc R . . C20 C -0.1504(2) -0.15811(17) 0.58898(14) 0.0362(7) Uani 1 1 d . . . H20 H -0.1631 -0.2020 0.5571 0.043 Uiso 1 1 calc R . . C21 C -0.0375(2) -0.14849(16) 0.63959(13) 0.0280(6) Uani 1 1 d . . . H21 H 0.0263 -0.1867 0.6425 0.034 Uiso 1 1 calc R . . C22 C -0.0884(2) 0.04592(18) 0.72775(15) 0.0379(7) Uani 1 1 d . . . H22A H -0.1650 0.0772 0.7187 0.057 Uiso 1 1 calc R . . H22B H -0.0228 0.0789 0.7181 0.057 Uiso 1 1 calc R . . H22C H -0.0635 0.0287 0.7773 0.057 Uiso 1 1 calc R . . C23 C 0.3349(2) -0.19066(15) 0.84916(12) 0.0218(5) Uani 1 1 d . . . C24 C 0.4657(2) -0.19232(16) 0.86662(12) 0.0268(6) Uani 1 1 d . . . C25 C 0.5278(2) -0.25848(19) 0.90323(13) 0.0353(7) Uani 1 1 d . . . H25 H 0.6155 -0.2609 0.9139 0.042 Uiso 1 1 calc R . . C26 C 0.4644(3) -0.32059(18) 0.92434(14) 0.0398(7) Uani 1 1 d . . . H26 H 0.5085 -0.3650 0.9491 0.048 Uiso 1 1 calc R . . C27 C 0.3382(3) -0.31763(17) 0.90929(13) 0.0372(7) Uani 1 1 d . . . H27 H 0.2946 -0.3598 0.9243 0.045 Uiso 1 1 calc R . . C28 C 0.2735(2) -0.25332(16) 0.87220(12) 0.0285(6) Uani 1 1 d . . . H28 H 0.1858 -0.2519 0.8623 0.034 Uiso 1 1 calc R . . C29 C 0.5361(2) -0.12418(19) 0.84610(15) 0.0381(7) Uani 1 1 d . . . H29A H 0.6245 -0.1374 0.8585 0.057 Uiso 1 1 calc R . . H29B H 0.5239 -0.0758 0.8714 0.057 Uiso 1 1 calc R . . H29C H 0.5058 -0.1150 0.7950 0.057 Uiso 1 1 calc R . . C30 C 0.1588(2) -0.13386(15) 0.77029(12) 0.0206(5) Uani 1 1 d . . . H30 H 0.1204 -0.1850 0.7652 0.025 Uiso 1 1 calc R . . C31 C 0.1688(3) -0.00102(19) 0.91686(16) 0.0465(8) Uani 1 1 d . . . H31A H 0.2310 -0.0440 0.9323 0.056 Uiso 1 1 calc R . . H31B H 0.0886 -0.0259 0.8921 0.056 Uiso 1 1 calc R . . C32 C 0.1564(5) 0.0445(2) 0.9781(2) 0.0913(15) Uani 1 1 d . . . H32A H 0.2083 0.0205 1.0224 0.110 Uiso 1 1 calc R . . H32B H 0.0691 0.0445 0.9798 0.110 Uiso 1 1 calc R . . C33 C 0.1988(3) 0.12845(18) 0.96953(15) 0.0395(7) Uani 1 1 d . . . H33A H 0.2859 0.1367 0.9972 0.047 Uiso 1 1 calc R . . H33B H 0.1457 0.1684 0.9843 0.047 Uiso 1 1 calc R . . C34 C 0.1850(2) 0.13342(16) 0.89045(14) 0.0313(6) Uani 1 1 d . . . H34A H 0.1006 0.1514 0.8646 0.038 Uiso 1 1 calc R . . H34B H 0.2462 0.1710 0.8805 0.038 Uiso 1 1 calc R . . C35 C 0.4315(2) 0.00295(17) 0.64551(14) 0.0333(6) Uani 1 1 d . . . H35A H 0.5188 0.0055 0.6746 0.040 Uiso 1 1 calc R . . H35B H 0.4000 0.0581 0.6349 0.040 Uiso 1 1 calc R . . C36 C 0.4216(2) -0.04297(18) 0.57790(14) 0.0353(7) Uani 1 1 d . . . H36A H 0.4961 -0.0353 0.5609 0.042 Uiso 1 1 calc R . . H36B H 0.3471 -0.0271 0.5401 0.042 Uiso 1 1 calc R . . C37 C 0.4117(3) -0.12856(18) 0.60184(15) 0.0409(7) Uani 1 1 d . . . H37A H 0.3739 -0.1639 0.5612 0.049 Uiso 1 1 calc R . . H37B H 0.4938 -0.1501 0.6277 0.049 Uiso 1 1 calc R . . C38 C 0.3285(3) -0.11922(17) 0.65012(15) 0.0382(7) Uani 1 1 d . . . H38A H 0.2403 -0.1226 0.6228 0.046 Uiso 1 1 calc R . . H38B H 0.3458 -0.1614 0.6869 0.046 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ca1 0.0223(3) 0.0190(3) 0.0208(3) 0.0010(2) 0.00554(19) -0.0014(2) O1 0.0390(10) 0.0225(10) 0.0268(9) -0.0030(8) 0.0157(7) -0.0045(8) O2 0.0413(10) 0.0233(10) 0.0305(10) -0.0037(8) 0.0191(8) -0.0073(8) N1 0.0218(10) 0.0231(12) 0.0196(10) 0.0037(9) -0.0007(8) -0.0010(9) N2 0.0214(10) 0.0235(12) 0.0178(10) 0.0026(9) 0.0010(8) -0.0028(8) N3 0.0188(10) 0.0194(11) 0.0276(11) 0.0022(9) 0.0027(8) 0.0006(8) N4 0.0202(10) 0.0218(12) 0.0224(10) 0.0039(9) 0.0060(8) 0.0030(8) C1 0.0186(11) 0.0235(14) 0.0198(12) 0.0026(10) 0.0055(9) -0.0017(10) C2 0.0241(12) 0.0285(15) 0.0199(12) 0.0020(11) 0.0076(9) -0.0010(11) C3 0.0218(12) 0.0381(17) 0.0213(13) 0.0058(12) 0.0027(10) 0.0005(11) C4 0.0241(13) 0.0357(17) 0.0300(14) 0.0094(12) 0.0073(11) 0.0113(11) C5 0.0306(13) 0.0255(15) 0.0373(15) 0.0018(12) 0.0123(11) 0.0064(11) C6 0.0230(12) 0.0297(16) 0.0235(13) 0.0000(11) 0.0047(10) 0.0021(11) C7 0.0391(15) 0.0312(17) 0.0265(14) 0.0003(12) -0.0017(11) -0.0012(12) C8 0.0222(12) 0.0154(13) 0.0206(12) 0.0002(10) 0.0026(9) -0.0012(9) C9 0.0230(12) 0.0258(15) 0.0201(12) -0.0001(11) 0.0044(9) 0.0001(10) C10 0.0275(13) 0.0292(15) 0.0217(13) 0.0004(11) 0.0013(10) -0.0010(11) C11 0.0212(12) 0.0237(14) 0.0285(14) -0.0009(11) 0.0028(10) -0.0022(10) C12 0.0259(12) 0.0214(14) 0.0288(13) -0.0001(11) 0.0107(10) -0.0045(10) C13 0.0288(13) 0.0197(13) 0.0190(12) 0.0006(10) 0.0042(10) -0.0031(10) C14 0.0337(14) 0.071(2) 0.0194(13) 0.0014(14) 0.0077(11) -0.0072(14) C15 0.0252(12) 0.0167(13) 0.0201(12) -0.0013(10) 0.0070(9) -0.0017(10) C16 0.0224(12) 0.0184(13) 0.0230(12) 0.0014(10) 0.0066(9) -0.0028(10) C17 0.0259(13) 0.0248(15) 0.0273(13) -0.0004(11) 0.0070(10) 0.0032(11) C18 0.0268(14) 0.0359(17) 0.0397(16) -0.0022(14) -0.0008(11) 0.0080(12) C19 0.0309(15) 0.0399(19) 0.0415(17) -0.0039(14) -0.0086(12) -0.0040(13) C20 0.0427(16) 0.0270(16) 0.0325(15) -0.0073(13) -0.0004(12) -0.0051(13) C21 0.0308(13) 0.0221(15) 0.0300(14) -0.0012(11) 0.0066(11) 0.0036(11) C22 0.0367(15) 0.0321(17) 0.0389(16) -0.0077(14) 0.0003(12) 0.0128(13) C23 0.0314(13) 0.0202(14) 0.0138(11) 0.0000(10) 0.0062(9) 0.0063(10) C24 0.0297(13) 0.0308(16) 0.0181(12) -0.0049(11) 0.0038(10) 0.0081(11) C25 0.0314(14) 0.0471(19) 0.0212(13) -0.0048(13) -0.0034(11) 0.0185(13) C26 0.063(2) 0.0281(17) 0.0226(14) 0.0012(12) 0.0023(13) 0.0202(15) C27 0.0607(19) 0.0253(16) 0.0238(14) 0.0042(12) 0.0082(12) 0.0022(14) C28 0.0405(14) 0.0237(15) 0.0210(13) 0.0001(11) 0.0081(11) 0.0018(12) C29 0.0247(13) 0.052(2) 0.0361(16) 0.0017(14) 0.0060(11) 0.0030(13) C30 0.0244(12) 0.0170(13) 0.0236(12) -0.0020(10) 0.0118(10) -0.0005(10) C31 0.073(2) 0.038(2) 0.0361(17) 0.0016(14) 0.0272(15) -0.0155(15) C32 0.201(5) 0.033(2) 0.073(3) -0.002(2) 0.094(3) -0.006(3) C33 0.0535(17) 0.0345(18) 0.0386(16) -0.0050(14) 0.0262(13) 0.0001(14) C34 0.0348(14) 0.0253(15) 0.0369(15) -0.0028(12) 0.0150(12) 0.0008(12) C35 0.0401(15) 0.0302(17) 0.0361(15) -0.0006(12) 0.0213(12) -0.0062(12) C36 0.0443(16) 0.0384(18) 0.0275(14) -0.0004(13) 0.0168(12) -0.0013(13) C37 0.0599(19) 0.0334(18) 0.0359(16) -0.0043(14) 0.0243(14) -0.0023(14) C38 0.0589(18) 0.0256(16) 0.0375(16) -0.0086(13) 0.0257(13) -0.0111(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 Ca1 O1 2.3668(16) . ? Ca1 O2 2.3688(17) . ? Ca1 N1 2.415(2) . ? Ca1 N4 2.425(2) . ? Ca1 N3 2.4244(19) . ? Ca1 N2 2.442(2) . ? Ca1 C15 2.799(2) . ? Ca1 C30 2.802(2) . ? O1 C31 1.436(3) . ? O1 C34 1.438(3) . ? O2 C35 1.445(3) . ? O2 C38 1.454(3) . ? N1 C15 1.332(3) . ? N1 C1 1.406(3) . ? N2 C15 1.317(3) . ? N2 C8 1.412(3) . ? N3 C30 1.319(3) . ? N3 C16 1.407(3) . ? N4 C30 1.330(3) . ? N4 C23 1.402(3) . ? C1 C6 1.393(4) . ? C1 C2 1.418(3) . ? C2 C3 1.388(3) . ? C2 C7 1.500(4) . ? C3 C4 1.381(4) . ? C4 C5 1.384(3) . ? C5 C6 1.393(3) . ? C8 C13 1.395(3) . ? C8 C9 1.409(3) . ? C9 C10 1.397(3) . ? C9 C14 1.497(3) . ? C10 C11 1.381(3) . ? C11 C12 1.382(3) . ? C12 C13 1.392(3) . ? C16 C21 1.394(3) . ? C16 C17 1.411(3) . ? C17 C18 1.391(3) . ? C17 C22 1.498(4) . ? C18 C19 1.386(4) . ? C19 C20 1.382(4) . ? C20 C21 1.389(3) . ? C23 C28 1.397(3) . ? C23 C24 1.413(3) . ? C24 C25 1.397(4) . ? C24 C29 1.504(4) . ? C25 C26 1.385(4) . ? C26 C27 1.367(4) . ? C27 C28 1.388(4) . ? C31 C32 1.461(4) . ? C32 C33 1.507(5) . ? C33 C34 1.521(4) . ? C35 C36 1.512(4) . ? C36 C37 1.521(4) . ? C37 C38 1.511(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ca1 O2 174.04(6) . . ? O1 Ca1 N1 94.90(7) . . ? O2 Ca1 N1 91.06(7) . . ? O1 Ca1 N4 88.95(6) . . ? O2 Ca1 N4 85.20(6) . . ? N1 Ca1 N4 169.60(6) . . ? O1 Ca1 N3 87.34(6) . . ? O2 Ca1 N3 90.37(6) . . ? N1 Ca1 N3 114.15(6) . . ? N4 Ca1 N3 56.29(6) . . ? O1 Ca1 N2 89.60(6) . . ? O2 Ca1 N2 93.58(6) . . ? N1 Ca1 N2 56.41(6) . . ? N4 Ca1 N2 133.43(6) . . ? N3 Ca1 N2 169.78(7) . . ? O1 Ca1 C15 93.69(6) . . ? O2 Ca1 C15 91.48(6) . . ? N1 Ca1 C15 28.38(6) . . ? N4 Ca1 C15 161.07(6) . . ? N3 Ca1 C15 142.51(7) . . ? N2 Ca1 C15 28.07(6) . . ? O1 Ca1 C30 89.67(6) . . ? O2 Ca1 C30 85.73(6) . . ? N1 Ca1 C30 141.78(6) . . ? N4 Ca1 C30 28.33(6) . . ? N3 Ca1 C30 28.06(6) . . ? N2 Ca1 C30 161.76(7) . . ? C15 Ca1 C30 169.87(7) . . ? C31 O1 C34 108.1(2) . . ? C31 O1 Ca1 124.18(16) . . ? C34 O1 Ca1 127.60(14) . . ? C35 O2 C38 109.13(19) . . ? C35 O2 Ca1 124.57(15) . . ? C38 O2 Ca1 126.13(14) . . ? C15 N1 C1 118.2(2) . . ? C15 N1 Ca1 92.07(14) . . ? C1 N1 Ca1 149.08(15) . . ? C15 N2 C8 117.6(2) . . ? C15 N2 Ca1 91.22(13) . . ? C8 N2 Ca1 148.64(16) . . ? C30 N3 C16 118.6(2) . . ? C30 N3 Ca1 92.10(13) . . ? C16 N3 Ca1 145.65(15) . . ? C30 N4 C23 118.8(2) . . ? C30 N4 Ca1 91.79(14) . . ? C23 N4 Ca1 149.27(15) . . ? C6 C1 N1 122.4(2) . . ? C6 C1 C2 119.1(2) . . ? N1 C1 C2 118.5(2) . . ? C3 C2 C1 118.0(2) . . ? C3 C2 C7 120.9(2) . . ? C1 C2 C7 121.1(2) . . ? C4 C3 C2 122.5(2) . . ? C3 C4 C5 119.7(2) . . ? C6 C5 C4 119.2(3) . . ? C5 C6 C1 121.5(2) . . ? C13 C8 C9 119.3(2) . . ? C13 C8 N2 122.2(2) . . ? C9 C8 N2 118.5(2) . . ? C10 C9 C8 118.4(2) . . ? C10 C9 C14 120.6(2) . . ? C8 C9 C14 121.0(2) . . ? C11 C10 C9 122.0(2) . . ? C12 C11 C10 119.6(2) . . ? C11 C12 C13 119.8(2) . . ? C8 C13 C12 121.1(2) . . ? N2 C15 N1 120.1(2) . . ? N2 C15 Ca1 60.71(12) . . ? N1 C15 Ca1 59.54(13) . . ? C21 C16 N3 122.8(2) . . ? C21 C16 C17 119.2(2) . . ? N3 C16 C17 117.9(2) . . ? C18 C17 C16 118.3(2) . . ? C18 C17 C22 120.9(2) . . ? C16 C17 C22 120.9(2) . . ? C19 C18 C17 121.9(2) . . ? C18 C19 C20 119.7(2) . . ? C19 C20 C21 119.4(3) . . ? C20 C21 C16 121.3(2) . . ? C28 C23 N4 123.5(2) . . ? C28 C23 C24 118.6(2) . . ? N4 C23 C24 117.8(2) . . ? C25 C24 C23 118.6(2) . . ? C25 C24 C29 121.0(2) . . ? C23 C24 C29 120.5(2) . . ? C26 C25 C24 121.6(2) . . ? C27 C26 C25 119.7(3) . . ? C26 C27 C28 120.3(3) . . ? C27 C28 C23 121.2(2) . . ? N3 C30 N4 119.4(2) . . ? N3 C30 Ca1 59.84(12) . . ? N4 C30 Ca1 59.88(12) . . ? O1 C31 C32 107.9(3) . . ? C31 C32 C33 106.8(3) . . ? C32 C33 C34 102.6(3) . . ? O1 C34 C33 104.6(2) . . ? O2 C35 C36 105.6(2) . . ? C35 C36 C37 101.6(2) . . ? C38 C37 C36 101.9(2) . . ? O2 C38 C37 105.5(2) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.352 _refine_diff_density_min -0.385 _refine_diff_density_rms 0.060 _chemical_compound_source THF #===END data_COMPOUND_2 _database_code_depnum_ccdc_archive 'CCDC 298095' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point 429-431 _chemical_formula_moiety 'C42 H54 Ca N4 O2' _chemical_formula_sum 'C42 H54 Ca N4 O2' _chemical_formula_weight 686.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_int_tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.3852(3) _cell_length_b 11.1831(2) _cell_length_c 18.1765(4) _cell_angle_alpha 90.00 _cell_angle_beta 101.7590(10) _cell_angle_gamma 90.00 _cell_volume 3857.73(12) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'rectangular block' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.183 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1480 _exptl_absorpt_coefficient_mu 0.202 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9418 _exptl_absorpt_correction_T_max 0.9607 _exptl_absorpt_process_details 'performed as part of the DENZO-SMN package' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'psi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12570 _diffrn_reflns_av_R_equivalents 0.0572 _diffrn_reflns_av_sigmaI/netI 0.0635 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 27.90 _reflns_number_total 4599 _reflns_number_gt 3223 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction X-Seed _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed / POV-Ray' _computing_publication_material 'Microsoft Office 2000' _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^)+(0.0596P)^2^+4.2348P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4599 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0995 _refine_ls_R_factor_gt 0.0574 _refine_ls_wR_factor_ref 0.1882 _refine_ls_wR_factor_gt 0.1331 _refine_ls_goodness_of_fit_ref 1.408 _refine_ls_restrained_S_all 1.408 _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 Ca1 Ca 0.5000 0.57357(6) 0.7500 0.0193(2) Uani 1 2 d S . . O1 O 0.48764(11) 0.40896(16) 0.66347(11) 0.0287(5) Uani 1 1 d . . . N1 N 0.58212(11) 0.7006(2) 0.83259(12) 0.0229(5) Uani 1 1 d . . . N2 N 0.61679(11) 0.6241(2) 0.72826(13) 0.0234(5) Uani 1 1 d . . . C1 C 0.60134(13) 0.7520(2) 0.90512(15) 0.0219(6) Uani 1 1 d . . . C2 C 0.57230(13) 0.8634(2) 0.91828(15) 0.0218(6) Uani 1 1 d . . . C3 C 0.58697(14) 0.9114(2) 0.99031(16) 0.0258(6) Uani 1 1 d . . . H3 H 0.5670 0.9862 0.9994 0.031 Uiso 1 1 calc R . . C4 C 0.63019(16) 0.8522(3) 1.04893(16) 0.0315(7) Uani 1 1 d . . . H4 H 0.6401 0.8863 1.0978 0.038 Uiso 1 1 calc R . . C5 C 0.65894(15) 0.7428(3) 1.03586(17) 0.0326(7) Uani 1 1 d . . . H5 H 0.6887 0.7024 1.0762 0.039 Uiso 1 1 calc R . . C6 C 0.64510(14) 0.6910(2) 0.96477(16) 0.0269(6) Uani 1 1 d . . . C7 C 0.52738(15) 0.9310(3) 0.85396(16) 0.0268(6) Uani 1 1 d . . . H7A H 0.5015 0.9943 0.8739 0.040 Uiso 1 1 calc R . . H7B H 0.4939 0.8759 0.8235 0.040 Uiso 1 1 calc R . . H7C H 0.5576 0.9666 0.8227 0.040 Uiso 1 1 calc R . . C8 C 0.67559(16) 0.5695(3) 0.95389(19) 0.0359(7) Uani 1 1 d . . . H8A H 0.7211 0.5794 0.9390 0.054 Uiso 1 1 calc R . . H8B H 0.6432 0.5259 0.9145 0.054 Uiso 1 1 calc R . . H8C H 0.6823 0.5245 1.0011 0.054 Uiso 1 1 calc R . . C9 C 0.67289(13) 0.6109(2) 0.68915(15) 0.0238(6) Uani 1 1 d . . . C10 C 0.68611(14) 0.7000(3) 0.64024(15) 0.0264(6) Uani 1 1 d . . . C11 C 0.74221(15) 0.6856(3) 0.60342(16) 0.0329(7) Uani 1 1 d . . . H11 H 0.7518 0.7464 0.5704 0.039 Uiso 1 1 calc R . . C12 C 0.78372(15) 0.5847(3) 0.61427(17) 0.0338(7) Uani 1 1 d . . . H12 H 0.8222 0.5766 0.5896 0.041 Uiso 1 1 calc R . . C13 C 0.76916(15) 0.4956(3) 0.66101(18) 0.0340(7) Uani 1 1 d . . . H13 H 0.7976 0.4257 0.6679 0.041 Uiso 1 1 calc R . . C14 C 0.71354(14) 0.5063(3) 0.69836(17) 0.0301(7) Uani 1 1 d . . . C15 C 0.64114(17) 0.8114(3) 0.62780(18) 0.0362(7) Uani 1 1 d . . . H15A H 0.5917 0.7889 0.6102 0.054 Uiso 1 1 calc R . . H15B H 0.6563 0.8619 0.5900 0.054 Uiso 1 1 calc R . . H15C H 0.6462 0.8556 0.6751 0.054 Uiso 1 1 calc R . . C16 C 0.69682(18) 0.4072(3) 0.7475(2) 0.0498(10) Uani 1 1 d . . . H16A H 0.7251 0.3367 0.7414 0.075 Uiso 1 1 calc R . . H16B H 0.6467 0.3871 0.7331 0.075 Uiso 1 1 calc R . . H16C H 0.7077 0.4330 0.8001 0.075 Uiso 1 1 calc R . . C17 C 0.63165(13) 0.6803(2) 0.79338(16) 0.0229(6) Uani 1 1 d . . . H17 H 0.6785 0.7065 0.8125 0.027 Uiso 1 1 calc R . . C18 C 0.4570(3) 0.2928(3) 0.6558(2) 0.0710(15) Uani 1 1 d . . . H18A H 0.4177 0.2888 0.6830 0.085 Uiso 1 1 calc R . . H18B H 0.4927 0.2324 0.6776 0.085 Uiso 1 1 calc R . . C19 C 0.4311(2) 0.2681(3) 0.57704(19) 0.0487(9) Uani 1 1 d . . . H19A H 0.3799 0.2839 0.5627 0.058 Uiso 1 1 calc R . . H19B H 0.4400 0.1837 0.5654 0.058 Uiso 1 1 calc R . . C20 C 0.47137(19) 0.3512(3) 0.53628(18) 0.0416(8) Uani 1 1 d . . . H20A H 0.5045 0.3058 0.5120 0.050 Uiso 1 1 calc R . . H20B H 0.4387 0.3966 0.4972 0.050 Uiso 1 1 calc R . . C21 C 0.5100(3) 0.4323(4) 0.5937(2) 0.0687(14) Uani 1 1 d . . . H21A H 0.5613 0.4187 0.6000 0.082 Uiso 1 1 calc R . . H21B H 0.4998 0.5164 0.5782 0.082 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ca1 0.0193(4) 0.0140(4) 0.0248(4) 0.000 0.0047(3) 0.000 O1 0.0419(12) 0.0191(10) 0.0277(11) -0.0036(8) 0.0130(9) -0.0061(8) N1 0.0216(11) 0.0208(12) 0.0274(12) -0.0054(9) 0.0077(9) -0.0026(9) N2 0.0197(11) 0.0232(12) 0.0285(13) -0.0035(10) 0.0074(9) 0.0003(9) C1 0.0194(12) 0.0205(13) 0.0266(14) -0.0028(11) 0.0063(10) -0.0067(10) C2 0.0201(12) 0.0198(14) 0.0272(14) -0.0009(11) 0.0089(10) -0.0048(10) C3 0.0291(14) 0.0204(14) 0.0302(15) -0.0050(12) 0.0115(11) -0.0066(11) C4 0.0358(16) 0.0314(16) 0.0267(15) -0.0061(13) 0.0051(12) -0.0099(13) C5 0.0306(15) 0.0317(16) 0.0316(16) 0.0032(13) -0.0029(12) -0.0050(13) C6 0.0238(14) 0.0204(14) 0.0353(16) 0.0001(12) 0.0035(12) -0.0035(11) C7 0.0290(14) 0.0228(14) 0.0298(15) -0.0007(12) 0.0083(11) 0.0014(12) C8 0.0308(16) 0.0255(16) 0.0483(19) 0.0009(14) 0.0007(13) 0.0018(13) C9 0.0194(13) 0.0240(14) 0.0277(15) -0.0068(11) 0.0040(10) 0.0016(11) C10 0.0283(14) 0.0306(16) 0.0198(14) -0.0039(12) 0.0042(11) 0.0055(12) C11 0.0349(16) 0.0420(19) 0.0238(15) -0.0003(13) 0.0110(12) 0.0056(14) C12 0.0252(15) 0.0439(19) 0.0345(17) -0.0129(14) 0.0110(12) 0.0043(13) C13 0.0231(14) 0.0293(16) 0.050(2) -0.0097(15) 0.0092(13) 0.0055(12) C14 0.0214(14) 0.0245(15) 0.0448(18) -0.0044(13) 0.0075(12) 0.0008(11) C15 0.0398(17) 0.0391(18) 0.0313(17) 0.0098(14) 0.0109(13) 0.0153(14) C16 0.0349(18) 0.0275(18) 0.092(3) 0.0123(18) 0.0244(18) 0.0078(14) C17 0.0183(12) 0.0171(13) 0.0331(15) -0.0012(11) 0.0052(11) -0.0005(10) C18 0.149(4) 0.034(2) 0.036(2) -0.0121(16) 0.034(2) -0.049(2) C19 0.071(3) 0.0307(18) 0.043(2) -0.0089(16) 0.0083(17) -0.0115(17) C20 0.055(2) 0.045(2) 0.0303(17) 0.0035(15) 0.0222(15) 0.0138(17) C21 0.102(3) 0.055(2) 0.070(3) -0.027(2) 0.068(3) -0.038(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ca1 O1 2.4013(19) . ? Ca1 O1 2.4013(19) 2_656 ? Ca1 N1 2.415(2) . ? Ca1 N1 2.415(2) 2_656 ? Ca1 N2 2.442(2) 2_656 ? Ca1 N2 2.442(2) . ? Ca1 C17 2.782(3) . ? Ca1 C17 2.782(3) 2_656 ? O1 C18 1.423(4) . ? O1 C21 1.445(4) . ? N1 C17 1.327(3) . ? N1 C1 1.417(3) . ? N2 C17 1.319(3) . ? N2 C9 1.423(3) . ? C1 C2 1.407(4) . ? C1 C6 1.409(4) . ? C2 C3 1.390(4) . ? C2 C7 1.510(4) . ? C3 C4 1.383(4) . ? C4 C5 1.384(4) . ? C5 C6 1.392(4) . ? C6 C8 1.510(4) . ? C9 C10 1.393(4) . ? C9 C14 1.401(4) . ? C10 C11 1.397(4) . ? C10 C15 1.511(4) . ? C11 C12 1.377(4) . ? C12 C13 1.375(4) . ? C13 C14 1.391(4) . ? C14 C16 1.499(4) . ? C18 C19 1.444(5) . ? C19 C20 1.502(5) . ? C20 C21 1.467(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ca1 O1 79.90(9) . 2_656 ? O1 Ca1 N1 145.42(7) . . ? O1 Ca1 N1 94.52(7) 2_656 . ? O1 Ca1 N1 94.52(7) . 2_656 ? O1 Ca1 N1 145.42(7) 2_656 2_656 ? N1 Ca1 N1 107.92(11) . 2_656 ? O1 Ca1 N2 108.13(7) . 2_656 ? O1 Ca1 N2 92.48(7) 2_656 2_656 ? N1 Ca1 N2 106.19(8) . 2_656 ? N1 Ca1 N2 56.58(7) 2_656 2_656 ? O1 Ca1 N2 92.48(7) . . ? O1 Ca1 N2 108.13(7) 2_656 . ? N1 Ca1 N2 56.58(7) . . ? N1 Ca1 N2 106.19(8) 2_656 . ? N2 Ca1 N2 153.27(11) 2_656 . ? O1 Ca1 C17 118.54(7) . . ? O1 Ca1 C17 100.36(7) 2_656 . ? N1 Ca1 C17 28.48(7) . . ? N1 Ca1 C17 111.98(8) 2_656 . ? N2 Ca1 C17 133.01(8) 2_656 . ? N2 Ca1 C17 28.31(7) . . ? O1 Ca1 C17 100.36(7) . 2_656 ? O1 Ca1 C17 118.54(7) 2_656 2_656 ? N1 Ca1 C17 111.98(8) . 2_656 ? N1 Ca1 C17 28.48(7) 2_656 2_656 ? N2 Ca1 C17 28.31(7) 2_656 2_656 ? N2 Ca1 C17 133.01(8) . 2_656 ? C17 Ca1 C17 129.20(11) . 2_656 ? C18 O1 C21 105.8(2) . . ? C18 O1 Ca1 138.41(19) . . ? C21 O1 Ca1 115.39(18) . . ? C17 N1 C1 119.2(2) . . ? C17 N1 Ca1 91.29(16) . . ? C1 N1 Ca1 146.32(16) . . ? C17 N2 C9 116.6(2) . . ? C17 N2 Ca1 90.29(15) . . ? C9 N2 Ca1 152.24(18) . . ? C2 C1 C6 119.8(2) . . ? C2 C1 N1 118.6(2) . . ? C6 C1 N1 121.5(2) . . ? C3 C2 C1 119.3(2) . . ? C3 C2 C7 120.7(2) . . ? C1 C2 C7 119.9(2) . . ? C4 C3 C2 121.1(3) . . ? C3 C4 C5 119.5(3) . . ? C4 C5 C6 121.3(3) . . ? C5 C6 C1 119.0(3) . . ? C5 C6 C8 119.3(3) . . ? C1 C6 C8 121.7(3) . . ? C10 C9 C14 120.1(2) . . ? C10 C9 N2 120.2(2) . . ? C14 C9 N2 119.7(3) . . ? C9 C10 C11 119.1(3) . . ? C9 C10 C15 120.6(2) . . ? C11 C10 C15 120.3(3) . . ? C12 C11 C10 121.0(3) . . ? C13 C12 C11 119.6(3) . . ? C12 C13 C14 121.1(3) . . ? C13 C14 C9 119.1(3) . . ? C13 C14 C16 120.7(3) . . ? C9 C14 C16 120.2(3) . . ? N2 C17 N1 120.9(2) . . ? N2 C17 Ca1 61.40(13) . . ? N1 C17 Ca1 60.23(14) . . ? O1 C18 C19 109.0(3) . . ? C18 C19 C20 105.1(3) . . ? C21 C20 C19 105.8(3) . . ? O1 C21 C20 108.2(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.90 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.654 _refine_diff_density_min -0.696 _refine_diff_density_rms 0.178 _chemical_compound_source THF #===END data_COMPOUND_4 _database_code_depnum_ccdc_archive 'CCDC 298096' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point 429-432 _chemical_formula_moiety 'C42 H54 N4 O3 Sr' _chemical_formula_sum 'C42 H54 N4 O3 Sr' _chemical_formula_weight 750.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sr Sr -1.5307 3.2498 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C c' _symmetry_int_tables_number 9 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 21.4128(8) _cell_length_b 9.8514(4) _cell_length_c 18.7930(8) _cell_angle_alpha 90.00 _cell_angle_beta 100.313(3) _cell_angle_gamma 90.00 _cell_volume 3900.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'rectangular block' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.278 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1584 _exptl_absorpt_coefficient_mu 1.425 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7637 _exptl_absorpt_correction_T_max 0.9322 _exptl_absorpt_process_details 'performed as part of the DENZO-SMN package' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'psi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15560 _diffrn_reflns_av_R_equivalents 0.1114 _diffrn_reflns_av_sigmaI/netI 0.1869 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.87 _diffrn_reflns_theta_max 28.10 _reflns_number_total 7223 _reflns_number_gt 4314 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction X-Seed _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed / POV-Ray' _computing_publication_material 'Microsoft Office 2000' _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^)+(0.0819P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.004(9) _refine_ls_number_reflns 7223 _refine_ls_number_parameters 455 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1438 _refine_ls_R_factor_gt 0.0605 _refine_ls_wR_factor_ref 0.1494 _refine_ls_wR_factor_gt 0.1159 _refine_ls_goodness_of_fit_ref 0.872 _refine_ls_restrained_S_all 0.872 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sr1 Sr 0.49946(3) 0.55228(6) 0.25016(3) 0.02081(17) Uani 1 1 d . . . O1 O 0.5046(2) 0.7065(5) 0.1401(2) 0.0249(11) Uani 1 1 d . . . O2 O 0.4020(2) 0.7206(5) 0.2309(2) 0.0313(12) Uani 1 1 d . . . O3 O 0.6199(2) 0.6159(5) 0.2503(2) 0.0265(11) Uani 1 1 d . . . N1 N 0.5225(3) 0.6476(6) 0.3810(3) 0.0224(13) Uani 1 1 d . . . N2 N 0.4475(2) 0.4758(5) 0.3625(3) 0.0207(13) Uani 1 1 d . . . N3 N 0.5558(2) 0.3199(6) 0.2357(3) 0.0214(13) Uani 1 1 d . . . N4 N 0.4606(2) 0.3505(6) 0.1576(3) 0.0239(13) Uani 1 1 d . . . C1 C 0.5678(3) 0.7144(7) 0.4319(4) 0.0216(16) Uani 1 1 d . . . C2 C 0.5833(3) 0.8481(7) 0.4180(4) 0.0249(16) Uani 1 1 d . . . C3 C 0.6308(3) 0.9134(7) 0.4658(4) 0.0319(18) Uani 1 1 d . . . H3 H 0.6424 1.0033 0.4554 0.038 Uiso 1 1 calc R . . C4 C 0.6618(3) 0.8501(8) 0.5287(4) 0.0354(19) Uani 1 1 d . . . H4 H 0.6931 0.8971 0.5618 0.043 Uiso 1 1 calc R . . C5 C 0.6461(3) 0.7180(8) 0.5418(4) 0.0324(19) Uani 1 1 d . . . H5 H 0.6673 0.6728 0.5840 0.039 Uiso 1 1 calc R . . C6 C 0.5998(3) 0.6508(8) 0.4940(4) 0.0282(17) Uani 1 1 d . . . H6 H 0.5895 0.5596 0.5038 0.034 Uiso 1 1 calc R . . C7 C 0.5495(4) 0.9204(8) 0.3509(4) 0.040(2) Uani 1 1 d . . . H7A H 0.5649 1.0141 0.3509 0.060 Uiso 1 1 calc R . . H7B H 0.5037 0.9207 0.3507 0.060 Uiso 1 1 calc R . . H7C H 0.5581 0.8732 0.3078 0.060 Uiso 1 1 calc R . . C8 C 0.3994(3) 0.4088(7) 0.3913(4) 0.0258(17) Uani 1 1 d . . . C9 C 0.3876(3) 0.2700(7) 0.3748(4) 0.0253(17) Uani 1 1 d . . . C10 C 0.3418(3) 0.2037(8) 0.4061(4) 0.0323(18) Uani 1 1 d . . . H10 H 0.3341 0.1100 0.3960 0.039 Uiso 1 1 calc R . . C11 C 0.3070(4) 0.2694(8) 0.4515(4) 0.035(2) Uani 1 1 d . . . H11 H 0.2766 0.2210 0.4727 0.042 Uiso 1 1 calc R . . C12 C 0.3171(3) 0.4060(8) 0.4653(4) 0.0321(19) Uani 1 1 d . . . H12 H 0.2926 0.4529 0.4949 0.039 Uiso 1 1 calc R . . C13 C 0.3630(3) 0.4750(8) 0.4361(3) 0.0259(17) Uani 1 1 d . . . H13 H 0.3700 0.5688 0.4465 0.031 Uiso 1 1 calc R . . C14 C 0.4241(4) 0.1949(8) 0.3259(4) 0.0362(19) Uani 1 1 d . . . H14A H 0.4162 0.0973 0.3289 0.054 Uiso 1 1 calc R . . H14B H 0.4696 0.2128 0.3409 0.054 Uiso 1 1 calc R . . H14C H 0.4104 0.2257 0.2759 0.054 Uiso 1 1 calc R . . C15 C 0.4829(3) 0.5627(7) 0.4055(3) 0.0195(15) Uani 1 1 d . . . H15 H 0.4801 0.5648 0.4553 0.023 Uiso 1 1 calc R . . C16 C 0.6085(3) 0.2361(6) 0.2587(3) 0.0175(15) Uani 1 1 d . . . C17 C 0.6420(3) 0.2478(7) 0.3303(4) 0.0227(16) Uani 1 1 d . . . C18 C 0.6943(3) 0.1619(8) 0.3518(4) 0.0281(17) Uani 1 1 d . . . H18 H 0.7177 0.1707 0.3995 0.034 Uiso 1 1 calc R . . C19 C 0.7134(3) 0.0663(7) 0.3074(4) 0.0301(18) Uani 1 1 d . . . H19 H 0.7479 0.0073 0.3247 0.036 Uiso 1 1 calc R . . C20 C 0.6812(3) 0.0573(8) 0.2365(4) 0.0273(16) Uani 1 1 d . . . H20 H 0.6943 -0.0069 0.2044 0.033 Uiso 1 1 calc R . . C21 C 0.6298(3) 0.1418(7) 0.2122(3) 0.0211(16) Uani 1 1 d . . . H21 H 0.6087 0.1358 0.1634 0.025 Uiso 1 1 calc R . . C22 C 0.6228(4) 0.3481(8) 0.3814(4) 0.032(2) Uani 1 1 d . . . H22A H 0.6479 0.3336 0.4298 0.047 Uiso 1 1 calc R . . H22B H 0.5776 0.3366 0.3831 0.047 Uiso 1 1 calc R . . H22C H 0.6302 0.4402 0.3650 0.047 Uiso 1 1 calc R . . C23 C 0.4163(3) 0.2908(7) 0.1027(4) 0.0224(17) Uani 1 1 d . . . C24 C 0.3505(3) 0.3181(8) 0.0994(4) 0.0270(18) Uani 1 1 d . . . C25 C 0.3070(4) 0.2543(8) 0.0468(4) 0.035(2) Uani 1 1 d . . . H25 H 0.2630 0.2694 0.0457 0.042 Uiso 1 1 calc R . . C26 C 0.3253(4) 0.1690(8) -0.0045(4) 0.040(2) Uani 1 1 d . . . H26 H 0.2944 0.1272 -0.0403 0.048 Uiso 1 1 calc R . . C27 C 0.3895(4) 0.1456(8) -0.0026(4) 0.037(2) Uani 1 1 d . . . H27 H 0.4028 0.0874 -0.0374 0.044 Uiso 1 1 calc R . . C28 C 0.4342(3) 0.2069(7) 0.0497(4) 0.0291(18) Uani 1 1 d . . . H28 H 0.4781 0.1917 0.0497 0.035 Uiso 1 1 calc R . . C29 C 0.3295(3) 0.4137(8) 0.1532(4) 0.037(2) Uani 1 1 d . . . H29A H 0.3494 0.5026 0.1502 0.056 Uiso 1 1 calc R . . H29B H 0.3423 0.3771 0.2022 0.056 Uiso 1 1 calc R . . H29C H 0.2832 0.4235 0.1424 0.056 Uiso 1 1 calc R . . C30 C 0.5097(3) 0.2740(7) 0.1860(3) 0.0219(16) Uani 1 1 d . . . H30 H 0.5116 0.1829 0.1699 0.026 Uiso 1 1 calc R . . C31 C 0.4895(4) 0.6614(8) 0.0659(4) 0.037(2) Uani 1 1 d . . . H31A H 0.4434 0.6690 0.0473 0.045 Uiso 1 1 calc R . . H31B H 0.5026 0.5657 0.0616 0.045 Uiso 1 1 calc R . . C32 C 0.5252(5) 0.7511(11) 0.0257(4) 0.064(3) Uani 1 1 d . . . H32A H 0.5029 0.7619 -0.0248 0.076 Uiso 1 1 calc R . . H32B H 0.5682 0.7144 0.0255 0.076 Uiso 1 1 calc R . . C33 C 0.5288(6) 0.8803(10) 0.0641(5) 0.065(3) Uani 1 1 d . . . H33A H 0.4911 0.9368 0.0461 0.079 Uiso 1 1 calc R . . H33B H 0.5674 0.9310 0.0580 0.079 Uiso 1 1 calc R . . C34 C 0.5311(4) 0.8425(7) 0.1423(4) 0.0326(18) Uani 1 1 d . . . H34A H 0.5754 0.8433 0.1691 0.039 Uiso 1 1 calc R . . H34B H 0.5056 0.9064 0.1659 0.039 Uiso 1 1 calc R . . C35 C 0.3651(4) 0.7394(9) 0.2876(5) 0.043(2) Uani 1 1 d . . . H35A H 0.3925 0.7722 0.3324 0.052 Uiso 1 1 calc R . . H35B H 0.3453 0.6528 0.2983 0.052 Uiso 1 1 calc R . . C36 C 0.3145(4) 0.8441(9) 0.2598(5) 0.046(2) Uani 1 1 d . . . H36A H 0.2749 0.8267 0.2786 0.055 Uiso 1 1 calc R . . H36B H 0.3295 0.9373 0.2732 0.055 Uiso 1 1 calc R . . C37 C 0.3049(4) 0.8234(11) 0.1796(5) 0.059(3) Uani 1 1 d . . . H37A H 0.2875 0.9059 0.1532 0.071 Uiso 1 1 calc R . . H37B H 0.2762 0.7459 0.1643 0.071 Uiso 1 1 calc R . . C38 C 0.3720(4) 0.7939(10) 0.1680(4) 0.052(3) Uani 1 1 d . . . H38A H 0.3712 0.7386 0.1238 0.062 Uiso 1 1 calc R . . H38B H 0.3950 0.8795 0.1628 0.062 Uiso 1 1 calc R . . C39 C 0.6444(3) 0.5565(8) 0.1905(4) 0.0294(16) Uani 1 1 d . . . H39A H 0.6108 0.5498 0.1470 0.035 Uiso 1 1 calc R . . H39B H 0.6620 0.4650 0.2031 0.035 Uiso 1 1 calc R . . C40 C 0.6959(3) 0.6543(8) 0.1783(4) 0.0370(19) Uani 1 1 d . . . H40A H 0.7266 0.6104 0.1519 0.044 Uiso 1 1 calc R . . H40B H 0.6779 0.7357 0.1512 0.044 Uiso 1 1 calc R . . C41 C 0.7265(3) 0.6898(8) 0.2550(4) 0.041(2) Uani 1 1 d . . . H41A H 0.7455 0.7817 0.2576 0.049 Uiso 1 1 calc R . . H41B H 0.7598 0.6231 0.2746 0.049 Uiso 1 1 calc R . . C42 C 0.6717(4) 0.6838(9) 0.2952(4) 0.047(2) Uani 1 1 d . . . H42A H 0.6842 0.6338 0.3412 0.056 Uiso 1 1 calc R . . H42B H 0.6588 0.7768 0.3064 0.056 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sr1 0.0215(3) 0.0203(3) 0.0202(3) -0.0012(4) 0.0027(2) 0.0016(4) O1 0.034(3) 0.023(3) 0.017(2) 0.001(2) 0.004(2) -0.001(2) O2 0.023(3) 0.038(3) 0.033(3) 0.004(2) 0.005(2) 0.016(2) O3 0.021(2) 0.030(3) 0.029(3) -0.005(2) 0.005(2) -0.003(2) N1 0.022(3) 0.021(4) 0.024(3) 0.001(3) 0.003(3) -0.007(3) N2 0.020(3) 0.023(4) 0.022(3) 0.005(2) 0.009(2) -0.004(2) N3 0.015(3) 0.029(4) 0.018(3) -0.001(3) -0.001(2) 0.008(3) N4 0.018(3) 0.022(3) 0.030(3) -0.008(3) 0.001(3) -0.001(3) C1 0.013(3) 0.033(5) 0.021(4) -0.008(3) 0.008(3) 0.001(3) C2 0.026(4) 0.021(4) 0.030(4) -0.003(3) 0.011(3) 0.000(3) C3 0.039(4) 0.026(5) 0.036(4) -0.007(3) 0.018(4) -0.012(3) C4 0.035(4) 0.044(5) 0.030(4) -0.011(4) 0.012(4) -0.014(4) C5 0.030(4) 0.047(5) 0.020(4) 0.008(4) 0.007(4) -0.010(4) C6 0.023(4) 0.034(5) 0.029(4) -0.002(3) 0.009(3) -0.008(3) C7 0.046(5) 0.028(5) 0.043(5) 0.008(4) -0.001(4) -0.010(4) C8 0.024(4) 0.029(5) 0.023(4) 0.001(3) 0.001(3) -0.003(3) C9 0.025(4) 0.020(4) 0.031(4) 0.004(3) 0.005(3) -0.003(3) C10 0.044(5) 0.016(4) 0.037(4) 0.005(3) 0.008(4) -0.006(3) C11 0.036(5) 0.041(5) 0.032(4) 0.003(4) 0.017(4) -0.020(4) C12 0.024(4) 0.046(6) 0.028(4) -0.003(4) 0.008(3) -0.002(4) C13 0.022(4) 0.033(5) 0.024(4) 0.000(3) 0.009(3) -0.003(3) C14 0.039(5) 0.030(5) 0.042(5) 0.002(4) 0.013(4) -0.001(4) C15 0.023(3) 0.018(4) 0.018(3) -0.003(3) 0.003(3) 0.009(3) C16 0.022(4) 0.012(4) 0.018(3) 0.005(3) 0.001(3) -0.007(3) C17 0.022(4) 0.020(4) 0.026(4) 0.000(3) 0.002(3) -0.004(3) C18 0.024(4) 0.028(5) 0.032(4) 0.007(4) 0.002(3) -0.003(3) C19 0.018(4) 0.023(4) 0.047(5) 0.005(4) -0.001(3) 0.004(3) C20 0.012(3) 0.033(4) 0.037(4) -0.005(4) 0.004(3) -0.001(3) C21 0.022(4) 0.026(4) 0.016(3) 0.001(3) 0.005(3) -0.002(3) C22 0.035(5) 0.030(5) 0.027(4) -0.002(4) -0.002(4) 0.001(4) C23 0.022(4) 0.022(4) 0.022(4) 0.004(3) 0.000(3) -0.004(3) C24 0.022(4) 0.028(5) 0.029(4) 0.005(4) 0.000(3) -0.001(3) C25 0.028(4) 0.037(5) 0.039(5) 0.008(4) -0.002(4) -0.003(4) C26 0.038(5) 0.038(5) 0.035(4) -0.005(4) -0.015(4) -0.004(4) C27 0.043(5) 0.037(5) 0.026(4) -0.008(4) -0.008(4) 0.008(4) C28 0.034(4) 0.022(4) 0.030(4) -0.003(3) 0.003(4) 0.002(3) C29 0.026(4) 0.044(5) 0.042(5) -0.002(4) 0.006(4) 0.007(4) C30 0.016(3) 0.029(4) 0.021(4) -0.002(3) 0.003(3) 0.000(3) C31 0.052(5) 0.037(5) 0.021(4) 0.001(4) 0.001(4) -0.005(4) C32 0.088(7) 0.074(7) 0.030(5) -0.005(5) 0.014(5) -0.030(6) C33 0.108(8) 0.043(6) 0.045(5) 0.007(5) 0.012(6) -0.006(6) C34 0.046(5) 0.020(4) 0.035(4) 0.002(3) 0.015(4) 0.000(4) C35 0.040(5) 0.042(6) 0.048(5) -0.002(4) 0.009(4) 0.014(4) C36 0.043(5) 0.030(5) 0.068(6) 0.002(4) 0.019(5) 0.018(4) C37 0.034(5) 0.069(7) 0.072(7) 0.011(6) 0.003(5) 0.023(5) C38 0.040(5) 0.063(7) 0.049(5) 0.024(5) -0.001(4) 0.032(5) C39 0.030(4) 0.032(4) 0.029(4) 0.002(4) 0.016(3) 0.001(4) C40 0.033(4) 0.025(5) 0.058(5) 0.005(4) 0.021(4) 0.005(4) C41 0.022(4) 0.029(5) 0.069(6) 0.005(4) 0.000(4) 0.003(4) C42 0.042(5) 0.057(6) 0.039(5) 0.000(4) -0.003(4) -0.019(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sr1 O1 2.585(4) . ? Sr1 N1 2.595(5) . ? Sr1 N3 2.623(5) . ? Sr1 O2 2.640(4) . ? Sr1 O3 2.654(4) . ? Sr1 N2 2.666(5) . ? Sr1 N4 2.674(5) . ? Sr1 C15 3.004(6) . ? Sr1 C30 3.019(7) . ? O1 C31 1.445(8) . ? O1 C34 1.452(8) . ? O2 C38 1.436(8) . ? O2 C35 1.446(9) . ? O3 C39 1.445(8) . ? O3 C42 1.432(8) . ? N1 C15 1.330(8) . ? N1 C1 1.399(8) . ? N2 C15 1.320(8) . ? N2 C8 1.409(9) . ? N3 C30 1.311(8) . ? N3 C16 1.403(8) . ? N4 C30 1.327(8) . ? N4 C23 1.399(8) . ? C1 C2 1.395(10) . ? C1 C6 1.392(9) . ? C2 C3 1.387(9) . ? C2 C7 1.514(10) . ? C3 C4 1.395(10) . ? C4 C5 1.377(10) . ? C5 C6 1.382(10) . ? C8 C9 1.415(9) . ? C8 C13 1.406(10) . ? C9 C10 1.394(10) . ? C9 C14 1.503(10) . ? C10 C11 1.390(10) . ? C11 C12 1.381(11) . ? C12 C13 1.387(10) . ? C16 C17 1.412(9) . ? C16 C21 1.405(9) . ? C17 C18 1.404(9) . ? C17 C22 1.487(10) . ? C18 C19 1.367(10) . ? C19 C20 1.391(10) . ? C20 C21 1.390(9) . ? C23 C28 1.400(10) . ? C23 C24 1.425(9) . ? C24 C25 1.382(10) . ? C24 C29 1.509(11) . ? C25 C26 1.386(11) . ? C26 C27 1.388(11) . ? C27 C28 1.383(9) . ? C31 C32 1.462(12) . ? C32 C33 1.458(13) . ? C33 C34 1.508(11) . ? C35 C36 1.520(11) . ? C36 C37 1.497(12) . ? C37 C38 1.520(11) . ? C39 C40 1.514(10) . ? C40 C41 1.514(11) . ? C41 C42 1.507(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 O1 Sr1 N1 121.15(17) . . ? O1 Sr1 N3 110.10(16) . . ? N1 Sr1 N3 113.63(16) . . ? O1 Sr1 O2 70.58(15) . . ? N1 Sr1 O2 85.06(16) . . ? N3 Sr1 O2 154.24(16) . . ? O1 Sr1 O3 71.40(14) . . ? N1 Sr1 O3 83.91(15) . . ? N3 Sr1 O3 75.02(16) . . ? O2 Sr1 O3 126.62(17) . . ? O1 Sr1 N2 152.10(15) . . ? N1 Sr1 N2 52.22(17) . . ? N3 Sr1 N2 95.75(17) . . ? O2 Sr1 N2 81.59(16) . . ? O3 Sr1 N2 127.55(15) . . ? O1 Sr1 N4 88.24(16) . . ? N1 Sr1 N4 150.39(17) . . ? N3 Sr1 N4 51.65(16) . . ? O2 Sr1 N4 103.37(15) . . ? O3 Sr1 N4 111.44(15) . . ? N2 Sr1 N4 100.35(17) . . ? O1 Sr1 C15 141.88(16) . . ? N1 Sr1 C15 26.19(16) . . ? N3 Sr1 C15 105.47(17) . . ? O2 Sr1 C15 83.32(15) . . ? O3 Sr1 C15 105.93(15) . . ? N2 Sr1 C15 26.05(17) . . ? N4 Sr1 C15 125.48(18) . . ? O1 Sr1 C30 101.41(16) . . ? N1 Sr1 C30 133.76(18) . . ? N3 Sr1 C30 25.66(15) . . ? O2 Sr1 C30 128.92(16) . . ? O3 Sr1 C30 94.27(16) . . ? N2 Sr1 C30 97.48(17) . . ? N4 Sr1 C30 26.07(15) . . ? C15 Sr1 C30 116.66(18) . . ? C31 O1 C34 109.3(5) . . ? C31 O1 Sr1 123.9(4) . . ? C34 O1 Sr1 126.3(4) . . ? C38 O2 C35 108.6(5) . . ? C38 O2 Sr1 130.9(4) . . ? C35 O2 Sr1 120.1(4) . . ? C39 O3 C42 107.3(5) . . ? C39 O3 Sr1 113.0(4) . . ? C42 O3 Sr1 139.5(4) . . ? C15 N1 C1 117.7(6) . . ? C15 N1 Sr1 94.3(4) . . ? C1 N1 Sr1 144.0(4) . . ? C15 N2 C8 116.7(5) . . ? C15 N2 Sr1 91.4(4) . . ? C8 N2 Sr1 150.8(4) . . ? C30 N3 C16 118.5(6) . . ? C30 N3 Sr1 94.3(4) . . ? C16 N3 Sr1 147.2(4) . . ? C30 N4 C23 116.2(6) . . ? C30 N4 Sr1 91.6(4) . . ? C23 N4 Sr1 152.0(4) . . ? C2 C1 N1 118.4(6) . . ? C2 C1 C6 118.9(6) . . ? N1 C1 C6 122.6(7) . . ? C3 C2 C1 119.2(6) . . ? C3 C2 C7 120.4(6) . . ? C1 C2 C7 120.4(6) . . ? C2 C3 C4 121.6(7) . . ? C5 C4 C3 118.7(7) . . ? C6 C5 C4 120.4(7) . . ? C5 C6 C1 121.2(7) . . ? N2 C8 C9 118.8(6) . . ? N2 C8 C13 122.3(6) . . ? C9 C8 C13 118.9(6) . . ? C10 C9 C8 118.2(7) . . ? C10 C9 C14 120.6(6) . . ? C8 C9 C14 121.2(6) . . ? C11 C10 C9 122.4(7) . . ? C10 C11 C12 119.1(7) . . ? C11 C12 C13 120.1(7) . . ? C12 C13 C8 121.2(7) . . ? N2 C15 N1 121.9(6) . . ? N2 C15 Sr1 62.5(3) . . ? N1 C15 Sr1 59.5(3) . . ? N3 C16 C17 119.3(6) . . ? N3 C16 C21 122.0(5) . . ? C17 C16 C21 118.7(6) . . ? C18 C17 C16 117.9(6) . . ? C18 C17 C22 120.9(6) . . ? C16 C17 C22 121.2(6) . . ? C19 C18 C17 123.4(6) . . ? C18 C19 C20 118.5(6) . . ? C21 C20 C19 120.3(7) . . ? C20 C21 C16 121.2(6) . . ? N4 C23 C28 122.5(6) . . ? N4 C23 C24 119.1(6) . . ? C28 C23 C24 118.3(6) . . ? C25 C24 C23 118.7(7) . . ? C25 C24 C29 121.4(6) . . ? C23 C24 C29 120.0(6) . . ? C24 C25 C26 122.3(7) . . ? C27 C26 C25 119.0(7) . . ? C26 C27 C28 120.1(7) . . ? C27 C28 C23 121.4(7) . . ? N3 C30 N4 122.1(6) . . ? N3 C30 Sr1 60.1(4) . . ? N4 C30 Sr1 62.3(4) . . ? O1 C31 C32 105.3(6) . . ? C31 C32 C33 105.0(8) . . ? C32 C33 C34 104.8(7) . . ? O1 C34 C33 104.8(6) . . ? O2 C35 C36 106.5(7) . . ? C37 C36 C35 102.4(7) . . ? C36 C37 C38 102.0(7) . . ? O2 C38 C37 105.8(7) . . ? O3 C39 C40 103.7(6) . . ? C41 C40 C39 101.8(6) . . ? C40 C41 C42 103.0(6) . . ? O3 C42 C41 108.3(6) . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 28.10 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.569 _refine_diff_density_min -0.606 _refine_diff_density_rms 0.109 _chemical_compound_source THF #===END data_COMPOUND_5 _database_code_depnum_ccdc_archive 'CCDC 298097' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point 428-431 _chemical_formula_moiety 'C58 H86 N4 O6 Sr' _chemical_formula_sum 'C58 H86 N4 O6 Sr' _chemical_formula_weight 1022.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sr Sr -1.5307 3.2498 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _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 10.9388(3) _cell_length_b 33.5561(10) _cell_length_c 16.2284(5) _cell_angle_alpha 90.00 _cell_angle_beta 109.591(2) _cell_angle_gamma 90.00 _cell_volume 5612.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'rectangular block' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.211 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2192 _exptl_absorpt_coefficient_mu 1.012 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8233 _exptl_absorpt_correction_T_max 0.9056 _exptl_absorpt_process_details 'performed as part of the DENZO-SMN package' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'psi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34805 _diffrn_reflns_av_R_equivalents 0.0880 _diffrn_reflns_av_sigmaI/netI 0.1369 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -44 _diffrn_reflns_limit_k_max 42 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.61 _diffrn_reflns_theta_max 28.24 _reflns_number_total 12813 _reflns_number_gt 7102 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction X-Seed _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed / POV-Ray' _computing_publication_material 'Microsoft Office 2000' _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^)+(0.0684P)^2^+5.6811P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12813 _refine_ls_number_parameters 640 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1626 _refine_ls_R_factor_gt 0.0763 _refine_ls_wR_factor_ref 0.1761 _refine_ls_wR_factor_gt 0.1458 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sr1 Sr 0.40486(3) 0.154433(12) 0.81540(2) 0.02665(12) Uani 1 1 d . . . O1 O 0.5603(3) 0.19894(10) 0.9334(2) 0.0468(8) Uani 1 1 d . . . O2 O 0.2301(3) 0.11418(10) 0.6975(2) 0.0459(8) Uani 1 1 d . . . O3 O 0.2266(3) 0.17770(9) 0.8806(2) 0.0434(8) Uani 1 1 d . B . O4 O 0.5389(10) 0.0450(4) 0.3282(7) 0.297(7) Uani 1 1 d . . . O5 O -0.2057(8) 0.1801(4) 0.2466(6) 0.189(4) Uani 1 1 d . . . O6 O -0.0095(7) 0.0263(3) 0.3080(8) 0.206(4) Uani 1 1 d . . . N1 N 0.4246(3) 0.09253(10) 0.9186(2) 0.0325(8) Uani 1 1 d . . . N2 N 0.5867(3) 0.09896(10) 0.8578(2) 0.0324(8) Uani 1 1 d . . . N3 N 0.3352(3) 0.22181(10) 0.7266(2) 0.0349(9) Uani 1 1 d . . . N4 N 0.4753(3) 0.18163(11) 0.6842(2) 0.0330(8) Uani 1 1 d . . . C1 C 0.3754(4) 0.06931(13) 0.9737(3) 0.0329(10) Uani 1 1 d . . . C2 C 0.3768(4) 0.08586(15) 1.0536(3) 0.0442(12) Uani 1 1 d . . . C3 C 0.3193(5) 0.06528(17) 1.1046(3) 0.0534(14) Uani 1 1 d . . . H3 H 0.3179 0.0769 1.1577 0.064 Uiso 1 1 calc R . . C4 C 0.2640(5) 0.02835(17) 1.0802(4) 0.0558(15) Uani 1 1 d . . . H4 H 0.2257 0.0145 1.1164 0.067 Uiso 1 1 calc R . . C5 C 0.2650(4) 0.01186(15) 1.0034(4) 0.0495(14) Uani 1 1 d . . . H5 H 0.2263 -0.0135 0.9864 0.059 Uiso 1 1 calc R . . C6 C 0.3216(4) 0.03160(13) 0.9492(3) 0.0375(11) Uani 1 1 d . . . C7 C 0.4396(5) 0.12609(17) 1.0817(3) 0.0598(15) Uani 1 1 d . . . H7A H 0.4214 0.1351 1.1339 0.090 Uiso 1 1 calc R . . H7B H 0.4044 0.1454 1.0344 0.090 Uiso 1 1 calc R . . H7C H 0.5336 0.1238 1.0952 0.090 Uiso 1 1 calc R . . C8 C 0.3234(5) 0.01223(16) 0.8662(3) 0.0588(14) Uani 1 1 d . . . H8A H 0.3003 0.0319 0.8189 0.088 Uiso 1 1 calc R . . H8B H 0.2606 -0.0097 0.8509 0.088 Uiso 1 1 calc R . . H8C H 0.4104 0.0018 0.8746 0.088 Uiso 1 1 calc R . . C9 C 0.7127(4) 0.08631(13) 0.8628(3) 0.0350(11) Uani 1 1 d . . . C10 C 0.7313(4) 0.07145(13) 0.7867(3) 0.0396(11) Uani 1 1 d . . . C11 C 0.8547(5) 0.05918(15) 0.7906(4) 0.0541(14) Uani 1 1 d . . . H11 H 0.8678 0.0496 0.7391 0.065 Uiso 1 1 calc R . . C12 C 0.9574(5) 0.06067(17) 0.8670(5) 0.0637(17) Uani 1 1 d . . . H12 H 1.0403 0.0515 0.8686 0.076 Uiso 1 1 calc R . . C13 C 0.9409(4) 0.07533(16) 0.9411(4) 0.0589(16) Uani 1 1 d . . . H13 H 1.0131 0.0763 0.9938 0.071 Uiso 1 1 calc R . . C14 C 0.8184(4) 0.08905(14) 0.9408(3) 0.0435(12) Uani 1 1 d . . . C15 C 0.6170(5) 0.06795(16) 0.7037(3) 0.0511(13) Uani 1 1 d . . . H15A H 0.5543 0.0490 0.7124 0.077 Uiso 1 1 calc R . . H15B H 0.6466 0.0585 0.6564 0.077 Uiso 1 1 calc R . . H15C H 0.5756 0.0941 0.6882 0.077 Uiso 1 1 calc R . . C16 C 0.8048(5) 0.10648(16) 1.0229(3) 0.0569(14) Uani 1 1 d . . . H16A H 0.7356 0.1265 1.0072 0.085 Uiso 1 1 calc R . . H16B H 0.8867 0.1190 1.0578 0.085 Uiso 1 1 calc R . . H16C H 0.7830 0.0853 1.0571 0.085 Uiso 1 1 calc R . . C17 C 0.5356(4) 0.08082(13) 0.9107(3) 0.0303(10) Uani 1 1 d . . . H17 H 0.5798 0.0587 0.9442 0.036 Uiso 1 1 calc R . . C18 C 0.2695(4) 0.25846(13) 0.7160(3) 0.0339(10) Uani 1 1 d . . . C19 C 0.1320(4) 0.25823(15) 0.6895(3) 0.0430(12) Uani 1 1 d . . . C20 C 0.0672(4) 0.29420(16) 0.6849(3) 0.0491(13) Uani 1 1 d . . . H20 H -0.0247 0.2942 0.6679 0.059 Uiso 1 1 calc R . . C21 C 0.1327(5) 0.32988(17) 0.7043(3) 0.0513(14) Uani 1 1 d . . . H21 H 0.0862 0.3541 0.7006 0.062 Uiso 1 1 calc R . . C22 C 0.2666(5) 0.33015(15) 0.7294(3) 0.0454(12) Uani 1 1 d . . . H22 H 0.3118 0.3548 0.7425 0.054 Uiso 1 1 calc R . . C23 C 0.3365(4) 0.29468(14) 0.7357(3) 0.0361(11) Uani 1 1 d . . . C24 C 0.0597(4) 0.21956(16) 0.6660(4) 0.0555(14) Uani 1 1 d . . . H24A H -0.0332 0.2243 0.6528 0.083 Uiso 1 1 calc R . . H24B H 0.0909 0.2010 0.7152 0.083 Uiso 1 1 calc R . . H24C H 0.0744 0.2081 0.6145 0.083 Uiso 1 1 calc R . . C25 C 0.4825(4) 0.29568(15) 0.7663(3) 0.0455(12) Uani 1 1 d . . . H25A H 0.5172 0.2761 0.8131 0.068 Uiso 1 1 calc R . . H25B H 0.5129 0.3224 0.7884 0.068 Uiso 1 1 calc R . . H25C H 0.5124 0.2892 0.7173 0.068 Uiso 1 1 calc R . . C26 C 0.5237(4) 0.17164(13) 0.6162(3) 0.0331(10) Uani 1 1 d . . . C27 C 0.6585(4) 0.16570(13) 0.6367(3) 0.0385(11) Uani 1 1 d . . . C28 C 0.7062(5) 0.15357(15) 0.5716(3) 0.0506(13) Uani 1 1 d . . . H28 H 0.7970 0.1498 0.5854 0.061 Uiso 1 1 calc R . . C29 C 0.6250(5) 0.14682(17) 0.4873(4) 0.0578(15) Uani 1 1 d . . . H29 H 0.6593 0.1383 0.4437 0.069 Uiso 1 1 calc R . . C30 C 0.4932(5) 0.15255(16) 0.4671(3) 0.0554(14) Uani 1 1 d . . . H30 H 0.4372 0.1481 0.4088 0.066 Uiso 1 1 calc R . . C31 C 0.4398(4) 0.16479(14) 0.5302(3) 0.0399(11) Uani 1 1 d . . . C32 C 0.7474(4) 0.17341(16) 0.7278(3) 0.0465(12) Uani 1 1 d . . . H32A H 0.8370 0.1677 0.7315 0.070 Uiso 1 1 calc R . . H32B H 0.7233 0.1562 0.7686 0.070 Uiso 1 1 calc R . . H32C H 0.7404 0.2014 0.7429 0.070 Uiso 1 1 calc R . . C33 C 0.2941(4) 0.16901(16) 0.5034(3) 0.0510(13) Uani 1 1 d . . . H33A H 0.2695 0.1967 0.4866 0.077 Uiso 1 1 calc R . . H33B H 0.2656 0.1616 0.5525 0.077 Uiso 1 1 calc R . . H33C H 0.2526 0.1514 0.4536 0.077 Uiso 1 1 calc R . . C34 C 0.4015(4) 0.21351(13) 0.6743(3) 0.0332(10) Uani 1 1 d . . . H34 H 0.3959 0.2312 0.6275 0.040 Uiso 1 1 calc R . . C35 C 0.5546(5) 0.22264(19) 1.0054(4) 0.0694(17) Uani 1 1 d . . . H35A H 0.5141 0.2074 1.0417 0.083 Uiso 1 1 calc R . . H35B H 0.5030 0.2471 0.9840 0.083 Uiso 1 1 calc R . . C36 C 0.6876(6) 0.2327(2) 1.0556(4) 0.0782(19) Uani 1 1 d . . . H36A H 0.7267 0.2121 1.1002 0.094 Uiso 1 1 calc R . . H36B H 0.6918 0.2587 1.0854 0.094 Uiso 1 1 calc R . . C37 C 0.7548(6) 0.2347(2) 0.9921(4) 0.082(2) Uani 1 1 d . . . H37A H 0.8454 0.2253 1.0182 0.098 Uiso 1 1 calc R . . H37B H 0.7558 0.2624 0.9711 0.098 Uiso 1 1 calc R . . C38 C 0.6802(4) 0.20811(15) 0.9185(3) 0.0441(12) Uani 1 1 d . . . H38A H 0.6626 0.2218 0.8617 0.053 Uiso 1 1 calc R . . H38B H 0.7297 0.1834 0.9183 0.053 Uiso 1 1 calc R . . C39 C 0.0997(5) 0.1051(2) 0.6899(4) 0.0766(19) Uani 1 1 d . . . H39A H 0.0511 0.1300 0.6903 0.092 Uiso 1 1 calc R . . H39B H 0.0979 0.0883 0.7395 0.092 Uiso 1 1 calc R . . C40 C 0.0414(6) 0.0841(2) 0.6081(5) 0.101(3) Uani 1 1 d . . . H40A H -0.0131 0.0618 0.6159 0.122 Uiso 1 1 calc R . . H40B H -0.0136 0.1023 0.5627 0.122 Uiso 1 1 calc R . . C41 C 0.1446(7) 0.0696(3) 0.5838(6) 0.146(4) Uani 1 1 d . . . H41A H 0.1351 0.0786 0.5238 0.175 Uiso 1 1 calc R . . H41B H 0.1447 0.0401 0.5844 0.175 Uiso 1 1 calc R . . C42 C 0.2687(5) 0.08493(17) 0.6468(4) 0.0610(15) Uani 1 1 d . . . H42A H 0.3184 0.0632 0.6846 0.073 Uiso 1 1 calc R . . H42B H 0.3230 0.0971 0.6155 0.073 Uiso 1 1 calc R . . C43 C 0.2040(5) 0.21736(15) 0.9050(4) 0.0605(15) Uani 1 1 d . . . H43A H 0.2846 0.2334 0.9202 0.073 Uiso 1 1 calc R A 1 H43B H 0.1361 0.2307 0.8565 0.073 Uiso 1 1 calc R A 1 C44A C 0.1634(16) 0.2130(3) 0.9782(8) 0.056(4) Uani 0.61(2) 1 d P B 1 H44A H 0.1060 0.2354 0.9814 0.067 Uiso 0.61(2) 1 calc PR B 1 H44B H 0.2390 0.2125 1.0329 0.067 Uiso 0.61(2) 1 calc PR B 1 C44B C 0.0847(19) 0.2163(4) 0.9296(14) 0.044(5) Uani 0.39(2) 1 d P B 2 H44C H 0.0057 0.2208 0.8783 0.052 Uiso 0.39(2) 1 calc PR B 2 H44D H 0.0882 0.2363 0.9753 0.052 Uiso 0.39(2) 1 calc PR B 2 C45 C 0.0897(6) 0.17341(19) 0.9648(4) 0.0756(18) Uani 1 1 d . . . H45A H 0.1109 0.1585 1.0206 0.091 Uiso 1 1 calc R B 1 H45B H -0.0052 0.1778 0.9411 0.091 Uiso 1 1 calc R B 1 C46 C 0.1356(4) 0.15152(15) 0.9009(3) 0.0454(12) Uani 1 1 d . B . H46A H 0.1786 0.1263 0.9267 0.055 Uiso 1 1 calc R . . H46B H 0.0618 0.1452 0.8474 0.055 Uiso 1 1 calc R . . C47 C 0.6473(17) 0.0522(6) 0.3169(9) 0.313(14) Uani 1 1 d . . . H47A H 0.6783 0.0272 0.2980 0.376 Uiso 1 1 calc R . . H47B H 0.6317 0.0716 0.2686 0.376 Uiso 1 1 calc R . . C48 C 0.7325(7) 0.0649(3) 0.3798(7) 0.110(3) Uani 1 1 d . . . H48A H 0.7202 0.0937 0.3874 0.132 Uiso 1 1 calc R . . H48B H 0.8185 0.0609 0.3733 0.132 Uiso 1 1 calc R . . C49 C 0.7231(8) 0.0436(2) 0.4499(6) 0.128(4) Uani 1 1 d . . . H49A H 0.7470 0.0603 0.5032 0.154 Uiso 1 1 calc R . . H49B H 0.7806 0.0200 0.4616 0.154 Uiso 1 1 calc R . . C50 C 0.5860(9) 0.0314(3) 0.4238(6) 0.135(3) Uani 1 1 d . . . H50A H 0.5398 0.0454 0.4584 0.162 Uiso 1 1 calc R . . H50B H 0.5769 0.0023 0.4290 0.162 Uiso 1 1 calc R . . C51 C -0.1569(9) 0.2055(3) 0.3134(6) 0.109(3) Uani 1 1 d . . . H51A H -0.2283 0.2190 0.3270 0.131 Uiso 1 1 calc R . . H51B H -0.1036 0.2260 0.2976 0.131 Uiso 1 1 calc R . . C52 C -0.0712(7) 0.1813(3) 0.3951(6) 0.139(4) Uani 1 1 d . . . H52A H 0.0200 0.1906 0.4153 0.167 Uiso 1 1 calc R . . H52B H -0.1059 0.1829 0.4440 0.167 Uiso 1 1 calc R . . C53 C -0.0832(7) 0.1405(3) 0.3582(6) 0.108(3) Uani 1 1 d . . . H53A H -0.0015 0.1321 0.3497 0.129 Uiso 1 1 calc R . . H53B H -0.1053 0.1211 0.3970 0.129 Uiso 1 1 calc R . . C54 C -0.1895(13) 0.1439(4) 0.2735(9) 0.165(6) Uani 1 1 d . . . H54A H -0.1694 0.1272 0.2295 0.198 Uiso 1 1 calc R . . H54B H -0.2709 0.1339 0.2800 0.198 Uiso 1 1 calc R . . C55 C 0.1012(8) 0.0179(3) 0.3782(4) 0.101(3) Uani 1 1 d . . . H55A H 0.0861 0.0242 0.4337 0.121 Uiso 1 1 calc R . . H55B H 0.1219 -0.0108 0.3784 0.121 Uiso 1 1 calc R . . C56 C 0.2009(10) 0.0396(4) 0.3723(6) 0.179(6) Uani 1 1 d . . . H56A H 0.2746 0.0216 0.3766 0.215 Uiso 1 1 calc R . . H56B H 0.2293 0.0584 0.4221 0.215 Uiso 1 1 calc R . . C57 C 0.1705(8) 0.0602(3) 0.2972(7) 0.136(4) Uani 1 1 d . . . H57A H 0.2299 0.0531 0.2650 0.164 Uiso 1 1 calc R . . H57B H 0.1779 0.0892 0.3093 0.164 Uiso 1 1 calc R . . C58 C 0.0327(11) 0.0495(3) 0.2439(6) 0.130(4) Uani 1 1 d . . . H58A H -0.0213 0.0736 0.2240 0.156 Uiso 1 1 calc R . . H58B H 0.0292 0.0331 0.1925 0.156 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sr1 0.02388(18) 0.0263(2) 0.0313(2) 0.00241(19) 0.01136(14) 0.00084(18) O1 0.0441(18) 0.051(2) 0.047(2) -0.0195(16) 0.0177(15) -0.0151(16) O2 0.0304(16) 0.056(2) 0.0482(19) -0.0094(16) 0.0093(14) -0.0087(15) O3 0.0478(18) 0.034(2) 0.063(2) 0.0060(16) 0.0381(16) 0.0032(15) O4 0.191(9) 0.416(18) 0.186(9) 0.113(10) -0.067(7) -0.083(10) O5 0.099(5) 0.336(16) 0.141(7) -0.022(9) 0.051(5) 0.023(8) O6 0.130(6) 0.178(8) 0.314(12) 0.058(8) 0.079(7) 0.026(6) N1 0.0336(19) 0.033(2) 0.036(2) 0.0091(16) 0.0193(16) 0.0033(16) N2 0.0277(17) 0.035(2) 0.036(2) 0.0059(16) 0.0127(16) 0.0043(15) N3 0.038(2) 0.030(2) 0.043(2) 0.0118(17) 0.0228(18) 0.0102(16) N4 0.0301(18) 0.037(2) 0.036(2) 0.0085(17) 0.0163(16) 0.0065(16) C1 0.024(2) 0.035(3) 0.041(3) 0.013(2) 0.0111(19) 0.0076(18) C2 0.044(3) 0.047(3) 0.047(3) 0.009(2) 0.022(2) 0.003(2) C3 0.062(3) 0.062(4) 0.050(3) 0.017(3) 0.037(3) 0.010(3) C4 0.053(3) 0.051(4) 0.076(4) 0.030(3) 0.039(3) 0.011(3) C5 0.033(2) 0.039(3) 0.077(4) 0.024(3) 0.020(2) 0.000(2) C6 0.025(2) 0.031(3) 0.054(3) 0.007(2) 0.009(2) 0.0031(19) C7 0.076(4) 0.063(4) 0.052(3) -0.013(3) 0.038(3) -0.014(3) C8 0.062(3) 0.048(3) 0.061(3) -0.006(3) 0.013(3) -0.010(3) C9 0.028(2) 0.029(3) 0.049(3) 0.014(2) 0.014(2) 0.0022(18) C10 0.038(3) 0.029(3) 0.061(3) 0.012(2) 0.029(2) 0.004(2) C11 0.044(3) 0.041(3) 0.092(4) 0.021(3) 0.043(3) 0.011(2) C12 0.034(3) 0.061(4) 0.108(5) 0.031(4) 0.039(3) 0.012(3) C13 0.027(2) 0.053(4) 0.089(4) 0.031(3) 0.009(3) -0.003(2) C14 0.034(2) 0.040(3) 0.056(3) 0.016(2) 0.014(2) -0.002(2) C15 0.054(3) 0.053(4) 0.054(3) 0.000(2) 0.028(3) 0.005(2) C16 0.051(3) 0.051(4) 0.058(3) 0.010(3) 0.004(3) -0.009(3) C17 0.028(2) 0.029(2) 0.033(2) 0.0066(19) 0.0086(18) 0.0035(18) C18 0.041(2) 0.035(3) 0.034(2) 0.011(2) 0.023(2) 0.010(2) C19 0.040(3) 0.050(3) 0.044(3) 0.007(2) 0.020(2) 0.007(2) C20 0.036(3) 0.058(4) 0.056(3) 0.007(3) 0.019(2) 0.020(2) C21 0.057(3) 0.046(3) 0.052(3) 0.009(2) 0.021(3) 0.026(3) C22 0.055(3) 0.037(3) 0.044(3) 0.006(2) 0.017(2) 0.006(2) C23 0.041(2) 0.038(3) 0.035(3) 0.009(2) 0.021(2) 0.009(2) C24 0.033(3) 0.057(4) 0.078(4) 0.007(3) 0.020(3) 0.006(2) C25 0.046(3) 0.044(3) 0.049(3) 0.004(2) 0.020(2) 0.000(2) C26 0.041(2) 0.026(2) 0.041(3) 0.009(2) 0.024(2) 0.0059(19) C27 0.035(2) 0.039(3) 0.048(3) 0.004(2) 0.021(2) 0.0028(19) C28 0.046(3) 0.053(3) 0.063(3) 0.002(3) 0.032(3) 0.008(3) C29 0.063(3) 0.072(4) 0.051(3) -0.008(3) 0.035(3) 0.002(3) C30 0.064(3) 0.061(4) 0.040(3) -0.009(3) 0.016(2) -0.004(3) C31 0.042(3) 0.040(3) 0.041(3) 0.001(2) 0.018(2) 0.002(2) C32 0.031(2) 0.054(3) 0.058(3) -0.002(3) 0.020(2) -0.001(2) C33 0.047(3) 0.049(3) 0.052(3) 0.000(2) 0.010(2) 0.003(2) C34 0.031(2) 0.034(3) 0.036(3) 0.011(2) 0.0132(19) 0.0033(19) C35 0.071(4) 0.073(4) 0.074(4) -0.030(3) 0.038(3) -0.022(3) C36 0.067(4) 0.098(5) 0.064(4) -0.034(4) 0.014(3) -0.021(4) C37 0.066(4) 0.118(6) 0.069(4) -0.030(4) 0.034(3) -0.041(4) C38 0.040(3) 0.050(3) 0.046(3) 0.000(2) 0.020(2) -0.003(2) C39 0.047(3) 0.080(5) 0.110(5) -0.036(4) 0.035(3) -0.017(3) C40 0.057(4) 0.126(7) 0.105(6) -0.041(5) 0.004(4) -0.027(4) C41 0.089(6) 0.178(10) 0.178(9) -0.129(8) 0.055(6) -0.053(6) C42 0.053(3) 0.056(4) 0.078(4) -0.001(3) 0.027(3) 0.007(3) C43 0.074(4) 0.034(3) 0.092(4) 0.001(3) 0.052(3) 0.010(3) C44A 0.077(9) 0.053(6) 0.042(7) -0.010(5) 0.025(6) 0.002(5) C44B 0.047(10) 0.043(9) 0.051(12) -0.011(7) 0.029(9) 0.015(7) C45 0.086(4) 0.074(5) 0.096(5) -0.008(4) 0.069(4) -0.011(4) C46 0.039(2) 0.045(3) 0.061(3) 0.005(3) 0.028(2) -0.003(2) C47 0.33(2) 0.51(3) 0.181(13) -0.218(17) 0.204(14) -0.33(2) C48 0.060(4) 0.132(8) 0.154(8) -0.027(7) 0.059(5) -0.019(5) C49 0.112(7) 0.072(6) 0.138(8) 0.014(5) -0.042(6) -0.002(5) C50 0.145(8) 0.146(9) 0.120(7) -0.005(6) 0.051(6) -0.066(7) C51 0.109(7) 0.108(7) 0.123(7) -0.008(6) 0.057(6) 0.034(5) C52 0.068(5) 0.187(11) 0.137(8) -0.048(8) 0.000(5) 0.025(6) C53 0.078(5) 0.119(7) 0.114(6) -0.011(5) 0.016(4) 0.027(5) C54 0.138(10) 0.171(13) 0.146(11) -0.045(9) -0.007(8) 0.014(9) C55 0.096(5) 0.154(8) 0.044(4) 0.011(4) 0.012(4) -0.058(5) C56 0.135(8) 0.266(15) 0.114(7) 0.057(8) 0.012(6) -0.103(9) C57 0.105(7) 0.157(9) 0.160(9) 0.078(7) 0.062(7) 0.001(6) C58 0.169(10) 0.079(6) 0.104(6) 0.002(5) -0.004(6) 0.028(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sr1 O1 2.571(3) . ? Sr1 O2 2.586(3) . ? Sr1 O3 2.630(3) . ? Sr1 N1 2.631(3) . ? Sr1 N2 2.642(3) . ? Sr1 N3 2.652(3) . ? Sr1 N4 2.657(3) . ? Sr1 C17 3.009(4) . ? Sr1 C34 3.020(4) . ? O1 C35 1.431(6) . ? O1 C38 1.444(5) . ? O2 C39 1.422(6) . ? O2 C42 1.433(6) . ? O3 C43 1.433(6) . ? O3 C46 1.446(5) . ? O4 C47 1.282(14) . ? O4 C50 1.531(11) . ? O5 C54 1.282(14) . ? O5 C51 1.341(11) . ? O6 C55 1.386(10) . ? O6 C58 1.491(11) . ? N1 C17 1.322(5) . ? N1 C1 1.422(5) . ? N2 C17 1.321(5) . ? N2 C9 1.418(5) . ? N3 C34 1.319(5) . ? N3 C18 1.405(5) . ? N4 C34 1.317(5) . ? N4 C26 1.415(5) . ? C1 C6 1.396(6) . ? C1 C2 1.405(6) . ? C2 C3 1.381(6) . ? C2 C7 1.514(7) . ? C3 C4 1.377(7) . ? C4 C5 1.368(7) . ? C5 C6 1.401(6) . ? C6 C8 1.501(7) . ? C9 C14 1.402(6) . ? C9 C10 1.409(6) . ? C10 C11 1.393(6) . ? C10 C15 1.504(6) . ? C11 C12 1.367(8) . ? C12 C13 1.365(8) . ? C13 C14 1.415(7) . ? C14 C16 1.509(7) . ? C18 C23 1.400(6) . ? C18 C19 1.419(6) . ? C19 C20 1.389(7) . ? C19 C24 1.501(7) . ? C20 C21 1.376(7) . ? C21 C22 1.383(6) . ? C22 C23 1.400(6) . ? C23 C25 1.505(6) . ? C26 C31 1.408(6) . ? C26 C27 1.412(6) . ? C27 C28 1.388(6) . ? C27 C32 1.494(6) . ? C28 C29 1.376(7) . ? C29 C30 1.381(7) . ? C30 C31 1.400(7) . ? C31 C33 1.512(6) . ? C35 C36 1.450(7) . ? C36 C37 1.456(8) . ? C37 C38 1.494(7) . ? C39 C40 1.449(8) . ? C40 C41 1.403(9) . ? C41 C42 1.491(8) . ? C43 C44A 1.408(10) . ? C43 C44B 1.489(14) . ? C44A C45 1.532(11) . ? C44B C45 1.542(16) . ? C45 C46 1.489(7) . ? C47 C48 1.206(12) . ? C48 C49 1.378(10) . ? C49 C50 1.472(11) . ? C51 C52 1.568(11) . ? C52 C53 1.482(11) . ? C53 C54 1.478(13) . ? C55 C56 1.341(9) . ? C56 C57 1.344(10) . ? C57 C58 1.508(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 O1 Sr1 O2 174.33(10) . . ? O1 Sr1 O3 85.53(10) . . ? O2 Sr1 O3 89.37(10) . . ? O1 Sr1 N1 95.27(11) . . ? O2 Sr1 N1 86.62(11) . . ? O3 Sr1 N1 83.80(10) . . ? O1 Sr1 N2 87.88(11) . . ? O2 Sr1 N2 97.47(10) . . ? O3 Sr1 N2 134.40(10) . . ? N1 Sr1 N2 51.97(10) . . ? O1 Sr1 N3 84.67(11) . . ? O2 Sr1 N3 92.12(11) . . ? O3 Sr1 N3 81.30(10) . . ? N1 Sr1 N3 165.06(10) . . ? N2 Sr1 N3 142.79(11) . . ? O1 Sr1 N4 95.76(10) . . ? O2 Sr1 N4 85.85(10) . . ? O3 Sr1 N4 132.37(10) . . ? N1 Sr1 N4 142.85(11) . . ? N2 Sr1 N4 93.17(10) . . ? N3 Sr1 N4 51.65(11) . . ? O1 Sr1 C17 90.70(11) . . ? O2 Sr1 C17 93.30(11) . . ? O3 Sr1 C17 108.99(10) . . ? N1 Sr1 C17 26.01(10) . . ? N2 Sr1 C17 26.00(10) . . ? N3 Sr1 C17 168.41(11) . . ? N4 Sr1 C17 118.59(11) . . ? O1 Sr1 C34 91.17(11) . . ? O2 Sr1 C34 87.93(11) . . ? O3 Sr1 C34 106.75(10) . . ? N1 Sr1 C34 168.07(11) . . ? N2 Sr1 C34 118.47(11) . . ? N3 Sr1 C34 25.86(10) . . ? N4 Sr1 C34 25.83(10) . . ? C17 Sr1 C34 144.25(11) . . ? C35 O1 C38 108.0(3) . . ? C35 O1 Sr1 137.0(3) . . ? C38 O1 Sr1 114.2(2) . . ? C39 O2 C42 106.5(4) . . ? C39 O2 Sr1 130.3(3) . . ? C42 O2 Sr1 119.7(3) . . ? C43 O3 C46 107.8(3) . . ? C43 O3 Sr1 127.3(3) . . ? C46 O3 Sr1 124.8(3) . . ? C47 O4 C50 100.8(10) . . ? C54 O5 C51 110.7(12) . . ? C55 O6 C58 106.9(7) . . ? C17 N1 C1 116.8(3) . . ? C17 N1 Sr1 93.2(2) . . ? C1 N1 Sr1 150.0(3) . . ? C17 N2 C9 116.1(3) . . ? C17 N2 Sr1 92.7(2) . . ? C9 N2 Sr1 149.2(3) . . ? C34 N3 C18 118.3(3) . . ? C34 N3 Sr1 92.9(2) . . ? C18 N3 Sr1 148.8(3) . . ? C34 N4 C26 118.1(3) . . ? C34 N4 Sr1 92.7(3) . . ? C26 N4 Sr1 145.9(3) . . ? C6 C1 C2 119.7(4) . . ? C6 C1 N1 122.0(4) . . ? C2 C1 N1 118.3(4) . . ? C3 C2 C1 119.3(5) . . ? C3 C2 C7 121.1(5) . . ? C1 C2 C7 119.7(4) . . ? C4 C3 C2 121.5(5) . . ? C5 C4 C3 119.3(5) . . ? C4 C5 C6 121.4(5) . . ? C1 C6 C5 118.8(5) . . ? C1 C6 C8 121.2(4) . . ? C5 C6 C8 120.0(5) . . ? C14 C9 C10 119.8(4) . . ? C14 C9 N2 121.6(4) . . ? C10 C9 N2 118.6(4) . . ? C11 C10 C9 119.2(5) . . ? C11 C10 C15 121.3(5) . . ? C9 C10 C15 119.5(4) . . ? C12 C11 C10 121.3(5) . . ? C13 C12 C11 120.1(5) . . ? C12 C13 C14 121.2(5) . . ? C9 C14 C13 118.4(5) . . ? C9 C14 C16 121.8(4) . . ? C13 C14 C16 119.8(5) . . ? N2 C17 N1 121.9(4) . . ? N2 C17 Sr1 61.3(2) . . ? N1 C17 Sr1 60.8(2) . . ? C23 C18 N3 121.6(4) . . ? C23 C18 C19 119.6(4) . . ? N3 C18 C19 118.6(4) . . ? C20 C19 C18 118.8(5) . . ? C20 C19 C24 121.5(4) . . ? C18 C19 C24 119.7(4) . . ? C21 C20 C19 121.8(4) . . ? C20 C21 C22 119.4(5) . . ? C21 C22 C23 121.0(5) . . ? C18 C23 C22 119.3(4) . . ? C18 C23 C25 120.7(4) . . ? C22 C23 C25 119.9(4) . . ? C31 C26 C27 119.5(4) . . ? C31 C26 N4 121.4(4) . . ? C27 C26 N4 118.9(4) . . ? C28 C27 C26 119.4(4) . . ? C28 C27 C32 121.1(4) . . ? C26 C27 C32 119.4(4) . . ? C29 C28 C27 121.5(4) . . ? C28 C29 C30 119.2(5) . . ? C29 C30 C31 121.6(5) . . ? C30 C31 C26 118.7(4) . . ? C30 C31 C33 118.3(4) . . ? C26 C31 C33 123.0(4) . . ? N4 C34 N3 122.7(4) . . ? N4 C34 Sr1 61.5(2) . . ? N3 C34 Sr1 61.3(2) . . ? O1 C35 C36 106.2(4) . . ? C35 C36 C37 105.2(5) . . ? C36 C37 C38 105.6(4) . . ? O1 C38 C37 106.1(4) . . ? O2 C39 C40 107.8(5) . . ? C41 C40 C39 106.1(5) . . ? C40 C41 C42 108.7(6) . . ? O2 C42 C41 104.8(5) . . ? C44A C43 O3 105.6(6) . . ? C44A C43 C44B 38.5(6) . . ? O3 C43 C44B 107.4(6) . . ? C43 C44A C45 105.7(7) . . ? C43 C44B C45 101.3(9) . . ? C46 C45 C44A 104.0(5) . . ? C46 C45 C44B 100.4(7) . . ? C44A C45 C44B 36.3(6) . . ? O3 C46 C45 106.1(4) . . ? C48 C47 O4 115.8(10) . . ? C47 C48 C49 105.3(10) . . ? C48 C49 C50 104.9(7) . . ? C49 C50 O4 100.0(7) . . ? O5 C51 C52 108.6(9) . . ? C53 C52 C51 100.9(7) . . ? C54 C53 C52 103.9(8) . . ? O5 C54 C53 111.5(12) . . ? C56 C55 O6 109.7(7) . . ? C55 C56 C57 112.7(8) . . ? C56 C57 C58 107.0(8) . . ? O6 C58 C57 102.0(7) . . ? _diffrn_measured_fraction_theta_max 0.923 _diffrn_reflns_theta_full 28.24 _diffrn_measured_fraction_theta_full 0.923 _refine_diff_density_max 0.611 _refine_diff_density_min -0.571 _refine_diff_density_rms 0.077 _chemical_compound_source THF #===END data_COMPOUND_6 _database_code_depnum_ccdc_archive 'CCDC 298098' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point 408-413 _chemical_formula_moiety 'C70 H78 N4 O5 Sr' _chemical_formula_sum 'C70 H78 N4 O5 Sr' _chemical_formula_weight 1142.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sr Sr -1.5307 3.2498 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c c n' _symmetry_int_tables_number 56 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' 'x+1/2, -y, -z+1/2' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' '-x-1/2, y, z-1/2' 'x, -y-1/2, z-1/2' _cell_length_a 26.6486(4) _cell_length_b 10.17120(10) _cell_length_c 21.9266(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5943.17(13) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'rectangular block' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.277 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2416 _exptl_absorpt_coefficient_mu 0.962 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6714 _exptl_absorpt_correction_T_max 0.9357 _exptl_absorpt_process_details 'performed as part of the DENZO-SMN package' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'psi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 49571 _diffrn_reflns_av_R_equivalents 0.1274 _diffrn_reflns_av_sigmaI/netI 0.0881 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6710 _reflns_number_gt 4107 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction X-Seed _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed / POV-Ray' _computing_publication_material 'Microsoft Office 2000' _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^)+(0.0448P)^2^+11.6459P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6710 _refine_ls_number_parameters 390 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1442 _refine_ls_R_factor_gt 0.0783 _refine_ls_wR_factor_ref 0.1606 _refine_ls_wR_factor_gt 0.1374 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sr1 Sr 0.7500 0.7500 0.78833(2) 0.02849(16) Uani 1 2 d S . . O1 O 0.80948(12) 0.9409(3) 0.81307(14) 0.0423(8) Uani 1 1 d . . . O2 O 0.7500 0.7500 0.90792(16) 0.0431(11) Uani 1 2 d S . . O3 O 0.9600(3) 0.6641(7) 0.4357(3) 0.074(3) Uani 0.602(6) 1 d P A 1 O4 O 0.9973(3) 0.6935(10) 0.5296(4) 0.062(3) Uani 0.398(6) 1 d P A 2 N1 N 0.82394(13) 0.5804(3) 0.80996(14) 0.0306(8) Uani 1 1 d . . . N2 N 0.79257(11) 0.5746(3) 0.71143(14) 0.0289(8) Uani 1 1 d . . . C1 C 0.85359(16) 0.5128(4) 0.85368(18) 0.0312(10) Uani 1 1 d . . . C2 C 0.90250(16) 0.4629(4) 0.84260(19) 0.0353(11) Uani 1 1 d . . . C3 C 0.92638(17) 0.3925(5) 0.8891(2) 0.0445(12) Uani 1 1 d . . . H3 H 0.9587 0.3567 0.8814 0.053 Uiso 1 1 calc R . . C4 C 0.90493(19) 0.3728(5) 0.9453(2) 0.0469(13) Uani 1 1 d . . . H4 H 0.9221 0.3243 0.9759 0.056 Uiso 1 1 calc R . . C5 C 0.85809(19) 0.4246(4) 0.9568(2) 0.0422(11) Uani 1 1 d . . . H5 H 0.8432 0.4132 0.9958 0.051 Uiso 1 1 calc R . . C6 C 0.83250(18) 0.4934(4) 0.91171(18) 0.0361(11) Uani 1 1 d . . . H6 H 0.8001 0.5280 0.9203 0.043 Uiso 1 1 calc R . . C7 C 0.93013(15) 0.4843(5) 0.78453(19) 0.0369(11) Uani 1 1 d . . . C8 C 0.93815(16) 0.6105(5) 0.7610(2) 0.0399(11) Uani 1 1 d . . . H8 H 0.9248 0.6849 0.7817 0.048 Uiso 1 1 calc R . . C9 C 0.96549(16) 0.6277(6) 0.7076(2) 0.0487(13) Uani 1 1 d . . . H9 H 0.9709 0.7138 0.6922 0.058 Uiso 1 1 calc R . . C10 C 0.98493(16) 0.5202(6) 0.6764(2) 0.0531(14) Uani 1 1 d . . . H10 H 1.0033 0.5321 0.6397 0.064 Uiso 1 1 calc R . . C11 C 0.97707(17) 0.3957(6) 0.6998(2) 0.0520(14) Uani 1 1 d . . . H11 H 0.9903 0.3216 0.6789 0.062 Uiso 1 1 calc R . . C12 C 0.95010(15) 0.3772(5) 0.7532(2) 0.0446(12) Uani 1 1 d . . . H12 H 0.9452 0.2908 0.7686 0.054 Uiso 1 1 calc R . . C13 C 0.79931(15) 0.5164(4) 0.65378(17) 0.0270(9) Uani 1 1 d . . . C14 C 0.75777(15) 0.4770(4) 0.61776(16) 0.0276(9) Uani 1 1 d . . . C15 C 0.76695(16) 0.4175(4) 0.56150(18) 0.0303(10) Uani 1 1 d . . . H15 H 0.7392 0.3905 0.5373 0.036 Uiso 1 1 calc R . . C16 C 0.81510(16) 0.3963(4) 0.53979(19) 0.0338(10) Uani 1 1 d . . . H16 H 0.8201 0.3558 0.5012 0.041 Uiso 1 1 calc R . . C17 C 0.85558(17) 0.4345(4) 0.57443(19) 0.0368(11) Uani 1 1 d . . . H17 H 0.8888 0.4206 0.5600 0.044 Uiso 1 1 calc R . . C18 C 0.84760(15) 0.4934(4) 0.63061(18) 0.0314(10) Uani 1 1 d . . . H18 H 0.8758 0.5191 0.6543 0.038 Uiso 1 1 calc R . . C19 C 0.70499(15) 0.4933(4) 0.63730(17) 0.0282(9) Uani 1 1 d . . . C20 C 0.68517(15) 0.6162(4) 0.65233(17) 0.0325(10) Uani 1 1 d . . . H20 H 0.7067 0.6906 0.6534 0.039 Uiso 1 1 calc R . . C21 C 0.63486(16) 0.6321(5) 0.6657(2) 0.0390(11) Uani 1 1 d . . . H21 H 0.6221 0.7169 0.6751 0.047 Uiso 1 1 calc R . . C22 C 0.60295(17) 0.5243(5) 0.6654(2) 0.0448(12) Uani 1 1 d . . . H22 H 0.5684 0.5349 0.6746 0.054 Uiso 1 1 calc R . . C23 C 0.62189(17) 0.4016(5) 0.6517(2) 0.0465(13) Uani 1 1 d . . . H23 H 0.6003 0.3273 0.6517 0.056 Uiso 1 1 calc R . . C24 C 0.67224(16) 0.3863(4) 0.63787(18) 0.0367(11) Uani 1 1 d . . . H24 H 0.6848 0.3012 0.6286 0.044 Uiso 1 1 calc R . . C25 C 0.82187(14) 0.5268(4) 0.75492(17) 0.0263(9) Uani 1 1 d . . . H25 H 0.8420 0.4519 0.7464 0.032 Uiso 1 1 calc R . . C26 C 0.79244(18) 1.0753(4) 0.8123(2) 0.0466(12) Uani 1 1 d . . . H26A H 0.7659 1.0885 0.8432 0.056 Uiso 1 1 calc R . . H26B H 0.7786 1.0976 0.7717 0.056 Uiso 1 1 calc R . . C27 C 0.83624(19) 1.1593(5) 0.8261(3) 0.0639(16) Uani 1 1 d . . . H27A H 0.8266 1.2336 0.8528 0.077 Uiso 1 1 calc R . . H27B H 0.8513 1.1947 0.7882 0.077 Uiso 1 1 calc R . . C28 C 0.87240(18) 1.0680(5) 0.8583(2) 0.0506(13) Uani 1 1 d . . . H28A H 0.9076 1.0965 0.8525 0.061 Uiso 1 1 calc R . . H28B H 0.8651 1.0629 0.9025 0.061 Uiso 1 1 calc R . . C29 C 0.86250(18) 0.9388(4) 0.8272(2) 0.0414(11) Uani 1 1 d . . . H29A H 0.8828 0.9308 0.7896 0.050 Uiso 1 1 calc R . . H29B H 0.8706 0.8644 0.8546 0.050 Uiso 1 1 calc R . . C30 C 0.7098(2) 0.7009(5) 0.94586(19) 0.0468(13) Uani 1 1 d . . . H30A H 0.7089 0.6036 0.9449 0.056 Uiso 1 1 calc R . . H30B H 0.6771 0.7352 0.9318 0.056 Uiso 1 1 calc R . . C31 C 0.72146(18) 0.7499(5) 1.00990(18) 0.0496(12) Uani 1 1 d . . . H31A H 0.7078 0.8392 1.0167 0.059 Uiso 1 1 calc R . . H31B H 0.7079 0.6896 1.0413 0.059 Uiso 1 1 calc R . . C32 C 0.9665(5) 0.7894(12) 0.4430(4) 0.160(5) Uani 0.602(6) 1 d P A 1 H32A H 0.9452 0.8382 0.4137 0.193 Uiso 0.602(6) 1 calc PR A 1 H32B H 1.0019 0.8123 0.4347 0.193 Uiso 0.602(6) 1 calc PR A 1 C33 C 0.9523(3) 0.8309(9) 0.5106(4) 0.053(2) Uani 0.602(6) 1 d P A 1 H33A H 0.9777 0.8912 0.5281 0.064 Uiso 0.602(6) 1 calc PR A 1 H33B H 0.9189 0.8733 0.5123 0.064 Uiso 0.602(6) 1 calc PR A 1 C34 C 0.9522(3) 0.7155(10) 0.5394(3) 0.110(3) Uani 0.602(6) 1 d P A 1 H34A H 0.9253 0.7123 0.5705 0.132 Uiso 0.602(6) 1 calc PR A 1 H34B H 0.9849 0.6991 0.5595 0.132 Uiso 0.602(6) 1 calc PR A 1 C35 C 0.9419(4) 0.6073(9) 0.4848(4) 0.058(3) Uani 0.602(6) 1 d P A 1 H35A H 0.9595 0.5236 0.4933 0.069 Uiso 0.602(6) 1 calc PR A 1 H35B H 0.9055 0.5895 0.4803 0.069 Uiso 0.602(6) 1 calc PR A 1 C36 C 0.9522(3) 0.7155(10) 0.5394(3) 0.110(3) Uani 0.40 1 d P A 2 H36A H 0.9508 0.7909 0.5679 0.132 Uiso 0.398(6) 1 calc PR A 2 H36B H 0.9390 0.6385 0.5619 0.132 Uiso 0.398(6) 1 calc PR A 2 C37 C 0.9176(5) 0.7425(17) 0.4922(7) 0.065(4) Uani 0.398(6) 1 d P A 2 H37A H 0.8942 0.8150 0.5020 0.078 Uiso 0.398(6) 1 calc PR A 2 H37B H 0.8990 0.6638 0.4781 0.078 Uiso 0.398(6) 1 calc PR A 2 C38 C 0.9665(5) 0.7894(12) 0.4430(4) 0.160(5) Uani 0.40 1 d P A 2 H38A H 0.9575 0.7828 0.3992 0.193 Uiso 0.398(6) 1 calc PR A 2 H38B H 0.9805 0.8773 0.4523 0.193 Uiso 0.398(6) 1 calc PR A 2 C39 C 0.9993(6) 0.6768(16) 0.4651(7) 0.060(4) Uani 0.398(6) 1 d P A 2 H39A H 0.9854 0.5906 0.4527 0.072 Uiso 0.398(6) 1 calc PR A 2 H39B H 1.0341 0.6851 0.4497 0.072 Uiso 0.398(6) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sr1 0.0389(3) 0.0304(3) 0.0162(2) 0.000 0.000 -0.0119(3) O1 0.051(2) 0.0370(19) 0.0392(18) 0.0012(14) -0.0105(15) -0.0159(15) O2 0.077(3) 0.036(2) 0.0165(19) 0.000 0.000 -0.010(3) O3 0.131(7) 0.041(4) 0.051(4) 0.011(3) 0.016(5) -0.013(4) O4 0.030(5) 0.090(7) 0.066(7) 0.008(5) -0.013(5) 0.003(5) N1 0.037(2) 0.033(2) 0.0214(17) 0.0019(15) -0.0041(16) -0.0166(16) N2 0.0264(17) 0.040(2) 0.0205(17) 0.0001(16) -0.0013(15) -0.0137(15) C1 0.039(2) 0.029(2) 0.025(2) 0.0018(18) -0.0096(19) -0.0109(19) C2 0.033(2) 0.043(3) 0.030(2) 0.004(2) -0.009(2) -0.015(2) C3 0.037(3) 0.058(3) 0.038(3) 0.005(2) -0.010(2) -0.008(2) C4 0.050(3) 0.056(3) 0.034(3) 0.008(2) -0.014(2) -0.010(3) C5 0.060(3) 0.043(3) 0.024(2) 0.002(2) -0.005(2) -0.019(2) C6 0.047(3) 0.035(3) 0.027(2) -0.0029(19) -0.003(2) -0.013(2) C7 0.025(2) 0.057(3) 0.029(2) 0.005(2) -0.009(2) -0.011(2) C8 0.029(2) 0.053(3) 0.037(2) 0.004(2) -0.010(2) -0.013(2) C9 0.025(2) 0.077(4) 0.044(3) 0.023(3) -0.007(2) -0.020(2) C10 0.023(2) 0.092(5) 0.044(3) 0.014(3) 0.002(2) -0.005(3) C11 0.031(3) 0.079(4) 0.046(3) 0.003(3) 0.002(2) 0.000(3) C12 0.029(2) 0.061(3) 0.044(3) 0.010(3) -0.004(2) -0.004(2) C13 0.029(2) 0.029(2) 0.023(2) -0.0002(17) 0.0010(18) -0.0093(18) C14 0.033(2) 0.029(2) 0.0206(19) 0.0058(16) -0.0009(18) -0.0090(18) C15 0.043(3) 0.027(2) 0.021(2) 0.0021(17) -0.0042(18) -0.0064(18) C16 0.053(3) 0.026(2) 0.023(2) 0.0016(18) 0.007(2) -0.0052(19) C17 0.038(3) 0.038(3) 0.034(2) 0.004(2) 0.011(2) -0.008(2) C18 0.033(2) 0.035(2) 0.026(2) 0.0014(19) -0.0002(19) -0.0132(19) C19 0.035(2) 0.033(2) 0.017(2) -0.0022(17) -0.0068(18) -0.0050(19) C20 0.034(2) 0.043(3) 0.021(2) 0.0003(19) -0.0051(18) -0.016(2) C21 0.034(2) 0.047(3) 0.036(3) -0.005(2) 0.001(2) -0.006(2) C22 0.032(2) 0.061(4) 0.041(3) -0.003(2) -0.001(2) -0.007(2) C23 0.039(3) 0.057(3) 0.043(3) -0.009(2) 0.001(2) -0.026(2) C24 0.044(3) 0.038(3) 0.028(2) -0.0062(19) -0.001(2) -0.017(2) C25 0.020(2) 0.035(2) 0.024(2) 0.0001(18) 0.0022(17) -0.0139(17) C26 0.050(3) 0.035(3) 0.055(3) 0.001(2) -0.014(2) -0.009(2) C27 0.050(3) 0.047(3) 0.095(5) -0.007(3) -0.017(3) -0.009(3) C28 0.048(3) 0.043(3) 0.061(3) -0.013(3) -0.015(3) -0.006(2) C29 0.052(3) 0.037(3) 0.035(3) 0.000(2) -0.008(2) -0.011(2) C30 0.085(4) 0.030(2) 0.025(2) -0.0002(18) 0.010(2) -0.007(3) C31 0.099(4) 0.031(2) 0.0188(19) 0.004(2) 0.005(2) 0.014(3) C32 0.214(12) 0.185(12) 0.083(6) 0.047(7) 0.011(7) 0.031(10) C33 0.046(5) 0.048(6) 0.066(6) -0.001(5) 0.000(5) -0.001(4) C34 0.087(6) 0.181(10) 0.063(5) 0.026(6) -0.002(4) -0.003(6) C35 0.068(6) 0.039(5) 0.066(6) 0.001(5) 0.012(5) -0.009(5) C36 0.087(6) 0.181(10) 0.063(5) 0.026(6) -0.002(4) -0.003(6) C37 0.036(7) 0.077(11) 0.082(10) 0.018(9) -0.008(7) 0.009(8) C38 0.214(12) 0.185(12) 0.083(6) 0.047(7) 0.011(7) 0.031(10) C39 0.045(8) 0.087(11) 0.047(8) -0.017(8) -0.004(7) -0.003(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sr1 O1 2.565(3) 2_665 ? Sr1 O1 2.565(3) . ? Sr1 O2 2.622(4) . ? Sr1 N1 2.661(4) . ? Sr1 N1 2.661(4) 2_665 ? Sr1 N2 2.704(3) 2_665 ? Sr1 N2 2.704(3) . ? Sr1 C25 3.059(4) 2_665 ? Sr1 C25 3.059(4) . ? O1 C26 1.440(5) . ? O1 C29 1.447(5) . ? O2 C30 1.444(5) . ? O2 C30 1.444(5) 2_665 ? O3 C32 1.297(12) . ? O3 C35 1.315(10) . ? O4 C39 1.425(16) . ? N1 C25 1.326(5) . ? N1 C1 1.420(5) . ? N2 C25 1.325(5) . ? N2 C13 1.407(5) . ? C1 C6 1.405(6) . ? C1 C2 1.419(6) . ? C2 C3 1.399(6) . ? C2 C7 1.487(6) . ? C3 C4 1.375(6) . ? C4 C5 1.378(7) . ? C5 C6 1.390(6) . ? C7 C12 1.393(6) . ? C7 C8 1.400(6) . ? C8 C9 1.391(6) . ? C9 C10 1.389(7) . ? C10 C11 1.382(7) . ? C11 C12 1.388(6) . ? C13 C18 1.403(5) . ? C13 C14 1.418(5) . ? C14 C15 1.396(5) . ? C14 C19 1.480(6) . ? C15 C16 1.385(6) . ? C16 C17 1.375(6) . ? C17 C18 1.386(6) . ? C19 C24 1.395(6) . ? C19 C20 1.397(6) . ? C20 C21 1.382(6) . ? C21 C22 1.387(6) . ? C22 C23 1.380(7) . ? C23 C24 1.384(6) . ? C26 C27 1.478(6) . ? C27 C28 1.514(7) . ? C28 C29 1.503(6) . ? C30 C31 1.522(6) . ? C31 C31 1.521(10) 2_665 ? C32 C33 1.587(13) . ? C33 C34 1.332(11) . ? C34 C35 1.649(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 O1 Sr1 O1 155.58(14) 2_665 . ? O1 Sr1 O2 77.79(7) 2_665 . ? O1 Sr1 O2 77.79(7) . . ? O1 Sr1 N1 85.94(10) 2_665 . ? O1 Sr1 N1 89.74(10) . . ? O2 Sr1 N1 79.74(7) . . ? O1 Sr1 N1 89.74(10) 2_665 2_665 ? O1 Sr1 N1 85.94(10) . 2_665 ? O2 Sr1 N1 79.74(7) . 2_665 ? N1 Sr1 N1 159.47(14) . 2_665 ? O1 Sr1 N2 111.85(10) 2_665 2_665 ? O1 Sr1 N2 83.78(9) . 2_665 ? O2 Sr1 N2 128.58(7) . 2_665 ? N1 Sr1 N2 148.13(10) . 2_665 ? N1 Sr1 N2 51.17(10) 2_665 2_665 ? O1 Sr1 N2 83.78(9) 2_665 . ? O1 Sr1 N2 111.85(10) . . ? O2 Sr1 N2 128.58(7) . . ? N1 Sr1 N2 51.17(10) . . ? N1 Sr1 N2 148.13(10) 2_665 . ? N2 Sr1 N2 102.85(14) 2_665 . ? O1 Sr1 C25 103.04(10) 2_665 2_665 ? O1 Sr1 C25 82.85(10) . 2_665 ? O2 Sr1 C25 103.86(7) . 2_665 ? N1 Sr1 C25 170.81(10) . 2_665 ? N1 Sr1 C25 25.60(10) 2_665 2_665 ? N2 Sr1 C25 25.64(9) 2_665 2_665 ? N2 Sr1 C25 127.07(11) . 2_665 ? O1 Sr1 C25 82.85(10) 2_665 . ? O1 Sr1 C25 103.04(10) . . ? O2 Sr1 C25 103.86(7) . . ? N1 Sr1 C25 25.60(10) . . ? N1 Sr1 C25 170.81(10) 2_665 . ? N2 Sr1 C25 127.07(11) 2_665 . ? N2 Sr1 C25 25.64(9) . . ? C25 Sr1 C25 152.29(14) 2_665 . ? C26 O1 C29 108.9(3) . . ? C26 O1 Sr1 121.4(3) . . ? C29 O1 Sr1 129.6(3) . . ? C30 O2 C30 109.7(4) . 2_665 ? C30 O2 Sr1 125.2(2) . . ? C30 O2 Sr1 125.2(2) 2_665 . ? C32 O3 C35 112.3(8) . . ? C25 N1 C1 116.0(4) . . ? C25 N1 Sr1 94.2(3) . . ? C1 N1 Sr1 147.8(3) . . ? C25 N2 C13 114.6(3) . . ? C25 N2 Sr1 92.3(2) . . ? C13 N2 Sr1 153.0(3) . . ? C6 C1 N1 117.2(4) . . ? C6 C1 C2 118.2(4) . . ? N1 C1 C2 124.6(4) . . ? C3 C2 C1 118.4(4) . . ? C3 C2 C7 118.2(4) . . ? C1 C2 C7 123.3(4) . . ? C4 C3 C2 122.6(5) . . ? C3 C4 C5 119.0(4) . . ? C4 C5 C6 120.5(4) . . ? C5 C6 C1 121.2(4) . . ? C12 C7 C8 118.5(4) . . ? C12 C7 C2 119.8(4) . . ? C8 C7 C2 121.7(4) . . ? C9 C8 C7 120.3(5) . . ? C8 C9 C10 120.7(5) . . ? C11 C10 C9 118.8(5) . . ? C10 C11 C12 121.1(5) . . ? C11 C12 C7 120.5(5) . . ? C18 C13 N2 120.8(3) . . ? C18 C13 C14 117.8(3) . . ? N2 C13 C14 121.3(3) . . ? C15 C14 C13 118.6(4) . . ? C15 C14 C19 118.1(3) . . ? C13 C14 C19 123.3(3) . . ? C16 C15 C14 122.2(4) . . ? C17 C16 C15 119.5(4) . . ? C16 C17 C18 119.5(4) . . ? C17 C18 C13 122.3(4) . . ? C24 C19 C20 117.4(4) . . ? C24 C19 C14 120.7(4) . . ? C20 C19 C14 121.8(4) . . ? C21 C20 C19 121.4(4) . . ? C20 C21 C22 120.1(5) . . ? C23 C22 C21 119.5(4) . . ? C22 C23 C24 120.2(4) . . ? C23 C24 C19 121.4(4) . . ? N2 C25 N1 121.9(4) . . ? N2 C25 Sr1 62.0(2) . . ? N1 C25 Sr1 60.2(2) . . ? O1 C26 C27 107.3(4) . . ? C26 C27 C28 104.1(4) . . ? C29 C28 C27 102.3(4) . . ? O1 C29 C28 104.8(4) . . ? O2 C30 C31 105.5(4) . . ? C31 C31 C30 101.8(3) 2_665 . ? O3 C32 C33 110.1(8) . . ? C34 C33 C32 102.1(8) . . ? C33 C34 C35 104.1(7) . . ? O3 C35 C34 103.9(7) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.529 _refine_diff_density_min -0.707 _refine_diff_density_rms 0.079 _chemical_compound_source THF #===END