Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Norbert W. Mitzel' _publ_contact_author_address ; Institut fur Anorganische und Analytische Chemie Universitat Munster Corrensstrasse 30 Munster D-48149 GERMANY ; _publ_contact_author_email MITZEL@UNI-MUENSTER.DE _publ_section_title ; Hydroxylaminato Yttrate and Samarate Complexes ; loop_ _publ_author_name 'Norbert Mitzel' 'Alexander Hepp' 'Ajay Venugopal' 'Alexander Willner' data_smon _database_code_depnum_ccdc_archive 'CCDC 643871' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H56 K N4 O4 Sm' _chemical_formula_weight 654.18 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' K K 0.2009 0.2494 '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 Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 15.254(3) _cell_length_b 18.595(2) _cell_length_c 22.165(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6287.3(15) _cell_formula_units_Z 8 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used 2000 _cell_measurement_theta_min 4.24 _cell_measurement_theta_max 26.01 _exptl_crystal_description Needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.382 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2728 _exptl_absorpt_coefficient_mu 2.032 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS-1' _diffrn_measurement_method 'phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 67814 _diffrn_reflns_av_R_equivalents 0.3035 _diffrn_reflns_av_sigmaI/netI 0.1872 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 4.24 _diffrn_reflns_theta_max 26.01 _reflns_number_total 12236 _reflns_number_gt 7310 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE IPDS-1 software package' _computing_cell_refinement 'STOE IPDS-1 software package' _computing_data_reduction 'STOE IPDS-1 software package' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0342P)^2^+0.3783P] 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 geom _refine_ls_extinction_method noref _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(2) _refine_ls_number_reflns 12236 _refine_ls_number_parameters 644 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1529 _refine_ls_R_factor_gt 0.0743 _refine_ls_wR_factor_ref 0.1403 _refine_ls_wR_factor_gt 0.1154 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.023 _refine_ls_shift/su_mean 0.001 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 0.46715(5) 0.46899(3) 0.85157(3) 0.01983(16) Uani 1 1 d . . . Sm2 Sm 0.96721(5) 0.50900(3) 0.89102(3) 0.01968(16) Uani 1 1 d . . . K1 K 0.71760(17) 0.49956(17) 0.88703(15) 0.0255(7) Uani 1 1 d . . . K2 K 1.21845(19) 0.48241(17) 0.85854(15) 0.0277(7) Uani 1 1 d . . . O1 O 0.3633(6) 0.4670(6) 0.7823(5) 0.029(2) Uani 1 1 d . . . N1 N 0.2892(7) 0.4630(7) 0.7438(5) 0.029(3) Uani 1 1 d . . . O2 O 0.3649(5) 0.4744(6) 0.9251(5) 0.030(2) Uani 1 1 d . . . N2 N 0.4265(8) 0.4328(7) 0.9571(7) 0.036(3) Uani 1 1 d . . . O3 O 0.5593(5) 0.5588(5) 0.8808(5) 0.029(3) Uani 1 1 d . . . N3 N 0.4912(7) 0.6029(6) 0.8551(7) 0.032(3) Uani 1 1 d . . . O4 O 0.6005(5) 0.4127(4) 0.8496(5) 0.024(2) Uani 1 1 d . . . N4 N 0.5544(7) 0.3538(6) 0.8253(6) 0.024(3) Uani 1 1 d . . . O5 O 0.8636(5) 0.4983(6) 0.8170(4) 0.033(3) Uani 1 1 d . . . N5 N 0.9237(7) 0.5451(6) 0.7858(5) 0.023(3) Uani 1 1 d . . . O6 O 0.8656(5) 0.5132(5) 0.9614(4) 0.025(2) Uani 1 1 d . . . N6 N 0.7916(7) 0.5187(6) 1.0018(5) 0.024(3) Uani 1 1 d . . . O7 O 1.0982(6) 0.5690(5) 0.8887(6) 0.032(3) Uani 1 1 d . . . N7 N 1.0482(9) 0.6289(6) 0.9111(5) 0.027(3) Uani 1 1 d . . . O8 O 1.0623(6) 0.4188(5) 0.8658(5) 0.028(3) Uani 1 1 d . . . N8 N 0.9956(6) 0.3734(6) 0.8909(6) 0.020(3) Uani 1 1 d . . . C11 C 0.2955(9) 0.5195(9) 0.6967(6) 0.035(4) Uani 1 1 d . . . H11A H 0.2412 0.5159 0.6716 0.041 Uiso 1 1 calc R . . C12 C 0.3721(9) 0.5148(10) 0.6542(7) 0.047(4) Uani 1 1 d . . . H12A H 0.3673 0.4709 0.6300 0.070 Uiso 1 1 calc R . . H12B H 0.4267 0.5136 0.6774 0.070 Uiso 1 1 calc R . . H12C H 0.3722 0.5568 0.6275 0.070 Uiso 1 1 calc R . . C13 C 0.2920(14) 0.5914(10) 0.7287(10) 0.050(5) Uani 1 1 d . . . H13A H 0.2411 0.5927 0.7557 0.075 Uiso 1 1 calc R . . H13B H 0.2871 0.6300 0.6988 0.075 Uiso 1 1 calc R . . H13C H 0.3457 0.5981 0.7523 0.075 Uiso 1 1 calc R . . C14 C 0.2856(13) 0.3886(9) 0.7186(8) 0.038(4) Uani 1 1 d . . . H14A H 0.3428 0.3774 0.6986 0.046 Uiso 1 1 calc R . . C15 C 0.2711(13) 0.3373(11) 0.7684(10) 0.053(5) Uani 1 1 d . . . H15A H 0.3183 0.3421 0.7981 0.079 Uiso 1 1 calc R . . H15B H 0.2708 0.2881 0.7524 0.079 Uiso 1 1 calc R . . H15C H 0.2147 0.3475 0.7878 0.079 Uiso 1 1 calc R . . C16 C 0.2103(15) 0.3790(10) 0.6720(9) 0.064(6) Uani 1 1 d . . . H16A H 0.1997 0.3277 0.6655 0.095 Uiso 1 1 calc R . . H16B H 0.2270 0.4017 0.6338 0.095 Uiso 1 1 calc R . . H16C H 0.1569 0.4017 0.6875 0.095 Uiso 1 1 calc R . . C21 C 0.4724(13) 0.4774(9) 1.0017(6) 0.045(4) Uani 1 1 d . . . H21A H 0.5085 0.5119 0.9775 0.054 Uiso 1 1 calc R . . C22 C 0.5393(16) 0.4305(10) 1.0361(8) 0.055(5) Uani 1 1 d . . . H22A H 0.5724 0.4012 1.0072 0.083 Uiso 1 1 calc R . . H22B H 0.5082 0.3989 1.0643 0.083 Uiso 1 1 calc R . . H22C H 0.5798 0.4615 1.0585 0.083 Uiso 1 1 calc R . . C23 C 0.4203(12) 0.5233(11) 1.0440(8) 0.061(6) Uani 1 1 d . . . H23A H 0.3796 0.5532 1.0208 0.091 Uiso 1 1 calc R . . H23B H 0.4600 0.5541 1.0671 0.091 Uiso 1 1 calc R . . H23C H 0.3872 0.4925 1.0717 0.091 Uiso 1 1 calc R . . C25 C 0.3424(14) 0.3269(10) 0.9290(10) 0.063(6) Uani 1 1 d . . . H25A H 0.3857 0.3211 0.8967 0.095 Uiso 1 1 calc R . . H25B H 0.2921 0.3542 0.9139 0.095 Uiso 1 1 calc R . . H25C H 0.3227 0.2794 0.9427 0.095 Uiso 1 1 calc R . . C26 C 0.3138(13) 0.3830(12) 1.0296(10) 0.062(6) Uani 1 1 d . . . H26A H 0.3412 0.3877 1.0694 0.094 Uiso 1 1 calc R . . H26B H 0.2716 0.3433 1.0303 0.094 Uiso 1 1 calc R . . H26C H 0.2835 0.4278 1.0194 0.094 Uiso 1 1 calc R . . C31 C 0.5261(13) 0.6456(7) 0.8060(7) 0.031(3) Uani 1 1 d . . . H31A H 0.4754 0.6711 0.7870 0.037 Uiso 1 1 calc R . . C32 C 0.5944(10) 0.7019(9) 0.8202(9) 0.041(5) Uani 1 1 d . . . H32A H 0.5679 0.7401 0.8447 0.062 Uiso 1 1 calc R . . H32B H 0.6168 0.7225 0.7826 0.062 Uiso 1 1 calc R . . H32C H 0.6427 0.6798 0.8426 0.062 Uiso 1 1 calc R . . C33 C 0.5624(12) 0.5947(10) 0.7593(10) 0.056(6) Uani 1 1 d . . . H33A H 0.5146 0.5655 0.7426 0.083 Uiso 1 1 calc R . . H33B H 0.6060 0.5631 0.7781 0.083 Uiso 1 1 calc R . . H33C H 0.5901 0.6223 0.7268 0.083 Uiso 1 1 calc R . . C34 C 0.4471(10) 0.6458(9) 0.9035(8) 0.040(4) Uani 1 1 d . . . H34A H 0.4121 0.6097 0.9267 0.048 Uiso 1 1 calc R . . C24 C 0.3844(12) 0.3676(11) 0.9823(9) 0.054(5) Uani 1 1 d . . . H24A H 0.4306 0.3365 1.0008 0.065 Uiso 1 1 calc R . . C35 C 0.3806(12) 0.6980(10) 0.8801(10) 0.052(5) Uani 1 1 d . . . H35A H 0.3384 0.6726 0.8544 0.078 Uiso 1 1 calc R . . H35B H 0.4101 0.7354 0.8565 0.078 Uiso 1 1 calc R . . H35C H 0.3496 0.7202 0.9141 0.078 Uiso 1 1 calc R . . C36 C 0.5045(12) 0.6807(12) 0.9499(10) 0.061(7) Uani 1 1 d . . . H36A H 0.5461 0.6453 0.9659 0.091 Uiso 1 1 calc R . . H36B H 0.4682 0.6992 0.9829 0.091 Uiso 1 1 calc R . . H36C H 0.5369 0.7205 0.9314 0.091 Uiso 1 1 calc R . . C41 C 0.5594(10) 0.2949(8) 0.8699(8) 0.035(4) Uani 1 1 d . . . H41A H 0.5274 0.3130 0.9062 0.042 Uiso 1 1 calc R . . C42 C 0.5103(11) 0.2285(9) 0.8503(9) 0.052(5) Uani 1 1 d . . . H42A H 0.4537 0.2425 0.8329 0.078 Uiso 1 1 calc R . . H42B H 0.5005 0.1972 0.8852 0.078 Uiso 1 1 calc R . . H42C H 0.5447 0.2026 0.8199 0.078 Uiso 1 1 calc R . . C43 C 0.6492(12) 0.2741(9) 0.8921(9) 0.052(5) Uani 1 1 d . . . H43A H 0.6833 0.3176 0.9004 0.078 Uiso 1 1 calc R . . H43B H 0.6791 0.2455 0.8611 0.078 Uiso 1 1 calc R . . H43C H 0.6436 0.2457 0.9291 0.078 Uiso 1 1 calc R . . C61 C 0.7947(10) 0.5908(8) 1.0285(8) 0.032(4) Uani 1 1 d . . . H61A H 0.8518 0.5968 1.0501 0.039 Uiso 1 1 calc R . . C44 C 0.5882(11) 0.3357(9) 0.7656(8) 0.037(4) Uani 1 1 d . . . H44A H 0.5613 0.2883 0.7550 0.044 Uiso 1 1 calc R . . C45 C 0.5556(12) 0.3881(11) 0.7189(9) 0.060(6) Uani 1 1 d . . . H45A H 0.4921 0.3944 0.7234 0.090 Uiso 1 1 calc R . . H45B H 0.5684 0.3694 0.6785 0.090 Uiso 1 1 calc R . . H45C H 0.5850 0.4345 0.7243 0.090 Uiso 1 1 calc R . . C62 C 0.7885(13) 0.6476(10) 0.9790(10) 0.052(6) Uani 1 1 d . . . H62A H 0.8366 0.6409 0.9503 0.078 Uiso 1 1 calc R . . H62B H 0.7925 0.6956 0.9970 0.078 Uiso 1 1 calc R . . H62C H 0.7323 0.6427 0.9579 0.078 Uiso 1 1 calc R . . C63 C 0.7208(13) 0.6009(11) 1.0734(10) 0.065(6) Uani 1 1 d . . . H63A H 0.7362 0.5776 1.1116 0.097 Uiso 1 1 calc R . . H63B H 0.6670 0.5793 1.0573 0.097 Uiso 1 1 calc R . . H63C H 0.7112 0.6524 1.0802 0.097 Uiso 1 1 calc R . . C46 C 0.6864(13) 0.3255(13) 0.7593(10) 0.069(7) Uani 1 1 d . . . H46A H 0.7033 0.2792 0.7771 0.103 Uiso 1 1 calc R . . H46B H 0.7170 0.3645 0.7803 0.103 Uiso 1 1 calc R . . H46C H 0.7024 0.3260 0.7165 0.103 Uiso 1 1 calc R . . C51 C 0.9782(10) 0.5045(9) 0.7430(6) 0.039(4) Uani 1 1 d . . . H51A H 1.0148 0.4716 0.7682 0.047 Uiso 1 1 calc R . . C52 C 1.0421(13) 0.5542(10) 0.7120(7) 0.049(5) Uani 1 1 d . . . H52A H 1.0792 0.5776 0.7423 0.074 Uiso 1 1 calc R . . H52B H 1.0097 0.5909 0.6894 0.074 Uiso 1 1 calc R . . H52C H 1.0789 0.5265 0.6842 0.074 Uiso 1 1 calc R . . C53 C 0.9311(12) 0.4561(11) 0.6983(8) 0.055(5) Uani 1 1 d . . . H53A H 0.8772 0.4376 0.7167 0.082 Uiso 1 1 calc R . . H53B H 0.9693 0.4158 0.6873 0.082 Uiso 1 1 calc R . . H53C H 0.9163 0.4837 0.6620 0.082 Uiso 1 1 calc R . . C54 C 0.8770(10) 0.6091(9) 0.7633(8) 0.038(4) Uani 1 1 d . . . H54A H 0.9213 0.6429 0.7460 0.046 Uiso 1 1 calc R . . C55 C 0.8305(11) 0.6471(9) 0.8136(8) 0.043(4) Uani 1 1 d . . . H55A H 0.8692 0.6500 0.8488 0.064 Uiso 1 1 calc R . . H55B H 0.7773 0.6203 0.8243 0.064 Uiso 1 1 calc R . . H55C H 0.8145 0.6957 0.8006 0.064 Uiso 1 1 calc R . . C56 C 0.8086(13) 0.5916(12) 0.7135(8) 0.056(6) Uani 1 1 d . . . H56A H 0.8391 0.5765 0.6767 0.084 Uiso 1 1 calc R . . H56B H 0.7734 0.6346 0.7050 0.084 Uiso 1 1 calc R . . H56C H 0.7702 0.5528 0.7273 0.084 Uiso 1 1 calc R . . C64 C 0.7959(10) 0.4609(9) 1.0454(7) 0.034(4) Uani 1 1 d . . . H64A H 0.7414 0.4642 1.0704 0.041 Uiso 1 1 calc R . . C65 C 0.7922(13) 0.3891(9) 1.0125(9) 0.043(5) Uani 1 1 d . . . H65A H 0.7442 0.3899 0.9832 0.064 Uiso 1 1 calc R . . H65B H 0.7823 0.3504 1.0417 0.064 Uiso 1 1 calc R . . H65C H 0.8479 0.3809 0.9915 0.064 Uiso 1 1 calc R . . C66 C 0.8733(11) 0.4638(11) 1.0892(8) 0.052(5) Uani 1 1 d . . . H66A H 0.8744 0.5107 1.1093 0.078 Uiso 1 1 calc R . . H66B H 0.9281 0.4567 1.0669 0.078 Uiso 1 1 calc R . . H66C H 0.8669 0.4257 1.1195 0.078 Uiso 1 1 calc R . . C71 C 1.0527(10) 0.6869(8) 0.8653(7) 0.033(4) Uani 1 1 d . . . H71A H 1.0203 0.6673 0.8297 0.040 Uiso 1 1 calc R . . C72 C 0.9982(11) 0.7511(9) 0.8856(10) 0.047(5) Uani 1 1 d . . . H72A H 0.9435 0.7340 0.9038 0.071 Uiso 1 1 calc R . . H72B H 0.9847 0.7815 0.8507 0.071 Uiso 1 1 calc R . . H72C H 1.0314 0.7790 0.9154 0.071 Uiso 1 1 calc R . . C73 C 1.1419(11) 0.7080(10) 0.8405(8) 0.045(5) Uani 1 1 d . . . H73A H 1.1809 0.6662 0.8413 0.068 Uiso 1 1 calc R . . H73B H 1.1668 0.7465 0.8653 0.068 Uiso 1 1 calc R . . H73C H 1.1354 0.7249 0.7988 0.068 Uiso 1 1 calc R . . C74 C 1.0856(11) 0.6494(9) 0.9713(9) 0.039(4) Uani 1 1 d . . . H74A H 1.0610 0.6977 0.9815 0.047 Uiso 1 1 calc R . . C75 C 1.1823(17) 0.655(2) 0.9763(11) 0.148(17) Uani 1 1 d . . . H75A H 1.2032 0.6937 0.9496 0.222 Uiso 1 1 calc R . . H75B H 1.2093 0.6097 0.9645 0.222 Uiso 1 1 calc R . . H75C H 1.1982 0.6667 1.0180 0.222 Uiso 1 1 calc R . . C76 C 1.0547(15) 0.5993(14) 1.0186(8) 0.080(8) Uani 1 1 d . . . H76A H 1.0616 0.6217 1.0583 0.120 Uiso 1 1 calc R . . H76B H 1.0892 0.5549 1.0170 0.120 Uiso 1 1 calc R . . H76C H 0.9927 0.5880 1.0118 0.120 Uiso 1 1 calc R . . C81 C 1.0338(15) 0.3334(7) 0.9415(7) 0.033(3) Uani 1 1 d . . . H81A H 0.9850 0.3049 0.9597 0.040 Uiso 1 1 calc R . . C82 C 1.1049(12) 0.2805(10) 0.9263(9) 0.046(5) Uani 1 1 d . . . H82A H 1.0793 0.2391 0.9053 0.069 Uiso 1 1 calc R . . H82B H 1.1334 0.2643 0.9635 0.069 Uiso 1 1 calc R . . H82C H 1.1483 0.3036 0.9001 0.069 Uiso 1 1 calc R . . C83 C 1.0631(11) 0.3861(10) 0.9891(8) 0.044(5) Uani 1 1 d . . . H83A H 1.0164 0.4213 0.9964 0.065 Uiso 1 1 calc R . . H83B H 1.1160 0.4112 0.9753 0.065 Uiso 1 1 calc R . . H83C H 1.0759 0.3603 1.0266 0.065 Uiso 1 1 calc R . . C84 C 0.9557(12) 0.3320(8) 0.8405(8) 0.040(5) Uani 1 1 d . . . H84A H 0.9195 0.3670 0.8169 0.048 Uiso 1 1 calc R . . C85 C 1.0159(13) 0.2970(11) 0.7962(9) 0.055(5) Uani 1 1 d . . . H85A H 1.0611 0.3314 0.7837 0.082 Uiso 1 1 calc R . . H85B H 0.9823 0.2815 0.7608 0.082 Uiso 1 1 calc R . . H85C H 1.0437 0.2552 0.8150 0.082 Uiso 1 1 calc R . . C86 C 0.8902(12) 0.2751(10) 0.8665(12) 0.060(6) Uani 1 1 d . . . H86A H 0.8512 0.2984 0.8957 0.090 Uiso 1 1 calc R . . H86B H 0.9231 0.2366 0.8864 0.090 Uiso 1 1 calc R . . H86C H 0.8552 0.2549 0.8335 0.090 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 0.0161(3) 0.0214(4) 0.0220(4) -0.0009(3) -0.0001(4) -0.0004(4) Sm2 0.0153(3) 0.0227(4) 0.0211(3) -0.0019(3) 0.0001(3) 0.0010(3) K1 0.0173(14) 0.0287(18) 0.0306(16) -0.0009(17) 0.0002(13) -0.0042(13) K2 0.0171(15) 0.0323(18) 0.0338(18) -0.0032(17) 0.0010(13) 0.0046(11) O1 0.018(5) 0.041(6) 0.028(6) -0.010(5) -0.002(4) 0.003(4) N1 0.022(6) 0.038(7) 0.027(7) -0.005(6) -0.005(5) -0.002(5) O2 0.018(5) 0.042(7) 0.031(6) 0.003(5) 0.002(4) 0.004(4) N2 0.027(7) 0.037(8) 0.044(9) 0.008(7) -0.004(6) 0.002(6) O3 0.013(5) 0.027(5) 0.049(7) 0.009(5) -0.010(4) 0.009(3) N3 0.034(8) 0.029(7) 0.032(8) 0.003(7) -0.001(6) 0.009(5) O4 0.008(4) 0.018(5) 0.046(7) -0.014(5) -0.002(4) -0.003(3) N4 0.018(8) 0.019(6) 0.035(8) -0.002(6) -0.003(5) 0.005(4) O5 0.022(5) 0.051(7) 0.028(6) 0.013(6) 0.001(4) -0.007(5) N5 0.016(5) 0.031(7) 0.021(6) 0.007(6) -0.003(5) -0.001(5) O6 0.020(5) 0.040(6) 0.017(5) -0.004(5) 0.002(4) -0.003(4) N6 0.018(6) 0.027(7) 0.026(6) -0.001(6) 0.004(5) 0.003(5) O7 0.030(6) 0.022(5) 0.045(8) -0.020(6) 0.000(5) 0.000(4) N7 0.041(9) 0.015(5) 0.024(7) 0.000(5) 0.000(6) 0.016(5) O8 0.023(5) 0.023(5) 0.037(7) -0.001(5) 0.007(4) -0.006(4) N8 0.012(5) 0.017(6) 0.031(8) -0.009(6) 0.001(5) -0.006(4) C11 0.022(7) 0.059(12) 0.022(8) 0.003(8) -0.003(6) 0.005(7) C12 0.047(9) 0.067(12) 0.025(8) 0.013(10) 0.000(7) 0.005(8) C13 0.061(14) 0.041(11) 0.047(13) -0.002(10) -0.021(11) 0.001(9) C14 0.054(12) 0.036(10) 0.025(10) -0.017(8) 0.005(8) 0.011(8) C15 0.049(12) 0.047(12) 0.063(14) -0.021(11) -0.011(10) -0.001(9) C16 0.096(16) 0.044(11) 0.051(13) -0.005(10) -0.017(12) 0.002(10) C21 0.060(10) 0.045(10) 0.029(8) -0.008(8) -0.031(9) 0.004(11) C22 0.049(11) 0.081(13) 0.035(10) -0.002(9) -0.007(11) -0.001(12) C23 0.079(13) 0.073(15) 0.031(10) 0.000(11) 0.018(9) 0.026(11) C25 0.060(13) 0.050(12) 0.080(17) 0.016(11) -0.019(12) -0.006(10) C26 0.043(12) 0.081(16) 0.063(15) 0.025(13) 0.006(10) -0.010(10) C31 0.030(9) 0.025(7) 0.038(9) 0.000(7) 0.002(9) -0.003(8) C32 0.029(9) 0.042(10) 0.053(12) 0.012(9) 0.003(8) -0.007(7) C33 0.055(13) 0.055(12) 0.056(14) -0.003(11) 0.011(10) 0.017(9) C34 0.035(11) 0.049(10) 0.035(11) 0.007(8) 0.014(7) -0.005(7) C24 0.043(11) 0.077(15) 0.043(12) 0.012(11) 0.003(9) -0.004(10) C35 0.054(12) 0.045(11) 0.057(14) -0.008(10) 0.021(10) 0.012(8) C36 0.069(16) 0.057(12) 0.057(14) -0.026(11) -0.017(10) 0.018(9) C41 0.033(10) 0.046(10) 0.026(9) -0.004(8) 0.000(6) -0.009(7) C42 0.061(13) 0.051(10) 0.044(11) 0.006(10) -0.004(9) -0.011(8) C43 0.058(12) 0.042(10) 0.055(13) -0.022(10) 0.006(11) -0.023(9) C61 0.020(8) 0.036(10) 0.041(11) -0.021(8) 0.022(7) 0.000(6) C44 0.055(12) 0.032(10) 0.024(10) -0.003(8) -0.015(8) -0.006(7) C45 0.045(13) 0.088(15) 0.048(13) 0.007(11) -0.005(9) 0.007(9) C62 0.046(12) 0.027(10) 0.081(17) -0.010(10) 0.010(11) 0.003(8) C63 0.063(13) 0.063(13) 0.069(15) -0.033(11) 0.027(12) -0.004(10) C46 0.035(11) 0.108(18) 0.063(15) 0.020(14) 0.002(10) 0.042(11) C51 0.033(8) 0.054(10) 0.029(7) 0.005(8) -0.010(7) 0.014(8) C52 0.034(10) 0.078(13) 0.037(9) 0.004(9) 0.013(9) -0.004(10) C53 0.057(11) 0.065(13) 0.042(11) -0.018(10) -0.013(9) -0.002(9) C54 0.030(9) 0.042(10) 0.043(11) 0.010(9) 0.005(8) 0.005(7) C55 0.039(10) 0.050(11) 0.039(11) -0.007(9) 0.000(8) -0.001(8) C56 0.064(13) 0.081(15) 0.023(10) 0.006(10) -0.020(9) 0.014(11) C64 0.027(8) 0.051(10) 0.025(8) 0.000(8) 0.016(7) 0.006(7) C65 0.050(12) 0.028(9) 0.050(13) -0.006(9) 0.003(10) 0.004(8) C66 0.053(11) 0.059(12) 0.044(11) 0.005(10) -0.002(8) 0.016(9) C71 0.036(11) 0.034(8) 0.029(9) -0.021(7) -0.005(7) 0.010(6) C72 0.040(9) 0.042(10) 0.060(13) 0.013(10) 0.009(8) 0.012(6) C73 0.038(10) 0.062(11) 0.036(11) 0.014(9) 0.010(8) -0.007(8) C74 0.047(11) 0.031(9) 0.040(12) -0.009(8) -0.008(8) 0.008(7) C75 0.070(18) 0.33(5) 0.041(15) -0.02(2) -0.006(13) -0.12(2) C76 0.074(19) 0.15(2) 0.016(10) 0.012(12) 0.001(10) -0.026(14) C81 0.035(8) 0.029(8) 0.034(9) 0.011(7) -0.013(10) -0.004(9) C82 0.054(11) 0.042(11) 0.042(12) -0.008(9) -0.006(9) 0.010(8) C83 0.046(11) 0.054(11) 0.031(11) -0.003(9) -0.002(8) 0.000(8) C84 0.029(10) 0.033(8) 0.058(12) 0.007(8) -0.021(10) -0.007(7) C85 0.043(13) 0.062(12) 0.059(13) -0.028(10) -0.003(10) -0.002(9) C86 0.041(10) 0.049(11) 0.090(19) 0.006(11) -0.010(11) -0.018(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 O1 2.206(9) . ? Sm1 O2 2.257(9) . ? Sm1 O3 2.278(9) . ? Sm1 O4 2.288(8) . ? Sm1 N2 2.512(14) . ? Sm1 N3 2.519(12) . ? Sm1 N4 2.589(11) . ? Sm1 K2 3.805(3) 1_455 ? Sm1 K1 3.942(3) . ? Sm2 O6 2.200(9) . ? Sm2 O8 2.286(10) . ? Sm2 O5 2.287(9) . ? Sm2 O7 2.290(10) . ? Sm2 N5 2.515(11) . ? Sm2 N8 2.558(11) . ? Sm2 N7 2.587(12) . ? Sm2 K1 3.813(3) . ? Sm2 K2 3.931(3) . ? K1 O4 2.547(9) . ? K1 O3 2.658(8) . ? K1 O5 2.716(9) . ? K1 O6 2.807(9) . ? K1 N6 2.806(12) . ? K2 O7 2.530(10) . ? K2 O8 2.664(9) . ? K2 O2 2.681(9) 1_655 ? K2 N1 2.786(12) 1_655 ? K2 O1 2.797(10) 1_655 ? K2 C15 3.45(2) 1_655 ? K2 Sm1 3.805(3) 1_655 ? O1 N1 1.419(14) . ? O1 K2 2.797(10) 1_455 ? N1 C11 1.48(2) . ? N1 C14 1.49(2) . ? N1 K2 2.786(12) 1_455 ? O2 N2 1.409(15) . ? O2 K2 2.681(9) 1_455 ? N2 C21 1.468(19) . ? N2 C24 1.48(2) . ? O3 N3 1.441(14) . ? N3 C31 1.45(2) . ? N3 C34 1.49(2) . ? O4 N4 1.408(14) . ? N4 C44 1.46(2) . ? N4 C41 1.48(2) . ? O5 N5 1.440(14) . ? N5 C51 1.472(18) . ? N5 C54 1.474(19) . ? O6 N6 1.445(13) . ? N6 C64 1.45(2) . ? N6 C61 1.466(18) . ? O7 N7 1.437(14) . ? N7 C71 1.484(19) . ? N7 C74 1.50(2) . ? O8 N8 1.434(13) . ? N8 C81 1.466(19) . ? N8 C84 1.488(19) . ? C11 C12 1.504(19) . ? C11 C13 1.51(2) . ? C11 H11A 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.48(3) . ? C14 C16 1.55(3) . ? C14 H14A 1.0000 . ? C15 K2 3.45(2) 1_455 ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C21 C23 1.50(2) . ? C21 C22 1.54(2) . ? C21 H21A 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C25 C24 1.54(3) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C24 1.53(3) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C31 C33 1.51(2) . ? C31 C32 1.51(2) . ? C31 H31A 1.0000 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.50(2) . ? C34 C36 1.50(2) . ? C34 H34A 1.0000 . ? C24 H24A 1.0000 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C41 C43 1.51(2) . ? C41 C42 1.51(2) . ? C41 H41A 1.0000 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C61 C63 1.52(2) . ? C61 C62 1.53(3) . ? C61 H61A 1.0000 . ? C44 C45 1.51(2) . ? C44 C46 1.52(2) . ? C44 H44A 1.0000 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C51 C52 1.51(2) . ? C51 C53 1.52(2) . ? C51 H51A 1.0000 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 C55 1.50(2) . ? C54 C56 1.55(2) . ? C54 H54A 1.0000 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C64 C65 1.52(2) . ? C64 C66 1.53(2) . ? C64 H64A 1.0000 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C71 C72 1.52(2) . ? C71 C73 1.52(2) . ? C71 H71A 1.0000 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C74 C76 1.48(3) . ? C74 C75 1.48(3) . ? C74 H74A 1.0000 . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C81 C82 1.50(2) . ? C81 C83 1.51(2) . ? C81 H81A 1.0000 . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? C83 H83A 0.9800 . ? C83 H83B 0.9800 . ? C83 H83C 0.9800 . ? C84 C85 1.49(2) . ? C84 C86 1.56(2) . ? C84 H84A 1.0000 . ? C85 H85A 0.9800 . ? C85 H85B 0.9800 . ? C85 H85C 0.9800 . ? C86 H86A 0.9800 . ? C86 H86B 0.9800 . ? C86 H86C 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 90.4(3) . . ? O1 Sm1 O3 130.8(4) . . ? O2 Sm1 O3 100.9(4) . . ? O1 Sm1 O4 128.1(4) . . ? O2 Sm1 O4 130.4(4) . . ? O3 Sm1 O4 78.0(3) . . ? O1 Sm1 N2 117.8(4) . . ? O2 Sm1 N2 33.8(4) . . ? O3 Sm1 N2 94.8(4) . . ? O4 Sm1 N2 96.6(4) . . ? O1 Sm1 N3 98.2(4) . . ? O2 Sm1 N3 91.9(4) . . ? O3 Sm1 N3 34.5(3) . . ? O4 Sm1 N3 108.9(3) . . ? N2 Sm1 N3 105.7(5) . . ? O1 Sm1 N4 101.5(4) . . ? O2 Sm1 N4 123.6(4) . . ? O3 Sm1 N4 110.7(3) . . ? O4 Sm1 N4 32.8(3) . . ? N2 Sm1 N4 96.6(4) . . ? N3 Sm1 N4 138.7(4) . . ? O1 Sm1 K2 46.7(2) . 1_455 ? O2 Sm1 K2 43.9(2) . 1_455 ? O3 Sm1 K2 123.8(2) . 1_455 ? O4 Sm1 K2 156.5(2) . 1_455 ? N2 Sm1 K2 74.6(3) . 1_455 ? N3 Sm1 K2 94.5(3) . 1_455 ? N4 Sm1 K2 125.2(2) . 1_455 ? O1 Sm1 K1 146.8(3) . . ? O2 Sm1 K1 121.3(3) . . ? O3 Sm1 K1 40.5(2) . . ? O4 Sm1 K1 37.6(2) . . ? N2 Sm1 K1 95.3(3) . . ? N3 Sm1 K1 73.2(3) . . ? N4 Sm1 K1 70.5(2) . . ? K2 Sm1 K1 161.59(8) 1_455 . ? O6 Sm2 O8 130.2(4) . . ? O6 Sm2 O5 91.5(3) . . ? O8 Sm2 O5 101.5(4) . . ? O6 Sm2 O7 127.9(4) . . ? O8 Sm2 O7 78.4(3) . . ? O5 Sm2 O7 129.0(4) . . ? O6 Sm2 N5 117.5(3) . . ? O8 Sm2 N5 97.9(4) . . ? O5 Sm2 N5 34.5(3) . . ? O7 Sm2 N5 94.5(4) . . ? O6 Sm2 N8 98.9(4) . . ? O8 Sm2 N8 33.9(3) . . ? O5 Sm2 N8 91.7(4) . . ? O7 Sm2 N8 109.4(3) . . ? N5 Sm2 N8 107.9(4) . . ? O6 Sm2 N7 100.6(4) . . ? O8 Sm2 N7 111.8(4) . . ? O5 Sm2 N7 121.9(4) . . ? O7 Sm2 N7 33.6(4) . . ? N5 Sm2 N7 93.2(4) . . ? N8 Sm2 N7 140.2(4) . . ? O6 Sm2 K1 46.7(2) . . ? O8 Sm2 K1 126.5(2) . . ? O5 Sm2 K1 44.7(2) . . ? O7 Sm2 K1 153.3(2) . . ? N5 Sm2 K1 74.2(2) . . ? N8 Sm2 K1 97.1(2) . . ? N7 Sm2 K1 121.4(3) . . ? O6 Sm2 K2 145.2(2) . . ? O8 Sm2 K2 40.9(2) . . ? O5 Sm2 K2 122.1(2) . . ? O7 Sm2 K2 37.5(2) . . ? N5 Sm2 K2 97.0(2) . . ? N8 Sm2 K2 73.2(2) . . ? N7 Sm2 K2 71.0(3) . . ? K1 Sm2 K2 164.51(8) . . ? O4 K1 O3 67.0(3) . . ? O4 K1 O5 112.5(3) . . ? O3 K1 O5 136.0(3) . . ? O4 K1 O6 144.3(3) . . ? O3 K1 O6 136.4(3) . . ? O5 K1 O6 71.1(3) . . ? O4 K1 N6 131.1(4) . . ? O3 K1 N6 111.1(3) . . ? O5 K1 N6 100.9(3) . . ? O6 K1 N6 29.8(3) . . ? O4 K1 Sm2 137.5(2) . . ? O3 K1 Sm2 152.8(2) . . ? O5 K1 Sm2 36.3(2) . . ? O6 K1 Sm2 34.81(18) . . ? N6 K1 Sm2 64.6(2) . . ? O4 K1 Sm1 33.27(19) . . ? O3 K1 Sm1 33.8(2) . . ? O5 K1 Sm1 132.8(2) . . ? O6 K1 Sm1 155.5(2) . . ? N6 K1 Sm1 126.1(2) . . ? Sm2 K1 Sm1 168.30(10) . . ? O7 K2 O8 67.6(3) . . ? O7 K2 O2 119.6(3) . 1_655 ? O8 K2 O2 133.4(3) . 1_655 ? O7 K2 N1 127.1(4) . 1_655 ? O8 K2 N1 110.1(3) . 1_655 ? O2 K2 N1 99.9(3) 1_655 1_655 ? O7 K2 O1 142.9(4) . 1_655 ? O8 K2 O1 134.2(3) . 1_655 ? O2 K2 O1 70.6(3) 1_655 1_655 ? N1 K2 O1 29.5(3) 1_655 1_655 ? O7 K2 C15 145.0(4) . 1_655 ? O8 K2 C15 84.0(4) . 1_655 ? O2 K2 C15 94.6(4) 1_655 1_655 ? N1 K2 C15 44.0(5) 1_655 1_655 ? O1 K2 C15 52.2(4) 1_655 1_655 ? O7 K2 Sm1 140.8(2) . 1_655 ? O8 K2 Sm1 149.9(2) . 1_655 ? O2 K2 Sm1 35.7(2) 1_655 1_655 ? N1 K2 Sm1 64.4(2) 1_655 1_655 ? O1 K2 Sm1 35.0(2) 1_655 1_655 ? C15 K2 Sm1 72.1(3) 1_655 1_655 ? O7 K2 Sm2 33.4(2) . . ? O8 K2 Sm2 34.2(2) . . ? O2 K2 Sm2 136.0(2) 1_655 . ? N1 K2 Sm2 124.1(2) 1_655 . ? O1 K2 Sm2 153.4(2) 1_655 . ? C15 K2 Sm2 115.5(3) 1_655 . ? Sm1 K2 Sm2 171.04(10) 1_655 . ? N1 O1 Sm1 172.6(8) . . ? N1 O1 K2 74.9(6) . 1_455 ? Sm1 O1 K2 98.3(4) . 1_455 ? O1 N1 C11 109.5(10) . . ? O1 N1 C14 107.6(12) . . ? C11 N1 C14 113.3(13) . . ? O1 N1 K2 75.7(6) . 1_455 ? C11 N1 K2 125.1(9) . 1_455 ? C14 N1 K2 116.6(10) . 1_455 ? N2 O2 Sm1 83.1(7) . . ? N2 O2 K2 149.7(8) . 1_455 ? Sm1 O2 K2 100.4(4) . 1_455 ? O2 N2 C21 110.3(12) . . ? O2 N2 C24 110.5(12) . . ? C21 N2 C24 114.6(14) . . ? O2 N2 Sm1 63.1(7) . . ? C21 N2 Sm1 111.0(10) . . ? C24 N2 Sm1 132.6(12) . . ? N3 O3 Sm1 82.0(6) . . ? N3 O3 K1 155.7(8) . . ? Sm1 O3 K1 105.7(3) . . ? O3 N3 C31 110.1(12) . . ? O3 N3 C34 110.1(12) . . ? C31 N3 C34 114.4(12) . . ? O3 N3 Sm1 63.5(5) . . ? C31 N3 Sm1 124.8(9) . . ? C34 N3 Sm1 119.0(10) . . ? N4 O4 Sm1 85.4(6) . . ? N4 O4 K1 165.4(7) . . ? Sm1 O4 K1 109.1(3) . . ? O4 N4 C44 110.4(11) . . ? O4 N4 C41 107.2(11) . . ? C44 N4 C41 114.7(12) . . ? O4 N4 Sm1 61.8(5) . . ? C44 N4 Sm1 125.1(9) . . ? C41 N4 Sm1 119.4(10) . . ? N5 O5 Sm2 81.5(6) . . ? N5 O5 K1 142.2(8) . . ? Sm2 O5 K1 98.9(4) . . ? O5 N5 C51 111.0(11) . . ? O5 N5 C54 110.1(10) . . ? C51 N5 C54 118.0(12) . . ? O5 N5 Sm2 64.0(6) . . ? C51 N5 Sm2 108.2(8) . . ? C54 N5 Sm2 131.1(10) . . ? N6 O6 Sm2 172.9(7) . . ? N6 O6 K1 75.1(5) . . ? Sm2 O6 K1 98.5(3) . . ? O6 N6 C64 109.0(9) . . ? O6 N6 C61 106.9(10) . . ? C64 N6 C61 114.1(12) . . ? O6 N6 K1 75.1(6) . . ? C64 N6 K1 122.0(9) . . ? C61 N6 K1 119.7(10) . . ? N7 O7 Sm2 84.6(7) . . ? N7 O7 K2 165.6(8) . . ? Sm2 O7 K2 109.2(4) . . ? O7 N7 C71 107.6(11) . . ? O7 N7 C74 107.6(11) . . ? C71 N7 C74 114.0(11) . . ? O7 N7 Sm2 61.8(6) . . ? C71 N7 Sm2 122.1(9) . . ? C74 N7 Sm2 123.6(9) . . ? N8 O8 Sm2 83.5(6) . . ? N8 O8 K2 156.8(8) . . ? Sm2 O8 K2 104.9(3) . . ? O8 N8 C81 108.2(12) . . ? O8 N8 C84 107.7(11) . . ? C81 N8 C84 118.3(11) . . ? O8 N8 Sm2 62.6(5) . . ? C81 N8 Sm2 124.5(9) . . ? C84 N8 Sm2 116.2(9) . . ? N1 C11 C12 116.7(12) . . ? N1 C11 C13 107.1(13) . . ? C12 C11 C13 111.8(15) . . ? N1 C11 H11A 106.9 . . ? C12 C11 H11A 106.9 . . ? C13 C11 H11A 106.9 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 N1 109.0(15) . . ? C15 C14 C16 108.2(16) . . ? N1 C14 C16 112.4(14) . . ? C15 C14 H14A 109.1 . . ? N1 C14 H14A 109.1 . . ? C16 C14 H14A 109.1 . . ? C14 C15 K2 87.8(11) . 1_455 ? C14 C15 H15A 109.5 . . ? K2 C15 H15A 73.2 1_455 . ? C14 C15 H15B 109.5 . . ? K2 C15 H15B 159.5 1_455 . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? K2 C15 H15C 52.5 1_455 . ? 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 . . ? N2 C21 C23 119.4(17) . . ? N2 C21 C22 109.1(13) . . ? C23 C21 C22 111.4(13) . . ? N2 C21 H21A 105.3 . . ? C23 C21 H21A 105.3 . . ? C22 C21 H21A 105.3 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N3 C31 C33 107.9(13) . . ? N3 C31 C32 118.4(14) . . ? C33 C31 C32 109.0(16) . . ? N3 C31 H31A 107.0 . . ? C33 C31 H31A 107.0 . . ? C32 C31 H31A 107.0 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N3 C34 C35 113.7(15) . . ? N3 C34 C36 117.4(14) . . ? C35 C34 C36 110.6(15) . . ? N3 C34 H34A 104.5 . . ? C35 C34 H34A 104.5 . . ? C36 C34 H34A 104.5 . . ? N2 C24 C26 114.2(17) . . ? N2 C24 C25 107.0(16) . . ? C26 C24 C25 108.9(17) . . ? N2 C24 H24A 108.8 . . ? C26 C24 H24A 108.8 . . ? C25 C24 H24A 108.8 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N4 C41 C43 117.1(12) . . ? N4 C41 C42 112.9(14) . . ? C43 C41 C42 109.6(14) . . ? N4 C41 H41A 105.4 . . ? C43 C41 H41A 105.4 . . ? C42 C41 H41A 105.4 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? N6 C61 C63 110.8(13) . . ? N6 C61 C62 109.9(15) . . ? C63 C61 C62 109.9(15) . . ? N6 C61 H61A 108.8 . . ? C63 C61 H61A 108.8 . . ? C62 C61 H61A 108.8 . . ? N4 C44 C45 111.0(14) . . ? N4 C44 C46 117.5(15) . . ? C45 C44 C46 110.1(16) . . ? N4 C44 H44A 105.8 . . ? C45 C44 H44A 105.8 . . ? C46 C44 H44A 105.8 . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C44 C46 H46A 109.5 . . ? C44 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C44 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? N5 C51 C52 110.1(13) . . ? N5 C51 C53 117.2(13) . . ? C52 C51 C53 111.9(14) . . ? N5 C51 H51A 105.6 . . ? C52 C51 H51A 105.5 . . ? C53 C51 H51A 105.5 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C51 C53 H53A 109.5 . . ? C51 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C51 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? N5 C54 C55 110.9(14) . . ? N5 C54 C56 113.3(15) . . ? C55 C54 C56 108.0(14) . . ? N5 C54 H54A 108.1 . . ? C55 C54 H54A 108.1 . . ? C56 C54 H54A 108.1 . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C54 C56 H56A 109.5 . . ? C54 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C54 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? N6 C64 C65 109.2(14) . . ? N6 C64 C66 115.7(14) . . ? C65 C64 C66 111.3(15) . . ? N6 C64 H64A 106.7 . . ? C65 C64 H64A 106.7 . . ? C66 C64 H64A 106.7 . . ? C64 C65 H65A 109.5 . . ? C64 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C64 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C64 C66 H66A 109.5 . . ? C64 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C64 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? N7 C71 C72 110.1(13) . . ? N7 C71 C73 118.4(13) . . ? C72 C71 C73 113.2(13) . . ? N7 C71 H71A 104.6 . . ? C72 C71 H71A 104.6 . . ? C73 C71 H71A 104.6 . . ? C71 C72 H72A 109.5 . . ? C71 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C71 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C71 C73 H73A 109.5 . . ? C71 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C71 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C76 C74 C75 108(2) . . ? C76 C74 N7 110.5(14) . . ? C75 C74 N7 117.5(17) . . ? C76 C74 H74A 106.7 . . ? C75 C74 H74A 106.7 . . ? N7 C74 H74A 106.7 . . ? C74 C75 H75A 109.5 . . ? C74 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C74 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? C74 C76 H76A 109.5 . . ? C74 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C74 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? N8 C81 C82 116.6(14) . . ? N8 C81 C83 108.8(12) . . ? C82 C81 C83 111.7(16) . . ? N8 C81 H81A 106.4 . . ? C82 C81 H81A 106.4 . . ? C83 C81 H81A 106.4 . . ? C81 C82 H82A 109.5 . . ? C81 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C81 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? C81 C83 H83A 109.5 . . ? C81 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C81 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? N8 C84 C85 117.9(14) . . ? N8 C84 C86 109.5(15) . . ? C85 C84 C86 109.9(15) . . ? N8 C84 H84A 106.3 . . ? C85 C84 H84A 106.3 . . ? C86 C84 H84A 106.3 . . ? C84 C85 H85A 109.5 . . ? C84 C85 H85B 109.5 . . ? H85A C85 H85B 109.5 . . ? C84 C85 H85C 109.5 . . ? H85A C85 H85C 109.5 . . ? H85B C85 H85C 109.5 . . ? C84 C86 H86A 109.5 . . ? C84 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? C84 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.844 _refine_diff_density_min -0.818 _refine_diff_density_rms 0.176 # Attachment 'YON_B705593E.cif' data_sad _database_code_depnum_ccdc_archive 'CCDC 643872' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Potassium-tetrakis(N,N-diisopropylaminoxy)yttrate ; _chemical_name_common Potassium-tetrakis(N,N-diisopropylaminoxy)yttrate _chemical_melting_point ? _chemical_formula_moiety '(C48 H112 N8 O8 K2 Y2)*(C4 H8 O)*0.5(C5 H12)' _chemical_formula_sum 'C54.5 H125 N8 O9 K2 Y2' _chemical_formula_weight 1292.63 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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 21.745(4) _cell_length_b 22.440(4) _cell_length_c 28.767(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 14036(5) _cell_formula_units_Z 16 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 900 _cell_measurement_theta_min 1 _cell_measurement_theta_max 22.5 _exptl_crystal_description colourless _exptl_crystal_colour block _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.223 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5568 _exptl_absorpt_coefficient_mu 1.816 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; Corrections were done with the SADABS program, utilizing the none merged raw data obtained from the integration process. Integration and final cell refinement were done with SAINT. SADABS reports ratio of Tmin/Tmax = 0.178777 ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Omega and Phi scans' _diffrn_detector_area_resol_mean 80 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 138878 _diffrn_reflns_av_R_equivalents 0.2811 _diffrn_reflns_av_sigmaI/netI 0.1808 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 28.15 _reflns_number_total 17149 _reflns_number_gt 7598 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT (Bruker AXS, 2000)' _computing_data_reduction 'SAINT,SADABS (Bruker AXS, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0798P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ride _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17149 _refine_ls_number_parameters 643 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1954 _refine_ls_R_factor_gt 0.0727 _refine_ls_wR_factor_ref 0.1899 _refine_ls_wR_factor_gt 0.1473 _refine_ls_goodness_of_fit_ref 0.960 _refine_ls_restrained_S_all 0.960 _refine_ls_shift/su_max 0.007 _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 Y1 Y 0.75407(2) 0.32812(2) -0.233037(17) 0.02575(14) Uani 1 1 d . . . K1 K 0.80228(6) 0.33860(5) -0.10394(4) 0.0307(3) Uani 1 1 d . . . Y2 Y 0.80107(3) 0.27149(2) 0.019551(17) 0.02695(14) Uani 1 1 d . . . K2 K 0.79108(6) 0.19396(6) 0.13819(4) 0.0332(3) Uani 1 1 d . . . O1 O 0.72854(17) 0.38393(16) -0.17762(12) 0.0316(9) Uani 1 1 d . . . N1 N 0.7135(2) 0.4158(2) -0.13591(14) 0.0299(11) Uani 1 1 d . . . C11 C 0.7244(3) 0.4793(3) -0.1448(2) 0.0374(16) Uani 1 1 d . . . H11A H 0.7138 0.5010 -0.1155 0.045 Uiso 1 1 calc R . . C12 C 0.6853(3) 0.5065(3) -0.1834(2) 0.0500(18) Uani 1 1 d . . . H12A H 0.6417 0.4997 -0.1766 0.075 Uiso 1 1 calc R . . H12B H 0.6959 0.4878 -0.2131 0.075 Uiso 1 1 calc R . . H12C H 0.6933 0.5494 -0.1852 0.075 Uiso 1 1 calc R . . C13 C 0.7921(3) 0.4893(3) -0.1533(2) 0.0470(18) Uani 1 1 d . . . H13A H 0.8159 0.4719 -0.1278 0.071 Uiso 1 1 calc R . . H13B H 0.8003 0.5322 -0.1550 0.071 Uiso 1 1 calc R . . H13C H 0.8040 0.4704 -0.1827 0.071 Uiso 1 1 calc R . . C14 C 0.6503(3) 0.4010(3) -0.1240(2) 0.0361(15) Uani 1 1 d . . . H14A H 0.6239 0.4061 -0.1521 0.043 Uiso 1 1 calc R . . C15 C 0.6475(3) 0.3370(3) -0.1084(2) 0.0513(19) Uani 1 1 d . . . H15A H 0.6621 0.3111 -0.1335 0.077 Uiso 1 1 calc R . . H15B H 0.6049 0.3266 -0.1006 0.077 Uiso 1 1 calc R . . H15C H 0.6736 0.3316 -0.0809 0.077 Uiso 1 1 calc R . . C16 C 0.6262(3) 0.4416(3) -0.0851(2) 0.054(2) Uani 1 1 d . . . H16A H 0.6272 0.4832 -0.0955 0.082 Uiso 1 1 calc R . . H16B H 0.6522 0.4371 -0.0574 0.082 Uiso 1 1 calc R . . H16C H 0.5838 0.4304 -0.0774 0.082 Uiso 1 1 calc R . . O2 O 0.81969(16) 0.28428(16) -0.18679(12) 0.0295(9) Uani 1 1 d . . . N2 N 0.8561(2) 0.2807(2) -0.22842(15) 0.0314(11) Uani 1 1 d . . . C21 C 0.8631(3) 0.2168(3) -0.24163(19) 0.0363(15) Uani 1 1 d . . . H21A H 0.8223 0.2046 -0.2546 0.044 Uiso 1 1 calc R . . C22 C 0.9084(3) 0.2078(3) -0.2805(2) 0.0419(16) Uani 1 1 d . . . H22A H 0.8992 0.2356 -0.3058 0.063 Uiso 1 1 calc R . . H22B H 0.9055 0.1668 -0.2920 0.063 Uiso 1 1 calc R . . H22C H 0.9502 0.2152 -0.2690 0.063 Uiso 1 1 calc R . . C23 C 0.8761(3) 0.1735(3) -0.2025(2) 0.0497(18) Uani 1 1 d . . . H23A H 0.8459 0.1792 -0.1776 0.075 Uiso 1 1 calc R . . H23B H 0.9175 0.1807 -0.1903 0.075 Uiso 1 1 calc R . . H23C H 0.8734 0.1326 -0.2143 0.075 Uiso 1 1 calc R . . C24 C 0.9135(3) 0.3144(3) -0.2220(2) 0.0424(17) Uani 1 1 d . . . H24A H 0.9387 0.3088 -0.2507 0.051 Uiso 1 1 calc R . . C25 C 0.9525(3) 0.2940(3) -0.1809(2) 0.055(2) Uani 1 1 d . . . H25A H 0.9618 0.2515 -0.1842 0.082 Uiso 1 1 calc R . . H25B H 0.9297 0.3005 -0.1519 0.082 Uiso 1 1 calc R . . H25C H 0.9909 0.3168 -0.1801 0.082 Uiso 1 1 calc R . . C26 C 0.8987(3) 0.3799(3) -0.2183(2) 0.0523(19) Uani 1 1 d . . . H26A H 0.8746 0.3922 -0.2455 0.078 Uiso 1 1 calc R . . H26B H 0.9370 0.4029 -0.2172 0.078 Uiso 1 1 calc R . . H26C H 0.8749 0.3872 -0.1900 0.078 Uiso 1 1 calc R . . O3 O 0.70132(17) 0.26393(16) -0.27557(11) 0.0286(9) Uani 1 1 d . . . N3 N 0.6621(2) 0.2632(2) -0.23524(15) 0.0303(11) Uani 1 1 d . . . C31 C 0.6534(3) 0.2004(3) -0.2205(2) 0.0387(16) Uani 1 1 d . . . H31A H 0.6280 0.2008 -0.1916 0.046 Uiso 1 1 calc R . . C32 C 0.6190(3) 0.1638(3) -0.2565(2) 0.0501(18) Uani 1 1 d . . . H32A H 0.5797 0.1830 -0.2636 0.075 Uiso 1 1 calc R . . H32B H 0.6114 0.1237 -0.2442 0.075 Uiso 1 1 calc R . . H32C H 0.6438 0.1609 -0.2849 0.075 Uiso 1 1 calc R . . C33 C 0.7135(3) 0.1719(3) -0.2088(2) 0.0431(16) Uani 1 1 d . . . H33A H 0.7347 0.1958 -0.1852 0.065 Uiso 1 1 calc R . . H33B H 0.7391 0.1696 -0.2368 0.065 Uiso 1 1 calc R . . H33C H 0.7063 0.1317 -0.1967 0.065 Uiso 1 1 calc R . . C34 C 0.6037(3) 0.2920(3) -0.2480(2) 0.0371(15) Uani 1 1 d . . . H34A H 0.5863 0.2708 -0.2756 0.044 Uiso 1 1 calc R . . C35 C 0.6134(3) 0.3561(3) -0.2607(2) 0.0412(16) Uani 1 1 d . . . H35A H 0.6429 0.3587 -0.2863 0.062 Uiso 1 1 calc R . . H35B H 0.6293 0.3778 -0.2337 0.062 Uiso 1 1 calc R . . H35C H 0.5741 0.3736 -0.2704 0.062 Uiso 1 1 calc R . . C36 C 0.5571(3) 0.2883(3) -0.2082(2) 0.0488(18) Uani 1 1 d . . . H36A H 0.5504 0.2464 -0.1999 0.073 Uiso 1 1 calc R . . H36B H 0.5181 0.3061 -0.2181 0.073 Uiso 1 1 calc R . . H36C H 0.5730 0.3099 -0.1811 0.073 Uiso 1 1 calc R . . O4 O 0.73120(17) 0.11818(17) 0.20810(12) 0.0324(10) Uani 1 1 d . . . N4 N 0.7235(2) 0.0878(2) 0.16478(15) 0.0348(12) Uani 1 1 d . . . C41 C 0.7431(3) 0.0255(3) 0.1717(2) 0.0401(16) Uani 1 1 d . . . H41A H 0.7367 0.0043 0.1415 0.048 Uiso 1 1 calc R . . C42 C 0.7058(3) -0.0080(3) 0.2085(2) 0.0536(19) Uani 1 1 d . . . H42A H 0.6620 -0.0060 0.2007 0.080 Uiso 1 1 calc R . . H42B H 0.7127 0.0103 0.2390 0.080 Uiso 1 1 calc R . . H42C H 0.7189 -0.0498 0.2094 0.080 Uiso 1 1 calc R . . C43 C 0.8112(3) 0.0227(3) 0.1825(2) 0.0506(19) Uani 1 1 d . . . H43A H 0.8341 0.0444 0.1585 0.076 Uiso 1 1 calc R . . H43B H 0.8246 -0.0190 0.1830 0.076 Uiso 1 1 calc R . . H43C H 0.8189 0.0409 0.2129 0.076 Uiso 1 1 calc R . . C44 C 0.6588(3) 0.0936(3) 0.1511(2) 0.0409(16) Uani 1 1 d . . . H44A H 0.6323 0.0762 0.1761 0.049 Uiso 1 1 calc R . . C45 C 0.6424(3) 0.1583(3) 0.1449(2) 0.0486(18) Uani 1 1 d . . . H45A H 0.6490 0.1796 0.1742 0.073 Uiso 1 1 calc R . . H45B H 0.5991 0.1617 0.1358 0.073 Uiso 1 1 calc R . . H45C H 0.6685 0.1758 0.1207 0.073 Uiso 1 1 calc R . . C46 C 0.6482(3) 0.0588(3) 0.1058(2) 0.056(2) Uani 1 1 d . . . H46A H 0.6590 0.0168 0.1105 0.084 Uiso 1 1 calc R . . H46B H 0.6740 0.0756 0.0811 0.084 Uiso 1 1 calc R . . H46C H 0.6048 0.0618 0.0968 0.084 Uiso 1 1 calc R . . O5 O 0.85895(17) 0.21292(16) 0.05592(12) 0.0330(9) Uani 1 1 d . . . N5 N 0.8936(2) 0.1685(2) 0.08003(16) 0.0377(13) Uani 1 1 d . . . C51 C 0.9565(3) 0.1918(3) 0.0848(2) 0.0422(17) Uani 1 1 d . . . H51A H 0.9807 0.1614 0.1024 0.051 Uiso 1 1 calc R . . C52 C 0.9900(3) 0.2029(3) 0.0397(2) 0.056(2) Uani 1 1 d . . . H52A H 1.0311 0.2187 0.0463 0.084 Uiso 1 1 calc R . . H52B H 0.9670 0.2317 0.0210 0.084 Uiso 1 1 calc R . . H52C H 0.9938 0.1653 0.0225 0.084 Uiso 1 1 calc R . . C53 C 0.9556(3) 0.2473(3) 0.1137(2) 0.057(2) Uani 1 1 d . . . H53A H 0.9340 0.2394 0.1430 0.086 Uiso 1 1 calc R . . H53B H 0.9343 0.2790 0.0967 0.086 Uiso 1 1 calc R . . H53C H 0.9979 0.2598 0.1203 0.086 Uiso 1 1 calc R . . C54 C 0.8886(3) 0.1131(3) 0.0531(2) 0.0458(17) Uani 1 1 d . . . H54A H 0.9022 0.1214 0.0205 0.055 Uiso 1 1 calc R . . C55 C 0.8237(3) 0.0921(3) 0.0516(2) 0.0520(19) Uani 1 1 d . . . H55A H 0.7978 0.1227 0.0373 0.078 Uiso 1 1 calc R . . H55B H 0.8094 0.0842 0.0833 0.078 Uiso 1 1 calc R . . H55C H 0.8213 0.0553 0.0333 0.078 Uiso 1 1 calc R . . C56 C 0.9314(3) 0.0656(3) 0.0740(3) 0.074(3) Uani 1 1 d . . . H56A H 0.9739 0.0803 0.0735 0.110 Uiso 1 1 calc R . . H56B H 0.9286 0.0290 0.0556 0.110 Uiso 1 1 calc R . . H56C H 0.9191 0.0574 0.1061 0.110 Uiso 1 1 calc R . . O6 O 0.85412(17) 0.34118(16) -0.00938(12) 0.0325(9) Uani 1 1 d . . . N6 N 0.8799(2) 0.3941(2) -0.03048(15) 0.0327(12) Uani 1 1 d . . . C61 C 0.8538(3) 0.4450(3) -0.0055(2) 0.0394(16) Uani 1 1 d . . . H61A H 0.8601 0.4392 0.0286 0.047 Uiso 1 1 calc R . . C62 C 0.7862(3) 0.4477(3) -0.0155(2) 0.0499(18) Uani 1 1 d . . . H62A H 0.7667 0.4104 -0.0056 0.075 Uiso 1 1 calc R . . H62B H 0.7798 0.4533 -0.0490 0.075 Uiso 1 1 calc R . . H62C H 0.7679 0.4811 0.0015 0.075 Uiso 1 1 calc R . . C63 C 0.8837(3) 0.5032(3) -0.0203(2) 0.060(2) Uani 1 1 d . . . H63A H 0.9278 0.5019 -0.0130 0.090 Uiso 1 1 calc R . . H63B H 0.8645 0.5364 -0.0036 0.090 Uiso 1 1 calc R . . H63C H 0.8782 0.5088 -0.0538 0.090 Uiso 1 1 calc R . . C64 C 0.9477(3) 0.3904(3) -0.0257(2) 0.0441(17) Uani 1 1 d . . . H64A H 0.9649 0.4283 -0.0385 0.053 Uiso 1 1 calc R . . C65 C 0.9707(3) 0.3850(3) 0.0242(2) 0.0528(19) Uani 1 1 d . . . H65A H 0.9544 0.4180 0.0428 0.079 Uiso 1 1 calc R . . H65B H 1.0158 0.3864 0.0245 0.079 Uiso 1 1 calc R . . H65C H 0.9568 0.3470 0.0374 0.079 Uiso 1 1 calc R . . C66 C 0.9722(3) 0.3409(3) -0.0549(2) 0.055(2) Uani 1 1 d . . . H66A H 0.9578 0.3458 -0.0870 0.083 Uiso 1 1 calc R . . H66B H 0.9577 0.3027 -0.0426 0.083 Uiso 1 1 calc R . . H66C H 1.0173 0.3418 -0.0543 0.083 Uiso 1 1 calc R . . O7 O 0.74932(17) 0.26025(16) -0.04493(12) 0.0318(9) Uani 1 1 d . . . N7 N 0.7636(2) 0.1978(2) -0.03800(15) 0.0317(12) Uani 1 1 d . . . C71 C 0.7051(3) 0.1642(3) -0.03818(18) 0.0359(15) Uani 1 1 d . . . H71A H 0.7158 0.1212 -0.0337 0.043 Uiso 1 1 calc R . . C72 C 0.6656(3) 0.1819(3) 0.0021(2) 0.0490(18) Uani 1 1 d . . . H72A H 0.6893 0.1783 0.0309 0.073 Uiso 1 1 calc R . . H72B H 0.6296 0.1557 0.0035 0.073 Uiso 1 1 calc R . . H72C H 0.6521 0.2232 -0.0019 0.073 Uiso 1 1 calc R . . C73 C 0.6687(3) 0.1684(3) -0.0833(2) 0.054(2) Uani 1 1 d . . . H73A H 0.6949 0.1562 -0.1094 0.082 Uiso 1 1 calc R . . H73B H 0.6551 0.2096 -0.0880 0.082 Uiso 1 1 calc R . . H73C H 0.6328 0.1421 -0.0816 0.082 Uiso 1 1 calc R . . C74 C 0.8055(3) 0.1802(3) -0.0759(2) 0.0385(15) Uani 1 1 d . . . H74A H 0.7885 0.1959 -0.1057 0.046 Uiso 1 1 calc R . . C75 C 0.8683(3) 0.2083(3) -0.0682(2) 0.0395(16) Uani 1 1 d . . . H75A H 0.9009 0.1932 -0.0891 0.047 Uiso 1 1 calc R . . H75B H 0.8820 0.2085 -0.0353 0.047 Uiso 1 1 calc R . . C76 C 0.8125(3) 0.1137(3) -0.0806(2) 0.058(2) Uani 1 1 d . . . H76A H 0.7720 0.0957 -0.0862 0.087 Uiso 1 1 calc R . . H76B H 0.8300 0.0973 -0.0520 0.087 Uiso 1 1 calc R . . H76C H 0.8398 0.1047 -0.1068 0.087 Uiso 1 1 calc R . . O8 O 0.73695(17) 0.26782(16) 0.07767(12) 0.0300(9) Uani 1 1 d . . . N8 N 0.7262(2) 0.3289(2) 0.06588(15) 0.0336(12) Uani 1 1 d . . . C81 C 0.7449(3) 0.3664(3) 0.10577(19) 0.0352(14) Uani 1 1 d . . . H81A H 0.7363 0.4088 0.0972 0.042 Uiso 1 1 calc R . . C82 C 0.7118(3) 0.3541(3) 0.1510(2) 0.0486(18) Uani 1 1 d . . . H82A H 0.6674 0.3585 0.1463 0.073 Uiso 1 1 calc R . . H82B H 0.7257 0.3824 0.1747 0.073 Uiso 1 1 calc R . . H82C H 0.7209 0.3134 0.1612 0.073 Uiso 1 1 calc R . . C83 C 0.8138(3) 0.3606(3) 0.1124(2) 0.0452(18) Uani 1 1 d . . . H83A H 0.8346 0.3687 0.0828 0.068 Uiso 1 1 calc R . . H83B H 0.8236 0.3200 0.1226 0.068 Uiso 1 1 calc R . . H83C H 0.8276 0.3892 0.1358 0.068 Uiso 1 1 calc R . . C84 C 0.6609(3) 0.3354(3) 0.0499(2) 0.0405(16) Uani 1 1 d . . . H84A H 0.6596 0.3188 0.0177 0.049 Uiso 1 1 calc R . . C85 C 0.6123(3) 0.3021(3) 0.0772(2) 0.0478(18) Uani 1 1 d . . . H85A H 0.6240 0.2600 0.0797 0.072 Uiso 1 1 calc R . . H85B H 0.5727 0.3052 0.0610 0.072 Uiso 1 1 calc R . . H85C H 0.6086 0.3194 0.1083 0.072 Uiso 1 1 calc R . . C86 C 0.6424(3) 0.4009(3) 0.0455(2) 0.0515(19) Uani 1 1 d . . . H86A H 0.6738 0.4224 0.0276 0.077 Uiso 1 1 calc R . . H86B H 0.6388 0.4186 0.0765 0.077 Uiso 1 1 calc R . . H86C H 0.6028 0.4038 0.0294 0.077 Uiso 1 1 calc R . . O100 O 0.9951(9) 0.5957(8) -0.1615(6) 0.330(9) Uiso 1 1 d . . . C101 C 1.0093(7) 0.4964(7) -0.1795(5) 0.193(7) Uiso 1 1 d . . . H10A H 0.9820 0.4951 -0.2071 0.232 Uiso 1 1 calc R . . H10B H 1.0385 0.4625 -0.1802 0.232 Uiso 1 1 calc R . . C102 C 0.9452(8) 0.5604(9) -0.1504(6) 0.218(8) Uiso 1 1 d . . . H10C H 0.9167 0.5562 -0.1771 0.262 Uiso 1 1 calc R . . H10D H 0.9225 0.5764 -0.1233 0.262 Uiso 1 1 calc R . . C103 C 0.9774(8) 0.5000(8) -0.1386(6) 0.236(8) Uiso 1 1 d . . . H10E H 1.0048 0.5029 -0.1111 0.283 Uiso 1 1 calc R . . H10F H 0.9479 0.4668 -0.1345 0.283 Uiso 1 1 calc R . . C104 C 1.0394(9) 0.5529(10) -0.1740(7) 0.270(10) Uiso 1 1 d . . . H10G H 1.0713 0.5500 -0.1495 0.324 Uiso 1 1 calc R . . H10H H 1.0597 0.5646 -0.2034 0.324 Uiso 1 1 calc R . . C201 C 0.9944(6) -0.0472(6) 0.1638(5) 0.183(6) Uiso 1 1 d . . . H20A H 0.9918 -0.0227 0.1356 0.274 Uiso 1 1 calc R . . H20B H 0.9580 -0.0727 0.1659 0.274 Uiso 1 1 calc R . . H20C H 1.0314 -0.0720 0.1624 0.274 Uiso 1 1 calc R . . C202 C 0.9973(8) -0.0093(8) 0.2037(6) 0.230(8) Uiso 1 1 d . . . H20D H 1.0337 0.0164 0.1992 0.276 Uiso 1 1 calc R . . H20E H 0.9609 0.0171 0.2018 0.276 Uiso 1 1 calc R . . C203 C 1.0000 -0.0297(12) 0.2500 0.231(12) Uiso 1 2 d S . . H20F H 0.9640 -0.0566 0.2512 0.347 Uiso 0.50 1 calc PR . . H20G H 1.0360 -0.0566 0.2488 0.347 Uiso 0.50 1 calc PR . . 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 Y1 0.0288(3) 0.0263(3) 0.0221(3) 0.0006(2) 0.0003(2) -0.0010(3) K1 0.0359(7) 0.0318(7) 0.0243(6) 0.0013(5) -0.0007(6) 0.0008(6) Y2 0.0340(3) 0.0261(3) 0.0207(3) -0.0003(2) -0.0009(3) -0.0012(3) K2 0.0421(8) 0.0338(8) 0.0236(6) 0.0020(5) 0.0019(6) -0.0018(6) O1 0.036(2) 0.030(2) 0.028(2) -0.0071(17) 0.0001(18) 0.0015(18) N1 0.035(3) 0.033(3) 0.022(2) -0.006(2) -0.001(2) 0.003(2) C11 0.055(4) 0.031(4) 0.026(3) -0.006(3) -0.001(3) 0.001(3) C12 0.066(5) 0.033(4) 0.051(4) 0.008(3) -0.009(4) 0.011(3) C13 0.058(5) 0.034(4) 0.050(4) 0.000(3) 0.001(4) -0.010(3) C14 0.037(4) 0.044(4) 0.027(3) -0.003(3) -0.003(3) 0.002(3) C15 0.042(4) 0.069(5) 0.043(4) 0.013(4) 0.002(3) -0.014(4) C16 0.036(4) 0.081(6) 0.046(4) -0.012(4) 0.011(3) 0.008(4) O2 0.030(2) 0.037(2) 0.0215(19) -0.0010(17) 0.0066(17) 0.0026(18) N2 0.032(3) 0.037(3) 0.025(3) 0.000(2) 0.002(2) 0.001(2) C21 0.041(4) 0.041(4) 0.028(3) -0.002(3) 0.000(3) 0.011(3) C22 0.034(4) 0.057(5) 0.034(3) -0.008(3) 0.000(3) 0.006(3) C23 0.061(5) 0.046(4) 0.042(4) 0.002(3) 0.009(3) 0.023(4) C24 0.033(4) 0.065(5) 0.030(3) -0.010(3) 0.005(3) -0.009(3) C25 0.043(4) 0.079(6) 0.042(4) -0.014(4) -0.015(3) 0.002(4) C26 0.051(5) 0.051(5) 0.055(4) -0.005(4) 0.001(4) -0.012(4) O3 0.030(2) 0.037(2) 0.0194(18) -0.0017(16) 0.0037(17) -0.0051(19) N3 0.030(3) 0.035(3) 0.026(3) 0.000(2) 0.003(2) -0.003(2) C31 0.054(4) 0.036(4) 0.026(3) -0.003(3) 0.006(3) -0.014(3) C32 0.063(5) 0.040(4) 0.048(4) -0.006(3) 0.005(4) -0.019(4) C33 0.055(4) 0.034(4) 0.040(4) 0.008(3) 0.000(3) -0.007(3) C34 0.035(4) 0.051(4) 0.026(3) -0.001(3) -0.005(3) -0.009(3) C35 0.031(4) 0.048(4) 0.044(4) -0.005(3) -0.001(3) 0.003(3) C36 0.032(4) 0.076(5) 0.039(4) -0.004(4) -0.002(3) -0.003(4) O4 0.039(2) 0.032(2) 0.026(2) -0.0085(18) -0.0031(18) -0.0028(18) N4 0.052(3) 0.031(3) 0.022(2) -0.006(2) 0.000(2) 0.000(2) C41 0.053(5) 0.033(4) 0.034(3) -0.009(3) 0.000(3) -0.004(3) C42 0.077(5) 0.033(4) 0.051(4) -0.001(3) 0.007(4) -0.010(4) C43 0.070(6) 0.038(4) 0.043(4) 0.003(3) -0.001(4) 0.008(4) C44 0.040(4) 0.051(5) 0.032(4) 0.002(3) -0.003(3) -0.012(3) C45 0.045(4) 0.060(5) 0.041(4) 0.000(3) -0.002(3) 0.005(4) C46 0.070(5) 0.063(5) 0.034(4) -0.010(3) -0.014(4) -0.009(4) O5 0.037(2) 0.033(2) 0.029(2) 0.0040(18) -0.0021(19) 0.0049(19) N5 0.035(3) 0.042(3) 0.036(3) 0.012(3) 0.004(2) 0.008(3) C51 0.036(4) 0.052(5) 0.039(4) 0.012(3) -0.009(3) 0.010(3) C52 0.036(4) 0.080(6) 0.052(4) 0.016(4) 0.001(3) 0.003(4) C53 0.044(4) 0.088(6) 0.039(4) 0.012(4) -0.011(3) -0.016(4) C54 0.053(5) 0.043(4) 0.041(4) 0.010(3) 0.011(3) 0.013(4) C55 0.059(5) 0.049(5) 0.048(4) 0.005(3) 0.002(4) -0.007(4) C56 0.052(5) 0.054(5) 0.115(7) 0.030(5) 0.018(5) 0.011(4) O6 0.037(2) 0.027(2) 0.033(2) -0.0022(17) 0.0022(19) -0.0096(18) N6 0.038(3) 0.029(3) 0.032(3) 0.000(2) 0.002(2) -0.008(2) C61 0.057(5) 0.034(4) 0.027(3) -0.003(3) -0.002(3) -0.010(3) C62 0.059(5) 0.042(4) 0.049(4) -0.001(3) 0.007(4) 0.003(3) C63 0.078(6) 0.038(4) 0.063(5) -0.009(4) 0.001(4) -0.009(4) C64 0.046(4) 0.045(4) 0.041(4) 0.004(3) 0.001(3) -0.010(3) C65 0.049(4) 0.059(5) 0.050(4) -0.003(4) -0.014(3) -0.002(4) C66 0.050(5) 0.065(5) 0.051(4) -0.002(4) 0.011(4) -0.006(4) O7 0.045(3) 0.024(2) 0.027(2) 0.0047(16) -0.0077(19) -0.0046(19) N7 0.042(3) 0.027(3) 0.026(3) -0.003(2) 0.008(2) -0.005(2) C71 0.048(4) 0.031(4) 0.029(3) -0.001(3) -0.009(3) -0.014(3) C72 0.056(5) 0.038(4) 0.053(4) -0.004(3) 0.000(4) -0.012(3) C73 0.066(5) 0.058(5) 0.039(4) -0.003(3) -0.011(4) -0.027(4) C74 0.055(4) 0.032(4) 0.029(3) -0.004(3) 0.002(3) 0.001(3) C75 0.043(4) 0.051(4) 0.025(3) -0.006(3) 0.008(3) 0.009(3) C76 0.086(6) 0.038(4) 0.050(4) -0.020(3) 0.016(4) -0.002(4) O8 0.038(2) 0.024(2) 0.028(2) 0.0010(17) 0.0017(17) 0.0050(18) N8 0.044(3) 0.028(3) 0.030(3) 0.001(2) 0.003(2) 0.003(2) C81 0.043(4) 0.032(3) 0.031(3) -0.004(3) 0.003(3) -0.005(3) C82 0.065(5) 0.050(4) 0.031(3) -0.009(3) 0.009(3) -0.006(4) C83 0.068(5) 0.036(4) 0.032(3) 0.002(3) -0.003(3) -0.012(3) C84 0.043(4) 0.035(4) 0.043(4) 0.004(3) 0.001(3) 0.008(3) C85 0.041(4) 0.049(4) 0.054(4) 0.001(3) 0.003(3) 0.008(3) C86 0.056(5) 0.046(4) 0.053(4) 0.008(3) 0.006(4) 0.015(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y1 O1 2.102(4) . ? Y1 O4 2.103(4) 2_654 ? Y1 O2 2.185(4) . ? Y1 O3 2.211(4) . ? Y1 N2 2.463(5) . ? Y1 N3 2.474(5) . ? Y1 K2 3.8643(14) 2_654 ? Y1 K1 3.8658(14) . ? K1 O7 2.702(4) . ? K1 O2 2.703(4) . ? K1 N1 2.752(5) . ? K1 O1 2.846(4) . ? K1 O6 2.945(4) . ? K1 N6 2.977(5) . ? K1 C15 3.369(7) . ? K1 C75 3.415(6) . ? K1 Y2 3.8586(14) . ? Y2 O5 2.099(4) . ? Y2 O6 2.114(4) . ? Y2 O8 2.179(4) . ? Y2 O7 2.184(4) . ? Y2 N8 2.468(5) . ? Y2 N7 2.478(5) . ? Y2 K2 3.8367(14) . ? K2 O3 2.660(4) 2_655 ? K2 O8 2.677(4) . ? K2 O5 2.821(4) . ? K2 N5 2.846(5) . ? K2 N4 2.903(5) . ? K2 O4 2.938(4) . ? K2 Y1 3.8643(14) 2_655 ? O1 N1 1.435(5) . ? N1 C14 1.454(7) . ? N1 C11 1.467(7) . ? C11 C13 1.508(8) . ? C11 C12 1.526(8) . ? C11 H11A 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.507(8) . ? C14 C16 1.535(8) . ? C14 H14A 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? O2 N2 1.438(5) . ? N2 C24 1.471(7) . ? N2 C21 1.493(7) . ? C21 C22 1.505(7) . ? C21 C23 1.513(8) . ? C21 H21A 1.0000 . ? 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 C26 1.508(9) . ? C24 C25 1.526(8) . ? C24 H24A 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? O3 N3 1.440(5) . ? O3 K2 2.660(4) 2_654 ? N3 C34 1.471(7) . ? N3 C31 1.484(7) . ? C31 C33 1.494(8) . ? C31 C32 1.518(8) . ? C31 H31A 1.0000 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.498(8) . ? C34 C36 1.532(8) . ? C34 H34A 1.0000 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? O4 N4 1.431(5) . ? O4 Y1 2.103(4) 2_655 ? N4 C44 1.466(8) . ? N4 C41 1.475(7) . ? C41 C43 1.515(8) . ? C41 C42 1.531(8) . ? C41 H41A 1.0000 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 C45 1.507(8) . ? C44 C46 1.537(8) . ? C44 H44A 1.0000 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? O5 N5 1.429(6) . ? N5 C54 1.469(8) . ? N5 C51 1.470(8) . ? C51 C53 1.497(9) . ? C51 C52 1.508(8) . ? C51 H51A 1.0000 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 C55 1.487(8) . ? C54 C56 1.538(9) . ? C54 H54A 1.0000 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? O6 N6 1.446(6) . ? N6 C61 1.464(7) . ? N6 C64 1.483(8) . ? C61 C62 1.500(9) . ? C61 C63 1.519(8) . ? C61 H61A 1.0000 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 C66 1.490(8) . ? C64 C65 1.526(8) . ? C64 H64A 1.0000 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? O7 N7 1.450(6) . ? N7 C74 1.476(7) . ? N7 C71 1.479(7) . ? C71 C72 1.494(8) . ? C71 C73 1.523(8) . ? C71 H71A 1.0000 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C74 C76 1.505(8) . ? C74 C75 1.519(8) . ? C74 H74A 1.0000 . ? C75 H75A 0.9900 . ? C75 H75B 0.9900 . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? O8 N8 1.432(5) . ? N8 C81 1.480(7) . ? N8 C84 1.498(7) . ? C81 C82 1.512(8) . ? C81 C83 1.514(8) . ? C81 H81A 1.0000 . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? C83 H83A 0.9800 . ? C83 H83B 0.9800 . ? C83 H83C 0.9800 . ? C84 C85 1.514(8) . ? C84 C86 1.529(8) . ? C84 H84A 1.0000 . ? C85 H85A 0.9800 . ? C85 H85B 0.9800 . ? C85 H85C 0.9800 . ? C86 H86A 0.9800 . ? C86 H86B 0.9800 . ? C86 H86C 0.9800 . ? O100 C102 1.38(2) . ? O100 C104 1.41(2) . ? C101 C103 1.369(19) . ? C101 C104 1.44(2) . ? C101 H10A 0.9900 . ? C101 H10B 0.9900 . ? C102 C103 1.56(2) . ? C102 H10C 0.9900 . ? C102 H10D 0.9900 . ? C103 H10E 0.9900 . ? C103 H10F 0.9900 . ? C104 H10G 0.9900 . ? C104 H10H 0.9900 . ? C201 C202 1.429(18) . ? C201 H20A 0.9800 . ? C201 H20B 0.9800 . ? C201 H20C 0.9800 . ? C202 C203 1.410(17) . ? C202 H20D 0.9900 . ? C202 H20E 0.9900 . ? C203 C202 1.410(17) 3_755 ? C203 H20F 0.9900 . ? C203 H20G 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 Y1 O4 108.03(15) . 2_654 ? O1 Y1 O2 88.79(14) . . ? O4 Y1 O2 130.46(14) 2_654 . ? O1 Y1 O3 132.14(14) . . ? O4 Y1 O3 90.38(14) 2_654 . ? O2 Y1 O3 112.49(14) . . ? O1 Y1 N2 117.01(14) . . ? O4 Y1 N2 98.83(14) 2_654 . ? O2 Y1 N2 35.39(13) . . ? O3 Y1 N2 102.46(14) . . ? O1 Y1 N3 99.02(14) . . ? O4 Y1 N3 116.09(14) 2_654 . ? O2 Y1 N3 106.16(14) . . ? O3 Y1 N3 35.22(13) . . ? N2 Y1 N3 118.35(16) . . ? O1 Y1 K2 137.42(10) . 2_654 ? O4 Y1 K2 48.72(10) 2_654 2_654 ? O2 Y1 K2 133.78(9) . 2_654 ? O3 Y1 K2 41.76(9) . 2_654 ? N2 Y1 K2 103.01(10) . 2_654 ? N3 Y1 K2 72.22(10) . 2_654 ? O1 Y1 K1 46.12(10) . . ? O4 Y1 K1 134.22(11) 2_654 . ? O2 Y1 K1 42.72(9) . . ? O3 Y1 K1 135.40(9) . . ? N2 Y1 K1 74.35(10) . . ? N3 Y1 K1 106.23(10) . . ? K2 Y1 K1 176.01(3) 2_654 . ? O7 K1 O2 108.68(12) . . ? O7 K1 N1 108.69(13) . . ? O2 K1 N1 95.02(12) . . ? O7 K1 O1 117.42(12) . . ? O2 K1 O1 65.39(11) . . ? N1 K1 O1 29.64(11) . . ? O7 K1 O6 66.14(11) . . ? O2 K1 O6 140.31(12) . . ? N1 K1 O6 124.38(12) . . ? O1 K1 O6 153.71(11) . . ? O7 K1 N6 93.87(12) . . ? O2 K1 N6 137.30(13) . . ? N1 K1 N6 111.82(14) . . ? O1 K1 N6 134.32(13) . . ? O6 K1 N6 28.25(11) . . ? O7 K1 C15 65.84(13) . . ? O2 K1 C15 95.84(14) . . ? N1 K1 C15 45.03(15) . . ? O1 K1 C15 54.04(13) . . ? O6 K1 C15 114.68(13) . . ? N6 K1 C15 126.71(15) . . ? O7 K1 C75 55.44(13) . . ? O2 K1 C75 79.69(13) . . ? N1 K1 C75 159.10(15) . . ? O1 K1 C75 140.10(13) . . ? O6 K1 C75 65.01(12) . . ? N6 K1 C75 84.59(14) . . ? C15 K1 C75 114.95(16) . . ? O7 K1 Y2 33.34(8) . . ? O2 K1 Y2 129.54(9) . . ? N1 K1 Y2 123.26(10) . . ? O1 K1 Y2 145.23(9) . . ? O6 K1 Y2 32.85(7) . . ? N6 K1 Y2 60.88(9) . . ? C15 K1 Y2 91.36(11) . . ? C75 K1 Y2 52.50(10) . . ? O7 K1 Y1 116.65(8) . . ? O2 K1 Y1 33.25(8) . . ? N1 K1 Y1 61.78(9) . . ? O1 K1 Y1 32.17(7) . . ? O6 K1 Y1 172.86(8) . . ? N6 K1 Y1 149.44(10) . . ? C15 K1 Y1 72.07(11) . . ? C75 K1 Y1 110.57(10) . . ? Y2 K1 Y1 149.18(4) . . ? O5 Y2 O6 109.40(15) . . ? O5 Y2 O8 88.72(14) . . ? O6 Y2 O8 132.79(14) . . ? O5 Y2 O7 131.30(14) . . ? O6 Y2 O7 91.85(14) . . ? O8 Y2 O7 108.52(14) . . ? O5 Y2 N8 116.97(15) . . ? O6 Y2 N8 100.73(15) . . ? O8 Y2 N8 35.20(13) . . ? O7 Y2 N8 100.31(15) . . ? O5 Y2 N7 96.46(15) . . ? O6 Y2 N7 114.23(14) . . ? O8 Y2 N7 106.07(14) . . ? O7 Y2 N7 35.52(14) . . ? N8 Y2 N7 119.49(16) . . ? O5 Y2 K2 46.10(10) . . ? O6 Y2 K2 135.76(10) . . ? O8 Y2 K2 42.61(10) . . ? O7 Y2 K2 132.37(10) . . ? N8 Y2 K2 73.69(11) . . ? N7 Y2 K2 105.84(11) . . ? O5 Y2 K1 134.36(10) . . ? O6 Y2 K1 49.09(10) . . ? O8 Y2 K1 136.52(10) . . ? O7 Y2 K1 42.84(10) . . ? N8 Y2 K1 107.33(11) . . ? N7 Y2 K1 69.37(11) . . ? K2 Y2 K1 175.06(3) . . ? O3 K2 O8 114.46(12) 2_655 . ? O3 K2 O5 134.13(12) 2_655 . ? O8 K2 O5 65.86(11) . . ? O3 K2 N5 124.82(14) 2_655 . ? O8 K2 N5 94.96(13) . . ? O5 K2 N5 29.21(11) . . ? O3 K2 N4 94.43(12) 2_655 . ? O8 K2 N4 117.20(13) . . ? O5 K2 N4 127.58(12) . . ? N5 K2 N4 112.77(15) . . ? O3 K2 O4 66.09(11) 2_655 . ? O8 K2 O4 127.50(12) . . ? O5 K2 O4 153.30(11) . . ? N5 K2 O4 129.32(13) . . ? N4 K2 O4 28.35(10) . . ? O3 K2 Y2 131.69(9) 2_655 . ? O8 K2 Y2 33.44(8) . . ? O5 K2 Y2 32.42(8) . . ? N5 K2 Y2 61.55(10) . . ? N4 K2 Y2 129.45(10) . . ? O4 K2 Y2 153.69(8) . . ? O3 K2 Y1 33.61(8) 2_655 2_655 ? O8 K2 Y1 126.24(9) . 2_655 ? O5 K2 Y1 163.02(9) . 2_655 ? N5 K2 Y1 137.48(10) . 2_655 ? N4 K2 Y1 60.88(9) . 2_655 ? O4 K2 Y1 32.54(7) . 2_655 ? Y2 K2 Y1 157.70(4) . 2_655 ? N1 O1 Y1 172.6(3) . . ? N1 O1 K1 71.6(2) . . ? Y1 O1 K1 101.72(14) . . ? O1 N1 C14 107.4(4) . . ? O1 N1 C11 107.6(4) . . ? C14 N1 C11 114.6(5) . . ? O1 N1 K1 78.8(2) . . ? C14 N1 K1 116.1(3) . . ? C11 N1 K1 123.8(4) . . ? N1 C11 C13 109.4(5) . . ? N1 C11 C12 115.1(5) . . ? C13 C11 C12 111.4(5) . . ? N1 C11 H11A 106.8 . . ? C13 C11 H11A 106.8 . . ? C12 C11 H11A 106.8 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N1 C14 C15 109.1(5) . . ? N1 C14 C16 111.1(5) . . ? C15 C14 C16 109.6(5) . . ? N1 C14 H14A 109.0 . . ? C15 C14 H14A 109.0 . . ? C16 C14 H14A 109.0 . . ? C14 C15 K1 87.7(4) . . ? C14 C15 H15A 109.5 . . ? K1 C15 H15A 73.2 . . ? C14 C15 H15B 109.5 . . ? K1 C15 H15B 159.6 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? K1 C15 H15C 52.6 . . ? 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 . . ? N2 O2 Y1 82.9(2) . . ? N2 O2 K1 146.8(3) . . ? Y1 O2 K1 104.02(13) . . ? O2 N2 C24 109.5(4) . . ? O2 N2 C21 108.7(4) . . ? C24 N2 C21 116.1(5) . . ? O2 N2 Y1 61.7(2) . . ? C24 N2 Y1 123.3(4) . . ? C21 N2 Y1 119.5(3) . . ? N2 C21 C22 112.6(5) . . ? N2 C21 C23 116.5(5) . . ? C22 C21 C23 110.1(5) . . ? N2 C21 H21A 105.5 . . ? C22 C21 H21A 105.5 . . ? C23 C21 H21A 105.5 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N2 C24 C26 109.2(5) . . ? N2 C24 C25 114.5(5) . . ? C26 C24 C25 111.0(5) . . ? N2 C24 H24A 107.3 . . ? C26 C24 H24A 107.3 . . ? C25 C24 H24A 107.3 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N3 O3 Y1 82.4(2) . . ? N3 O3 K2 142.4(3) . 2_654 ? Y1 O3 K2 104.63(14) . 2_654 ? O3 N3 C34 107.8(4) . . ? O3 N3 C31 108.4(4) . . ? C34 N3 C31 112.2(5) . . ? O3 N3 Y1 62.3(2) . . ? C34 N3 Y1 116.4(3) . . ? C31 N3 Y1 130.9(4) . . ? N3 C31 C33 111.0(5) . . ? N3 C31 C32 112.5(5) . . ? C33 C31 C32 110.7(5) . . ? N3 C31 H31A 107.5 . . ? C33 C31 H31A 107.5 . . ? C32 C31 H31A 107.5 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N3 C34 C35 111.2(5) . . ? N3 C34 C36 111.1(5) . . ? C35 C34 C36 109.1(5) . . ? N3 C34 H34A 108.4 . . ? C35 C34 H34A 108.4 . . ? C36 C34 H34A 108.4 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N4 O4 Y1 173.0(3) . 2_655 ? N4 O4 K2 74.5(2) . . ? Y1 O4 K2 98.75(14) 2_655 . ? O4 N4 C44 107.7(4) . . ? O4 N4 C41 107.5(4) . . ? C44 N4 C41 113.4(5) . . ? O4 N4 K2 77.2(2) . . ? C44 N4 K2 110.0(3) . . ? C41 N4 K2 131.9(4) . . ? N4 C41 C43 110.4(5) . . ? N4 C41 C42 113.9(5) . . ? C43 C41 C42 110.8(5) . . ? N4 C41 H41A 107.1 . . ? C43 C41 H41A 107.1 . . ? C42 C41 H41A 107.1 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? N4 C44 C45 110.2(5) . . ? N4 C44 C46 109.0(5) . . ? C45 C44 C46 110.7(5) . . ? N4 C44 H44A 109.0 . . ? C45 C44 H44A 109.0 . . ? C46 C44 H44A 109.0 . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C44 C46 H46A 109.5 . . ? C44 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C44 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? N5 O5 Y2 174.1(3) . . ? N5 O5 K2 76.3(2) . . ? Y2 O5 K2 101.48(14) . . ? O5 N5 C54 107.1(4) . . ? O5 N5 C51 106.7(4) . . ? C54 N5 C51 114.9(5) . . ? O5 N5 K2 74.4(2) . . ? C54 N5 K2 114.9(4) . . ? C51 N5 K2 127.0(4) . . ? N5 C51 C53 109.7(5) . . ? N5 C51 C52 115.3(5) . . ? C53 C51 C52 110.3(6) . . ? N5 C51 H51A 107.1 . . ? C53 C51 H51A 107.1 . . ? C52 C51 H51A 107.1 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C51 C53 H53A 109.5 . . ? C51 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C51 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? N5 C54 C55 110.8(5) . . ? N5 C54 C56 109.5(6) . . ? C55 C54 C56 111.4(6) . . ? N5 C54 H54A 108.3 . . ? C55 C54 H54A 108.3 . . ? C56 C54 H54A 108.3 . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C54 C56 H56A 109.5 . . ? C54 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C54 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? N6 O6 Y2 169.7(3) . . ? N6 O6 K1 77.1(2) . . ? Y2 O6 K1 98.06(13) . . ? O6 N6 C61 106.6(4) . . ? O6 N6 C64 107.5(4) . . ? C61 N6 C64 112.5(5) . . ? O6 N6 K1 74.7(2) . . ? C61 N6 K1 117.1(4) . . ? C64 N6 K1 127.3(3) . . ? N6 C61 C62 108.5(5) . . ? N6 C61 C63 111.6(5) . . ? C62 C61 C63 109.4(6) . . ? N6 C61 H61A 109.1 . . ? C62 C61 H61A 109.1 . . ? C63 C61 H61A 109.1 . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? N6 C64 C66 110.2(5) . . ? N6 C64 C65 114.7(5) . . ? C66 C64 C65 110.7(6) . . ? N6 C64 H64A 107.0 . . ? C66 C64 H64A 107.0 . . ? C65 C64 H64A 107.0 . . ? C64 C65 H65A 109.5 . . ? C64 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C64 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C64 C66 H66A 109.5 . . ? C64 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C64 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? N7 O7 Y2 83.4(2) . . ? N7 O7 K1 128.7(3) . . ? Y2 O7 K1 103.82(14) . . ? O7 N7 C74 106.9(4) . . ? O7 N7 C71 108.0(4) . . ? C74 N7 C71 113.1(4) . . ? O7 N7 Y2 61.1(2) . . ? C74 N7 Y2 118.0(3) . . ? C71 N7 Y2 128.8(3) . . ? N7 C71 C72 110.8(5) . . ? N7 C71 C73 114.7(5) . . ? C72 C71 C73 110.2(5) . . ? N7 C71 H71A 106.9 . . ? C72 C71 H71A 106.9 . . ? C73 C71 H71A 106.9 . . ? C71 C72 H72A 109.5 . . ? C71 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C71 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C71 C73 H73A 109.5 . . ? C71 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C71 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? N7 C74 C76 113.2(5) . . ? N7 C74 C75 109.6(5) . . ? C76 C74 C75 109.6(5) . . ? N7 C74 H74A 108.1 . . ? C76 C74 H74A 108.1 . . ? C75 C74 H74A 108.1 . . ? C74 C75 K1 86.3(3) . . ? C74 C75 H75A 114.3 . . ? K1 C75 H75A 114.3 . . ? C74 C75 H75B 114.3 . . ? K1 C75 H75B 114.3 . . ? H75A C75 H75B 111.4 . . ? C74 C76 H76A 109.5 . . ? C74 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C74 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? N8 O8 Y2 83.5(2) . . ? N8 O8 K2 145.0(3) . . ? Y2 O8 K2 103.95(14) . . ? O8 N8 C81 108.4(4) . . ? O8 N8 C84 108.7(4) . . ? C81 N8 C84 116.3(5) . . ? O8 N8 Y2 61.3(2) . . ? C81 N8 Y2 122.3(4) . . ? C84 N8 Y2 120.7(4) . . ? N8 C81 C82 115.6(5) . . ? N8 C81 C83 108.7(5) . . ? C82 C81 C83 110.3(5) . . ? N8 C81 H81A 107.3 . . ? C82 C81 H81A 107.3 . . ? C83 C81 H81A 107.3 . . ? C81 C82 H82A 109.5 . . ? C81 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C81 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? C81 C83 H83A 109.5 . . ? C81 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C81 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? N8 C84 C85 117.1(5) . . ? N8 C84 C86 111.6(5) . . ? C85 C84 C86 109.6(5) . . ? N8 C84 H84A 105.9 . . ? C85 C84 H84A 105.9 . . ? C86 C84 H84A 105.9 . . ? C84 C85 H85A 109.5 . . ? C84 C85 H85B 109.5 . . ? H85A C85 H85B 109.5 . . ? C84 C85 H85C 109.5 . . ? H85A C85 H85C 109.5 . . ? H85B C85 H85C 109.5 . . ? C84 C86 H86A 109.5 . . ? C84 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? C84 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? C102 O100 C104 101.9(19) . . ? C103 C101 C104 94.7(16) . . ? C103 C101 H10A 112.8 . . ? C104 C101 H10A 112.8 . . ? C103 C101 H10B 112.8 . . ? C104 C101 H10B 112.8 . . ? H10A C101 H10B 110.2 . . ? O100 C102 C103 101.2(16) . . ? O100 C102 H10C 111.5 . . ? C103 C102 H10C 111.5 . . ? O100 C102 H10D 111.5 . . ? C103 C102 H10D 111.5 . . ? H10C C102 H10D 109.3 . . ? C101 C103 C102 95.2(15) . . ? C101 C103 H10E 112.7 . . ? C102 C103 H10E 112.7 . . ? C101 C103 H10F 112.7 . . ? C102 C103 H10F 112.7 . . ? H10E C103 H10F 110.2 . . ? O100 C104 C101 108.6(18) . . ? O100 C104 H10G 110.0 . . ? C101 C104 H10G 110.0 . . ? O100 C104 H10H 110.0 . . ? C101 C104 H10H 110.0 . . ? H10G C104 H10H 108.4 . . ? C202 C201 H20A 109.5 . . ? C202 C201 H20B 109.5 . . ? H20A C201 H20B 109.5 . . ? C202 C201 H20C 109.5 . . ? H20A C201 H20C 109.5 . . ? H20B C201 H20C 109.5 . . ? C203 C202 C201 124.7(18) . . ? C203 C202 H20D 106.1 . . ? C201 C202 H20D 106.2 . . ? C203 C202 H20E 106.1 . . ? C201 C202 H20E 106.2 . . ? H20D C202 H20E 106.3 . . ? C202 C203 C202 142(3) 3_755 . ? C202 C203 H20F 101.4 3_755 . ? C202 C203 H20F 101.4 . . ? C202 C203 H20G 101.4 3_755 . ? C202 C203 H20G 101.4 . . ? H20F C203 H20G 104.6 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.15 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.968 _refine_diff_density_min -0.592 _refine_diff_density_rms 0.100