Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Prof. Qi Shen' _publ_contact_author_address ; Department of Chemistry Suzhou University Suzhou, 215006 P. R. China ; _publ_contact_author_phone 86-512-65112513 _publ_contact_author_fax 86-512-65112371 _publ_contact_author_email qshen@suda.edu.cn _publ_section_title ; The novel lanthanide(II) complexes supported by carbon-bridged biphenolate ligands: synthesis, structure and catalytic activity ; loop_ _publ_author_name _publ_author_address 'Ming-yu Deng' ; Department of Chemistry and Chemical Engineering Suzhou University Suzhou, 215006 The People's Republic of China ; 'Ying-ming Yao' ; Department of Chemistry and Chemical Engineering Suzhou University Suzhou, 215006 The People's Republic of China ; 'Qi Shen' ; Department of Chemistry and Chemical Engineering Suzhou University Suzhou, 215006 The People's Republic of China ; 'Yong Zhang' ; Department of Chemistry and Chemical Engineering Suzhou University Suzhou, 215006 The People's Republic of China ; 'Jin Sun' ; Department of Chemistry and Chemical Engineering Suzhou University Suzhou, 215006 The People's Republic of China ; _publ_requested_journal 'Dalton Transactions' #============================================================================== data_complex3 _database_code_depnum_ccdc_archive 'CCDC 219106' _audit_creation_date 2003-12-26 _audit_creation_method 'by CrystalStructure v3.5.1' _audit_update_record ? #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C70 H132 N12 O8 P4 Sm2,2(C4 H8 O) ' _chemical_formula_moiety 'C78 H148 N12 O10 P4 Sm2 ' _chemical_formula_weight 1838.80 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/a ' _symmetry_space_group_name_Hall '-P 2yab' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z x+1/2,-y+1/2,z #------------------------------------------------------------------------------ _cell_length_a 12.051(2) _cell_length_b 28.238(3) _cell_length_c 16.433(3) _cell_angle_alpha 90 _cell_angle_beta 111.652(7) _cell_angle_gamma 90 _cell_volume 5197.3(13) _cell_formula_units_Z 2 _cell_measurement_reflns_used 9770 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 25.0 _cell_measurement_temperature 193.1 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.28 _exptl_crystal_density_diffrn 1.175 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1928.00 _exptl_absorpt_coefficient_mu 1.234 _exptl_absorpt_correction_type psi-scans _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.600 _exptl_absorpt_correction_T_max 0.708 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 47553 _diffrn_reflns_av_R_equivalents 0.043 _diffrn_reflns_theta_max 25.02 _diffrn_measured_fraction_theta_max 0.9768 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.9768 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 8976 _reflns_number_gt 7445 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0550 _refine_ls_wR_factor_ref 0.1730 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 7445 _refine_ls_number_parameters 552 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0059Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)' _refine_ls_shift/su_max 0.0010 _refine_diff_density_max 3.08 _refine_diff_density_min -0.79 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; P P 0.102 0.094 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Sm Sm -0.164 3.442 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Sm(1) Sm 0.44194(2) 0.55658(1) 0.54770(2) 0.03193(11) Uani 1.00 1 d . . . P(1) P 0.2529(1) 0.65680(6) 0.38546(11) 0.0464(4) Uani 1.00 1 d . . . P(2) P 0.2355(1) 0.58182(5) 0.67891(10) 0.0430(4) Uani 1.00 1 d . . . O(1) O 0.6082(4) 0.5917(1) 0.6531(3) 0.0460(11) Uani 1.00 1 d . . . O(2) O 0.4960(3) 0.47028(12) 0.5705(2) 0.0357(10) Uani 1.00 1 d . . . O(3) O 0.3350(4) 0.6213(2) 0.4438(3) 0.0513(12) Uani 1.00 1 d . . . O(4) O 0.2831(4) 0.5678(2) 0.6109(3) 0.0470(12) Uani 1.00 1 d . . . O(5) O 0.274(2) 0.4196(11) 1.005(2) 0.44(2) Uani 1.00 1 d . . . N(1) N 0.1160(5) 0.6425(2) 0.3668(5) 0.069(2) Uani 1.00 1 d . . . N(2) N 0.2578(7) 0.6662(3) 0.2905(5) 0.093(3) Uani 1.00 1 d . . . N(3) N 0.2814(9) 0.7084(2) 0.4317(7) 0.136(3) Uani 1.00 1 d . . . N(4) N 0.3467(5) 0.5925(2) 0.7712(4) 0.054(2) Uani 1.00 1 d . . . N(5) N 0.1475(5) 0.5425(2) 0.6979(4) 0.059(2) Uani 1.00 1 d . . . N(6) N 0.1516(6) 0.6289(2) 0.6489(4) 0.063(2) Uani 1.00 1 d . . . C(1) C 0.7128(5) 0.5911(2) 0.7161(4) 0.042(2) Uani 1.00 1 d . . . C(2) C 0.7675(6) 0.6335(2) 0.7628(4) 0.049(2) Uani 1.00 1 d . . . C(3) C 0.8809(6) 0.6286(3) 0.8287(5) 0.060(2) Uani 1.00 1 d . . . C(4) C 0.9436(6) 0.5866(3) 0.8525(5) 0.062(2) Uani 1.00 1 d . . . C(5) C 0.8879(6) 0.5471(3) 0.8065(5) 0.053(2) Uani 1.00 1 d . . . C(6) C 0.7769(5) 0.5483(2) 0.7394(4) 0.042(2) Uani 1.00 1 d . . . C(7) C 0.5212(5) 0.4617(2) 0.6552(3) 0.0339(13) Uani 1.00 1 d . . . C(8) C 0.4425(5) 0.4353(2) 0.6842(4) 0.038(2) Uani 1.00 1 d . . . C(9) C 0.4692(5) 0.4310(2) 0.7738(4) 0.042(2) Uani 1.00 1 d . . . C(10) C 0.5734(6) 0.4498(2) 0.8370(4) 0.045(2) Uani 1.00 1 d . . . C(11) C 0.6506(5) 0.4747(2) 0.8082(4) 0.041(2) Uani 1.00 1 d . . . C(12) C 0.6269(5) 0.4804(2) 0.7188(3) 0.036(1) Uani 1.00 1 d . . . C(13) C 0.7207(5) 0.5035(2) 0.6901(4) 0.042(2) Uani 1.00 1 d . . . C(14) C 0.7066(8) 0.6810(2) 0.7400(5) 0.064(2) Uani 1.00 1 d . . . C(15) C 0.5855(8) 0.6803(3) 0.7483(6) 0.072(3) Uani 1.00 1 d . . . C(16) C 0.6895(8) 0.6928(3) 0.6431(5) 0.072(2) Uani 1.00 1 d . . . C(17) C 0.7774(10) 0.7223(3) 0.7963(6) 0.088(3) Uani 1.00 1 d . . . C(18) C 1.0655(7) 0.5849(5) 0.9234(6) 0.093(3) Uani 1.00 1 d . . . C(19) C 0.3334(5) 0.4099(2) 0.6187(4) 0.041(2) Uani 1.00 1 d . . . C(20) C 0.2480(7) 0.4462(2) 0.5567(6) 0.062(2) Uani 1.00 1 d . . . C(21) C 0.2620(6) 0.3832(3) 0.6652(5) 0.058(2) Uani 1.00 1 d . . . C(22) C 0.3730(7) 0.3737(2) 0.5676(5) 0.061(2) Uani 1.00 1 d . . . C(23) C 0.5981(8) 0.4454(3) 0.9345(4) 0.067(2) Uani 1.00 1 d . . . C(24) C 0.0796(7) 0.6038(3) 0.4062(7) 0.090(3) Uani 1.00 1 d . . . C(25) C 0.0171(9) 0.6690(7) 0.309(1) 0.227(9) Uani 1.00 1 d . . . C(26) C 0.208(2) 0.6305(5) 0.2242(8) 0.290(12) Uani 1.00 1 d . . . C(27) C 0.3457(12) 0.6989(10) 0.2804(12) 0.303(12) Uani 1.00 1 d . . . C(28) C 0.205(3) 0.7490(5) 0.393(2) 0.43(2) Uani 1.00 1 d . . . C(29) C 0.3799(11) 0.7196(4) 0.5100(7) 0.113(4) Uani 1.00 1 d . . . C(30) C 0.3398(8) 0.6249(3) 0.8367(5) 0.077(3) Uani 1.00 1 d . . . C(31) C 0.4534(7) 0.5627(3) 0.7980(6) 0.066(2) Uani 1.00 1 d . . . C(32) C 0.1847(8) 0.5116(3) 0.7726(6) 0.074(3) Uani 1.00 1 d . . . C(33) C 0.0402(7) 0.5281(4) 0.6256(6) 0.082(3) Uani 1.00 1 d . . . C(34) C 0.0558(8) 0.6412(4) 0.6785(6) 0.087(3) Uani 1.00 1 d . . . C(35) C 0.1941(11) 0.6679(3) 0.6099(7) 0.100(4) Uani 1.00 1 d . . . C(36) C 0.151(3) 0.4332(11) 0.964(2) 0.27(2) Uani 1.00 1 d . . . C(37) C 0.137(2) 0.4106(8) 0.877(2) 0.272(13) Uani 1.00 1 d . . . C(38) C 0.245(3) 0.378(1) 0.909(2) 0.33(2) Uani 1.00 1 d . . . C(39) C 0.324(4) 0.3734(10) 1.006(2) 0.37(5) Uani 1.00 1 d . . . H(1) H 0.9169(6) 0.6565(3) 0.8595(5) 0.069(2) Uiso 1.00 1 c . . . H(2) H 0.9286(6) 0.5176(3) 0.8210(5) 0.063(2) Uiso 1.00 1 c . . . H(3) H 0.4155(5) 0.4140(2) 0.7932(4) 0.052(2) Uiso 1.00 1 c . . . H(4) H 0.7210(5) 0.4882(2) 0.8495(4) 0.049(2) Uiso 1.00 1 c . . . H(5) H 0.6842(5) 0.5113(2) 0.6297(4) 0.052(2) Uiso 1.00 1 c . . . H(6) H 0.7828(5) 0.4812(2) 0.6978(4) 0.052(2) Uiso 1.00 1 c . . . H(7) H 0.5367(8) 0.6572(3) 0.7094(6) 0.085(3) Uiso 1.00 1 c . . . H(8) H 0.5960(8) 0.6723(3) 0.8068(6) 0.085(3) Uiso 1.00 1 c . . . H(9) H 0.5483(8) 0.7105(3) 0.7344(6) 0.085(3) Uiso 1.00 1 c . . . H(10) H 0.6415(8) 0.6692(3) 0.6050(5) 0.082(3) Uiso 1.00 1 c . . . H(11) H 0.6522(8) 0.7228(3) 0.6273(5) 0.082(3) Uiso 1.00 1 c . . . H(12) H 0.7658(8) 0.6935(3) 0.6386(5) 0.082(3) Uiso 1.00 1 c . . . H(13) H 0.7360(10) 0.7514(3) 0.7780(6) 0.099(4) Uiso 1.00 1 c . . . H(14) H 0.7892(10) 0.7166(3) 0.8559(6) 0.099(4) Uiso 1.00 1 c . . . H(15) H 0.8526(10) 0.7240(3) 0.7900(6) 0.099(4) Uiso 1.00 1 c . . . H(16) H 1.0897(7) 0.6153(5) 0.9485(6) 0.103(4) Uiso 1.00 1 c . . . H(17) H 1.0611(7) 0.5637(5) 0.9670(6) 0.103(4) Uiso 1.00 1 c . . . H(18) H 1.1219(7) 0.5734(5) 0.9003(6) 0.103(4) Uiso 1.00 1 c . . . H(19) H 0.1818(7) 0.4301(2) 0.5155(6) 0.070(2) Uiso 1.00 1 c . . . H(20) H 0.2207(7) 0.4675(2) 0.5900(6) 0.070(2) Uiso 1.00 1 c . . . H(21) H 0.2889(7) 0.4634(2) 0.5266(6) 0.070(2) Uiso 1.00 1 c . . . H(22) H 0.3126(6) 0.3605(3) 0.7038(5) 0.071(3) Uiso 1.00 1 c . . . H(23) H 0.2346(6) 0.4050(3) 0.6977(5) 0.071(3) Uiso 1.00 1 c . . . H(24) H 0.1956(6) 0.3677(3) 0.6232(5) 0.071(3) Uiso 1.00 1 c . . . H(25) H 0.4170(7) 0.3888(2) 0.5374(5) 0.076(3) Uiso 1.00 1 c . . . H(26) H 0.4222(7) 0.3509(2) 0.6070(5) 0.076(3) Uiso 1.00 1 c . . . H(27) H 0.3052(7) 0.3584(2) 0.5265(5) 0.076(3) Uiso 1.00 1 c . . . H(28) H 0.6012(8) 0.4759(3) 0.9593(4) 0.079(3) Uiso 1.00 1 c . . . H(29) H 0.5361(8) 0.4275(3) 0.9423(4) 0.079(3) Uiso 1.00 1 c . . . H(30) H 0.6723(8) 0.4297(3) 0.9625(4) 0.079(3) Uiso 1.00 1 c . . . H(31) H 0.1483(7) 0.5862(3) 0.4401(7) 0.103(4) Uiso 1.00 1 c . . . H(32) H 0.0392(7) 0.6144(3) 0.4427(7) 0.103(4) Uiso 1.00 1 c . . . H(33) H 0.0278(7) 0.5842(3) 0.3612(7) 0.103(4) Uiso 1.00 1 c . . . H(34) H -0.0355(9) 0.6508(7) 0.262(1) 0.26(1) Uiso 1.00 1 c . . . H(35) H -0.0249(9) 0.6810(7) 0.343(1) 0.26(1) Uiso 1.00 1 c . . . H(36) H 0.0477(9) 0.6947(7) 0.286(1) 0.26(1) Uiso 1.00 1 c . . . H(37) H 0.270(2) 0.6092(5) 0.2265(8) 0.36(2) Uiso 1.00 1 c . . . H(38) H 0.145(2) 0.6135(5) 0.2321(8) 0.36(2) Uiso 1.00 1 c . . . H(39) H 0.179(2) 0.6459(5) 0.1689(8) 0.36(2) Uiso 1.00 1 c . . . H(40) H 0.3145(12) 0.7131(10) 0.2242(12) 0.36(2) Uiso 1.00 1 c . . . H(41) H 0.3801(12) 0.7226(10) 0.3235(12) 0.36(2) Uiso 1.00 1 c . . . H(42) H 0.4050(12) 0.6764(10) 0.2820(12) 0.36(2) Uiso 1.00 1 c . . . H(43) H 0.141(3) 0.7399(5) 0.340(2) 0.38(2) Uiso 1.00 1 c . . . H(44) H 0.172(3) 0.7613(5) 0.433(2) 0.38(2) Uiso 1.00 1 c . . . H(45) H 0.252(3) 0.7726(5) 0.380(2) 0.38(2) Uiso 1.00 1 c . . . H(46) H 0.4280(11) 0.7430(4) 0.4974(7) 0.133(5) Uiso 1.00 1 c . . . H(47) H 0.3491(11) 0.7318(4) 0.5512(7) 0.133(5) Uiso 1.00 1 c . . . H(48) H 0.4269(11) 0.6923(4) 0.5336(7) 0.133(5) Uiso 1.00 1 c . . . H(49) H 0.2685(8) 0.6431(3) 0.8141(5) 0.094(3) Uiso 1.00 1 c . . . H(50) H 0.3401(8) 0.6073(3) 0.8861(5) 0.094(3) Uiso 1.00 1 c . . . H(51) H 0.4069(8) 0.6455(3) 0.8536(5) 0.094(3) Uiso 1.00 1 c . . . H(52) H 0.5223(7) 0.5822(3) 0.8134(6) 0.078(3) Uiso 1.00 1 c . . . H(53) H 0.4569(7) 0.5441(3) 0.8470(6) 0.078(3) Uiso 1.00 1 c . . . H(54) H 0.4503(7) 0.5425(3) 0.7510(6) 0.078(3) Uiso 1.00 1 c . . . H(55) H 0.2559(8) 0.5235(3) 0.8156(6) 0.094(3) Uiso 1.00 1 c . . . H(56) H 0.1236(8) 0.5103(3) 0.7961(6) 0.094(3) Uiso 1.00 1 c . . . H(57) H 0.1988(8) 0.4807(3) 0.7556(6) 0.094(3) Uiso 1.00 1 c . . . H(58) H 0.0511(7) 0.4976(4) 0.6053(6) 0.101(4) Uiso 1.00 1 c . . . H(59) H -0.0248(7) 0.5272(4) 0.6451(6) 0.101(4) Uiso 1.00 1 c . . . H(60) H 0.0237(7) 0.5503(4) 0.5793(6) 0.101(4) Uiso 1.00 1 c . . . H(61) H 0.0345(8) 0.6137(4) 0.7027(6) 0.108(4) Uiso 1.00 1 c . . . H(62) H 0.0818(8) 0.6652(4) 0.7219(6) 0.108(4) Uiso 1.00 1 c . . . H(63) H -0.0115(8) 0.6521(4) 0.6306(6) 0.108(4) Uiso 1.00 1 c . . . H(64) H 0.1301(11) 0.6798(3) 0.5606(7) 0.130(6) Uiso 1.00 1 c . . . H(65) H 0.2240(11) 0.6924(3) 0.6520(7) 0.130(6) Uiso 1.00 1 c . . . H(66) H 0.2560(11) 0.6569(3) 0.5920(7) 0.130(6) Uiso 1.00 1 c . . . H(67) H 0.096(3) 0.4196(11) 0.986(2) 0.36(3) Uiso 1.00 1 c . . . H(68) H 0.139(3) 0.4664(11) 0.958(2) 0.36(3) Uiso 1.00 1 c . . . H(69) H 0.064(2) 0.3949(8) 0.848(2) 0.26(2) Uiso 1.00 1 c . . . H(70) H 0.150(2) 0.4336(8) 0.839(2) 0.26(2) Uiso 1.00 1 c . . . H(71) H 0.217(3) 0.348(1) 0.883(2) 0.39(2) Uiso 1.00 1 c . . . H(72) H 0.308(3) 0.388(1) 0.891(2) 0.39(2) Uiso 1.00 1 c . . . H(73) H 0.406(4) 0.3656(10) 1.033(2) 1.03(10) Uiso 1.00 1 c . . . H(74) H 0.278(4) 0.3530(10) 1.027(2) 1.03(10) Uiso 1.00 1 c . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Sm(1) 0.0345(2) 0.0259(2) 0.0364(2) 0.00266(10) 0.0142(1) -0.00006(10) P(1) 0.0413(8) 0.0405(8) 0.0584(10) 0.0116(6) 0.0196(7) 0.0174(7) P(2) 0.0482(9) 0.0420(8) 0.0459(8) 0.0116(7) 0.0256(7) 0.0056(6) O(1) 0.047(2) 0.039(2) 0.046(2) -0.006(2) 0.010(2) -0.000(2) O(2) 0.048(2) 0.025(2) 0.036(2) 0.005(2) 0.018(2) 0.004(1) O(3) 0.042(2) 0.048(2) 0.065(3) 0.013(2) 0.020(2) 0.023(2) O(4) 0.054(3) 0.044(2) 0.051(2) 0.010(2) 0.028(2) 0.003(2) O(5) 0.26(3) 0.37(4) 0.44(4) -0.06(3) -0.17(3) 0.03(3) N(1) 0.040(3) 0.071(4) 0.088(5) 0.006(3) 0.016(3) 0.032(4) N(2) 0.094(5) 0.126(6) 0.078(5) 0.066(5) 0.056(4) 0.064(5) N(3) 0.138(8) 0.036(4) 0.157(9) 0.010(4) -0.037(7) 0.006(4) N(4) 0.061(3) 0.054(3) 0.050(3) 0.008(3) 0.026(3) -0.004(3) N(5) 0.053(3) 0.067(4) 0.060(4) -0.003(3) 0.024(3) 0.013(3) N(6) 0.081(4) 0.058(3) 0.061(3) 0.037(3) 0.041(3) 0.014(3) C(1) 0.044(3) 0.044(3) 0.042(3) -0.011(3) 0.018(3) -0.008(3) C(2) 0.050(4) 0.047(3) 0.045(3) -0.016(3) 0.011(3) -0.007(3) C(3) 0.050(4) 0.073(5) 0.049(4) -0.020(3) 0.010(3) -0.014(3) C(4) 0.036(3) 0.087(6) 0.058(4) -0.014(3) 0.011(3) -0.008(4) C(5) 0.034(3) 0.063(4) 0.062(4) 0.001(3) 0.018(3) 0.007(3) C(6) 0.035(3) 0.052(3) 0.040(3) -0.006(3) 0.018(3) -0.001(3) C(7) 0.038(3) 0.028(3) 0.036(3) 0.009(2) 0.014(2) 0.006(2) C(8) 0.040(3) 0.036(3) 0.044(3) 0.006(2) 0.023(3) 0.007(2) C(9) 0.045(3) 0.042(3) 0.043(3) -0.001(3) 0.022(3) 0.006(3) C(10) 0.050(4) 0.054(4) 0.032(3) 0.003(3) 0.018(3) 0.007(3) C(11) 0.038(3) 0.044(3) 0.041(3) 0.001(2) 0.015(2) 0.005(2) C(12) 0.036(3) 0.036(3) 0.039(3) 0.006(2) 0.016(2) 0.004(2) C(13) 0.042(3) 0.039(3) 0.050(3) 0.001(2) 0.022(3) 0.001(3) C(14) 0.095(6) 0.041(3) 0.049(4) -0.015(4) 0.019(4) -0.013(3) C(15) 0.084(6) 0.056(4) 0.072(5) 0.014(4) 0.024(4) -0.004(4) C(16) 0.092(6) 0.045(4) 0.067(5) -0.014(4) 0.015(4) 0.001(3) C(17) 0.122(8) 0.045(4) 0.081(6) -0.019(5) 0.020(5) -0.022(4) C(18) 0.048(5) 0.136(9) 0.074(5) -0.010(5) -0.001(4) -0.019(6) C(19) 0.043(3) 0.035(3) 0.046(3) -0.003(2) 0.016(3) -0.007(2) C(20) 0.047(4) 0.059(4) 0.068(5) -0.003(3) 0.008(3) 0.000(3) C(21) 0.051(4) 0.064(4) 0.063(4) -0.018(3) 0.025(3) -0.005(3) C(22) 0.062(4) 0.050(4) 0.078(5) -0.020(3) 0.035(4) -0.019(3) C(23) 0.074(5) 0.089(6) 0.035(3) -0.016(4) 0.016(3) 0.006(3) C(24) 0.051(4) 0.086(6) 0.121(7) -0.011(4) 0.018(5) 0.047(6) C(25) 0.042(5) 0.29(2) 0.31(2) 0.009(8) 0.027(9) 0.23(2) C(26) 0.68(5) 0.135(12) 0.100(9) 0.23(2) 0.19(2) 0.067(9) C(27) 0.087(9) 0.60(5) 0.21(2) -0.02(2) 0.037(10) 0.29(3) C(28) 0.46(4) 0.076(10) 0.41(4) 0.10(2) -0.26(4) -0.05(2) C(29) 0.148(10) 0.089(7) 0.097(7) -0.045(7) 0.037(7) -0.007(6) C(30) 0.089(6) 0.084(6) 0.062(5) 0.001(5) 0.033(4) -0.023(4) C(31) 0.056(4) 0.073(5) 0.065(5) 0.020(4) 0.018(4) 0.014(4) C(32) 0.085(6) 0.061(5) 0.089(5) 0.011(4) 0.048(5) 0.034(4) C(33) 0.066(5) 0.104(7) 0.083(6) -0.020(5) 0.035(4) 0.000(5) C(34) 0.083(6) 0.110(7) 0.079(5) 0.054(5) 0.042(5) 0.011(5) C(35) 0.178(11) 0.050(5) 0.097(7) 0.049(6) 0.082(7) 0.032(5) C(36) 0.41(5) 0.23(3) 0.26(3) 0.05(3) 0.24(3) -0.01(3) C(37) 0.23(3) 0.19(2) 0.24(3) -0.06(2) -0.10(2) 0.10(2) C(38) 0.35(4) 0.48(5) 0.14(2) -0.04(4) 0.09(2) -0.18(3) C(39) 2.0(2) 0.12(2) 0.40(5) 0.11(6) 0.80(10) 0.05(3) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'DIRDIF99 (PATTY)' _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure Ver. 3.5.1' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Sm(1) O(1) 2.332(4) yes . . Sm(1) O(2) 2.515(3) yes . . Sm(1) O(3) 2.509(4) yes . . Sm(1) O(4) 2.512(5) yes . . P(1) O(3) 1.484(4) yes . . P(1) N(1) 1.613(6) yes . . P(1) N(2) 1.605(9) yes . . P(1) N(3) 1.621(8) yes . . P(2) O(4) 1.486(6) yes . . P(2) N(4) 1.639(5) yes . . P(2) N(5) 1.642(7) yes . . P(2) N(6) 1.632(6) yes . . O(1) C(1) 1.303(6) yes . . O(2) C(7) 1.334(7) yes . . O(5) C(36) 1.44(4) yes . . O(5) C(39) 1.43(4) yes . . N(1) C(24) 1.42(1) yes . . N(1) C(25) 1.43(2) yes . . N(2) C(26) 1.44(1) yes . . N(2) C(27) 1.46(2) yes . . N(3) C(28) 1.46(2) yes . . N(3) C(29) 1.43(1) yes . . N(4) C(30) 1.44(1) yes . . N(4) C(31) 1.46(1) yes . . N(5) C(32) 1.44(1) yes . . N(5) C(33) 1.455(9) yes . . N(6) C(34) 1.45(1) yes . . N(6) C(35) 1.46(1) yes . . C(1) C(2) 1.443(8) yes . . C(1) C(6) 1.409(8) yes . . C(2) C(3) 1.403(8) yes . . C(2) C(14) 1.510(9) yes . . C(3) C(4) 1.38(1) yes . . C(3) H(1) 0.95(1) no . . C(4) C(5) 1.37(1) yes . . C(4) C(18) 1.502(9) yes . . C(5) C(6) 1.386(8) yes . . C(5) H(2) 0.95(1) no . . C(6) C(13) 1.520(8) yes . . C(7) C(8) 1.420(9) yes . . C(7) C(12) 1.418(7) yes . . C(8) C(9) 1.391(9) yes . . C(8) C(19) 1.535(7) yes . . C(9) C(10) 1.406(8) yes . . C(9) H(3) 0.95(1) no . . C(10) C(11) 1.38(1) yes . . C(10) C(23) 1.52(1) yes . . C(11) C(12) 1.399(8) yes . . C(11) H(4) 0.950(7) no . . C(12) C(13) 1.523(9) yes . . C(13) H(5) 0.950(8) no . . C(13) H(6) 0.950(9) no . . C(14) C(15) 1.52(1) yes . . C(14) C(16) 1.56(1) yes . . C(14) C(17) 1.54(1) yes . . C(15) H(7) 0.95(1) no . . C(15) H(8) 0.95(1) no . . C(15) H(9) 0.95(1) no . . C(16) H(10) 0.95(1) no . . C(16) H(11) 0.95(1) no . . C(16) H(12) 0.95(1) no . . C(17) H(13) 0.95(1) no . . C(17) H(14) 0.95(1) no . . C(17) H(15) 0.95(2) no . . C(18) H(16) 0.95(2) no . . C(18) H(17) 0.95(2) no . . C(18) H(18) 0.95(2) no . . C(19) C(20) 1.540(8) yes . . C(19) C(21) 1.54(1) yes . . C(19) C(22) 1.51(1) yes . . C(20) H(19) 0.95(1) no . . C(20) H(20) 0.95(1) no . . C(20) H(21) 0.95(1) no . . C(21) H(22) 0.95(1) no . . C(21) H(23) 0.95(1) no . . C(21) H(24) 0.950(9) no . . C(22) H(25) 0.95(1) no . . C(22) H(26) 0.950(9) no . . C(22) H(27) 0.950(9) no . . C(23) H(28) 0.95(1) no . . C(23) H(29) 0.95(1) no . . C(23) H(30) 0.95(1) no . . C(24) H(31) 0.95(1) no . . C(24) H(32) 0.95(2) no . . C(24) H(33) 0.95(1) no . . C(25) H(34) 0.95(2) no . . C(25) H(35) 0.95(3) no . . C(25) H(36) 0.95(3) no . . C(26) H(37) 0.95(3) no . . C(26) H(38) 0.95(4) no . . C(26) H(39) 0.95(2) no . . C(27) H(40) 0.95(3) no . . C(27) H(41) 0.95(3) no . . C(27) H(42) 0.95(3) no . . C(28) H(43) 0.95(3) no . . C(28) H(44) 0.95(5) no . . C(28) H(45) 0.95(4) no . . C(29) H(46) 0.95(2) no . . C(29) H(47) 0.95(2) no . . C(29) H(48) 0.95(2) no . . C(30) H(49) 0.95(1) no . . C(30) H(50) 0.95(1) no . . C(30) H(51) 0.95(1) no . . C(31) H(52) 0.95(1) no . . C(31) H(53) 0.95(1) no . . C(31) H(54) 0.95(1) no . . C(32) H(55) 0.95(1) no . . C(32) H(56) 0.95(2) no . . C(32) H(57) 0.95(1) no . . C(33) H(58) 0.95(1) no . . C(33) H(59) 0.95(1) no . . C(33) H(60) 0.95(1) no . . C(34) H(61) 0.95(2) no . . C(34) H(62) 0.95(1) no . . C(34) H(63) 0.95(1) no . . C(35) H(64) 0.95(1) no . . C(35) H(65) 0.95(1) no . . C(35) H(66) 0.95(2) no . . C(36) C(37) 1.52(4) yes . . C(36) H(67) 0.95(5) no . . C(36) H(68) 0.95(4) no . . C(37) C(38) 1.52(4) yes . . C(37) H(69) 0.95(3) no . . C(37) H(70) 0.95(4) no . . C(38) C(39) 1.53(3) yes . . C(38) H(71) 0.95(5) no . . C(38) H(72) 0.95(5) no . . C(39) H(73) 0.95(6) no . . C(39) H(74) 0.95(6) no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 O(1) Sm(1) O(2) 101.4(1) yes . . . O(1) Sm(1) O(3) 106.3(1) yes . . . O(1) Sm(1) O(4) 102.5(2) yes . . . O(1) Sm(1) O2(3;1;1;1) 106.9(1) yes . . . O(2) Sm(1) O(3) 147.9(1) yes . . . O(2) Sm(1) O(4) 104.8(1) yes . . . O(2) Sm(1) O2(3;1;1;1) 71.3(1) yes . . . O(3) Sm(1) O(4) 84.9(2) yes . . . O(3) Sm(1) O2(3;1;1;1) 85.2(1) yes . . . O(4) Sm(1) O2(3;1;1;1) 150.53(9) yes . . . O(3) P(1) N(1) 110.2(3) yes . . . O(3) P(1) N(2) 119.0(4) yes . . . O(3) P(1) N(3) 109.2(4) yes . . . N(1) P(1) N(2) 105.0(4) yes . . . N(1) P(1) N(3) 109.8(5) yes . . . N(2) P(1) N(3) 103.3(5) yes . . . O(4) P(2) N(4) 109.5(3) yes . . . O(4) P(2) N(5) 114.7(3) yes . . . O(4) P(2) N(6) 110.9(3) yes . . . N(4) P(2) N(5) 108.3(3) yes . . . N(4) P(2) N(6) 109.5(3) yes . . . N(5) P(2) N(6) 103.7(3) yes . . . C(1) O(1) Sm(1) 153.9(4) yes . . . C(7) O(2) Sm1(3;1;1;1) 139.0(3) yes . . . C(7) O(2) Sm(1) 106.1(3) yes . . . Sm1(3;1;1;1) O(2) Sm(1) 108.7(1) yes . . . Sm(1) O(3) P(1) 169.9(3) yes . . . Sm(1) O(4) P(2) 155.4(2) yes . . . C(36) O(5) C(39) 126(2) yes . . . C(24) N(1) C(25) 112.6(9) yes . . . C(24) N(1) P(1) 124.8(5) yes . . . C(25) N(1) P(1) 122.5(9) yes . . . C(26) N(2) C(27) 118(1) yes . . . C(26) N(2) P(1) 117(1) yes . . . C(27) N(2) P(1) 120.2(9) yes . . . C(28) N(3) C(29) 113(1) yes . . . C(28) N(3) P(1) 120(1) yes . . . C(29) N(3) P(1) 125.7(7) yes . . . C(30) N(4) C(31) 115.3(6) yes . . . C(30) N(4) P(2) 123.8(5) yes . . . C(31) N(4) P(2) 120.0(5) yes . . . C(32) N(5) C(33) 115.5(7) yes . . . C(32) N(5) P(2) 123.6(5) yes . . . C(33) N(5) P(2) 118.5(6) yes . . . C(34) N(6) C(35) 114.7(8) yes . . . C(34) N(6) P(2) 125.0(6) yes . . . C(35) N(6) P(2) 118.0(7) yes . . . C(2) C(1) C(6) 118.0(5) yes . . . C(2) C(1) O(1) 121.9(5) yes . . . C(6) C(1) O(1) 120.0(5) yes . . . C(3) C(2) C(14) 121.6(6) yes . . . C(3) C(2) C(1) 117.0(6) yes . . . C(14) C(2) C(1) 121.4(5) yes . . . C(4) C(3) H(1) 117.8(7) no . . . C(4) C(3) C(2) 125.2(7) yes . . . H(1) C(3) C(2) 117.0(8) no . . . C(5) C(4) C(18) 122.7(8) yes . . . C(5) C(4) C(3) 115.9(6) yes . . . C(18) C(4) C(3) 121.5(8) yes . . . C(6) C(5) H(2) 118.6(7) no . . . C(6) C(5) C(4) 123.3(6) yes . . . H(2) C(5) C(4) 118.1(7) no . . . C(13) C(6) C(1) 118.5(5) yes . . . C(13) C(6) C(5) 120.9(6) yes . . . C(1) C(6) C(5) 120.6(6) yes . . . C(8) C(7) C(12) 118.6(5) yes . . . C(8) C(7) O(2) 121.6(4) yes . . . C(12) C(7) O(2) 119.8(5) yes . . . C(9) C(8) C(19) 120.3(6) yes . . . C(9) C(8) C(7) 118.6(5) yes . . . C(19) C(8) C(7) 121.0(5) yes . . . C(10) C(9) H(3) 118.4(7) no . . . C(10) C(9) C(8) 122.9(6) yes . . . H(3) C(9) C(8) 118.6(6) no . . . C(11) C(10) C(23) 120.5(6) yes . . . C(11) C(10) C(9) 118.0(6) yes . . . C(23) C(10) C(9) 121.4(7) yes . . . C(12) C(11) H(4) 119.1(8) no . . . C(12) C(11) C(10) 121.1(5) yes . . . H(4) C(11) C(10) 119.7(7) no . . . C(13) C(12) C(7) 120.0(5) yes . . . C(13) C(12) C(11) 119.2(5) yes . . . C(7) C(12) C(11) 120.7(6) yes . . . H(5) C(13) H(6) 109.5(9) no . . . H(5) C(13) C(6) 107.9(6) no . . . H(5) C(13) C(12) 108.1(6) no . . . H(6) C(13) C(6) 107.8(6) no . . . H(6) C(13) C(12) 108.2(7) no . . . C(6) C(13) C(12) 115.3(6) yes . . . C(15) C(14) C(16) 109.0(6) yes . . . C(15) C(14) C(17) 107.1(8) yes . . . C(15) C(14) C(2) 111.2(6) yes . . . C(16) C(14) C(17) 106.7(7) yes . . . C(16) C(14) C(2) 108.2(7) yes . . . C(17) C(14) C(2) 114.5(6) yes . . . H(7) C(15) H(8) 109(1) no . . . H(7) C(15) H(9) 109(1) no . . . H(7) C(15) C(14) 109(1) no . . . H(8) C(15) H(9) 109(1) no . . . H(8) C(15) C(14) 108.8(9) no . . . H(9) C(15) C(14) 110(1) no . . . H(10) C(16) H(11) 109(1) no . . . H(10) C(16) H(12) 109(1) no . . . H(10) C(16) C(14) 110.1(9) no . . . H(11) C(16) H(12) 109(1) no . . . H(11) C(16) C(14) 109(1) no . . . H(12) C(16) C(14) 108.5(8) no . . . H(13) C(17) H(14) 109(1) no . . . H(13) C(17) H(15) 109(1) no . . . H(13) C(17) C(14) 110.8(9) no . . . H(14) C(17) H(15) 109(1) no . . . H(14) C(17) C(14) 109(1) no . . . H(15) C(17) C(14) 108(1) no . . . H(16) C(18) H(17) 109(1) no . . . H(16) C(18) H(18) 109(1) no . . . H(16) C(18) C(4) 111(1) no . . . H(17) C(18) H(18) 109(1) no . . . H(17) C(18) C(4) 107(1) no . . . H(18) C(18) C(4) 109(1) no . . . C(20) C(19) C(21) 107.1(6) yes . . . C(20) C(19) C(22) 110.7(6) yes . . . C(20) C(19) C(8) 110.1(5) yes . . . C(21) C(19) C(22) 107.1(5) yes . . . C(21) C(19) C(8) 111.8(5) yes . . . C(22) C(19) C(8) 110.0(5) yes . . . H(19) C(20) H(20) 109(1) no . . . H(19) C(20) H(21) 109(1) no . . . H(19) C(20) C(19) 109.6(7) no . . . H(20) C(20) H(21) 109(1) no . . . H(20) C(20) C(19) 109.2(8) no . . . H(21) C(20) C(19) 109.6(8) no . . . H(22) C(21) H(23) 109(1) no . . . H(22) C(21) H(24) 109(1) no . . . H(22) C(21) C(19) 108.8(8) no . . . H(23) C(21) H(24) 109(1) no . . . H(23) C(21) C(19) 109.7(8) no . . . H(24) C(21) C(19) 109.9(8) no . . . H(25) C(22) H(26) 109(1) no . . . H(25) C(22) H(27) 109(1) no . . . H(25) C(22) C(19) 109.7(8) no . . . H(26) C(22) H(27) 109.5(9) no . . . H(26) C(22) C(19) 109.0(9) no . . . H(27) C(22) C(19) 109.7(9) no . . . H(28) C(23) H(29) 109(1) no . . . H(28) C(23) H(30) 109(1) no . . . H(28) C(23) C(10) 109.8(8) no . . . H(29) C(23) H(30) 109(1) no . . . H(29) C(23) C(10) 109.2(7) no . . . H(30) C(23) C(10) 109(1) no . . . H(31) C(24) H(32) 109(1) no . . . H(31) C(24) H(33) 109(1) no . . . H(31) C(24) N(1) 108(1) no . . . H(32) C(24) H(33) 109(1) no . . . H(32) C(24) N(1) 111(1) no . . . H(33) C(24) N(1) 108(1) no . . . H(34) C(25) H(35) 109(1) no . . . H(34) C(25) H(36) 109(2) no . . . H(34) C(25) N(1) 113(2) no . . . H(35) C(25) H(36) 109(2) no . . . H(35) C(25) N(1) 106(2) no . . . H(36) C(25) N(1) 108(1) no . . . H(37) C(26) H(38) 109(2) no . . . H(37) C(26) H(39) 109(2) no . . . H(37) C(26) N(2) 108(2) no . . . H(38) C(26) H(39) 109(2) no . . . H(38) C(26) N(2) 112(1) no . . . H(39) C(26) N(2) 107(1) no . . . H(40) C(27) H(41) 109(3) no . . . H(40) C(27) H(42) 109(2) no . . . H(40) C(27) N(2) 109(1) no . . . H(41) C(27) H(42) 109(2) no . . . H(41) C(27) N(2) 119(2) no . . . H(42) C(27) N(2) 98(2) no . . . H(43) C(28) H(44) 109(4) no . . . H(43) C(28) H(45) 109(3) no . . . H(43) C(28) N(3) 110(1) no . . . H(44) C(28) H(45) 109(2) no . . . H(44) C(28) N(3) 109(2) no . . . H(45) C(28) N(3) 108(3) no . . . H(46) C(29) H(47) 109(1) no . . . H(46) C(29) H(48) 109(1) no . . . H(46) C(29) N(3) 109(1) no . . . H(47) C(29) H(48) 109(1) no . . . H(47) C(29) N(3) 107(1) no . . . H(48) C(29) N(3) 111(1) no . . . H(49) C(30) H(50) 109(1) no . . . H(49) C(30) H(51) 109(1) no . . . H(49) C(30) N(4) 110.2(8) no . . . H(50) C(30) H(51) 109(1) no . . . H(50) C(30) N(4) 108(1) no . . . H(51) C(30) N(4) 109(1) no . . . H(52) C(31) H(53) 109(1) no . . . H(52) C(31) H(54) 109(1) no . . . H(52) C(31) N(4) 109.4(8) no . . . H(53) C(31) H(54) 109(1) no . . . H(53) C(31) N(4) 109(1) no . . . H(54) C(31) N(4) 109.6(8) no . . . H(55) C(32) H(56) 109(1) no . . . H(55) C(32) H(57) 109(1) no . . . H(55) C(32) N(5) 109.4(9) no . . . H(56) C(32) H(57) 109(1) no . . . H(56) C(32) N(5) 109.1(9) no . . . H(57) C(32) N(5) 109(1) no . . . H(58) C(33) H(59) 109(1) no . . . H(58) C(33) H(60) 109(1) no . . . H(58) C(33) N(5) 110.2(9) no . . . H(59) C(33) H(60) 109(1) no . . . H(59) C(33) N(5) 109(1) no . . . H(60) C(33) N(5) 109(1) no . . . H(61) C(34) H(62) 109(1) no . . . H(61) C(34) H(63) 109(1) no . . . H(61) C(34) N(6) 108(1) no . . . H(62) C(34) H(63) 109(1) no . . . H(62) C(34) N(6) 109(1) no . . . H(63) C(34) N(6) 110(1) no . . . H(64) C(35) H(65) 109(1) no . . . H(64) C(35) H(66) 109(1) no . . . H(64) C(35) N(6) 109(1) no . . . H(65) C(35) H(66) 109(1) no . . . H(65) C(35) N(6) 109(1) no . . . H(66) C(35) N(6) 109.4(9) no . . . C(37) C(36) H(67) 109(3) no . . . C(37) C(36) H(68) 110(3) no . . . C(37) C(36) O(5) 94(2) yes . . . H(67) C(36) H(68) 109(4) no . . . H(67) C(36) O(5) 117(3) no . . . H(68) C(36) O(5) 114(3) no . . . C(38) C(37) H(69) 114(2) no . . . C(38) C(37) H(70) 108(3) no . . . C(38) C(37) C(36) 98(1) yes . . . H(69) C(37) H(70) 109(2) no . . . H(69) C(37) C(36) 115(3) no . . . H(70) C(37) C(36) 110(2) no . . . C(39) C(38) H(71) 111(3) no . . . C(39) C(38) H(72) 95(3) no . . . C(39) C(38) C(37) 122(2) yes . . . H(71) C(38) H(72) 109(4) no . . . H(71) C(38) C(37) 105(3) no . . . H(72) C(38) C(37) 112(3) no . . . H(73) C(39) H(74) 109(4) no . . . H(73) C(39) O(5) 124(3) no . . . H(73) C(39) C(38) 130(4) no . . . H(74) C(39) O(5) 104(4) no . . . H(74) C(39) C(38) 101(3) no . . . O(5) C(39) C(38) 79(2) yes . . . #=================================================================END data_shelxl _database_code_depnum_ccdc_archive 'CCDC 219107' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H112 N6 O8 P2 Yb2, 6(C4 H8 O), C7 H8 ' _chemical_formula_sum 'C97 H168 N6 O14 P2 Yb2' _chemical_formula_weight 2050.39 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.4386(15) _cell_length_b 15.4095(18) _cell_length_c 16.036(2) _cell_angle_alpha 108.792(4) _cell_angle_beta 109.163(4) _cell_angle_gamma 99.71 _cell_volume 2615.9(6) _cell_formula_units_Z 1 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 6319 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description Chunk _exptl_crystal_colour Orange-red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.38 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.302 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1074 _exptl_absorpt_coefficient_mu 1.866 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4555 _exptl_absorpt_correction_T_max 0.5374 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.62 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27853 _diffrn_reflns_av_R_equivalents 0.0276 _diffrn_reflns_av_sigmaI/netI 0.0284 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 27.48 _reflns_number_total 11512 _reflns_number_gt 11090 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0345P)^2^+2.8985P] 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 11512 _refine_ls_number_parameters 555 _refine_ls_number_restraints 37 _refine_ls_R_factor_all 0.0359 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.0798 _refine_ls_wR_factor_gt 0.0785 _refine_ls_goodness_of_fit_ref 1.145 _refine_ls_restrained_S_all 1.182 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.957478(11) 0.602676(8) 0.978821(8) 0.02534(5) Uani 1 1 d . . . P1 P 0.70745(9) 0.56113(7) 0.74374(6) 0.0446(2) Uani 1 1 d . . . O1 O 0.95976(19) 0.71288(15) 1.10783(14) 0.0310(5) Uani 1 1 d . . . O2 O 1.12338(17) 0.54845(14) 1.02814(15) 0.0277(4) Uani 1 1 d . . . O3 O 0.8078(2) 0.5716(2) 0.83200(18) 0.0502(7) Uani 1 1 d . . . O4 O 1.0543(2) 0.74192(18) 0.95367(19) 0.0451(6) Uani 1 1 d D . . N1 N 0.6465(4) 0.6459(3) 0.7708(3) 0.0652(11) Uani 1 1 d . . . N2 N 0.5961(4) 0.4620(3) 0.6925(3) 0.0646(10) Uani 1 1 d . . . N3 N 0.7598(4) 0.5679(3) 0.6635(3) 0.0620(10) Uani 1 1 d . . . C1 C 1.0108(3) 0.7678(2) 1.2018(2) 0.0268(6) Uani 1 1 d . . . C2 C 0.9739(3) 0.8481(2) 1.2438(2) 0.0306(6) Uani 1 1 d . . . C3 C 1.0330(3) 0.9019(2) 1.3438(2) 0.0379(7) Uani 1 1 d . . . H3 H 1.0094 0.9556 1.3719 0.045 Uiso 1 1 calc R . . C4 C 1.1240(3) 0.8810(3) 1.4041(2) 0.0417(8) Uani 1 1 d . . . C5 C 1.1591(3) 0.8030(3) 1.3622(2) 0.0373(7) Uani 1 1 d . . . H5 H 1.2212 0.7875 1.4022 0.045 Uiso 1 1 calc R . . C6 C 1.1052(3) 0.7468(2) 1.2627(2) 0.0285(6) Uani 1 1 d . . . C7 C 1.2225(2) 0.6250(2) 1.0846(2) 0.0256(6) Uani 1 1 d . . . C8 C 1.3126(3) 0.6463(2) 1.0519(2) 0.0312(6) Uani 1 1 d . . . C9 C 1.4125(3) 0.7277(2) 1.1138(3) 0.0380(7) Uani 1 1 d . . . H9 H 1.4731 0.7425 1.0923 0.046 Uiso 1 1 calc R . . C10 C 1.4270(3) 0.7877(2) 1.2051(3) 0.0412(8) Uani 1 1 d . . . C11 C 1.3381(3) 0.7663(2) 1.2353(2) 0.0352(7) Uani 1 1 d . . . H11 H 1.3463 0.8072 1.2972 0.042 Uiso 1 1 calc R . . C12 C 1.2358(3) 0.6858(2) 1.1773(2) 0.0282(6) Uani 1 1 d . . . C13 C 1.1464(3) 0.6629(2) 1.2192(2) 0.0299(6) Uani 1 1 d . . . H13A H 1.0755 0.6094 1.1673 0.036 Uiso 1 1 calc R . . H13B H 1.1833 0.6402 1.2696 0.036 Uiso 1 1 calc R . . C14 C 0.8725(3) 0.8736(2) 1.1802(2) 0.0345(7) Uani 1 1 d . . . C15 C 0.9063(3) 0.8963(3) 1.1044(3) 0.0419(8) Uani 1 1 d . . . H15A H 0.9789 0.9516 1.1367 0.063 Uiso 1 1 calc R . . H15B H 0.8408 0.9114 1.0635 0.063 Uiso 1 1 calc R . . H15C H 0.9208 0.8403 1.0644 0.063 Uiso 1 1 calc R . . C16 C 0.8472(4) 0.9626(3) 1.2390(3) 0.0482(9) Uani 1 1 d . . . H16A H 0.9196 1.0181 1.2715 0.072 Uiso 1 1 calc R . . H16B H 0.8232 0.9498 1.2874 0.072 Uiso 1 1 calc R . . H16C H 0.7827 0.9764 1.1955 0.072 Uiso 1 1 calc R . . C17 C 0.7562(3) 0.7888(3) 1.1302(3) 0.0421(8) Uani 1 1 d . . . H17A H 0.6927 0.8045 1.0880 0.063 Uiso 1 1 calc R . . H17B H 0.7326 0.7769 1.1791 0.063 Uiso 1 1 calc R . . H17C H 0.7691 0.7310 1.0916 0.063 Uiso 1 1 calc R . . C18 C 1.1839(5) 0.9422(4) 1.5119(3) 0.0660(13) Uani 1 1 d . . . H18A H 1.1398 0.9169 1.5440 0.099 Uiso 1 1 calc R . . H18B H 1.1843 1.0088 1.5240 0.099 Uiso 1 1 calc R . . H18C H 1.2664 0.9405 1.5375 0.099 Uiso 1 1 calc R . . C19 C 1.3041(3) 0.5797(2) 0.9523(3) 0.0370(7) Uani 1 1 d . . . C20 C 1.1862(4) 0.5633(3) 0.8700(3) 0.0543(10) Uani 1 1 d . . . H20A H 1.1750 0.6256 0.8734 0.082 Uiso 1 1 calc R . . H20B H 1.1197 0.5254 0.8760 0.082 Uiso 1 1 calc R . . H20C H 1.1885 0.5284 0.8079 0.082 Uiso 1 1 calc R . . C21 C 1.3152(4) 0.4826(3) 0.9553(3) 0.0512(10) Uani 1 1 d . . . H21A H 1.2479 0.4514 0.9654 0.077 Uiso 1 1 calc R . . H21B H 1.3905 0.4937 1.0085 0.077 Uiso 1 1 calc R . . H21C H 1.3142 0.4410 0.8941 0.077 Uiso 1 1 calc R . . C22 C 1.4061(4) 0.6219(3) 0.9290(3) 0.0557(11) Uani 1 1 d . . . H22A H 1.3960 0.5792 0.8648 0.083 Uiso 1 1 calc R . . H22B H 1.4829 0.6279 0.9773 0.083 Uiso 1 1 calc R . . H22C H 1.4044 0.6856 0.9301 0.083 Uiso 1 1 calc R . . C23 C 1.5395(4) 0.8736(3) 1.2703(4) 0.0634(13) Uani 1 1 d . . . H23A H 1.5440 0.8981 1.3362 0.095 Uiso 1 1 calc R . . H23B H 1.5366 0.9245 1.2462 0.095 Uiso 1 1 calc R . . H23C H 1.6101 0.8535 1.2702 0.095 Uiso 1 1 calc R . . C24 C 0.5241(5) 0.6404(5) 0.7126(5) 0.0903(19) Uani 1 1 d . . . H24A H 0.4823 0.6584 0.7547 0.135 Uiso 1 1 calc R . . H24B H 0.4810 0.5745 0.6637 0.135 Uiso 1 1 calc R . . H24C H 0.5275 0.6848 0.6807 0.135 Uiso 1 1 calc R . . C25 C 0.7115(6) 0.7366(4) 0.8541(4) 0.092(2) Uani 1 1 d . . . H25A H 0.7270 0.7883 0.8324 0.138 Uiso 1 1 calc R . . H25B H 0.7877 0.7326 0.8942 0.138 Uiso 1 1 calc R . . H25C H 0.6639 0.7505 0.8920 0.138 Uiso 1 1 calc R . . C26 C 0.5775(5) 0.3789(4) 0.6064(4) 0.0780(17) Uani 1 1 d . . . H26A H 0.6086 0.3309 0.6259 0.117 Uiso 1 1 calc R . . H26B H 0.6197 0.3999 0.5709 0.117 Uiso 1 1 calc R . . H26C H 0.4919 0.3504 0.5648 0.117 Uiso 1 1 calc R . . C27 C 0.5336(5) 0.4397(5) 0.7499(5) 0.0812(16) Uani 1 1 d . . . H27A H 0.4471 0.4214 0.7129 0.122 Uiso 1 1 calc R . . H27B H 0.5583 0.4965 0.8100 0.122 Uiso 1 1 calc R . . H27C H 0.5537 0.3863 0.7652 0.122 Uiso 1 1 calc R . . C28 C 0.6920(6) 0.5871(5) 0.5804(4) 0.097(2) Uani 1 1 d . . . H28A H 0.7475 0.6284 0.5672 0.146 Uiso 1 1 calc R . . H28B H 0.6351 0.6194 0.5952 0.146 Uiso 1 1 calc R . . H28C H 0.6485 0.5260 0.5235 0.146 Uiso 1 1 calc R . . C29 C 0.8573(5) 0.5288(4) 0.6548(4) 0.0757(15) Uani 1 1 d . . . H29A H 0.8239 0.4649 0.6014 0.114 Uiso 1 1 calc R . . H29B H 0.9016 0.5236 0.7151 0.114 Uiso 1 1 calc R . . H29C H 0.9114 0.5718 0.6421 0.114 Uiso 1 1 calc R . . C30 C 1.0341(5) 0.7588(3) 0.8673(4) 0.0671(13) Uani 1 1 d D . . H30A H 0.9479 0.7328 0.8239 0.080 Uiso 1 1 calc R . . H30B H 1.0788 0.7270 0.8325 0.080 Uiso 1 1 calc R . . C31 C 1.0768(11) 0.8644(4) 0.8984(5) 0.181(6) Uani 1 1 d D . . H31A H 1.0080 0.8892 0.8807 0.217 Uiso 1 1 calc R . . H31B H 1.1281 0.8805 0.8662 0.217 Uiso 1 1 calc R . . C32 C 1.1461(5) 0.9085(3) 1.0050(4) 0.0712(14) Uani 1 1 d D . . H32A H 1.1070 0.9509 1.0370 0.085 Uiso 1 1 calc R . . H32B H 1.2284 0.9470 1.0224 0.085 Uiso 1 1 calc R . . C33 C 1.1479(4) 0.8253(3) 1.0350(3) 0.0504(9) Uani 1 1 d . . . H33A H 1.2267 0.8141 1.0490 0.060 Uiso 1 1 calc R . . H33B H 1.1315 0.8384 1.0936 0.060 Uiso 1 1 calc R . . C48 C 0.4707(14) 0.0829(8) 0.0256(14) 0.226(7) Uani 1 1 d D . . H48 H 0.4487 0.1402 0.0409 0.271 Uiso 1 1 calc R . . C46 C 0.4987(14) -0.0528(14) 0.0522(13) 0.251(10) Uani 1 1 d D . . H46 H 0.4963 -0.0919 0.0872 0.301 Uiso 1 1 calc R . . C47 C 0.4719(13) 0.0316(15) 0.0803(8) 0.238(8) Uani 1 1 d D . . H47 H 0.4548 0.0532 0.1357 0.285 Uiso 1 1 calc R . . C36 C 0.8356(7) 0.6816(5) 0.3449(5) 0.108(2) Uani 1 1 d D . . H36A H 0.7587 0.6348 0.2937 0.130 Uiso 1 1 calc R . . H36B H 0.8837 0.7062 0.3142 0.130 Uiso 1 1 calc R . . O5 O 0.9068(10) 0.6806(8) 0.4981(6) 0.206(4) Uani 1 1 d D . . C35 C 0.8142(8) 0.7632(6) 0.4130(7) 0.133(3) Uani 1 1 d D . . H35A H 0.7284 0.7487 0.4008 0.159 Uiso 1 1 calc R . . H35B H 0.8400 0.8238 0.4058 0.159 Uiso 1 1 calc R . . C37 C 0.9012(14) 0.6358(8) 0.4047(7) 0.197(6) Uani 1 1 d D . . H37A H 0.8588 0.5660 0.3772 0.237 Uiso 1 1 calc R . . H37B H 0.9828 0.6443 0.4067 0.237 Uiso 1 1 calc R . . C34 C 0.8885(13) 0.7714(8) 0.5126(7) 0.192(6) Uani 1 1 d D . . H34A H 0.9658 0.8229 0.5422 0.231 Uiso 1 1 calc R . . H34B H 0.8457 0.7860 0.5551 0.231 Uiso 1 1 calc R . . O7 O 0.7321(9) 0.3531(6) 0.4127(5) 0.192(4) Uani 1 1 d D . . C45 C 0.7168(11) 0.2603(8) 0.4055(7) 0.151(4) Uani 1 1 d D . . H45A H 0.6430 0.2372 0.4133 0.181 Uiso 1 1 calc R . . H45B H 0.7851 0.2587 0.4579 0.181 Uiso 1 1 calc R . . C40 C 0.3029(10) 0.0135(7) 0.2942(7) 0.167(5) Uani 1 1 d D . . H40A H 0.3440 0.0001 0.2502 0.200 Uiso 1 1 calc R . . H40B H 0.2344 -0.0440 0.2718 0.200 Uiso 1 1 calc R . . C41 C 0.3895(11) 0.0394(7) 0.3983(7) 0.167(5) Uani 1 1 d D . . H41A H 0.3536 0.0000 0.4260 0.200 Uiso 1 1 calc R . . H41B H 0.4648 0.0259 0.3992 0.200 Uiso 1 1 calc R . . C42 C 0.8090(12) 0.3640(11) 0.3651(13) 0.251(11) Uani 1 1 d D . . H42A H 0.8937 0.3886 0.4119 0.302 Uiso 1 1 calc R . . H42B H 0.7931 0.4101 0.3351 0.302 Uiso 1 1 calc R . . C44 C 0.7084(15) 0.1959(8) 0.3110(7) 0.227(8) Uani 1 1 d D . . H44A H 0.6248 0.1683 0.2619 0.272 Uiso 1 1 calc R . . H44B H 0.7423 0.1432 0.3159 0.272 Uiso 1 1 calc R . . C38 C 0.3578(15) 0.1713(7) 0.3840(10) 0.201(6) Uani 1 1 d D . . H38A H 0.4191 0.2018 0.3668 0.241 Uiso 1 1 calc R . . H38B H 0.3261 0.2218 0.4141 0.241 Uiso 1 1 calc R . . C43 C 0.7839(17) 0.2658(13) 0.2886(11) 0.272(12) Uani 1 1 d D . . H43A H 0.8593 0.2512 0.2920 0.327 Uiso 1 1 calc R . . H43B H 0.7398 0.2627 0.2233 0.327 Uiso 1 1 calc R . . C39 C 0.2619(13) 0.0991(9) 0.2969(11) 0.235(8) Uani 1 1 d D . . H39A H 0.2564 0.1131 0.2398 0.282 Uiso 1 1 calc R . . H39B H 0.1840 0.0916 0.3020 0.282 Uiso 1 1 calc R . . O6 O 0.413(2) 0.1361(9) 0.4525(10) 0.494(18) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Yb1 0.02803(7) 0.02016(7) 0.02347(7) 0.00630(5) 0.00744(5) 0.00836(5) P1 0.0474(5) 0.0444(5) 0.0287(4) 0.0120(4) 0.0013(4) 0.0173(4) O1 0.0331(11) 0.0257(11) 0.0247(10) 0.0025(8) 0.0077(9) 0.0102(9) O2 0.0220(9) 0.0214(10) 0.0321(10) 0.0069(8) 0.0071(8) 0.0039(8) O3 0.0501(15) 0.0517(16) 0.0338(13) 0.0162(11) -0.0002(11) 0.0172(12) O4 0.0540(15) 0.0342(13) 0.0521(15) 0.0240(12) 0.0231(13) 0.0101(11) N1 0.071(2) 0.058(2) 0.054(2) 0.0193(18) 0.0076(19) 0.034(2) N2 0.056(2) 0.058(2) 0.055(2) 0.0133(18) 0.0069(18) 0.0096(18) N3 0.067(2) 0.073(3) 0.0399(18) 0.0240(18) 0.0130(17) 0.024(2) C1 0.0261(14) 0.0230(14) 0.0263(13) 0.0044(11) 0.0117(11) 0.0046(11) C2 0.0319(15) 0.0240(14) 0.0320(15) 0.0054(12) 0.0148(12) 0.0074(12) C3 0.0426(18) 0.0293(16) 0.0334(16) 0.0004(13) 0.0188(14) 0.0089(13) C4 0.0424(19) 0.0409(19) 0.0271(15) 0.0015(14) 0.0114(14) 0.0073(15) C5 0.0352(17) 0.0411(19) 0.0271(15) 0.0081(13) 0.0088(13) 0.0107(14) C6 0.0289(14) 0.0261(15) 0.0286(14) 0.0089(12) 0.0122(12) 0.0072(11) C7 0.0184(12) 0.0221(14) 0.0334(14) 0.0101(11) 0.0082(11) 0.0065(10) C8 0.0262(14) 0.0260(15) 0.0395(16) 0.0094(13) 0.0148(13) 0.0089(11) C9 0.0271(15) 0.0310(17) 0.051(2) 0.0109(15) 0.0187(14) 0.0046(12) C10 0.0255(15) 0.0280(16) 0.052(2) 0.0037(14) 0.0105(14) -0.0006(12) C11 0.0288(15) 0.0281(16) 0.0339(16) 0.0015(13) 0.0080(13) 0.0047(12) C12 0.0225(13) 0.0257(15) 0.0324(15) 0.0096(12) 0.0087(12) 0.0072(11) C13 0.0297(15) 0.0272(15) 0.0301(14) 0.0089(12) 0.0115(12) 0.0088(12) C14 0.0371(17) 0.0248(15) 0.0384(17) 0.0065(13) 0.0162(14) 0.0135(13) C15 0.050(2) 0.0349(18) 0.0463(19) 0.0169(15) 0.0227(17) 0.0186(15) C16 0.052(2) 0.0359(19) 0.054(2) 0.0070(16) 0.0246(18) 0.0226(16) C17 0.0323(17) 0.0375(19) 0.050(2) 0.0115(15) 0.0136(15) 0.0128(14) C18 0.075(3) 0.067(3) 0.0288(19) -0.0041(18) 0.0115(19) 0.023(2) C19 0.0388(17) 0.0314(17) 0.0438(18) 0.0105(14) 0.0242(15) 0.0130(13) C20 0.055(2) 0.070(3) 0.0347(18) 0.0131(18) 0.0192(17) 0.026(2) C21 0.062(2) 0.038(2) 0.066(3) 0.0166(18) 0.041(2) 0.0245(18) C22 0.065(3) 0.043(2) 0.069(3) 0.0156(19) 0.048(2) 0.0122(19) C23 0.035(2) 0.047(2) 0.072(3) -0.003(2) 0.017(2) -0.0100(17) C24 0.077(4) 0.114(5) 0.093(4) 0.056(4) 0.021(3) 0.059(4) C25 0.120(5) 0.059(3) 0.076(4) 0.007(3) 0.028(4) 0.041(3) C26 0.073(3) 0.054(3) 0.057(3) 0.007(2) -0.012(2) 0.011(2) C27 0.056(3) 0.088(4) 0.090(4) 0.030(3) 0.028(3) 0.015(3) C28 0.116(5) 0.131(6) 0.056(3) 0.057(4) 0.026(3) 0.045(5) C29 0.080(4) 0.082(4) 0.056(3) 0.016(3) 0.029(3) 0.027(3) C30 0.097(4) 0.057(3) 0.063(3) 0.038(2) 0.038(3) 0.024(3) C31 0.352(16) 0.044(4) 0.084(5) 0.037(3) 0.040(7) -0.011(6) C32 0.088(4) 0.040(2) 0.093(4) 0.034(2) 0.043(3) 0.010(2) C33 0.047(2) 0.035(2) 0.065(3) 0.0197(18) 0.0213(19) 0.0065(16) C48 0.29(2) 0.219(16) 0.25(2) 0.160(16) 0.137(16) 0.113(15) C46 0.260(18) 0.29(2) 0.35(3) 0.21(2) 0.18(2) 0.182(18) C47 0.225(18) 0.26(2) 0.232(17) 0.122(18) 0.092(14) 0.039(16) C36 0.115(6) 0.102(5) 0.105(5) 0.034(4) 0.057(5) 0.019(4) O5 0.299(12) 0.241(10) 0.146(7) 0.108(7) 0.118(7) 0.133(9) C35 0.135(7) 0.098(6) 0.162(9) 0.030(6) 0.080(7) 0.035(5) C37 0.35(2) 0.161(10) 0.140(9) 0.072(8) 0.131(12) 0.137(12) C34 0.284(17) 0.132(9) 0.131(9) 0.003(7) 0.111(11) 0.036(10) O7 0.222(10) 0.166(8) 0.115(5) 0.032(5) 0.007(6) 0.060(7) C45 0.227(12) 0.165(10) 0.140(8) 0.106(8) 0.099(8) 0.114(9) C40 0.164(10) 0.110(7) 0.140(9) 0.020(6) -0.006(7) 0.031(7) C41 0.173(10) 0.088(6) 0.168(10) 0.006(6) 0.040(8) 0.024(6) C42 0.152(12) 0.30(2) 0.39(3) 0.26(2) 0.114(16) 0.048(13) C44 0.42(2) 0.166(11) 0.118(8) 0.064(8) 0.105(12) 0.149(14) C38 0.290(18) 0.061(5) 0.188(12) 0.034(7) 0.046(12) 0.041(8) C43 0.45(3) 0.38(3) 0.250(18) 0.23(2) 0.29(2) 0.27(3) C39 0.193(14) 0.155(12) 0.275(19) 0.100(13) 0.000(13) 0.023(11) O6 0.59(3) 0.192(13) 0.42(3) 0.111(16) -0.06(2) 0.039(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 O1 2.201(2) . ? Yb1 O3 2.309(2) . ? Yb1 O2 2.327(2) 2_767 ? Yb1 O2 2.349(2) . ? Yb1 O4 2.494(2) . ? Yb1 C7 3.071(3) . ? Yb1 Yb1 3.6927(4) 2_767 ? P1 O3 1.488(2) . ? P1 N1 1.629(4) . ? P1 N2 1.629(4) . ? P1 N3 1.644(4) . ? O1 C1 1.326(3) . ? O2 C7 1.349(3) . ? O2 Yb1 2.327(2) 2_767 ? O4 C30 1.439(5) . ? O4 C33 1.458(5) . ? N1 C25 1.449(6) . ? N1 C24 1.473(6) . ? N2 C26 1.467(6) . ? N2 C27 1.469(7) . ? N3 C29 1.469(7) . ? N3 C28 1.474(6) . ? C1 C6 1.420(4) . ? C1 C2 1.433(4) . ? C2 C3 1.400(4) . ? C2 C14 1.538(4) . ? C3 C4 1.388(5) . ? C3 H3 0.9500 . ? C4 C5 1.391(5) . ? C4 C18 1.517(5) . ? C5 C6 1.399(4) . ? C5 H5 0.9500 . ? C6 C13 1.517(4) . ? C7 C12 1.415(4) . ? C7 C8 1.419(4) . ? C8 C9 1.401(4) . ? C8 C19 1.552(4) . ? C9 C10 1.390(5) . ? C9 H9 0.9500 . ? C10 C11 1.377(5) . ? C10 C23 1.525(5) . ? C11 C12 1.403(4) . ? C11 H11 0.9500 . ? C12 C13 1.524(4) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.528(5) . ? C14 C17 1.539(5) . ? C14 C16 1.542(4) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.532(5) . ? C19 C22 1.537(5) . ? C19 C21 1.540(5) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.481(6) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.488(7) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.510(6) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C48 C47 1.355(9) . ? C48 C46 1.384(8) 2_655 ? C48 H48 0.9500 . ? C46 C47 1.368(9) . ? C46 C48 1.384(8) 2_655 ? C46 H46 0.9500 . ? C47 H47 0.9500 . ? C36 C37 1.483(8) . ? C36 C35 1.504(7) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? O5 C37 1.405(8) . ? O5 C34 1.412(8) . ? C35 C34 1.510(8) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? O7 C45 1.373(8) . ? O7 C42 1.427(9) . ? C45 C44 1.478(8) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C40 C39 1.485(9) . ? C40 C41 1.534(8) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 O6 1.383(9) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.511(9) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C44 C43 1.516(9) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C38 O6 1.410(9) . ? C38 C39 1.439(14) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Yb1 O3 117.00(9) . . ? O1 Yb1 O2 108.41(8) . 2_767 ? O3 Yb1 O2 92.05(9) . 2_767 ? O1 Yb1 O2 107.98(7) . . ? O3 Yb1 O2 134.95(9) . . ? O2 Yb1 O2 75.69(8) 2_767 . ? O1 Yb1 O4 85.15(9) . . ? O3 Yb1 O4 83.01(10) . . ? O2 Yb1 O4 166.33(8) 2_767 . ? O2 Yb1 O4 98.81(8) . . ? O1 Yb1 C7 91.44(8) . . ? O3 Yb1 C7 145.05(10) . . ? O2 Yb1 C7 97.95(7) 2_767 . ? O2 Yb1 C7 24.50(7) . . ? O4 Yb1 C7 79.46(8) . . ? O1 Yb1 Yb1 113.29(6) . 2_767 ? O3 Yb1 Yb1 118.16(7) . 2_767 ? O2 Yb1 Yb1 38.06(5) 2_767 2_767 ? O2 Yb1 Yb1 37.64(5) . 2_767 ? O4 Yb1 Yb1 135.22(6) . 2_767 ? C7 Yb1 Yb1 60.54(5) . 2_767 ? O3 P1 N1 109.76(18) . . ? O3 P1 N2 115.9(2) . . ? N1 P1 N2 103.9(2) . . ? O3 P1 N3 108.76(19) . . ? N1 P1 N3 110.4(2) . . ? N2 P1 N3 108.0(2) . . ? C1 O1 Yb1 150.98(19) . . ? C7 O2 Yb1 138.16(18) . 2_767 ? C7 O2 Yb1 109.27(16) . . ? Yb1 O2 Yb1 104.31(8) 2_767 . ? P1 O3 Yb1 173.28(19) . . ? C30 O4 C33 108.4(3) . . ? C30 O4 Yb1 131.0(3) . . ? C33 O4 Yb1 120.6(2) . . ? C25 N1 C24 113.6(5) . . ? C25 N1 P1 122.1(4) . . ? C24 N1 P1 124.3(4) . . ? C26 N2 C27 114.3(5) . . ? C26 N2 P1 124.2(4) . . ? C27 N2 P1 118.3(4) . . ? C29 N3 C28 115.0(4) . . ? C29 N3 P1 121.1(3) . . ? C28 N3 P1 121.8(4) . . ? O1 C1 C6 119.2(3) . . ? O1 C1 C2 122.0(3) . . ? C6 C1 C2 118.9(3) . . ? C3 C2 C1 117.9(3) . . ? C3 C2 C14 121.6(3) . . ? C1 C2 C14 120.4(3) . . ? C4 C3 C2 123.6(3) . . ? C4 C3 H3 118.2 . . ? C2 C3 H3 118.2 . . ? C3 C4 C5 117.8(3) . . ? C3 C4 C18 120.8(3) . . ? C5 C4 C18 121.4(4) . . ? C4 C5 C6 121.7(3) . . ? C4 C5 H5 119.1 . . ? C6 C5 H5 119.1 . . ? C5 C6 C1 120.0(3) . . ? C5 C6 C13 120.5(3) . . ? C1 C6 C13 119.5(3) . . ? O2 C7 C12 119.5(3) . . ? O2 C7 C8 121.0(3) . . ? C12 C7 C8 119.6(3) . . ? O2 C7 Yb1 46.23(12) . . ? C12 C7 Yb1 96.37(17) . . ? C8 C7 Yb1 124.9(2) . . ? C9 C8 C7 118.0(3) . . ? C9 C8 C19 120.6(3) . . ? C7 C8 C19 121.4(3) . . ? C10 C9 C8 123.1(3) . . ? C10 C9 H9 118.5 . . ? C8 C9 H9 118.5 . . ? C11 C10 C9 118.1(3) . . ? C11 C10 C23 121.3(3) . . ? C9 C10 C23 120.5(3) . . ? C10 C11 C12 121.9(3) . . ? C10 C11 H11 119.0 . . ? C12 C11 H11 119.0 . . ? C11 C12 C7 119.4(3) . . ? C11 C12 C13 118.6(3) . . ? C7 C12 C13 121.9(3) . . ? C6 C13 C12 114.6(3) . . ? C6 C13 H13A 108.6 . . ? C12 C13 H13A 108.6 . . ? C6 C13 H13B 108.6 . . ? C12 C13 H13B 108.6 . . ? H13A C13 H13B 107.6 . . ? C15 C14 C2 109.9(3) . . ? C15 C14 C17 109.9(3) . . ? C2 C14 C17 109.8(3) . . ? C15 C14 C16 107.3(3) . . ? C2 C14 C16 112.4(3) . . ? C17 C14 C16 107.4(3) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C4 C18 H18A 109.5 . . ? C4 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C4 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C22 107.3(3) . . ? C20 C19 C21 109.9(3) . . ? C22 C19 C21 107.3(3) . . ? C20 C19 C8 111.8(3) . . ? C22 C19 C8 111.9(3) . . ? C21 C19 C8 108.6(3) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C10 C23 H23A 109.5 . . ? C10 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C10 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N1 C24 H24A 109.5 . . ? N1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N1 C25 H25A 109.5 . . ? N1 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N1 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N2 C26 H26A 109.5 . . ? N2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N2 C27 H27A 109.5 . . ? N2 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N2 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N3 C28 H28A 109.5 . . ? N3 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? N3 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N3 C29 H29A 109.5 . . ? N3 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N3 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O4 C30 C31 106.7(4) . . ? O4 C30 H30A 110.4 . . ? C31 C30 H30A 110.4 . . ? O4 C30 H30B 110.4 . . ? C31 C30 H30B 110.4 . . ? H30A C30 H30B 108.6 . . ? C30 C31 C32 107.8(4) . . ? C30 C31 H31A 110.1 . . ? C32 C31 H31A 110.1 . . ? C30 C31 H31B 110.1 . . ? C32 C31 H31B 110.1 . . ? H31A C31 H31B 108.5 . . ? C31 C32 C33 105.7(4) . . ? C31 C32 H32A 110.6 . . ? C33 C32 H32A 110.6 . . ? C31 C32 H32B 110.6 . . ? C33 C32 H32B 110.6 . . ? H32A C32 H32B 108.7 . . ? O4 C33 C32 105.8(3) . . ? O4 C33 H33A 110.6 . . ? C32 C33 H33A 110.6 . . ? O4 C33 H33B 110.6 . . ? C32 C33 H33B 110.6 . . ? H33A C33 H33B 108.7 . . ? C47 C48 C46 120.8(7) . 2_655 ? C47 C48 H48 119.6 . . ? C46 C48 H48 119.6 2_655 . ? C47 C46 C48 122.0(8) . 2_655 ? C47 C46 H46 119.0 . . ? C48 C46 H46 119.0 2_655 . ? C48 C47 C46 117.1(8) . . ? C48 C47 H47 121.4 . . ? C46 C47 H47 121.4 . . ? C37 C36 C35 105.9(7) . . ? C37 C36 H36A 110.6 . . ? C35 C36 H36A 110.6 . . ? C37 C36 H36B 110.6 . . ? C35 C36 H36B 110.6 . . ? H36A C36 H36B 108.7 . . ? C37 O5 C34 110.3(7) . . ? C36 C35 C34 104.8(7) . . ? C36 C35 H35A 110.8 . . ? C34 C35 H35A 110.8 . . ? C36 C35 H35B 110.8 . . ? C34 C35 H35B 110.8 . . ? H35A C35 H35B 108.9 . . ? O5 C37 C36 107.4(7) . . ? O5 C37 H37A 110.2 . . ? C36 C37 H37A 110.2 . . ? O5 C37 H37B 110.2 . . ? C36 C37 H37B 110.2 . . ? H37A C37 H37B 108.5 . . ? O5 C34 C35 105.1(7) . . ? O5 C34 H34A 110.7 . . ? C35 C34 H34A 110.7 . . ? O5 C34 H34B 110.7 . . ? C35 C34 H34B 110.7 . . ? H34A C34 H34B 108.8 . . ? C45 O7 C42 103.4(8) . . ? O7 C45 C44 110.9(7) . . ? O7 C45 H45A 109.5 . . ? C44 C45 H45A 109.5 . . ? O7 C45 H45B 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 108.1 . . ? C39 C40 C41 105.4(8) . . ? C39 C40 H40A 110.7 . . ? C41 C40 H40A 110.7 . . ? C39 C40 H40B 110.7 . . ? C41 C40 H40B 110.7 . . ? H40A C40 H40B 108.8 . . ? O6 C41 C40 109.0(9) . . ? O6 C41 H41A 109.9 . . ? C40 C41 H41A 109.9 . . ? O6 C41 H41B 109.9 . . ? C40 C41 H41B 109.9 . . ? H41A C41 H41B 108.3 . . ? O7 C42 C43 107.2(8) . . ? O7 C42 H42A 110.3 . . ? C43 C42 H42A 110.3 . . ? O7 C42 H42B 110.3 . . ? C43 C42 H42B 110.3 . . ? H42A C42 H42B 108.5 . . ? C45 C44 C43 100.8(8) . . ? C45 C44 H44A 111.6 . . ? C43 C44 H44A 111.6 . . ? C45 C44 H44B 111.6 . . ? C43 C44 H44B 111.6 . . ? H44A C44 H44B 109.4 . . ? O6 C38 C39 114.4(9) . . ? O6 C38 H38A 108.7 . . ? C39 C38 H38A 108.7 . . ? O6 C38 H38B 108.7 . . ? C39 C38 H38B 108.7 . . ? H38A C38 H38B 107.6 . . ? C42 C43 C44 105.0(8) . . ? C42 C43 H43A 110.7 . . ? C44 C43 H43A 110.7 . . ? C42 C43 H43B 110.7 . . ? C44 C43 H43B 110.7 . . ? H43A C43 H43B 108.8 . . ? C38 C39 C40 99.6(9) . . ? C38 C39 H39A 111.8 . . ? C40 C39 H39A 111.8 . . ? C38 C39 H39B 111.8 . . ? C40 C39 H39B 111.8 . . ? H39A C39 H39B 109.6 . . ? C41 O6 C38 104.0(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Yb1 O1 C1 -173.9(4) . . . . ? O2 Yb1 O1 C1 83.9(4) 2_767 . . . ? O2 Yb1 O1 C1 3.5(4) . . . . ? O4 Yb1 O1 C1 -94.2(4) . . . . ? C7 Yb1 O1 C1 -14.9(4) . . . . ? Yb1 Yb1 O1 C1 43.4(4) 2_767 . . . ? O1 Yb1 O2 C7 -49.6(2) . . . . ? O3 Yb1 O2 C7 127.0(2) . . . . ? O2 Yb1 O2 C7 -154.6(2) 2_767 . . . ? O4 Yb1 O2 C7 38.1(2) . . . . ? Yb1 Yb1 O2 C7 -154.6(2) 2_767 . . . ? O1 Yb1 O2 Yb1 105.06(9) . . . 2_767 ? O3 Yb1 O2 Yb1 -78.32(14) . . . 2_767 ? O2 Yb1 O2 Yb1 0.0 2_767 . . 2_767 ? O4 Yb1 O2 Yb1 -167.21(9) . . . 2_767 ? C7 Yb1 O2 Yb1 154.6(2) . . . 2_767 ? N1 P1 O3 Yb1 3.6(18) . . . . ? N2 P1 O3 Yb1 -113.7(17) . . . . ? N3 P1 O3 Yb1 124.5(17) . . . . ? O1 Yb1 O3 P1 5.3(18) . . . . ? O2 Yb1 O3 P1 117.2(17) 2_767 . . . ? O2 Yb1 O3 P1 -171.1(17) . . . . ? O4 Yb1 O3 P1 -75.6(17) . . . . ? C7 Yb1 O3 P1 -135.8(17) . . . . ? Yb1 Yb1 O3 P1 146.2(17) 2_767 . . . ? O1 Yb1 O4 C30 -137.9(4) . . . . ? O3 Yb1 O4 C30 -19.9(4) . . . . ? O2 Yb1 O4 C30 49.5(6) 2_767 . . . ? O2 Yb1 O4 C30 114.7(4) . . . . ? C7 Yb1 O4 C30 129.8(4) . . . . ? Yb1 Yb1 O4 C30 103.6(4) 2_767 . . . ? O1 Yb1 O4 C33 41.4(3) . . . . ? O3 Yb1 O4 C33 159.4(3) . . . . ? O2 Yb1 O4 C33 -131.2(3) 2_767 . . . ? O2 Yb1 O4 C33 -66.1(3) . . . . ? C7 Yb1 O4 C33 -51.0(3) . . . . ? Yb1 Yb1 O4 C33 -77.1(3) 2_767 . . . ? O3 P1 N1 C25 24.4(5) . . . . ? N2 P1 N1 C25 149.0(5) . . . . ? N3 P1 N1 C25 -95.5(5) . . . . ? O3 P1 N1 C24 -158.3(5) . . . . ? N2 P1 N1 C24 -33.7(5) . . . . ? N3 P1 N1 C24 81.8(5) . . . . ? O3 P1 N2 C26 -100.9(4) . . . . ? N1 P1 N2 C26 138.5(4) . . . . ? N3 P1 N2 C26 21.3(4) . . . . ? O3 P1 N2 C27 58.0(4) . . . . ? N1 P1 N2 C27 -62.5(4) . . . . ? N3 P1 N2 C27 -179.8(4) . . . . ? O3 P1 N3 C29 34.9(4) . . . . ? N1 P1 N3 C29 155.4(4) . . . . ? N2 P1 N3 C29 -91.6(4) . . . . ? O3 P1 N3 C28 -162.8(4) . . . . ? N1 P1 N3 C28 -42.3(5) . . . . ? N2 P1 N3 C28 70.7(5) . . . . ? Yb1 O1 C1 C6 -13.7(6) . . . . ? Yb1 O1 C1 C2 166.0(3) . . . . ? O1 C1 C2 C3 180.0(3) . . . . ? C6 C1 C2 C3 -0.3(4) . . . . ? O1 C1 C2 C14 -0.1(5) . . . . ? C6 C1 C2 C14 179.6(3) . . . . ? C1 C2 C3 C4 -0.7(5) . . . . ? C14 C2 C3 C4 179.4(3) . . . . ? C2 C3 C4 C5 0.9(6) . . . . ? C2 C3 C4 C18 -179.8(4) . . . . ? C3 C4 C5 C6 0.0(6) . . . . ? C18 C4 C5 C6 -179.3(4) . . . . ? C4 C5 C6 C1 -1.1(5) . . . . ? C4 C5 C6 C13 179.3(3) . . . . ? O1 C1 C6 C5 -179.1(3) . . . . ? C2 C1 C6 C5 1.2(5) . . . . ? O1 C1 C6 C13 0.5(4) . . . . ? C2 C1 C6 C13 -179.2(3) . . . . ? Yb1 O2 C7 C12 -72.9(4) 2_767 . . . ? Yb1 O2 C7 C12 68.6(3) . . . . ? Yb1 O2 C7 C8 108.0(3) 2_767 . . . ? Yb1 O2 C7 C8 -110.4(3) . . . . ? Yb1 O2 C7 Yb1 -141.5(3) 2_767 . . . ? O1 Yb1 C7 O2 133.58(19) . . . . ? O3 Yb1 C7 O2 -80.5(2) . . . . ? O2 Yb1 C7 O2 24.8(2) 2_767 . . . ? O4 Yb1 C7 O2 -141.6(2) . . . . ? Yb1 Yb1 C7 O2 17.47(16) 2_767 . . . ? O1 Yb1 C7 C12 8.24(19) . . . . ? O3 Yb1 C7 C12 154.20(19) . . . . ? O2 Yb1 C7 C12 -100.57(19) 2_767 . . . ? O2 Yb1 C7 C12 -125.3(3) . . . . ? O4 Yb1 C7 C12 93.04(19) . . . . ? Yb1 Yb1 C7 C12 -107.86(19) 2_767 . . . ? O1 Yb1 C7 C8 -124.8(2) . . . . ? O3 Yb1 C7 C8 21.1(3) . . . . ? O2 Yb1 C7 C8 126.3(2) 2_767 . . . ? O2 Yb1 C7 C8 101.6(3) . . . . ? O4 Yb1 C7 C8 -40.1(2) . . . . ? Yb1 Yb1 C7 C8 119.1(2) 2_767 . . . ? O2 C7 C8 C9 179.2(3) . . . . ? C12 C7 C8 C9 0.1(4) . . . . ? Yb1 C7 C8 C9 123.6(3) . . . . ? O2 C7 C8 C19 -3.2(4) . . . . ? C12 C7 C8 C19 177.8(3) . . . . ? Yb1 C7 C8 C19 -58.8(4) . . . . ? C7 C8 C9 C10 0.2(5) . . . . ? C19 C8 C9 C10 -177.5(3) . . . . ? C8 C9 C10 C11 -0.7(6) . . . . ? C8 C9 C10 C23 178.2(4) . . . . ? C9 C10 C11 C12 0.8(5) . . . . ? C23 C10 C11 C12 -178.0(4) . . . . ? C10 C11 C12 C7 -0.5(5) . . . . ? C10 C11 C12 C13 175.3(3) . . . . ? O2 C7 C12 C11 -179.0(3) . . . . ? C8 C7 C12 C11 0.0(4) . . . . ? Yb1 C7 C12 C11 -136.5(3) . . . . ? O2 C7 C12 C13 5.3(4) . . . . ? C8 C7 C12 C13 -175.7(3) . . . . ? Yb1 C7 C12 C13 47.8(3) . . . . ? C5 C6 C13 C12 -96.9(4) . . . . ? C1 C6 C13 C12 83.4(3) . . . . ? C11 C12 C13 C6 51.7(4) . . . . ? C7 C12 C13 C6 -132.5(3) . . . . ? C3 C2 C14 C15 119.8(3) . . . . ? C1 C2 C14 C15 -60.0(4) . . . . ? C3 C2 C14 C17 -119.2(3) . . . . ? C1 C2 C14 C17 61.0(4) . . . . ? C3 C2 C14 C16 0.4(5) . . . . ? C1 C2 C14 C16 -179.5(3) . . . . ? C9 C8 C19 C20 -127.7(4) . . . . ? C7 C8 C19 C20 54.7(4) . . . . ? C9 C8 C19 C22 -7.3(5) . . . . ? C7 C8 C19 C22 175.1(3) . . . . ? C9 C8 C19 C21 110.9(4) . . . . ? C7 C8 C19 C21 -66.7(4) . . . . ? C33 O4 C30 C31 -22.6(7) . . . . ? Yb1 O4 C30 C31 156.7(6) . . . . ? O4 C30 C31 C32 11.9(10) . . . . ? C30 C31 C32 C33 2.7(10) . . . . ? C30 O4 C33 C32 24.2(5) . . . . ? Yb1 O4 C33 C32 -155.3(3) . . . . ? C31 C32 C33 O4 -16.1(7) . . . . ? C46 C48 C47 C46 -3.1(16) 2_655 . . . ? C48 C46 C47 C48 3.1(17) 2_655 . . . ? C37 C36 C35 C34 9.9(12) . . . . ? C34 O5 C37 C36 -20.5(16) . . . . ? C35 C36 C37 O5 5.5(14) . . . . ? C37 O5 C34 C35 26.6(16) . . . . ? C36 C35 C34 O5 -21.8(13) . . . . ? C42 O7 C45 C44 -37.7(14) . . . . ? C39 C40 C41 O6 -9.7(19) . . . . ? C45 O7 C42 C43 29.8(16) . . . . ? O7 C45 C44 C43 29.2(15) . . . . ? O7 C42 C43 C44 -12.2(19) . . . . ? C45 C44 C43 C42 -8.9(17) . . . . ? O6 C38 C39 C40 -29(2) . . . . ? C41 C40 C39 C38 21.4(16) . . . . ? C40 C41 O6 C38 -7(2) . . . . ? C39 C38 O6 C41 24(3) . . . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 1.214 _refine_diff_density_min -0.887 _refine_diff_density_rms 0.079 data_shelxl_b _database_code_depnum_ccdc_archive 'CCDC 219108' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C84 H160 N12 O8 P4 Sm2' _chemical_formula_sum 'C84 H160 N12 O8 P4 Sm2' _chemical_formula_weight 1890.82 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 '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_space_group_name_Hall '-C 2yc' _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 32.122(2) _cell_length_b 14.5658(9) _cell_length_c 21.2482(13) _cell_angle_alpha 90.00 _cell_angle_beta 100.534(2) _cell_angle_gamma 90.00 _cell_volume 9774.0(11) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 10082 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description platelet _exptl_crystal_colour black _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.285 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3984 _exptl_absorpt_coefficient_mu 1.310 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5605 _exptl_absorpt_correction_T_max 0.9139 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.62 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53026 _diffrn_reflns_av_R_equivalents 0.0473 _diffrn_reflns_av_sigmaI/netI 0.0327 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 27.48 _reflns_number_total 11067 _reflns_number_gt 10824 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0001P)^2^+42.3423P] 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 11067 _refine_ls_number_parameters 569 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0579 _refine_ls_R_factor_gt 0.0554 _refine_ls_wR_factor_ref 0.0959 _refine_ls_wR_factor_gt 0.0952 _refine_ls_goodness_of_fit_ref 1.373 _refine_ls_restrained_S_all 1.381 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm1 Sm 0.197363(6) 0.178099(13) 1.014382(9) 0.02377(6) Uani 1 1 d . . . P1 P 0.20863(3) -0.06037(7) 1.10793(5) 0.0301(2) Uani 1 1 d . . . P2 P 0.09660(4) 0.21115(8) 1.09496(5) 0.0348(2) Uani 1 1 d . . . O1 O 0.15329(9) 0.15229(19) 0.91592(12) 0.0312(6) Uani 1 1 d . . . O2 O 0.22689(8) 0.33467(17) 0.99278(12) 0.0263(5) Uani 1 1 d . . . O3 O 0.20802(10) 0.0272(2) 1.07235(13) 0.0374(7) Uani 1 1 d . . . O4 O 0.13994(10) 0.1912(2) 1.08398(14) 0.0430(7) Uani 1 1 d . . . N1 N 0.18890(13) -0.0447(3) 1.17280(17) 0.0415(9) Uani 1 1 d . . . N2 N 0.25499(12) -0.1087(3) 1.13013(18) 0.0427(9) Uani 1 1 d . . . N3 N 0.18203(13) -0.1394(3) 1.06231(17) 0.0425(9) Uani 1 1 d . . . N4 N 0.07372(15) 0.2995(3) 1.0549(2) 0.0520(10) Uani 1 1 d . . . N5 N 0.09738(13) 0.2292(3) 1.17176(18) 0.0459(10) Uani 1 1 d . . . N6 N 0.06393(12) 0.1264(3) 1.07187(18) 0.0432(9) Uani 1 1 d . . . C1 C 0.13152(12) 0.1786(3) 0.85945(16) 0.0262(7) Uani 1 1 d . . . C2 C 0.09685(12) 0.1267(3) 0.82565(17) 0.0263(8) Uani 1 1 d . . . C3 C 0.07434(12) 0.1615(3) 0.76788(18) 0.0289(8) Uani 1 1 d . . . H3 H 0.0506 0.1278 0.7465 0.035 Uiso 1 1 calc R . . C4 C 0.08477(12) 0.2429(3) 0.74005(18) 0.0293(8) Uani 1 1 d . . . C5 C 0.12014(12) 0.2902(3) 0.77260(18) 0.0284(8) Uani 1 1 d . . . H5 H 0.1287 0.3450 0.7543 0.034 Uiso 1 1 calc R . . C6 C 0.14317(12) 0.2604(3) 0.83036(17) 0.0254(7) Uani 1 1 d . . . C7 C 0.19386(11) 0.3907(2) 0.97522(17) 0.0237(7) Uani 1 1 d . . . C8 C 0.18182(12) 0.4563(3) 1.01812(17) 0.0276(8) Uani 1 1 d . . . C9 C 0.14707(12) 0.5134(3) 0.99599(18) 0.0294(8) Uani 1 1 d . . . H9 H 0.1392 0.5574 1.0247 0.035 Uiso 1 1 calc R . . C10 C 0.12323(13) 0.5091(3) 0.93371(19) 0.0324(9) Uani 1 1 d . . . C11 C 0.13504(13) 0.4423(3) 0.89369(19) 0.0325(9) Uani 1 1 d . . . H11 H 0.1192 0.4365 0.8515 0.039 Uiso 1 1 calc R . . C12 C 0.16916(12) 0.3836(2) 0.91291(17) 0.0267(8) Uani 1 1 d . . . C13 C 0.18111(12) 0.3137(3) 0.86522(17) 0.0266(7) Uani 1 1 d . . . H13 H 0.2004 0.2680 0.8909 0.032 Uiso 1 1 calc R . . C14 C 0.08536(13) 0.0331(3) 0.85087(18) 0.0311(8) Uani 1 1 d . . . C15 C 0.07364(13) 0.0434(3) 0.91762(19) 0.0348(9) Uani 1 1 d . . . H15A H 0.0688 -0.0175 0.9346 0.052 Uiso 1 1 calc R . . H15B H 0.0478 0.0802 0.9143 0.052 Uiso 1 1 calc R . . H15C H 0.0968 0.0739 0.9464 0.052 Uiso 1 1 calc R . . C16 C 0.12304(14) -0.0325(3) 0.8533(2) 0.0389(10) Uani 1 1 d . . . H16A H 0.1289 -0.0411 0.8100 0.058 Uiso 1 1 calc R . . H16B H 0.1162 -0.0918 0.8706 0.058 Uiso 1 1 calc R . . H16C H 0.1481 -0.0063 0.8808 0.058 Uiso 1 1 calc R . . C17 C 0.04692(15) -0.0115(3) 0.8080(2) 0.0427(11) Uani 1 1 d . . . H17A H 0.0528 -0.0195 0.7647 0.064 Uiso 1 1 calc R . . H17B H 0.0221 0.0281 0.8064 0.064 Uiso 1 1 calc R . . H17C H 0.0413 -0.0714 0.8257 0.064 Uiso 1 1 calc R . . C18 C 0.05980(14) 0.2780(3) 0.6758(2) 0.0405(10) Uani 1 1 d D . . C19A C 0.0216(3) 0.2204(7) 0.6492(4) 0.059(2) Uani 0.60 1 d P . . H19A H 0.0011 0.2233 0.6781 0.088 Uiso 0.60 1 calc PR . . H19B H 0.0304 0.1566 0.6452 0.088 Uiso 0.60 1 calc PR . . H19C H 0.0085 0.2438 0.6069 0.088 Uiso 0.60 1 calc PR . . C19B C 0.0147(4) 0.3003(13) 0.6873(7) 0.075(5) Uani 0.40 1 d PD . . H19D H 0.0140 0.2956 0.7331 0.113 Uiso 0.40 1 calc PR . . H19E H -0.0055 0.2565 0.6635 0.113 Uiso 0.40 1 calc PR . . H19F H 0.0070 0.3627 0.6724 0.113 Uiso 0.40 1 calc PR . . C20A C 0.0900(3) 0.2677(9) 0.6261(4) 0.072(3) Uani 0.60 1 d PD . . H20A H 0.1184 0.2505 0.6485 0.108 Uiso 0.60 1 calc PR . . H20B H 0.0915 0.3261 0.6038 0.108 Uiso 0.60 1 calc PR . . H20C H 0.0791 0.2199 0.5950 0.108 Uiso 0.60 1 calc PR . . C20B C 0.0565(6) 0.2064(10) 0.6261(6) 0.068(4) Uani 0.40 1 d P . . H20D H 0.0326 0.1659 0.6292 0.103 Uiso 0.40 1 calc PR . . H20E H 0.0827 0.1704 0.6325 0.103 Uiso 0.40 1 calc PR . . H20F H 0.0520 0.2353 0.5838 0.103 Uiso 0.40 1 calc PR . . C21A C 0.0502(4) 0.3782(7) 0.6775(6) 0.073(3) Uani 0.60 1 d P . . H21A H 0.0313 0.3893 0.7081 0.110 Uiso 0.60 1 calc PR . . H21B H 0.0363 0.3985 0.6349 0.110 Uiso 0.60 1 calc PR . . H21C H 0.0765 0.4126 0.6908 0.110 Uiso 0.60 1 calc PR . . C21B C 0.0780(5) 0.3650(11) 0.6536(6) 0.059(4) Uani 0.40 1 d P . . H21D H 0.0676 0.4178 0.6747 0.089 Uiso 0.40 1 calc PR . . H21E H 0.0692 0.3709 0.6071 0.089 Uiso 0.40 1 calc PR . . H21F H 0.1089 0.3627 0.6645 0.089 Uiso 0.40 1 calc PR . . C22 C 0.20745(13) 0.4661(3) 1.08698(18) 0.0310(8) Uani 1 1 d . . . C23 C 0.21471(16) 0.3723(3) 1.1206(2) 0.0450(11) Uani 1 1 d . . . H23A H 0.2359 0.3376 1.1026 0.067 Uiso 1 1 calc R . . H23B H 0.1880 0.3380 1.1142 0.067 Uiso 1 1 calc R . . H23C H 0.2249 0.3817 1.1666 0.067 Uiso 1 1 calc R . . C24 C 0.18472(16) 0.5261(4) 1.1296(2) 0.0476(12) Uani 1 1 d . . . H24A H 0.2019 0.5298 1.1727 0.071 Uiso 1 1 calc R . . H24B H 0.1571 0.4990 1.1321 0.071 Uiso 1 1 calc R . . H24C H 0.1806 0.5879 1.1113 0.071 Uiso 1 1 calc R . . C25 C 0.25011(14) 0.5113(3) 1.0842(2) 0.0427(11) Uani 1 1 d . . . H25A H 0.2643 0.4774 1.0543 0.064 Uiso 1 1 calc R . . H25B H 0.2679 0.5106 1.1269 0.064 Uiso 1 1 calc R . . H25C H 0.2455 0.5749 1.0696 0.064 Uiso 1 1 calc R . . C26 C 0.08623(15) 0.5754(3) 0.9105(2) 0.0420(10) Uani 1 1 d . . . C27A C 0.0535(3) 0.5693(9) 0.9549(6) 0.081(3) Uani 0.60 1 d P . . H27A H 0.0675 0.5821 0.9990 0.121 Uiso 0.60 1 calc PR . . H27B H 0.0413 0.5075 0.9525 0.121 Uiso 0.60 1 calc PR . . H27C H 0.0310 0.6145 0.9415 0.121 Uiso 0.60 1 calc PR . . C27B C 0.0761(6) 0.6344(11) 0.9645(7) 0.069(5) Uani 0.40 1 d P . . H27D H 0.0994 0.6305 1.0013 0.103 Uiso 0.40 1 calc PR . . H27E H 0.0499 0.6125 0.9769 0.103 Uiso 0.40 1 calc PR . . H27F H 0.0724 0.6983 0.9502 0.103 Uiso 0.40 1 calc PR . . C28A C 0.0624(4) 0.5541(8) 0.8420(5) 0.070(3) Uani 0.60 1 d P . . H28A H 0.0393 0.5983 0.8301 0.105 Uiso 0.60 1 calc PR . . H28B H 0.0507 0.4919 0.8407 0.105 Uiso 0.60 1 calc PR . . H28C H 0.0820 0.5587 0.8119 0.105 Uiso 0.60 1 calc PR . . C28B C 0.0474(4) 0.5206(10) 0.8813(9) 0.065(4) Uani 0.40 1 d P . . H28D H 0.0352 0.4920 0.9154 0.097 Uiso 0.40 1 calc PR . . H28E H 0.0555 0.4728 0.8534 0.097 Uiso 0.40 1 calc PR . . H28F H 0.0265 0.5615 0.8561 0.097 Uiso 0.40 1 calc PR . . C29A C 0.1018(4) 0.6737(7) 0.9116(8) 0.082(4) Uani 0.60 1 d P . . H29A H 0.1170 0.6888 0.9546 0.122 Uiso 0.60 1 calc PR . . H29B H 0.0775 0.7151 0.9001 0.122 Uiso 0.60 1 calc PR . . H29C H 0.1208 0.6808 0.8807 0.122 Uiso 0.60 1 calc PR . . C29B C 0.0988(6) 0.6389(15) 0.8615(11) 0.096(8) Uani 0.40 1 d P . . H29D H 0.1201 0.6824 0.8828 0.145 Uiso 0.40 1 calc PR . . H29E H 0.0738 0.6726 0.8399 0.145 Uiso 0.40 1 calc PR . . H29F H 0.1107 0.6030 0.8300 0.145 Uiso 0.40 1 calc PR . . C30 C 0.20674(15) 0.3601(3) 0.8198(2) 0.0427(11) Uani 1 1 d . . . H30A H 0.2163 0.3136 0.7923 0.064 Uiso 1 1 calc R . . H30B H 0.2313 0.3912 0.8449 0.064 Uiso 1 1 calc R . . H30C H 0.1889 0.4051 0.7931 0.064 Uiso 1 1 calc R . . C31 C 0.18742(17) 0.0445(4) 1.2027(2) 0.0500(12) Uani 1 1 d . . . H31A H 0.1592 0.0543 1.2128 0.075 Uiso 1 1 calc R . . H31B H 0.1934 0.0925 1.1733 0.075 Uiso 1 1 calc R . . H31C H 0.2087 0.0469 1.2421 0.075 Uiso 1 1 calc R . . C32 C 0.1795(2) -0.1211(4) 1.2127(3) 0.0710(18) Uani 1 1 d . . . H32A H 0.1971 -0.1160 1.2554 0.106 Uiso 1 1 calc R . . H32B H 0.1855 -0.1793 1.1930 0.106 Uiso 1 1 calc R . . H32C H 0.1495 -0.1190 1.2164 0.106 Uiso 1 1 calc R . . C33 C 0.2808(2) -0.1038(5) 1.1928(3) 0.0750(18) Uani 1 1 d . . . H33A H 0.2852 -0.1657 1.2108 0.112 Uiso 1 1 calc R . . H33B H 0.2666 -0.0659 1.2206 0.112 Uiso 1 1 calc R . . H33C H 0.3082 -0.0764 1.1897 0.112 Uiso 1 1 calc R . . C34 C 0.2797(2) -0.1367(5) 1.0829(3) 0.086(2) Uani 1 1 d . . . H34A H 0.3039 -0.0953 1.0846 0.129 Uiso 1 1 calc R . . H34B H 0.2620 -0.1342 1.0402 0.129 Uiso 1 1 calc R . . H34C H 0.2899 -0.1996 1.0920 0.129 Uiso 1 1 calc R . . C35 C 0.1485(2) -0.1148(4) 1.0100(3) 0.076(2) Uani 1 1 d . . . H35A H 0.1526 -0.1468 0.9711 0.114 Uiso 1 1 calc R . . H35B H 0.1489 -0.0483 1.0029 0.114 Uiso 1 1 calc R . . H35C H 0.1211 -0.1324 1.0205 0.114 Uiso 1 1 calc R . . C36 C 0.1887(2) -0.2363(4) 1.0702(3) 0.0752(19) Uani 1 1 d . . . H36A H 0.1631 -0.2651 1.0803 0.113 Uiso 1 1 calc R . . H36B H 0.2126 -0.2476 1.1052 0.113 Uiso 1 1 calc R . . H36C H 0.1950 -0.2626 1.0305 0.113 Uiso 1 1 calc R . . C37 C 0.0729(2) 0.3006(4) 0.9854(3) 0.0722(18) Uani 1 1 d . . . H37A H 0.0457 0.3252 0.9634 0.108 Uiso 1 1 calc R . . H37B H 0.0765 0.2379 0.9705 0.108 Uiso 1 1 calc R . . H37C H 0.0959 0.3393 0.9761 0.108 Uiso 1 1 calc R . . C38 C 0.0710(2) 0.3895(4) 1.0828(3) 0.0670(16) Uani 1 1 d . . . H38A H 0.0933 0.4290 1.0717 0.101 Uiso 1 1 calc R . . H38B H 0.0747 0.3839 1.1294 0.101 Uiso 1 1 calc R . . H38C H 0.0433 0.4165 1.0660 0.101 Uiso 1 1 calc R . . C39 C 0.13429(18) 0.2666(4) 1.2141(2) 0.0613(15) Uani 1 1 d . . . H39A H 0.1293 0.3313 1.2228 0.092 Uiso 1 1 calc R . . H39B H 0.1591 0.2614 1.1936 0.092 Uiso 1 1 calc R . . H39C H 0.1393 0.2322 1.2544 0.092 Uiso 1 1 calc R . . C40 C 0.0588(2) 0.2303(5) 1.1990(3) 0.0685(17) Uani 1 1 d . . . H40A H 0.0644 0.2012 1.2413 0.103 Uiso 1 1 calc R . . H40B H 0.0364 0.1964 1.1709 0.103 Uiso 1 1 calc R . . H40C H 0.0497 0.2939 1.2031 0.103 Uiso 1 1 calc R . . C41 C 0.01858(17) 0.1345(5) 1.0490(3) 0.0678(17) Uani 1 1 d . . . H41A H 0.0104 0.0975 1.0102 0.102 Uiso 1 1 calc R . . H41B H 0.0113 0.1990 1.0392 0.102 Uiso 1 1 calc R . . H41C H 0.0034 0.1126 1.0821 0.102 Uiso 1 1 calc R . . C42 C 0.0779(2) 0.0337(4) 1.0923(3) 0.0712(18) Uani 1 1 d . . . H42A H 0.0670 0.0175 1.1311 0.107 Uiso 1 1 calc R . . H42B H 0.1089 0.0315 1.1014 0.107 Uiso 1 1 calc R . . H42C H 0.0671 -0.0101 1.0582 0.107 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 Sm1 0.02354(10) 0.02560(9) 0.02141(9) 0.00108(8) 0.00215(7) -0.00522(8) P1 0.0337(6) 0.0312(5) 0.0252(5) 0.0066(4) 0.0048(4) -0.0006(4) P2 0.0339(6) 0.0377(6) 0.0351(6) -0.0034(4) 0.0123(5) -0.0070(5) O1 0.0305(15) 0.0347(15) 0.0260(13) 0.0021(11) -0.0014(11) -0.0040(11) O2 0.0259(13) 0.0234(13) 0.0285(13) 0.0003(10) 0.0027(10) -0.0003(10) O3 0.0482(18) 0.0349(15) 0.0305(14) 0.0070(12) 0.0106(13) -0.0046(13) O4 0.0358(17) 0.054(2) 0.0422(17) 0.0004(15) 0.0154(13) -0.0028(14) N1 0.055(2) 0.040(2) 0.0341(19) 0.0077(16) 0.0197(17) -0.0026(18) N2 0.037(2) 0.053(2) 0.037(2) 0.0118(17) 0.0048(16) 0.0065(18) N3 0.052(2) 0.0338(19) 0.0357(19) 0.0050(15) -0.0069(17) 0.0002(17) N4 0.063(3) 0.041(2) 0.050(2) -0.0018(18) 0.004(2) -0.002(2) N5 0.046(2) 0.057(2) 0.039(2) -0.0106(18) 0.0178(18) -0.0091(19) N6 0.043(2) 0.044(2) 0.045(2) -0.0035(17) 0.0130(17) -0.0125(17) C1 0.0269(18) 0.0295(18) 0.0216(16) -0.0019(15) 0.0028(14) 0.0001(16) C2 0.0271(19) 0.0305(19) 0.0213(17) -0.0021(14) 0.0042(14) -0.0027(15) C3 0.0256(19) 0.033(2) 0.0267(18) -0.0018(15) 0.0006(15) -0.0061(15) C4 0.0271(19) 0.035(2) 0.0248(18) -0.0002(15) 0.0015(15) -0.0015(16) C5 0.031(2) 0.0269(18) 0.0276(18) 0.0009(15) 0.0055(15) -0.0007(15) C6 0.0275(19) 0.0261(18) 0.0234(17) -0.0051(14) 0.0066(14) -0.0014(15) C7 0.0255(18) 0.0205(16) 0.0247(17) 0.0017(14) 0.0042(14) -0.0062(14) C8 0.0296(19) 0.0285(19) 0.0246(18) -0.0021(15) 0.0047(15) -0.0049(15) C9 0.030(2) 0.0268(19) 0.032(2) -0.0079(15) 0.0053(16) -0.0015(15) C10 0.032(2) 0.0281(19) 0.035(2) -0.0009(16) 0.0025(17) 0.0020(16) C11 0.033(2) 0.031(2) 0.0292(19) -0.0032(16) -0.0042(16) -0.0007(16) C12 0.030(2) 0.0227(17) 0.0264(18) -0.0016(14) 0.0036(15) -0.0034(15) C13 0.0287(19) 0.0252(18) 0.0247(17) -0.0036(14) 0.0016(15) -0.0034(15) C14 0.033(2) 0.032(2) 0.0271(19) 0.0001(16) 0.0018(16) -0.0061(17) C15 0.035(2) 0.040(2) 0.030(2) 0.0037(17) 0.0083(17) -0.0052(18) C16 0.047(3) 0.031(2) 0.039(2) 0.0008(18) 0.0083(19) 0.0001(19) C17 0.047(3) 0.039(2) 0.038(2) 0.0013(19) -0.002(2) -0.018(2) C18 0.041(3) 0.047(3) 0.030(2) 0.0122(19) -0.0039(18) -0.005(2) C19A 0.042(5) 0.077(6) 0.047(5) 0.017(5) -0.020(4) -0.016(5) C19B 0.042(7) 0.126(15) 0.056(8) 0.053(10) 0.003(6) 0.022(8) C20A 0.071(7) 0.115(9) 0.028(4) 0.028(5) 0.002(4) -0.003(6) C20B 0.105(13) 0.064(9) 0.028(6) 0.001(6) -0.009(7) 0.000(9) C21A 0.080(8) 0.050(6) 0.077(7) 0.020(5) -0.018(6) 0.013(5) C21B 0.068(10) 0.068(9) 0.035(7) 0.017(6) -0.009(6) -0.019(8) C22 0.032(2) 0.036(2) 0.0249(18) -0.0078(16) 0.0041(16) -0.0022(17) C23 0.057(3) 0.048(3) 0.027(2) 0.0032(19) 0.001(2) -0.003(2) C24 0.049(3) 0.064(3) 0.030(2) -0.012(2) 0.006(2) 0.006(2) C25 0.037(2) 0.050(3) 0.040(2) -0.016(2) 0.0031(19) -0.010(2) C26 0.038(2) 0.038(2) 0.045(3) -0.003(2) -0.004(2) 0.0087(19) C27A 0.052(6) 0.089(9) 0.100(9) 0.017(7) 0.011(6) 0.040(6) C27B 0.081(11) 0.051(8) 0.066(9) -0.013(7) -0.008(8) 0.040(8) C28A 0.058(7) 0.069(7) 0.070(7) -0.004(5) -0.026(5) 0.027(6) C28B 0.036(7) 0.046(8) 0.101(13) -0.019(8) -0.018(8) 0.013(6) C29A 0.055(6) 0.038(5) 0.145(12) 0.002(7) 0.002(8) 0.009(5) C29B 0.084(13) 0.094(15) 0.121(16) 0.075(13) 0.044(13) 0.059(12) C30 0.047(3) 0.048(3) 0.035(2) -0.0100(19) 0.014(2) -0.020(2) C31 0.063(3) 0.057(3) 0.034(2) 0.000(2) 0.020(2) -0.001(3) C32 0.111(5) 0.059(4) 0.051(3) 0.013(3) 0.038(3) -0.019(3) C33 0.062(4) 0.073(4) 0.077(4) -0.001(3) -0.021(3) 0.012(3) C34 0.072(4) 0.104(5) 0.093(5) 0.041(4) 0.046(4) 0.043(4) C35 0.088(5) 0.057(3) 0.065(4) -0.006(3) -0.037(3) 0.001(3) C36 0.103(5) 0.038(3) 0.078(4) -0.003(3) -0.004(4) -0.002(3) C37 0.108(5) 0.056(3) 0.045(3) 0.007(3) -0.007(3) -0.005(3) C38 0.071(4) 0.045(3) 0.090(4) -0.005(3) 0.027(3) 0.006(3) C39 0.064(4) 0.080(4) 0.041(3) -0.018(3) 0.012(3) -0.016(3) C40 0.073(4) 0.086(4) 0.057(3) -0.016(3) 0.040(3) -0.020(3) C41 0.043(3) 0.087(4) 0.076(4) -0.020(3) 0.019(3) -0.027(3) C42 0.111(5) 0.040(3) 0.060(3) -0.002(3) 0.009(3) -0.014(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 O1 2.332(3) . ? Sm1 O2 2.473(3) 7_557 ? Sm1 O3 2.513(3) . ? Sm1 O2 2.544(2) . ? Sm1 O4 2.573(3) . ? P1 O3 1.481(3) . ? P1 N1 1.635(4) . ? P1 N2 1.637(4) . ? P1 N3 1.641(4) . ? P2 O4 1.482(3) . ? P2 N6 1.636(4) . ? P2 N4 1.641(4) . ? P2 N5 1.649(4) . ? O1 C1 1.330(4) . ? O2 C7 1.337(4) . ? O2 Sm1 2.473(3) 7_557 ? N1 C31 1.450(6) . ? N1 C32 1.463(6) . ? N2 C33 1.435(7) . ? N2 C34 1.447(7) . ? N3 C36 1.433(6) . ? N3 C35 1.445(6) . ? N4 C38 1.447(6) . ? N4 C37 1.472(7) . ? N5 C39 1.456(6) . ? N5 C40 1.460(6) . ? N6 C41 1.454(7) . ? N6 C42 1.464(7) . ? C1 C6 1.424(5) . ? C1 C2 1.426(5) . ? C2 C3 1.401(5) . ? C2 C14 1.534(5) . ? C3 C4 1.393(5) . ? C3 H3 0.9500 . ? C4 C5 1.398(5) . ? C4 C18 1.538(5) . ? C5 C6 1.382(5) . ? C5 H5 0.9500 . ? C6 C13 1.519(5) . ? C7 C12 1.418(5) . ? C7 C8 1.422(5) . ? C8 C9 1.402(5) . ? C8 C22 1.549(5) . ? C9 C10 1.404(5) . ? C9 H9 0.9500 . ? C10 C11 1.390(5) . ? C10 C26 1.541(6) . ? C11 C12 1.391(5) . ? C11 H11 0.9500 . ? C12 C13 1.533(5) . ? C13 C30 1.535(5) . ? C13 H13 1.0000 . ? C14 C16 1.535(6) . ? C14 C17 1.538(5) . ? C14 C15 1.540(5) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C20B 1.474(14) . ? C18 C21A 1.494(11) . ? C18 C21B 1.506(14) . ? C18 C19A 1.508(9) . ? C18 C19B 1.546(12) . ? C18 C20A 1.567(9) . ? C19A H19A 0.9800 . ? C19A H19B 0.9800 . ? C19A H19C 0.9800 . ? C19B H19D 0.9800 . ? C19B H19E 0.9800 . ? C19B H19F 0.9800 . ? C20A H20A 0.9800 . ? C20A H20B 0.9800 . ? C20A H20C 0.9800 . ? C20B H20D 0.9800 . ? C20B H20E 0.9800 . ? C20B H20F 0.9800 . ? C21A H21A 0.9800 . ? C21A H21B 0.9800 . ? C21A H21C 0.9800 . ? C21B H21D 0.9800 . ? C21B H21E 0.9800 . ? C21B H21F 0.9800 . ? C22 C25 1.531(6) . ? C22 C24 1.537(6) . ? C22 C23 1.539(6) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C29B 1.500(16) . ? C26 C28B 1.514(14) . ? C26 C29A 1.516(11) . ? C26 C27B 1.516(14) . ? C26 C27A 1.538(12) . ? C26 C28A 1.546(10) . ? C27A H27A 0.9800 . ? C27A H27B 0.9800 . ? C27A H27C 0.9800 . ? C27B H27D 0.9800 . ? C27B H27E 0.9800 . ? C27B H27F 0.9800 . ? C28A H28A 0.9800 . ? C28A H28B 0.9800 . ? C28A H28C 0.9800 . ? C28B H28D 0.9800 . ? C28B H28E 0.9800 . ? C28B H28F 0.9800 . ? C29A H29A 0.9800 . ? C29A H29B 0.9800 . ? C29A H29C 0.9800 . ? C29B H29D 0.9800 . ? C29B H29E 0.9800 . ? C29B H29F 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? 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 Sm1 O2 112.05(9) . 7_557 ? O1 Sm1 O3 107.73(9) . . ? O2 Sm1 O3 85.23(9) 7_557 . ? O1 Sm1 O2 99.66(9) . . ? O2 Sm1 O2 69.68(9) 7_557 . ? O3 Sm1 O2 148.32(9) . . ? O1 Sm1 O4 98.40(10) . . ? O2 Sm1 O4 149.06(9) 7_557 . ? O3 Sm1 O4 80.26(10) . . ? O2 Sm1 O4 111.55(9) . . ? O3 P1 N1 109.83(18) . . ? O3 P1 N2 116.36(19) . . ? N1 P1 N2 106.8(2) . . ? O3 P1 N3 110.22(18) . . ? N1 P1 N3 110.8(2) . . ? N2 P1 N3 102.5(2) . . ? O4 P2 N6 112.0(2) . . ? O4 P2 N4 114.6(2) . . ? N6 P2 N4 103.6(2) . . ? O4 P2 N5 110.0(2) . . ? N6 P2 N5 108.1(2) . . ? N4 P2 N5 108.2(2) . . ? C1 O1 Sm1 153.6(2) . . ? C7 O2 Sm1 140.2(2) . 7_557 ? C7 O2 Sm1 107.2(2) . . ? Sm1 O2 Sm1 110.32(9) 7_557 . ? P1 O3 Sm1 172.59(19) . . ? P2 O4 Sm1 153.85(19) . . ? C31 N1 C32 113.6(4) . . ? C31 N1 P1 122.9(3) . . ? C32 N1 P1 122.3(3) . . ? C33 N2 C34 111.1(5) . . ? C33 N2 P1 125.9(4) . . ? C34 N2 P1 120.5(4) . . ? C36 N3 C35 114.2(4) . . ? C36 N3 P1 124.9(4) . . ? C35 N3 P1 121.0(3) . . ? C38 N4 C37 114.2(4) . . ? C38 N4 P2 123.6(4) . . ? C37 N4 P2 116.9(4) . . ? C39 N5 C40 113.9(4) . . ? C39 N5 P2 122.3(3) . . ? C40 N5 P2 122.3(4) . . ? C41 N6 C42 114.1(5) . . ? C41 N6 P2 126.0(4) . . ? C42 N6 P2 117.5(4) . . ? O1 C1 C6 119.8(3) . . ? O1 C1 C2 122.3(3) . . ? C6 C1 C2 117.9(3) . . ? C3 C2 C1 118.7(3) . . ? C3 C2 C14 120.6(3) . . ? C1 C2 C14 120.7(3) . . ? C4 C3 C2 123.7(3) . . ? C4 C3 H3 118.2 . . ? C2 C3 H3 118.2 . . ? C3 C4 C5 116.5(3) . . ? C3 C4 C18 122.2(4) . . ? C5 C4 C18 121.3(4) . . ? C6 C5 C4 122.6(4) . . ? C6 C5 H5 118.7 . . ? C4 C5 H5 118.7 . . ? C5 C6 C1 120.5(3) . . ? C5 C6 C13 121.6(3) . . ? C1 C6 C13 117.9(3) . . ? O2 C7 C12 119.7(3) . . ? O2 C7 C8 121.8(3) . . ? C12 C7 C8 118.5(3) . . ? C9 C8 C7 118.5(3) . . ? C9 C8 C22 121.0(3) . . ? C7 C8 C22 120.5(3) . . ? C8 C9 C10 123.6(3) . . ? C8 C9 H9 118.2 . . ? C10 C9 H9 118.2 . . ? C11 C10 C9 116.4(4) . . ? C11 C10 C26 121.6(4) . . ? C9 C10 C26 122.0(4) . . ? C10 C11 C12 122.7(4) . . ? C10 C11 H11 118.7 . . ? C12 C11 H11 118.7 . . ? C11 C12 C7 120.3(3) . . ? C11 C12 C13 119.5(3) . . ? C7 C12 C13 120.1(3) . . ? C6 C13 C12 112.7(3) . . ? C6 C13 C30 113.2(3) . . ? C12 C13 C30 110.6(3) . . ? C6 C13 H13 106.6 . . ? C12 C13 H13 106.6 . . ? C30 C13 H13 106.6 . . ? C2 C14 C16 109.0(3) . . ? C2 C14 C17 112.8(3) . . ? C16 C14 C17 107.4(4) . . ? C2 C14 C15 110.5(3) . . ? C16 C14 C15 110.7(3) . . ? C17 C14 C15 106.3(3) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C20B C18 C21A 136.1(8) . . ? C20B C18 C21B 110.6(9) . . ? C21A C18 C21B 44.0(7) . . ? C20B C18 C19A 52.4(8) . . ? C21A C18 C19A 113.3(7) . . ? C21B C18 C19A 133.3(7) . . ? C20B C18 C4 110.9(6) . . ? C21A C18 C4 112.3(5) . . ? C21B C18 C4 112.9(6) . . ? C19A C18 C4 113.9(4) . . ? C20B C18 C19B 108.3(11) . . ? C21A C18 C19B 65.6(9) . . ? C21B C18 C19B 107.5(10) . . ? C19A C18 C19B 57.0(8) . . ? C4 C18 C19B 106.4(6) . . ? C20B C18 C20A 54.7(8) . . ? C21A C18 C20A 105.5(7) . . ? C21B C18 C20A 63.0(8) . . ? C19A C18 C20A 104.8(7) . . ? C4 C18 C20A 106.2(5) . . ? C19B C18 C20A 147.1(7) . . ? C18 C19A H19A 109.5 . . ? C18 C19A H19B 109.5 . . ? H19A C19A H19B 109.5 . . ? C18 C19A H19C 109.5 . . ? H19A C19A H19C 109.5 . . ? H19B C19A H19C 109.5 . . ? C18 C19B H19D 109.5 . . ? C18 C19B H19E 109.5 . . ? H19D C19B H19E 109.5 . . ? C18 C19B H19F 109.5 . . ? H19D C19B H19F 109.5 . . ? H19E C19B H19F 109.5 . . ? C18 C20A H20A 109.5 . . ? C18 C20A H20B 109.5 . . ? H20A C20A H20B 109.5 . . ? C18 C20A H20C 109.5 . . ? H20A C20A H20C 109.5 . . ? H20B C20A H20C 109.5 . . ? C18 C20B H20D 109.5 . . ? C18 C20B H20E 109.5 . . ? H20D C20B H20E 109.5 . . ? C18 C20B H20F 109.5 . . ? H20D C20B H20F 109.5 . . ? H20E C20B H20F 109.5 . . ? C18 C21A H21A 109.5 . . ? C18 C21A H21B 109.5 . . ? H21A C21A H21B 109.5 . . ? C18 C21A H21C 109.5 . . ? H21A C21A H21C 109.5 . . ? H21B C21A H21C 109.5 . . ? C18 C21B H21D 109.5 . . ? C18 C21B H21E 109.5 . . ? H21D C21B H21E 109.5 . . ? C18 C21B H21F 109.5 . . ? H21D C21B H21F 109.5 . . ? H21E C21B H21F 109.5 . . ? C25 C22 C24 107.6(4) . . ? C25 C22 C23 109.8(4) . . ? C24 C22 C23 106.2(4) . . ? C25 C22 C8 109.2(3) . . ? C24 C22 C8 112.4(3) . . ? C23 C22 C8 111.5(3) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C29B C26 C28B 110.3(13) . . ? C29B C26 C29A 45.5(10) . . ? C28B C26 C29A 138.5(8) . . ? C29B C26 C27B 107.3(12) . . ? C28B C26 C27B 109.5(11) . . ? C29A C26 C27B 64.4(9) . . ? C29B C26 C27A 139.6(8) . . ? C28B C26 C27A 67.5(9) . . ? C29A C26 C27A 107.8(8) . . ? C27B C26 C27A 45.8(8) . . ? C29B C26 C10 108.6(7) . . ? C28B C26 C10 109.3(6) . . ? C29A C26 C10 110.8(5) . . ? C27B C26 C10 111.8(6) . . ? C27A C26 C10 109.9(5) . . ? C29B C26 C28A 67.8(11) . . ? C28B C26 C28A 43.9(8) . . ? C29A C26 C28A 108.0(8) . . ? C27B C26 C28A 133.4(7) . . ? C27A C26 C28A 106.8(8) . . ? C10 C26 C28A 113.4(5) . . ? C26 C27A H27A 109.5 . . ? C26 C27A H27B 109.5 . . ? H27A C27A H27B 109.5 . . ? C26 C27A H27C 109.5 . . ? H27A C27A H27C 109.5 . . ? H27B C27A H27C 109.5 . . ? C26 C27B H27D 109.5 . . ? C26 C27B H27E 109.5 . . ? H27D C27B H27E 109.5 . . ? C26 C27B H27F 109.5 . . ? H27D C27B H27F 109.5 . . ? H27E C27B H27F 109.5 . . ? C26 C28A H28A 109.5 . . ? C26 C28A H28B 109.5 . . ? H28A C28A H28B 109.5 . . ? C26 C28A H28C 109.5 . . ? H28A C28A H28C 109.5 . . ? H28B C28A H28C 109.5 . . ? C26 C28B H28D 109.5 . . ? C26 C28B H28E 109.5 . . ? H28D C28B H28E 109.5 . . ? C26 C28B H28F 109.5 . . ? H28D C28B H28F 109.5 . . ? H28E C28B H28F 109.5 . . ? C26 C29A H29A 109.5 . . ? C26 C29A H29B 109.5 . . ? H29A C29A H29B 109.5 . . ? C26 C29A H29C 109.5 . . ? H29A C29A H29C 109.5 . . ? H29B C29A H29C 109.5 . . ? C26 C29B H29D 109.5 . . ? C26 C29B H29E 109.5 . . ? H29D C29B H29E 109.5 . . ? C26 C29B H29F 109.5 . . ? H29D C29B H29F 109.5 . . ? H29E C29B H29F 109.5 . . ? C13 C30 H30A 109.5 . . ? C13 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C13 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N1 C31 H31A 109.5 . . ? N1 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N1 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N1 C32 H32A 109.5 . . ? N1 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N1 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N2 C33 H33A 109.5 . . ? N2 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? N2 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N2 C34 H34A 109.5 . . ? N2 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? N2 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N3 C35 H35A 109.5 . . ? N3 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N3 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N3 C36 H36A 109.5 . . ? N3 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N3 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N4 C37 H37A 109.5 . . ? N4 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? N4 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N4 C38 H38A 109.5 . . ? N4 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? N4 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N5 C39 H39A 109.5 . . ? N5 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? N5 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N5 C40 H40A 109.5 . . ? N5 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? N5 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N6 C41 H41A 109.5 . . ? N6 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? N6 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N6 C42 H42A 109.5 . . ? N6 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? N6 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.068 _refine_diff_density_min -0.656 _refine_diff_density_rms 0.075 #===========================================================END OF CIF