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 Michael David Ward' _publ_contact_author_address ; Department of Chemistry University of Sheffield Dainton Building Sheffield South Yorks. S3 7HF UNITED KINGDOM ; _publ_contact_author_fax '0114 2229346' _publ_contact_author_email m.d.ward@sheffield.ac.uk _publ_section_title ; Structural and near-infrared photophysical studies on ternary lanthanide complexes containing poly(pyrazolyl)borate and 1,3-diketonate ligands ; _publ_contact_letter ; This CIF file contains details of the nine crystal structure in the paper Structural and near-infrared photophysical studies on ternary lanthanide complexes... by G. M. Davies et al., submitted to Dalton Trans. for publication. ; loop_ _publ_author_name 'Michael David Ward' 'Rebecca J. Aarons' 'Harry Adams' 'Graham M. Davies' 'Stephen Faulkner' 'John C. Jeffery' ; G.R.Motson ; #======================================================== data_sad _database_code_depnum_ccdc_archive 'CCDC 229463' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H41 B Eu N9 O4' _chemical_formula_weight 1042.73 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' B B 0.0013 0.0007 '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' Eu Eu -0.1578 3.6682 '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 11.3843(14) _cell_length_b 14.1792(17) _cell_length_c 16.376(2) _cell_angle_alpha 108.294(2) _cell_angle_beta 91.575(2) _cell_angle_gamma 110.801(2) _cell_volume 2317.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.494 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 1.412 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8717 _exptl_absorpt_correction_T_max 0.8717 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24399 _diffrn_reflns_av_R_equivalents 0.0292 _diffrn_reflns_av_sigmaI/netI 0.0488 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 27.49 _reflns_number_total 10522 _reflns_number_gt 8898 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0204P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10522 _refine_ls_number_parameters 626 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0356 _refine_ls_R_factor_gt 0.0262 _refine_ls_wR_factor_ref 0.0512 _refine_ls_wR_factor_gt 0.0495 _refine_ls_goodness_of_fit_ref 0.941 _refine_ls_restrained_S_all 0.941 _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 Eu1 Eu 0.538957(11) -0.051037(9) 0.747924(7) 0.02259(4) Uani 1 1 d . . . B1 B 0.5717(3) 0.2616(2) 0.83312(18) 0.0294(6) Uani 1 1 d . . . H1 H 0.663(2) 0.3014(16) 0.8778(13) 0.023(6) Uiso 1 1 d . . . N11 N 0.59946(17) 0.21331(14) 0.73983(12) 0.0283(4) Uani 1 1 d . . . N12 N 0.58644(17) 0.10979(13) 0.69903(11) 0.0252(4) Uani 1 1 d . . . C13 C 0.6360(2) 0.10683(17) 0.62519(14) 0.0247(5) Uani 1 1 d . . . C14 C 0.6809(2) 0.20854(19) 0.61817(16) 0.0352(6) Uani 1 1 d . . . H14 H 0.7192 0.2283 0.5734 0.042 Uiso 1 1 calc R . . C15 C 0.6564(2) 0.27263(19) 0.69132(17) 0.0378(6) Uani 1 1 d . . . H15 H 0.6759 0.3459 0.7056 0.045 Uiso 1 1 calc R . . N21 N 0.60002(17) -0.07892(14) 0.59438(12) 0.0262(4) Uani 1 1 d . . . C22 C 0.6335(2) 0.00466(17) 0.56493(14) 0.0245(5) Uani 1 1 d . . . C23 C 0.6614(2) -0.00658(19) 0.48151(15) 0.0307(5) Uani 1 1 d . . . H23 H 0.6849 0.0523 0.4630 0.037 Uiso 1 1 calc R . . C24 C 0.6544(2) -0.10513(19) 0.42573(15) 0.0340(6) Uani 1 1 d . . . H24 H 0.6717 -0.1140 0.3693 0.041 Uiso 1 1 calc R . . C25 C 0.6210(2) -0.18988(19) 0.45615(15) 0.0341(6) Uani 1 1 d . . . H25 H 0.6159 -0.2572 0.4205 0.041 Uiso 1 1 calc R . . C26 C 0.5953(2) -0.17379(18) 0.53975(15) 0.0318(5) Uani 1 1 d . . . H26 H 0.5735 -0.2316 0.5596 0.038 Uiso 1 1 calc R . . N31 N 0.47107(17) 0.17733(14) 0.86348(12) 0.0264(4) Uani 1 1 d . . . N32 N 0.47808(17) 0.08269(13) 0.86174(11) 0.0253(4) Uani 1 1 d . . . C33 C 0.3924(2) 0.04393(17) 0.90993(14) 0.0263(5) Uani 1 1 d . . . C34 C 0.3316(2) 0.11432(19) 0.94387(16) 0.0357(6) Uani 1 1 d . . . H34 H 0.2692 0.1069 0.9795 0.043 Uiso 1 1 calc R . . C35 C 0.3842(2) 0.19662(19) 0.91297(16) 0.0364(6) Uani 1 1 d . . . H35 H 0.3631 0.2567 0.9244 0.044 Uiso 1 1 calc R . . N41 N 0.42987(18) -0.11917(14) 0.86380(12) 0.0285(4) Uani 1 1 d . . . C42 C 0.3727(2) -0.06120(17) 0.91693(14) 0.0257(5) Uani 1 1 d . . . C43 C 0.2989(2) -0.09888(18) 0.97405(15) 0.0316(5) Uani 1 1 d . . . H43 H 0.2598 -0.0578 1.0098 0.038 Uiso 1 1 calc R . . C44 C 0.2838(2) -0.19921(19) 0.97731(16) 0.0356(6) Uani 1 1 d . . . H44 H 0.2361 -0.2255 1.0162 0.043 Uiso 1 1 calc R . . C45 C 0.3402(2) -0.25891(18) 0.92253(15) 0.0345(6) Uani 1 1 d . . . H45 H 0.3302 -0.3268 0.9228 0.041 Uiso 1 1 calc R . . C46 C 0.4121(2) -0.21636(18) 0.86694(16) 0.0341(6) Uani 1 1 d . . . H46 H 0.4501 -0.2572 0.8298 0.041 Uiso 1 1 calc R . . N51 N 0.51761(18) 0.34599(14) 0.83208(12) 0.0307(4) Uani 1 1 d . . . N52 N 0.41216(19) 0.32055(14) 0.77503(12) 0.0314(4) Uani 1 1 d . . . C53 C 0.3833(2) 0.40824(17) 0.79847(15) 0.0291(5) Uani 1 1 d . . . C54 C 0.4693(2) 0.48939(19) 0.87036(17) 0.0397(6) Uani 1 1 d . . . H54 H 0.4700 0.5577 0.8988 0.048 Uiso 1 1 calc R . . C55 C 0.5517(2) 0.44657(18) 0.88964(17) 0.0384(6) Uani 1 1 d . . . H55 H 0.6200 0.4810 0.9349 0.046 Uiso 1 1 calc R . . N61 N 0.2626(2) 0.50539(16) 0.77096(14) 0.0410(5) Uani 1 1 d . . . C62 C 0.2710(2) 0.40886(18) 0.75261(15) 0.0315(5) Uani 1 1 d . . . C63 C 0.1779(3) 0.3144(2) 0.69634(16) 0.0407(6) Uani 1 1 d . . . H63 H 0.1877 0.2492 0.6838 0.049 Uiso 1 1 calc R . . C64 C 0.0711(3) 0.3189(3) 0.65952(18) 0.0551(8) Uani 1 1 d . . . H64 H 0.0063 0.2565 0.6231 0.066 Uiso 1 1 calc R . . C65 C 0.0611(3) 0.4170(3) 0.67712(19) 0.0543(8) Uani 1 1 d . . . H65 H -0.0096 0.4223 0.6523 0.065 Uiso 1 1 calc R . . C66 C 0.1589(3) 0.5073(2) 0.73269(19) 0.0514(8) Uani 1 1 d . . . H66 H 0.1521 0.5735 0.7441 0.062 Uiso 1 1 calc R . . C71 C 0.8184(2) -0.21016(19) 0.80101(15) 0.0328(5) Uani 1 1 d . . . C72 C 0.7240(3) -0.3111(2) 0.78156(18) 0.0437(7) Uani 1 1 d . . . H72 H 0.6393 -0.3198 0.7724 0.052 Uiso 1 1 calc R . . C73 C 0.7530(3) -0.3993(2) 0.7754(2) 0.0541(8) Uani 1 1 d . . . H73 H 0.6881 -0.4665 0.7629 0.065 Uiso 1 1 calc R . . C74 C 0.8780(3) -0.3878(2) 0.7879(2) 0.0561(8) Uani 1 1 d . . . H74 H 0.8976 -0.4472 0.7840 0.067 Uiso 1 1 calc R . . C75 C 0.9742(3) -0.2883(2) 0.80621(19) 0.0534(8) Uani 1 1 d . . . H75 H 1.0587 -0.2808 0.8141 0.064 Uiso 1 1 calc R . . C76 C 0.9450(3) -0.1994(2) 0.81279(17) 0.0443(7) Uani 1 1 d . . . H76 H 1.0101 -0.1323 0.8251 0.053 Uiso 1 1 calc R . . O77 O 0.66748(14) -0.14042(12) 0.77402(10) 0.0316(4) Uani 1 1 d . . . C77 C 0.7815(2) -0.11657(18) 0.80656(14) 0.0278(5) Uani 1 1 d . . . C78 C 0.8703(2) -0.01128(18) 0.84595(15) 0.0310(5) Uani 1 1 d . . . H78 H 0.9487 -0.0010 0.8734 0.037 Uiso 1 1 calc R . . O79 O 0.74184(14) 0.07491(12) 0.81458(10) 0.0300(4) Uani 1 1 d . . . C79 C 0.8474(2) 0.07962(18) 0.84632(14) 0.0278(5) Uani 1 1 d . . . C81 C 0.9489(2) 0.19004(18) 0.88450(14) 0.0285(5) Uani 1 1 d . . . C82 C 1.0517(2) 0.2163(2) 0.94643(17) 0.0407(6) Uani 1 1 d . . . H82 H 1.0618 0.1632 0.9644 0.049 Uiso 1 1 calc R . . C83 C 1.1393(3) 0.3212(2) 0.98151(19) 0.0518(7) Uani 1 1 d . . . H83 H 1.2085 0.3382 1.0226 0.062 Uiso 1 1 calc R . . C84 C 1.1247(3) 0.4011(2) 0.95590(19) 0.0544(8) Uani 1 1 d . . . H84 H 1.1833 0.4716 0.9802 0.065 Uiso 1 1 calc R . . C85 C 1.0233(3) 0.3758(2) 0.89449(18) 0.0470(7) Uani 1 1 d . . . H85 H 1.0138 0.4290 0.8765 0.056 Uiso 1 1 calc R . . C86 C 0.9356(2) 0.27125(19) 0.85942(16) 0.0368(6) Uani 1 1 d . . . H86 H 0.8667 0.2549 0.8184 0.044 Uiso 1 1 calc R . . C91 C 0.2875(2) -0.40226(17) 0.56644(15) 0.0313(5) Uani 1 1 d . . . C92 C 0.3714(2) -0.44621(19) 0.58525(17) 0.0409(6) Uani 1 1 d . . . H92 H 0.4371 -0.4061 0.6321 0.049 Uiso 1 1 calc R . . C93 C 0.3584(3) -0.5493(2) 0.5349(2) 0.0520(8) Uani 1 1 d . . . H93 H 0.4151 -0.5779 0.5484 0.062 Uiso 1 1 calc R . . C94 C 0.2623(3) -0.6093(2) 0.4656(2) 0.0575(8) Uani 1 1 d . . . H94 H 0.2541 -0.6783 0.4317 0.069 Uiso 1 1 calc R . . C95 C 0.1782(3) -0.5673(2) 0.44623(18) 0.0531(8) Uani 1 1 d . . . H95 H 0.1126 -0.6083 0.3993 0.064 Uiso 1 1 calc R . . C96 C 0.1898(3) -0.4649(2) 0.49559(17) 0.0425(6) Uani 1 1 d . . . H96 H 0.1322 -0.4373 0.4816 0.051 Uiso 1 1 calc R . . O97 O 0.41804(14) -0.23271(11) 0.66656(10) 0.0289(4) Uani 1 1 d . . . C97 C 0.3090(2) -0.28859(17) 0.62075(14) 0.0273(5) Uani 1 1 d . . . C98 C 0.2124(2) -0.25017(18) 0.61727(16) 0.0338(6) Uani 1 1 d . . . H98 H 0.1320 -0.2988 0.5876 0.041 Uiso 1 1 calc R . . O99 O 0.33500(14) -0.06856(11) 0.69936(10) 0.0286(3) Uani 1 1 d . . . C99 C 0.2310(2) -0.14173(18) 0.65653(14) 0.0272(5) Uani 1 1 d . . . C101 C 0.1261(2) -0.10338(18) 0.64457(15) 0.0297(5) Uani 1 1 d . . . C102 C 0.1335(2) -0.0059(2) 0.70287(16) 0.0356(6) Uani 1 1 d . . . H102 H 0.1985 0.0316 0.7504 0.043 Uiso 1 1 calc R . . C103 C 0.0441(3) 0.0363(2) 0.69053(19) 0.0455(7) Uani 1 1 d . . . H103 H 0.0479 0.1010 0.7305 0.055 Uiso 1 1 calc R . . C104 C -0.0505(3) -0.0182(3) 0.6188(2) 0.0580(8) Uani 1 1 d . . . H104 H -0.1095 0.0105 0.6098 0.070 Uiso 1 1 calc R . . C105 C -0.0573(3) -0.1147(3) 0.5606(2) 0.0614(9) Uani 1 1 d . . . H105 H -0.1207 -0.1509 0.5121 0.074 Uiso 1 1 calc R . . C106 C 0.0291(2) -0.1583(2) 0.57378(19) 0.0466(7) Uani 1 1 d . . . H106 H 0.0223 -0.2246 0.5351 0.056 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.02309(6) 0.02139(6) 0.02404(6) 0.00676(4) 0.00179(4) 0.01048(4) B1 0.0315(16) 0.0212(13) 0.0325(15) 0.0066(11) -0.0019(12) 0.0094(11) N11 0.0307(11) 0.0215(10) 0.0339(11) 0.0092(8) 0.0029(9) 0.0118(8) N12 0.0266(10) 0.0235(9) 0.0270(10) 0.0081(8) 0.0022(8) 0.0120(8) C13 0.0177(11) 0.0288(12) 0.0304(13) 0.0131(10) 0.0022(10) 0.0098(9) C14 0.0328(14) 0.0380(14) 0.0411(15) 0.0201(12) 0.0108(12) 0.0148(11) C15 0.0398(15) 0.0255(12) 0.0509(16) 0.0172(12) 0.0087(13) 0.0121(11) N21 0.0255(10) 0.0281(10) 0.0280(10) 0.0105(8) 0.0057(8) 0.0130(8) C22 0.0168(11) 0.0307(12) 0.0287(13) 0.0121(10) 0.0016(9) 0.0107(9) C23 0.0264(13) 0.0374(13) 0.0352(14) 0.0182(11) 0.0071(11) 0.0151(11) C24 0.0287(13) 0.0481(15) 0.0277(13) 0.0124(12) 0.0077(11) 0.0182(12) C25 0.0334(14) 0.0353(13) 0.0321(14) 0.0048(11) 0.0064(11) 0.0174(11) C26 0.0334(14) 0.0301(12) 0.0357(14) 0.0107(11) 0.0091(11) 0.0168(11) N31 0.0303(11) 0.0235(9) 0.0276(10) 0.0063(8) 0.0011(9) 0.0151(8) N32 0.0282(10) 0.0224(9) 0.0252(10) 0.0064(8) -0.0002(8) 0.0116(8) C33 0.0277(13) 0.0269(12) 0.0233(12) 0.0053(9) 0.0000(10) 0.0124(10) C34 0.0402(15) 0.0371(14) 0.0400(15) 0.0156(12) 0.0163(12) 0.0236(12) C35 0.0435(16) 0.0342(13) 0.0385(15) 0.0098(11) 0.0105(12) 0.0250(12) N41 0.0330(11) 0.0276(10) 0.0286(11) 0.0100(8) 0.0058(9) 0.0153(9) C42 0.0263(12) 0.0266(12) 0.0231(12) 0.0056(9) -0.0005(10) 0.0116(10) C43 0.0335(14) 0.0360(13) 0.0304(13) 0.0116(11) 0.0101(11) 0.0187(11) C44 0.0394(15) 0.0384(14) 0.0363(14) 0.0195(12) 0.0144(12) 0.0171(12) C45 0.0427(15) 0.0269(12) 0.0367(14) 0.0126(11) 0.0103(12) 0.0151(11) C46 0.0410(15) 0.0309(13) 0.0356(14) 0.0104(11) 0.0124(12) 0.0202(11) N51 0.0343(12) 0.0236(10) 0.0316(11) 0.0061(9) 0.0002(9) 0.0116(9) N52 0.0370(12) 0.0270(10) 0.0295(11) 0.0051(9) -0.0003(9) 0.0161(9) C53 0.0357(14) 0.0241(12) 0.0312(13) 0.0099(10) 0.0100(11) 0.0151(10) C54 0.0398(15) 0.0236(12) 0.0519(17) 0.0048(12) 0.0014(13) 0.0156(11) C55 0.0380(15) 0.0227(12) 0.0435(15) 0.0024(11) -0.0054(12) 0.0079(11) N61 0.0468(14) 0.0404(12) 0.0466(13) 0.0168(11) 0.0082(11) 0.0276(11) C62 0.0377(14) 0.0337(13) 0.0303(13) 0.0124(11) 0.0095(11) 0.0205(11) C63 0.0462(17) 0.0402(15) 0.0376(15) 0.0090(12) 0.0034(13) 0.0228(13) C64 0.0524(19) 0.065(2) 0.0420(17) 0.0040(15) -0.0075(14) 0.0296(16) C65 0.057(2) 0.077(2) 0.0459(18) 0.0217(17) 0.0041(15) 0.0452(18) C66 0.063(2) 0.0560(18) 0.059(2) 0.0266(16) 0.0165(17) 0.0426(17) C71 0.0387(15) 0.0382(14) 0.0318(14) 0.0142(11) 0.0088(11) 0.0243(12) C72 0.0454(17) 0.0395(15) 0.0560(18) 0.0179(13) 0.0139(14) 0.0260(13) C73 0.066(2) 0.0399(16) 0.069(2) 0.0237(15) 0.0218(17) 0.0299(15) C74 0.076(2) 0.0549(19) 0.066(2) 0.0289(17) 0.0215(18) 0.0500(18) C75 0.057(2) 0.065(2) 0.060(2) 0.0224(16) 0.0110(16) 0.0464(17) C76 0.0436(17) 0.0461(16) 0.0515(17) 0.0177(14) 0.0073(14) 0.0261(13) O77 0.0268(9) 0.0289(8) 0.0431(10) 0.0141(8) 0.0029(8) 0.0138(7) C77 0.0301(13) 0.0339(13) 0.0271(13) 0.0129(10) 0.0089(10) 0.0188(11) C78 0.0257(13) 0.0370(13) 0.0334(14) 0.0104(11) 0.0016(11) 0.0172(11) O79 0.0240(9) 0.0282(8) 0.0362(9) 0.0082(7) -0.0041(7) 0.0115(7) C79 0.0277(13) 0.0337(13) 0.0209(12) 0.0064(10) 0.0055(10) 0.0132(10) C81 0.0243(12) 0.0316(12) 0.0253(12) 0.0033(10) 0.0047(10) 0.0115(10) C82 0.0327(15) 0.0416(15) 0.0435(16) 0.0076(12) -0.0026(12) 0.0163(12) C83 0.0313(16) 0.0511(17) 0.0527(18) 0.0000(14) -0.0142(13) 0.0099(13) C84 0.0382(17) 0.0376(16) 0.064(2) 0.0044(14) -0.0059(15) 0.0010(13) C85 0.0417(17) 0.0380(15) 0.0545(18) 0.0176(14) 0.0019(14) 0.0067(13) C86 0.0294(14) 0.0378(14) 0.0384(15) 0.0129(12) 0.0010(11) 0.0080(11) C91 0.0333(14) 0.0236(12) 0.0333(14) 0.0092(10) 0.0090(11) 0.0069(10) C92 0.0370(15) 0.0301(13) 0.0478(17) 0.0070(12) 0.0054(13) 0.0097(12) C93 0.0510(18) 0.0279(14) 0.074(2) 0.0119(14) 0.0123(16) 0.0165(13) C94 0.066(2) 0.0234(14) 0.066(2) 0.0011(14) 0.0165(17) 0.0100(14) C95 0.058(2) 0.0330(15) 0.0433(17) -0.0021(13) -0.0034(14) 0.0026(14) C96 0.0441(16) 0.0349(14) 0.0431(16) 0.0106(12) 0.0027(13) 0.0116(12) O97 0.0279(9) 0.0248(8) 0.0309(9) 0.0069(7) 0.0016(7) 0.0091(7) C97 0.0276(13) 0.0248(11) 0.0275(12) 0.0104(10) 0.0063(10) 0.0065(10) C98 0.0247(13) 0.0280(12) 0.0398(15) 0.0061(11) -0.0004(11) 0.0051(10) O99 0.0257(9) 0.0255(8) 0.0312(9) 0.0051(7) -0.0025(7) 0.0105(7) C99 0.0244(12) 0.0333(13) 0.0265(13) 0.0125(10) 0.0066(10) 0.0120(10) C101 0.0222(12) 0.0335(13) 0.0364(14) 0.0171(11) 0.0072(10) 0.0095(10) C102 0.0320(14) 0.0424(14) 0.0388(15) 0.0185(12) 0.0103(12) 0.0174(12) C103 0.0415(17) 0.0495(16) 0.0619(19) 0.0278(15) 0.0246(15) 0.0277(14) C104 0.0302(16) 0.070(2) 0.091(3) 0.039(2) 0.0101(17) 0.0299(15) C105 0.0316(16) 0.062(2) 0.084(2) 0.0230(19) -0.0161(16) 0.0144(15) C106 0.0310(15) 0.0437(15) 0.0587(19) 0.0131(14) -0.0060(13) 0.0120(12) _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 Eu1 O79 2.3288(15) . ? Eu1 O99 2.3346(15) . ? Eu1 O97 2.3520(15) . ? Eu1 O77 2.3563(14) . ? Eu1 N32 2.5169(18) . ? Eu1 N12 2.5355(17) . ? Eu1 N41 2.5505(18) . ? Eu1 N21 2.5747(18) . ? B1 N51 1.531(3) . ? B1 N31 1.555(3) . ? B1 N11 1.558(3) . ? N11 C15 1.349(3) . ? N11 N12 1.359(2) . ? N12 C13 1.343(3) . ? C13 C14 1.392(3) . ? C13 C22 1.465(3) . ? C14 C15 1.361(3) . ? N21 C26 1.343(3) . ? N21 C22 1.353(3) . ? C22 C23 1.384(3) . ? C23 C24 1.382(3) . ? C24 C25 1.378(3) . ? C25 C26 1.373(3) . ? N31 C35 1.344(3) . ? N31 N32 1.364(2) . ? N32 C33 1.345(3) . ? C33 C34 1.396(3) . ? C33 C42 1.469(3) . ? C34 C35 1.367(3) . ? N41 C46 1.338(3) . ? N41 C42 1.349(3) . ? C42 C43 1.380(3) . ? C43 C44 1.390(3) . ? C44 C45 1.369(3) . ? C45 C46 1.377(3) . ? N51 C55 1.347(3) . ? N51 N52 1.365(3) . ? N52 C53 1.341(3) . ? C53 C54 1.398(3) . ? C53 C62 1.469(3) . ? C54 C55 1.363(3) . ? N61 C66 1.334(3) . ? N61 C62 1.345(3) . ? C62 C63 1.389(3) . ? C63 C64 1.373(4) . ? C64 C65 1.375(4) . ? C65 C66 1.381(4) . ? C71 C72 1.381(3) . ? C71 C76 1.396(3) . ? C71 C77 1.506(3) . ? C72 C73 1.377(3) . ? C73 C74 1.376(4) . ? C74 C75 1.377(4) . ? C75 C76 1.388(3) . ? O77 C77 1.273(3) . ? C77 C78 1.398(3) . ? C78 C79 1.401(3) . ? O79 C79 1.267(3) . ? C79 C81 1.496(3) . ? C81 C82 1.388(3) . ? C81 C86 1.391(3) . ? C82 C83 1.385(4) . ? C83 C84 1.383(4) . ? C84 C85 1.374(4) . ? C85 C86 1.381(3) . ? C91 C92 1.387(3) . ? C91 C96 1.398(3) . ? C91 C97 1.502(3) . ? C92 C93 1.386(3) . ? C93 C94 1.369(4) . ? C94 C95 1.370(4) . ? C95 C96 1.379(4) . ? O97 C97 1.268(3) . ? C97 C98 1.397(3) . ? C98 C99 1.401(3) . ? O99 C99 1.263(3) . ? C99 C101 1.508(3) . ? C101 C102 1.384(3) . ? C101 C106 1.386(3) . ? C102 C103 1.390(3) . ? C103 C104 1.380(4) . ? C104 C105 1.375(4) . ? C105 C106 1.378(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O79 Eu1 O99 143.09(5) . . ? O79 Eu1 O97 145.11(5) . . ? O99 Eu1 O97 71.00(5) . . ? O79 Eu1 O77 70.65(5) . . ? O99 Eu1 O77 146.03(5) . . ? O97 Eu1 O77 76.59(5) . . ? O79 Eu1 N32 81.05(6) . . ? O99 Eu1 N32 71.33(5) . . ? O97 Eu1 N32 129.63(6) . . ? O77 Eu1 N32 126.13(6) . . ? O79 Eu1 N12 70.86(5) . . ? O99 Eu1 N12 78.20(5) . . ? O97 Eu1 N12 127.70(5) . . ? O77 Eu1 N12 131.79(5) . . ? N32 Eu1 N12 74.05(6) . . ? O79 Eu1 N41 107.22(6) . . ? O99 Eu1 N41 83.16(6) . . ? O97 Eu1 N41 78.28(6) . . ? O77 Eu1 N41 80.57(5) . . ? N32 Eu1 N41 65.13(6) . . ? N12 Eu1 N41 138.72(6) . . ? O79 Eu1 N21 92.66(6) . . ? O99 Eu1 N21 92.11(5) . . ? O97 Eu1 N21 74.82(5) . . ? O77 Eu1 N21 88.98(5) . . ? N32 Eu1 N21 138.31(5) . . ? N12 Eu1 N21 65.05(6) . . ? N41 Eu1 N21 152.75(6) . . ? N51 B1 N31 106.9(2) . . ? N51 B1 N11 107.77(18) . . ? N31 B1 N11 113.50(18) . . ? C15 N11 N12 109.05(18) . . ? C15 N11 B1 123.92(19) . . ? N12 N11 B1 126.54(17) . . ? C13 N12 N11 106.47(17) . . ? C13 N12 Eu1 118.29(13) . . ? N11 N12 Eu1 133.55(13) . . ? N12 C13 C14 110.4(2) . . ? N12 C13 C22 119.86(18) . . ? C14 C13 C22 129.8(2) . . ? C15 C14 C13 104.7(2) . . ? N11 C15 C14 109.4(2) . . ? C26 N21 C22 117.56(19) . . ? C26 N21 Eu1 123.51(14) . . ? C22 N21 Eu1 118.86(14) . . ? N21 C22 C23 121.6(2) . . ? N21 C22 C13 116.55(18) . . ? C23 C22 C13 121.8(2) . . ? C24 C23 C22 120.1(2) . . ? C25 C24 C23 118.1(2) . . ? C26 C25 C24 119.2(2) . . ? N21 C26 C25 123.4(2) . . ? C35 N31 N32 109.34(18) . . ? C35 N31 B1 125.05(19) . . ? N32 N31 B1 123.89(18) . . ? C33 N32 N31 106.22(17) . . ? C33 N32 Eu1 117.11(13) . . ? N31 N32 Eu1 130.72(13) . . ? N32 C33 C34 110.42(19) . . ? N32 C33 C42 119.24(19) . . ? C34 C33 C42 130.3(2) . . ? C35 C34 C33 104.5(2) . . ? N31 C35 C34 109.5(2) . . ? C46 N41 C42 118.00(19) . . ? C46 N41 Eu1 122.87(15) . . ? C42 N41 Eu1 118.52(13) . . ? N41 C42 C43 121.95(19) . . ? N41 C42 C33 116.18(19) . . ? C43 C42 C33 121.9(2) . . ? C42 C43 C44 119.0(2) . . ? C45 C44 C43 119.2(2) . . ? C44 C45 C46 118.6(2) . . ? N41 C46 C45 123.2(2) . . ? C55 N51 N52 110.27(19) . . ? C55 N51 B1 127.9(2) . . ? N52 N51 B1 121.33(18) . . ? C53 N52 N51 105.44(18) . . ? N52 C53 C54 110.8(2) . . ? N52 C53 C62 120.7(2) . . ? C54 C53 C62 128.4(2) . . ? C55 C54 C53 104.9(2) . . ? N51 C55 C54 108.6(2) . . ? C66 N61 C62 116.9(2) . . ? N61 C62 C63 122.8(2) . . ? N61 C62 C53 115.8(2) . . ? C63 C62 C53 121.4(2) . . ? C64 C63 C62 118.8(2) . . ? C63 C64 C65 119.2(3) . . ? C64 C65 C66 118.3(3) . . ? N61 C66 C65 124.0(3) . . ? C72 C71 C76 118.4(2) . . ? C72 C71 C77 119.1(2) . . ? C76 C71 C77 122.4(2) . . ? C73 C72 C71 121.3(3) . . ? C74 C73 C72 119.9(3) . . ? C73 C74 C75 120.1(3) . . ? C74 C75 C76 120.0(3) . . ? C75 C76 C71 120.3(3) . . ? C77 O77 Eu1 138.23(14) . . ? O77 C77 C78 124.0(2) . . ? O77 C77 C71 115.9(2) . . ? C78 C77 C71 120.1(2) . . ? C77 C78 C79 123.5(2) . . ? C79 O79 Eu1 140.05(14) . . ? O79 C79 C78 123.3(2) . . ? O79 C79 C81 115.5(2) . . ? C78 C79 C81 121.2(2) . . ? C82 C81 C86 118.6(2) . . ? C82 C81 C79 123.4(2) . . ? C86 C81 C79 118.0(2) . . ? C83 C82 C81 120.2(2) . . ? C84 C83 C82 120.4(3) . . ? C85 C84 C83 119.7(3) . . ? C84 C85 C86 120.0(3) . . ? C85 C86 C81 121.0(2) . . ? C92 C91 C96 118.1(2) . . ? C92 C91 C97 118.6(2) . . ? C96 C91 C97 123.3(2) . . ? C93 C92 C91 120.7(3) . . ? C94 C93 C92 120.3(3) . . ? C93 C94 C95 119.7(3) . . ? C94 C95 C96 120.7(3) . . ? C95 C96 C91 120.4(3) . . ? C97 O97 Eu1 137.93(14) . . ? O97 C97 C98 124.2(2) . . ? O97 C97 C91 115.9(2) . . ? C98 C97 C91 119.9(2) . . ? C97 C98 C99 122.9(2) . . ? C99 O99 Eu1 138.84(14) . . ? O99 C99 C98 124.4(2) . . ? O99 C99 C101 114.89(19) . . ? C98 C99 C101 120.6(2) . . ? C102 C101 C106 119.4(2) . . ? C102 C101 C99 118.3(2) . . ? C106 C101 C99 122.1(2) . . ? C101 C102 C103 120.2(2) . . ? C104 C103 C102 119.8(3) . . ? C105 C104 C103 120.0(3) . . ? C104 C105 C106 120.4(3) . . ? C105 C106 C101 120.2(3) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.600 _refine_diff_density_min -0.659 _refine_diff_density_rms 0.068 #=END data_sad_b _database_code_depnum_ccdc_archive 'CCDC 229464' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C108 H82 B2 N18 Nd2 O8' _chemical_formula_weight 2070.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' Nd Nd -0.1943 3.0179 '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 11.8548(14) _cell_length_b 12.9275(15) _cell_length_c 15.7597(19) _cell_angle_alpha 86.820(2) _cell_angle_beta 88.945(2) _cell_angle_gamma 72.779(2) _cell_volume 2303.4(5) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.492 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1050 _exptl_absorpt_coefficient_mu 1.186 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8906 _exptl_absorpt_correction_T_max 0.8906 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 24376 _diffrn_reflns_av_R_equivalents 0.0365 _diffrn_reflns_av_sigmaI/netI 0.0599 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 27.49 _reflns_number_total 10483 _reflns_number_gt 7189 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material '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^)+(0.0255P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10483 _refine_ls_number_parameters 625 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0529 _refine_ls_R_factor_gt 0.0281 _refine_ls_wR_factor_ref 0.0620 _refine_ls_wR_factor_gt 0.0572 _refine_ls_goodness_of_fit_ref 0.900 _refine_ls_restrained_S_all 0.900 _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 Nd1 Nd 0.0000 0.5000 0.5000 0.01814(6) Uani 1 2 d S . . B1 B -0.3411(3) 0.6336(2) 0.5227(2) 0.0235(7) Uani 1 1 d . . . H1 H -0.4282 0.6678 0.5283 0.028 Uiso 1 1 calc R . . N11 N 0.27919(19) 0.27796(17) 0.49452(14) 0.0221(5) Uani 1 1 d . . . N12 N 0.16028(19) 0.30279(17) 0.50640(13) 0.0199(5) Uani 1 1 d . . . C13 C 0.1373(2) 0.2082(2) 0.52321(17) 0.0232(6) Uani 1 1 d . . . C14 C 0.2421(3) 0.1215(2) 0.52184(19) 0.0306(7) Uani 1 1 d . . . H14 H 0.2509 0.0464 0.5317 0.037 Uiso 1 1 calc R . . C15 C 0.3285(3) 0.1696(2) 0.50318(18) 0.0292(7) Uani 1 1 d . . . H15 H 0.4102 0.1327 0.4972 0.035 Uiso 1 1 calc R . . N21 N 0.06994(19) 0.69982(17) 0.46722(14) 0.0225(5) Uani 1 1 d . . . C22 C -0.0172(2) 0.7947(2) 0.45749(17) 0.0235(6) Uani 1 1 d . . . C23 C 0.0041(3) 0.8908(2) 0.4287(2) 0.0343(7) Uani 1 1 d . . . H23 H -0.0591 0.9561 0.4231 0.041 Uiso 1 1 calc R . . C24 C 0.1182(3) 0.8904(2) 0.4081(2) 0.0367(8) Uani 1 1 d . . . H24 H 0.1344 0.9551 0.3877 0.044 Uiso 1 1 calc R . . C25 C 0.2073(3) 0.7948(2) 0.41786(18) 0.0314(7) Uani 1 1 d . . . H25 H 0.2865 0.7918 0.4040 0.038 Uiso 1 1 calc R . . C26 C 0.1795(2) 0.7026(2) 0.44833(17) 0.0256(6) Uani 1 1 d . . . H26 H 0.2423 0.6373 0.4563 0.031 Uiso 1 1 calc R . . N31 N -0.31547(18) 0.55691(17) 0.44938(14) 0.0219(5) Uani 1 1 d . . . N32 N -0.20275(18) 0.50086(16) 0.42772(13) 0.0197(5) Uani 1 1 d . . . C33 C -0.2123(2) 0.4451(2) 0.36039(17) 0.0219(6) Uani 1 1 d . . . C34 C -0.3311(2) 0.4647(2) 0.33878(19) 0.0303(7) Uani 1 1 d . . . H34 H -0.3623 0.4354 0.2939 0.036 Uiso 1 1 calc R . . C35 C -0.3925(3) 0.5356(2) 0.39664(18) 0.0297(7) Uani 1 1 d . . . H35 H -0.4760 0.5649 0.3991 0.036 Uiso 1 1 calc R . . N41 N -0.00204(19) 0.36919(16) 0.35744(14) 0.0212(5) Uani 1 1 d . . . C42 C -0.1063(2) 0.3756(2) 0.32055(16) 0.0213(6) Uani 1 1 d . . . C43 C -0.1147(3) 0.3194(2) 0.24944(18) 0.0284(6) Uani 1 1 d . . . H43 H -0.1896 0.3273 0.2248 0.034 Uiso 1 1 calc R . . C44 C -0.0137(3) 0.2520(2) 0.21485(19) 0.0340(7) Uani 1 1 d . . . H44 H -0.0175 0.2122 0.1667 0.041 Uiso 1 1 calc R . . C45 C 0.0932(3) 0.2442(2) 0.25218(18) 0.0289(7) Uani 1 1 d . . . H45 H 0.1645 0.1984 0.2301 0.035 Uiso 1 1 calc R . . C46 C 0.0951(2) 0.3033(2) 0.32152(17) 0.0245(6) Uani 1 1 d . . . H46 H 0.1696 0.2975 0.3458 0.029 Uiso 1 1 calc R . . N51 N 0.29187(19) 0.43142(17) 0.39433(14) 0.0211(5) Uani 1 1 d . . . N52 N 0.17505(19) 0.48801(16) 0.38667(13) 0.0189(5) Uani 1 1 d . . . C53 C 0.1638(2) 0.5388(2) 0.30935(16) 0.0208(6) Uani 1 1 d . . . C54 C 0.2731(2) 0.5152(2) 0.26701(18) 0.0274(6) Uani 1 1 d . . . H54 H 0.2893 0.5405 0.2117 0.033 Uiso 1 1 calc R . . C55 C 0.3511(2) 0.4473(2) 0.32376(18) 0.0270(6) Uani 1 1 d . . . H55 H 0.4335 0.4167 0.3146 0.032 Uiso 1 1 calc R . . N61 N -0.04468(19) 0.61125(16) 0.33200(13) 0.0208(5) Uani 1 1 d . . . C62 C 0.0482(2) 0.6104(2) 0.28106(17) 0.0221(6) Uani 1 1 d . . . C63 C 0.0386(3) 0.6747(2) 0.20670(18) 0.0302(7) Uani 1 1 d . . . H63 H 0.1063 0.6712 0.1725 0.036 Uiso 1 1 calc R . . C64 C -0.0700(3) 0.7437(2) 0.18267(19) 0.0344(7) Uani 1 1 d . . . H64 H -0.0782 0.7898 0.1326 0.041 Uiso 1 1 calc R . . C65 C -0.1666(3) 0.7444(2) 0.23294(18) 0.0282(6) Uani 1 1 d . . . H65 H -0.2430 0.7901 0.2178 0.034 Uiso 1 1 calc R . . C66 C -0.1498(2) 0.6773(2) 0.30556(17) 0.0241(6) Uani 1 1 d . . . H66 H -0.2171 0.6779 0.3393 0.029 Uiso 1 1 calc R . . Nd2 Nd 0.0000 0.0000 0.0000 0.01884(6) Uani 1 2 d S . . C111 C 0.3138(2) 0.1580(2) 0.01011(17) 0.0240(6) Uani 1 1 d . . . C112 C 0.2481(3) 0.2375(2) 0.06263(18) 0.0330(7) Uani 1 1 d . . . H112 H 0.1665 0.2455 0.0712 0.040 Uiso 1 1 calc R . . C113 C 0.2993(3) 0.3046(3) 0.1024(2) 0.0403(8) Uani 1 1 d . . . H113 H 0.2533 0.3587 0.1377 0.048 Uiso 1 1 calc R . . C114 C 0.4187(3) 0.2925(3) 0.0905(2) 0.0395(8) Uani 1 1 d . . . H114 H 0.4547 0.3378 0.1184 0.047 Uiso 1 1 calc R . . C115 C 0.4851(3) 0.2151(2) 0.0385(2) 0.0350(7) Uani 1 1 d . . . H115 H 0.5669 0.2070 0.0306 0.042 Uiso 1 1 calc R . . C116 C 0.4327(2) 0.1486(2) -0.00267(19) 0.0295(7) Uani 1 1 d . . . H116 H 0.4784 0.0965 -0.0397 0.035 Uiso 1 1 calc R . . O117 O 0.15729(16) 0.08243(15) 0.01025(12) 0.0291(5) Uani 1 1 d . . . C117 C 0.2514(2) 0.0857(2) -0.02713(17) 0.0221(6) Uani 1 1 d . . . C118 C 0.2943(2) 0.0301(2) -0.10040(17) 0.0237(6) Uani 1 1 d . . . H118 H 0.3694 0.0313 -0.1218 0.028 Uiso 1 1 calc R . . C121 C -0.2776(2) 0.0767(2) 0.22580(17) 0.0247(6) Uani 1 1 d . . . C122 C -0.1972(3) 0.0945(2) 0.28239(18) 0.0285(6) Uani 1 1 d . . . H122 H -0.1154 0.0726 0.2690 0.034 Uiso 1 1 calc R . . C123 C -0.2350(3) 0.1438(2) 0.35808(19) 0.0321(7) Uani 1 1 d . . . H123 H -0.1792 0.1551 0.3963 0.039 Uiso 1 1 calc R . . C124 C -0.3543(3) 0.1767(2) 0.3778(2) 0.0362(8) Uani 1 1 d . . . H124 H -0.3805 0.2109 0.4294 0.043 Uiso 1 1 calc R . . C125 C -0.4346(3) 0.1597(2) 0.3226(2) 0.0370(8) Uani 1 1 d . . . H125 H -0.5163 0.1823 0.3364 0.044 Uiso 1 1 calc R . . C126 C -0.3976(3) 0.1099(2) 0.24689(19) 0.0323(7) Uani 1 1 d . . . H126 H -0.4540 0.0983 0.2093 0.039 Uiso 1 1 calc R . . O127 O -0.13283(16) 0.03868(15) 0.11912(12) 0.0280(5) Uani 1 1 d . . . C127 C -0.2317(2) 0.0271(2) 0.14355(17) 0.0231(6) Uani 1 1 d . . . C131 C 0.3106(2) -0.1400(2) 0.18900(17) 0.0255(6) Uani 1 1 d . . . C132 C 0.2908(3) -0.0395(3) 0.2218(2) 0.0471(9) Uani 1 1 d . . . H132 H 0.2220 0.0172 0.2053 0.056 Uiso 1 1 calc R . . C133 C 0.3680(3) -0.0194(3) 0.2776(3) 0.0641(12) Uani 1 1 d . . . H133 H 0.3520 0.0506 0.2994 0.077 Uiso 1 1 calc R . . C134 C 0.4686(3) -0.0998(3) 0.3025(2) 0.0502(9) Uani 1 1 d . . . H134 H 0.5229 -0.0852 0.3403 0.060 Uiso 1 1 calc R . . C135 C 0.4896(3) -0.2008(3) 0.2723(2) 0.0410(8) Uani 1 1 d . . . H135 H 0.5579 -0.2572 0.2901 0.049 Uiso 1 1 calc R . . C136 C 0.4115(3) -0.2212(2) 0.2157(2) 0.0364(7) Uani 1 1 d . . . H136 H 0.4271 -0.2917 0.1949 0.044 Uiso 1 1 calc R . . O137 O 0.12487(16) -0.08060(14) 0.12202(12) 0.0272(4) Uani 1 1 d . . . C137 C 0.2230(2) -0.1538(2) 0.12604(17) 0.0230(6) Uani 1 1 d . . . C138 C 0.2541(2) -0.2439(2) 0.07504(17) 0.0237(6) Uani 1 1 d . . . H138 H 0.3309 -0.2936 0.0814 0.028 Uiso 1 1 calc R . . O139 O 0.07813(17) -0.20107(14) -0.00526(12) 0.0274(4) Uani 1 1 d . . . C139 C 0.1781(2) -0.2646(2) 0.01510(17) 0.0235(6) Uani 1 1 d . . . C141 C 0.2158(3) -0.3715(2) -0.02608(18) 0.0257(6) Uani 1 1 d . . . C142 C 0.1311(3) -0.4214(2) -0.0454(2) 0.0359(7) Uani 1 1 d . . . H142 H 0.0507 -0.3885 -0.0311 0.043 Uiso 1 1 calc R . . C143 C 0.1632(3) -0.5191(2) -0.0856(2) 0.0434(8) Uani 1 1 d . . . H143 H 0.1049 -0.5529 -0.0982 0.052 Uiso 1 1 calc R . . C144 C 0.2792(3) -0.5668(2) -0.1072(2) 0.0449(9) Uani 1 1 d . . . H144 H 0.3009 -0.6333 -0.1349 0.054 Uiso 1 1 calc R . . C145 C 0.3640(3) -0.5179(2) -0.0886(2) 0.0417(8) Uani 1 1 d . . . H145 H 0.4439 -0.5506 -0.1040 0.050 Uiso 1 1 calc R . . C146 C 0.3333(3) -0.4216(2) -0.04740(19) 0.0340(7) Uani 1 1 d . . . H146 H 0.3925 -0.3894 -0.0336 0.041 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 Nd1 0.01462(12) 0.01902(11) 0.01938(13) -0.00239(9) 0.00173(9) -0.00268(9) B1 0.0167(15) 0.0265(16) 0.0245(17) -0.0029(13) 0.0014(13) -0.0019(13) N11 0.0191(12) 0.0228(12) 0.0207(12) -0.0007(9) 0.0004(9) -0.0007(10) N12 0.0181(12) 0.0198(11) 0.0198(12) -0.0004(9) 0.0010(9) -0.0029(10) C13 0.0284(16) 0.0217(14) 0.0186(14) -0.0018(11) 0.0018(12) -0.0057(12) C14 0.0311(17) 0.0188(14) 0.0383(19) -0.0001(13) 0.0020(14) -0.0021(13) C15 0.0230(15) 0.0212(14) 0.0358(18) -0.0008(12) 0.0027(13) 0.0051(12) N21 0.0242(13) 0.0216(11) 0.0215(12) -0.0039(9) 0.0010(10) -0.0059(10) C22 0.0271(15) 0.0238(14) 0.0203(14) -0.0058(11) 0.0012(12) -0.0079(12) C23 0.0324(18) 0.0204(14) 0.047(2) 0.0032(13) 0.0008(15) -0.0036(13) C24 0.0409(19) 0.0268(16) 0.046(2) 0.0039(14) 0.0012(16) -0.0167(15) C25 0.0295(17) 0.0369(17) 0.0325(17) -0.0047(13) 0.0058(13) -0.0168(14) C26 0.0251(15) 0.0290(15) 0.0232(15) -0.0053(12) -0.0002(12) -0.0080(13) N31 0.0154(11) 0.0242(12) 0.0239(13) -0.0023(9) 0.0013(9) -0.0022(9) N32 0.0178(12) 0.0204(11) 0.0203(12) -0.0013(9) 0.0000(9) -0.0046(9) C33 0.0235(15) 0.0220(13) 0.0213(15) -0.0006(11) -0.0009(11) -0.0084(12) C34 0.0235(15) 0.0408(17) 0.0295(17) -0.0083(13) -0.0030(13) -0.0125(14) C35 0.0197(15) 0.0351(16) 0.0352(18) -0.0067(13) -0.0016(13) -0.0083(13) N41 0.0221(12) 0.0194(11) 0.0211(12) -0.0026(9) 0.0030(10) -0.0046(10) C42 0.0248(15) 0.0215(13) 0.0182(14) -0.0007(11) 0.0004(11) -0.0075(12) C43 0.0305(17) 0.0307(16) 0.0267(16) -0.0050(13) 0.0002(13) -0.0125(14) C44 0.0424(19) 0.0364(17) 0.0261(16) -0.0138(13) 0.0035(14) -0.0142(15) C45 0.0310(17) 0.0255(15) 0.0274(16) -0.0048(13) 0.0047(13) -0.0035(13) C46 0.0233(15) 0.0231(14) 0.0253(15) -0.0023(12) 0.0025(12) -0.0042(12) N51 0.0165(12) 0.0232(12) 0.0223(12) -0.0027(10) 0.0034(10) -0.0040(10) N52 0.0175(12) 0.0186(11) 0.0200(12) -0.0019(9) 0.0026(10) -0.0044(10) C53 0.0237(14) 0.0196(13) 0.0205(14) -0.0035(11) 0.0047(11) -0.0083(12) C54 0.0249(15) 0.0313(16) 0.0248(16) 0.0011(12) 0.0069(12) -0.0071(13) C55 0.0190(14) 0.0322(16) 0.0306(17) -0.0051(13) 0.0086(12) -0.0086(13) N61 0.0202(12) 0.0211(11) 0.0203(12) -0.0011(9) 0.0024(9) -0.0052(10) C62 0.0252(15) 0.0222(13) 0.0209(14) -0.0022(11) 0.0008(12) -0.0100(12) C63 0.0271(16) 0.0372(17) 0.0261(16) 0.0088(13) 0.0034(13) -0.0110(14) C64 0.0368(18) 0.0370(17) 0.0272(17) 0.0119(13) -0.0019(14) -0.0101(15) C65 0.0254(16) 0.0264(15) 0.0311(17) 0.0045(12) -0.0064(13) -0.0056(13) C66 0.0227(15) 0.0252(14) 0.0242(15) -0.0019(12) 0.0012(12) -0.0067(12) Nd2 0.01525(12) 0.02286(12) 0.01795(12) -0.00384(9) 0.00154(9) -0.00452(10) C111 0.0245(15) 0.0234(14) 0.0232(15) 0.0040(11) 0.0004(12) -0.0067(12) C112 0.0283(17) 0.0442(18) 0.0309(17) -0.0089(14) 0.0063(13) -0.0164(14) C113 0.044(2) 0.048(2) 0.0360(19) -0.0157(15) 0.0125(16) -0.0225(17) C114 0.047(2) 0.047(2) 0.0343(19) -0.0016(15) -0.0003(16) -0.0289(17) C115 0.0243(16) 0.0362(17) 0.047(2) 0.0081(15) -0.0018(14) -0.0150(14) C116 0.0244(15) 0.0262(15) 0.0361(18) 0.0051(13) -0.0001(13) -0.0061(13) O117 0.0224(11) 0.0403(12) 0.0280(11) -0.0088(9) 0.0079(9) -0.0135(9) C117 0.0179(14) 0.0222(14) 0.0242(15) 0.0052(11) -0.0024(11) -0.0038(11) C118 0.0169(14) 0.0244(14) 0.0269(16) 0.0017(12) 0.0054(12) -0.0026(11) C121 0.0260(15) 0.0219(14) 0.0235(15) -0.0016(11) 0.0062(12) -0.0031(12) C122 0.0261(16) 0.0274(15) 0.0293(16) -0.0024(12) 0.0059(13) -0.0041(13) C123 0.0385(18) 0.0296(16) 0.0272(17) -0.0059(13) 0.0032(14) -0.0078(14) C124 0.041(2) 0.0313(17) 0.0315(18) -0.0053(14) 0.0143(16) -0.0036(15) C125 0.0279(17) 0.0381(18) 0.0373(19) -0.0042(14) 0.0127(14) 0.0019(14) C126 0.0260(16) 0.0359(17) 0.0318(17) -0.0047(13) 0.0054(13) -0.0040(14) O127 0.0219(11) 0.0396(12) 0.0243(11) -0.0078(9) 0.0067(9) -0.0111(9) C127 0.0205(15) 0.0239(14) 0.0196(15) 0.0028(11) 0.0020(12) 0.0007(12) C131 0.0238(15) 0.0318(15) 0.0218(15) -0.0001(12) -0.0018(12) -0.0100(13) C132 0.042(2) 0.0319(17) 0.064(2) -0.0048(17) -0.0271(18) -0.0035(16) C133 0.064(3) 0.042(2) 0.088(3) -0.014(2) -0.039(2) -0.013(2) C134 0.050(2) 0.061(2) 0.047(2) 0.0014(18) -0.0242(18) -0.0260(19) C135 0.0278(18) 0.050(2) 0.042(2) 0.0077(16) -0.0110(15) -0.0075(16) C136 0.0307(18) 0.0362(17) 0.0382(19) -0.0019(14) -0.0049(15) -0.0032(14) O137 0.0257(11) 0.0268(10) 0.0245(11) -0.0043(8) -0.0043(9) 0.0000(9) C137 0.0237(15) 0.0259(14) 0.0201(14) 0.0021(11) 0.0025(12) -0.0090(12) C138 0.0190(14) 0.0234(14) 0.0264(15) -0.0009(12) 0.0003(12) -0.0026(12) O139 0.0274(11) 0.0247(10) 0.0290(11) -0.0052(8) -0.0056(9) -0.0052(9) C139 0.0265(16) 0.0214(15) 0.0219(15) 0.0016(12) 0.0044(12) -0.0067(13) C141 0.0320(17) 0.0200(14) 0.0217(15) 0.0004(11) -0.0016(13) -0.0027(12) C142 0.0363(18) 0.0292(16) 0.042(2) -0.0035(14) -0.0021(15) -0.0094(14) C143 0.053(2) 0.0338(18) 0.047(2) -0.0064(15) -0.0116(17) -0.0172(17) C144 0.062(3) 0.0256(16) 0.041(2) -0.0090(14) -0.0097(18) -0.0015(17) C145 0.040(2) 0.0350(18) 0.042(2) -0.0111(15) 0.0024(16) 0.0031(15) C146 0.0351(18) 0.0291(16) 0.0368(18) -0.0072(13) 0.0033(14) -0.0071(14) _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 Nd1 N32 2.676(2) . ? Nd1 N32 2.676(2) 2_566 ? Nd1 N52 2.688(2) . ? Nd1 N52 2.688(2) 2_566 ? Nd1 N12 2.689(2) 2_566 ? Nd1 N12 2.689(2) . ? Nd1 N41 2.891(2) . ? Nd1 N41 2.891(2) 2_566 ? Nd1 N61 2.922(2) 2_566 ? Nd1 N61 2.922(2) . ? Nd1 N21 2.955(2) . ? Nd1 N21 2.955(2) 2_566 ? B1 N31 1.532(4) . ? B1 N51 1.540(4) 2_566 ? B1 N11 1.541(4) 2_566 ? N11 C15 1.349(3) . ? N11 N12 1.362(3) . ? N11 B1 1.541(4) 2_566 ? N12 C13 1.341(3) . ? C13 C14 1.406(4) . ? C13 C22 1.462(4) 2_566 ? C14 C15 1.366(4) . ? N21 C26 1.338(3) . ? N21 C22 1.353(3) . ? C22 C23 1.389(4) . ? C22 C13 1.462(4) 2_566 ? C23 C24 1.384(4) . ? C24 C25 1.370(4) . ? C25 C26 1.387(4) . ? N31 C35 1.343(3) . ? N31 N32 1.365(3) . ? N32 C33 1.340(3) . ? C33 C34 1.401(4) . ? C33 C42 1.465(4) . ? C34 C35 1.369(4) . ? N41 C46 1.349(3) . ? N41 C42 1.354(3) . ? C42 C43 1.390(4) . ? C43 C44 1.379(4) . ? C44 C45 1.380(4) . ? C45 C46 1.372(4) . ? N51 C55 1.343(3) . ? N51 N52 1.365(3) . ? N51 B1 1.540(4) 2_566 ? N52 C53 1.341(3) . ? C53 C54 1.404(4) . ? C53 C62 1.469(4) . ? C54 C55 1.374(4) . ? N61 C66 1.343(3) . ? N61 C62 1.349(3) . ? C62 C63 1.385(3) . ? C63 C64 1.378(4) . ? C64 C65 1.378(4) . ? C65 C66 1.377(4) . ? Nd2 O127 2.4047(18) 2 ? Nd2 O127 2.4048(18) . ? Nd2 O117 2.4177(18) 2 ? Nd2 O117 2.4177(18) . ? Nd2 O137 2.4381(18) 2 ? Nd2 O137 2.4381(18) . ? Nd2 O139 2.4934(18) 2 ? Nd2 O139 2.4934(18) . ? C111 C116 1.391(4) . ? C111 C112 1.394(4) . ? C111 C117 1.500(4) . ? C112 C113 1.379(4) . ? C113 C114 1.387(4) . ? C114 C115 1.377(4) . ? C115 C116 1.392(4) . ? O117 C117 1.262(3) . ? C117 C118 1.401(4) . ? C118 C127 1.400(4) 2 ? C121 C122 1.393(4) . ? C121 C126 1.399(4) . ? C121 C127 1.499(4) . ? C122 C123 1.387(4) . ? C123 C124 1.386(4) . ? C124 C125 1.373(4) . ? C125 C126 1.389(4) . ? O127 C127 1.274(3) . ? C127 C118 1.400(4) 2 ? C131 C132 1.379(4) . ? C131 C136 1.391(4) . ? C131 C137 1.504(4) . ? C132 C133 1.370(4) . ? C133 C134 1.376(5) . ? C134 C135 1.365(5) . ? C135 C136 1.387(4) . ? O137 C137 1.264(3) . ? C137 C138 1.406(4) . ? C138 C139 1.407(4) . ? O139 C139 1.261(3) . ? C139 C141 1.501(4) . ? C141 C142 1.390(4) . ? C141 C146 1.395(4) . ? C142 C143 1.392(4) . ? C143 C144 1.375(5) . ? C144 C145 1.380(5) . ? C145 C146 1.385(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N32 Nd1 N32 180.0 . 2_566 ? N32 Nd1 N52 112.86(6) . . ? N32 Nd1 N52 67.14(6) 2_566 . ? N32 Nd1 N52 67.14(6) . 2_566 ? N32 Nd1 N52 112.86(6) 2_566 2_566 ? N52 Nd1 N52 179.999(1) . 2_566 ? N32 Nd1 N12 67.33(6) . 2_566 ? N32 Nd1 N12 112.67(6) 2_566 2_566 ? N52 Nd1 N12 111.92(6) . 2_566 ? N52 Nd1 N12 68.08(6) 2_566 2_566 ? N32 Nd1 N12 112.67(6) . . ? N32 Nd1 N12 67.33(6) 2_566 . ? N52 Nd1 N12 68.08(6) . . ? N52 Nd1 N12 111.92(6) 2_566 . ? N12 Nd1 N12 180.00(9) 2_566 . ? N32 Nd1 N41 58.79(6) . . ? N32 Nd1 N41 121.21(6) 2_566 . ? N52 Nd1 N41 64.96(6) . . ? N52 Nd1 N41 115.04(6) 2_566 . ? N12 Nd1 N41 115.41(6) 2_566 . ? N12 Nd1 N41 64.59(6) . . ? N32 Nd1 N41 121.21(6) . 2_566 ? N32 Nd1 N41 58.79(6) 2_566 2_566 ? N52 Nd1 N41 115.04(6) . 2_566 ? N52 Nd1 N41 64.96(6) 2_566 2_566 ? N12 Nd1 N41 64.59(6) 2_566 2_566 ? N12 Nd1 N41 115.41(6) . 2_566 ? N41 Nd1 N41 180.0 . 2_566 ? N32 Nd1 N61 115.10(6) . 2_566 ? N32 Nd1 N61 64.90(6) 2_566 2_566 ? N52 Nd1 N61 121.57(6) . 2_566 ? N52 Nd1 N61 58.43(6) 2_566 2_566 ? N12 Nd1 N61 115.99(6) 2_566 2_566 ? N12 Nd1 N61 64.01(6) . 2_566 ? N41 Nd1 N61 117.32(6) . 2_566 ? N41 Nd1 N61 62.68(6) 2_566 2_566 ? N32 Nd1 N61 64.90(6) . . ? N32 Nd1 N61 115.10(6) 2_566 . ? N52 Nd1 N61 58.43(6) . . ? N52 Nd1 N61 121.57(6) 2_566 . ? N12 Nd1 N61 64.01(6) 2_566 . ? N12 Nd1 N61 115.99(6) . . ? N41 Nd1 N61 62.68(6) . . ? N41 Nd1 N61 117.32(6) 2_566 . ? N61 Nd1 N61 180.0 2_566 . ? N32 Nd1 N21 115.22(6) . . ? N32 Nd1 N21 64.78(6) 2_566 . ? N52 Nd1 N21 63.91(6) . . ? N52 Nd1 N21 116.10(6) 2_566 . ? N12 Nd1 N21 58.39(6) 2_566 . ? N12 Nd1 N21 121.61(6) . . ? N41 Nd1 N21 117.69(6) . . ? N41 Nd1 N21 62.31(6) 2_566 . ? N61 Nd1 N21 118.62(6) 2_566 . ? N61 Nd1 N21 61.38(6) . . ? N32 Nd1 N21 64.78(6) . 2_566 ? N32 Nd1 N21 115.22(6) 2_566 2_566 ? N52 Nd1 N21 116.10(6) . 2_566 ? N52 Nd1 N21 63.90(6) 2_566 2_566 ? N12 Nd1 N21 121.61(6) 2_566 2_566 ? N12 Nd1 N21 58.39(6) . 2_566 ? N41 Nd1 N21 62.31(6) . 2_566 ? N41 Nd1 N21 117.69(6) 2_566 2_566 ? N61 Nd1 N21 61.38(6) 2_566 2_566 ? N61 Nd1 N21 118.62(6) . 2_566 ? N21 Nd1 N21 180.0 . 2_566 ? N31 B1 N51 109.1(2) . 2_566 ? N31 B1 N11 109.4(2) . 2_566 ? N51 B1 N11 108.7(2) 2_566 2_566 ? C15 N11 N12 109.8(2) . . ? C15 N11 B1 128.3(2) . 2_566 ? N12 N11 B1 121.9(2) . 2_566 ? C13 N12 N11 106.2(2) . . ? C13 N12 Nd1 125.81(17) . . ? N11 N12 Nd1 128.00(15) . . ? N12 C13 C14 110.4(2) . . ? N12 C13 C22 120.8(2) . 2_566 ? C14 C13 C22 128.8(2) . 2_566 ? C15 C14 C13 104.5(2) . . ? N11 C15 C14 109.1(3) . . ? C26 N21 C22 116.5(2) . . ? C26 N21 Nd1 124.98(17) . . ? C22 N21 Nd1 117.65(16) . . ? N21 C22 C23 122.6(3) . . ? N21 C22 C13 116.8(2) . 2_566 ? C23 C22 C13 120.6(2) . 2_566 ? C24 C23 C22 119.4(3) . . ? C25 C24 C23 118.6(3) . . ? C24 C25 C26 118.6(3) . . ? N21 C26 C25 124.2(3) . . ? C35 N31 N32 110.0(2) . . ? C35 N31 B1 128.4(2) . . ? N32 N31 B1 121.6(2) . . ? C33 N32 N31 106.0(2) . . ? C33 N32 Nd1 125.43(17) . . ? N31 N32 Nd1 128.58(15) . . ? N32 C33 C34 110.5(2) . . ? N32 C33 C42 120.3(2) . . ? C34 C33 C42 129.3(3) . . ? C35 C34 C33 104.7(3) . . ? N31 C35 C34 108.9(2) . . ? C46 N41 C42 115.9(2) . . ? C46 N41 Nd1 124.80(17) . . ? C42 N41 Nd1 119.21(17) . . ? N41 C42 C43 122.9(3) . . ? N41 C42 C33 116.2(2) . . ? C43 C42 C33 120.9(2) . . ? C44 C43 C42 119.5(3) . . ? C43 C44 C45 118.1(3) . . ? C46 C45 C44 119.2(3) . . ? N41 C46 C45 124.2(3) . . ? C55 N51 N52 110.4(2) . . ? C55 N51 B1 128.4(2) . 2_566 ? N52 N51 B1 121.1(2) . 2_566 ? C53 N52 N51 105.6(2) . . ? C53 N52 Nd1 125.85(17) . . ? N51 N52 Nd1 128.59(15) . . ? N52 C53 C54 111.0(2) . . ? N52 C53 C62 119.9(2) . . ? C54 C53 C62 129.1(2) . . ? C55 C54 C53 104.3(2) . . ? N51 C55 C54 108.8(2) . . ? C66 N61 C62 115.9(2) . . ? C66 N61 Nd1 124.69(17) . . ? C62 N61 Nd1 118.63(16) . . ? N61 C62 C63 123.0(3) . . ? N61 C62 C53 116.5(2) . . ? C63 C62 C53 120.4(2) . . ? C64 C63 C62 119.5(3) . . ? C63 C64 C65 118.4(3) . . ? C66 C65 C64 118.5(3) . . ? N61 C66 C65 124.5(3) . . ? O127 Nd2 O127 180.0 2 . ? O127 Nd2 O117 111.66(6) 2 2 ? O127 Nd2 O117 68.34(6) . 2 ? O127 Nd2 O117 68.34(6) 2 . ? O127 Nd2 O117 111.66(6) . . ? O117 Nd2 O117 180.0 2 . ? O127 Nd2 O137 76.15(6) 2 2 ? O127 Nd2 O137 103.85(6) . 2 ? O117 Nd2 O137 69.88(6) 2 2 ? O117 Nd2 O137 110.12(6) . 2 ? O127 Nd2 O137 103.85(6) 2 . ? O127 Nd2 O137 76.15(6) . . ? O117 Nd2 O137 110.12(6) 2 . ? O117 Nd2 O137 69.88(6) . . ? O137 Nd2 O137 180.0 2 . ? O127 Nd2 O139 107.50(6) 2 2 ? O127 Nd2 O139 72.50(6) . 2 ? O117 Nd2 O139 111.68(6) 2 2 ? O117 Nd2 O139 68.32(6) . 2 ? O137 Nd2 O139 68.25(6) 2 2 ? O137 Nd2 O139 111.75(6) . 2 ? O127 Nd2 O139 72.50(6) 2 . ? O127 Nd2 O139 107.50(6) . . ? O117 Nd2 O139 68.32(6) 2 . ? O117 Nd2 O139 111.68(6) . . ? O137 Nd2 O139 111.75(6) 2 . ? O137 Nd2 O139 68.25(6) . . ? O139 Nd2 O139 180.0 2 . ? C116 C111 C112 118.5(3) . . ? C116 C111 C117 124.2(3) . . ? C112 C111 C117 117.3(2) . . ? C113 C112 C111 121.3(3) . . ? C112 C113 C114 119.5(3) . . ? C115 C114 C113 120.3(3) . . ? C114 C115 C116 120.1(3) . . ? C111 C116 C115 120.4(3) . . ? C117 O117 Nd2 140.44(18) . . ? O117 C117 C118 123.6(2) . . ? O117 C117 C111 115.4(2) . . ? C118 C117 C111 121.0(2) . . ? C127 C118 C117 123.0(2) 2 . ? C122 C121 C126 118.5(3) . . ? C122 C121 C127 118.3(2) . . ? C126 C121 C127 123.2(3) . . ? C123 C122 C121 120.9(3) . . ? C124 C123 C122 119.8(3) . . ? C125 C124 C123 119.9(3) . . ? C124 C125 C126 120.7(3) . . ? C125 C126 C121 120.2(3) . . ? C127 O127 Nd2 139.57(18) . . ? O127 C127 C118 124.4(3) . 2 ? O127 C127 C121 115.2(2) . . ? C118 C127 C121 120.4(2) 2 . ? C132 C131 C136 117.5(3) . . ? C132 C131 C137 117.9(3) . . ? C136 C131 C137 124.6(3) . . ? C133 C132 C131 121.5(3) . . ? C132 C133 C134 120.5(3) . . ? C135 C134 C133 119.3(3) . . ? C134 C135 C136 120.2(3) . . ? C135 C136 C131 120.9(3) . . ? C137 O137 Nd2 130.34(17) . . ? O137 C137 C138 124.1(3) . . ? O137 C137 C131 116.4(2) . . ? C138 C137 C131 119.5(2) . . ? C137 C138 C139 123.8(3) . . ? C139 O139 Nd2 130.21(17) . . ? O139 C139 C138 124.8(3) . . ? O139 C139 C141 116.9(2) . . ? C138 C139 C141 118.3(2) . . ? C142 C141 C146 118.7(3) . . ? C142 C141 C139 119.3(3) . . ? C146 C141 C139 121.9(3) . . ? C141 C142 C143 120.5(3) . . ? C144 C143 C142 120.2(3) . . ? C143 C144 C145 119.8(3) . . ? C144 C145 C146 120.5(3) . . ? C145 C146 C141 120.3(3) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.492 _refine_diff_density_min -0.504 _refine_diff_density_rms 0.074 #=END data_donald _database_code_depnum_ccdc_archive 'CCDC 229465' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46.25 H36.50 B Cl0.50 N6 Nd O4' _chemical_formula_sum 'C46.25 H36.50 B Cl0.50 N6 Nd O4' _chemical_formula_weight 913.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' O O 0.0106 0.0060 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.194(4) _cell_length_b 26.548(5) _cell_length_c 17.996(4) _cell_angle_alpha 90.00 _cell_angle_beta 117.64(3) _cell_angle_gamma 90.00 _cell_volume 8123(3) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3134 _cell_measurement_theta_min 5.111 _cell_measurement_theta_max 50.407 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.493 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3692 _exptl_absorpt_coefficient_mu 1.364 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.686942 _exptl_absorpt_correction_T_max 0.760725 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'CCD Area detector' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35906 _diffrn_reflns_av_R_equivalents 0.0656 _diffrn_reflns_av_sigmaI/netI 0.1116 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 27.49 _reflns_number_total 18149 _reflns_number_gt 11900 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART APEX' _computing_cell_refinement SAINT _computing_data_reduction SHELXS _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXS _computing_publication_material SHELXS/XCIF _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^)+(0.0309P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18149 _refine_ls_number_parameters 1075 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0951 _refine_ls_R_factor_gt 0.0533 _refine_ls_wR_factor_ref 0.1055 _refine_ls_wR_factor_gt 0.0914 _refine_ls_goodness_of_fit_ref 0.947 _refine_ls_restrained_S_all 0.947 _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 Nd1 Nd 0.004882(16) 0.489665(10) 0.282291(18) 0.01587(7) Uani 1 1 d . . . B1 B 0.0325(4) 0.6410(2) 0.3212(5) 0.0262(15) Uani 1 1 d . . . C101 C 0.1454(3) 0.34594(19) 0.4363(3) 0.0195(12) Uani 1 1 d . . . C102 C 0.0762(3) 0.31821(19) 0.4114(4) 0.0257(13) Uani 1 1 d . . . H102 H 0.0287 0.3317 0.3718 0.031 Uiso 1 1 calc R . . C103 C 0.0773(4) 0.2708(2) 0.4448(4) 0.0312(14) Uani 1 1 d . . . H103 H 0.0307 0.2529 0.4279 0.037 Uiso 1 1 calc R . . C104 C 0.1479(4) 0.2503(2) 0.5033(4) 0.0331(15) Uani 1 1 d . . . H104 H 0.1487 0.2189 0.5266 0.040 Uiso 1 1 calc R . . C105 C 0.2168(4) 0.2764(2) 0.5270(4) 0.0327(15) Uani 1 1 d . . . H105 H 0.2644 0.2620 0.5644 0.039 Uiso 1 1 calc R . . C106 C 0.2157(3) 0.3243(2) 0.4952(4) 0.0259(13) Uani 1 1 d . . . H106 H 0.2625 0.3422 0.5135 0.031 Uiso 1 1 calc R . . O111 O 0.07053(19) 0.41316(13) 0.3495(2) 0.0218(8) Uani 1 1 d . . . C112 C 0.1390(3) 0.39857(19) 0.4023(3) 0.0196(12) Uani 1 1 d . . . C113 C 0.2060(3) 0.42932(19) 0.4304(4) 0.0222(12) Uani 1 1 d . . . H113 H 0.2547 0.4149 0.4643 0.027 Uiso 1 1 calc R . . C114 C 0.2037(3) 0.4806(2) 0.4102(3) 0.0191(12) Uani 1 1 d . . . O115 O 0.14040(19) 0.50371(13) 0.3662(2) 0.0213(8) Uani 1 1 d . . . C121 C 0.2772(3) 0.51174(19) 0.4440(3) 0.0177(11) Uani 1 1 d . . . C122 C 0.2700(3) 0.5633(2) 0.4232(4) 0.0240(13) Uani 1 1 d . . . H122 H 0.2206 0.5773 0.3905 0.029 Uiso 1 1 calc R . . C123 C 0.3364(3) 0.5931(2) 0.4514(4) 0.0299(14) Uani 1 1 d . . . H123 H 0.3313 0.6271 0.4377 0.036 Uiso 1 1 calc R . . C124 C 0.4096(3) 0.5732(2) 0.4994(4) 0.0335(15) Uani 1 1 d . . . H124 H 0.4539 0.5937 0.5180 0.040 Uiso 1 1 calc R . . C125 C 0.4178(3) 0.5228(2) 0.5200(4) 0.0345(15) Uani 1 1 d . . . H125 H 0.4675 0.5091 0.5525 0.041 Uiso 1 1 calc R . . C126 C 0.3521(3) 0.4930(2) 0.4923(4) 0.0268(13) Uani 1 1 d . . . H126 H 0.3581 0.4590 0.5065 0.032 Uiso 1 1 calc R . . C131 C -0.2230(3) 0.54938(19) 0.0550(3) 0.0195(12) Uani 1 1 d . . . C132 C -0.2002(3) 0.5984(2) 0.0837(4) 0.0279(13) Uani 1 1 d . . . H132 H -0.1555 0.6037 0.1346 0.033 Uiso 1 1 calc R . . C133 C -0.2433(3) 0.6392(2) 0.0374(4) 0.0336(15) Uani 1 1 d . . . H133 H -0.2267 0.6718 0.0563 0.040 Uiso 1 1 calc R . . C134 C -0.3110(3) 0.6315(2) -0.0367(4) 0.0303(14) Uani 1 1 d . . . H134 H -0.3406 0.6589 -0.0674 0.036 Uiso 1 1 calc R . . C135 C -0.3347(3) 0.5830(2) -0.0655(4) 0.0329(15) Uani 1 1 d . . . H135 H -0.3803 0.5777 -0.1156 0.039 Uiso 1 1 calc R . . C136 C -0.2906(3) 0.5424(2) -0.0197(4) 0.0254(13) Uani 1 1 d . . . H136 H -0.3066 0.5099 -0.0396 0.030 Uiso 1 1 calc R . . O141 O -0.1201(2) 0.51910(13) 0.1811(2) 0.0223(8) Uani 1 1 d . . . C142 C -0.1700(3) 0.50734(19) 0.1070(3) 0.0176(11) Uani 1 1 d . . . C143 C -0.1745(3) 0.45940(18) 0.0716(3) 0.0190(11) Uani 1 1 d . . . H143 H -0.2129 0.4539 0.0167 0.023 Uiso 1 1 calc R . . C144 C -0.1240(3) 0.41952(19) 0.1148(3) 0.0161(11) Uani 1 1 d . . . O145 O -0.0707(2) 0.42132(13) 0.1915(2) 0.0206(8) Uani 1 1 d . . . C151 C -0.1261(3) 0.37104(19) 0.0698(3) 0.0213(12) Uani 1 1 d . . . C152 C -0.0675(3) 0.33530(19) 0.1117(4) 0.0228(12) Uani 1 1 d . . . H152 H -0.0297 0.3417 0.1666 0.027 Uiso 1 1 calc R . . C153 C -0.0640(4) 0.2902(2) 0.0738(4) 0.0316(14) Uani 1 1 d . . . H153 H -0.0237 0.2672 0.1021 0.038 Uiso 1 1 calc R . . C154 C -0.1215(4) 0.2804(2) -0.0065(4) 0.0349(15) Uani 1 1 d . . . H154 H -0.1206 0.2504 -0.0327 0.042 Uiso 1 1 calc R . . C155 C -0.1803(4) 0.3149(2) -0.0481(4) 0.0314(14) Uani 1 1 d . . . H155 H -0.2192 0.3076 -0.1020 0.038 Uiso 1 1 calc R . . C156 C -0.1831(3) 0.3602(2) -0.0115(4) 0.0257(13) Uani 1 1 d . . . H156 H -0.2228 0.3833 -0.0412 0.031 Uiso 1 1 calc R . . N161 N -0.0259(3) 0.61404(15) 0.3442(3) 0.0216(10) Uani 1 1 d . . . N162 N -0.0269(2) 0.56321(15) 0.3547(3) 0.0186(10) Uani 1 1 d . . . C163 C -0.0760(3) 0.5547(2) 0.3873(3) 0.0205(12) Uani 1 1 d . . . C164 C -0.1072(3) 0.5998(2) 0.3987(4) 0.0256(13) Uani 1 1 d . . . H164 H -0.1427 0.6043 0.4200 0.031 Uiso 1 1 calc R . . C165 C -0.0733(3) 0.6361(2) 0.3713(4) 0.0259(13) Uani 1 1 d . . . H165 H -0.0818 0.6705 0.3715 0.031 Uiso 1 1 calc R . . N171 N -0.0627(2) 0.46601(16) 0.3741(3) 0.0225(10) Uani 1 1 d . . . C172 C -0.0906(3) 0.50298(19) 0.4049(3) 0.0187(11) Uani 1 1 d . . . C173 C -0.1281(3) 0.4921(2) 0.4532(3) 0.0250(12) Uani 1 1 d . . . H173 H -0.1469 0.5180 0.4738 0.030 Uiso 1 1 calc R . . C174 C -0.1371(3) 0.4428(2) 0.4701(4) 0.0262(13) Uani 1 1 d . . . H174 H -0.1619 0.4351 0.5025 0.031 Uiso 1 1 calc R . . C175 C -0.1094(3) 0.4047(2) 0.4389(3) 0.0238(12) Uani 1 1 d . . . H175 H -0.1152 0.3710 0.4492 0.029 Uiso 1 1 calc R . . C176 C -0.0724(3) 0.4185(2) 0.3914(4) 0.0245(13) Uani 1 1 d . . . H176 H -0.0532 0.3930 0.3705 0.029 Uiso 1 1 calc R . . N181 N 0.0274(3) 0.62124(15) 0.2379(3) 0.0241(11) Uani 1 1 d . . . N182 N 0.0371(2) 0.57178(15) 0.2249(3) 0.0192(10) Uani 1 1 d . . . C183 C 0.0507(3) 0.5698(2) 0.1585(3) 0.0209(12) Uani 1 1 d . . . C184 C 0.0489(3) 0.6182(2) 0.1269(4) 0.0288(14) Uani 1 1 d . . . H184 H 0.0563 0.6274 0.0812 0.035 Uiso 1 1 calc R . . C185 C 0.0336(3) 0.6488(2) 0.1786(4) 0.0286(14) Uani 1 1 d . . . H185 H 0.0283 0.6836 0.1735 0.034 Uiso 1 1 calc R . . N191 N 0.0520(2) 0.47975(16) 0.1663(3) 0.0196(10) Uani 1 1 d . . . C192 C 0.0656(3) 0.52085(19) 0.1306(3) 0.0200(12) Uani 1 1 d . . . C193 C 0.0921(3) 0.5163(2) 0.0710(4) 0.0269(13) Uani 1 1 d . . . H193 H 0.1019 0.5449 0.0475 0.032 Uiso 1 1 calc R . . C194 C 0.1037(3) 0.4689(2) 0.0469(4) 0.0282(14) Uani 1 1 d . . . H194 H 0.1205 0.4652 0.0064 0.034 Uiso 1 1 calc R . . C195 C 0.0900(3) 0.4271(2) 0.0839(4) 0.0273(13) Uani 1 1 d . . . H195 H 0.0977 0.3948 0.0690 0.033 Uiso 1 1 calc R . . C196 C 0.0646(3) 0.4343(2) 0.1436(4) 0.0236(13) Uani 1 1 d . . . H196 H 0.0559 0.4062 0.1689 0.028 Uiso 1 1 calc R . . Nd2 Nd 0.492697(16) 0.196699(10) 0.231089(19) 0.01560(7) Uani 1 1 d . . . B2 B 0.5101(4) 0.3456(2) 0.2580(5) 0.0287(16) Uani 1 1 d . . . C201 C 0.3326(3) 0.06102(19) 0.2305(4) 0.0207(12) Uani 1 1 d . . . C202 C 0.3619(3) 0.02734(19) 0.1927(4) 0.0238(13) Uani 1 1 d . . . H202 H 0.3908 0.0394 0.1669 0.029 Uiso 1 1 calc R . . C203 C 0.3487(3) -0.0238(2) 0.1931(4) 0.0295(14) Uani 1 1 d . . . H203 H 0.3685 -0.0459 0.1674 0.035 Uiso 1 1 calc R . . C204 C 0.3057(3) -0.0423(2) 0.2319(4) 0.0298(15) Uani 1 1 d . . . H204 H 0.2971 -0.0767 0.2330 0.036 Uiso 1 1 calc R . . C205 C 0.2760(3) -0.0090(2) 0.2686(4) 0.0275(13) Uani 1 1 d . . . H205 H 0.2471 -0.0212 0.2944 0.033 Uiso 1 1 calc R . . C206 C 0.2884(3) 0.0421(2) 0.2680(4) 0.0247(13) Uani 1 1 d . . . H206 H 0.2674 0.0641 0.2926 0.030 Uiso 1 1 calc R . . O211 O 0.4109(2) 0.12598(12) 0.2183(2) 0.0221(9) Uani 1 1 d . . . C212 C 0.3521(3) 0.11584(19) 0.2312(3) 0.0198(12) Uani 1 1 d . . . C213 C 0.3052(3) 0.15250(18) 0.2424(4) 0.0220(12) Uani 1 1 d . . . H213 H 0.2627 0.1418 0.2498 0.026 Uiso 1 1 calc R . . C214 C 0.3187(3) 0.20391(19) 0.2429(3) 0.0195(12) Uani 1 1 d . . . O215 O 0.3772(2) 0.22334(12) 0.2374(2) 0.0211(8) Uani 1 1 d . . . C221 C 0.2608(3) 0.24038(18) 0.2474(3) 0.0197(12) Uani 1 1 d . . . C222 C 0.2603(3) 0.28986(19) 0.2210(4) 0.0236(12) Uani 1 1 d . . . H222 H 0.2943 0.2992 0.1998 0.028 Uiso 1 1 calc R . . C223 C 0.2095(3) 0.3252(2) 0.2259(4) 0.0262(13) Uani 1 1 d . . . H223 H 0.2096 0.3581 0.2084 0.031 Uiso 1 1 calc R . . C224 C 0.1588(3) 0.3111(2) 0.2571(4) 0.0294(14) Uani 1 1 d . . . H224 H 0.1243 0.3347 0.2601 0.035 Uiso 1 1 calc R . . C225 C 0.1589(4) 0.2620(2) 0.2841(4) 0.0328(15) Uani 1 1 d . . . H225 H 0.1251 0.2529 0.3056 0.039 Uiso 1 1 calc R . . C226 C 0.2098(3) 0.2269(2) 0.2789(4) 0.0263(13) Uani 1 1 d . . . H226 H 0.2097 0.1940 0.2965 0.032 Uiso 1 1 calc R . . C231 C 0.6438(3) 0.05460(19) 0.2380(3) 0.0188(11) Uani 1 1 d . . . C232 C 0.5827(3) 0.0226(2) 0.2289(4) 0.0260(13) Uani 1 1 d . . . H232 H 0.5353 0.0360 0.2219 0.031 Uiso 1 1 calc R . . C233 C 0.5924(3) -0.0293(2) 0.2302(4) 0.0281(14) Uani 1 1 d . . . H233 H 0.5515 -0.0504 0.2243 0.034 Uiso 1 1 calc R . . C234 C 0.6623(3) -0.0498(2) 0.2400(4) 0.0258(13) Uani 1 1 d . . . H234 H 0.6683 -0.0846 0.2405 0.031 Uiso 1 1 calc R . . C235 C 0.7228(3) -0.0187(2) 0.2492(4) 0.0274(13) Uani 1 1 d . . . H235 H 0.7699 -0.0325 0.2558 0.033 Uiso 1 1 calc R . . C236 C 0.7141(3) 0.0337(2) 0.2486(4) 0.0249(13) Uani 1 1 d . . . H236 H 0.7555 0.0546 0.2553 0.030 Uiso 1 1 calc R . . O241 O 0.56092(19) 0.12335(12) 0.2250(2) 0.0202(8) Uani 1 1 d . . . C242 C 0.6280(3) 0.11049(19) 0.2329(3) 0.0180(11) Uani 1 1 d . . . C243 C 0.6839(3) 0.14494(18) 0.2357(3) 0.0190(12) Uani 1 1 d . . . H243 H 0.7307 0.1326 0.2393 0.023 Uiso 1 1 calc R . . C244 C 0.6731(3) 0.19707(19) 0.2333(3) 0.0166(11) Uani 1 1 d . . . O245 O 0.61438(19) 0.21853(12) 0.2341(2) 0.0202(8) Uani 1 1 d . . . C251 C 0.7345(3) 0.23213(18) 0.2330(3) 0.0192(11) Uani 1 1 d . . . C252 C 0.7359(3) 0.28191(19) 0.2602(3) 0.0226(12) Uani 1 1 d . . . H252 H 0.6994 0.2921 0.2775 0.027 Uiso 1 1 calc R . . C253 C 0.7907(3) 0.3156(2) 0.2615(4) 0.0240(13) Uani 1 1 d . . . H253 H 0.7910 0.3484 0.2798 0.029 Uiso 1 1 calc R . . C254 C 0.8454(3) 0.3014(2) 0.2360(3) 0.0239(12) Uani 1 1 d . . . H254 H 0.8826 0.3244 0.2377 0.029 Uiso 1 1 calc R . . C255 C 0.8450(3) 0.2527(2) 0.2078(4) 0.0280(14) Uani 1 1 d . . . H255 H 0.8804 0.2432 0.1886 0.034 Uiso 1 1 calc R . . C256 C 0.7906(3) 0.2183(2) 0.2086(3) 0.0211(12) Uani 1 1 d . . . H256 H 0.7919 0.1851 0.1924 0.025 Uiso 1 1 calc R . . N261 N 0.5703(3) 0.31300(15) 0.3324(3) 0.0205(10) Uani 1 1 d . . . N262 N 0.5565(3) 0.26418(15) 0.3441(3) 0.0203(10) Uani 1 1 d . . . C263 C 0.6179(3) 0.2500(2) 0.4167(4) 0.0221(12) Uani 1 1 d . . . C264 C 0.6717(3) 0.2890(2) 0.4518(4) 0.0295(14) Uani 1 1 d . . . H264 H 0.7188 0.2888 0.5014 0.035 Uiso 1 1 calc R . . C265 C 0.6392(3) 0.3281(2) 0.3962(4) 0.0305(14) Uani 1 1 d . . . H265 H 0.6613 0.3599 0.4016 0.037 Uiso 1 1 calc R . . N271 N 0.5711(2) 0.16520(15) 0.3874(3) 0.0196(10) Uani 1 1 d . . . C272 C 0.6201(3) 0.19783(19) 0.4457(3) 0.0194(11) Uani 1 1 d . . . C273 C 0.6709(3) 0.1830(2) 0.5281(4) 0.0247(13) Uani 1 1 d . . . H273 H 0.7042 0.2060 0.5674 0.030 Uiso 1 1 calc R . . C274 C 0.6699(3) 0.1333(2) 0.5493(4) 0.0292(14) Uani 1 1 d . . . H274 H 0.7029 0.1224 0.6036 0.035 Uiso 1 1 calc R . . C275 C 0.6204(3) 0.0997(2) 0.4906(4) 0.0265(13) Uani 1 1 d . . . H275 H 0.6194 0.0660 0.5042 0.032 Uiso 1 1 calc R . . C276 C 0.5717(3) 0.1174(2) 0.4103(4) 0.0241(13) Uani 1 1 d . . . H276 H 0.5379 0.0947 0.3705 0.029 Uiso 1 1 calc R . . N281 N 0.5017(2) 0.32520(15) 0.1742(3) 0.0198(10) Uani 1 1 d . . . N282 N 0.4733(2) 0.27844(16) 0.1457(3) 0.0190(10) Uani 1 1 d . . . C283 C 0.4682(3) 0.2741(2) 0.0689(3) 0.0218(12) Uani 1 1 d . . . C284 C 0.4942(3) 0.3189(2) 0.0483(4) 0.0305(14) Uani 1 1 d . . . H284 H 0.4968 0.3260 -0.0009 0.037 Uiso 1 1 calc R . . C285 C 0.5145(3) 0.3495(2) 0.1159(4) 0.0270(14) Uani 1 1 d . . . H285 H 0.5342 0.3821 0.1211 0.032 Uiso 1 1 calc R . . N291 N 0.4397(2) 0.18737(15) 0.0699(3) 0.0204(10) Uani 1 1 d . . . C292 C 0.4452(3) 0.22620(19) 0.0242(3) 0.0193(12) Uani 1 1 d . . . C293 C 0.4319(3) 0.2203(2) -0.0577(4) 0.0247(13) Uani 1 1 d . . . H293 H 0.4370 0.2476 -0.0874 0.030 Uiso 1 1 calc R . . C294 C 0.4112(3) 0.1738(2) -0.0947(4) 0.0275(13) Uani 1 1 d . . . H294 H 0.4019 0.1692 -0.1498 0.033 Uiso 1 1 calc R . . C295 C 0.4043(3) 0.1338(2) -0.0495(4) 0.0283(14) Uani 1 1 d . . . H295 H 0.3897 0.1020 -0.0735 0.034 Uiso 1 1 calc R . . C296 C 0.4195(3) 0.1422(2) 0.0323(4) 0.0237(12) Uani 1 1 d . . . H296 H 0.4156 0.1152 0.0630 0.028 Uiso 1 1 calc R . . C300 C 0.5457(7) 0.9710(5) 0.5266(8) 0.039(3) Uani 0.50 1 d P . . H30A H 0.5367 0.9355 0.5319 0.047 Uiso 0.50 1 calc PR . . H30B H 0.6017 0.9764 0.5477 0.047 Uiso 0.50 1 calc PR . . Cl1 Cl 0.49125(11) 0.99116(7) 0.41646(12) 0.0543(5) Uani 1 1 d . . . H2A H 0.453(4) 0.343(2) 0.253(4) 0.065 Uiso 1 1 d . . . H2B H 0.532(4) 0.384(2) 0.264(4) 0.065 Uiso 1 1 d . . . H1A H 0.092(4) 0.639(2) 0.372(4) 0.065 Uiso 1 1 d . . . H1B H 0.013(4) 0.682(2) 0.308(4) 0.065 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.01470(14) 0.01599(14) 0.01670(15) 0.00004(12) 0.00710(12) -0.00017(12) B1 0.032(4) 0.020(3) 0.029(4) -0.008(3) 0.016(3) -0.007(3) C101 0.023(3) 0.016(3) 0.023(3) -0.004(2) 0.014(3) 0.001(2) C102 0.025(3) 0.019(3) 0.034(4) 0.004(3) 0.015(3) 0.004(2) C103 0.032(3) 0.017(3) 0.044(4) 0.000(3) 0.018(3) -0.003(3) C104 0.050(4) 0.017(3) 0.036(4) 0.004(3) 0.023(3) 0.001(3) C105 0.034(3) 0.027(3) 0.027(4) 0.009(3) 0.007(3) 0.006(3) C106 0.023(3) 0.024(3) 0.026(3) 0.002(3) 0.007(3) 0.001(2) O111 0.0143(19) 0.020(2) 0.026(2) -0.0015(17) 0.0054(17) 0.0005(16) C112 0.028(3) 0.014(3) 0.021(3) 0.001(2) 0.016(3) 0.003(2) C113 0.020(3) 0.021(3) 0.027(3) 0.002(2) 0.012(3) 0.005(2) C114 0.012(3) 0.027(3) 0.017(3) -0.005(2) 0.006(2) -0.002(2) O115 0.0159(18) 0.018(2) 0.024(2) 0.0017(16) 0.0043(17) 0.0022(15) C121 0.016(3) 0.023(3) 0.011(3) -0.003(2) 0.005(2) -0.002(2) C122 0.020(3) 0.026(3) 0.027(3) 0.003(3) 0.011(3) 0.003(2) C123 0.035(3) 0.025(3) 0.035(4) -0.005(3) 0.021(3) -0.010(3) C124 0.020(3) 0.045(4) 0.036(4) -0.013(3) 0.014(3) -0.015(3) C125 0.017(3) 0.041(4) 0.037(4) -0.008(3) 0.006(3) 0.002(3) C126 0.019(3) 0.029(3) 0.030(3) -0.006(3) 0.009(3) -0.003(3) C131 0.019(3) 0.019(3) 0.023(3) 0.006(2) 0.012(3) 0.005(2) C132 0.026(3) 0.024(3) 0.031(4) -0.002(3) 0.011(3) 0.004(3) C133 0.037(4) 0.024(3) 0.037(4) -0.003(3) 0.014(3) 0.003(3) C134 0.035(3) 0.023(3) 0.037(4) 0.009(3) 0.020(3) 0.013(3) C135 0.021(3) 0.043(4) 0.031(4) 0.003(3) 0.009(3) 0.007(3) C136 0.021(3) 0.028(3) 0.026(3) 0.001(3) 0.010(3) 0.005(2) O141 0.0206(19) 0.023(2) 0.019(2) -0.0051(16) 0.0060(17) -0.0010(16) C142 0.012(2) 0.023(3) 0.020(3) 0.001(2) 0.010(2) -0.002(2) C143 0.017(3) 0.022(3) 0.015(3) 0.000(2) 0.005(2) -0.002(2) C144 0.008(2) 0.022(3) 0.015(3) -0.002(2) 0.002(2) -0.005(2) O145 0.0196(19) 0.0199(19) 0.024(2) 0.0033(16) 0.0118(18) -0.0003(16) C151 0.025(3) 0.018(3) 0.022(3) -0.005(2) 0.011(3) -0.009(2) C152 0.023(3) 0.023(3) 0.020(3) -0.002(2) 0.008(3) -0.003(2) C153 0.039(4) 0.021(3) 0.037(4) -0.001(3) 0.021(3) 0.000(3) C154 0.048(4) 0.021(3) 0.042(4) -0.010(3) 0.027(4) -0.006(3) C155 0.037(4) 0.032(4) 0.022(3) -0.008(3) 0.011(3) -0.008(3) C156 0.034(3) 0.021(3) 0.023(3) 0.000(2) 0.014(3) 0.000(3) N161 0.026(3) 0.013(2) 0.023(3) -0.0038(19) 0.010(2) 0.0009(19) N162 0.017(2) 0.017(2) 0.019(3) -0.0036(19) 0.006(2) -0.0037(18) C163 0.018(3) 0.024(3) 0.016(3) -0.005(2) 0.005(2) -0.002(2) C164 0.024(3) 0.028(3) 0.027(3) -0.002(3) 0.014(3) 0.002(3) C165 0.029(3) 0.021(3) 0.025(3) -0.003(2) 0.010(3) 0.005(3) N171 0.021(2) 0.019(2) 0.027(3) -0.001(2) 0.011(2) -0.002(2) C172 0.012(2) 0.024(3) 0.018(3) -0.004(2) 0.005(2) -0.001(2) C173 0.028(3) 0.027(3) 0.026(3) -0.005(3) 0.017(3) 0.000(3) C174 0.021(3) 0.037(3) 0.024(3) -0.004(3) 0.013(3) -0.005(3) C175 0.027(3) 0.023(3) 0.025(3) -0.002(2) 0.016(3) -0.007(2) C176 0.023(3) 0.024(3) 0.030(4) -0.001(3) 0.016(3) 0.003(2) N181 0.023(2) 0.014(2) 0.033(3) 0.000(2) 0.011(2) -0.001(2) N182 0.015(2) 0.019(2) 0.016(2) 0.0022(19) 0.002(2) -0.0010(19) C183 0.018(3) 0.027(3) 0.020(3) 0.001(2) 0.010(2) -0.004(2) C184 0.034(3) 0.027(3) 0.025(3) 0.001(3) 0.013(3) -0.008(3) C185 0.038(3) 0.018(3) 0.028(4) 0.008(3) 0.013(3) -0.001(3) N191 0.019(2) 0.021(2) 0.018(2) -0.0028(19) 0.008(2) -0.0006(19) C192 0.017(3) 0.024(3) 0.016(3) 0.005(2) 0.005(2) -0.003(2) C193 0.029(3) 0.029(3) 0.027(3) 0.001(3) 0.017(3) -0.002(3) C194 0.029(3) 0.039(4) 0.023(3) -0.004(3) 0.018(3) 0.000(3) C195 0.022(3) 0.028(3) 0.032(4) -0.003(3) 0.013(3) 0.005(3) C196 0.023(3) 0.023(3) 0.028(3) 0.005(2) 0.015(3) -0.001(2) Nd2 0.01589(14) 0.01346(13) 0.01892(15) -0.00007(12) 0.00931(12) 0.00003(12) B2 0.040(4) 0.015(3) 0.042(5) 0.008(3) 0.027(4) 0.004(3) C201 0.018(3) 0.017(3) 0.029(3) -0.002(2) 0.012(3) -0.001(2) C202 0.018(3) 0.024(3) 0.031(3) 0.000(2) 0.013(3) 0.000(2) C203 0.028(3) 0.023(3) 0.041(4) -0.004(3) 0.018(3) 0.004(3) C204 0.025(3) 0.013(3) 0.047(4) 0.001(3) 0.013(3) -0.007(2) C205 0.026(3) 0.024(3) 0.036(4) 0.002(3) 0.018(3) -0.004(3) C206 0.024(3) 0.021(3) 0.034(4) 0.000(3) 0.017(3) 0.003(2) O211 0.0177(19) 0.0162(19) 0.035(2) -0.0026(17) 0.0143(18) -0.0007(15) C212 0.015(3) 0.022(3) 0.018(3) -0.003(2) 0.004(2) -0.001(2) C213 0.021(3) 0.017(3) 0.032(3) 0.004(2) 0.016(3) -0.001(2) C214 0.018(3) 0.024(3) 0.018(3) 0.000(2) 0.010(2) 0.000(2) O215 0.023(2) 0.0139(18) 0.028(2) -0.0025(16) 0.0135(18) -0.0016(16) C221 0.019(3) 0.015(3) 0.023(3) -0.003(2) 0.009(2) 0.001(2) C222 0.019(3) 0.023(3) 0.025(3) -0.004(2) 0.007(3) 0.001(2) C223 0.028(3) 0.017(3) 0.031(4) -0.002(3) 0.012(3) 0.003(2) C224 0.021(3) 0.030(3) 0.032(4) -0.007(3) 0.008(3) 0.011(3) C225 0.038(4) 0.032(4) 0.041(4) 0.002(3) 0.030(3) 0.008(3) C226 0.029(3) 0.021(3) 0.035(4) 0.001(3) 0.020(3) 0.006(2) C231 0.021(3) 0.016(3) 0.019(3) -0.001(2) 0.010(2) 0.002(2) C232 0.020(3) 0.025(3) 0.030(3) 0.002(3) 0.008(3) 0.003(2) C233 0.021(3) 0.020(3) 0.037(4) 0.000(3) 0.009(3) -0.004(2) C234 0.030(3) 0.014(3) 0.029(4) 0.003(2) 0.010(3) 0.005(2) C235 0.033(3) 0.023(3) 0.031(4) 0.001(3) 0.019(3) 0.010(3) C236 0.023(3) 0.021(3) 0.031(4) 0.004(3) 0.013(3) 0.002(2) O241 0.0153(18) 0.0198(19) 0.025(2) -0.0001(16) 0.0094(17) 0.0017(15) C242 0.015(3) 0.020(3) 0.015(3) 0.000(2) 0.004(2) 0.000(2) C243 0.017(3) 0.015(3) 0.025(3) 0.000(2) 0.009(2) 0.003(2) C244 0.015(3) 0.019(3) 0.016(3) 0.000(2) 0.008(2) -0.002(2) O245 0.0193(19) 0.0165(18) 0.026(2) 0.0032(16) 0.0111(17) 0.0049(16) C251 0.020(3) 0.015(3) 0.021(3) 0.000(2) 0.008(2) 0.000(2) C252 0.023(3) 0.023(3) 0.022(3) 0.000(2) 0.011(3) 0.003(2) C253 0.024(3) 0.017(3) 0.027(3) 0.002(2) 0.008(3) -0.002(2) C254 0.015(3) 0.025(3) 0.027(3) 0.006(3) 0.006(2) -0.006(2) C255 0.022(3) 0.033(3) 0.031(4) 0.007(3) 0.014(3) 0.005(3) C256 0.021(3) 0.017(3) 0.023(3) 0.002(2) 0.009(3) 0.003(2) N261 0.025(2) 0.013(2) 0.027(3) -0.0023(19) 0.015(2) -0.0035(19) N262 0.025(2) 0.013(2) 0.028(3) -0.001(2) 0.017(2) 0.0031(19) C263 0.022(3) 0.021(3) 0.024(3) -0.006(2) 0.012(3) -0.002(2) C264 0.029(3) 0.026(3) 0.026(3) -0.004(3) 0.007(3) -0.004(3) C265 0.036(3) 0.021(3) 0.028(4) -0.008(3) 0.009(3) -0.012(3) N271 0.025(2) 0.015(2) 0.021(3) -0.0042(19) 0.013(2) -0.0010(19) C272 0.017(3) 0.019(3) 0.020(3) 0.002(2) 0.008(2) 0.002(2) C273 0.024(3) 0.024(3) 0.023(3) 0.001(2) 0.009(3) 0.003(2) C274 0.025(3) 0.030(3) 0.028(4) 0.007(3) 0.009(3) 0.008(3) C275 0.035(3) 0.015(3) 0.033(4) 0.003(3) 0.018(3) 0.002(3) C276 0.027(3) 0.021(3) 0.020(3) -0.001(2) 0.007(3) -0.001(2) N281 0.023(2) 0.008(2) 0.033(3) 0.002(2) 0.017(2) 0.0013(18) N282 0.014(2) 0.019(2) 0.020(3) 0.0014(19) 0.005(2) 0.0019(19) C283 0.021(3) 0.023(3) 0.022(3) 0.004(2) 0.010(3) 0.001(2) C284 0.042(4) 0.024(3) 0.036(4) 0.009(3) 0.027(3) 0.006(3) C285 0.032(3) 0.017(3) 0.040(4) 0.008(3) 0.023(3) 0.001(2) N291 0.020(2) 0.017(2) 0.026(3) 0.001(2) 0.013(2) 0.0007(19) C292 0.016(3) 0.019(3) 0.026(3) 0.005(2) 0.012(2) 0.007(2) C293 0.025(3) 0.032(3) 0.022(3) 0.005(3) 0.014(3) 0.005(3) C294 0.020(3) 0.041(4) 0.019(3) -0.001(3) 0.007(3) 0.008(3) C295 0.018(3) 0.037(3) 0.028(4) -0.008(3) 0.009(3) 0.000(3) C296 0.022(3) 0.024(3) 0.025(3) 0.001(2) 0.011(3) 0.003(2) C300 0.032(7) 0.039(7) 0.032(8) 0.004(6) 0.003(6) 0.003(6) Cl1 0.0518(11) 0.0449(10) 0.0553(12) -0.0096(9) 0.0157(10) -0.0072(9) _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 Nd1 O115 2.354(3) . ? Nd1 O141 2.372(4) . ? Nd1 O111 2.400(3) . ? Nd1 O145 2.422(4) . ? Nd1 N162 2.573(4) . ? Nd1 N171 2.607(4) . ? Nd1 N182 2.607(4) . ? Nd1 N191 2.644(4) . ? B1 N161 1.540(8) . ? B1 N181 1.548(8) . ? C101 C106 1.395(7) . ? C101 C102 1.398(7) . ? C101 C112 1.507(7) . ? C102 C103 1.391(7) . ? C103 C104 1.384(8) . ? C104 C105 1.374(8) . ? C105 C106 1.391(7) . ? O111 C112 1.273(6) . ? C112 C113 1.405(7) . ? C113 C114 1.405(7) . ? C114 O115 1.260(6) . ? C114 C121 1.498(7) . ? C121 C126 1.382(7) . ? C121 C122 1.409(7) . ? C122 C123 1.381(7) . ? C123 C124 1.368(8) . ? C124 C125 1.378(8) . ? C125 C126 1.373(7) . ? C131 C136 1.381(8) . ? C131 C132 1.394(7) . ? C131 C142 1.507(7) . ? C132 C133 1.384(7) . ? C133 C134 1.378(8) . ? C134 C135 1.386(8) . ? C135 C136 1.382(7) . ? O141 C142 1.269(6) . ? C142 C143 1.408(7) . ? C143 C144 1.402(7) . ? C144 O145 1.282(6) . ? C144 C151 1.511(7) . ? C151 C156 1.391(7) . ? C151 C152 1.395(7) . ? C152 C153 1.395(7) . ? C153 C154 1.376(8) . ? C154 C155 1.374(8) . ? C155 C156 1.383(7) . ? N161 C165 1.349(6) . ? N161 N162 1.364(5) . ? N162 C163 1.340(6) . ? C163 C164 1.398(7) . ? C163 C172 1.464(7) . ? C164 C165 1.375(7) . ? N171 C176 1.333(6) . ? N171 C172 1.353(6) . ? C172 C173 1.393(7) . ? C173 C174 1.373(7) . ? C174 C175 1.378(7) . ? C175 C176 1.390(7) . ? N181 C185 1.344(7) . ? N181 N182 1.361(6) . ? N182 C183 1.337(6) . ? C183 C184 1.399(7) . ? C183 C192 1.468(7) . ? C184 C185 1.366(8) . ? N191 C196 1.331(6) . ? N191 C192 1.353(6) . ? C192 C193 1.388(7) . ? C193 C194 1.383(7) . ? C194 C195 1.380(8) . ? C195 C196 1.384(7) . ? Nd2 O241 2.377(3) . ? Nd2 O215 2.380(3) . ? Nd2 O245 2.383(3) . ? Nd2 O211 2.390(3) . ? Nd2 N262 2.557(4) . ? Nd2 N282 2.584(4) . ? Nd2 N291 2.603(5) . ? Nd2 N271 2.636(5) . ? B2 N281 1.539(8) . ? B2 N261 1.562(8) . ? C201 C202 1.390(7) . ? C201 C206 1.400(7) . ? C201 C212 1.501(7) . ? C202 C203 1.382(7) . ? C203 C204 1.396(8) . ? C204 C205 1.374(8) . ? C205 C206 1.379(7) . ? O211 C212 1.280(6) . ? C212 C213 1.402(7) . ? C213 C214 1.388(7) . ? C214 O215 1.280(6) . ? C214 C221 1.504(7) . ? C221 C226 1.386(7) . ? C221 C222 1.396(7) . ? C222 C223 1.384(7) . ? C223 C224 1.382(8) . ? C224 C225 1.391(8) . ? C225 C226 1.386(7) . ? C231 C236 1.388(7) . ? C231 C232 1.395(7) . ? C231 C242 1.509(7) . ? C232 C233 1.389(7) . ? C233 C234 1.381(7) . ? C234 C235 1.371(7) . ? C235 C236 1.401(7) . ? O241 C242 1.274(6) . ? C242 C243 1.393(7) . ? C243 C244 1.397(7) . ? C244 O245 1.268(5) . ? C244 C251 1.505(7) . ? C251 C256 1.387(7) . ? C251 C252 1.406(7) . ? C252 C253 1.371(7) . ? C253 C254 1.379(7) . ? C254 C255 1.387(7) . ? C255 C256 1.393(7) . ? N261 C265 1.349(7) . ? N261 N262 1.359(5) . ? N262 C263 1.345(7) . ? C263 C264 1.392(7) . ? C263 C272 1.473(7) . ? C264 C265 1.374(8) . ? N271 C276 1.333(6) . ? N271 C272 1.349(6) . ? C272 C273 1.402(7) . ? C273 C274 1.376(7) . ? C274 C275 1.371(8) . ? C275 C276 1.388(7) . ? N281 C285 1.349(7) . ? N281 N282 1.357(5) . ? N282 C283 1.346(7) . ? C283 C284 1.403(7) . ? C283 C292 1.459(7) . ? C284 C285 1.362(8) . ? N291 C296 1.343(6) . ? N291 C292 1.352(6) . ? C292 C293 1.384(7) . ? C293 C294 1.371(8) . ? C294 C295 1.382(8) . ? C295 C296 1.378(8) . ? C300 Cl1 1.799(13) 3_676 ? C300 Cl1 1.840(13) . ? Cl1 C300 1.799(13) 3_676 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O115 Nd1 O141 149.66(12) . . ? O115 Nd1 O111 69.23(12) . . ? O141 Nd1 O111 140.63(12) . . ? O115 Nd1 O145 133.54(12) . . ? O141 Nd1 O145 69.72(12) . . ? O111 Nd1 O145 73.50(12) . . ? O115 Nd1 N162 90.36(13) . . ? O141 Nd1 N162 75.27(13) . . ? O111 Nd1 N162 125.41(13) . . ? O145 Nd1 N162 134.55(12) . . ? O115 Nd1 N171 111.01(13) . . ? O141 Nd1 N171 86.71(13) . . ? O111 Nd1 N171 77.06(13) . . ? O145 Nd1 N171 85.92(13) . . ? N162 Nd1 N171 63.70(13) . . ? O115 Nd1 N182 74.15(12) . . ? O141 Nd1 N182 76.20(12) . . ? O111 Nd1 N182 137.89(12) . . ? O145 Nd1 N182 122.47(13) . . ? N162 Nd1 N182 73.85(14) . . ? N171 Nd1 N182 137.05(13) . . ? O115 Nd1 N191 80.85(13) . . ? O141 Nd1 N191 91.22(13) . . ? O111 Nd1 N191 91.23(13) . . ? O145 Nd1 N191 73.14(12) . . ? N162 Nd1 N191 136.35(13) . . ? N171 Nd1 N191 158.30(13) . . ? N182 Nd1 N191 62.59(13) . . ? N161 B1 N181 112.1(5) . . ? C106 C101 C102 117.9(5) . . ? C106 C101 C112 123.9(5) . . ? C102 C101 C112 118.1(5) . . ? C103 C102 C101 121.1(5) . . ? C104 C103 C102 119.8(6) . . ? C105 C104 C103 120.0(5) . . ? C104 C105 C106 120.4(6) . . ? C105 C106 C101 120.8(5) . . ? C112 O111 Nd1 138.8(3) . . ? O111 C112 C113 123.2(5) . . ? O111 C112 C101 116.6(5) . . ? C113 C112 C101 120.3(5) . . ? C112 C113 C114 123.9(5) . . ? O115 C114 C113 122.6(5) . . ? O115 C114 C121 116.0(4) . . ? C113 C114 C121 121.3(5) . . ? C114 O115 Nd1 141.5(3) . . ? C126 C121 C122 117.6(5) . . ? C126 C121 C114 124.4(5) . . ? C122 C121 C114 118.0(5) . . ? C123 C122 C121 119.9(5) . . ? C124 C123 C122 121.0(5) . . ? C123 C124 C125 119.9(5) . . ? C126 C125 C124 119.5(5) . . ? C125 C126 C121 122.2(5) . . ? C136 C131 C132 118.6(5) . . ? C136 C131 C142 124.3(5) . . ? C132 C131 C142 117.1(5) . . ? C133 C132 C131 120.7(5) . . ? C134 C133 C132 119.9(6) . . ? C133 C134 C135 119.9(6) . . ? C136 C135 C134 119.9(6) . . ? C131 C136 C135 121.0(5) . . ? C142 O141 Nd1 136.7(3) . . ? O141 C142 C143 123.8(5) . . ? O141 C142 C131 115.7(5) . . ? C143 C142 C131 120.5(5) . . ? C144 C143 C142 123.4(5) . . ? O145 C144 C143 124.7(5) . . ? O145 C144 C151 114.7(5) . . ? C143 C144 C151 120.4(5) . . ? C144 O145 Nd1 133.1(3) . . ? C156 C151 C152 118.1(5) . . ? C156 C151 C144 123.6(5) . . ? C152 C151 C144 118.3(5) . . ? C151 C152 C153 121.9(5) . . ? C154 C153 C152 118.6(6) . . ? C155 C154 C153 120.1(6) . . ? C154 C155 C156 121.5(6) . . ? C155 C156 C151 119.7(5) . . ? C165 N161 N162 108.8(4) . . ? C165 N161 B1 126.4(5) . . ? N162 N161 B1 123.8(4) . . ? C163 N162 N161 106.7(4) . . ? C163 N162 Nd1 118.2(3) . . ? N161 N162 Nd1 131.2(3) . . ? N162 C163 C164 110.8(5) . . ? N162 C163 C172 119.8(4) . . ? C164 C163 C172 129.4(5) . . ? C165 C164 C163 103.9(5) . . ? N161 C165 C164 109.7(5) . . ? C176 N171 C172 117.8(5) . . ? C176 N171 Nd1 122.7(3) . . ? C172 N171 Nd1 119.5(3) . . ? N171 C172 C173 121.5(5) . . ? N171 C172 C163 116.1(5) . . ? C173 C172 C163 122.3(5) . . ? C174 C173 C172 119.4(5) . . ? C173 C174 C175 119.8(5) . . ? C174 C175 C176 117.5(5) . . ? N171 C176 C175 124.0(5) . . ? C185 N181 N182 108.6(5) . . ? C185 N181 B1 126.5(5) . . ? N182 N181 B1 122.8(5) . . ? C183 N182 N181 106.9(4) . . ? C183 N182 Nd1 120.1(3) . . ? N181 N182 Nd1 131.5(3) . . ? N182 C183 C184 110.4(5) . . ? N182 C183 C192 119.4(5) . . ? C184 C183 C192 130.2(5) . . ? C185 C184 C183 104.0(5) . . ? N181 C185 C184 110.1(5) . . ? C196 N191 C192 118.8(5) . . ? C196 N191 Nd1 120.6(3) . . ? C192 N191 Nd1 120.5(3) . . ? N191 C192 C193 121.2(5) . . ? N191 C192 C183 116.1(5) . . ? C193 C192 C183 122.7(5) . . ? C194 C193 C192 119.4(5) . . ? C195 C194 C193 119.1(5) . . ? C194 C195 C196 118.6(5) . . ? N191 C196 C195 122.9(5) . . ? O241 Nd2 O215 142.26(11) . . ? O241 Nd2 O245 69.22(11) . . ? O215 Nd2 O245 148.42(11) . . ? O241 Nd2 O211 72.75(11) . . ? O215 Nd2 O211 69.67(11) . . ? O245 Nd2 O211 141.91(11) . . ? O241 Nd2 N262 122.68(13) . . ? O215 Nd2 N262 82.32(13) . . ? O245 Nd2 N262 73.11(13) . . ? O211 Nd2 N262 132.67(13) . . ? O241 Nd2 N282 126.25(13) . . ? O215 Nd2 N282 84.15(12) . . ? O245 Nd2 N282 71.26(12) . . ? O211 Nd2 N282 134.07(13) . . ? N262 Nd2 N282 76.61(14) . . ? O241 Nd2 N291 79.02(13) . . ? O215 Nd2 N291 101.00(13) . . ? O245 Nd2 N291 85.41(13) . . ? O211 Nd2 N291 85.33(13) . . ? N262 Nd2 N291 138.49(13) . . ? N282 Nd2 N291 62.82(13) . . ? O241 Nd2 N271 74.64(12) . . ? O215 Nd2 N271 97.27(13) . . ? O245 Nd2 N271 89.13(13) . . ? O211 Nd2 N271 82.98(13) . . ? N262 Nd2 N271 63.10(13) . . ? N282 Nd2 N271 138.97(13) . . ? N291 Nd2 N271 153.33(13) . . ? N281 B2 N261 110.2(5) . . ? C202 C201 C206 118.6(5) . . ? C202 C201 C212 118.2(5) . . ? C206 C201 C212 123.2(5) . . ? C203 C202 C201 120.8(5) . . ? C202 C203 C204 120.1(5) . . ? C205 C204 C203 119.2(5) . . ? C204 C205 C206 121.1(5) . . ? C205 C206 C201 120.2(5) . . ? C212 O211 Nd2 137.9(3) . . ? O211 C212 C213 123.9(5) . . ? O211 C212 C201 116.0(4) . . ? C213 C212 C201 120.0(4) . . ? C214 C213 C212 123.6(5) . . ? O215 C214 C213 124.2(5) . . ? O215 C214 C221 116.2(4) . . ? C213 C214 C221 119.6(4) . . ? C214 O215 Nd2 138.9(3) . . ? C226 C221 C222 119.2(5) . . ? C226 C221 C214 122.3(5) . . ? C222 C221 C214 118.4(5) . . ? C223 C222 C221 120.6(5) . . ? C224 C223 C222 119.5(5) . . ? C223 C224 C225 120.5(5) . . ? C226 C225 C224 119.6(5) . . ? C221 C226 C225 120.5(5) . . ? C236 C231 C232 118.9(5) . . ? C236 C231 C242 123.8(5) . . ? C232 C231 C242 117.3(4) . . ? C233 C232 C231 120.2(5) . . ? C234 C233 C232 120.6(5) . . ? C235 C234 C233 119.8(5) . . ? C234 C235 C236 120.4(5) . . ? C231 C236 C235 120.2(5) . . ? C242 O241 Nd2 139.8(3) . . ? O241 C242 C243 123.3(5) . . ? O241 C242 C231 115.7(4) . . ? C243 C242 C231 120.9(4) . . ? C242 C243 C244 123.2(5) . . ? O245 C244 C243 124.4(4) . . ? O245 C244 C251 115.1(4) . . ? C243 C244 C251 120.5(4) . . ? C244 O245 Nd2 139.2(3) . . ? C256 C251 C252 117.9(5) . . ? C256 C251 C244 124.2(5) . . ? C252 C251 C244 117.9(4) . . ? C253 C252 C251 120.6(5) . . ? C252 C253 C254 120.8(5) . . ? C253 C254 C255 120.0(5) . . ? C254 C255 C256 119.0(5) . . ? C251 C256 C255 121.6(5) . . ? C265 N261 N262 109.7(5) . . ? C265 N261 B2 127.5(5) . . ? N262 N261 B2 122.8(5) . . ? C263 N262 N261 105.8(4) . . ? C263 N262 Nd2 117.1(3) . . ? N261 N262 Nd2 126.9(3) . . ? N262 C263 C264 111.3(5) . . ? N262 C263 C272 118.4(5) . . ? C264 C263 C272 130.3(5) . . ? C265 C264 C263 104.0(5) . . ? N261 C265 C264 109.2(5) . . ? C276 N271 C272 117.9(5) . . ? C276 N271 Nd2 123.4(4) . . ? C272 N271 Nd2 118.2(3) . . ? N271 C272 C273 122.2(5) . . ? N271 C272 C263 115.6(5) . . ? C273 C272 C263 122.1(5) . . ? C274 C273 C272 118.1(5) . . ? C275 C274 C273 120.2(6) . . ? C274 C275 C276 118.3(5) . . ? N271 C276 C275 123.2(5) . . ? C285 N281 N282 109.3(5) . . ? C285 N281 B2 128.4(5) . . ? N282 N281 B2 122.2(4) . . ? C283 N282 N281 107.0(4) . . ? C283 N282 Nd2 117.4(3) . . ? N281 N282 Nd2 128.4(3) . . ? N282 C283 C284 109.5(5) . . ? N282 C283 C292 120.0(5) . . ? C284 C283 C292 130.3(5) . . ? C285 C284 C283 105.1(5) . . ? N281 C285 C284 109.1(5) . . ? C296 N291 C292 117.5(5) . . ? C296 N291 Nd2 121.2(4) . . ? C292 N291 Nd2 120.3(3) . . ? N291 C292 C293 122.2(5) . . ? N291 C292 C283 114.8(5) . . ? C293 C292 C283 123.0(5) . . ? C294 C293 C292 119.2(5) . . ? C293 C294 C295 119.5(6) . . ? C296 C295 C294 118.3(6) . . ? N291 C296 C295 123.4(5) . . ? Cl1 C300 Cl1 105.9(6) 3_676 . ? C300 Cl1 C300 74.1(6) 3_676 . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 2.122 _refine_diff_density_min -1.237 _refine_diff_density_rms 0.137 #=END data_imw15g _database_code_depnum_ccdc_archive 'CCDC 229466' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46.25 H36.50 B Cl0.50 Er N6 O4' _chemical_formula_sum 'C46.25 H36.50 B Cl0.50 Er N6 O4' _chemical_formula_weight 936.11 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' B B 0.0013 0.0007 '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' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.232(3) _cell_length_b 26.871(4) _cell_length_c 17.501(2) _cell_angle_alpha 90.00 _cell_angle_beta 116.158(2) _cell_angle_gamma 90.00 _cell_volume 8117.8(18) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3835 _cell_measurement_theta_min 4.525 _cell_measurement_theta_max 42.374 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.532 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3756 _exptl_absorpt_coefficient_mu 2.153 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4579 _exptl_absorpt_correction_T_max 0.8135 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 65690 _diffrn_reflns_av_R_equivalents 0.1952 _diffrn_reflns_av_sigmaI/netI 0.2359 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 27.59 _reflns_number_total 18254 _reflns_number_gt 7975 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0004P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18254 _refine_ls_number_parameters 1063 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1919 _refine_ls_R_factor_gt 0.0669 _refine_ls_wR_factor_ref 0.1852 _refine_ls_wR_factor_gt 0.1324 _refine_ls_goodness_of_fit_ref 0.944 _refine_ls_restrained_S_all 0.944 _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 Er1 Er 0.49151(3) 0.807191(15) 0.26768(3) 0.02568(13) Uani 1 1 d . . . B1 B 0.4989(7) 0.6612(4) 0.2566(8) 0.035(3) Uani 1 1 d . . . H1A H 0.4475 0.6620 0.2065 0.042 Uiso 1 1 calc R . . H1B H 0.5155 0.6260 0.2685 0.042 Uiso 1 1 calc R . . C101 C 0.7268(5) 0.7685(3) 0.4925(6) 0.024(2) Uani 1 1 d . . . C102 C 0.7241(5) 0.7192(4) 0.4643(7) 0.033(3) Uani 1 1 d . . . H102 H 0.6851 0.7095 0.4101 0.039 Uiso 1 1 calc R . . C103 C 0.7782(6) 0.6850(4) 0.5154(7) 0.039(3) Uani 1 1 d . . . H103 H 0.7764 0.6518 0.4960 0.047 Uiso 1 1 calc R . . C104 C 0.8346(6) 0.6986(4) 0.5940(7) 0.038(3) Uani 1 1 d . . . H104 H 0.8722 0.6750 0.6285 0.046 Uiso 1 1 calc R . . C105 C 0.8362(6) 0.7474(4) 0.6231(6) 0.039(3) Uani 1 1 d . . . H105 H 0.8734 0.7566 0.6786 0.047 Uiso 1 1 calc R . . C106 C 0.7840(6) 0.7821(4) 0.5712(6) 0.037(3) Uani 1 1 d . . . H106 H 0.7874 0.8157 0.5897 0.044 Uiso 1 1 calc R . . O111 O 0.6045(4) 0.7838(2) 0.3791(4) 0.0338(17) Uani 1 1 d . . . C112 C 0.6663(6) 0.8037(4) 0.4334(6) 0.028(2) Uani 1 1 d . . . C113 C 0.6798(5) 0.8549(3) 0.4400(6) 0.029(2) Uani 1 1 d . . . H113 H 0.7291 0.8667 0.4800 0.034 Uiso 1 1 calc R . . C114 C 0.6236(6) 0.8899(3) 0.3900(6) 0.027(2) Uani 1 1 d . . . O115 O 0.5556(4) 0.8774(2) 0.3369(4) 0.0316(16) Uani 1 1 d . . . C121 C 0.6405(6) 0.9447(4) 0.4003(6) 0.030(2) Uani 1 1 d . . . C122 C 0.5812(6) 0.9771(4) 0.3506(7) 0.040(3) Uani 1 1 d . . . H122 H 0.5326 0.9640 0.3113 0.047 Uiso 1 1 calc R . . C123 C 0.5925(6) 1.0275(4) 0.3579(7) 0.041(3) Uani 1 1 d . . . H123 H 0.5518 1.0494 0.3236 0.049 Uiso 1 1 calc R . . C124 C 0.6629(7) 1.0466(4) 0.4150(8) 0.044(3) Uani 1 1 d . . . H124 H 0.6704 1.0817 0.4196 0.053 Uiso 1 1 calc R . . C125 C 0.7222(7) 1.0155(4) 0.4653(7) 0.039(3) Uani 1 1 d . . . H125 H 0.7704 1.0287 0.5052 0.047 Uiso 1 1 calc R . . C126 C 0.7103(6) 0.9649(4) 0.4565(7) 0.039(3) Uani 1 1 d . . . H126 H 0.7515 0.9432 0.4903 0.047 Uiso 1 1 calc R . . C131 C 0.3386(6) 0.9379(4) 0.1068(7) 0.031(2) Uani 1 1 d . . . C132 C 0.3671(6) 0.9727(4) 0.1714(7) 0.037(3) Uani 1 1 d . . . H132 H 0.3968 0.9620 0.2285 0.045 Uiso 1 1 calc R . . C133 C 0.3525(6) 1.0233(4) 0.1536(7) 0.041(3) Uani 1 1 d . . . H133 H 0.3722 1.0470 0.1984 0.049 Uiso 1 1 calc R . . C134 C 0.3099(6) 1.0388(4) 0.0714(8) 0.047(3) Uani 1 1 d . . . H134 H 0.3013 1.0734 0.0594 0.056 Uiso 1 1 calc R . . C135 C 0.2794(6) 1.0048(4) 0.0059(7) 0.043(3) Uani 1 1 d . . . H135 H 0.2486 1.0156 -0.0508 0.052 Uiso 1 1 calc R . . C136 C 0.2944(6) 0.9538(4) 0.0240(7) 0.038(3) Uani 1 1 d . . . H136 H 0.2740 0.9301 -0.0208 0.046 Uiso 1 1 calc R . . O141 O 0.4164(4) 0.8749(2) 0.1996(4) 0.0294(16) Uani 1 1 d . . . C142 C 0.3575(5) 0.8838(4) 0.1282(6) 0.028(2) Uani 1 1 d . . . C143 C 0.3126(6) 0.8470(4) 0.0742(7) 0.040(3) Uani 1 1 d . . . H143 H 0.2705 0.8566 0.0221 0.047 Uiso 1 1 calc R . . C144 C 0.3262(5) 0.7962(3) 0.0924(6) 0.028(2) Uani 1 1 d . . . O145 O 0.3841(4) 0.7783(2) 0.1561(4) 0.0337(17) Uani 1 1 d . . . C151 C 0.2699(5) 0.7591(4) 0.0335(6) 0.030(2) Uani 1 1 d . . . C152 C 0.2718(6) 0.7111(4) 0.0645(7) 0.039(3) Uani 1 1 d . . . H152 H 0.3077 0.7027 0.1209 0.047 Uiso 1 1 calc R . . C153 C 0.2191(6) 0.6748(4) 0.0104(8) 0.052(3) Uani 1 1 d . . . H153 H 0.2190 0.6422 0.0311 0.063 Uiso 1 1 calc R . . C154 C 0.1689(7) 0.6869(4) -0.0710(7) 0.047(3) Uani 1 1 d . . . H154 H 0.1346 0.6623 -0.1069 0.056 Uiso 1 1 calc R . . C155 C 0.1672(7) 0.7336(5) -0.1018(7) 0.056(4) Uani 1 1 d . . . H155 H 0.1317 0.7417 -0.1586 0.067 Uiso 1 1 calc R . . C156 C 0.2184(7) 0.7699(4) -0.0490(7) 0.052(4) Uani 1 1 d . . . H156 H 0.2174 0.8025 -0.0706 0.063 Uiso 1 1 calc R . . N161 N 0.4926(5) 0.6837(3) 0.3336(5) 0.032(2) Uani 1 1 d . . . N162 N 0.4677(4) 0.7317(3) 0.3331(5) 0.0276(19) Uani 1 1 d . . . C163 C 0.4607(6) 0.7374(3) 0.4056(6) 0.030(2) Uani 1 1 d . . . C164 C 0.4794(6) 0.6926(4) 0.4527(7) 0.041(3) Uani 1 1 d . . . H164 H 0.4785 0.6859 0.5055 0.049 Uiso 1 1 calc R . . C165 C 0.4992(6) 0.6613(4) 0.4039(7) 0.041(3) Uani 1 1 d . . . H165 H 0.5156 0.6278 0.4186 0.049 Uiso 1 1 calc R . . N171 N 0.4372(5) 0.8230(3) 0.3720(5) 0.031(2) Uani 1 1 d . . . C172 C 0.4389(5) 0.7853(4) 0.4252(6) 0.031(2) Uani 1 1 d . . . C173 C 0.4260(6) 0.7941(4) 0.4944(6) 0.037(3) Uani 1 1 d . . . H173 H 0.4293 0.7676 0.5319 0.045 Uiso 1 1 calc R . . C174 C 0.4079(6) 0.8421(4) 0.5099(7) 0.040(3) Uani 1 1 d . . . H174 H 0.3986 0.8489 0.5579 0.048 Uiso 1 1 calc R . . C175 C 0.4037(6) 0.8795(5) 0.4543(7) 0.047(3) Uani 1 1 d . . . H175 H 0.3895 0.9123 0.4623 0.057 Uiso 1 1 calc R . . C176 C 0.4200(5) 0.8690(4) 0.3873(6) 0.033(3) Uani 1 1 d . . . H176 H 0.4192 0.8953 0.3505 0.039 Uiso 1 1 calc R . . N181 N 0.5601(5) 0.6917(3) 0.2362(5) 0.036(2) Uani 1 1 d . . . N182 N 0.5467(5) 0.7405(3) 0.2149(5) 0.029(2) Uani 1 1 d . . . C183 C 0.6062(6) 0.7536(4) 0.1973(6) 0.034(3) Uani 1 1 d . . . C184 C 0.6548(7) 0.7138(4) 0.2072(8) 0.052(3) Uani 1 1 d . . . H184 H 0.6998 0.7132 0.1978 0.063 Uiso 1 1 calc R . . C185 C 0.6235(7) 0.6754(4) 0.2335(7) 0.050(3) Uani 1 1 d . . . H185 H 0.6440 0.6427 0.2473 0.060 Uiso 1 1 calc R . . N191 N 0.5645(5) 0.8380(3) 0.1873(5) 0.030(2) Uani 1 1 d . . . C192 C 0.6119(6) 0.8049(4) 0.1739(6) 0.031(2) Uani 1 1 d . . . C193 C 0.6608(6) 0.8197(4) 0.1377(6) 0.039(3) Uani 1 1 d . . . H193 H 0.6927 0.7961 0.1277 0.047 Uiso 1 1 calc R . . C194 C 0.6620(7) 0.8689(4) 0.1169(7) 0.045(3) Uani 1 1 d . . . H194 H 0.6956 0.8800 0.0937 0.054 Uiso 1 1 calc R . . C195 C 0.6132(6) 0.9023(4) 0.1306(7) 0.043(3) Uani 1 1 d . . . H195 H 0.6133 0.9365 0.1170 0.052 Uiso 1 1 calc R . . C196 C 0.5640(6) 0.8851(4) 0.1643(6) 0.038(3) Uani 1 1 d . . . H196 H 0.5292 0.9077 0.1711 0.046 Uiso 1 1 calc R . . Er2 Er 0.00773(3) 0.995192(15) 0.22597(3) 0.02509(13) Uani 1 1 d . . . B2 B 0.0384(7) 1.1415(5) 0.2164(8) 0.046(4) Uani 1 1 d . . . H2A H 0.0267 1.1775 0.2118 0.055 Uiso 1 1 calc R . . H2B H 0.0914 1.1371 0.2215 0.055 Uiso 1 1 calc R . . C201 C -0.2165(6) 1.0557(4) 0.2212(6) 0.027(2) Uani 1 1 d . . . C202 C -0.1943(6) 1.1034(4) 0.2147(7) 0.043(3) Uani 1 1 d . . . H202 H -0.1464 1.1086 0.2125 0.052 Uiso 1 1 calc R . . C203 C -0.2392(6) 1.1443(4) 0.2114(7) 0.042(3) Uani 1 1 d . . . H203 H -0.2236 1.1768 0.2045 0.050 Uiso 1 1 calc R . . C204 C -0.3079(6) 1.1369(4) 0.2183(7) 0.040(3) Uani 1 1 d . . . H204 H -0.3391 1.1644 0.2175 0.048 Uiso 1 1 calc R . . C205 C -0.3299(6) 1.0892(4) 0.2263(7) 0.051(3) Uani 1 1 d . . . H205 H -0.3768 1.0841 0.2309 0.061 Uiso 1 1 calc R . . C206 C -0.2854(6) 1.0484(4) 0.2278(7) 0.044(3) Uani 1 1 d . . . H206 H -0.3016 1.0158 0.2334 0.053 Uiso 1 1 calc R . . C212 C -0.1648(6) 1.0139(4) 0.2256(6) 0.029(2) Uani 1 1 d . . . O212 O -0.1077(4) 1.0259(2) 0.2092(4) 0.0310(16) Uani 1 1 d . . . C213 C -0.1732(6) 0.9647(3) 0.2494(6) 0.027(2) Uani 1 1 d . . . H213 H -0.2162 0.9575 0.2608 0.033 Uiso 1 1 calc R . . C214 C -0.1220(6) 0.9262(3) 0.2571(6) 0.027(2) Uani 1 1 d . . . O215 O -0.0663(4) 0.9301(2) 0.2371(4) 0.0281(16) Uani 1 1 d . . . C221 C -0.1292(6) 0.8775(4) 0.2939(6) 0.030(2) Uani 1 1 d . . . C222 C -0.0727(6) 0.8400(4) 0.3073(6) 0.038(3) Uani 1 1 d . . . H222 H -0.0333 0.8468 0.2900 0.046 Uiso 1 1 calc R . . C223 C -0.0717(7) 0.7949(4) 0.3436(7) 0.051(3) Uani 1 1 d . . . H223 H -0.0320 0.7712 0.3529 0.062 Uiso 1 1 calc R . . C224 C -0.1310(7) 0.7847(4) 0.3666(7) 0.049(3) Uani 1 1 d . . . H224 H -0.1321 0.7537 0.3919 0.059 Uiso 1 1 calc R . . C225 C -0.1874(6) 0.8189(4) 0.3531(7) 0.041(3) Uani 1 1 d . . . H225 H -0.2288 0.8107 0.3666 0.049 Uiso 1 1 calc R . . C226 C -0.1857(6) 0.8654(4) 0.3200(6) 0.037(3) Uani 1 1 d . . . H226 H -0.2237 0.8894 0.3150 0.045 Uiso 1 1 calc R . . C231 C 0.1434(6) 0.8531(4) 0.2205(6) 0.031(2) Uani 1 1 d . . . C232 C 0.0766(6) 0.8241(4) 0.1828(7) 0.044(3) Uani 1 1 d . . . H232 H 0.0288 0.8374 0.1771 0.053 Uiso 1 1 calc R . . C233 C 0.0781(7) 0.7767(4) 0.1535(8) 0.056(4) Uani 1 1 d . . . H233 H 0.0319 0.7577 0.1271 0.068 Uiso 1 1 calc R . . C234 C 0.1475(8) 0.7576(4) 0.1632(8) 0.058(4) Uani 1 1 d . . . H234 H 0.1487 0.7255 0.1410 0.070 Uiso 1 1 calc R . . C235 C 0.2162(7) 0.7840(4) 0.2047(7) 0.046(3) Uani 1 1 d . . . H235 H 0.2643 0.7693 0.2140 0.055 Uiso 1 1 calc R . . C236 C 0.2135(6) 0.8317(4) 0.2322(7) 0.042(3) Uani 1 1 d . . . H236 H 0.2601 0.8503 0.2594 0.050 Uiso 1 1 calc R . . O241 O 0.0678(4) 0.9208(2) 0.2250(4) 0.0293(16) Uani 1 1 d . . . C242 C 0.1360(6) 0.9060(4) 0.2437(6) 0.029(2) Uani 1 1 d . . . C243 C 0.2013(6) 0.9361(4) 0.2815(6) 0.034(3) Uani 1 1 d . . . H243 H 0.2509 0.9209 0.3026 0.041 Uiso 1 1 calc R . . C244 C 0.1979(6) 0.9875(4) 0.2900(6) 0.030(2) Uani 1 1 d . . . O245 O 0.1342(4) 1.0113(2) 0.2641(4) 0.0296(16) Uani 1 1 d . . . C251 C 0.2691(6) 1.0190(3) 0.3295(6) 0.026(2) Uani 1 1 d . . . C252 C 0.2619(6) 1.0684(4) 0.3440(6) 0.035(3) Uani 1 1 d . . . H252 H 0.2116 1.0820 0.3265 0.041 Uiso 1 1 calc R . . C253 C 0.3259(6) 1.0991(4) 0.3834(6) 0.037(3) Uani 1 1 d . . . H253 H 0.3191 1.1333 0.3923 0.044 Uiso 1 1 calc R . . C254 C 0.3987(7) 1.0802(4) 0.4092(7) 0.049(3) Uani 1 1 d . . . H254 H 0.4427 1.1012 0.4357 0.059 Uiso 1 1 calc R . . C255 C 0.4082(6) 1.0304(4) 0.3966(7) 0.042(3) Uani 1 1 d . . . H255 H 0.4587 1.0168 0.4153 0.051 Uiso 1 1 calc R . . C256 C 0.3434(5) 1.0002(4) 0.3563(6) 0.034(3) Uani 1 1 d . . . H256 H 0.3501 0.9661 0.3469 0.041 Uiso 1 1 calc R . . N261 N -0.0205(4) 1.1143(3) 0.1359(5) 0.033(2) Uani 1 1 d . . . N262 N -0.0215(5) 1.0651(3) 0.1245(5) 0.032(2) Uani 1 1 d . . . C263 C -0.0720(5) 1.0558(4) 0.0425(6) 0.031(2) Uani 1 1 d . . . C264 C -0.1019(6) 1.1002(4) 0.0011(7) 0.041(3) Uani 1 1 d . . . H264 H -0.1383 1.1044 -0.0567 0.049 Uiso 1 1 calc R . . C265 C -0.0686(6) 1.1367(4) 0.0602(7) 0.041(3) Uani 1 1 d . . . H265 H -0.0771 1.1715 0.0507 0.050 Uiso 1 1 calc R . . N271 N -0.0576(5) 0.9696(3) 0.0740(5) 0.032(2) Uani 1 1 d . . . C272 C -0.0857(6) 1.0048(4) 0.0133(6) 0.029(2) Uani 1 1 d . . . C273 C -0.1268(6) 0.9924(4) -0.0735(6) 0.040(3) Uani 1 1 d . . . H273 H -0.1475 1.0178 -0.1154 0.048 Uiso 1 1 calc R . . C274 C -0.1365(6) 0.9434(4) -0.0967(7) 0.042(3) Uani 1 1 d . . . H274 H -0.1632 0.9346 -0.1552 0.051 Uiso 1 1 calc R . . C275 C -0.1074(5) 0.9065(4) -0.0352(6) 0.036(3) Uani 1 1 d . . . H275 H -0.1135 0.8722 -0.0499 0.044 Uiso 1 1 calc R . . C276 C -0.0698(6) 0.9216(4) 0.0469(7) 0.041(3) Uani 1 1 d . . . H276 H -0.0504 0.8964 0.0892 0.049 Uiso 1 1 calc R . . N281 N 0.0342(5) 1.1197(3) 0.2975(6) 0.038(2) Uani 1 1 d . . . N282 N 0.0406(4) 1.0711(3) 0.3155(5) 0.030(2) Uani 1 1 d . . . C283 C 0.0579(5) 1.0671(4) 0.3996(6) 0.029(2) Uani 1 1 d . . . C284 C 0.0601(7) 1.1141(4) 0.4344(7) 0.046(3) Uani 1 1 d . . . H284 H 0.0702 1.1221 0.4913 0.056 Uiso 1 1 calc R . . C285 C 0.0441(6) 1.1468(4) 0.3666(8) 0.043(3) Uani 1 1 d . . . H285 H 0.0408 1.1821 0.3688 0.051 Uiso 1 1 calc R . . N291 N 0.0554(5) 0.9796(3) 0.3826(5) 0.032(2) Uani 1 1 d . . . C292 C 0.0687(6) 1.0180(4) 0.4369(6) 0.031(2) Uani 1 1 d . . . C293 C 0.0926(6) 1.0108(4) 0.5225(7) 0.040(3) Uani 1 1 d . . . H293 H 0.1046 1.0385 0.5601 0.048 Uiso 1 1 calc R . . C294 C 0.0988(6) 0.9631(4) 0.5530(7) 0.044(3) Uani 1 1 d . . . H294 H 0.1115 0.9578 0.6114 0.053 Uiso 1 1 calc R . . C295 C 0.0868(6) 0.9234(4) 0.5001(7) 0.041(3) Uani 1 1 d . . . H295 H 0.0932 0.8902 0.5207 0.049 Uiso 1 1 calc R . . C296 C 0.0648(6) 0.9338(4) 0.4147(6) 0.035(3) Uani 1 1 d . . . H296 H 0.0559 0.9066 0.3769 0.042 Uiso 1 1 calc R . . Cl1 Cl 0.4967(2) 1.01564(14) 0.0777(3) 0.0850(12) Uani 1 1 d . . . C500 C 0.4549(16) 0.9720(9) -0.015(2) 0.084(10) Uani 0.50 1 d P . . H50A H 0.4632 0.9370 0.0044 0.100 Uiso 0.50 1 calc PR . . H50B H 0.3986 0.9778 -0.0485 0.100 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 Er1 0.0279(3) 0.0227(3) 0.0255(3) -0.0012(2) 0.0109(2) -0.0012(2) B1 0.059(9) 0.009(6) 0.046(8) 0.005(5) 0.032(7) -0.007(6) C101 0.023(5) 0.019(5) 0.027(6) 0.002(4) 0.008(5) 0.005(4) C102 0.018(5) 0.034(6) 0.045(7) 0.001(5) 0.013(5) 0.001(5) C103 0.028(6) 0.035(7) 0.052(8) -0.005(5) 0.016(6) 0.010(5) C104 0.025(6) 0.032(7) 0.048(7) 0.011(5) 0.007(5) 0.005(5) C105 0.038(7) 0.044(7) 0.026(6) -0.002(5) 0.005(5) 0.004(5) C106 0.042(7) 0.027(6) 0.037(7) 0.005(5) 0.013(6) -0.006(5) O111 0.028(4) 0.024(4) 0.043(4) -0.006(3) 0.009(4) -0.001(3) C112 0.037(6) 0.034(6) 0.025(6) 0.002(5) 0.024(5) -0.007(5) C113 0.022(6) 0.026(6) 0.032(6) -0.008(4) 0.007(5) -0.003(4) C114 0.033(6) 0.029(6) 0.017(5) -0.002(4) 0.009(5) -0.001(5) O115 0.027(4) 0.034(4) 0.026(4) 0.001(3) 0.005(3) 0.000(3) C121 0.030(6) 0.030(6) 0.035(6) -0.006(5) 0.020(5) -0.006(5) C122 0.035(7) 0.029(6) 0.048(7) -0.007(5) 0.013(6) -0.003(5) C123 0.036(7) 0.034(7) 0.055(8) 0.012(6) 0.021(6) 0.002(5) C124 0.053(8) 0.028(7) 0.069(9) -0.007(6) 0.043(7) -0.006(6) C125 0.046(7) 0.032(7) 0.042(7) 0.001(5) 0.022(6) 0.004(5) C126 0.047(7) 0.033(7) 0.039(7) -0.002(5) 0.018(6) -0.006(5) C131 0.032(6) 0.032(6) 0.037(6) 0.011(5) 0.021(5) 0.004(5) C132 0.042(7) 0.028(6) 0.038(7) -0.002(5) 0.014(6) 0.008(5) C133 0.041(7) 0.030(6) 0.038(7) -0.007(5) 0.004(6) -0.010(5) C134 0.046(8) 0.030(7) 0.061(9) 0.005(6) 0.020(7) 0.005(6) C135 0.036(7) 0.050(8) 0.033(7) 0.009(6) 0.005(5) 0.003(6) C136 0.034(7) 0.042(7) 0.031(6) -0.011(5) 0.008(5) 0.005(5) O141 0.027(4) 0.027(4) 0.024(4) -0.004(3) 0.003(3) 0.004(3) C142 0.025(6) 0.031(6) 0.031(6) 0.000(5) 0.014(5) -0.001(5) C143 0.032(6) 0.040(7) 0.037(7) 0.003(5) 0.006(5) 0.002(5) C144 0.027(6) 0.022(6) 0.028(6) -0.004(4) 0.006(5) -0.008(4) O145 0.024(4) 0.034(4) 0.031(4) -0.001(3) 0.001(3) 0.002(3) C151 0.023(6) 0.037(6) 0.033(6) -0.004(5) 0.014(5) -0.005(5) C152 0.033(6) 0.040(7) 0.043(7) -0.003(5) 0.017(6) -0.002(5) C153 0.045(8) 0.036(7) 0.071(9) -0.008(6) 0.020(7) -0.003(6) C154 0.050(8) 0.033(7) 0.042(7) -0.011(5) 0.005(6) -0.016(6) C155 0.050(8) 0.068(9) 0.024(6) -0.012(6) -0.006(6) -0.014(7) C156 0.067(9) 0.037(7) 0.029(6) -0.006(5) 0.000(6) -0.028(6) N161 0.041(5) 0.022(5) 0.028(5) 0.005(4) 0.012(4) 0.003(4) N162 0.034(5) 0.015(4) 0.031(5) -0.002(3) 0.012(4) 0.001(4) C163 0.036(6) 0.024(6) 0.024(6) 0.003(4) 0.007(5) -0.002(5) C164 0.048(7) 0.041(7) 0.025(6) 0.010(5) 0.009(5) -0.003(6) C165 0.055(8) 0.030(6) 0.032(7) 0.000(5) 0.014(6) 0.004(5) N171 0.034(5) 0.036(5) 0.028(5) 0.005(4) 0.018(4) 0.007(4) C172 0.025(6) 0.033(6) 0.028(6) 0.005(5) 0.006(5) 0.000(5) C173 0.040(7) 0.047(7) 0.029(6) 0.004(5) 0.020(5) -0.011(6) C174 0.034(7) 0.061(8) 0.034(7) -0.002(6) 0.022(6) 0.000(6) C175 0.036(7) 0.061(8) 0.049(8) 0.009(6) 0.022(6) 0.011(6) C176 0.027(6) 0.031(6) 0.037(6) 0.007(5) 0.011(5) 0.005(5) N181 0.037(5) 0.034(6) 0.037(5) -0.004(4) 0.017(4) -0.001(4) N182 0.040(5) 0.022(5) 0.035(5) -0.006(4) 0.025(4) -0.004(4) C183 0.038(7) 0.038(7) 0.033(6) -0.007(5) 0.023(5) -0.001(5) C184 0.062(9) 0.034(7) 0.086(10) 0.000(6) 0.055(8) 0.005(6) C185 0.047(8) 0.046(8) 0.061(9) 0.001(6) 0.028(7) 0.014(6) N191 0.032(5) 0.021(5) 0.040(5) -0.006(4) 0.017(4) -0.012(4) C192 0.038(6) 0.034(6) 0.024(5) -0.002(4) 0.017(5) 0.003(5) C193 0.034(6) 0.046(7) 0.040(7) -0.007(5) 0.018(5) -0.003(5) C194 0.056(8) 0.041(7) 0.048(8) 0.005(6) 0.031(6) -0.004(6) C195 0.044(7) 0.048(8) 0.038(7) 0.007(5) 0.019(6) -0.004(6) C196 0.034(6) 0.038(7) 0.035(6) 0.010(5) 0.009(5) 0.009(5) Er2 0.0243(3) 0.0248(3) 0.0269(3) 0.0011(2) 0.0119(2) 0.0007(2) B2 0.035(8) 0.046(9) 0.051(9) -0.001(7) 0.014(7) -0.004(7) C201 0.029(6) 0.030(6) 0.022(5) 0.001(4) 0.013(5) 0.007(5) C202 0.026(6) 0.045(7) 0.054(8) 0.010(6) 0.013(6) 0.001(5) C203 0.052(8) 0.022(6) 0.061(8) 0.001(5) 0.033(7) 0.003(5) C204 0.039(7) 0.043(7) 0.048(7) -0.001(5) 0.027(6) 0.017(6) C205 0.037(7) 0.059(9) 0.066(9) 0.007(7) 0.030(7) 0.009(6) C206 0.035(7) 0.037(7) 0.064(8) 0.008(6) 0.024(6) -0.002(5) C212 0.023(6) 0.037(6) 0.020(5) -0.005(4) 0.002(5) -0.003(5) O212 0.027(4) 0.027(4) 0.043(4) 0.002(3) 0.018(4) 0.001(3) C213 0.031(6) 0.023(6) 0.024(5) 0.001(4) 0.009(5) 0.001(5) C214 0.027(6) 0.028(6) 0.024(6) -0.012(4) 0.010(5) -0.005(5) O215 0.027(4) 0.033(4) 0.028(4) -0.001(3) 0.016(3) 0.001(3) C221 0.029(6) 0.038(6) 0.021(5) 0.000(4) 0.007(5) -0.010(5) C222 0.039(7) 0.043(7) 0.036(7) 0.007(5) 0.020(5) 0.002(5) C223 0.057(8) 0.036(7) 0.055(8) 0.015(6) 0.019(7) 0.012(6) C224 0.076(9) 0.027(7) 0.061(8) 0.002(6) 0.045(8) -0.014(6) C225 0.036(7) 0.048(8) 0.047(7) 0.010(6) 0.025(6) -0.013(6) C226 0.037(7) 0.033(7) 0.047(7) 0.006(5) 0.024(6) 0.006(5) C231 0.039(7) 0.025(6) 0.037(6) 0.001(5) 0.022(5) 0.005(5) C232 0.034(7) 0.033(7) 0.061(8) -0.003(6) 0.018(6) -0.001(5) C233 0.045(8) 0.049(8) 0.071(9) -0.018(7) 0.023(7) -0.009(6) C234 0.070(10) 0.036(8) 0.081(10) -0.008(7) 0.045(9) 0.011(7) C235 0.048(8) 0.033(7) 0.062(8) -0.003(6) 0.028(7) 0.012(6) C236 0.035(7) 0.043(7) 0.048(7) -0.013(6) 0.019(6) 0.000(5) O241 0.021(4) 0.028(4) 0.040(4) -0.001(3) 0.015(3) 0.000(3) C242 0.030(6) 0.030(6) 0.021(5) 0.004(4) 0.007(5) 0.005(5) C243 0.032(6) 0.035(7) 0.036(6) -0.002(5) 0.015(5) 0.011(5) C244 0.034(6) 0.036(6) 0.020(5) 0.002(4) 0.011(5) 0.003(5) O245 0.021(4) 0.031(4) 0.036(4) 0.001(3) 0.012(3) 0.003(3) C251 0.031(6) 0.025(6) 0.028(6) 0.004(4) 0.018(5) -0.003(4) C252 0.019(6) 0.057(8) 0.024(6) -0.006(5) 0.006(5) -0.006(5) C253 0.048(7) 0.028(6) 0.032(6) -0.001(5) 0.016(6) -0.007(5) C254 0.039(7) 0.048(8) 0.050(8) 0.007(6) 0.010(6) -0.014(6) C255 0.023(6) 0.050(8) 0.051(8) 0.003(6) 0.014(6) -0.008(5) C256 0.023(6) 0.036(6) 0.041(6) 0.007(5) 0.011(5) 0.006(5) N261 0.024(5) 0.027(5) 0.041(5) 0.003(4) 0.009(4) -0.005(4) N262 0.033(5) 0.025(5) 0.037(5) 0.011(4) 0.016(4) 0.007(4) C263 0.023(6) 0.035(6) 0.031(6) 0.011(5) 0.007(5) 0.003(5) C264 0.044(7) 0.039(7) 0.040(7) 0.010(5) 0.018(6) 0.004(6) C265 0.047(7) 0.028(6) 0.053(8) 0.018(6) 0.025(6) 0.011(5) N271 0.036(5) 0.034(5) 0.028(5) 0.005(4) 0.017(4) 0.003(4) C272 0.031(6) 0.031(6) 0.026(6) 0.004(5) 0.014(5) 0.005(5) C273 0.024(6) 0.069(9) 0.023(6) 0.007(5) 0.007(5) -0.001(6) C274 0.042(7) 0.056(8) 0.034(7) -0.004(6) 0.021(6) -0.009(6) C275 0.027(6) 0.048(7) 0.033(6) -0.001(5) 0.012(5) 0.002(5) C276 0.026(6) 0.045(7) 0.048(8) -0.001(6) 0.013(6) -0.005(5) N281 0.041(6) 0.022(5) 0.052(6) 0.000(4) 0.021(5) -0.012(4) N282 0.026(5) 0.029(5) 0.044(6) 0.000(4) 0.022(4) -0.004(4) C283 0.028(6) 0.027(6) 0.034(6) -0.003(5) 0.015(5) 0.001(5) C284 0.072(9) 0.037(7) 0.040(7) -0.005(6) 0.034(7) 0.002(6) C285 0.042(7) 0.024(6) 0.064(9) -0.011(6) 0.025(6) -0.004(5) N291 0.030(5) 0.031(5) 0.030(5) 0.005(4) 0.009(4) 0.001(4) C292 0.030(6) 0.033(6) 0.029(6) -0.001(5) 0.012(5) 0.003(5) C293 0.043(7) 0.043(7) 0.034(7) -0.004(5) 0.016(6) -0.001(6) C294 0.046(7) 0.057(8) 0.031(7) -0.005(6) 0.019(6) -0.011(6) C295 0.039(7) 0.045(7) 0.045(7) 0.011(6) 0.024(6) 0.003(6) C296 0.046(7) 0.022(6) 0.036(7) -0.010(5) 0.019(6) -0.006(5) Cl1 0.095(3) 0.065(3) 0.110(3) 0.001(2) 0.059(3) 0.010(2) C500 0.07(2) 0.030(15) 0.17(3) 0.024(18) 0.07(2) 0.017(14) _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 Er1 O145 2.264(6) . ? Er1 O111 2.278(6) . ? Er1 O115 2.286(6) . ? Er1 O141 2.301(6) . ? Er1 N182 2.462(7) . ? Er1 N162 2.469(7) . ? Er1 N171 2.508(8) . ? Er1 N191 2.525(8) . ? B1 N161 1.530(13) . ? B1 N181 1.600(13) . ? C101 C106 1.381(12) . ? C101 C102 1.406(12) . ? C101 C112 1.502(12) . ? C102 C103 1.382(13) . ? C103 C104 1.374(14) . ? C104 C105 1.403(13) . ? C105 C106 1.378(13) . ? O111 C112 1.267(10) . ? C112 C113 1.395(12) . ? C113 C114 1.409(12) . ? C114 O115 1.272(10) . ? C114 C121 1.501(13) . ? C121 C126 1.378(13) . ? C121 C122 1.394(13) . ? C122 C123 1.371(13) . ? C123 C124 1.379(14) . ? C124 C125 1.375(14) . ? C125 C126 1.378(13) . ? C131 C132 1.379(13) . ? C131 C136 1.385(13) . ? C131 C142 1.506(13) . ? C132 C133 1.397(13) . ? C133 C134 1.369(14) . ? C134 C135 1.380(14) . ? C135 C136 1.408(13) . ? O141 C142 1.287(10) . ? C142 C143 1.376(13) . ? C143 C144 1.401(13) . ? C144 O145 1.272(10) . ? C144 C151 1.499(12) . ? C151 C156 1.375(13) . ? C151 C152 1.392(13) . ? C152 C153 1.424(14) . ? C153 C154 1.361(15) . ? C154 C155 1.362(14) . ? C155 C156 1.403(13) . ? N161 C165 1.325(12) . ? N161 N162 1.375(9) . ? N162 C163 1.342(11) . ? C163 C164 1.412(12) . ? C163 C172 1.443(13) . ? C164 C165 1.368(14) . ? N171 C176 1.336(11) . ? N171 C172 1.366(11) . ? C172 C173 1.359(13) . ? C173 C174 1.395(14) . ? C174 C175 1.375(14) . ? C175 C176 1.372(14) . ? N181 C185 1.315(13) . ? N181 N182 1.355(10) . ? N182 C183 1.356(12) . ? C183 C184 1.379(13) . ? C183 C192 1.455(13) . ? C184 C185 1.372(15) . ? N191 C196 1.326(11) . ? N191 C192 1.367(11) . ? C192 C193 1.404(13) . ? C193 C194 1.374(13) . ? C194 C195 1.394(14) . ? C195 C196 1.396(14) . ? Er2 O245 2.263(6) . ? Er2 O212 2.264(6) . ? Er2 O241 2.311(6) . ? Er2 O215 2.316(6) . ? Er2 N262 2.473(7) . ? Er2 N282 2.480(8) . ? Er2 N271 2.486(8) . ? Er2 N291 2.513(8) . ? B2 N261 1.548(14) . ? B2 N281 1.569(15) . ? C201 C202 1.371(13) . ? C201 C206 1.395(13) . ? C201 C212 1.479(13) . ? C202 C203 1.383(13) . ? C203 C204 1.391(14) . ? C204 C205 1.377(14) . ? C205 C206 1.383(14) . ? C212 O212 1.293(11) . ? C212 C213 1.417(12) . ? C213 C214 1.393(12) . ? C214 O215 1.269(10) . ? C214 C221 1.494(13) . ? C221 C226 1.390(13) . ? C221 C222 1.422(13) . ? C222 C223 1.365(13) . ? C223 C224 1.393(15) . ? C224 C225 1.359(14) . ? C225 C226 1.384(13) . ? C231 C232 1.395(13) . ? C231 C236 1.396(13) . ? C231 C242 1.502(13) . ? C232 C233 1.378(14) . ? C233 C234 1.368(15) . ? C234 C235 1.389(15) . ? C235 C236 1.379(13) . ? O241 C242 1.268(10) . ? C242 C243 1.393(13) . ? C243 C244 1.391(13) . ? C244 O245 1.275(11) . ? C244 C251 1.496(13) . ? C251 C252 1.368(13) . ? C251 C256 1.388(13) . ? C252 C253 1.387(12) . ? C253 C254 1.366(14) . ? C254 C255 1.382(14) . ? C255 C256 1.391(13) . ? N261 N262 1.337(10) . ? N261 C265 1.376(12) . ? N262 C263 1.355(12) . ? C263 C264 1.382(13) . ? C263 C272 1.446(13) . ? C264 C265 1.363(14) . ? N271 C272 1.347(11) . ? N271 C276 1.358(12) . ? C272 C273 1.410(13) . ? C273 C274 1.367(14) . ? C274 C275 1.387(14) . ? C275 C276 1.354(13) . ? N281 N282 1.336(10) . ? N281 C285 1.352(12) . ? N282 C283 1.361(12) . ? C283 C284 1.397(13) . ? C283 C292 1.444(13) . ? C284 C285 1.398(14) . ? N291 C296 1.332(11) . ? N291 C292 1.349(12) . ? C292 C293 1.374(13) . ? C293 C294 1.373(14) . ? C294 C295 1.364(14) . ? C295 C296 1.390(13) . ? Cl1 C500 1.75(3) 3_675 ? Cl1 C500 1.88(3) . ? C500 Cl1 1.75(3) 3_675 ? 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 O145 Er1 O111 143.8(2) . . ? O145 Er1 O115 144.4(2) . . ? O111 Er1 O115 71.7(2) . . ? O145 Er1 O141 72.5(2) . . ? O111 Er1 O141 143.7(2) . . ? O115 Er1 O141 72.0(2) . . ? O145 Er1 N182 78.9(2) . . ? O111 Er1 N182 73.4(2) . . ? O115 Er1 N182 125.4(2) . . ? O141 Er1 N182 131.1(2) . . ? O145 Er1 N162 80.4(2) . . ? O111 Er1 N162 71.2(2) . . ? O115 Er1 N162 126.8(2) . . ? O141 Er1 N162 133.4(2) . . ? N182 Er1 N162 77.0(3) . . ? O145 Er1 N171 99.9(3) . . ? O111 Er1 N171 88.3(2) . . ? O115 Er1 N171 77.0(2) . . ? O141 Er1 N171 82.8(2) . . ? N182 Er1 N171 141.6(3) . . ? N162 Er1 N171 65.1(3) . . ? O145 Er1 N191 98.7(2) . . ? O111 Er1 N191 90.7(3) . . ? O115 Er1 N191 73.9(2) . . ? O141 Er1 N191 80.1(2) . . ? N182 Er1 N191 65.9(3) . . ? N162 Er1 N191 142.2(3) . . ? N171 Er1 N191 149.6(3) . . ? N161 B1 N181 110.2(8) . . ? C106 C101 C102 119.3(9) . . ? C106 C101 C112 123.7(9) . . ? C102 C101 C112 117.0(8) . . ? C103 C102 C101 119.9(9) . . ? C104 C103 C102 120.5(10) . . ? C103 C104 C105 119.6(9) . . ? C106 C105 C104 120.0(10) . . ? C105 C106 C101 120.5(10) . . ? C112 O111 Er1 138.6(6) . . ? O111 C112 C113 124.0(9) . . ? O111 C112 C101 115.8(8) . . ? C113 C112 C101 120.3(9) . . ? C112 C113 C114 122.8(9) . . ? O115 C114 C113 122.5(9) . . ? O115 C114 C121 116.5(8) . . ? C113 C114 C121 120.9(9) . . ? C114 O115 Er1 138.3(6) . . ? C126 C121 C122 118.1(9) . . ? C126 C121 C114 124.3(10) . . ? C122 C121 C114 117.6(9) . . ? C123 C122 C121 120.5(10) . . ? C122 C123 C124 120.0(10) . . ? C125 C124 C123 120.7(10) . . ? C124 C125 C126 118.7(11) . . ? C125 C126 C121 122.0(10) . . ? C132 C131 C136 119.3(9) . . ? C132 C131 C142 119.0(9) . . ? C136 C131 C142 121.7(10) . . ? C131 C132 C133 120.5(10) . . ? C134 C133 C132 120.0(10) . . ? C133 C134 C135 120.6(10) . . ? C134 C135 C136 119.2(10) . . ? C131 C136 C135 120.3(10) . . ? C142 O141 Er1 137.2(6) . . ? O141 C142 C143 123.4(9) . . ? O141 C142 C131 115.7(8) . . ? C143 C142 C131 120.9(9) . . ? C142 C143 C144 123.1(9) . . ? O145 C144 C143 124.8(9) . . ? O145 C144 C151 116.1(8) . . ? C143 C144 C151 119.2(9) . . ? C144 O145 Er1 137.7(6) . . ? C156 C151 C152 119.2(9) . . ? C156 C151 C144 123.3(9) . . ? C152 C151 C144 117.5(9) . . ? C151 C152 C153 119.1(10) . . ? C154 C153 C152 120.0(11) . . ? C155 C154 C153 121.1(10) . . ? C154 C155 C156 119.5(11) . . ? C151 C156 C155 121.0(11) . . ? C165 N161 N162 108.9(8) . . ? C165 N161 B1 128.7(9) . . ? N162 N161 B1 121.9(8) . . ? C163 N162 N161 106.3(7) . . ? C163 N162 Er1 117.5(6) . . ? N161 N162 Er1 129.7(6) . . ? N162 C163 C164 110.5(9) . . ? N162 C163 C172 119.1(8) . . ? C164 C163 C172 130.4(10) . . ? C165 C164 C163 103.3(9) . . ? N161 C165 C164 111.1(9) . . ? C176 N171 C172 118.9(9) . . ? C176 N171 Er1 121.4(7) . . ? C172 N171 Er1 118.5(6) . . ? C173 C172 N171 121.4(10) . . ? C173 C172 C163 123.5(10) . . ? N171 C172 C163 115.0(9) . . ? C172 C173 C174 119.5(10) . . ? C175 C174 C173 118.7(10) . . ? C176 C175 C174 119.4(11) . . ? N171 C176 C175 122.0(10) . . ? C185 N181 N182 112.3(9) . . ? C185 N181 B1 128.5(9) . . ? N182 N181 B1 119.2(8) . . ? N181 N182 C183 103.7(8) . . ? N181 N182 Er1 131.4(6) . . ? C183 N182 Er1 116.2(6) . . ? N182 C183 C184 111.3(9) . . ? N182 C183 C192 119.1(9) . . ? C184 C183 C192 129.6(10) . . ? C185 C184 C183 104.6(10) . . ? N181 C185 C184 108.2(10) . . ? C196 N191 C192 119.0(9) . . ? C196 N191 Er1 123.4(7) . . ? C192 N191 Er1 117.3(6) . . ? N191 C192 C193 121.5(9) . . ? N191 C192 C183 115.4(9) . . ? C193 C192 C183 123.1(9) . . ? C194 C193 C192 119.0(10) . . ? C193 C194 C195 118.9(11) . . ? C194 C195 C196 119.4(10) . . ? N191 C196 C195 122.0(10) . . ? O245 Er2 O212 146.5(2) . . ? O245 Er2 O241 72.1(2) . . ? O212 Er2 O241 141.2(2) . . ? O245 Er2 O215 137.7(2) . . ? O212 Er2 O215 71.5(2) . . ? O241 Er2 O215 71.1(2) . . ? O245 Er2 N262 86.6(2) . . ? O212 Er2 N262 74.3(2) . . ? O241 Er2 N262 127.4(2) . . ? O215 Er2 N262 132.8(2) . . ? O245 Er2 N282 73.4(2) . . ? O212 Er2 N282 75.2(2) . . ? O241 Er2 N282 136.6(2) . . ? O215 Er2 N282 124.3(2) . . ? N262 Er2 N282 75.1(3) . . ? O245 Er2 N271 109.8(2) . . ? O212 Er2 N271 87.6(2) . . ? O241 Er2 N271 76.8(2) . . ? O215 Er2 N271 80.9(2) . . ? N262 Er2 N271 66.1(3) . . ? N282 Er2 N271 140.6(3) . . ? O245 Er2 N291 83.2(2) . . ? O212 Er2 N291 93.9(2) . . ? O241 Er2 N291 85.5(2) . . ? O215 Er2 N291 74.0(2) . . ? N262 Er2 N291 140.1(3) . . ? N282 Er2 N291 65.1(3) . . ? N271 Er2 N291 152.9(3) . . ? N261 B2 N281 109.8(9) . . ? C202 C201 C206 118.7(9) . . ? C202 C201 C212 119.2(9) . . ? C206 C201 C212 122.0(9) . . ? C201 C202 C203 122.4(10) . . ? C202 C203 C204 118.8(10) . . ? C205 C204 C203 119.2(10) . . ? C204 C205 C206 121.6(10) . . ? C205 C206 C201 119.3(10) . . ? O212 C212 C213 121.2(9) . . ? O212 C212 C201 114.5(9) . . ? C213 C212 C201 124.3(9) . . ? C212 O212 Er2 139.5(6) . . ? C214 C213 C212 123.5(10) . . ? O215 C214 C213 124.1(9) . . ? O215 C214 C221 116.2(9) . . ? C213 C214 C221 119.7(9) . . ? C214 O215 Er2 135.2(6) . . ? C226 C221 C222 115.5(9) . . ? C226 C221 C214 125.5(9) . . ? C222 C221 C214 118.9(9) . . ? C223 C222 C221 124.0(11) . . ? C222 C223 C224 117.5(11) . . ? C225 C224 C223 120.7(10) . . ? C224 C225 C226 121.1(10) . . ? C225 C226 C221 121.0(10) . . ? C232 C231 C236 117.9(9) . . ? C232 C231 C242 118.6(9) . . ? C236 C231 C242 123.5(10) . . ? C233 C232 C231 121.8(10) . . ? C234 C233 C232 118.6(11) . . ? C233 C234 C235 121.7(11) . . ? C236 C235 C234 118.8(11) . . ? C235 C236 C231 121.0(10) . . ? C242 O241 Er2 137.1(6) . . ? O241 C242 C243 123.6(9) . . ? O241 C242 C231 116.0(9) . . ? C243 C242 C231 120.3(9) . . ? C242 C243 C244 123.5(9) . . ? O245 C244 C243 122.9(9) . . ? O245 C244 C251 114.8(9) . . ? C243 C244 C251 122.3(9) . . ? C244 O245 Er2 138.4(6) . . ? C252 C251 C256 117.6(9) . . ? C252 C251 C244 119.2(9) . . ? C256 C251 C244 123.1(9) . . ? C251 C252 C253 121.9(10) . . ? C254 C253 C252 119.9(10) . . ? C253 C254 C255 119.7(10) . . ? C254 C255 C256 119.6(10) . . ? C255 C256 C251 121.2(10) . . ? N262 N261 C265 109.3(8) . . ? N262 N261 B2 123.9(9) . . ? C265 N261 B2 125.7(9) . . ? N261 N262 C263 107.2(8) . . ? N261 N262 Er2 131.4(6) . . ? C263 N262 Er2 116.8(6) . . ? N262 C263 C264 109.6(9) . . ? N262 C263 C272 118.9(8) . . ? C264 C263 C272 131.6(10) . . ? C265 C264 C263 106.0(10) . . ? C264 C265 N261 107.9(9) . . ? C272 N271 C276 116.4(9) . . ? C272 N271 Er2 119.1(6) . . ? C276 N271 Er2 124.4(7) . . ? N271 C272 C273 121.6(9) . . ? N271 C272 C263 116.1(9) . . ? C273 C272 C263 122.3(9) . . ? C274 C273 C272 119.1(10) . . ? C273 C274 C275 120.1(10) . . ? C276 C275 C274 117.0(11) . . ? C275 C276 N271 125.7(11) . . ? N282 N281 C285 110.7(9) . . ? N282 N281 B2 122.7(9) . . ? C285 N281 B2 124.5(9) . . ? N281 N282 C283 106.7(8) . . ? N281 N282 Er2 133.1(7) . . ? C283 N282 Er2 119.3(6) . . ? N282 C283 C284 110.2(9) . . ? N282 C283 C292 118.7(9) . . ? C284 C283 C292 131.1(10) . . ? C283 C284 C285 104.2(10) . . ? N281 C285 C284 108.2(9) . . ? C296 N291 C292 117.5(9) . . ? C296 N291 Er2 122.0(7) . . ? C292 N291 Er2 120.4(6) . . ? N291 C292 C293 121.9(10) . . ? N291 C292 C283 115.7(9) . . ? C293 C292 C283 122.3(10) . . ? C292 C293 C294 119.0(10) . . ? C295 C294 C293 120.4(11) . . ? C294 C295 C296 116.9(10) . . ? N291 C296 C295 124.1(9) . . ? C500 Cl1 C500 73.7(13) 3_675 . ? Cl1 C500 Cl1 106.3(13) 3_675 . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 27.59 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 1.419 _refine_diff_density_min -2.167 _refine_diff_density_rms 0.186 #=END data_imw22m _database_code_depnum_ccdc_archive 'CCDC 229467' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46.25 H36.50 B Cl0.50 N6 O4 Pr' _chemical_formula_sum 'C46.25 H36.50 B Cl0.50 N6 O4 Pr' _chemical_formula_weight 909.76 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' B B 0.0013 0.0007 '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' Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.2028(12) _cell_length_b 26.5714(17) _cell_length_c 18.1524(12) _cell_angle_alpha 90.00 _cell_angle_beta 117.7670(10) _cell_angle_gamma 90.00 _cell_volume 8195.6(9) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 15555 _cell_measurement_theta_min 4.488 _cell_measurement_theta_max 53.111 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.475 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3684 _exptl_absorpt_coefficient_mu 1.274 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.6432 _exptl_absorpt_correction_T_max 0.7848 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 91231 _diffrn_reflns_av_R_equivalents 0.0753 _diffrn_reflns_av_sigmaI/netI 0.0815 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.20 _diffrn_reflns_theta_max 27.53 _reflns_number_total 18617 _reflns_number_gt 12728 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0306P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18617 _refine_ls_number_parameters 1087 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0743 _refine_ls_R_factor_gt 0.0385 _refine_ls_wR_factor_ref 0.0733 _refine_ls_wR_factor_gt 0.0667 _refine_ls_goodness_of_fit_ref 0.880 _refine_ls_restrained_S_all 0.880 _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 C113 C 0.81611(19) 0.35497(12) 0.2638(2) 0.0274(8) Uani 1 1 d . . . H113 H 0.7686 0.3676 0.2610 0.033 Uiso 1 1 calc R . . Pr1 Pr 1.007018(11) 0.302923(7) 0.266974(11) 0.02134(5) Uani 1 1 d . . . B1 B 0.9894(3) 0.15410(16) 0.2376(3) 0.0345(10) Uani 1 1 d . . . H1A H 1.0504(18) 0.1568(11) 0.2437(18) 0.031(9) Uiso 1 1 d . . . H1B H 0.9658(17) 0.1138(11) 0.2292(17) 0.026(8) Uiso 1 1 d . . . C101 C 0.76505(19) 0.26780(12) 0.26516(19) 0.0240(7) Uani 1 1 d . . . C102 C 0.7642(2) 0.21819(13) 0.2390(2) 0.0299(8) Uani 1 1 d . . . H102 H 0.8020 0.2078 0.2222 0.036 Uiso 1 1 calc R . . C103 C 0.7091(2) 0.18406(13) 0.2372(2) 0.0333(9) Uani 1 1 d . . . H103 H 0.7085 0.1507 0.2181 0.040 Uiso 1 1 calc R . . C104 C 0.6544(2) 0.19846(14) 0.2634(2) 0.0344(9) Uani 1 1 d . . . H104 H 0.6169 0.1749 0.2627 0.041 Uiso 1 1 calc R . . C105 C 0.6551(2) 0.24692(14) 0.2903(2) 0.0353(9) Uani 1 1 d . . . H105 H 0.6183 0.2567 0.3087 0.042 Uiso 1 1 calc R . . C106 C 0.70968(19) 0.28181(13) 0.2907(2) 0.0299(8) Uani 1 1 d . . . H106 H 0.7090 0.3154 0.3084 0.036 Uiso 1 1 calc R . . O111 O 0.88466(13) 0.28169(8) 0.26379(14) 0.0281(5) Uani 1 1 d . . . C112 C 0.82616(18) 0.30279(12) 0.26530(19) 0.0233(7) Uani 1 1 d . . . C114 C 0.87178(19) 0.38966(12) 0.26618(19) 0.0228(7) Uani 1 1 d . . . O115 O 0.93810(13) 0.37675(8) 0.27294(14) 0.0278(5) Uani 1 1 d . . . C121 C 0.85651(19) 0.44527(12) 0.26229(19) 0.0241(7) Uani 1 1 d . . . C122 C 0.9166(2) 0.47722(13) 0.2705(2) 0.0363(9) Uani 1 1 d . . . H122 H 0.9646 0.4636 0.2763 0.044 Uiso 1 1 calc R . . C123 C 0.9071(2) 0.52907(14) 0.2704(2) 0.0446(10) Uani 1 1 d . . . H123 H 0.9489 0.5507 0.2766 0.054 Uiso 1 1 calc R . . C124 C 0.8379(2) 0.54899(13) 0.2614(2) 0.0375(9) Uani 1 1 d . . . H124 H 0.8316 0.5845 0.2614 0.045 Uiso 1 1 calc R . . C125 C 0.7783(2) 0.51795(13) 0.2525(2) 0.0375(9) Uani 1 1 d . . . H125 H 0.7302 0.5318 0.2461 0.045 Uiso 1 1 calc R . . C126 C 0.7871(2) 0.46627(13) 0.2525(2) 0.0345(9) Uani 1 1 d . . . H126 H 0.7447 0.4450 0.2458 0.041 Uiso 1 1 calc R . . C131 C 1.1678(2) 0.43889(12) 0.2681(2) 0.0274(8) Uani 1 1 d . . . C132 C 1.1378(2) 0.47261(13) 0.3057(2) 0.0344(9) Uani 1 1 d . . . H132 H 1.1078 0.4604 0.3313 0.041 Uiso 1 1 calc R . . C133 C 1.1519(2) 0.52351(14) 0.3056(3) 0.0428(10) Uani 1 1 d . . . H133 H 1.1327 0.5461 0.3325 0.051 Uiso 1 1 calc R . . C134 C 1.1937(2) 0.54182(14) 0.2665(2) 0.0403(10) Uani 1 1 d . . . H134 H 1.2014 0.5770 0.2645 0.048 Uiso 1 1 calc R . . C135 C 1.2239(2) 0.50903(14) 0.2308(2) 0.0389(9) Uani 1 1 d . . . H135 H 1.2542 0.5215 0.2056 0.047 Uiso 1 1 calc R . . C136 C 1.2109(2) 0.45797(13) 0.2307(2) 0.0343(9) Uani 1 1 d . . . H136 H 1.2316 0.4357 0.2050 0.041 Uiso 1 1 calc R . . O141 O 1.09008(13) 0.37371(8) 0.28072(14) 0.0314(6) Uani 1 1 d . . . C142 C 1.14838(19) 0.38418(12) 0.2679(2) 0.0261(8) Uani 1 1 d . . . C143 C 1.1947(2) 0.34768(13) 0.2563(2) 0.0295(8) Uani 1 1 d . . . H143 H 1.2378(16) 0.3593(10) 0.2504(17) 0.014(8) Uiso 1 1 d . . . C144 C 1.18175(19) 0.29587(12) 0.25597(19) 0.0260(8) Uani 1 1 d . . . O145 O 1.12332(13) 0.27639(8) 0.26127(14) 0.0279(5) Uani 1 1 d . . . C151 C 1.23925(19) 0.25928(12) 0.25091(19) 0.0264(8) Uani 1 1 d . . . C152 C 1.2395(2) 0.21011(12) 0.2757(2) 0.0304(8) Uani 1 1 d . . . H152 H 1.2042 0.2002 0.2961 0.037 Uiso 1 1 calc R . . C153 C 1.2908(2) 0.17512(14) 0.2710(2) 0.0371(9) Uani 1 1 d . . . H153 H 1.2910 0.1415 0.2891 0.044 Uiso 1 1 calc R . . C154 C 1.3414(2) 0.18885(14) 0.2403(2) 0.0409(10) Uani 1 1 d . . . H154 H 1.3765 0.1649 0.2369 0.049 Uiso 1 1 calc R . . C155 C 1.3409(2) 0.23773(15) 0.2146(2) 0.0467(11) Uani 1 1 d . . . H155 H 1.3752 0.2472 0.1926 0.056 Uiso 1 1 calc R . . C156 C 1.2909(2) 0.27301(14) 0.2204(2) 0.0368(9) Uani 1 1 d . . . H156 H 1.2919 0.3067 0.2036 0.044 Uiso 1 1 calc R . . N161 N 0.99741(16) 0.17383(10) 0.32201(17) 0.0279(7) Uani 1 1 d . . . N162 N 1.02596(15) 0.22028(10) 0.35123(16) 0.0251(6) Uani 1 1 d . . . C163 C 1.02911(19) 0.22369(13) 0.4267(2) 0.0287(8) Uani 1 1 d . . . C164 C 1.0036(2) 0.17920(14) 0.4466(2) 0.0395(10) Uani 1 1 d . . . H164 H 1.0006 0.1715 0.4961 0.047 Uiso 1 1 calc R . . C165 C 0.9837(2) 0.14896(14) 0.3786(2) 0.0392(10) Uani 1 1 d . . . H165 H 0.9634 0.1157 0.3724 0.047 Uiso 1 1 calc R . . N171 N 1.05913(16) 0.31088(10) 0.42839(16) 0.0270(7) Uani 1 1 d . . . C172 C 1.05285(19) 0.27139(13) 0.4718(2) 0.0280(8) Uani 1 1 d . . . C173 C 1.0658(2) 0.27682(16) 0.5539(2) 0.0397(10) Uani 1 1 d . . . H173 H 1.0604 0.2488 0.5834 0.048 Uiso 1 1 calc R . . C174 C 1.0864(2) 0.32335(16) 0.5913(2) 0.0437(10) Uani 1 1 d . . . H174 H 1.0950 0.3277 0.6469 0.052 Uiso 1 1 calc R . . C175 C 1.0944(2) 0.36331(15) 0.5482(2) 0.0375(9) Uani 1 1 d . . . H175 H 1.1100 0.3955 0.5735 0.045 Uiso 1 1 calc R . . C176 C 1.0794(2) 0.35563(14) 0.4668(2) 0.0343(9) Uani 1 1 d . . . H176 H 1.0836 0.3836 0.4365 0.041 Uiso 1 1 calc R . . N181 N 0.92903(17) 0.18608(10) 0.16434(18) 0.0305(7) Uani 1 1 d . . . N182 N 0.94299(16) 0.23482(10) 0.15288(17) 0.0277(7) Uani 1 1 d . . . C183 C 0.8815(2) 0.24972(13) 0.0809(2) 0.0293(8) Uani 1 1 d . . . C184 C 0.8275(2) 0.21052(14) 0.0460(2) 0.0416(10) Uani 1 1 d . . . H184 H 0.7793 0.2109 -0.0042 0.050 Uiso 1 1 calc R . . C185 C 0.8603(2) 0.17125(14) 0.1011(2) 0.0434(10) Uani 1 1 d . . . H185 H 0.8377 0.1387 0.0952 0.052 Uiso 1 1 calc R . . N191 N 0.92872(16) 0.33411(10) 0.11025(17) 0.0282(7) Uani 1 1 d . . . C192 C 0.8790(2) 0.30143(13) 0.0522(2) 0.0285(8) Uani 1 1 d . . . C193 C 0.8282(2) 0.31680(14) -0.0289(2) 0.0363(9) Uani 1 1 d . . . H193 H 0.7937 0.2933 -0.0686 0.044 Uiso 1 1 calc R . . C194 C 0.8287(2) 0.36618(14) -0.0504(2) 0.0397(10) Uani 1 1 d . . . H194 H 0.7946 0.3772 -0.1054 0.048 Uiso 1 1 calc R . . C195 C 0.8788(2) 0.39966(14) 0.0081(2) 0.0374(9) Uani 1 1 d . . . H195 H 0.8798 0.4340 -0.0058 0.045 Uiso 1 1 calc R . . C196 C 0.9276(2) 0.38219(13) 0.0876(2) 0.0354(9) Uani 1 1 d . . . H196 H 0.9620 0.4054 0.1279 0.042 Uiso 1 1 calc R . . Pr2 Pr 0.494459(11) 0.011352(7) 0.217125(11) 0.02152(5) Uani 1 1 d . . . B2 B 0.4664(3) -0.14055(17) 0.1785(3) 0.0352(10) Uani 1 1 d . . . H2A H 0.4850(17) -0.1814(12) 0.1885(19) 0.032(9) Uiso 1 1 d . . . H2B H 0.4052(19) -0.1366(12) 0.128(2) 0.037(10) Uiso 1 1 d . . . C201 C 0.22175(19) -0.00945(12) 0.05469(19) 0.0253(7) Uani 1 1 d . . . C202 C 0.2279(2) -0.06027(13) 0.0756(2) 0.0330(9) Uani 1 1 d . . . H202 H 0.2782 -0.0746 0.1092 0.040 Uiso 1 1 calc R . . C203 C 0.1616(2) -0.09011(15) 0.0481(2) 0.0422(10) Uani 1 1 d . . . H203 H 0.1666 -0.1247 0.0631 0.051 Uiso 1 1 calc R . . C204 C 0.0892(2) -0.07009(17) -0.0005(3) 0.0486(11) Uani 1 1 d . . . H204 H 0.0438 -0.0909 -0.0196 0.058 Uiso 1 1 calc R . . C205 C 0.0812(2) -0.02038(16) -0.0219(3) 0.0501(11) Uani 1 1 d . . . H205 H 0.0305 -0.0065 -0.0555 0.060 Uiso 1 1 calc R . . C206 C 0.1475(2) 0.00950(14) 0.0059(2) 0.0374(9) Uani 1 1 d . . . H206 H 0.1417 0.0441 -0.0091 0.045 Uiso 1 1 calc R . . O211 O 0.35856(13) -0.00207(8) 0.13312(14) 0.0290(5) Uani 1 1 d . . . C212 C 0.29551(19) 0.02122(12) 0.0876(2) 0.0246(8) Uani 1 1 d . . . C213 C 0.2935(2) 0.07235(14) 0.0667(2) 0.0296(8) Uani 1 1 d . . . H213 H 0.2476(17) 0.0864(11) 0.0342(18) 0.014(8) Uiso 1 1 d . . . C214 C 0.3604(2) 0.10291(12) 0.0954(2) 0.0253(8) Uani 1 1 d . . . O215 O 0.42863(13) 0.08840(8) 0.14854(14) 0.0285(5) Uani 1 1 d . . . C221 C 0.3547(2) 0.15527(12) 0.0608(2) 0.0259(8) Uani 1 1 d . . . C222 C 0.4239(2) 0.18279(13) 0.0867(2) 0.0345(9) Uani 1 1 d . . . H222 H 0.4723 0.1692 0.1278 0.041 Uiso 1 1 calc R . . C223 C 0.4229(2) 0.22984(14) 0.0530(2) 0.0434(10) Uani 1 1 d . . . H223 H 0.4706 0.2479 0.0698 0.052 Uiso 1 1 calc R . . C224 C 0.3530(3) 0.25029(14) -0.0045(2) 0.0477(11) Uani 1 1 d . . . H224 H 0.3524 0.2825 -0.0276 0.057 Uiso 1 1 calc R . . C225 C 0.2845(3) 0.22452(15) -0.0285(2) 0.0476(11) Uani 1 1 d . . . H225 H 0.2361 0.2392 -0.0672 0.057 Uiso 1 1 calc R . . C226 C 0.2851(2) 0.17702(13) 0.0034(2) 0.0363(9) Uani 1 1 d . . . H226 H 0.2370 0.1592 -0.0146 0.044 Uiso 1 1 calc R . . C231 C 0.6252(2) 0.12964(12) 0.4294(2) 0.0258(8) Uani 1 1 d . . . C232 C 0.5673(2) 0.16538(12) 0.3884(2) 0.0311(8) Uani 1 1 d . . . H232 H 0.5286 0.1591 0.3327 0.037 Uiso 1 1 calc R . . C233 C 0.5643(2) 0.21011(14) 0.4264(2) 0.0418(10) Uani 1 1 d . . . H233 H 0.5234 0.2337 0.3975 0.050 Uiso 1 1 calc R . . C234 C 0.6212(3) 0.21984(15) 0.5063(3) 0.0478(11) Uani 1 1 d . . . H234 H 0.6200 0.2505 0.5327 0.057 Uiso 1 1 calc R . . C235 C 0.6796(3) 0.18544(15) 0.5480(2) 0.0482(11) Uani 1 1 d . . . H235 H 0.7191 0.1926 0.6030 0.058 Uiso 1 1 calc R . . C236 C 0.6819(2) 0.14031(13) 0.5109(2) 0.0354(9) Uani 1 1 d . . . H236 H 0.7222 0.1165 0.5409 0.043 Uiso 1 1 calc R . . O241 O 0.57124(13) 0.07949(8) 0.30880(13) 0.0265(5) Uani 1 1 d . . . C242 C 0.62289(19) 0.08141(12) 0.3849(2) 0.0241(8) Uani 1 1 d . . . N261 N 0.47252(17) -0.12022(10) 0.26176(17) 0.0296(7) Uani 1 1 d . . . N262 N 0.46130(16) -0.07124(10) 0.27365(17) 0.0276(7) Uani 1 1 d . . . C263 C 0.4491(2) -0.06916(13) 0.3410(2) 0.0286(8) Uani 1 1 d . . . C264 C 0.4527(2) -0.11771(13) 0.3728(2) 0.0390(9) Uani 1 1 d . . . H264 H 0.4465 -0.1272 0.4199 0.047 Uiso 1 1 calc R . . C265 C 0.4671(2) -0.14819(14) 0.3209(2) 0.0393(9) Uani 1 1 d . . . H265 H 0.4725 -0.1837 0.3256 0.047 Uiso 1 1 calc R . . N271 N 0.44714(16) 0.02060(10) 0.33277(16) 0.0266(7) Uani 1 1 d . . . C272 C 0.43433(19) -0.02048(13) 0.3686(2) 0.0276(8) Uani 1 1 d . . . C273 C 0.4082(2) -0.01653(15) 0.4281(2) 0.0375(9) Uani 1 1 d . . . H273 H 0.3988 -0.0459 0.4521 0.045 Uiso 1 1 calc R . . C274 C 0.3961(2) 0.03050(15) 0.4519(2) 0.0422(10) Uani 1 1 d . . . H274 H 0.3788 0.0339 0.4929 0.051 Uiso 1 1 calc R . . C275 C 0.4093(2) 0.07259(14) 0.4161(2) 0.0371(9) Uani 1 1 d . . . H275 H 0.4015 0.1054 0.4318 0.044 Uiso 1 1 calc R . . C276 C 0.4343(2) 0.06585(13) 0.3567(2) 0.0312(8) Uani 1 1 d . . . H276 H 0.4428 0.0949 0.3315 0.037 Uiso 1 1 calc R . . N281 N 0.52534(16) -0.11360(10) 0.15543(17) 0.0295(7) Uani 1 1 d . . . N282 N 0.52646(16) -0.06286(10) 0.14523(16) 0.0253(6) Uani 1 1 d . . . C283 C 0.57652(19) -0.05448(13) 0.1132(2) 0.0269(8) Uani 1 1 d . . . C284 C 0.6066(2) -0.10000(13) 0.1025(2) 0.0350(9) Uani 1 1 d . . . H284 H 0.6427 -0.1050 0.0810 0.042 Uiso 1 1 calc R . . C285 C 0.5731(2) -0.13590(14) 0.1295(2) 0.0387(9) Uani 1 1 d . . . H285 H 0.5820 -0.1711 0.1300 0.046 Uiso 1 1 calc R . . N291 N 0.56257(16) 0.03401(10) 0.12473(16) 0.0274(7) Uani 1 1 d . . . C292 C 0.59094(19) -0.00319(12) 0.09510(19) 0.0254(8) Uani 1 1 d . . . C293 C 0.6292(2) 0.00723(14) 0.0482(2) 0.0343(9) Uani 1 1 d . . . H293 H 0.6489 -0.0194 0.0284 0.041 Uiso 1 1 calc R . . C294 C 0.6383(2) 0.05618(14) 0.0306(2) 0.0361(9) Uani 1 1 d . . . H294 H 0.6640 0.0638 -0.0020 0.043 Uiso 1 1 calc R . . C295 C 0.6099(2) 0.09426(14) 0.0607(2) 0.0330(9) Uani 1 1 d . . . H295 H 0.6158 0.1285 0.0496 0.040 Uiso 1 1 calc R . . C296 C 0.5727(2) 0.08161(13) 0.1072(2) 0.0327(9) Uani 1 1 d . . . H296 H 0.5533 0.1080 0.1279 0.039 Uiso 1 1 calc R . . O245 O 0.61926(13) -0.01818(8) 0.31948(13) 0.0288(5) Uani 1 1 d . . . C244 C 0.66883(19) -0.00644(13) 0.3928(2) 0.0248(7) Uani 1 1 d . . . C243 C 0.67318(19) 0.04131(12) 0.4277(2) 0.0263(8) Uani 1 1 d . . . H243 H 0.7123 0.0468 0.4835 0.032 Uiso 1 1 calc R . . C251 C 0.7213(2) -0.04855(13) 0.4440(2) 0.0268(8) Uani 1 1 d . . . C252 C 0.6985(2) -0.09748(13) 0.4156(2) 0.0350(9) Uani 1 1 d . . . H252 H 0.6525 -0.1030 0.3643 0.042 Uiso 1 1 calc R . . C256 C 0.7892(2) -0.04181(14) 0.5195(2) 0.0380(9) Uani 1 1 d . . . H256 H 0.8056 -0.0087 0.5401 0.046 Uiso 1 1 calc R . . C254 C 0.8095(2) -0.13080(15) 0.5362(2) 0.0446(10) Uani 1 1 d . . . H254 H 0.8394 -0.1588 0.5677 0.054 Uiso 1 1 calc R . . C253 C 0.7425(2) -0.13827(15) 0.4618(2) 0.0459(10) Uani 1 1 d . . . H253 H 0.7263 -0.1715 0.4420 0.055 Uiso 1 1 calc R . . C255 C 0.8327(2) -0.08245(15) 0.5646(2) 0.0451(10) Uani 1 1 d . . . H255 H 0.8791 -0.0771 0.6156 0.054 Uiso 1 1 calc R . . Cl1 Cl 0.99228(9) 1.00831(5) 0.41717(9) 0.0923(5) Uani 1 1 d . . . C500 C 0.9534(6) 0.9704(3) 0.4746(6) 0.069(3) Uani 0.50 1 d P . . H50A H 0.8962 0.9762 0.4527 0.083 Uiso 0.50 1 calc PR . . H50B H 0.9624 0.9341 0.4702 0.083 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 C113 0.023(2) 0.024(2) 0.039(2) -0.0004(15) 0.0178(17) 0.0025(15) Pr1 0.02251(11) 0.01865(10) 0.02524(10) -0.00007(8) 0.01311(8) -0.00002(8) B1 0.037(3) 0.025(2) 0.043(3) 0.001(2) 0.020(2) 0.003(2) C101 0.024(2) 0.0243(19) 0.0214(17) 0.0033(14) 0.0083(15) 0.0006(15) C102 0.026(2) 0.030(2) 0.034(2) 0.0007(16) 0.0138(17) -0.0004(16) C103 0.032(2) 0.027(2) 0.039(2) -0.0028(16) 0.0148(18) -0.0050(17) C104 0.023(2) 0.036(2) 0.039(2) 0.0083(18) 0.0108(17) -0.0039(17) C105 0.029(2) 0.039(2) 0.045(2) 0.0081(18) 0.0234(19) 0.0040(18) C106 0.030(2) 0.026(2) 0.033(2) 0.0033(16) 0.0140(17) 0.0024(16) O111 0.0274(14) 0.0200(13) 0.0418(14) 0.0010(11) 0.0203(12) 0.0016(11) C112 0.0207(19) 0.0255(19) 0.0229(17) -0.0008(15) 0.0096(15) -0.0010(15) C114 0.0227(19) 0.0241(19) 0.0200(17) 0.0012(14) 0.0085(15) 0.0014(15) O115 0.0261(14) 0.0231(13) 0.0371(14) -0.0008(10) 0.0172(12) 0.0006(10) C121 0.026(2) 0.0245(19) 0.0204(18) 0.0020(14) 0.0094(15) 0.0028(15) C122 0.029(2) 0.023(2) 0.055(3) 0.0019(17) 0.018(2) 0.0004(16) C123 0.036(3) 0.024(2) 0.062(3) 0.0011(19) 0.013(2) -0.0079(18) C124 0.048(3) 0.018(2) 0.036(2) 0.0002(16) 0.011(2) 0.0048(19) C125 0.042(2) 0.025(2) 0.050(2) 0.0072(18) 0.025(2) 0.0131(19) C126 0.034(2) 0.030(2) 0.045(2) 0.0048(17) 0.022(2) 0.0015(17) C131 0.026(2) 0.0201(19) 0.035(2) -0.0005(15) 0.0132(17) -0.0013(15) C132 0.033(2) 0.026(2) 0.052(2) -0.0029(17) 0.026(2) 0.0004(17) C133 0.041(3) 0.027(2) 0.063(3) -0.0079(19) 0.026(2) 0.0016(18) C134 0.034(2) 0.023(2) 0.059(3) 0.0030(18) 0.018(2) -0.0057(18) C135 0.036(2) 0.033(2) 0.052(2) 0.0048(19) 0.024(2) -0.0051(19) C136 0.033(2) 0.029(2) 0.044(2) 0.0014(17) 0.0210(19) 0.0025(17) O141 0.0321(15) 0.0249(14) 0.0476(16) -0.0031(11) 0.0272(13) -0.0012(11) C142 0.023(2) 0.0248(19) 0.0291(19) -0.0007(15) 0.0105(16) -0.0013(15) C143 0.027(2) 0.026(2) 0.044(2) -0.0025(16) 0.0233(19) -0.0020(16) C144 0.027(2) 0.027(2) 0.0249(18) -0.0011(15) 0.0127(16) 0.0016(16) O145 0.0278(14) 0.0199(13) 0.0398(14) -0.0018(10) 0.0190(12) -0.0017(11) C151 0.025(2) 0.027(2) 0.0270(18) -0.0039(15) 0.0120(16) 0.0036(15) C152 0.026(2) 0.027(2) 0.036(2) -0.0025(16) 0.0121(17) 0.0010(16) C153 0.039(2) 0.025(2) 0.042(2) -0.0005(17) 0.0144(19) 0.0085(18) C154 0.036(2) 0.040(3) 0.047(2) -0.0061(19) 0.020(2) 0.0148(19) C155 0.049(3) 0.046(3) 0.062(3) -0.001(2) 0.040(2) 0.010(2) C156 0.040(2) 0.030(2) 0.049(2) 0.0017(18) 0.028(2) 0.0061(18) N161 0.0303(18) 0.0178(16) 0.0376(17) 0.0063(13) 0.0176(15) 0.0024(13) N162 0.0250(16) 0.0220(16) 0.0310(16) 0.0053(12) 0.0154(14) 0.0033(13) C163 0.027(2) 0.032(2) 0.0312(19) 0.0092(16) 0.0171(17) 0.0080(16) C164 0.045(3) 0.040(2) 0.042(2) 0.0111(19) 0.028(2) 0.0023(19) C165 0.042(2) 0.031(2) 0.054(3) 0.0142(19) 0.030(2) 0.0009(18) N171 0.0266(17) 0.0290(17) 0.0270(15) -0.0017(13) 0.0138(13) 0.0005(13) C172 0.0200(19) 0.037(2) 0.0287(19) 0.0055(16) 0.0130(16) 0.0079(16) C173 0.037(2) 0.057(3) 0.029(2) 0.0119(19) 0.0189(18) 0.012(2) C174 0.038(2) 0.064(3) 0.028(2) -0.004(2) 0.0145(19) 0.010(2) C175 0.029(2) 0.046(3) 0.032(2) -0.0117(18) 0.0106(18) -0.0008(18) C176 0.034(2) 0.035(2) 0.034(2) -0.0044(17) 0.0161(18) -0.0016(18) N181 0.0382(19) 0.0201(17) 0.0356(17) -0.0055(13) 0.0191(15) -0.0041(14) N182 0.0335(18) 0.0208(16) 0.0313(16) -0.0015(13) 0.0171(14) 0.0016(13) C183 0.037(2) 0.0255(19) 0.0262(18) -0.0030(15) 0.0156(17) -0.0002(17) C184 0.045(3) 0.033(2) 0.033(2) -0.0078(17) 0.0078(19) -0.0075(19) C185 0.051(3) 0.028(2) 0.045(2) -0.0097(19) 0.017(2) -0.014(2) N191 0.0374(19) 0.0213(16) 0.0292(16) 0.0023(12) 0.0184(15) 0.0027(13) C192 0.031(2) 0.030(2) 0.0263(18) -0.0035(16) 0.0150(16) 0.0034(17) C193 0.038(2) 0.035(2) 0.032(2) -0.0025(17) 0.0127(18) 0.0015(18) C194 0.041(2) 0.042(2) 0.033(2) 0.0053(18) 0.0147(19) 0.013(2) C195 0.047(3) 0.026(2) 0.042(2) 0.0087(18) 0.022(2) 0.0082(18) C196 0.046(3) 0.027(2) 0.035(2) -0.0012(17) 0.020(2) -0.0013(18) Pr2 0.02154(10) 0.02154(10) 0.02090(9) 0.00006(8) 0.00940(8) 0.00004(8) B2 0.039(3) 0.026(3) 0.039(3) -0.006(2) 0.017(2) -0.005(2) C201 0.028(2) 0.0269(19) 0.0233(17) -0.0034(15) 0.0142(16) -0.0019(16) C202 0.031(2) 0.033(2) 0.035(2) 0.0004(17) 0.0160(18) -0.0049(17) C203 0.049(3) 0.042(2) 0.041(2) -0.0045(19) 0.025(2) -0.013(2) C204 0.035(3) 0.061(3) 0.053(3) -0.017(2) 0.023(2) -0.022(2) C205 0.028(2) 0.056(3) 0.057(3) -0.005(2) 0.011(2) -0.001(2) C206 0.027(2) 0.037(2) 0.042(2) -0.0024(18) 0.0111(18) -0.0018(18) O211 0.0265(14) 0.0235(14) 0.0312(13) 0.0022(10) 0.0085(11) 0.0008(11) C212 0.027(2) 0.027(2) 0.0223(17) -0.0029(14) 0.0137(16) 0.0013(16) C213 0.022(2) 0.031(2) 0.034(2) 0.0044(16) 0.0109(18) 0.0066(17) C214 0.028(2) 0.026(2) 0.0260(19) -0.0031(15) 0.0162(17) 0.0037(16) O215 0.0224(14) 0.0260(14) 0.0314(13) 0.0018(11) 0.0078(11) 0.0018(11) C221 0.030(2) 0.0217(19) 0.0266(19) -0.0013(14) 0.0142(17) 0.0020(16) C222 0.037(2) 0.025(2) 0.044(2) -0.0021(16) 0.0213(19) 0.0033(17) C223 0.049(3) 0.028(2) 0.058(3) -0.005(2) 0.029(2) -0.008(2) C224 0.071(3) 0.024(2) 0.047(3) 0.0039(19) 0.027(2) -0.007(2) C225 0.051(3) 0.036(2) 0.041(2) 0.0090(19) 0.009(2) 0.008(2) C226 0.035(2) 0.031(2) 0.037(2) 0.0059(17) 0.0119(19) -0.0009(18) C231 0.031(2) 0.0244(19) 0.0266(19) -0.0005(15) 0.0175(17) -0.0046(16) C232 0.033(2) 0.027(2) 0.033(2) 0.0002(16) 0.0153(18) -0.0043(17) C233 0.054(3) 0.026(2) 0.051(3) 0.0015(18) 0.029(2) 0.0021(19) C234 0.070(3) 0.028(2) 0.052(3) -0.011(2) 0.034(3) -0.002(2) C235 0.063(3) 0.042(3) 0.035(2) -0.0128(19) 0.019(2) -0.007(2) C236 0.041(2) 0.030(2) 0.032(2) -0.0018(17) 0.0151(19) 0.0014(18) O241 0.0277(14) 0.0255(13) 0.0239(13) -0.0012(10) 0.0098(11) -0.0033(10) C242 0.023(2) 0.028(2) 0.0243(18) -0.0010(15) 0.0138(16) -0.0060(15) N261 0.0362(18) 0.0194(16) 0.0316(17) 0.0017(13) 0.0143(14) -0.0005(13) N262 0.0288(17) 0.0244(16) 0.0294(16) 0.0023(13) 0.0133(14) -0.0014(13) C263 0.024(2) 0.031(2) 0.0288(19) 0.0044(16) 0.0114(17) -0.0027(16) C264 0.054(3) 0.031(2) 0.033(2) 0.0067(17) 0.021(2) -0.0057(19) C265 0.048(3) 0.026(2) 0.037(2) 0.0069(17) 0.013(2) -0.0052(18) N271 0.0270(17) 0.0281(17) 0.0285(16) 0.0003(13) 0.0160(14) -0.0019(13) C272 0.026(2) 0.030(2) 0.0255(18) 0.0030(15) 0.0110(16) -0.0006(16) C273 0.038(2) 0.045(3) 0.038(2) 0.0103(19) 0.0249(19) 0.0009(19) C274 0.046(3) 0.053(3) 0.041(2) 0.002(2) 0.031(2) 0.005(2) C275 0.042(2) 0.037(2) 0.040(2) -0.0053(18) 0.026(2) 0.0061(19) C276 0.030(2) 0.029(2) 0.038(2) 0.0010(16) 0.0191(18) 0.0006(16) N281 0.0337(18) 0.0221(16) 0.0284(16) -0.0034(12) 0.0107(14) -0.0003(13) N282 0.0264(17) 0.0224(16) 0.0264(16) -0.0023(12) 0.0117(14) 0.0000(12) C283 0.024(2) 0.029(2) 0.0228(19) -0.0062(15) 0.0073(16) 0.0001(16) C284 0.036(2) 0.036(2) 0.035(2) -0.0019(17) 0.0182(19) 0.0080(18) C285 0.043(2) 0.029(2) 0.040(2) -0.0045(17) 0.016(2) 0.0088(19) N291 0.0281(17) 0.0284(17) 0.0265(16) -0.0044(13) 0.0135(14) -0.0031(13) C292 0.0212(19) 0.032(2) 0.0181(16) -0.0028(14) 0.0049(14) -0.0012(15) C293 0.037(2) 0.041(2) 0.0298(19) -0.0067(17) 0.0198(18) -0.0005(18) C294 0.037(2) 0.045(2) 0.031(2) -0.0031(18) 0.0200(19) -0.0092(19) C295 0.034(2) 0.032(2) 0.034(2) -0.0005(17) 0.0161(18) -0.0060(17) C296 0.036(2) 0.029(2) 0.039(2) -0.0010(17) 0.0214(19) -0.0029(17) O245 0.0283(14) 0.0282(14) 0.0256(13) -0.0040(10) 0.0090(11) 0.0018(11) C244 0.0195(19) 0.033(2) 0.0249(18) 0.0014(15) 0.0128(15) -0.0004(15) C243 0.022(2) 0.032(2) 0.0207(18) -0.0015(15) 0.0068(15) -0.0028(16) C251 0.025(2) 0.031(2) 0.0277(19) 0.0024(15) 0.0152(17) 0.0037(16) C252 0.034(2) 0.034(2) 0.031(2) 0.0001(17) 0.0095(18) 0.0058(18) C256 0.030(2) 0.035(2) 0.040(2) -0.0039(18) 0.0094(19) 0.0030(18) C254 0.046(3) 0.043(3) 0.042(2) 0.014(2) 0.018(2) 0.022(2) C253 0.050(3) 0.031(2) 0.049(3) -0.0009(19) 0.017(2) 0.007(2) C255 0.038(3) 0.048(3) 0.036(2) 0.0043(19) 0.0054(19) 0.013(2) Cl1 0.0893(11) 0.0702(10) 0.0945(11) 0.0126(8) 0.0235(9) 0.0114(8) C500 0.072(7) 0.059(7) 0.068(7) -0.006(5) 0.025(6) -0.010(5) _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 C113 C114 1.397(4) . ? C113 C112 1.398(4) . ? Pr1 O145 2.390(2) . ? Pr1 O111 2.391(2) . ? Pr1 O115 2.397(2) . ? Pr1 O141 2.403(2) . ? Pr1 N182 2.589(3) . ? Pr1 N162 2.603(3) . ? Pr1 N171 2.627(3) . ? Pr1 N191 2.656(3) . ? B1 N181 1.549(5) . ? B1 N161 1.557(5) . ? C101 C106 1.393(4) . ? C101 C102 1.399(4) . ? C101 C112 1.496(4) . ? C102 C103 1.382(4) . ? C103 C104 1.392(5) . ? C104 C105 1.375(5) . ? C105 C106 1.396(4) . ? O111 C112 1.267(3) . ? C114 O115 1.269(3) . ? C114 C121 1.502(4) . ? C121 C126 1.379(4) . ? C121 C122 1.383(4) . ? C122 C123 1.389(5) . ? C123 C124 1.368(5) . ? C124 C125 1.358(5) . ? C125 C126 1.384(5) . ? C131 C136 1.388(4) . ? C131 C132 1.402(4) . ? C131 C142 1.500(4) . ? C132 C133 1.379(5) . ? C133 C134 1.385(5) . ? C134 C135 1.366(5) . ? C135 C136 1.379(5) . ? O141 C142 1.275(3) . ? C142 C143 1.397(4) . ? C143 C144 1.398(4) . ? C144 O145 1.279(4) . ? C144 C151 1.506(4) . ? C151 C152 1.381(4) . ? C151 C156 1.392(4) . ? C152 C153 1.385(4) . ? C153 C154 1.376(5) . ? C154 C155 1.379(5) . ? C155 C156 1.380(5) . ? N161 C165 1.347(4) . ? N161 N162 1.354(4) . ? N162 C163 1.346(4) . ? C163 C164 1.390(5) . ? C163 C172 1.462(5) . ? C164 C165 1.369(5) . ? N171 C176 1.341(4) . ? N171 C172 1.351(4) . ? C172 C173 1.400(4) . ? C173 C174 1.377(5) . ? C174 C175 1.371(5) . ? C175 C176 1.381(5) . ? N181 C185 1.343(4) . ? N181 N182 1.358(3) . ? N182 C183 1.349(4) . ? C183 C184 1.396(5) . ? C183 C192 1.462(4) . ? C184 C185 1.378(5) . ? N191 C196 1.339(4) . ? N191 C192 1.356(4) . ? C192 C193 1.395(5) . ? C193 C194 1.370(5) . ? C194 C195 1.375(5) . ? C195 C196 1.384(5) . ? Pr2 O211 2.357(2) . ? Pr2 O245 2.380(2) . ? Pr2 O215 2.423(2) . ? Pr2 O241 2.436(2) . ? Pr2 N282 2.592(3) . ? Pr2 N262 2.624(3) . ? Pr2 N291 2.633(3) . ? Pr2 N271 2.659(2) . ? B2 N281 1.553(5) . ? B2 N261 1.557(5) . ? C201 C206 1.376(5) . ? C201 C202 1.393(4) . ? C201 C212 1.496(4) . ? C202 C203 1.380(5) . ? C203 C204 1.361(5) . ? C204 C205 1.365(5) . ? C205 C206 1.381(5) . ? O211 C212 1.265(4) . ? C212 C213 1.406(5) . ? C213 C214 1.400(5) . ? C214 O215 1.272(4) . ? C214 C221 1.509(4) . ? C221 C226 1.382(5) . ? C221 C222 1.393(5) . ? C222 C223 1.388(5) . ? C223 C224 1.371(5) . ? C224 C225 1.362(5) . ? C225 C226 1.386(5) . ? C231 C232 1.385(5) . ? C231 C236 1.397(5) . ? C231 C242 1.505(4) . ? C232 C233 1.389(5) . ? C233 C234 1.373(5) . ? C234 C235 1.370(5) . ? C235 C236 1.386(5) . ? O241 C242 1.272(4) . ? C242 C243 1.405(4) . ? N261 C265 1.348(4) . ? N261 N262 1.353(3) . ? N262 C263 1.349(4) . ? C263 C264 1.402(4) . ? C263 C272 1.462(5) . ? C264 C265 1.366(5) . ? N271 C276 1.340(4) . ? N271 C272 1.351(4) . ? C272 C273 1.392(4) . ? C273 C274 1.377(5) . ? C274 C275 1.375(5) . ? C275 C276 1.380(4) . ? N281 C285 1.346(4) . ? N281 N282 1.363(3) . ? N282 C283 1.353(4) . ? C283 C284 1.393(4) . ? C283 C292 1.459(4) . ? C284 C285 1.364(5) . ? N291 C296 1.340(4) . ? N291 C292 1.355(4) . ? C292 C293 1.386(4) . ? C293 C294 1.370(5) . ? C294 C295 1.378(5) . ? C295 C296 1.377(4) . ? O245 C244 1.263(4) . ? C244 C243 1.403(4) . ? C244 C251 1.502(4) . ? C251 C252 1.391(5) . ? C251 C256 1.395(5) . ? C252 C253 1.390(5) . ? C256 C255 1.378(5) . ? C254 C253 1.378(5) . ? C254 C255 1.379(5) . ? Cl1 C500 1.832(9) 3_776 ? Cl1 C500 1.840(9) . ? C500 Cl1 1.832(9) 3_776 ? 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 C114 C113 C112 123.8(3) . . ? O145 Pr1 O111 149.00(7) . . ? O145 Pr1 O115 142.20(7) . . ? O111 Pr1 O115 68.72(7) . . ? O145 Pr1 O141 69.32(7) . . ? O111 Pr1 O141 141.68(7) . . ? O115 Pr1 O141 73.05(7) . . ? O145 Pr1 N182 82.20(8) . . ? O111 Pr1 N182 73.78(8) . . ? O115 Pr1 N182 122.80(8) . . ? O141 Pr1 N182 132.46(8) . . ? O145 Pr1 N162 84.20(7) . . ? O111 Pr1 N162 71.45(8) . . ? O115 Pr1 N162 126.36(7) . . ? O141 Pr1 N162 134.03(8) . . ? N182 Pr1 N162 76.39(8) . . ? O145 Pr1 N171 101.19(8) . . ? O111 Pr1 N171 84.57(8) . . ? O115 Pr1 N171 79.35(8) . . ? O141 Pr1 N171 86.08(8) . . ? N182 Pr1 N171 137.80(8) . . ? N162 Pr1 N171 62.36(8) . . ? O145 Pr1 N191 96.88(8) . . ? O111 Pr1 N191 89.32(8) . . ? O115 Pr1 N191 75.17(8) . . ? O141 Pr1 N191 83.34(8) . . ? N182 Pr1 N191 62.64(8) . . ? N162 Pr1 N191 138.33(8) . . ? N171 Pr1 N191 154.29(8) . . ? N181 B1 N161 110.6(3) . . ? C106 C101 C102 118.3(3) . . ? C106 C101 C112 123.5(3) . . ? C102 C101 C112 118.1(3) . . ? C103 C102 C101 121.0(3) . . ? C102 C103 C104 120.1(3) . . ? C105 C104 C103 119.6(3) . . ? C104 C105 C106 120.5(3) . . ? C101 C106 C105 120.5(3) . . ? C112 O111 Pr1 140.0(2) . . ? O111 C112 C113 123.6(3) . . ? O111 C112 C101 115.3(3) . . ? C113 C112 C101 121.0(3) . . ? O115 C114 C113 123.0(3) . . ? O115 C114 C121 115.8(3) . . ? C113 C114 C121 121.2(3) . . ? C114 O115 Pr1 140.1(2) . . ? C126 C121 C122 118.3(3) . . ? C126 C121 C114 124.1(3) . . ? C122 C121 C114 117.7(3) . . ? C121 C122 C123 120.5(3) . . ? C124 C123 C122 120.2(3) . . ? C125 C124 C123 119.8(3) . . ? C124 C125 C126 120.5(3) . . ? C121 C126 C125 120.8(3) . . ? C136 C131 C132 118.6(3) . . ? C136 C131 C142 123.8(3) . . ? C132 C131 C142 117.6(3) . . ? C133 C132 C131 120.1(3) . . ? C132 C133 C134 120.4(3) . . ? C135 C134 C133 119.7(3) . . ? C134 C135 C136 120.7(3) . . ? C135 C136 C131 120.6(3) . . ? C142 O141 Pr1 138.4(2) . . ? O141 C142 C143 123.4(3) . . ? O141 C142 C131 116.7(3) . . ? C143 C142 C131 119.9(3) . . ? C142 C143 C144 124.1(3) . . ? O145 C144 C143 123.9(3) . . ? O145 C144 C151 115.9(3) . . ? C143 C144 C151 120.1(3) . . ? C144 O145 Pr1 138.9(2) . . ? C152 C151 C156 118.8(3) . . ? C152 C151 C144 118.9(3) . . ? C156 C151 C144 122.3(3) . . ? C151 C152 C153 120.7(3) . . ? C154 C153 C152 120.2(3) . . ? C153 C154 C155 119.5(3) . . ? C154 C155 C156 120.7(4) . . ? C155 C156 C151 120.2(3) . . ? C165 N161 N162 109.6(3) . . ? C165 N161 B1 128.3(3) . . ? N162 N161 B1 121.9(3) . . ? C163 N162 N161 106.2(3) . . ? C163 N162 Pr1 118.0(2) . . ? N161 N162 Pr1 128.20(19) . . ? N162 C163 C164 110.6(3) . . ? N162 C163 C172 118.9(3) . . ? C164 C163 C172 130.4(3) . . ? C165 C164 C163 104.5(3) . . ? N161 C165 C164 109.1(3) . . ? C176 N171 C172 117.9(3) . . ? C176 N171 Pr1 121.3(2) . . ? C172 N171 Pr1 119.8(2) . . ? N171 C172 C173 121.4(3) . . ? N171 C172 C163 115.9(3) . . ? C173 C172 C163 122.7(3) . . ? C174 C173 C172 119.1(4) . . ? C175 C174 C173 119.7(3) . . ? C174 C175 C176 118.3(4) . . ? N171 C176 C175 123.6(3) . . ? C185 N181 N182 109.5(3) . . ? C185 N181 B1 128.1(3) . . ? N182 N181 B1 122.2(3) . . ? C183 N182 N181 106.4(3) . . ? C183 N182 Pr1 116.4(2) . . ? N181 N182 Pr1 126.7(2) . . ? N182 C183 C184 110.5(3) . . ? N182 C183 C192 119.3(3) . . ? C184 C183 C192 130.2(3) . . ? C185 C184 C183 104.2(3) . . ? N181 C185 C184 109.4(3) . . ? C196 N191 C192 117.9(3) . . ? C196 N191 Pr1 123.2(2) . . ? C192 N191 Pr1 118.4(2) . . ? N191 C192 C193 121.7(3) . . ? N191 C192 C183 115.5(3) . . ? C193 C192 C183 122.8(3) . . ? C194 C193 C192 119.1(4) . . ? C193 C194 C195 119.7(4) . . ? C194 C195 C196 118.6(3) . . ? N191 C196 C195 123.1(3) . . ? O211 Pr2 O245 149.77(8) . . ? O211 Pr2 O215 68.91(7) . . ? O245 Pr2 O215 140.74(7) . . ? O211 Pr2 O241 133.61(7) . . ? O245 Pr2 O241 69.08(7) . . ? O215 Pr2 O241 74.21(7) . . ? O211 Pr2 N282 90.56(8) . . ? O245 Pr2 N282 75.72(8) . . ? O215 Pr2 N282 124.98(8) . . ? O241 Pr2 N282 134.38(8) . . ? O211 Pr2 N262 74.28(8) . . ? O245 Pr2 N262 76.02(8) . . ? O215 Pr2 N262 138.08(8) . . ? O241 Pr2 N262 122.30(8) . . ? N282 Pr2 N262 73.63(8) . . ? O211 Pr2 N291 110.58(8) . . ? O245 Pr2 N291 87.38(8) . . ? O215 Pr2 N291 76.97(8) . . ? O241 Pr2 N291 86.73(8) . . ? N282 Pr2 N291 63.16(8) . . ? N262 Pr2 N291 136.35(8) . . ? O211 Pr2 N271 80.92(8) . . ? O245 Pr2 N271 90.25(8) . . ? O215 Pr2 N271 92.25(8) . . ? O241 Pr2 N271 73.30(8) . . ? N282 Pr2 N271 135.75(8) . . ? N262 Pr2 N271 62.23(8) . . ? N291 Pr2 N271 159.36(8) . . ? N281 B2 N261 111.5(3) . . ? C206 C201 C202 117.4(3) . . ? C206 C201 C212 124.2(3) . . ? C202 C201 C212 118.4(3) . . ? C203 C202 C201 120.8(4) . . ? C204 C203 C202 120.1(4) . . ? C203 C204 C205 120.5(4) . . ? C204 C205 C206 119.4(4) . . ? C201 C206 C205 121.8(4) . . ? C212 O211 Pr2 141.5(2) . . ? O211 C212 C213 123.2(3) . . ? O211 C212 C201 115.7(3) . . ? C213 C212 C201 121.1(3) . . ? C214 C213 C212 123.7(3) . . ? O215 C214 C213 123.3(3) . . ? O215 C214 C221 116.4(3) . . ? C213 C214 C221 120.3(3) . . ? C214 O215 Pr2 138.8(2) . . ? C226 C221 C222 118.1(3) . . ? C226 C221 C214 123.8(3) . . ? C222 C221 C214 118.1(3) . . ? C223 C222 C221 120.6(4) . . ? C224 C223 C222 120.0(4) . . ? C225 C224 C223 120.1(4) . . ? C224 C225 C226 120.4(4) . . ? C221 C226 C225 120.8(4) . . ? C232 C231 C236 117.7(3) . . ? C232 C231 C242 118.7(3) . . ? C236 C231 C242 123.7(3) . . ? C231 C232 C233 121.9(3) . . ? C234 C233 C232 119.3(4) . . ? C235 C234 C233 120.1(4) . . ? C234 C235 C236 120.8(4) . . ? C235 C236 C231 120.3(4) . . ? C242 O241 Pr2 133.6(2) . . ? O241 C242 C243 123.9(3) . . ? O241 C242 C231 115.5(3) . . ? C243 C242 C231 120.5(3) . . ? C265 N261 N262 109.0(3) . . ? C265 N261 B2 125.6(3) . . ? N262 N261 B2 122.9(3) . . ? C263 N262 N261 107.0(3) . . ? C263 N262 Pr2 119.8(2) . . ? N261 N262 Pr2 131.04(19) . . ? N262 C263 C264 109.9(3) . . ? N262 C263 C272 119.4(3) . . ? C264 C263 C272 130.8(3) . . ? C265 C264 C263 104.4(3) . . ? N261 C265 C264 109.8(3) . . ? C276 N271 C272 117.8(3) . . ? C276 N271 Pr2 121.5(2) . . ? C272 N271 Pr2 120.7(2) . . ? N271 C272 C273 121.7(3) . . ? N271 C272 C263 116.3(3) . . ? C273 C272 C263 122.0(3) . . ? C274 C273 C272 119.1(3) . . ? C275 C274 C273 119.7(3) . . ? C274 C275 C276 118.1(3) . . ? N271 C276 C275 123.6(3) . . ? C285 N281 N282 109.4(3) . . ? C285 N281 B2 126.3(3) . . ? N282 N281 B2 123.5(3) . . ? C283 N282 N281 106.3(3) . . ? C283 N282 Pr2 118.3(2) . . ? N281 N282 Pr2 131.46(19) . . ? N282 C283 C284 109.9(3) . . ? N282 C283 C292 119.9(3) . . ? C284 C283 C292 130.2(3) . . ? C285 C284 C283 105.1(3) . . ? N281 C285 C284 109.3(3) . . ? C296 N291 C292 117.7(3) . . ? C296 N291 Pr2 122.5(2) . . ? C292 N291 Pr2 119.8(2) . . ? N291 C292 C293 121.6(3) . . ? N291 C292 C283 116.0(3) . . ? C293 C292 C283 122.4(3) . . ? C294 C293 C292 119.7(3) . . ? C293 C294 C295 119.1(3) . . ? C294 C295 C296 118.6(3) . . ? N291 C296 C295 123.3(3) . . ? C244 O245 Pr2 137.0(2) . . ? O245 C244 C243 123.8(3) . . ? O245 C244 C251 115.2(3) . . ? C243 C244 C251 120.8(3) . . ? C242 C243 C244 123.7(3) . . ? C252 C251 C256 118.2(3) . . ? C252 C251 C244 117.6(3) . . ? C256 C251 C244 124.2(3) . . ? C253 C252 C251 120.5(4) . . ? C255 C256 C251 120.9(4) . . ? C253 C254 C255 119.5(4) . . ? C254 C253 C252 120.4(4) . . ? C256 C255 C254 120.5(4) . . ? C500 Cl1 C500 74.9(5) 3_776 . ? Cl1 C500 Cl1 105.1(5) 3_776 . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.007 _refine_diff_density_min -0.865 _refine_diff_density_rms 0.085 #=END data_imw24g _database_code_depnum_ccdc_archive 'CCDC 229468' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H36 B Gd N6 O4' _chemical_formula_sum 'C46 H36 B Gd N6 O4' _chemical_formula_weight 904.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.2403(18) _cell_length_b 26.613(2) _cell_length_c 17.8124(16) _cell_angle_alpha 90.00 _cell_angle_beta 117.1740(10) _cell_angle_gamma 90.00 _cell_volume 8114.1(13) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7571 _cell_measurement_theta_min 4.493 _cell_measurement_theta_max 54.732 _exptl_crystal_description NEEDLE _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.481 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3640 _exptl_absorpt_coefficient_mu 1.687 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7511 _exptl_absorpt_correction_T_max 0.8106 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'CCD Area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 68424 _diffrn_reflns_av_R_equivalents 0.0559 _diffrn_reflns_av_sigmaI/netI 0.0613 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.19 _diffrn_reflns_theta_max 27.56 _reflns_number_total 18339 _reflns_number_gt 12737 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0341P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18339 _refine_ls_number_parameters 1045 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0655 _refine_ls_R_factor_gt 0.0377 _refine_ls_wR_factor_ref 0.0812 _refine_ls_wR_factor_gt 0.0737 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 0.992 _refine_ls_shift/su_max 0.004 _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 Gd1 Gd 0.491393(10) 0.694247(6) 0.262675(10) 0.02158(5) Uani 1 1 d . . . O111 O 0.37884(14) 0.72248(8) 0.14610(15) 0.0286(6) Uani 1 1 d . . . O145 O 0.60946(14) 0.71735(8) 0.37657(14) 0.0279(6) Uani 1 1 d . . . O115 O 0.41171(14) 0.62491(9) 0.19596(14) 0.0297(6) Uani 1 1 d . . . O141 O 0.55795(14) 0.62214(9) 0.33478(14) 0.0287(6) Uani 1 1 d . . . N161 N 0.49735(17) 0.82092(10) 0.32639(17) 0.0272(7) Uani 1 1 d . . . N162 N 0.47107(17) 0.77399(10) 0.32736(17) 0.0256(7) Uani 1 1 d . . . N191 N 0.56250(18) 0.66187(11) 0.18052(18) 0.0288(7) Uani 1 1 d . . . C121 C 0.3374(2) 0.56075(13) 0.1030(2) 0.0288(8) Uani 1 1 d . . . C131 C 0.6412(2) 0.55466(13) 0.4035(2) 0.0259(8) Uani 1 1 d . . . C112 C 0.3218(2) 0.70370(13) 0.0821(2) 0.0247(8) Uani 1 1 d . . . C183 C 0.6112(2) 0.74533(14) 0.1958(2) 0.0303(9) Uani 1 1 d . . . N171 N 0.43850(17) 0.68278(11) 0.36854(17) 0.0273(7) Uani 1 1 d . . . C196 C 0.5617(2) 0.61349(15) 0.1581(2) 0.0403(10) Uani 1 1 d . . . H196 H 0.5270 0.5909 0.1653 0.048 Uiso 1 1 calc R . . C144 C 0.6688(2) 0.69708(13) 0.4347(2) 0.0240(8) Uani 1 1 d . . . C101 C 0.2649(2) 0.74042(13) 0.0210(2) 0.0270(8) Uani 1 1 d . . . C114 C 0.3548(2) 0.61534(13) 0.1243(2) 0.0252(8) Uani 1 1 d . . . C106 C 0.2646(2) 0.78916(14) 0.0481(2) 0.0339(9) Uani 1 1 d . . . H106 H 0.2997 0.7984 0.1043 0.041 Uiso 1 1 calc R . . C185 C 0.6318(3) 0.82383(16) 0.2345(3) 0.0440(11) Uani 1 1 d . . . H185 H 0.6540 0.8564 0.2493 0.053 Uiso 1 1 calc R . . C156 C 0.7278(2) 0.78181(13) 0.4684(2) 0.0303(9) Uani 1 1 d . . . H156 H 0.6894 0.7920 0.4141 0.036 Uiso 1 1 calc R . . C113 C 0.3087(2) 0.65221(13) 0.0671(2) 0.0292(9) Uani 1 1 d . . . H113 H 0.2664 0.6417 0.0155 0.035 Uiso 1 1 calc R . . C152 C 0.7848(2) 0.71874(14) 0.5749(2) 0.0329(9) Uani 1 1 d . . . H152 H 0.7868 0.6850 0.5932 0.039 Uiso 1 1 calc R . . N181 N 0.56487(19) 0.80909(11) 0.23392(18) 0.0305(7) Uani 1 1 d . . . N182 N 0.55133(18) 0.76025(10) 0.21022(17) 0.0277(7) Uani 1 1 d . . . C143 C 0.6809(2) 0.64482(13) 0.4434(2) 0.0285(8) Uani 1 1 d . . . H143 H 0.7293 0.6327 0.4861 0.034 Uiso 1 1 calc R . . C142 C 0.6253(2) 0.61015(13) 0.3925(2) 0.0242(8) Uani 1 1 d . . . C104 C 0.1634(2) 0.81120(16) -0.0882(3) 0.0449(11) Uani 1 1 d . . . H104 H 0.1287 0.8355 -0.1256 0.054 Uiso 1 1 calc R . . C193 C 0.6625(2) 0.67708(15) 0.1382(2) 0.0371(10) Uani 1 1 d . . . H193 H 0.6977 0.6999 0.1322 0.044 Uiso 1 1 calc R . . C195 C 0.6095(3) 0.59510(16) 0.1248(3) 0.0451(11) Uani 1 1 d . . . H195 H 0.6070 0.5608 0.1091 0.054 Uiso 1 1 calc R . . C136 C 0.5819(2) 0.52210(14) 0.3544(3) 0.0375(10) Uani 1 1 d . . . H136 H 0.5333 0.5353 0.3138 0.045 Uiso 1 1 calc R . . C176 C 0.4196(2) 0.63740(15) 0.3857(2) 0.0336(9) Uani 1 1 d . . . H176 H 0.4171 0.6100 0.3503 0.040 Uiso 1 1 calc R . . C103 C 0.1633(3) 0.76305(16) -0.1161(3) 0.0490(12) Uani 1 1 d . . . H103 H 0.1287 0.7540 -0.1727 0.059 Uiso 1 1 calc R . . C155 C 0.7828(2) 0.81608(14) 0.5212(2) 0.0361(9) Uani 1 1 d . . . H155 H 0.7828 0.8494 0.5020 0.043 Uiso 1 1 calc R . . C123 C 0.2840(3) 0.49225(16) 0.0057(3) 0.0501(12) Uani 1 1 d . . . H123 H 0.2557 0.4805 -0.0506 0.060 Uiso 1 1 calc R . . C105 C 0.2135(2) 0.82455(15) -0.0060(3) 0.0404(10) Uani 1 1 d . . . H105 H 0.2130 0.8578 0.0132 0.049 Uiso 1 1 calc R . . C133 C 0.7225(2) 0.48266(14) 0.4700(2) 0.0369(10) Uani 1 1 d . . . H133 H 0.7711 0.4691 0.5098 0.044 Uiso 1 1 calc R . . C134 C 0.6624(2) 0.45105(14) 0.4214(3) 0.0372(10) Uani 1 1 d . . . H134 H 0.6694 0.4157 0.4279 0.045 Uiso 1 1 calc R . . C154 C 0.8374(2) 0.80246(15) 0.6013(2) 0.0362(9) Uani 1 1 d . . . H154 H 0.8741 0.8264 0.6373 0.043 Uiso 1 1 calc R . . C153 C 0.8382(2) 0.75396(15) 0.6287(2) 0.0373(10) Uani 1 1 d . . . H153 H 0.8751 0.7444 0.6841 0.045 Uiso 1 1 calc R . . C173 C 0.4276(2) 0.71446(16) 0.4888(2) 0.0400(10) Uani 1 1 d . . . H173 H 0.4304 0.7420 0.5240 0.048 Uiso 1 1 calc R . . C192 C 0.6129(2) 0.69321(14) 0.1701(2) 0.0311(9) Uani 1 1 d . . . C175 C 0.4035(2) 0.62847(17) 0.4527(2) 0.0400(10) Uani 1 1 d . . . H175 H 0.3890 0.5958 0.4621 0.048 Uiso 1 1 calc R . . C151 C 0.7292(2) 0.73257(13) 0.4952(2) 0.0248(8) Uani 1 1 d . . . C102 C 0.2136(2) 0.72823(15) -0.0615(2) 0.0405(10) Uani 1 1 d . . . H102 H 0.2133 0.6949 -0.0808 0.049 Uiso 1 1 calc R . . C164 C 0.4871(2) 0.81438(15) 0.4446(2) 0.0402(10) Uani 1 1 d . . . H164 H 0.4875 0.8218 0.4970 0.048 Uiso 1 1 calc R . . C126 C 0.3656(2) 0.52625(14) 0.1684(3) 0.0400(10) Uani 1 1 d . . . H126 H 0.3935 0.5377 0.2250 0.048 Uiso 1 1 calc R . . C132 C 0.7127(2) 0.53453(14) 0.4614(2) 0.0317(9) Uani 1 1 d . . . H132 H 0.7547 0.5562 0.4949 0.038 Uiso 1 1 calc R . . C194 C 0.6600(3) 0.62734(16) 0.1152(3) 0.0444(11) Uani 1 1 d . . . H194 H 0.6934 0.6156 0.0928 0.053 Uiso 1 1 calc R . . C124 C 0.3136(3) 0.45825(15) 0.0710(3) 0.0493(12) Uani 1 1 d . . . H124 H 0.3062 0.4232 0.0599 0.059 Uiso 1 1 calc R . . C135 C 0.5920(3) 0.47038(15) 0.3632(3) 0.0444(11) Uani 1 1 d . . . H135 H 0.5505 0.4485 0.3293 0.053 Uiso 1 1 calc R . . C172 C 0.4425(2) 0.72126(14) 0.4199(2) 0.0292(9) Uani 1 1 d . . . C122 C 0.2947(2) 0.54313(14) 0.0209(2) 0.0394(10) Uani 1 1 d . . . H122 H 0.2730 0.5662 -0.0247 0.047 Uiso 1 1 calc R . . C184 C 0.6632(3) 0.78449(15) 0.2103(3) 0.0436(11) Uani 1 1 d . . . H184 H 0.7100 0.7842 0.2048 0.052 Uiso 1 1 calc R . . C163 C 0.4651(2) 0.76965(14) 0.3993(2) 0.0305(9) Uani 1 1 d . . . C125 C 0.3537(3) 0.47542(15) 0.1523(3) 0.0483(12) Uani 1 1 d . . . H125 H 0.3735 0.4522 0.1978 0.058 Uiso 1 1 calc R . . C174 C 0.4086(2) 0.66726(17) 0.5051(3) 0.0420(11) Uani 1 1 d . . . H174 H 0.3993 0.6617 0.5524 0.050 Uiso 1 1 calc R . . C165 C 0.5078(2) 0.84508(15) 0.3972(2) 0.0392(10) Uani 1 1 d . . . H165 H 0.5268 0.8784 0.4118 0.047 Uiso 1 1 calc R . . Gd2 Gd 0.994037(10) 0.492652(6) 0.775778(10) 0.02145(5) Uani 1 1 d . . . N281 N 0.96880(19) 0.62089(11) 0.70673(19) 0.0319(7) Uani 1 1 d . . . N291 N 0.94681(17) 0.47946(11) 0.61661(17) 0.0276(7) Uani 1 1 d . . . O241 O 1.06943(14) 0.42564(9) 0.76379(14) 0.0269(6) Uani 1 1 d . . . N282 N 0.96030(17) 0.57140(10) 0.68562(18) 0.0267(7) Uani 1 1 d . . . C231 C 1.1274(2) 0.37343(13) 0.7016(2) 0.0266(8) Uani 1 1 d . . . C201 C 0.8568(2) 0.34955(13) 0.7870(2) 0.0260(8) Uani 1 1 d . . . C244 C 1.1670(2) 0.51054(13) 0.7751(2) 0.0257(8) Uani 1 1 d . . . N261 N 1.02271(18) 0.61488(11) 0.86703(19) 0.0310(7) Uani 1 1 d . . . N271 N 1.06065(17) 0.46789(11) 0.93094(18) 0.0280(7) Uani 1 1 d . . . O211 O 0.93127(14) 0.41695(9) 0.77720(15) 0.0277(6) Uani 1 1 d . . . O215 O 0.86314(14) 0.50792(9) 0.73188(15) 0.0272(6) Uani 1 1 d . . . N262 N 1.02450(17) 0.56412(11) 0.87825(18) 0.0264(7) Uani 1 1 d . . . C285 C 0.9585(2) 0.64839(15) 0.6381(3) 0.0412(10) Uani 1 1 d . . . H285 H 0.9607 0.6840 0.6360 0.049 Uiso 1 1 calc R . . C242 C 1.1231(2) 0.42233(13) 0.7408(2) 0.0241(8) Uani 1 1 d . . . C212 C 0.8628(2) 0.40230(13) 0.7607(2) 0.0241(8) Uani 1 1 d . . . C243 C 1.1736(2) 0.46228(13) 0.7482(2) 0.0276(8) Uani 1 1 d . . . H243 H 1.2147 0.4561 0.7339 0.033 Uiso 1 1 calc R . . C252 C 1.2884(2) 0.54500(16) 0.7704(3) 0.0423(11) Uani 1 1 d . . . H252 H 1.3052 0.5119 0.7668 0.051 Uiso 1 1 calc R . . C264 C 1.1047(2) 0.60096(15) 1.0006(3) 0.0423(11) Uani 1 1 d . . . H264 H 1.1413 0.6057 1.0581 0.051 Uiso 1 1 calc R . . C226 C 0.7341(2) 0.56626(14) 0.6545(2) 0.0320(9) Uani 1 1 d . . . H226 H 0.7844 0.5806 0.6720 0.038 Uiso 1 1 calc R . . B2 B 0.9644(3) 0.64117(17) 0.7862(3) 0.0390(12) Uani 1 1 d . . . H2A H 0.9753 0.6777 0.7914 0.047 Uiso 1 1 calc R . . H2B H 0.9109 0.6362 0.7794 0.047 Uiso 1 1 calc R . . C254 C 1.3090(3) 0.63413(17) 0.7746(3) 0.0476(11) Uani 1 1 d . . . H254 H 1.3395 0.6620 0.7735 0.057 Uiso 1 1 calc R . . C294 C 0.8987(2) 0.46548(16) 0.4462(2) 0.0408(10) Uani 1 1 d . . . H294 H 0.8824 0.4605 0.3877 0.049 Uiso 1 1 calc R . . C276 C 1.0713(2) 0.41995(14) 0.9569(2) 0.0341(9) Uani 1 1 d . . . H276 H 1.0522 0.3942 0.9155 0.041 Uiso 1 1 calc R . . C236 C 1.0695(2) 0.33730(13) 0.6861(2) 0.0335(9) Uani 1 1 d . . . H236 H 1.0298 0.3441 0.7024 0.040 Uiso 1 1 calc R . . C221 C 0.7268(2) 0.51527(13) 0.6688(2) 0.0250(8) Uani 1 1 d . . . C293 C 0.9078(2) 0.51322(16) 0.4783(2) 0.0382(10) Uani 1 1 d . . . H293 H 0.8971 0.5415 0.4422 0.046 Uiso 1 1 calc R . . C202 C 0.7867(2) 0.32846(14) 0.7766(2) 0.0363(9) Uani 1 1 d . . . H202 H 0.7395 0.3470 0.7490 0.044 Uiso 1 1 calc R . . C214 C 0.7994(2) 0.48439(13) 0.7090(2) 0.0248(8) Uani 1 1 d . . . C203 C 0.7857(3) 0.28041(15) 0.8066(3) 0.0451(11) Uani 1 1 d . . . H203 H 0.7374 0.2660 0.7977 0.054 Uiso 1 1 calc R . . C253 C 1.3322(3) 0.58584(17) 0.7695(3) 0.0499(12) Uani 1 1 d . . . H253 H 1.3792 0.5806 0.7652 0.060 Uiso 1 1 calc R . . C263 C 1.0746(2) 0.55564(14) 0.9597(2) 0.0293(9) Uani 1 1 d . . . C235 C 1.0685(3) 0.29197(15) 0.6478(3) 0.0418(10) Uani 1 1 d . . . H235 H 1.0284 0.2681 0.6374 0.050 Uiso 1 1 calc R . . C292 C 0.9332(2) 0.51973(14) 0.5647(2) 0.0280(8) Uani 1 1 d . . . C251 C 1.2197(2) 0.55220(14) 0.7765(2) 0.0262(8) Uani 1 1 d . . . C232 C 1.1853(2) 0.36197(14) 0.6776(2) 0.0353(9) Uani 1 1 d . . . H232 H 1.2253 0.3857 0.6869 0.042 Uiso 1 1 calc R . . C234 C 1.1265(3) 0.28174(16) 0.6249(3) 0.0474(12) Uani 1 1 d . . . H234 H 1.1262 0.2508 0.5983 0.057 Uiso 1 1 calc R . . C225 C 0.6682(3) 0.59575(15) 0.6149(2) 0.0393(10) Uani 1 1 d . . . H225 H 0.6735 0.6303 0.6049 0.047 Uiso 1 1 calc R . . C213 C 0.7963(2) 0.43271(13) 0.7230(2) 0.0299(9) Uani 1 1 d . . . H213 H 0.7466 0.4177 0.7062 0.036 Uiso 1 1 calc R . . C272 C 1.0893(2) 0.50409(14) 0.9906(2) 0.0281(8) Uani 1 1 d . . . C265 C 1.0707(2) 0.63687(15) 0.9412(3) 0.0392(10) Uani 1 1 d . . . H265 H 1.0793 0.6720 0.9502 0.047 Uiso 1 1 calc R . . C233 C 1.1845(3) 0.31606(16) 0.6404(3) 0.0470(11) Uani 1 1 d . . . H233 H 1.2248 0.3083 0.6255 0.056 Uiso 1 1 calc R . . C275 C 1.1090(2) 0.40607(15) 1.0413(2) 0.0350(9) Uani 1 1 d . . . H275 H 1.1147 0.3716 1.0571 0.042 Uiso 1 1 calc R . . C283 C 0.9454(2) 0.56884(14) 0.6048(2) 0.0296(9) Uani 1 1 d . . . C223 C 0.5870(2) 0.52652(18) 0.6032(3) 0.0510(12) Uani 1 1 d . . . H223 H 0.5363 0.5128 0.5854 0.061 Uiso 1 1 calc R . . C296 C 0.9365(2) 0.43390(14) 0.5831(2) 0.0310(9) Uani 1 1 d . . . H296 H 0.9457 0.4058 0.6193 0.037 Uiso 1 1 calc R . . C256 C 1.1977(2) 0.60120(14) 0.7830(2) 0.0338(9) Uani 1 1 d . . . H256 H 1.1516 0.6068 0.7888 0.041 Uiso 1 1 calc R . . C222 C 0.6526(2) 0.49630(15) 0.6429(3) 0.0390(10) Uani 1 1 d . . . H222 H 0.6463 0.4618 0.6523 0.047 Uiso 1 1 calc R . . C284 C 0.9446(2) 0.61654(14) 0.5726(3) 0.0397(10) Uani 1 1 d . . . H284 H 0.9362 0.6251 0.5173 0.048 Uiso 1 1 calc R . . C224 C 0.5957(3) 0.57600(17) 0.5899(3) 0.0466(11) Uani 1 1 d . . . H224 H 0.5509 0.5969 0.5632 0.056 Uiso 1 1 calc R . . C273 C 1.1286(2) 0.49258(15) 1.0759(2) 0.0367(10) Uani 1 1 d . . . H273 H 1.1492 0.5187 1.1166 0.044 Uiso 1 1 calc R . . C274 C 1.1377(2) 0.44288(16) 1.1012(2) 0.0391(10) Uani 1 1 d . . . H274 H 1.1636 0.4345 1.1594 0.047 Uiso 1 1 calc R . . C295 C 0.9132(2) 0.42498(15) 0.4988(2) 0.0359(10) Uani 1 1 d . . . H295 H 0.9073 0.3916 0.4776 0.043 Uiso 1 1 calc R . . O245 O 1.11382(14) 0.52313(9) 0.79473(15) 0.0289(6) Uani 1 1 d . . . C206 C 0.9244(2) 0.32118(14) 0.8272(2) 0.0357(9) Uani 1 1 d . . . H206 H 0.9723 0.3345 0.8326 0.043 Uiso 1 1 calc R . . C204 C 0.8530(3) 0.25354(15) 0.8485(3) 0.0486(12) Uani 1 1 d . . . H204 H 0.8517 0.2211 0.8701 0.058 Uiso 1 1 calc R . . C255 C 1.2415(2) 0.64164(16) 0.7813(3) 0.0442(11) Uani 1 1 d . . . H255 H 1.2249 0.6748 0.7846 0.053 Uiso 1 1 calc R . . C205 C 0.9238(3) 0.27407(15) 0.8595(3) 0.0471(11) Uani 1 1 d . . . H205 H 0.9711 0.2558 0.8888 0.056 Uiso 1 1 calc R . . B1 B 0.5056(3) 0.84128(17) 0.2500(3) 0.0367(11) Uani 1 1 d . . . H1A H 0.5237 0.8766 0.2606 0.044 Uiso 1 1 calc R . . H1B H 0.4541 0.8406 0.1993 0.044 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 Gd1 0.02292(10) 0.01836(9) 0.02239(9) 0.00056(7) 0.00943(7) 0.00004(7) O111 0.0263(15) 0.0220(14) 0.0316(14) 0.0010(11) 0.0083(12) -0.0005(11) O145 0.0259(14) 0.0214(13) 0.0293(13) 0.0028(10) 0.0065(12) 0.0002(11) O115 0.0300(15) 0.0236(13) 0.0253(13) 0.0029(10) 0.0036(12) -0.0014(11) O141 0.0283(15) 0.0224(13) 0.0311(14) 0.0012(11) 0.0097(12) -0.0041(11) N161 0.0299(18) 0.0195(16) 0.0251(16) 0.0009(12) 0.0065(14) 0.0017(13) N162 0.0260(17) 0.0240(16) 0.0248(16) -0.0009(12) 0.0098(14) 0.0033(13) N191 0.036(2) 0.0254(17) 0.0296(17) 0.0018(13) 0.0192(15) 0.0012(14) C121 0.027(2) 0.024(2) 0.033(2) 0.0001(16) 0.0119(18) 0.0014(16) C131 0.030(2) 0.0241(19) 0.0277(19) 0.0009(15) 0.0170(17) 0.0007(16) C112 0.024(2) 0.025(2) 0.0256(19) 0.0027(15) 0.0115(16) 0.0022(16) C183 0.035(2) 0.030(2) 0.033(2) 0.0076(16) 0.0218(19) 0.0033(18) N171 0.0246(17) 0.0302(18) 0.0259(16) 0.0042(13) 0.0105(14) -0.0003(14) C196 0.050(3) 0.032(2) 0.044(2) 0.0035(19) 0.026(2) 0.005(2) C144 0.026(2) 0.0259(19) 0.0231(18) -0.0004(15) 0.0140(16) -0.0010(16) C101 0.024(2) 0.029(2) 0.030(2) 0.0063(16) 0.0139(17) 0.0030(16) C114 0.024(2) 0.026(2) 0.0243(19) -0.0014(15) 0.0092(16) -0.0027(16) C106 0.029(2) 0.031(2) 0.040(2) 0.0046(17) 0.0146(19) 0.0014(18) C185 0.054(3) 0.034(2) 0.057(3) 0.004(2) 0.037(2) -0.011(2) C156 0.031(2) 0.030(2) 0.030(2) 0.0001(16) 0.0141(18) -0.0036(17) C113 0.026(2) 0.027(2) 0.0233(19) -0.0003(15) 0.0018(16) 0.0007(16) C152 0.031(2) 0.032(2) 0.034(2) 0.0000(17) 0.0135(18) 0.0033(18) N181 0.037(2) 0.0226(17) 0.0333(17) 0.0053(13) 0.0173(15) -0.0005(14) N182 0.0341(19) 0.0198(16) 0.0303(16) 0.0023(13) 0.0157(15) 0.0017(14) C143 0.026(2) 0.024(2) 0.031(2) 0.0016(15) 0.0089(17) 0.0023(16) C142 0.026(2) 0.0244(19) 0.0240(18) 0.0051(15) 0.0134(16) 0.0054(16) C104 0.038(3) 0.044(3) 0.050(3) 0.023(2) 0.017(2) 0.017(2) C193 0.034(2) 0.041(2) 0.039(2) 0.0035(19) 0.019(2) 0.0054(19) C195 0.058(3) 0.033(2) 0.049(3) -0.001(2) 0.029(2) 0.012(2) C136 0.030(2) 0.025(2) 0.051(3) -0.0011(18) 0.013(2) -0.0022(17) C176 0.028(2) 0.039(2) 0.032(2) 0.0052(17) 0.0113(18) -0.0006(18) C103 0.052(3) 0.046(3) 0.036(2) 0.008(2) 0.009(2) 0.017(2) C155 0.036(2) 0.027(2) 0.048(2) -0.0029(18) 0.022(2) -0.0070(18) C123 0.062(3) 0.035(3) 0.040(2) -0.011(2) 0.012(2) -0.004(2) C105 0.037(3) 0.026(2) 0.059(3) 0.008(2) 0.023(2) 0.0054(19) C133 0.037(3) 0.032(2) 0.041(2) 0.0070(18) 0.017(2) 0.0129(19) C134 0.048(3) 0.019(2) 0.058(3) 0.0056(18) 0.037(2) 0.0056(19) C154 0.026(2) 0.036(2) 0.044(2) -0.0114(19) 0.0137(19) -0.0072(18) C153 0.029(2) 0.041(2) 0.033(2) -0.0066(18) 0.0059(19) -0.0016(19) C173 0.039(3) 0.050(3) 0.034(2) -0.0013(19) 0.019(2) 0.008(2) C192 0.027(2) 0.039(2) 0.030(2) 0.0056(17) 0.0151(17) 0.0037(18) C175 0.033(2) 0.051(3) 0.040(2) 0.011(2) 0.020(2) -0.003(2) C151 0.024(2) 0.026(2) 0.0283(19) -0.0027(15) 0.0154(17) -0.0010(16) C102 0.044(3) 0.038(2) 0.031(2) 0.0032(18) 0.010(2) 0.011(2) C164 0.049(3) 0.039(2) 0.032(2) -0.0060(18) 0.018(2) 0.002(2) C126 0.041(3) 0.030(2) 0.034(2) -0.0016(18) 0.005(2) -0.0034(19) C132 0.031(2) 0.029(2) 0.033(2) -0.0009(17) 0.0125(18) 0.0023(17) C194 0.048(3) 0.049(3) 0.046(3) 0.001(2) 0.030(2) 0.014(2) C124 0.051(3) 0.024(2) 0.064(3) -0.011(2) 0.019(3) -0.009(2) C135 0.040(3) 0.027(2) 0.065(3) -0.006(2) 0.023(2) -0.005(2) C172 0.023(2) 0.037(2) 0.0241(19) 0.0007(16) 0.0076(16) 0.0045(17) C122 0.046(3) 0.029(2) 0.033(2) -0.0030(17) 0.009(2) 0.0050(19) C184 0.046(3) 0.038(2) 0.064(3) 0.002(2) 0.040(2) -0.005(2) C163 0.029(2) 0.039(2) 0.0201(18) -0.0006(16) 0.0079(17) 0.0033(18) C125 0.052(3) 0.026(2) 0.054(3) 0.004(2) 0.013(2) -0.001(2) C174 0.037(3) 0.060(3) 0.036(2) 0.009(2) 0.023(2) 0.004(2) C165 0.044(3) 0.029(2) 0.037(2) -0.0110(18) 0.012(2) -0.0027(19) Gd2 0.02068(10) 0.02038(9) 0.02503(9) -0.00071(7) 0.01193(8) -0.00033(7) N281 0.039(2) 0.0200(16) 0.0414(18) 0.0023(14) 0.0219(16) -0.0016(14) N291 0.0246(18) 0.0303(18) 0.0259(16) 0.0016(13) 0.0098(14) 0.0041(14) O241 0.0243(14) 0.0318(14) 0.0288(13) 0.0017(11) 0.0158(12) 0.0026(11) N282 0.0266(18) 0.0205(16) 0.0336(17) 0.0034(13) 0.0143(15) 0.0001(13) C231 0.031(2) 0.026(2) 0.0222(18) 0.0025(15) 0.0119(16) 0.0046(17) C201 0.026(2) 0.0216(19) 0.030(2) -0.0009(15) 0.0124(17) -0.0038(16) C244 0.025(2) 0.031(2) 0.0182(17) 0.0035(15) 0.0072(15) -0.0001(16) N261 0.0309(19) 0.0215(17) 0.0418(19) -0.0046(14) 0.0177(16) 0.0000(14) N271 0.0275(18) 0.0276(17) 0.0294(17) -0.0006(13) 0.0135(14) 0.0014(14) O211 0.0249(15) 0.0237(13) 0.0384(14) -0.0012(11) 0.0177(12) -0.0020(11) O215 0.0231(14) 0.0237(13) 0.0368(14) -0.0015(11) 0.0154(12) -0.0044(11) N262 0.0242(18) 0.0255(17) 0.0316(17) -0.0039(13) 0.0144(15) 0.0001(13) C285 0.052(3) 0.022(2) 0.059(3) 0.0109(19) 0.033(2) 0.0071(19) C242 0.025(2) 0.026(2) 0.0173(17) 0.0037(14) 0.0060(15) 0.0052(16) C212 0.026(2) 0.0245(19) 0.0226(18) -0.0056(14) 0.0121(16) -0.0055(16) C243 0.026(2) 0.029(2) 0.033(2) -0.0006(16) 0.0177(18) 0.0017(16) C252 0.034(3) 0.043(3) 0.056(3) -0.014(2) 0.025(2) -0.009(2) C264 0.047(3) 0.041(3) 0.038(2) -0.014(2) 0.019(2) -0.007(2) C226 0.029(2) 0.032(2) 0.035(2) 0.0009(17) 0.0147(18) 0.0023(17) B2 0.043(3) 0.026(2) 0.052(3) -0.004(2) 0.024(3) 0.002(2) C254 0.048(3) 0.045(3) 0.055(3) -0.007(2) 0.028(2) -0.022(2) C294 0.045(3) 0.050(3) 0.029(2) -0.0002(19) 0.017(2) -0.002(2) C276 0.035(2) 0.032(2) 0.031(2) -0.0040(17) 0.0114(19) 0.0010(18) C236 0.035(2) 0.028(2) 0.036(2) 0.0044(17) 0.0148(19) 0.0039(18) C221 0.023(2) 0.028(2) 0.0238(18) -0.0049(15) 0.0102(16) 0.0004(16) C293 0.039(3) 0.044(3) 0.031(2) 0.0057(18) 0.0148(19) 0.000(2) C202 0.038(3) 0.028(2) 0.046(2) 0.0036(18) 0.021(2) 0.0001(18) C214 0.026(2) 0.029(2) 0.0203(17) -0.0040(15) 0.0113(16) -0.0014(16) C203 0.047(3) 0.036(3) 0.062(3) 0.000(2) 0.033(2) -0.012(2) C253 0.039(3) 0.057(3) 0.070(3) -0.019(2) 0.038(2) -0.021(2) C263 0.027(2) 0.034(2) 0.033(2) -0.0053(17) 0.0184(18) -0.0012(17) C235 0.051(3) 0.025(2) 0.047(3) -0.0022(18) 0.021(2) -0.006(2) C292 0.023(2) 0.034(2) 0.029(2) 0.0046(16) 0.0137(17) 0.0044(16) C251 0.024(2) 0.033(2) 0.0205(18) -0.0005(15) 0.0091(16) -0.0032(16) C232 0.039(3) 0.030(2) 0.044(2) -0.0031(18) 0.026(2) -0.0003(18) C234 0.069(3) 0.028(2) 0.052(3) -0.005(2) 0.034(3) 0.007(2) C225 0.046(3) 0.034(2) 0.040(2) 0.0034(18) 0.021(2) 0.014(2) C213 0.022(2) 0.028(2) 0.035(2) 0.0001(16) 0.0085(17) -0.0033(16) C272 0.023(2) 0.035(2) 0.031(2) -0.0027(16) 0.0159(17) 0.0024(17) C265 0.043(3) 0.028(2) 0.047(3) -0.0106(19) 0.020(2) -0.0066(19) C233 0.057(3) 0.040(3) 0.061(3) -0.009(2) 0.042(3) 0.003(2) C275 0.037(2) 0.033(2) 0.036(2) 0.0032(18) 0.0170(19) 0.0067(18) C283 0.031(2) 0.029(2) 0.032(2) 0.0086(16) 0.0179(18) 0.0052(17) C223 0.023(2) 0.057(3) 0.066(3) -0.004(2) 0.014(2) -0.002(2) C296 0.029(2) 0.031(2) 0.029(2) 0.0004(16) 0.0106(18) 0.0006(17) C256 0.035(2) 0.030(2) 0.043(2) -0.0021(17) 0.023(2) -0.0024(18) C222 0.030(2) 0.033(2) 0.054(3) -0.0056(19) 0.019(2) -0.0032(18) C284 0.051(3) 0.033(2) 0.043(2) 0.0149(19) 0.028(2) 0.010(2) C224 0.033(3) 0.056(3) 0.043(3) 0.000(2) 0.011(2) 0.019(2) C273 0.040(3) 0.042(2) 0.025(2) -0.0093(18) 0.0123(18) -0.001(2) C274 0.040(3) 0.049(3) 0.027(2) 0.0042(19) 0.0145(19) 0.010(2) C295 0.036(2) 0.041(2) 0.033(2) -0.0082(18) 0.0175(19) -0.0047(19) O245 0.0243(14) 0.0291(14) 0.0375(14) -0.0085(11) 0.0179(12) -0.0046(11) C206 0.035(2) 0.025(2) 0.045(2) -0.0049(17) 0.017(2) -0.0034(18) C204 0.067(3) 0.024(2) 0.064(3) 0.010(2) 0.038(3) -0.001(2) C255 0.047(3) 0.036(2) 0.055(3) -0.005(2) 0.028(2) -0.010(2) C205 0.049(3) 0.024(2) 0.063(3) 0.007(2) 0.021(2) 0.007(2) B1 0.042(3) 0.024(2) 0.041(3) 0.004(2) 0.016(2) 0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O145 2.333(2) . ? Gd1 O111 2.336(2) . ? Gd1 O141 2.339(2) . ? Gd1 O115 2.346(2) . ? Gd1 N182 2.505(3) . ? Gd1 N162 2.529(3) . ? Gd1 N171 2.537(3) . ? Gd1 N191 2.566(3) . ? O111 C112 1.269(4) . ? O145 C144 1.260(4) . ? O115 C114 1.272(4) . ? O141 C142 1.273(4) . ? N161 C165 1.346(4) . ? N161 N162 1.351(4) . ? N161 B1 1.539(5) . ? N162 C163 1.342(4) . ? N191 C196 1.346(5) . ? N191 C192 1.354(4) . ? C121 C126 1.384(5) . ? C121 C122 1.391(5) . ? C121 C114 1.500(5) . ? C131 C136 1.381(5) . ? C131 C132 1.395(5) . ? C131 C142 1.503(5) . ? C112 C113 1.397(5) . ? C112 C101 1.500(5) . ? C183 N182 1.349(4) . ? C183 C184 1.385(5) . ? C183 C192 1.466(5) . ? N171 C176 1.336(4) . ? N171 C172 1.352(4) . ? C196 C195 1.391(5) . ? C144 C143 1.407(5) . ? C144 C151 1.503(5) . ? C101 C102 1.384(5) . ? C101 C106 1.385(5) . ? C114 C113 1.400(5) . ? C106 C105 1.384(5) . ? C185 N181 1.342(5) . ? C185 C184 1.372(5) . ? C156 C155 1.388(5) . ? C156 C151 1.391(5) . ? C152 C151 1.381(5) . ? C152 C153 1.397(5) . ? N181 N182 1.355(4) . ? N181 B1 1.553(5) . ? C143 C142 1.390(5) . ? C104 C103 1.375(6) . ? C104 C105 1.381(6) . ? C193 C194 1.380(5) . ? C193 C192 1.385(5) . ? C195 C194 1.365(6) . ? C136 C135 1.389(5) . ? C176 C175 1.384(5) . ? C103 C102 1.372(5) . ? C155 C154 1.378(5) . ? C123 C124 1.375(6) . ? C123 C122 1.378(5) . ? C133 C134 1.371(5) . ? C133 C132 1.392(5) . ? C134 C135 1.374(5) . ? C154 C153 1.377(5) . ? C173 C174 1.375(6) . ? C173 C172 1.394(5) . ? C175 C174 1.365(6) . ? C164 C165 1.359(5) . ? C164 C163 1.391(5) . ? C126 C125 1.380(5) . ? C124 C125 1.372(6) . ? C172 C163 1.460(5) . ? Gd2 O215 2.307(2) . ? Gd2 O245 2.318(2) . ? Gd2 O211 2.355(2) . ? Gd2 O241 2.369(2) . ? Gd2 N262 2.513(3) . ? Gd2 N282 2.538(3) . ? Gd2 N271 2.546(3) . ? Gd2 N291 2.576(3) . ? N281 N282 1.359(4) . ? N281 C285 1.360(5) . ? N281 B2 1.554(5) . ? N291 C296 1.326(4) . ? N291 C292 1.361(4) . ? O241 C242 1.276(4) . ? N282 C283 1.335(4) . ? C231 C232 1.396(5) . ? C231 C236 1.400(5) . ? C231 C242 1.497(5) . ? C201 C206 1.388(5) . ? C201 C202 1.392(5) . ? C201 C212 1.501(5) . ? C244 O245 1.268(4) . ? C244 C243 1.397(5) . ? C244 C251 1.494(5) . ? N261 C265 1.351(5) . ? N261 N262 1.364(4) . ? N261 B2 1.531(5) . ? N271 C276 1.341(4) . ? N271 C272 1.352(4) . ? O211 C212 1.272(4) . ? O215 C214 1.266(4) . ? N262 C263 1.345(4) . ? C285 C284 1.366(5) . ? C242 C243 1.405(5) . ? C212 C213 1.400(5) . ? C252 C253 1.381(5) . ? C252 C251 1.390(5) . ? C264 C265 1.352(5) . ? C264 C263 1.391(5) . ? C226 C225 1.379(5) . ? C226 C221 1.400(5) . ? C254 C255 1.373(6) . ? C254 C253 1.377(6) . ? C294 C293 1.371(5) . ? C294 C295 1.370(5) . ? C276 C275 1.388(5) . ? C236 C235 1.382(5) . ? C221 C222 1.380(5) . ? C221 C214 1.493(5) . ? C293 C292 1.397(5) . ? C202 C203 1.389(5) . ? C214 C213 1.404(5) . ? C203 C204 1.364(6) . ? C263 C272 1.457(5) . ? C235 C234 1.378(6) . ? C292 C283 1.456(5) . ? C251 C256 1.392(5) . ? C232 C233 1.387(5) . ? C234 C233 1.369(6) . ? C225 C224 1.362(6) . ? C272 C273 1.387(5) . ? C275 C274 1.365(5) . ? C283 C284 1.390(5) . ? C223 C224 1.361(6) . ? C223 C222 1.387(5) . ? C296 C295 1.378(5) . ? C256 C255 1.377(5) . ? C273 C274 1.382(5) . ? C206 C205 1.382(5) . ? C204 C205 1.397(6) . ? 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 O145 Gd1 O111 145.80(8) . . ? O145 Gd1 O141 70.57(8) . . ? O111 Gd1 O141 143.59(8) . . ? O145 Gd1 O115 143.05(8) . . ? O111 Gd1 O115 71.14(8) . . ? O141 Gd1 O115 72.54(8) . . ? O145 Gd1 N182 73.04(9) . . ? O111 Gd1 N182 80.83(9) . . ? O141 Gd1 N182 123.40(9) . . ? O115 Gd1 N182 131.94(9) . . ? O145 Gd1 N162 71.00(9) . . ? O111 Gd1 N162 82.05(8) . . ? O141 Gd1 N162 126.74(8) . . ? O115 Gd1 N162 133.60(9) . . ? N182 Gd1 N162 76.98(9) . . ? O145 Gd1 N171 86.97(9) . . ? O111 Gd1 N171 100.11(9) . . ? O141 Gd1 N171 78.35(9) . . ? O115 Gd1 N171 83.73(9) . . ? N182 Gd1 N171 140.44(9) . . ? N162 Gd1 N171 64.18(9) . . ? O145 Gd1 N191 91.34(9) . . ? O111 Gd1 N191 96.91(9) . . ? O141 Gd1 N191 74.74(9) . . ? O115 Gd1 N191 80.93(9) . . ? N182 Gd1 N191 64.31(9) . . ? N162 Gd1 N191 140.83(9) . . ? N171 Gd1 N191 151.98(9) . . ? C112 O111 Gd1 137.9(2) . . ? C144 O145 Gd1 139.4(2) . . ? C114 O115 Gd1 136.9(2) . . ? C142 O141 Gd1 138.5(2) . . ? C165 N161 N162 109.0(3) . . ? C165 N161 B1 129.0(3) . . ? N162 N161 B1 121.8(3) . . ? C163 N162 N161 106.7(3) . . ? C163 N162 Gd1 117.5(2) . . ? N161 N162 Gd1 129.3(2) . . ? C196 N191 C192 117.4(3) . . ? C196 N191 Gd1 123.6(3) . . ? C192 N191 Gd1 118.2(2) . . ? C126 C121 C122 118.5(3) . . ? C126 C121 C114 118.3(3) . . ? C122 C121 C114 123.3(3) . . ? C136 C131 C132 118.5(3) . . ? C136 C131 C142 118.3(3) . . ? C132 C131 C142 123.2(3) . . ? O111 C112 C113 124.3(3) . . ? O111 C112 C101 116.1(3) . . ? C113 C112 C101 119.5(3) . . ? N182 C183 C184 110.5(3) . . ? N182 C183 C192 118.7(3) . . ? C184 C183 C192 130.8(4) . . ? C176 N171 C172 117.9(3) . . ? C176 N171 Gd1 121.5(2) . . ? C172 N171 Gd1 119.6(2) . . ? N191 C196 C195 122.9(4) . . ? O145 C144 C143 123.8(3) . . ? O145 C144 C151 115.7(3) . . ? C143 C144 C151 120.5(3) . . ? C102 C101 C106 118.3(3) . . ? C102 C101 C112 123.2(3) . . ? C106 C101 C112 118.4(3) . . ? O115 C114 C113 124.0(3) . . ? O115 C114 C121 116.0(3) . . ? C113 C114 C121 120.1(3) . . ? C105 C106 C101 120.7(4) . . ? N181 C185 C184 109.4(4) . . ? C155 C156 C151 119.8(3) . . ? C112 C113 C114 123.4(3) . . ? C151 C152 C153 120.5(4) . . ? C185 N181 N182 109.3(3) . . ? C185 N181 B1 128.3(3) . . ? N182 N181 B1 122.3(3) . . ? C183 N182 N181 106.4(3) . . ? C183 N182 Gd1 116.3(2) . . ? N181 N182 Gd1 127.8(2) . . ? C142 C143 C144 123.0(3) . . ? O141 C142 C143 123.8(3) . . ? O141 C142 C131 115.0(3) . . ? C143 C142 C131 121.1(3) . . ? C103 C104 C105 120.6(4) . . ? C194 C193 C192 118.8(4) . . ? C194 C195 C196 118.7(4) . . ? C131 C136 C135 121.2(4) . . ? N171 C176 C175 123.0(4) . . ? C102 C103 C104 119.2(4) . . ? C154 C155 C156 120.9(4) . . ? C124 C123 C122 120.9(4) . . ? C104 C105 C106 119.5(4) . . ? C134 C133 C132 120.4(4) . . ? C133 C134 C135 120.2(4) . . ? C153 C154 C155 119.5(4) . . ? C154 C153 C152 120.0(4) . . ? C174 C173 C172 119.0(4) . . ? N191 C192 C193 122.4(4) . . ? N191 C192 C183 114.9(3) . . ? C193 C192 C183 122.7(4) . . ? C174 C175 C176 119.0(4) . . ? C152 C151 C156 119.2(3) . . ? C152 C151 C144 123.5(3) . . ? C156 C151 C144 117.3(3) . . ? C103 C102 C101 121.7(4) . . ? C165 C164 C163 104.5(3) . . ? C125 C126 C121 120.7(4) . . ? C133 C132 C131 120.0(4) . . ? C195 C194 C193 119.7(4) . . ? C125 C124 C123 119.3(4) . . ? C134 C135 C136 119.7(4) . . ? N171 C172 C173 121.8(4) . . ? N171 C172 C163 115.4(3) . . ? C173 C172 C163 122.8(3) . . ? C123 C122 C121 120.1(4) . . ? C185 C184 C183 104.4(4) . . ? N162 C163 C164 110.2(3) . . ? N162 C163 C172 118.8(3) . . ? C164 C163 C172 130.9(3) . . ? C124 C125 C126 120.4(4) . . ? C175 C174 C173 119.3(4) . . ? N161 C165 C164 109.5(3) . . ? O215 Gd2 O245 147.86(8) . . ? O215 Gd2 O211 70.64(8) . . ? O245 Gd2 O211 141.12(8) . . ? O215 Gd2 O241 136.11(8) . . ? O245 Gd2 O241 70.58(8) . . ? O211 Gd2 O241 72.25(8) . . ? O215 Gd2 N262 88.24(9) . . ? O245 Gd2 N262 75.10(9) . . ? O211 Gd2 N262 126.17(9) . . ? O241 Gd2 N262 133.30(9) . . ? O215 Gd2 N282 73.49(9) . . ? O245 Gd2 N282 75.71(9) . . ? O211 Gd2 N282 136.81(9) . . ? O241 Gd2 N282 123.69(8) . . ? N262 Gd2 N282 75.05(9) . . ? O215 Gd2 N271 110.13(9) . . ? O245 Gd2 N271 87.61(9) . . ? O211 Gd2 N271 76.89(9) . . ? O241 Gd2 N271 82.97(8) . . ? N262 Gd2 N271 64.70(9) . . ? N282 Gd2 N271 139.23(9) . . ? O215 Gd2 N291 82.48(9) . . ? O245 Gd2 N291 92.03(9) . . ? O211 Gd2 N291 88.30(9) . . ? O241 Gd2 N291 73.79(8) . . ? N262 Gd2 N291 138.65(9) . . ? N282 Gd2 N291 63.66(9) . . ? N271 Gd2 N291 155.43(9) . . ? N282 N281 C285 108.9(3) . . ? N282 N281 B2 122.6(3) . . ? C285 N281 B2 125.9(3) . . ? C296 N291 C292 118.1(3) . . ? C296 N291 Gd2 121.7(2) . . ? C292 N291 Gd2 120.2(2) . . ? C242 O241 Gd2 134.4(2) . . ? C283 N282 N281 106.7(3) . . ? C283 N282 Gd2 120.5(2) . . ? N281 N282 Gd2 131.4(2) . . ? C232 C231 C236 117.6(3) . . ? C232 C231 C242 123.7(3) . . ? C236 C231 C242 118.7(3) . . ? C206 C201 C202 118.2(3) . . ? C206 C201 C212 118.8(3) . . ? C202 C201 C212 123.0(3) . . ? O245 C244 C243 123.2(3) . . ? O245 C244 C251 115.2(3) . . ? C243 C244 C251 121.4(3) . . ? C265 N261 N262 109.0(3) . . ? C265 N261 B2 127.0(3) . . ? N262 N261 B2 123.3(3) . . ? C276 N271 C272 117.6(3) . . ? C276 N271 Gd2 122.9(2) . . ? C272 N271 Gd2 119.5(2) . . ? C212 O211 Gd2 137.8(2) . . ? C214 O215 Gd2 140.2(2) . . ? C263 N262 N261 106.4(3) . . ? C263 N262 Gd2 118.1(2) . . ? N261 N262 Gd2 131.4(2) . . ? N281 C285 C284 109.0(3) . . ? O241 C242 C243 122.9(3) . . ? O241 C242 C231 115.8(3) . . ? C243 C242 C231 121.2(3) . . ? O211 C212 C213 123.9(3) . . ? O211 C212 C201 115.7(3) . . ? C213 C212 C201 120.4(3) . . ? C244 C243 C242 124.1(3) . . ? C253 C252 C251 120.1(4) . . ? C265 C264 C263 105.5(4) . . ? C225 C226 C221 120.0(4) . . ? N261 B2 N281 112.1(3) . . ? C255 C254 C253 119.4(4) . . ? C293 C294 C295 119.8(4) . . ? N271 C276 C275 123.3(4) . . ? C235 C236 C231 121.8(4) . . ? C222 C221 C226 117.9(3) . . ? C222 C221 C214 123.9(3) . . ? C226 C221 C214 118.1(3) . . ? C294 C293 C292 119.2(4) . . ? C203 C202 C201 120.2(4) . . ? O215 C214 C213 122.8(3) . . ? O215 C214 C221 116.0(3) . . ? C213 C214 C221 121.1(3) . . ? C204 C203 C202 121.1(4) . . ? C254 C253 C252 121.0(4) . . ? N262 C263 C264 109.9(3) . . ? N262 C263 C272 119.1(3) . . ? C264 C263 C272 131.0(4) . . ? C234 C235 C236 119.2(4) . . ? N291 C292 C293 120.9(3) . . ? N291 C292 C283 115.8(3) . . ? C293 C292 C283 123.3(3) . . ? C252 C251 C256 118.2(4) . . ? C252 C251 C244 124.0(3) . . ? C256 C251 C244 117.9(3) . . ? C233 C232 C231 120.2(4) . . ? C233 C234 C235 120.2(4) . . ? C224 C225 C226 120.9(4) . . ? C212 C213 C214 123.1(3) . . ? N271 C272 C273 121.8(3) . . ? N271 C272 C263 115.7(3) . . ? C273 C272 C263 122.5(3) . . ? N261 C265 C264 109.2(3) . . ? C234 C233 C232 120.9(4) . . ? C274 C275 C276 118.7(4) . . ? N282 C283 C284 110.8(3) . . ? N282 C283 C292 118.8(3) . . ? C284 C283 C292 130.4(3) . . ? C224 C223 C222 119.6(4) . . ? N291 C296 C295 123.8(4) . . ? C255 C256 C251 121.2(4) . . ? C221 C222 C223 121.3(4) . . ? C285 C284 C283 104.7(3) . . ? C225 C224 C223 120.3(4) . . ? C274 C273 C272 119.5(4) . . ? C275 C274 C273 119.1(4) . . ? C294 C295 C296 118.2(4) . . ? C244 O245 Gd2 137.8(2) . . ? C205 C206 C201 121.6(4) . . ? C203 C204 C205 119.5(4) . . ? C254 C255 C256 120.1(4) . . ? C206 C205 C204 119.3(4) . . ? N161 B1 N181 110.5(3) . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.255 _refine_diff_density_min -1.241 _refine_diff_density_rms 0.109 #=END data_mick _database_code_depnum_ccdc_archive 'CCDC 229469' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46.25 H36.50 B Cl0.50 Eu N6 O4' _chemical_formula_sum 'C46.25 H36.50 B Cl0.50 Eu N6 O4' _chemical_formula_weight 920.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -8.9294 11.1857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.21030(10) _cell_length_b 26.6410(2) _cell_length_c 17.80700(10) _cell_angle_alpha 90.00 _cell_angle_beta 117.45(2) _cell_angle_gamma 90.00 _cell_volume 8087.48(9) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6949 _cell_measurement_theta_min 5.184 _cell_measurement_theta_max 140.113 _exptl_crystal_description Needle _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.513 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3716 _exptl_absorpt_coefficient_mu 11.830 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.1559 _exptl_absorpt_correction_T_max 0.2699 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 55578 _diffrn_reflns_av_R_equivalents 0.0379 _diffrn_reflns_av_sigmaI/netI 0.0329 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 70.13 _reflns_number_total 14537 _reflns_number_gt 13520 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0387P)^2^+2.7714P] 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 14537 _refine_ls_number_parameters 1069 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0294 _refine_ls_R_factor_gt 0.0264 _refine_ls_wR_factor_ref 0.0677 _refine_ls_wR_factor_gt 0.0662 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 Eu1 Eu 0.494690(7) 0.992083(5) 0.276435(8) 0.00693(4) Uani 1 1 d . . . Eu2 Eu 1.007864(7) 0.804871(5) 0.236025(8) 0.00675(4) Uani 1 1 d . . . B1 B 0.46635(16) 1.14171(10) 0.28754(19) 0.0182(6) Uani 1 1 d . . . H1A H 0.4781 1.1781 0.2932 0.022 Uiso 1 1 calc R . . H1B H 0.4124 1.1372 0.2800 0.022 Uiso 1 1 calc R . . C101 C 0.35553(13) 0.84899(8) 0.28668(15) 0.0131(5) Uani 1 1 d . . . C102 C 0.42352(14) 0.82084(9) 0.32810(17) 0.0191(5) Uani 1 1 d . . . H102 H 0.4719 0.8342 0.3347 0.023 Uiso 1 1 calc R . . C103 C 0.42228(16) 0.77363(9) 0.35996(18) 0.0254(6) Uani 1 1 d . . . H103 H 0.4697 0.7554 0.3896 0.031 Uiso 1 1 calc R . . C104 C 0.35192(16) 0.75304(10) 0.34861(18) 0.0261(6) Uani 1 1 d . . . H104 H 0.3508 0.7207 0.3705 0.031 Uiso 1 1 calc R . . C105 C 0.28333(16) 0.77996(9) 0.30524(18) 0.0249(6) Uani 1 1 d . . . H105 H 0.2347 0.7656 0.2959 0.030 Uiso 1 1 calc R . . C106 C 0.28504(14) 0.82761(9) 0.27539(16) 0.0191(5) Uani 1 1 d . . . H106 H 0.2376 0.8460 0.2468 0.023 Uiso 1 1 calc R . . O111 O 0.43050(9) 0.91621(6) 0.27663(10) 0.0136(3) Uani 1 1 d . . . C112 C 0.36186(13) 0.90176(8) 0.26002(14) 0.0119(5) Uani 1 1 d . . . C113 C 0.29503(13) 0.93231(8) 0.22162(15) 0.0144(5) Uani 1 1 d . . . H113 H 0.2450 0.9174 0.2043 0.017 Uiso 1 1 calc R . . C114 C 0.29862(13) 0.98391(8) 0.20763(14) 0.0110(5) Uani 1 1 d . . . O115 O 0.36285(9) 1.00743(5) 0.23016(10) 0.0126(3) Uani 1 1 d . . . C121 C 0.22637(13) 1.01538(8) 0.16791(14) 0.0118(5) Uani 1 1 d . . . C122 C 0.15119(14) 0.99631(9) 0.14178(17) 0.0186(5) Uani 1 1 d . . . H122 H 0.1446 0.9618 0.1507 0.022 Uiso 1 1 calc R . . C123 C 0.08581(15) 1.02701(10) 0.10293(17) 0.0250(6) Uani 1 1 d . . . H123 H 0.0349 1.0135 0.0852 0.030 Uiso 1 1 calc R . . C124 C 0.09469(15) 1.07708(10) 0.09007(17) 0.0249(6) Uani 1 1 d . . . H124 H 0.0499 1.0981 0.0634 0.030 Uiso 1 1 calc R . . C125 C 0.16894(15) 1.09667(9) 0.11599(16) 0.0197(5) Uani 1 1 d . . . H125 H 0.1750 1.1312 0.1073 0.024 Uiso 1 1 calc R . . C126 C 0.23443(14) 1.06624(9) 0.15451(15) 0.0153(5) Uani 1 1 d . . . H126 H 0.2852 1.0800 0.1719 0.018 Uiso 1 1 calc R . . C131 C 0.62703(13) 0.87324(8) 0.19991(15) 0.0127(5) Uani 1 1 d . . . C132 C 0.56861(14) 0.83760(8) 0.18438(16) 0.0167(5) Uani 1 1 d . . . H132 H 0.5293 0.8444 0.2012 0.020 Uiso 1 1 calc R . . C133 C 0.56704(15) 0.79242(9) 0.14479(17) 0.0226(6) Uani 1 1 d . . . H133 H 0.5264 0.7688 0.1340 0.027 Uiso 1 1 calc R . . C134 C 0.62455(17) 0.78179(9) 0.12114(18) 0.0264(6) Uani 1 1 d . . . H134 H 0.6238 0.7508 0.0943 0.032 Uiso 1 1 calc R . . C135 C 0.68295(16) 0.81621(10) 0.13671(18) 0.0257(6) Uani 1 1 d . . . H135 H 0.7228 0.8087 0.1210 0.031 Uiso 1 1 calc R . . C136 C 0.68448(14) 0.86192(9) 0.17516(16) 0.0185(5) Uani 1 1 d . . . H136 H 0.7248 0.8855 0.1846 0.022 Uiso 1 1 calc R . . O141 O 0.57044(9) 0.92492(6) 0.26420(10) 0.0129(3) Uani 1 1 d . . . C142 C 0.62345(12) 0.92203(8) 0.24074(14) 0.0108(5) Uani 1 1 d . . . C143 C 0.67442(13) 0.96172(8) 0.24798(15) 0.0123(5) Uani 1 1 d . . . H143 H 0.7151 0.9556 0.2329 0.015 Uiso 1 1 calc R . . C144 C 0.66842(13) 1.00991(8) 0.27631(14) 0.0111(5) Uani 1 1 d . . . O145 O 0.61608(9) 1.02194(6) 0.29800(11) 0.0151(3) Uani 1 1 d . . . C151 C 0.72111(13) 1.05186(8) 0.27837(14) 0.0116(5) Uani 1 1 d . . . C152 C 0.78987(14) 1.04491(9) 0.27124(17) 0.0191(5) Uani 1 1 d . . . H152 H 0.8065 1.0119 0.2668 0.023 Uiso 1 1 calc R . . C153 C 0.83414(15) 1.08602(9) 0.27058(17) 0.0228(6) Uani 1 1 d . . . H153 H 0.8813 1.0810 0.2667 0.027 Uiso 1 1 calc R . . C154 C 0.80995(15) 1.13419(9) 0.27552(17) 0.0226(6) Uani 1 1 d . . . H154 H 0.8399 1.1622 0.2741 0.027 Uiso 1 1 calc R . . C155 C 0.74181(15) 1.14148(9) 0.28253(17) 0.0228(6) Uani 1 1 d . . . H155 H 0.7252 1.1746 0.2862 0.027 Uiso 1 1 calc R . . C156 C 0.69790(14) 1.10078(9) 0.28423(16) 0.0189(5) Uani 1 1 d . . . H156 H 0.6514 1.1061 0.2894 0.023 Uiso 1 1 calc R . . N161 N 0.56132(11) 0.96722(7) 0.43302(12) 0.0137(4) Uani 1 1 d . . . C162 C 0.58930(13) 1.00321(9) 0.49293(16) 0.0132(5) Uani 1 1 d . . . C163 C 0.62721(14) 0.99217(9) 0.57848(16) 0.0180(5) Uani 1 1 d . . . H163 H 0.6467 1.0184 0.6191 0.022 Uiso 1 1 calc R . . C164 C 0.63643(14) 0.94234(9) 0.60433(16) 0.0195(5) Uani 1 1 d . . . H164 H 0.6616 0.9339 0.6627 0.023 Uiso 1 1 calc R . . C165 C 0.60811(14) 0.90533(9) 0.54292(16) 0.0178(5) Uani 1 1 d . . . H165 H 0.6134 0.8709 0.5585 0.021 Uiso 1 1 calc R . . C166 C 0.57223(14) 0.91906(9) 0.45923(16) 0.0176(5) Uani 1 1 d . . . H166 H 0.5542 0.8933 0.4176 0.021 Uiso 1 1 calc R . . N171 N 0.52482(11) 1.11448(7) 0.36934(13) 0.0151(4) Uani 1 1 d . . . N172 N 0.52559(11) 1.06381(7) 0.37973(13) 0.0125(4) Uani 1 1 d . . . C173 C 0.57541(13) 1.05513(8) 0.46157(15) 0.0124(5) Uani 1 1 d . . . C174 C 0.60617(14) 1.09997(9) 0.50444(17) 0.0198(5) Uani 1 1 d . . . H174 H 0.6422 1.1043 0.5625 0.024 Uiso 1 1 calc R . . C175 C 0.57245(14) 1.13651(9) 0.44349(17) 0.0199(5) Uani 1 1 d . . . H175 H 0.5814 1.1716 0.4523 0.024 Uiso 1 1 calc R . . N181 N 0.47105(11) 1.12110(7) 0.20814(13) 0.0148(4) Uani 1 1 d . . . N182 N 0.46169(11) 1.07163(7) 0.18685(13) 0.0126(4) Uani 1 1 d . . . C183 C 0.44746(13) 1.06928(9) 0.10565(15) 0.0141(5) Uani 1 1 d . . . C184 C 0.44706(15) 1.11714(9) 0.07345(17) 0.0216(6) Uani 1 1 d . . . H184 H 0.4382 1.1260 0.0181 0.026 Uiso 1 1 calc R . . C185 C 0.46254(15) 1.14847(9) 0.14088(17) 0.0207(6) Uani 1 1 d . . . H185 H 0.4666 1.1840 0.1400 0.025 Uiso 1 1 calc R . . N191 N 0.44758(11) 0.98012(7) 0.11626(12) 0.0128(4) Uani 1 1 d . . . C192 C 0.43354(13) 1.01994(9) 0.06458(15) 0.0140(5) Uani 1 1 d . . . C193 C 0.40748(14) 1.01466(9) -0.02196(16) 0.0189(5) Uani 1 1 d . . . H193 H 0.3967 1.0434 -0.0571 0.023 Uiso 1 1 calc R . . C194 C 0.39745(14) 0.96697(10) -0.05607(16) 0.0212(5) Uani 1 1 d . . . H194 H 0.3808 0.9625 -0.1148 0.025 Uiso 1 1 calc R . . C195 C 0.41204(14) 0.92575(9) -0.00341(16) 0.0186(5) Uani 1 1 d . . . H195 H 0.4056 0.8926 -0.0252 0.022 Uiso 1 1 calc R . . C196 C 0.43617(13) 0.93407(8) 0.08148(15) 0.0148(5) Uani 1 1 d . . . H196 H 0.4452 0.9058 0.1173 0.018 Uiso 1 1 calc R . . B2 B 0.99404(16) 0.65684(10) 0.24611(19) 0.0170(6) Uani 1 1 d . . . H2A H 1.0457 0.6576 0.2972 0.020 Uiso 1 1 calc R . . H2B H 0.9762 0.6215 0.2347 0.020 Uiso 1 1 calc R . . C201 C 1.16550(13) 0.93890(8) 0.39602(15) 0.0133(5) Uani 1 1 d . . . C202 C 1.13620(14) 0.97315(8) 0.32971(16) 0.0167(5) Uani 1 1 d . . . H202 H 1.1061 0.9614 0.2734 0.020 Uiso 1 1 calc R . . C203 C 1.15010(15) 1.02389(9) 0.34412(17) 0.0218(6) Uani 1 1 d . . . H203 H 1.1304 1.0467 0.2980 0.026 Uiso 1 1 calc R . . C204 C 1.19288(15) 1.04149(9) 0.42616(18) 0.0230(6) Uani 1 1 d . . . H204 H 1.2014 1.0765 0.4365 0.028 Uiso 1 1 calc R . . C205 C 1.22298(15) 1.00807(9) 0.49254(18) 0.0227(6) Uani 1 1 d . . . H205 H 1.2530 1.0201 0.5487 0.027 Uiso 1 1 calc R . . C206 C 1.20972(14) 0.95677(9) 0.47807(16) 0.0182(5) Uani 1 1 d . . . H206 H 1.2309 0.9339 0.5242 0.022 Uiso 1 1 calc R . . O211 O 1.08739(9) 0.87468(6) 0.30453(10) 0.0142(3) Uani 1 1 d . . . C212 C 1.14564(13) 0.88436(8) 0.37528(15) 0.0114(5) Uani 1 1 d . . . C213 C 1.19253(14) 0.84756(8) 0.43281(15) 0.0154(5) Uani 1 1 d . . . H213 H 1.2357 0.8582 0.4841 0.018 Uiso 1 1 calc R . . C214 C 1.17876(13) 0.79597(8) 0.41835(15) 0.0121(5) Uani 1 1 d . . . O215 O 1.12040(9) 0.77729(5) 0.35415(10) 0.0142(3) Uani 1 1 d . . . C221 C 1.23549(13) 0.75930(8) 0.47937(15) 0.0134(5) Uani 1 1 d . . . C222 C 1.28700(15) 0.77172(9) 0.56226(17) 0.0213(6) Uani 1 1 d . . . H222 H 1.2874 0.8050 0.5815 0.026 Uiso 1 1 calc R . . C223 C 1.33820(16) 0.73632(10) 0.61780(18) 0.0281(6) Uani 1 1 d . . . H223 H 1.3732 0.7454 0.6744 0.034 Uiso 1 1 calc R . . C224 C 1.33756(15) 0.68787(9) 0.58968(18) 0.0240(6) Uani 1 1 d . . . H224 H 1.3720 0.6634 0.6272 0.029 Uiso 1 1 calc R . . C225 C 1.28677(14) 0.67492(9) 0.50689(17) 0.0202(6) Uani 1 1 d . . . H225 H 1.2869 0.6417 0.4877 0.024 Uiso 1 1 calc R . . C226 C 1.23582(13) 0.71016(8) 0.45193(16) 0.0161(5) Uani 1 1 d . . . H226 H 1.2009 0.7009 0.3953 0.019 Uiso 1 1 calc R . . C231 C 0.85803(13) 0.94513(8) 0.09593(15) 0.0118(5) Uani 1 1 d . . . C232 C 0.78754(14) 0.96586(9) 0.03741(16) 0.0164(5) Uani 1 1 d . . . H232 H 0.7455 0.9444 0.0025 0.020 Uiso 1 1 calc R . . C233 C 0.77762(15) 1.01762(9) 0.02926(17) 0.0188(5) Uani 1 1 d . . . H233 H 0.7293 1.0313 -0.0117 0.023 Uiso 1 1 calc R . . C234 C 0.83800(15) 1.04918(9) 0.08069(17) 0.0193(5) Uani 1 1 d . . . H234 H 0.8311 1.0845 0.0754 0.023 Uiso 1 1 calc R . . C235 C 0.90860(15) 1.02910(9) 0.13997(18) 0.0226(6) Uani 1 1 d . . . H235 H 0.9502 1.0507 0.1753 0.027 Uiso 1 1 calc R . . C236 C 0.91852(14) 0.97750(9) 0.14780(16) 0.0176(5) Uani 1 1 d . . . H236 H 0.9669 0.9640 0.1888 0.021 Uiso 1 1 calc R . . O241 O 0.94131(9) 0.87718(5) 0.16356(10) 0.0133(3) Uani 1 1 d . . . C242 C 0.87378(13) 0.88984(8) 0.10667(14) 0.0104(5) Uani 1 1 d . . . C243 C 0.81695(13) 0.85517(8) 0.05482(15) 0.0137(5) Uani 1 1 d . . . H243 H 0.7680 0.8675 0.0128 0.016 Uiso 1 1 calc R . . C244 C 0.82934(13) 0.80316(8) 0.06244(15) 0.0107(5) Uani 1 1 d . . . O245 O 0.88949(9) 0.78236(5) 0.12035(10) 0.0136(3) Uani 1 1 d . . . C251 C 0.76805(12) 0.76806(8) 0.00166(15) 0.0114(5) Uani 1 1 d . . . C252 C 0.71213(13) 0.78212(9) -0.07870(16) 0.0160(5) Uani 1 1 d . . . H252 H 0.7108 0.8157 -0.0973 0.019 Uiso 1 1 calc R . . C253 C 0.65794(14) 0.74732(9) -0.13220(16) 0.0191(5) Uani 1 1 d . . . H253 H 0.6204 0.7571 -0.1875 0.023 Uiso 1 1 calc R . . C254 C 0.65846(14) 0.69832(9) -0.10514(17) 0.0178(5) Uani 1 1 d . . . H254 H 0.6213 0.6746 -0.1416 0.021 Uiso 1 1 calc R . . C255 C 0.71343(14) 0.68433(9) -0.02475(17) 0.0183(5) Uani 1 1 d . . . H255 H 0.7132 0.6511 -0.0055 0.022 Uiso 1 1 calc R . . C256 C 0.76883(13) 0.71844(8) 0.02796(16) 0.0149(5) Uani 1 1 d . . . H256 H 0.8076 0.7081 0.0823 0.018 Uiso 1 1 calc R . . N261 N 0.93196(11) 0.83586(7) 0.31552(12) 0.0144(4) Uani 1 1 d . . . C262 C 0.88286(13) 0.80318(8) 0.32534(15) 0.0144(5) Uani 1 1 d . . . C263 C 0.83310(14) 0.81799(9) 0.35833(16) 0.0184(5) Uani 1 1 d . . . H263 H 0.7995 0.7943 0.3653 0.022 Uiso 1 1 calc R . . C264 C 0.83309(15) 0.86752(9) 0.38085(17) 0.0208(5) Uani 1 1 d . . . H264 H 0.7993 0.8784 0.4032 0.025 Uiso 1 1 calc R . . C265 C 0.88286(15) 0.90116(9) 0.37054(16) 0.0199(5) Uani 1 1 d . . . H265 H 0.8839 0.9354 0.3858 0.024 Uiso 1 1 calc R . . C266 C 0.93112(14) 0.88394(9) 0.33756(16) 0.0168(5) Uani 1 1 d . . . H266 H 0.9651 0.9071 0.3302 0.020 Uiso 1 1 calc R . . N271 N 0.93383(12) 0.68864(7) 0.26173(13) 0.0153(4) Uani 1 1 d . . . N272 N 0.94682(11) 0.73735(7) 0.28627(12) 0.0118(4) Uani 1 1 d . . . C273 C 0.88592(13) 0.75153(8) 0.29941(15) 0.0140(5) Uani 1 1 d . . . C274 C 0.83369(15) 0.71171(9) 0.28306(18) 0.0228(6) Uani 1 1 d . . . H274 H 0.7863 0.7115 0.2875 0.027 Uiso 1 1 calc R . . C275 C 0.86623(15) 0.67282(9) 0.25917(17) 0.0222(6) Uani 1 1 d . . . H275 H 0.8445 0.6401 0.2434 0.027 Uiso 1 1 calc R . . N281 N 1.00195(11) 0.67853(7) 0.16934(12) 0.0129(4) Uani 1 1 d . . . N282 N 1.02967(11) 0.72546(7) 0.17061(12) 0.0116(4) Uani 1 1 d . . . C283 C 1.03488(13) 0.73035(8) 0.09799(15) 0.0137(5) Uani 1 1 d . . . C284 C 1.01160(15) 0.68612(9) 0.05077(16) 0.0205(5) Uani 1 1 d . . . H284 H 1.0101 0.6793 -0.0023 0.025 Uiso 1 1 calc R . . C285 C 0.99135(14) 0.65478(9) 0.09847(16) 0.0193(5) Uani 1 1 d . . . H285 H 0.9727 0.6214 0.0836 0.023 Uiso 1 1 calc R . . N291 N 1.06200(10) 0.81708(7) 0.12978(12) 0.0119(4) Uani 1 1 d . . . C292 C 1.05766(12) 0.77920(8) 0.07792(15) 0.0124(5) Uani 1 1 d . . . C293 C 1.07137(14) 0.78615(9) 0.00850(16) 0.0182(5) Uani 1 1 d . . . H293 H 1.0670 0.7589 -0.0278 0.022 Uiso 1 1 calc R . . C294 C 1.09142(14) 0.83347(10) -0.00678(16) 0.0203(6) Uani 1 1 d . . . H294 H 1.1011 0.8391 -0.0538 0.024 Uiso 1 1 calc R . . C295 C 1.09731(13) 0.87232(9) 0.04675(16) 0.0183(5) Uani 1 1 d . . . H295 H 1.1120 0.9050 0.0379 0.022 Uiso 1 1 calc R . . C296 C 1.08135(13) 0.86291(9) 0.11386(15) 0.0148(5) Uani 1 1 d . . . H296 H 1.0842 0.8899 0.1500 0.018 Uiso 1 1 calc R . . C300 C 0.9534(3) 0.0290(2) 0.4808(4) 0.0305(13) Uani 0.50 1 d P . . Cl1 Cl 1.00764(5) 0.01142(3) 0.42412(6) 0.04214(19) Uani 1 1 d . . . H302 H 0.967(4) 0.066(3) 0.504(4) 0.051 Uiso 0.50 1 d P . . H301 H 0.897(4) 0.021(2) 0.445(4) 0.051 Uiso 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.00572(7) 0.00572(7) 0.00990(8) -0.00018(5) 0.00408(6) -0.00014(4) Eu2 0.00706(7) 0.00405(7) 0.00828(8) 0.00031(4) 0.00280(6) 0.00020(4) B1 0.0192(15) 0.0092(14) 0.0276(18) -0.0003(11) 0.0121(13) 0.0043(10) C101 0.0168(12) 0.0098(12) 0.0141(13) -0.0024(9) 0.0083(10) -0.0022(9) C102 0.0170(13) 0.0118(12) 0.0279(15) -0.0009(10) 0.0098(11) -0.0017(9) C103 0.0257(15) 0.0149(13) 0.0315(17) 0.0025(11) 0.0096(13) 0.0051(10) C104 0.0383(17) 0.0127(13) 0.0332(17) 0.0042(11) 0.0215(14) -0.0003(11) C105 0.0255(15) 0.0171(14) 0.0387(18) 0.0014(11) 0.0205(13) -0.0047(10) C106 0.0184(13) 0.0145(13) 0.0265(15) 0.0009(10) 0.0122(11) -0.0002(9) O111 0.0098(8) 0.0106(8) 0.0208(9) 0.0006(6) 0.0074(7) -0.0022(6) C112 0.0165(12) 0.0098(11) 0.0104(13) -0.0045(9) 0.0070(10) -0.0032(8) C113 0.0095(11) 0.0114(12) 0.0194(14) -0.0003(9) 0.0043(10) -0.0034(8) C114 0.0101(11) 0.0140(12) 0.0101(12) -0.0032(9) 0.0057(10) -0.0018(8) O115 0.0092(8) 0.0106(8) 0.0191(10) -0.0001(6) 0.0074(7) -0.0007(6) C121 0.0115(12) 0.0159(12) 0.0083(12) -0.0011(9) 0.0046(10) 0.0006(8) C122 0.0152(13) 0.0161(13) 0.0243(15) -0.0032(10) 0.0090(11) -0.0014(9) C123 0.0127(13) 0.0319(16) 0.0272(16) -0.0051(12) 0.0064(12) 0.0010(10) C124 0.0166(14) 0.0304(16) 0.0222(15) 0.0012(11) 0.0041(12) 0.0119(11) C125 0.0254(14) 0.0152(13) 0.0196(14) 0.0028(10) 0.0113(11) 0.0077(10) C126 0.0129(12) 0.0163(12) 0.0172(14) 0.0003(9) 0.0072(10) 0.0017(9) C131 0.0147(12) 0.0107(12) 0.0108(13) 0.0033(9) 0.0043(10) 0.0038(8) C132 0.0163(12) 0.0124(12) 0.0205(14) 0.0028(9) 0.0078(11) 0.0021(9) C133 0.0287(15) 0.0110(13) 0.0272(16) -0.0002(10) 0.0121(12) -0.0019(10) C134 0.0397(17) 0.0129(13) 0.0286(17) -0.0050(11) 0.0174(14) 0.0034(11) C135 0.0335(16) 0.0213(14) 0.0320(17) -0.0042(11) 0.0234(14) 0.0040(11) C136 0.0210(13) 0.0154(13) 0.0222(15) -0.0007(10) 0.0126(11) -0.0003(9) O141 0.0125(8) 0.0124(8) 0.0169(9) 0.0006(6) 0.0094(7) 0.0020(6) C142 0.0092(11) 0.0136(12) 0.0075(12) 0.0059(9) 0.0019(9) 0.0052(8) C143 0.0087(11) 0.0142(12) 0.0154(13) -0.0002(9) 0.0068(10) 0.0016(8) C144 0.0076(11) 0.0170(12) 0.0059(12) 0.0013(9) 0.0007(9) 0.0003(8) O145 0.0115(8) 0.0155(8) 0.0225(10) -0.0041(7) 0.0115(7) -0.0022(6) C151 0.0102(11) 0.0146(12) 0.0082(12) -0.0002(9) 0.0027(9) -0.0020(8) C152 0.0164(13) 0.0170(13) 0.0265(15) -0.0047(10) 0.0121(11) -0.0030(9) C153 0.0150(13) 0.0269(15) 0.0311(16) -0.0044(11) 0.0146(12) -0.0057(10) C154 0.0221(14) 0.0204(14) 0.0275(16) -0.0029(11) 0.0133(12) -0.0111(10) C155 0.0229(14) 0.0148(13) 0.0326(17) -0.0023(11) 0.0145(13) -0.0038(10) C156 0.0164(13) 0.0181(13) 0.0240(15) -0.0020(10) 0.0109(11) -0.0012(9) N161 0.0129(10) 0.0130(10) 0.0151(11) -0.0006(8) 0.0063(9) 0.0000(7) C162 0.0081(12) 0.0172(12) 0.0160(14) -0.0028(9) 0.0069(10) -0.0003(8) C163 0.0197(13) 0.0196(13) 0.0154(14) -0.0045(10) 0.0086(11) -0.0002(9) C164 0.0167(13) 0.0282(15) 0.0140(14) 0.0034(10) 0.0076(11) 0.0071(10) C165 0.0172(13) 0.0160(13) 0.0200(14) 0.0039(10) 0.0084(11) 0.0049(9) C166 0.0184(13) 0.0155(13) 0.0158(14) -0.0014(10) 0.0051(11) 0.0011(9) N171 0.0171(11) 0.0070(10) 0.0233(12) -0.0019(8) 0.0111(9) -0.0002(7) N172 0.0123(10) 0.0099(10) 0.0190(12) -0.0011(8) 0.0104(9) -0.0004(7) C173 0.0104(11) 0.0132(12) 0.0157(13) -0.0023(9) 0.0079(10) 0.0008(8) C174 0.0187(13) 0.0196(13) 0.0200(15) -0.0081(10) 0.0078(11) -0.0035(10) C175 0.0232(14) 0.0118(13) 0.0277(16) -0.0078(10) 0.0142(12) -0.0056(9) N181 0.0178(11) 0.0075(10) 0.0206(12) 0.0006(8) 0.0102(9) 0.0006(7) N182 0.0117(10) 0.0082(10) 0.0181(12) -0.0012(8) 0.0070(9) -0.0001(7) C183 0.0111(12) 0.0162(12) 0.0159(14) 0.0036(9) 0.0069(10) 0.0022(9) C184 0.0260(14) 0.0173(13) 0.0255(16) 0.0084(10) 0.0153(12) 0.0055(10) C185 0.0275(14) 0.0082(12) 0.0308(16) 0.0060(10) 0.0172(12) 0.0035(9) N191 0.0099(10) 0.0136(10) 0.0142(11) 0.0023(8) 0.0050(8) 0.0012(7) C192 0.0096(11) 0.0159(12) 0.0167(14) 0.0019(9) 0.0062(10) 0.0005(8) C193 0.0187(13) 0.0210(14) 0.0160(14) 0.0040(10) 0.0071(11) -0.0002(10) C194 0.0197(13) 0.0318(15) 0.0096(14) -0.0032(10) 0.0048(11) -0.0033(10) C195 0.0139(13) 0.0208(13) 0.0180(15) -0.0058(10) 0.0049(11) -0.0021(9) C196 0.0145(12) 0.0121(12) 0.0159(14) -0.0003(9) 0.0053(10) 0.0001(9) B2 0.0191(15) 0.0078(13) 0.0206(16) 0.0029(11) 0.0061(12) 0.0022(10) C201 0.0116(12) 0.0098(12) 0.0170(13) -0.0003(9) 0.0052(10) -0.0004(8) C202 0.0158(12) 0.0125(12) 0.0174(14) -0.0007(9) 0.0038(11) -0.0013(9) C203 0.0219(14) 0.0138(13) 0.0255(16) 0.0047(10) 0.0073(12) -0.0005(10) C204 0.0225(14) 0.0090(12) 0.0358(17) -0.0062(11) 0.0122(13) -0.0032(9) C205 0.0229(14) 0.0178(14) 0.0224(16) -0.0082(10) 0.0061(12) -0.0040(10) C206 0.0172(13) 0.0157(13) 0.0158(14) -0.0014(10) 0.0026(11) 0.0011(9) O211 0.0134(8) 0.0090(8) 0.0133(9) -0.0006(6) 0.0002(7) -0.0022(6) C212 0.0106(11) 0.0103(12) 0.0133(13) -0.0005(9) 0.0056(10) -0.0015(8) C213 0.0141(12) 0.0123(12) 0.0131(13) -0.0006(9) 0.0006(10) -0.0007(9) C214 0.0100(11) 0.0126(12) 0.0127(13) 0.0009(9) 0.0044(10) 0.0011(8) O215 0.0114(8) 0.0097(8) 0.0165(9) 0.0009(6) 0.0022(7) 0.0005(6) C221 0.0106(12) 0.0132(12) 0.0167(13) 0.0045(9) 0.0065(10) 0.0016(8) C222 0.0252(14) 0.0142(13) 0.0201(15) 0.0024(10) 0.0067(12) 0.0062(10) C223 0.0270(15) 0.0305(16) 0.0177(15) 0.0063(12) 0.0027(12) 0.0074(11) C224 0.0187(14) 0.0201(14) 0.0299(17) 0.0132(11) 0.0084(12) 0.0097(10) C225 0.0184(13) 0.0108(12) 0.0309(16) 0.0054(10) 0.0109(12) 0.0024(9) C226 0.0128(12) 0.0121(12) 0.0226(15) 0.0032(10) 0.0075(11) -0.0001(9) C231 0.0142(12) 0.0097(12) 0.0158(13) 0.0006(9) 0.0106(10) 0.0008(8) C232 0.0155(13) 0.0135(13) 0.0176(14) -0.0001(9) 0.0053(11) 0.0027(9) C233 0.0208(13) 0.0130(13) 0.0229(15) 0.0041(10) 0.0104(12) 0.0079(9) C234 0.0260(14) 0.0067(12) 0.0332(16) 0.0042(10) 0.0206(13) 0.0047(9) C235 0.0190(14) 0.0122(13) 0.0370(17) -0.0063(11) 0.0133(12) -0.0049(9) C236 0.0133(12) 0.0126(12) 0.0252(15) -0.0004(10) 0.0074(11) 0.0010(9) O241 0.0110(8) 0.0099(8) 0.0153(9) 0.0012(6) 0.0028(7) 0.0003(6) C242 0.0116(12) 0.0105(11) 0.0126(13) 0.0021(9) 0.0087(10) 0.0018(8) C243 0.0128(12) 0.0093(12) 0.0159(13) 0.0024(9) 0.0039(10) 0.0012(8) C244 0.0086(11) 0.0124(12) 0.0135(13) 0.0006(9) 0.0072(10) 0.0002(8) O245 0.0116(8) 0.0090(8) 0.0159(9) 0.0002(6) 0.0027(7) 0.0006(6) C251 0.0082(11) 0.0108(11) 0.0166(13) -0.0016(9) 0.0069(10) -0.0010(8) C252 0.0141(12) 0.0112(12) 0.0211(14) -0.0012(9) 0.0067(11) 0.0002(9) C253 0.0123(12) 0.0213(14) 0.0182(14) -0.0022(10) 0.0024(11) 0.0019(9) C254 0.0120(12) 0.0150(13) 0.0253(15) -0.0083(10) 0.0075(11) -0.0051(9) C255 0.0205(13) 0.0110(12) 0.0266(15) -0.0025(10) 0.0136(12) -0.0046(9) C256 0.0139(12) 0.0125(12) 0.0182(14) 0.0008(9) 0.0073(10) 0.0000(9) N261 0.0171(10) 0.0104(10) 0.0174(11) 0.0008(8) 0.0094(9) 0.0006(7) C262 0.0133(12) 0.0130(12) 0.0146(14) 0.0037(9) 0.0044(10) 0.0018(9) C263 0.0190(13) 0.0175(13) 0.0217(15) 0.0018(10) 0.0121(11) 0.0004(9) C264 0.0204(13) 0.0221(14) 0.0246(15) 0.0021(10) 0.0144(12) 0.0061(10) C265 0.0239(14) 0.0131(12) 0.0240(15) -0.0030(10) 0.0122(12) 0.0039(9) C266 0.0218(13) 0.0123(12) 0.0199(14) -0.0014(9) 0.0127(11) -0.0014(9) N271 0.0201(11) 0.0067(10) 0.0205(12) 0.0019(8) 0.0105(9) -0.0007(7) N272 0.0145(10) 0.0061(9) 0.0139(11) 0.0012(7) 0.0057(8) -0.0003(7) C273 0.0159(12) 0.0119(12) 0.0164(13) 0.0044(9) 0.0092(10) 0.0027(9) C274 0.0252(14) 0.0137(13) 0.0393(17) 0.0004(11) 0.0232(13) -0.0039(10) C275 0.0292(15) 0.0119(13) 0.0315(16) 0.0002(10) 0.0191(13) -0.0069(10) N281 0.0125(10) 0.0070(9) 0.0157(11) -0.0013(7) 0.0035(8) 0.0014(7) N282 0.0123(10) 0.0074(10) 0.0141(11) 0.0007(7) 0.0053(8) 0.0017(7) C283 0.0113(12) 0.0152(12) 0.0130(13) -0.0001(9) 0.0042(10) 0.0034(9) C284 0.0280(15) 0.0170(13) 0.0151(14) -0.0049(10) 0.0088(12) 0.0024(10) C285 0.0232(14) 0.0119(12) 0.0185(14) -0.0043(10) 0.0060(11) 0.0016(9) N291 0.0079(9) 0.0134(10) 0.0127(11) 0.0002(8) 0.0033(8) -0.0005(7) C292 0.0075(11) 0.0148(12) 0.0119(13) 0.0000(9) 0.0018(9) 0.0030(8) C293 0.0164(13) 0.0220(13) 0.0172(14) -0.0019(10) 0.0085(11) 0.0036(9) C294 0.0162(13) 0.0300(15) 0.0189(15) 0.0079(11) 0.0117(11) 0.0045(10) C295 0.0129(12) 0.0209(13) 0.0222(15) 0.0058(10) 0.0091(11) 0.0000(9) C296 0.0119(12) 0.0141(12) 0.0179(14) 0.0002(9) 0.0065(10) -0.0019(9) C300 0.026(3) 0.024(3) 0.042(4) -0.002(3) 0.016(3) 0.003(2) Cl1 0.0417(4) 0.0347(4) 0.0577(5) -0.0010(3) 0.0295(4) -0.0087(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 Eu1 O115 2.3102(15) . ? Eu1 O145 2.3222(15) . ? Eu1 O111 2.3685(14) . ? Eu1 O141 2.3788(14) . ? Eu1 N172 2.5259(19) . ? Eu1 N182 2.5506(19) . ? Eu1 N161 2.562(2) . ? Eu1 N191 2.584(2) . ? Eu2 O215 2.3336(15) . ? Eu2 O245 2.3357(15) . ? Eu2 O241 2.3430(15) . ? Eu2 O211 2.3585(15) . ? Eu2 N272 2.5256(18) . ? Eu2 N282 2.5412(18) . ? Eu2 N291 2.5651(18) . ? Eu2 N261 2.5912(18) . ? B1 N171 1.550(3) . ? B1 N181 1.558(3) . ? C101 C102 1.387(3) . ? C101 C106 1.396(3) . ? C101 C112 1.507(3) . ? C102 C103 1.384(3) . ? C103 C104 1.384(4) . ? C104 C105 1.382(4) . ? C105 C106 1.382(3) . ? O111 C112 1.271(3) . ? C112 C113 1.403(3) . ? C113 C114 1.404(3) . ? C114 O115 1.273(3) . ? C114 C121 1.492(3) . ? C121 C122 1.393(3) . ? C121 C126 1.397(3) . ? C122 C123 1.387(3) . ? C123 C124 1.377(4) . ? C124 C125 1.383(4) . ? C125 C126 1.384(3) . ? C131 C132 1.397(3) . ? C131 C136 1.397(3) . ? C131 C142 1.506(3) . ? C132 C133 1.388(3) . ? C133 C134 1.381(4) . ? C134 C135 1.375(4) . ? C135 C136 1.391(3) . ? O141 C142 1.269(3) . ? C142 C143 1.406(3) . ? C143 C144 1.403(3) . ? C144 O145 1.273(3) . ? C144 C151 1.497(3) . ? C151 C152 1.396(3) . ? C151 C156 1.397(3) . ? C152 C153 1.390(3) . ? C153 C154 1.381(4) . ? C154 C155 1.385(3) . ? C155 C156 1.383(3) . ? N161 C162 1.348(3) . ? N161 C166 1.348(3) . ? C162 C163 1.384(4) . ? C162 C173 1.469(3) . ? C163 C164 1.389(3) . ? C164 C165 1.384(3) . ? C165 C166 1.372(3) . ? N171 C175 1.346(3) . ? N171 N172 1.362(3) . ? N172 C173 1.344(3) . ? C173 C174 1.394(3) . ? C174 C175 1.377(4) . ? N181 C185 1.346(3) . ? N181 N182 1.360(3) . ? N182 C183 1.344(3) . ? C183 C184 1.397(3) . ? C183 C192 1.468(3) . ? C184 C185 1.377(4) . ? N191 C196 1.346(3) . ? N191 C192 1.348(3) . ? C192 C193 1.391(4) . ? C193 C194 1.383(4) . ? C194 C195 1.386(4) . ? C195 C196 1.379(3) . ? B2 N281 1.555(3) . ? B2 N271 1.559(3) . ? C201 C202 1.390(3) . ? C201 C206 1.392(3) . ? C201 C212 1.504(3) . ? C202 C203 1.379(3) . ? C203 C204 1.387(4) . ? C204 C205 1.376(4) . ? C205 C206 1.392(3) . ? O211 C212 1.267(3) . ? C212 C213 1.404(3) . ? C213 C214 1.401(3) . ? C214 O215 1.277(3) . ? C214 C221 1.494(3) . ? C221 C222 1.386(4) . ? C221 C226 1.398(3) . ? C222 C223 1.392(3) . ? C223 C224 1.383(4) . ? C224 C225 1.385(4) . ? C225 C226 1.384(3) . ? C231 C232 1.387(3) . ? C231 C236 1.399(3) . ? C231 C242 1.498(3) . ? C232 C233 1.390(3) . ? C233 C234 1.383(4) . ? C234 C235 1.386(4) . ? C235 C236 1.386(3) . ? O241 C242 1.269(3) . ? C242 C243 1.403(3) . ? C243 C244 1.402(3) . ? C244 O245 1.268(3) . ? C244 C251 1.502(3) . ? C251 C252 1.387(3) . ? C251 C256 1.400(3) . ? C252 C253 1.392(3) . ? C253 C254 1.390(3) . ? C254 C255 1.382(4) . ? C255 C256 1.385(3) . ? N261 C266 1.342(3) . ? N261 C262 1.353(3) . ? C262 C263 1.390(3) . ? C262 C273 1.461(3) . ? C263 C264 1.379(3) . ? C264 C265 1.383(3) . ? C265 C266 1.385(3) . ? N271 C275 1.346(3) . ? N271 N272 1.355(3) . ? N272 C273 1.348(3) . ? C273 C274 1.395(3) . ? C274 C275 1.375(3) . ? N281 C285 1.341(3) . ? N281 N282 1.355(3) . ? N282 C283 1.349(3) . ? C283 C284 1.396(3) . ? C283 C292 1.469(3) . ? C284 C285 1.369(4) . ? N291 C296 1.344(3) . ? N291 C292 1.344(3) . ? C292 C293 1.390(3) . ? C293 C294 1.381(3) . ? C294 C295 1.376(4) . ? C295 C296 1.387(3) . ? C300 Cl1 1.814(6) . ? C300 Cl1 1.848(6) 3_756 ? Cl1 C300 1.848(6) 3_756 ? 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 O115 Eu1 O145 148.28(5) . . ? O115 Eu1 O111 70.46(5) . . ? O145 Eu1 O111 140.88(5) . . ? O115 Eu1 O141 135.79(5) . . ? O145 Eu1 O141 70.29(5) . . ? O111 Eu1 O141 72.49(5) . . ? O115 Eu1 N172 88.68(6) . . ? O145 Eu1 N172 74.90(6) . . ? O111 Eu1 N172 126.32(6) . . ? O141 Eu1 N172 133.42(6) . . ? O115 Eu1 N182 73.40(5) . . ? O145 Eu1 N182 76.11(6) . . ? O111 Eu1 N182 136.92(6) . . ? O141 Eu1 N182 123.63(5) . . ? N172 Eu1 N182 74.58(6) . . ? O115 Eu1 N161 110.46(6) . . ? O145 Eu1 N161 87.06(6) . . ? O111 Eu1 N161 77.12(6) . . ? O141 Eu1 N161 83.42(6) . . ? N172 Eu1 N161 64.60(6) . . ? N182 Eu1 N161 138.68(6) . . ? O115 Eu1 N191 81.92(6) . . ? O145 Eu1 N191 92.23(6) . . ? O111 Eu1 N191 88.78(6) . . ? O141 Eu1 N191 73.97(6) . . ? N172 Eu1 N191 137.93(6) . . ? N182 Eu1 N191 63.42(6) . . ? N161 Eu1 N191 156.17(6) . . ? O215 Eu2 O245 146.61(5) . . ? O215 Eu2 O241 143.02(5) . . ? O245 Eu2 O241 70.31(5) . . ? O215 Eu2 O211 70.85(5) . . ? O245 Eu2 O211 142.54(5) . . ? O241 Eu2 O211 72.27(5) . . ? O215 Eu2 N272 81.08(6) . . ? O245 Eu2 N272 72.98(6) . . ? O241 Eu2 N272 123.79(5) . . ? O211 Eu2 N272 132.39(6) . . ? O215 Eu2 N282 82.60(6) . . ? O245 Eu2 N282 71.41(6) . . ? O241 Eu2 N282 126.54(6) . . ? O211 Eu2 N282 133.57(6) . . ? N272 Eu2 N282 76.76(6) . . ? O215 Eu2 N291 100.52(6) . . ? O245 Eu2 N291 86.73(6) . . ? O241 Eu2 N291 78.07(6) . . ? O211 Eu2 N291 83.99(6) . . ? N272 Eu2 N291 139.81(6) . . ? N282 Eu2 N291 63.83(6) . . ? O215 Eu2 N261 97.39(6) . . ? O245 Eu2 N261 89.96(6) . . ? O241 Eu2 N261 74.77(6) . . ? O211 Eu2 N261 81.93(6) . . ? N272 Eu2 N261 64.10(6) . . ? N282 Eu2 N261 140.24(6) . . ? N291 Eu2 N261 152.13(6) . . ? N171 B1 N181 111.59(19) . . ? C102 C101 C106 118.0(2) . . ? C102 C101 C112 118.6(2) . . ? C106 C101 C112 123.3(2) . . ? C103 C102 C101 121.3(2) . . ? C104 C103 C102 120.0(2) . . ? C105 C104 C103 119.4(2) . . ? C104 C105 C106 120.4(2) . . ? C105 C106 C101 120.9(2) . . ? C112 O111 Eu1 138.01(14) . . ? O111 C112 C113 123.8(2) . . ? O111 C112 C101 115.8(2) . . ? C113 C112 C101 120.41(19) . . ? C112 C113 C114 123.1(2) . . ? O115 C114 C113 123.1(2) . . ? O115 C114 C121 115.33(19) . . ? C113 C114 C121 121.55(19) . . ? C114 O115 Eu1 140.31(14) . . ? C122 C121 C126 118.4(2) . . ? C122 C121 C114 123.2(2) . . ? C126 C121 C114 118.3(2) . . ? C123 C122 C121 120.8(2) . . ? C124 C123 C122 120.1(2) . . ? C123 C124 C125 119.8(2) . . ? C124 C125 C126 120.4(2) . . ? C125 C126 C121 120.4(2) . . ? C132 C131 C136 118.0(2) . . ? C132 C131 C142 118.1(2) . . ? C136 C131 C142 123.8(2) . . ? C133 C132 C131 121.2(2) . . ? C134 C133 C132 120.0(2) . . ? C135 C134 C133 119.7(2) . . ? C134 C135 C136 120.9(2) . . ? C135 C136 C131 120.3(2) . . ? C142 O141 Eu1 133.92(14) . . ? O141 C142 C143 123.7(2) . . ? O141 C142 C131 115.69(19) . . ? C143 C142 C131 120.56(19) . . ? C144 C143 C142 123.5(2) . . ? O145 C144 C143 123.1(2) . . ? O145 C144 C151 115.10(19) . . ? C143 C144 C151 121.67(19) . . ? C144 O145 Eu1 137.46(14) . . ? C152 C151 C156 118.6(2) . . ? C152 C151 C144 123.8(2) . . ? C156 C151 C144 117.57(19) . . ? C153 C152 C151 120.3(2) . . ? C154 C153 C152 120.4(2) . . ? C153 C154 C155 119.7(2) . . ? C156 C155 C154 120.2(2) . . ? C155 C156 C151 120.7(2) . . ? C162 N161 C166 117.5(2) . . ? C162 N161 Eu1 119.63(15) . . ? C166 N161 Eu1 122.87(15) . . ? N161 C162 C163 122.4(2) . . ? N161 C162 C173 115.6(2) . . ? C163 C162 C173 122.0(2) . . ? C162 C163 C164 119.3(2) . . ? C165 C164 C163 118.4(2) . . ? C166 C165 C164 119.1(2) . . ? N161 C166 C165 123.4(2) . . ? C175 N171 N172 109.8(2) . . ? C175 N171 B1 126.0(2) . . ? N172 N171 B1 123.34(19) . . ? C173 N172 N171 105.99(18) . . ? C173 N172 Eu1 118.05(14) . . ? N171 N172 Eu1 131.82(15) . . ? N172 C173 C174 110.9(2) . . ? N172 C173 C162 119.2(2) . . ? C174 C173 C162 129.9(2) . . ? C175 C174 C173 104.3(2) . . ? N171 C175 C174 109.0(2) . . ? C185 N181 N182 109.30(19) . . ? C185 N181 B1 125.63(19) . . ? N182 N181 B1 122.61(18) . . ? C183 N182 N181 106.28(18) . . ? C183 N182 Eu1 120.20(14) . . ? N181 N182 Eu1 131.91(15) . . ? N182 C183 C184 111.0(2) . . ? N182 C183 C192 118.6(2) . . ? C184 C183 C192 130.4(2) . . ? C185 C184 C183 103.7(2) . . ? N181 C185 C184 109.6(2) . . ? C196 N191 C192 117.7(2) . . ? C196 N191 Eu1 121.36(15) . . ? C192 N191 Eu1 120.98(15) . . ? N191 C192 C193 122.3(2) . . ? N191 C192 C183 115.6(2) . . ? C193 C192 C183 122.2(2) . . ? C194 C193 C192 119.1(2) . . ? C193 C194 C195 119.1(2) . . ? C196 C195 C194 118.4(2) . . ? N191 C196 C195 123.5(2) . . ? N281 B2 N271 109.64(19) . . ? C202 C201 C206 118.6(2) . . ? C202 C201 C212 117.9(2) . . ? C206 C201 C212 123.4(2) . . ? C203 C202 C201 121.2(2) . . ? C202 C203 C204 119.8(2) . . ? C205 C204 C203 119.8(2) . . ? C204 C205 C206 120.5(2) . . ? C205 C206 C201 120.1(2) . . ? C212 O211 Eu2 137.67(14) . . ? O211 C212 C213 124.0(2) . . ? O211 C212 C201 116.64(19) . . ? C213 C212 C201 119.4(2) . . ? C214 C213 C212 123.2(2) . . ? O215 C214 C213 124.1(2) . . ? O215 C214 C221 116.22(19) . . ? C213 C214 C221 119.7(2) . . ? C214 O215 Eu2 138.66(14) . . ? C222 C221 C226 118.7(2) . . ? C222 C221 C214 122.8(2) . . ? C226 C221 C214 118.5(2) . . ? C221 C222 C223 121.3(2) . . ? C224 C223 C222 119.3(3) . . ? C223 C224 C225 120.2(2) . . ? C226 C225 C224 120.4(2) . . ? C225 C226 C221 120.2(2) . . ? C232 C231 C236 118.5(2) . . ? C232 C231 C242 123.9(2) . . ? C236 C231 C242 117.7(2) . . ? C231 C232 C233 120.8(2) . . ? C234 C233 C232 120.1(2) . . ? C233 C234 C235 119.8(2) . . ? C234 C235 C236 120.0(2) . . ? C235 C236 C231 120.7(2) . . ? C242 O241 Eu2 139.06(14) . . ? O241 C242 C243 123.3(2) . . ? O241 C242 C231 115.79(19) . . ? C243 C242 C231 120.9(2) . . ? C244 C243 C242 122.8(2) . . ? O245 C244 C243 124.1(2) . . ? O245 C244 C251 115.58(19) . . ? C243 C244 C251 120.2(2) . . ? C244 O245 Eu2 139.20(14) . . ? C252 C251 C256 118.9(2) . . ? C252 C251 C244 123.5(2) . . ? C256 C251 C244 117.6(2) . . ? C251 C252 C253 120.4(2) . . ? C254 C253 C252 120.3(2) . . ? C255 C254 C253 119.5(2) . . ? C254 C255 C256 120.4(2) . . ? C255 C256 C251 120.4(2) . . ? C266 N261 C262 118.25(19) . . ? C266 N261 Eu2 123.33(15) . . ? C262 N261 Eu2 117.84(14) . . ? N261 C262 C263 121.9(2) . . ? N261 C262 C273 115.7(2) . . ? C263 C262 C273 122.4(2) . . ? C264 C263 C262 119.1(2) . . ? C263 C264 C265 119.2(2) . . ? C264 C265 C266 118.7(2) . . ? N261 C266 C265 122.8(2) . . ? C275 N271 N272 110.01(19) . . ? C275 N271 B2 127.4(2) . . ? N272 N271 B2 122.44(18) . . ? C273 N272 N271 106.18(18) . . ? C273 N272 Eu2 116.33(14) . . ? N271 N272 Eu2 127.90(14) . . ? N272 C273 C274 110.4(2) . . ? N272 C273 C262 118.9(2) . . ? C274 C273 C262 130.7(2) . . ? C275 C274 C273 104.6(2) . . ? N271 C275 C274 108.8(2) . . ? C285 N281 N282 109.82(19) . . ? C285 N281 B2 128.2(2) . . ? N282 N281 B2 121.69(18) . . ? C283 N282 N281 105.99(18) . . ? C283 N282 Eu2 117.38(14) . . ? N281 N282 Eu2 128.99(13) . . ? N282 C283 C284 110.6(2) . . ? N282 C283 C292 118.8(2) . . ? C284 C283 C292 130.5(2) . . ? C285 C284 C283 104.2(2) . . ? N281 C285 C284 109.4(2) . . ? C296 N291 C292 118.2(2) . . ? C296 N291 Eu2 121.08(15) . . ? C292 N291 Eu2 119.58(14) . . ? N291 C292 C293 122.3(2) . . ? N291 C292 C283 115.4(2) . . ? C293 C292 C283 122.3(2) . . ? C294 C293 C292 118.8(2) . . ? C295 C294 C293 119.4(2) . . ? C294 C295 C296 118.7(2) . . ? N291 C296 C295 122.6(2) . . ? Cl1 C300 Cl1 105.4(3) . 3_756 ? C300 Cl1 C300 74.6(3) . 3_756 ? _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_theta_full 70.13 _diffrn_measured_fraction_theta_full 0.945 _refine_diff_density_max 0.513 _refine_diff_density_min -0.654 _refine_diff_density_rms 0.080 #=END data_minniem _database_code_depnum_ccdc_archive 'CCDC 229470' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46.25 H36.50 B Cl0.50 N6 O4 Yb' _chemical_formula_sum 'C46.25 H36.50 B Cl0.50 N6 O4 Yb' _chemical_formula_weight 941.89 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' B B 0.0013 0.0007 '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' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.133(4) _cell_length_b 26.895(5) _cell_length_c 17.426(4) _cell_angle_alpha 90.00 _cell_angle_beta 115.92(3) _cell_angle_gamma 90.00 _cell_volume 8065(3) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 15279 _cell_measurement_theta_min 4.476 _cell_measurement_theta_max 54.906 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.125 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.551 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3772 _exptl_absorpt_coefficient_mu 2.405 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.626 _exptl_absorpt_correction_T_max 0.735 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 57155 _diffrn_reflns_av_R_equivalents 0.0314 _diffrn_reflns_av_sigmaI/netI 0.0367 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.18 _diffrn_reflns_theta_max 27.48 _reflns_number_total 18498 _reflns_number_gt 14393 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SAINT' _computing_data_reduction 'BRUKER SHELXS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXS _computing_publication_material SHELXS/XCIF _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^)+(0.0330P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18498 _refine_ls_number_parameters 1079 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0404 _refine_ls_R_factor_gt 0.0270 _refine_ls_wR_factor_ref 0.0642 _refine_ls_wR_factor_gt 0.0583 _refine_ls_goodness_of_fit_ref 0.962 _refine_ls_restrained_S_all 0.962 _refine_ls_shift/su_max 0.005 _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 1.008794(7) 0.307775(4) 0.230848(7) 0.01562(3) Uani 1 1 d . . . B1 B 1.0010(2) 0.16202(13) 0.2420(2) 0.0261(8) Uani 1 1 d . . . C101 C 0.85996(16) 0.44432(10) 0.09987(17) 0.0178(6) Uani 1 1 d . . . C102 C 0.78916(17) 0.46461(10) 0.04282(17) 0.0215(6) Uani 1 1 d . . . H102 H 0.7479 0.4432 0.0081 0.026 Uiso 1 1 calc R . . C103 C 0.77826(19) 0.51596(11) 0.03624(19) 0.0255(7) Uani 1 1 d . . . H103 H 0.7301 0.5294 -0.0036 0.031 Uiso 1 1 calc R . . C104 C 0.83759(19) 0.54731(11) 0.0877(2) 0.0272(7) Uani 1 1 d . . . H104 H 0.8300 0.5823 0.0836 0.033 Uiso 1 1 calc R . . C105 C 0.90777(19) 0.52775(11) 0.1448(2) 0.0293(7) Uani 1 1 d . . . H105 H 0.9485 0.5493 0.1799 0.035 Uiso 1 1 calc R . . C106 C 0.91908(18) 0.47674(10) 0.15135(19) 0.0254(7) Uani 1 1 d . . . H106 H 0.9675 0.4636 0.1912 0.030 Uiso 1 1 calc R . . O111 O 0.94508(11) 0.37768(7) 0.16238(11) 0.0186(4) Uani 1 1 d . . . C112 C 0.87701(16) 0.38967(10) 0.10912(16) 0.0176(6) Uani 1 1 d . . . C113 C 0.81982(17) 0.35513(10) 0.06042(17) 0.0201(6) Uani 1 1 d . . . H113 H 0.7698 0.3668 0.0221 0.024 Uiso 1 1 calc R . . C114 C 0.83428(16) 0.30391(10) 0.06659(16) 0.0175(6) Uani 1 1 d . . . O115 O 0.89661(11) 0.28414(7) 0.12077(11) 0.0204(4) Uani 1 1 d . . . C121 C 0.77443(16) 0.26836(10) 0.00910(17) 0.0188(6) Uani 1 1 d . . . C122 C 0.71582(17) 0.28166(11) -0.07086(18) 0.0241(6) Uani 1 1 d . . . H122 H 0.7122 0.3150 -0.0902 0.029 Uiso 1 1 calc R . . C123 C 0.66294(18) 0.24631(11) -0.12215(19) 0.0281(7) Uani 1 1 d . . . H123 H 0.6242 0.2554 -0.1770 0.034 Uiso 1 1 calc R . . C124 C 0.66653(18) 0.19793(11) -0.0935(2) 0.0276(7) Uani 1 1 d . . . H124 H 0.6299 0.1739 -0.1283 0.033 Uiso 1 1 calc R . . C125 C 0.72370(18) 0.18468(11) -0.01412(19) 0.0255(7) Uani 1 1 d . . . H125 H 0.7258 0.1516 0.0059 0.031 Uiso 1 1 calc R . . C126 C 0.77774(17) 0.21909(10) 0.03627(18) 0.0219(6) Uani 1 1 d . . . H126 H 0.8176 0.2092 0.0899 0.026 Uiso 1 1 calc R . . C131 C 1.16138(17) 0.43772(10) 0.39181(17) 0.0211(6) Uani 1 1 d . . . C132 C 1.20551(18) 0.45374(11) 0.47548(18) 0.0274(7) Uani 1 1 d . . . H132 H 1.2255 0.4302 0.5205 0.033 Uiso 1 1 calc R . . C133 C 1.2203(2) 0.50410(11) 0.4931(2) 0.0334(8) Uani 1 1 d . . . H133 H 1.2506 0.5148 0.5501 0.040 Uiso 1 1 calc R . . C134 C 1.19115(19) 0.53854(11) 0.4281(2) 0.0319(8) Uani 1 1 d . . . H134 H 1.2002 0.5730 0.4406 0.038 Uiso 1 1 calc R . . C135 C 1.14855(19) 0.52288(11) 0.3446(2) 0.0294(7) Uani 1 1 d . . . H135 H 1.1298 0.5465 0.2995 0.035 Uiso 1 1 calc R . . C136 C 1.13343(18) 0.47293(10) 0.32688(18) 0.0238(6) Uani 1 1 d . . . H136 H 1.1036 0.4625 0.2696 0.029 Uiso 1 1 calc R . . O141 O 1.08342(11) 0.37524(7) 0.29775(11) 0.0202(4) Uani 1 1 d . . . C142 C 1.14165(16) 0.38395(10) 0.36898(16) 0.0182(6) Uani 1 1 d . . . C143 C 1.18764(18) 0.34694(10) 0.42410(17) 0.0231(6) Uani 1 1 d . . . H143 H 1.2304 0.3566 0.4756 0.028 Uiso 1 1 calc R . . C144 C 1.17349(17) 0.29636(10) 0.40683(17) 0.0200(6) Uani 1 1 d . . . O145 O 1.11538(11) 0.27890(7) 0.34171(11) 0.0206(4) Uani 1 1 d . . . C151 C 1.22920(17) 0.25862(10) 0.46417(17) 0.0214(6) Uani 1 1 d . . . C152 C 1.2817(2) 0.26962(12) 0.54810(19) 0.0339(8) Uani 1 1 d . . . H152 H 1.2833 0.3021 0.5702 0.041 Uiso 1 1 calc R . . C153 C 1.3315(2) 0.23305(13) 0.5991(2) 0.0448(10) Uani 1 1 d . . . H153 H 1.3665 0.2406 0.6565 0.054 Uiso 1 1 calc R . . C154 C 1.3309(2) 0.18628(12) 0.5679(2) 0.0365(8) Uani 1 1 d . . . H154 H 1.3656 0.1617 0.6033 0.044 Uiso 1 1 calc R . . C155 C 1.27963(18) 0.17489(11) 0.4848(2) 0.0303(7) Uani 1 1 d . . . H155 H 1.2793 0.1425 0.4630 0.036 Uiso 1 1 calc R . . C156 C 1.22866(17) 0.21089(10) 0.43323(19) 0.0243(6) Uani 1 1 d . . . H156 H 1.1931 0.2028 0.3763 0.029 Uiso 1 1 calc R . . N161 N 1.00861(14) 0.18497(8) 0.16495(14) 0.0203(5) Uani 1 1 d . . . N162 N 1.03304(13) 0.23242(8) 0.16555(14) 0.0183(5) Uani 1 1 d . . . C163 C 1.04062(16) 0.23846(10) 0.09302(16) 0.0189(6) Uani 1 1 d . . . C164 C 1.02179(18) 0.19462(10) 0.04561(18) 0.0264(7) Uani 1 1 d . . . H164 H 1.0228 0.1885 -0.0076 0.032 Uiso 1 1 calc R . . C165 C 1.00150(18) 0.16228(11) 0.09319(18) 0.0255(7) Uani 1 1 d . . . H165 H 0.9849 0.1289 0.0778 0.031 Uiso 1 1 calc R . . N171 N 1.06289(13) 0.32414(8) 0.12745(13) 0.0183(5) Uani 1 1 d . . . C172 C 1.06078(16) 0.28759(10) 0.07327(16) 0.0185(6) Uani 1 1 d . . . C173 C 1.07490(17) 0.29654(11) 0.00276(18) 0.0237(6) Uani 1 1 d . . . H173 H 1.0724 0.2702 -0.0347 0.028 Uiso 1 1 calc R . . C174 C 1.09262(17) 0.34409(11) -0.01201(18) 0.0254(7) Uani 1 1 d . . . H174 H 1.1022 0.3511 -0.0600 0.030 Uiso 1 1 calc R . . C175 C 1.09634(17) 0.38134(11) 0.04359(17) 0.0232(6) Uani 1 1 d . . . H175 H 1.1098 0.4142 0.0354 0.028 Uiso 1 1 calc R . . C176 C 1.08021(16) 0.37028(10) 0.11181(17) 0.0210(6) Uani 1 1 d . . . H176 H 1.0815 0.3964 0.1491 0.025 Uiso 1 1 calc R . . N181 N 0.94269(16) 0.19283(8) 0.26197(15) 0.0240(6) Uani 1 1 d . . . N182 N 0.95276(14) 0.24173(8) 0.28361(14) 0.0205(5) Uani 1 1 d . . . C183 C 0.89389(18) 0.25463(10) 0.30186(18) 0.0225(6) Uani 1 1 d . . . C184 C 0.8453(2) 0.21435(11) 0.2929(2) 0.0310(7) Uani 1 1 d . . . H184 H 0.8001 0.2133 0.3024 0.037 Uiso 1 1 calc R . . C185 C 0.8783(2) 0.17649(11) 0.2672(2) 0.0309(7) Uani 1 1 d . . . H185 H 0.8586 0.1435 0.2548 0.037 Uiso 1 1 calc R . . N191 N 0.93731(14) 0.33820(8) 0.31290(14) 0.0207(5) Uani 1 1 d . . . C192 C 0.88934(17) 0.30612(10) 0.32614(17) 0.0209(6) Uani 1 1 d . . . C193 C 0.83996(18) 0.32095(11) 0.36139(18) 0.0267(7) Uani 1 1 d . . . H193 H 0.8073 0.2975 0.3707 0.032 Uiso 1 1 calc R . . C194 C 0.83905(19) 0.37046(11) 0.38276(19) 0.0297(7) Uani 1 1 d . . . H194 H 0.8053 0.3816 0.4061 0.036 Uiso 1 1 calc R . . C195 C 0.88804(19) 0.40341(11) 0.36953(19) 0.0289(7) Uani 1 1 d . . . H195 H 0.8890 0.4375 0.3844 0.035 Uiso 1 1 calc R . . C196 C 0.93565(18) 0.38623(11) 0.33434(17) 0.0248(6) Uani 1 1 d . . . H196 H 0.9687 0.4093 0.3248 0.030 Uiso 1 1 calc R . . Yb2 Yb 0.492321(7) 0.495870(4) 0.273840(7) 0.01537(3) Uani 1 1 d . . . B2 B 0.4620(2) 0.64204(13) 0.2835(2) 0.0258(8) Uani 1 1 d . . . C201 C 0.35600(17) 0.35417(10) 0.27722(17) 0.0200(6) Uani 1 1 d . . . C202 C 0.28618(19) 0.33327(11) 0.26662(19) 0.0269(7) Uani 1 1 d . . . H202 H 0.2397 0.3522 0.2405 0.032 Uiso 1 1 calc R . . C203 C 0.2830(2) 0.28506(11) 0.2937(2) 0.0331(8) Uani 1 1 d . . . H203 H 0.2346 0.2710 0.2850 0.040 Uiso 1 1 calc R . . C204 C 0.3507(2) 0.25760(12) 0.3332(2) 0.0355(8) Uani 1 1 d . . . H204 H 0.3491 0.2250 0.3535 0.043 Uiso 1 1 calc R . . C205 C 0.4207(2) 0.27763(11) 0.3431(2) 0.0344(8) Uani 1 1 d . . . H205 H 0.4670 0.2586 0.3692 0.041 Uiso 1 1 calc R . . C206 C 0.42324(18) 0.32552(11) 0.31485(19) 0.0261(7) Uani 1 1 d . . . H206 H 0.4714 0.3389 0.3213 0.031 Uiso 1 1 calc R . . O211 O 0.43240(11) 0.42262(7) 0.27508(12) 0.0196(4) Uani 1 1 d . . . C212 C 0.36392(17) 0.40736(10) 0.25506(16) 0.0180(6) Uani 1 1 d . . . C213 C 0.29839(17) 0.43767(10) 0.21660(17) 0.0216(6) Uani 1 1 d . . . H213 H 0.2484 0.4227 0.1947 0.026 Uiso 1 1 calc R . . C214 C 0.30346(17) 0.48917(10) 0.20903(16) 0.0186(6) Uani 1 1 d . . . O215 O 0.36769(11) 0.51253(7) 0.23712(11) 0.0186(4) Uani 1 1 d . . . C221 C 0.23191(16) 0.52070(10) 0.16943(16) 0.0178(6) Uani 1 1 d . . . C222 C 0.15702(18) 0.50200(11) 0.14217(18) 0.0238(6) Uani 1 1 d . . . H222 H 0.1499 0.4679 0.1509 0.029 Uiso 1 1 calc R . . C223 C 0.09265(18) 0.53237(12) 0.10256(19) 0.0312(7) Uani 1 1 d . . . H223 H 0.0419 0.5190 0.0840 0.037 Uiso 1 1 calc R . . C224 C 0.10239(19) 0.58193(12) 0.09019(19) 0.0300(7) Uani 1 1 d . . . H224 H 0.0584 0.6029 0.0629 0.036 Uiso 1 1 calc R . . C225 C 0.17649(18) 0.60112(11) 0.11763(17) 0.0257(7) Uani 1 1 d . . . H225 H 0.1832 0.6354 0.1093 0.031 Uiso 1 1 calc R . . C226 C 0.24060(17) 0.57113(10) 0.15679(17) 0.0218(6) Uani 1 1 d . . . H226 H 0.2912 0.5848 0.1754 0.026 Uiso 1 1 calc R . . C231 C 0.71671(16) 0.55585(10) 0.27964(16) 0.0183(6) Uani 1 1 d . . . C232 C 0.78617(18) 0.54962(11) 0.27324(19) 0.0256(7) Uani 1 1 d . . . H232 H 0.8031 0.5172 0.2675 0.031 Uiso 1 1 calc R . . C233 C 0.83067(19) 0.59056(12) 0.2752(2) 0.0311(7) Uani 1 1 d . . . H233 H 0.8783 0.5860 0.2714 0.037 Uiso 1 1 calc R . . C234 C 0.80651(19) 0.63798(11) 0.28265(18) 0.0280(7) Uani 1 1 d . . . H234 H 0.8372 0.6660 0.2836 0.034 Uiso 1 1 calc R . . C235 C 0.73802(19) 0.64431(11) 0.28860(19) 0.0295(7) Uani 1 1 d . . . H235 H 0.7212 0.6769 0.2935 0.035 Uiso 1 1 calc R . . C236 C 0.69303(18) 0.60364(11) 0.28749(18) 0.0260(7) Uani 1 1 d . . . H236 H 0.6458 0.6085 0.2921 0.031 Uiso 1 1 calc R . . O241 O 0.60664(11) 0.52609(7) 0.29023(12) 0.0204(4) Uani 1 1 d . . . C242 C 0.66318(16) 0.51402(10) 0.27511(16) 0.0178(6) Uani 1 1 d . . . C243 C 0.67335(17) 0.46583(10) 0.25066(17) 0.0199(6) Uani 1 1 d . . . H243 H 0.7165 0.4594 0.2388 0.024 Uiso 1 1 calc R . . C244 C 0.62192(16) 0.42689(10) 0.24317(16) 0.0174(6) Uani 1 1 d . . . O245 O 0.56604(11) 0.43088(7) 0.26301(11) 0.0190(4) Uani 1 1 d . . . C251 C 0.62845(16) 0.37719(10) 0.20630(16) 0.0187(6) Uani 1 1 d . . . C252 C 0.68680(18) 0.36549(10) 0.18195(18) 0.0241(6) Uani 1 1 d . . . H252 H 0.7257 0.3893 0.1888 0.029 Uiso 1 1 calc R . . C253 C 0.6883(2) 0.31909(12) 0.1477(2) 0.0323(8) Uani 1 1 d . . . H253 H 0.7292 0.3111 0.1328 0.039 Uiso 1 1 calc R . . C254 C 0.6312(2) 0.28441(11) 0.1352(2) 0.0332(8) Uani 1 1 d . . . H254 H 0.6323 0.2529 0.1111 0.040 Uiso 1 1 calc R . . C255 C 0.5724(2) 0.29571(11) 0.15780(19) 0.0307(7) Uani 1 1 d . . . H255 H 0.5325 0.2722 0.1486 0.037 Uiso 1 1 calc R . . C256 C 0.57163(18) 0.34145(10) 0.19404(18) 0.0228(6) Uani 1 1 d . . . H256 H 0.5317 0.3486 0.2108 0.027 Uiso 1 1 calc R . . N261 N 0.52041(14) 0.61487(8) 0.36461(15) 0.0221(5) Uani 1 1 d . . . N262 N 0.52159(14) 0.56471(8) 0.37527(14) 0.0198(5) Uani 1 1 d . . . C263 C 0.57134(17) 0.55578(10) 0.45685(17) 0.0207(6) Uani 1 1 d . . . C264 C 0.60222(18) 0.60036(11) 0.49973(19) 0.0281(7) Uani 1 1 d . . . H264 H 0.6384 0.6046 0.5577 0.034 Uiso 1 1 calc R . . C265 C 0.56868(19) 0.63622(11) 0.4396(2) 0.0292(7) Uani 1 1 d . . . H265 H 0.5777 0.6709 0.4487 0.035 Uiso 1 1 calc R . . N271 N 0.55787(14) 0.46952(8) 0.42502(14) 0.0206(5) Uani 1 1 d . . . C272 C 0.58620(16) 0.50446(10) 0.48666(17) 0.0199(6) Uani 1 1 d . . . C273 C 0.62544(18) 0.49208(11) 0.57241(18) 0.0269(7) Uani 1 1 d . . . H273 H 0.6457 0.5174 0.6144 0.032 Uiso 1 1 calc R . . C274 C 0.63483(19) 0.44279(12) 0.59629(18) 0.0289(7) Uani 1 1 d . . . H274 H 0.6604 0.4337 0.6548 0.035 Uiso 1 1 calc R . . C275 C 0.60638(17) 0.40674(11) 0.53347(18) 0.0250(7) Uani 1 1 d . . . H275 H 0.6126 0.3724 0.5478 0.030 Uiso 1 1 calc R . . C276 C 0.56883(18) 0.42178(11) 0.44946(18) 0.0241(6) Uani 1 1 d . . . H276 H 0.5497 0.3969 0.4065 0.029 Uiso 1 1 calc R . . N281 N 0.46627(15) 0.62055(8) 0.20240(15) 0.0229(5) Uani 1 1 d . . . N282 N 0.45893(14) 0.57134(8) 0.18349(14) 0.0198(5) Uani 1 1 d . . . C283 C 0.44272(17) 0.56747(10) 0.10055(17) 0.0210(6) Uani 1 1 d . . . C284 C 0.43879(19) 0.61453(11) 0.06476(19) 0.0284(7) Uani 1 1 d . . . H284 H 0.4279 0.6225 0.0075 0.034 Uiso 1 1 calc R . . C285 C 0.45426(18) 0.64643(11) 0.13149(19) 0.0276(7) Uani 1 1 d . . . H285 H 0.4562 0.6816 0.1283 0.033 Uiso 1 1 calc R . . N291 N 0.44486(13) 0.47981(8) 0.11800(13) 0.0176(5) Uani 1 1 d . . . C292 C 0.43115(16) 0.51805(10) 0.06256(17) 0.0193(6) Uani 1 1 d . . . C293 C 0.40727(18) 0.51039(11) -0.02417(18) 0.0264(7) Uani 1 1 d . . . H293 H 0.3962 0.5379 -0.0620 0.032 Uiso 1 1 calc R . . C294 C 0.39983(18) 0.46232(11) -0.05470(18) 0.0265(7) Uani 1 1 d . . . H294 H 0.3851 0.4563 -0.1135 0.032 Uiso 1 1 calc R . . C295 C 0.41414(17) 0.42306(11) 0.00162(17) 0.0235(6) Uani 1 1 d . . . H295 H 0.4093 0.3897 -0.0178 0.028 Uiso 1 1 calc R . . C296 C 0.43567(17) 0.43352(10) 0.08663(17) 0.0219(6) Uani 1 1 d . . . H296 H 0.4444 0.4065 0.1248 0.026 Uiso 1 1 calc R . . H2B H 0.4015(17) 0.6379(10) 0.2789(16) 0.019(7) Uiso 1 1 d . . . H2A H 0.4797(16) 0.6815(11) 0.2896(17) 0.023(8) Uiso 1 1 d . . . H1A H 0.9740(17) 0.1233(10) 0.2224(17) 0.023(8) Uiso 1 1 d . . . H1B H 1.0623(16) 0.1596(9) 0.3007(17) 0.016(7) Uiso 1 1 d . . . Cl1 Cl 1.00504(7) 0.51626(4) 0.42278(7) 0.0546(3) Uani 1 1 d . . . C300 C 0.9527(4) 0.5272(2) 0.4835(5) 0.0387(17) Uani 0.50 1 d P . . H30A H 0.8967 0.5203 0.4490 0.046 Uiso 0.50 1 calc PR . . H30B H 0.9588 0.5622 0.5030 0.046 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 Yb1 0.01698(6) 0.01252(6) 0.01610(6) 0.00084(4) 0.00606(5) 0.00081(5) B1 0.028(2) 0.0204(18) 0.0284(18) 0.0067(14) 0.0114(16) 0.0026(15) C101 0.0208(15) 0.0146(14) 0.0211(13) 0.0011(11) 0.0121(12) 0.0010(11) C102 0.0227(16) 0.0179(15) 0.0234(14) 0.0010(11) 0.0096(13) 0.0022(12) C103 0.0275(17) 0.0224(16) 0.0279(15) 0.0047(12) 0.0131(14) 0.0080(13) C104 0.0354(19) 0.0145(15) 0.0400(18) 0.0034(13) 0.0242(16) 0.0043(13) C105 0.0305(18) 0.0180(16) 0.0389(18) -0.0034(13) 0.0148(15) -0.0025(13) C106 0.0234(16) 0.0192(15) 0.0321(16) -0.0001(12) 0.0107(14) 0.0009(12) O111 0.0187(10) 0.0157(10) 0.0190(9) 0.0003(8) 0.0059(8) -0.0011(8) C112 0.0211(15) 0.0168(14) 0.0171(13) 0.0031(11) 0.0104(12) 0.0023(11) C113 0.0179(15) 0.0172(14) 0.0207(14) 0.0025(11) 0.0043(12) 0.0023(11) C114 0.0184(15) 0.0175(14) 0.0183(13) 0.0003(11) 0.0096(12) -0.0006(11) O115 0.0201(11) 0.0153(10) 0.0211(10) 0.0019(8) 0.0048(8) 0.0019(8) C121 0.0186(15) 0.0171(14) 0.0219(14) -0.0026(11) 0.0099(12) -0.0010(11) C122 0.0218(16) 0.0184(15) 0.0278(15) -0.0002(12) 0.0069(13) 0.0006(12) C123 0.0222(17) 0.0268(17) 0.0282(15) -0.0035(13) 0.0044(13) 0.0001(13) C124 0.0200(16) 0.0231(16) 0.0355(17) -0.0090(13) 0.0084(14) -0.0065(13) C125 0.0248(17) 0.0174(15) 0.0366(17) -0.0003(13) 0.0156(14) -0.0029(12) C126 0.0217(15) 0.0183(15) 0.0274(15) 0.0011(12) 0.0123(13) 0.0012(12) C131 0.0202(15) 0.0180(15) 0.0237(14) -0.0024(11) 0.0084(12) -0.0012(12) C132 0.0305(18) 0.0197(15) 0.0234(15) 0.0014(12) 0.0039(13) 0.0033(13) C133 0.036(2) 0.0287(18) 0.0260(16) -0.0087(13) 0.0049(15) -0.0028(15) C134 0.0333(19) 0.0179(16) 0.0406(19) -0.0069(13) 0.0124(16) -0.0047(14) C135 0.0318(19) 0.0203(16) 0.0314(17) 0.0026(13) 0.0094(15) -0.0013(13) C136 0.0237(16) 0.0230(16) 0.0214(14) -0.0026(12) 0.0068(13) -0.0029(13) O141 0.0201(11) 0.0174(10) 0.0181(9) 0.0009(8) 0.0037(8) -0.0007(8) C142 0.0183(15) 0.0188(14) 0.0188(13) -0.0007(11) 0.0093(12) -0.0009(11) C143 0.0242(16) 0.0190(15) 0.0187(14) -0.0012(11) 0.0026(12) 0.0021(12) C144 0.0188(15) 0.0234(15) 0.0183(13) 0.0025(11) 0.0085(12) 0.0025(12) O145 0.0199(11) 0.0159(10) 0.0222(10) 0.0009(8) 0.0057(9) 0.0011(8) C151 0.0191(15) 0.0213(15) 0.0247(14) 0.0061(12) 0.0106(12) 0.0034(12) C152 0.038(2) 0.0295(18) 0.0258(16) 0.0019(13) 0.0068(15) 0.0125(15) C153 0.047(2) 0.044(2) 0.0277(17) 0.0071(16) 0.0018(17) 0.0178(18) C154 0.032(2) 0.0304(19) 0.0394(19) 0.0150(15) 0.0088(16) 0.0153(15) C155 0.0253(17) 0.0179(16) 0.047(2) 0.0068(14) 0.0154(15) 0.0036(13) C156 0.0180(15) 0.0209(15) 0.0304(16) 0.0036(12) 0.0072(13) 0.0005(12) N161 0.0215(13) 0.0129(11) 0.0251(12) -0.0008(9) 0.0091(11) 0.0023(10) N162 0.0180(13) 0.0144(12) 0.0209(11) 0.0011(9) 0.0070(10) 0.0020(9) C163 0.0167(15) 0.0205(15) 0.0170(13) -0.0002(11) 0.0051(11) 0.0029(11) C164 0.0325(18) 0.0228(16) 0.0223(15) -0.0018(12) 0.0104(14) 0.0037(13) C165 0.0278(17) 0.0192(15) 0.0254(15) -0.0039(12) 0.0078(13) 0.0004(13) N171 0.0164(12) 0.0201(12) 0.0162(11) 0.0006(9) 0.0052(10) -0.0007(10) C172 0.0135(14) 0.0196(14) 0.0189(13) 0.0006(11) 0.0038(11) 0.0027(11) C173 0.0252(16) 0.0246(16) 0.0225(14) -0.0017(12) 0.0113(13) 0.0038(13) C174 0.0224(16) 0.0311(17) 0.0243(15) 0.0031(13) 0.0116(13) 0.0000(13) C175 0.0202(15) 0.0245(16) 0.0241(14) 0.0065(12) 0.0089(12) -0.0017(12) C176 0.0195(15) 0.0196(15) 0.0211(14) -0.0008(11) 0.0061(12) -0.0019(12) N181 0.0381(16) 0.0093(12) 0.0246(12) 0.0050(9) 0.0138(12) 0.0006(10) N182 0.0234(14) 0.0153(12) 0.0211(11) 0.0022(9) 0.0082(11) 0.0026(10) C183 0.0250(16) 0.0193(15) 0.0267(14) 0.0050(12) 0.0145(13) 0.0015(12) C184 0.037(2) 0.0225(16) 0.0433(19) 0.0018(14) 0.0262(16) -0.0040(14) C185 0.041(2) 0.0192(16) 0.0409(18) 0.0030(13) 0.0257(16) -0.0049(14) N191 0.0215(13) 0.0185(12) 0.0222(12) 0.0013(10) 0.0098(11) 0.0012(10) C192 0.0211(15) 0.0247(16) 0.0178(13) 0.0044(11) 0.0093(12) 0.0050(12) C193 0.0269(17) 0.0263(16) 0.0306(16) 0.0020(13) 0.0160(14) -0.0008(13) C194 0.0309(18) 0.0309(18) 0.0322(16) -0.0008(14) 0.0183(15) 0.0058(14) C195 0.0353(19) 0.0224(16) 0.0298(16) -0.0036(13) 0.0150(15) 0.0043(14) C196 0.0295(17) 0.0201(15) 0.0248(15) -0.0010(12) 0.0119(13) -0.0013(13) Yb2 0.01469(6) 0.01369(6) 0.01761(6) -0.00127(4) 0.00694(5) -0.00052(5) B2 0.027(2) 0.0205(18) 0.0320(18) -0.0042(14) 0.0146(16) 0.0005(15) C201 0.0233(16) 0.0172(14) 0.0199(13) -0.0043(11) 0.0099(12) -0.0046(12) C202 0.0277(17) 0.0210(16) 0.0328(16) -0.0008(13) 0.0139(14) -0.0007(13) C203 0.036(2) 0.0237(17) 0.047(2) -0.0020(14) 0.0249(17) -0.0081(15) C204 0.045(2) 0.0166(16) 0.0446(19) 0.0033(14) 0.0198(18) -0.0039(15) C205 0.034(2) 0.0223(17) 0.0413(19) 0.0044(14) 0.0108(16) 0.0051(14) C206 0.0240(17) 0.0184(15) 0.0341(17) -0.0010(12) 0.0110(14) -0.0011(13) O211 0.0166(10) 0.0187(10) 0.0235(10) 0.0004(8) 0.0086(9) -0.0014(8) C212 0.0222(15) 0.0156(14) 0.0163(13) -0.0038(10) 0.0084(12) -0.0027(11) C213 0.0156(15) 0.0196(15) 0.0257(15) -0.0017(12) 0.0054(12) -0.0028(12) C214 0.0198(15) 0.0203(15) 0.0155(13) -0.0024(11) 0.0076(12) -0.0010(12) O215 0.0179(10) 0.0169(10) 0.0225(10) -0.0010(8) 0.0103(8) -0.0020(8) C221 0.0180(15) 0.0214(15) 0.0153(13) -0.0014(11) 0.0085(11) 0.0015(11) C222 0.0215(16) 0.0215(16) 0.0264(15) -0.0037(12) 0.0085(13) -0.0012(12) C223 0.0185(16) 0.0382(19) 0.0325(17) -0.0067(14) 0.0071(14) -0.0015(14) C224 0.0267(18) 0.0327(18) 0.0255(16) -0.0001(13) 0.0067(14) 0.0114(14) C225 0.0302(18) 0.0230(16) 0.0224(14) 0.0001(12) 0.0102(13) 0.0052(13) C226 0.0192(15) 0.0236(15) 0.0210(14) -0.0017(11) 0.0072(12) 0.0014(12) C231 0.0173(15) 0.0214(15) 0.0132(12) -0.0010(11) 0.0038(11) -0.0028(11) C232 0.0238(16) 0.0213(16) 0.0344(17) -0.0049(13) 0.0153(14) -0.0028(13) C233 0.0244(17) 0.0325(18) 0.0406(18) -0.0063(14) 0.0182(15) -0.0082(14) C234 0.0311(18) 0.0252(17) 0.0296(16) -0.0050(13) 0.0151(14) -0.0127(14) C235 0.0347(19) 0.0193(16) 0.0378(18) -0.0004(13) 0.0190(16) -0.0005(14) C236 0.0232(16) 0.0238(16) 0.0328(16) -0.0025(13) 0.0141(14) -0.0021(13) O241 0.0184(11) 0.0183(10) 0.0264(10) -0.0030(8) 0.0116(9) -0.0008(8) C242 0.0165(14) 0.0213(15) 0.0135(12) 0.0007(11) 0.0045(11) -0.0016(11) C243 0.0173(15) 0.0202(15) 0.0220(14) 0.0009(11) 0.0083(12) 0.0019(12) C244 0.0170(14) 0.0194(14) 0.0131(12) 0.0021(10) 0.0042(11) 0.0049(11) O245 0.0213(11) 0.0170(10) 0.0204(10) -0.0005(8) 0.0105(9) 0.0002(8) C251 0.0211(15) 0.0171(14) 0.0150(12) 0.0024(11) 0.0053(11) 0.0032(11) C252 0.0270(17) 0.0197(15) 0.0280(15) -0.0004(12) 0.0141(13) -0.0004(12) C253 0.041(2) 0.0292(18) 0.0363(18) -0.0031(14) 0.0261(16) 0.0049(15) C254 0.046(2) 0.0202(16) 0.0348(17) -0.0036(13) 0.0196(16) 0.0049(15) C255 0.0359(19) 0.0195(16) 0.0346(17) -0.0013(13) 0.0136(15) -0.0023(14) C256 0.0250(16) 0.0192(15) 0.0252(15) 0.0021(12) 0.0120(13) 0.0034(12) N261 0.0222(13) 0.0156(12) 0.0274(13) -0.0054(10) 0.0098(11) -0.0019(10) N262 0.0199(13) 0.0150(12) 0.0253(12) -0.0038(9) 0.0106(11) 0.0001(10) C263 0.0176(15) 0.0238(15) 0.0210(14) -0.0056(11) 0.0087(12) -0.0007(12) C264 0.0240(17) 0.0305(17) 0.0246(15) -0.0087(13) 0.0057(13) -0.0054(13) C265 0.0288(18) 0.0222(16) 0.0364(17) -0.0083(13) 0.0140(15) -0.0050(13) N271 0.0196(13) 0.0207(13) 0.0208(12) -0.0020(10) 0.0083(10) 0.0018(10) C272 0.0143(14) 0.0245(16) 0.0211(14) -0.0028(11) 0.0080(12) 0.0017(12) C273 0.0274(17) 0.0308(17) 0.0203(14) -0.0059(12) 0.0083(13) 0.0013(13) C274 0.0281(18) 0.0381(19) 0.0193(14) -0.0001(13) 0.0093(13) 0.0062(14) C275 0.0240(16) 0.0256(16) 0.0264(15) 0.0054(12) 0.0120(13) 0.0071(13) C276 0.0260(17) 0.0220(16) 0.0237(15) -0.0032(12) 0.0104(13) -0.0010(13) N281 0.0298(15) 0.0116(12) 0.0293(13) 0.0006(10) 0.0147(11) -0.0002(10) N282 0.0188(13) 0.0145(12) 0.0262(12) -0.0002(9) 0.0099(11) 0.0001(10) C283 0.0181(15) 0.0231(15) 0.0222(14) 0.0018(11) 0.0093(12) 0.0017(12) C284 0.0345(19) 0.0232(16) 0.0294(16) 0.0074(13) 0.0157(14) 0.0033(14) C285 0.0318(18) 0.0153(15) 0.0387(17) 0.0067(13) 0.0182(15) 0.0046(13) N291 0.0167(12) 0.0177(12) 0.0165(11) -0.0008(9) 0.0056(10) -0.0005(9) C292 0.0165(14) 0.0200(15) 0.0222(14) 0.0023(11) 0.0092(12) 0.0004(11) C293 0.0254(17) 0.0273(17) 0.0234(15) 0.0057(12) 0.0079(13) -0.0005(13) C294 0.0237(17) 0.0342(18) 0.0195(14) -0.0028(13) 0.0075(13) -0.0031(13) C295 0.0227(16) 0.0234(16) 0.0224(14) -0.0045(12) 0.0080(13) -0.0004(12) C296 0.0226(16) 0.0188(15) 0.0205(14) 0.0008(11) 0.0060(12) -0.0005(12) Cl1 0.0585(7) 0.0493(6) 0.0664(7) -0.0050(5) 0.0369(6) -0.0101(5) C300 0.036(4) 0.031(4) 0.054(4) -0.008(3) 0.025(4) -0.001(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 Yb1 O145 2.247(2) . ? Yb1 O115 2.256(2) . ? Yb1 O111 2.2743(18) . ? Yb1 O141 2.2879(19) . ? Yb1 N182 2.452(2) . ? Yb1 N162 2.466(2) . ? Yb1 N171 2.478(2) . ? Yb1 N191 2.509(2) . ? B1 N161 1.542(4) . ? B1 N181 1.546(4) . ? C101 C102 1.394(4) . ? C101 C106 1.399(4) . ? C101 C112 1.499(4) . ? C102 C103 1.394(4) . ? C103 C104 1.383(4) . ? C104 C105 1.379(4) . ? C105 C106 1.386(4) . ? O111 C112 1.267(3) . ? C112 C113 1.403(4) . ? C113 C114 1.400(4) . ? C114 O115 1.270(3) . ? C114 C121 1.492(4) . ? C121 C126 1.399(4) . ? C121 C122 1.400(4) . ? C122 C123 1.391(4) . ? C123 C124 1.385(4) . ? C124 C125 1.384(4) . ? C125 C126 1.379(4) . ? C131 C136 1.391(4) . ? C131 C132 1.396(4) . ? C131 C142 1.504(4) . ? C132 C133 1.390(4) . ? C133 C134 1.378(4) . ? C134 C135 1.387(4) . ? C135 C136 1.380(4) . ? O141 C142 1.276(3) . ? C142 C143 1.396(4) . ? C143 C144 1.394(4) . ? C144 O145 1.281(3) . ? C144 C151 1.495(4) . ? C151 C156 1.391(4) . ? C151 C152 1.397(4) . ? C152 C153 1.388(4) . ? C153 C154 1.369(5) . ? C154 C155 1.382(5) . ? C155 C156 1.389(4) . ? N161 C165 1.344(4) . ? N161 N162 1.358(3) . ? N162 C163 1.344(3) . ? C163 C164 1.394(4) . ? C163 C172 1.459(4) . ? C164 C165 1.370(4) . ? N171 C176 1.343(3) . ? N171 C172 1.351(3) . ? C172 C173 1.390(4) . ? C173 C174 1.376(4) . ? C174 C175 1.374(4) . ? C175 C176 1.385(4) . ? N181 C185 1.348(4) . ? N181 N182 1.359(3) . ? N182 C183 1.343(4) . ? C183 C184 1.391(4) . ? C183 C192 1.462(4) . ? C184 C185 1.372(4) . ? N191 C196 1.349(3) . ? N191 C192 1.351(4) . ? C192 C193 1.392(4) . ? C193 C194 1.385(4) . ? C194 C195 1.381(4) . ? C195 C196 1.381(4) . ? Yb2 O215 2.228(2) . ? Yb2 O241 2.232(2) . ? Yb2 O211 2.2841(19) . ? Yb2 O245 2.3051(19) . ? Yb2 N262 2.450(2) . ? Yb2 N271 2.475(2) . ? Yb2 N282 2.475(2) . ? Yb2 N291 2.496(2) . ? B2 N261 1.549(4) . ? B2 N281 1.561(4) . ? C201 C202 1.385(4) . ? C201 C206 1.393(4) . ? C201 C212 1.507(4) . ? C202 C203 1.390(4) . ? C203 C204 1.384(5) . ? C204 C205 1.382(5) . ? C205 C206 1.387(4) . ? O211 C212 1.268(3) . ? C212 C213 1.397(4) . ? C213 C214 1.399(4) . ? C214 O215 1.272(3) . ? C214 C221 1.498(4) . ? C221 C222 1.392(4) . ? C221 C226 1.396(4) . ? C222 C223 1.385(4) . ? C223 C224 1.376(4) . ? C224 C225 1.383(4) . ? C225 C226 1.374(4) . ? C231 C236 1.389(4) . ? C231 C232 1.391(4) . ? C231 C242 1.500(4) . ? C232 C233 1.383(4) . ? C233 C234 1.382(4) . ? C234 C235 1.369(4) . ? C235 C236 1.387(4) . ? O241 C242 1.263(3) . ? C242 C243 1.404(4) . ? C243 C244 1.403(4) . ? C244 O245 1.264(3) . ? C244 C251 1.512(4) . ? C251 C252 1.393(4) . ? C251 C256 1.396(4) . ? C252 C253 1.389(4) . ? C253 C254 1.380(5) . ? C254 C255 1.377(5) . ? C255 C256 1.386(4) . ? N261 C265 1.354(4) . ? N261 N262 1.361(3) . ? N262 C263 1.342(3) . ? C263 C264 1.400(4) . ? C263 C272 1.458(4) . ? C264 C265 1.361(4) . ? N271 C276 1.340(3) . ? N271 C272 1.350(3) . ? C272 C273 1.388(4) . ? C273 C274 1.377(4) . ? C274 C275 1.383(4) . ? C275 C276 1.380(4) . ? N281 C285 1.348(4) . ? N281 N282 1.356(3) . ? N282 C283 1.343(3) . ? C283 C284 1.399(4) . ? C283 C292 1.458(4) . ? C284 C285 1.369(4) . ? N291 C296 1.340(3) . ? N291 C292 1.356(3) . ? C292 C293 1.390(4) . ? C293 C294 1.382(4) . ? C294 C295 1.385(4) . ? C295 C296 1.382(4) . ? Cl1 C300 1.771(7) . ? Cl1 C300 1.880(7) 3_766 ? C300 Cl1 1.880(7) 3_766 ? 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 O145 Yb1 O115 143.33(7) . . ? O145 Yb1 O111 144.44(6) . . ? O115 Yb1 O111 72.20(7) . . ? O145 Yb1 O141 72.92(7) . . ? O115 Yb1 O141 143.75(6) . . ? O111 Yb1 O141 71.56(7) . . ? O145 Yb1 N182 78.96(7) . . ? O115 Yb1 N182 72.86(7) . . ? O111 Yb1 N182 125.01(7) . . ? O141 Yb1 N182 131.39(7) . . ? O145 Yb1 N162 80.19(7) . . ? O115 Yb1 N162 71.16(7) . . ? O111 Yb1 N162 127.10(7) . . ? O141 Yb1 N162 133.29(7) . . ? N182 Yb1 N162 77.22(8) . . ? O145 Yb1 N171 100.13(7) . . ? O115 Yb1 N171 88.64(7) . . ? O111 Yb1 N171 76.72(7) . . ? O141 Yb1 N171 82.17(7) . . ? N182 Yb1 N171 142.31(7) . . ? N162 Yb1 N171 65.66(7) . . ? O145 Yb1 N191 97.97(7) . . ? O115 Yb1 N191 91.34(7) . . ? O111 Yb1 N191 74.25(7) . . ? O141 Yb1 N191 79.93(7) . . ? N182 Yb1 N191 65.54(8) . . ? N162 Yb1 N191 142.24(7) . . ? N171 Yb1 N191 149.47(7) . . ? N161 B1 N181 109.5(2) . . ? C102 C101 C106 118.3(3) . . ? C102 C101 C112 123.9(3) . . ? C106 C101 C112 117.7(3) . . ? C103 C102 C101 120.7(3) . . ? C104 C103 C102 120.0(3) . . ? C105 C104 C103 120.0(3) . . ? C104 C105 C106 120.3(3) . . ? C105 C106 C101 120.7(3) . . ? C112 O111 Yb1 137.59(17) . . ? O111 C112 C113 123.7(2) . . ? O111 C112 C101 115.7(2) . . ? C113 C112 C101 120.6(2) . . ? C114 C113 C112 122.0(3) . . ? O115 C114 C113 124.0(2) . . ? O115 C114 C121 115.3(2) . . ? C113 C114 C121 120.7(2) . . ? C114 O115 Yb1 138.55(17) . . ? C126 C121 C122 118.5(3) . . ? C126 C121 C114 118.1(2) . . ? C122 C121 C114 123.4(2) . . ? C123 C122 C121 120.4(3) . . ? C124 C123 C122 120.2(3) . . ? C125 C124 C123 119.7(3) . . ? C126 C125 C124 120.6(3) . . ? C125 C126 C121 120.6(3) . . ? C136 C131 C132 118.8(3) . . ? C136 C131 C142 118.5(2) . . ? C132 C131 C142 122.7(3) . . ? C133 C132 C131 120.2(3) . . ? C134 C133 C132 120.2(3) . . ? C133 C134 C135 120.0(3) . . ? C136 C135 C134 120.0(3) . . ? C135 C136 C131 120.8(3) . . ? C142 O141 Yb1 136.59(17) . . ? O141 C142 C143 123.9(2) . . ? O141 C142 C131 116.5(2) . . ? C143 C142 C131 119.6(2) . . ? C144 C143 C142 122.9(3) . . ? O145 C144 C143 124.1(3) . . ? O145 C144 C151 115.6(2) . . ? C143 C144 C151 120.3(3) . . ? C144 O145 Yb1 138.15(17) . . ? C156 C151 C152 118.8(3) . . ? C156 C151 C144 119.0(3) . . ? C152 C151 C144 122.2(3) . . ? C153 C152 C151 119.9(3) . . ? C154 C153 C152 120.8(3) . . ? C153 C154 C155 120.0(3) . . ? C154 C155 C156 119.9(3) . . ? C155 C156 C151 120.6(3) . . ? C165 N161 N162 109.2(2) . . ? C165 N161 B1 128.3(3) . . ? N162 N161 B1 122.2(2) . . ? C163 N162 N161 106.5(2) . . ? C163 N162 Yb1 117.01(17) . . ? N161 N162 Yb1 130.00(17) . . ? N162 C163 C164 110.4(2) . . ? N162 C163 C172 118.7(2) . . ? C164 C163 C172 130.8(3) . . ? C165 C164 C163 104.3(3) . . ? N161 C165 C164 109.6(3) . . ? C176 N171 C172 117.7(2) . . ? C176 N171 Yb1 122.03(18) . . ? C172 N171 Yb1 118.97(18) . . ? N171 C172 C173 122.3(3) . . ? N171 C172 C163 115.1(2) . . ? C173 C172 C163 122.6(2) . . ? C174 C173 C172 119.0(3) . . ? C175 C174 C173 119.1(3) . . ? C174 C175 C176 119.1(3) . . ? N171 C176 C175 122.7(3) . . ? C185 N181 N182 108.7(2) . . ? C185 N181 B1 127.7(3) . . ? N182 N181 B1 123.5(3) . . ? C183 N182 N181 106.5(2) . . ? C183 N182 Yb1 116.81(17) . . ? N181 N182 Yb1 129.01(17) . . ? N182 C183 C184 111.1(3) . . ? N182 C183 C192 118.4(3) . . ? C184 C183 C192 130.5(3) . . ? C185 C184 C183 103.6(3) . . ? N181 C185 C184 110.1(3) . . ? C196 N191 C192 117.7(3) . . ? C196 N191 Yb1 123.71(19) . . ? C192 N191 Yb1 117.99(18) . . ? N191 C192 C193 122.4(3) . . ? N191 C192 C183 115.1(3) . . ? C193 C192 C183 122.5(3) . . ? C194 C193 C192 119.0(3) . . ? C195 C194 C193 118.9(3) . . ? C194 C195 C196 119.2(3) . . ? N191 C196 C195 122.9(3) . . ? O215 Yb2 O241 146.07(7) . . ? O215 Yb2 O211 72.39(7) . . ? O241 Yb2 O211 141.34(7) . . ? O215 Yb2 O245 138.20(7) . . ? O241 Yb2 O245 71.71(7) . . ? O211 Yb2 O245 70.99(7) . . ? O215 Yb2 N262 86.19(8) . . ? O241 Yb2 N262 74.35(7) . . ? O211 Yb2 N262 127.04(7) . . ? O245 Yb2 N262 132.63(7) . . ? O215 Yb2 N271 110.12(8) . . ? O241 Yb2 N271 87.47(8) . . ? O211 Yb2 N271 76.46(7) . . ? O245 Yb2 N271 80.01(7) . . ? N262 Yb2 N271 66.35(8) . . ? O215 Yb2 N282 72.91(7) . . ? O241 Yb2 N282 75.45(8) . . ? O211 Yb2 N282 136.24(7) . . ? O245 Yb2 N282 124.53(7) . . ? N262 Yb2 N282 75.71(8) . . ? N271 Yb2 N282 141.40(7) . . ? O215 Yb2 N291 83.55(8) . . ? O241 Yb2 N291 94.15(8) . . ? O211 Yb2 N291 85.16(7) . . ? O245 Yb2 N291 74.00(7) . . ? N262 Yb2 N291 140.85(7) . . ? N271 Yb2 N291 151.95(7) . . ? N282 Yb2 N291 65.16(7) . . ? N261 B2 N281 110.5(2) . . ? C202 C201 C206 118.5(3) . . ? C202 C201 C212 123.4(3) . . ? C206 C201 C212 118.0(3) . . ? C201 C202 C203 121.0(3) . . ? C204 C203 C202 119.8(3) . . ? C205 C204 C203 119.9(3) . . ? C204 C205 C206 120.0(3) . . ? C205 C206 C201 120.8(3) . . ? C212 O211 Yb2 137.68(17) . . ? O211 C212 C213 123.1(3) . . ? O211 C212 C201 116.4(2) . . ? C213 C212 C201 120.5(3) . . ? C212 C213 C214 122.6(3) . . ? O215 C214 C213 123.2(3) . . ? O215 C214 C221 115.6(2) . . ? C213 C214 C221 121.1(3) . . ? C214 O215 Yb2 138.06(18) . . ? C222 C221 C226 118.2(3) . . ? C222 C221 C214 123.4(3) . . ? C226 C221 C214 118.4(3) . . ? C223 C222 C221 121.0(3) . . ? C224 C223 C222 119.9(3) . . ? C223 C224 C225 119.7(3) . . ? C226 C225 C224 120.7(3) . . ? C225 C226 C221 120.4(3) . . ? C236 C231 C232 118.9(3) . . ? C236 C231 C242 117.0(3) . . ? C232 C231 C242 124.0(3) . . ? C233 C232 C231 120.1(3) . . ? C234 C233 C232 120.6(3) . . ? C235 C234 C233 119.5(3) . . ? C234 C235 C236 120.6(3) . . ? C235 C236 C231 120.3(3) . . ? C242 O241 Yb2 139.54(18) . . ? O241 C242 C243 123.1(3) . . ? O241 C242 C231 115.1(2) . . ? C243 C242 C231 121.8(3) . . ? C244 C243 C242 122.2(3) . . ? O245 C244 C243 123.6(3) . . ? O245 C244 C251 115.4(2) . . ? C243 C244 C251 121.0(3) . . ? C244 O245 Yb2 135.05(17) . . ? C252 C251 C256 118.2(3) . . ? C252 C251 C244 123.7(3) . . ? C256 C251 C244 118.1(3) . . ? C253 C252 C251 120.3(3) . . ? C254 C253 C252 120.7(3) . . ? C255 C254 C253 119.7(3) . . ? C254 C255 C256 119.9(3) . . ? C255 C256 C251 121.2(3) . . ? C265 N261 N262 109.0(2) . . ? C265 N261 B2 126.6(2) . . ? N262 N261 B2 123.7(2) . . ? C263 N262 N261 106.5(2) . . ? C263 N262 Yb2 117.48(18) . . ? N261 N262 Yb2 131.76(17) . . ? N262 C263 C264 110.5(3) . . ? N262 C263 C272 119.0(2) . . ? C264 C263 C272 130.5(3) . . ? C265 C264 C263 104.4(3) . . ? N261 C265 C264 109.6(3) . . ? C276 N271 C272 117.5(2) . . ? C276 N271 Yb2 123.28(18) . . ? C272 N271 Yb2 119.21(18) . . ? N271 C272 C273 122.0(3) . . ? N271 C272 C263 115.3(2) . . ? C273 C272 C263 122.7(3) . . ? C274 C273 C272 119.6(3) . . ? C273 C274 C275 118.8(3) . . ? C276 C275 C274 118.4(3) . . ? N271 C276 C275 123.7(3) . . ? C285 N281 N282 108.9(2) . . ? C285 N281 B2 125.7(2) . . ? N282 N281 B2 122.7(2) . . ? C283 N282 N281 106.7(2) . . ? C283 N282 Yb2 119.65(17) . . ? N281 N282 Yb2 132.46(17) . . ? N282 C283 C284 110.6(2) . . ? N282 C283 C292 118.5(2) . . ? C284 C283 C292 130.9(3) . . ? C285 C284 C283 103.8(3) . . ? N281 C285 C284 110.0(3) . . ? C296 N291 C292 117.7(2) . . ? C296 N291 Yb2 121.67(17) . . ? C292 N291 Yb2 120.60(17) . . ? N291 C292 C293 122.1(3) . . ? N291 C292 C283 115.1(2) . . ? C293 C292 C283 122.8(3) . . ? C294 C293 C292 119.1(3) . . ? C293 C294 C295 119.1(3) . . ? C296 C295 C294 118.6(3) . . ? N291 C296 C295 123.4(3) . . ? C300 Cl1 C300 74.1(3) . 3_766 ? Cl1 C300 Cl1 105.9(3) . 3_766 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.915 _refine_diff_density_min -0.699 _refine_diff_density_rms 0.090 #=END data_plutom _database_code_depnum_ccdc_archive 'CCDC 229471' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46.25 H36.50 B Cl0.50 N6 O4 Tb' _chemical_formula_sum 'C46.25 H36.50 B Cl0.50 N6 O4 Tb' _chemical_formula_weight 927.77 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' B B 0.0013 0.0007 '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' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.624(4) _cell_length_b 26.721(5) _cell_length_c 19.177(4) _cell_angle_alpha 90.00 _cell_angle_beta 116.84(3) _cell_angle_gamma 90.00 _cell_volume 8058(3) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 24101 _cell_measurement_theta_min 4.502 _cell_measurement_theta_max 54.959 _exptl_crystal_description Needle _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.529 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3732 _exptl_absorpt_coefficient_mu 1.841 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.588008 _exptl_absorpt_correction_T_max 0.719341 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 87683 _diffrn_reflns_av_R_equivalents 0.0361 _diffrn_reflns_av_sigmaI/netI 0.0404 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 27.50 _reflns_number_total 17377 _reflns_number_gt 13889 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL/XCIF' _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^)+(0.0283P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17377 _refine_ls_number_parameters 1063 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0364 _refine_ls_R_factor_gt 0.0263 _refine_ls_wR_factor_ref 0.0596 _refine_ls_wR_factor_gt 0.0573 _refine_ls_goodness_of_fit_ref 0.937 _refine_ls_restrained_S_all 0.937 _refine_ls_shift/su_max 0.005 _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 Tb1 Tb 1.008203(7) 0.694024(4) 0.234214(8) 0.01504(4) Uani 1 1 d . . . Tb2 Tb 0.493861(7) 0.506373(5) 0.275619(8) 0.01532(4) Uani 1 1 d . . . B1 B 0.9966(2) 0.84100(12) 0.2446(2) 0.0249(8) Uani 1 1 d . . . H1A H 1.0533 0.8410 0.2905 0.030 Uiso 1 1 calc R . . H1B H 0.9757 0.8759 0.2344 0.030 Uiso 1 1 calc R . . C101 C 0.77042(15) 0.73176(10) 0.00399(16) 0.0175(6) Uani 1 1 d . . . C102 C 0.77209(16) 0.78114(10) 0.03078(17) 0.0217(6) Uani 1 1 d . . . H10B H 0.8099 0.7905 0.0828 0.026 Uiso 1 1 calc R . . C103 C 0.71703(16) 0.81517(10) -0.02129(18) 0.0249(7) Uani 1 1 d . . . H10D H 0.7154 0.8484 -0.0044 0.030 Uiso 1 1 calc R . . C104 C 0.66154(16) 0.80133(10) -0.10145(18) 0.0265(7) Uani 1 1 d . . . H10E H 0.6252 0.8260 -0.1361 0.032 Uiso 1 1 calc R . . C105 C 0.65983(16) 0.75277(11) -0.12935(18) 0.0265(7) Uani 1 1 d . . . H10C H 0.6236 0.7440 -0.1821 0.032 Uiso 1 1 calc R . . C106 C 0.71369(15) 0.71795(10) -0.07623(17) 0.0224(6) Uani 1 1 d . . . H10A H 0.7134 0.6844 -0.0927 0.027 Uiso 1 1 calc R . . O111 O 0.89194(10) 0.71695(6) 0.12013(11) 0.0204(4) Uani 1 1 d . . . C112 C 0.83121(15) 0.69652(10) 0.06365(16) 0.0175(6) Uani 1 1 d . . . C113 C 0.81825(16) 0.64478(9) 0.05644(17) 0.0202(6) Uani 1 1 d . . . H11A H 0.7677 0.6327 0.0142 0.024 Uiso 1 1 calc R . . C114 C 0.87472(15) 0.61003(9) 0.10717(16) 0.0166(6) Uani 1 1 d . . . O115 O 0.94255(10) 0.62242(6) 0.16304(11) 0.0199(4) Uani 1 1 d . . . C121 C 0.85882(16) 0.55492(10) 0.09734(16) 0.0178(6) Uani 1 1 d . . . C122 C 0.91850(16) 0.52266(10) 0.14879(18) 0.0244(7) Uani 1 1 d . . . H12B H 0.9682 0.5359 0.1906 0.029 Uiso 1 1 calc R . . C123 C 0.90795(18) 0.47124(10) 0.1412(2) 0.0305(7) Uani 1 1 d . . . H12E H 0.9506 0.4498 0.1774 0.037 Uiso 1 1 calc R . . C124 C 0.83772(18) 0.45143(10) 0.08305(19) 0.0269(7) Uani 1 1 d . . . H12D H 0.8302 0.4162 0.0778 0.032 Uiso 1 1 calc R . . C125 C 0.77788(18) 0.48279(10) 0.03200(18) 0.0253(7) Uani 1 1 d . . . H12C H 0.7281 0.4692 -0.0094 0.030 Uiso 1 1 calc R . . C126 C 0.78802(16) 0.53443(10) 0.03919(17) 0.0221(6) Uani 1 1 d . . . H12A H 0.7449 0.5556 0.0030 0.027 Uiso 1 1 calc R . . C131 C 1.16413(15) 0.56131(10) 0.39464(17) 0.0191(6) Uani 1 1 d . . . C132 C 1.20837(16) 0.54395(10) 0.47735(18) 0.0252(7) Uani 1 1 d . . . H13C H 1.2270 0.5675 0.5189 0.030 Uiso 1 1 calc R . . C133 C 1.22217(18) 0.49308(11) 0.49313(19) 0.0293(7) Uani 1 1 d . . . H13A H 1.2502 0.4809 0.5452 0.035 Uiso 1 1 calc R . . C134 C 1.19212(17) 0.45937(11) 0.42691(19) 0.0300(7) Uani 1 1 d . . . H13D H 1.2004 0.4245 0.4370 0.036 Uiso 1 1 calc R . . C135 C 1.14936(17) 0.47604(10) 0.34458(19) 0.0287(7) Uani 1 1 d . . . H13E H 1.1321 0.4524 0.3032 0.034 Uiso 1 1 calc R . . C136 C 1.13484(16) 0.52669(10) 0.32867(18) 0.0239(6) Uani 1 1 d . . . H13B H 1.1067 0.5385 0.2764 0.029 Uiso 1 1 calc R . . O141 O 1.08590(10) 0.62480(6) 0.30256(11) 0.0202(4) Uani 1 1 d . . . C142 C 1.14435(15) 0.61563(10) 0.37332(16) 0.0180(6) Uani 1 1 d . . . C143 C 1.19077(16) 0.65252(10) 0.42979(17) 0.0221(6) Uani 1 1 d . . . H14A H 1.2327 0.6421 0.4797 0.027 Uiso 1 1 calc R . . C144 C 1.17700(16) 0.70371(10) 0.41447(16) 0.0197(6) Uani 1 1 d . . . O145 O 1.11849(11) 0.72190(6) 0.35006(11) 0.0215(4) Uani 1 1 d . . . C151 C 1.23354(16) 0.74071(10) 0.47423(17) 0.0212(6) Uani 1 1 d . . . C152 C 1.28536(17) 0.72875(11) 0.55736(18) 0.0292(7) Uani 1 1 d . . . H15D H 1.2844 0.6956 0.5748 0.035 Uiso 1 1 calc R . . C153 C 1.33600(19) 0.76457(12) 0.6115(2) 0.0368(8) Uani 1 1 d . . . H15E H 1.3691 0.7567 0.6652 0.044 Uiso 1 1 calc R . . C154 C 1.33523(18) 0.81257(11) 0.5821(2) 0.0330(8) Uani 1 1 d . . . H15C H 1.3688 0.8380 0.6170 0.040 Uiso 1 1 calc R . . C155 C 1.28415(17) 0.82496(11) 0.49912(19) 0.0296(7) Uani 1 1 d . . . H15B H 1.2861 0.8580 0.4817 0.036 Uiso 1 1 calc R . . C156 C 1.23311(16) 0.78942(10) 0.44566(18) 0.0244(7) Uani 1 1 d . . . H15A H 1.1994 0.7976 0.3922 0.029 Uiso 1 1 calc R . . N161 N 1.06234(12) 0.68014(8) 0.12909(13) 0.0187(5) Uani 1 1 d . . . C162 C 1.05873(15) 0.71762(10) 0.07616(16) 0.0188(6) Uani 1 1 d . . . C163 C 1.07303(16) 0.70984(11) 0.00647(17) 0.0238(6) Uani 1 1 d . . . H16C H 1.0692 0.7370 -0.0270 0.029 Uiso 1 1 calc R . . C164 C 1.09193(16) 0.66255(11) -0.00848(18) 0.0266(7) Uani 1 1 d . . . H16D H 1.1012 0.6555 -0.0526 0.032 Uiso 1 1 calc R . . C165 C 1.09694(16) 0.62427(11) 0.04587(17) 0.0242(7) Uani 1 1 d . . . H16B H 1.1113 0.5912 0.0381 0.029 Uiso 1 1 calc R . . C166 C 1.08074(15) 0.63449(10) 0.11289(17) 0.0210(6) Uani 1 1 d . . . H16A H 1.0834 0.6075 0.1462 0.025 Uiso 1 1 calc R . . N171 N 1.00473(13) 0.81904(8) 0.16789(13) 0.0189(5) Uani 1 1 d . . . N172 N 1.03107(13) 0.77204(8) 0.16873(13) 0.0186(5) Uani 1 1 d . . . C173 C 1.03693(15) 0.76670(10) 0.09615(16) 0.0196(6) Uani 1 1 d . . . C174 C 1.01534(17) 0.81062(10) 0.04867(18) 0.0252(7) Uani 1 1 d . . . H174 H 1.0149 0.8166 -0.0004 0.030 Uiso 1 1 calc R . . C175 C 0.99500(16) 0.84245(10) 0.09633(17) 0.0249(7) Uani 1 1 d . . . H175 H 0.9767 0.8761 0.0828 0.030 Uiso 1 1 calc R . . N181 N 0.93712(14) 0.80997(8) 0.26158(14) 0.0209(5) Uani 1 1 d . . . N182 N 0.94898(13) 0.76125(8) 0.28528(13) 0.0195(5) Uani 1 1 d . . . C183 C 0.88838(16) 0.74746(10) 0.29997(17) 0.0207(6) Uani 1 1 d . . . C184 C 0.83752(18) 0.78730(10) 0.28591(19) 0.0292(7) Uani 1 1 d . . . H18A H 0.7870 0.7885 0.2920 0.035 Uiso 1 1 calc R . . C185 C 0.87040(18) 0.82587(10) 0.26139(19) 0.0289(7) Uani 1 1 d . . . H18B H 0.8470 0.8585 0.2470 0.035 Uiso 1 1 calc R . . N191 N 0.93354(13) 0.66347(8) 0.31414(14) 0.0205(5) Uani 1 1 d . . . C192 C 0.88506(16) 0.69589(10) 0.32557(16) 0.0200(6) Uani 1 1 d . . . C193 C 0.83504(17) 0.68108(11) 0.35928(18) 0.0253(7) Uani 1 1 d . . . H19B H 0.7997 0.7049 0.3673 0.030 Uiso 1 1 calc R . . C194 C 0.83521(17) 0.63182(11) 0.38184(18) 0.0276(7) Uani 1 1 d . . . H19D H 0.8003 0.6220 0.4054 0.033 Uiso 1 1 calc R . . C195 C 0.88442(17) 0.59827(11) 0.37041(18) 0.0275(7) Uani 1 1 d . . . H19C H 0.8857 0.5642 0.3851 0.033 Uiso 1 1 calc R . . C196 C 0.93282(17) 0.61537(10) 0.33659(17) 0.0234(6) Uani 1 1 d . . . H19A H 0.9685 0.5920 0.3281 0.028 Uiso 1 1 calc R . . B2 B 0.4651(2) 0.35824(12) 0.2864(2) 0.0254(8) Uani 1 1 d . . . H2A H 0.4053 0.3607 0.2773 0.031 Uiso 1 1 calc R . . H2B H 0.4802 0.3223 0.2923 0.031 Uiso 1 1 calc R . . C201 C 0.22814(15) 0.48250(10) 0.16813(16) 0.0175(6) Uani 1 1 d . . . C202 C 0.15281(16) 0.50157(10) 0.14211(18) 0.0246(7) Uani 1 1 d . . . H20B H 0.1442 0.5357 0.1507 0.030 Uiso 1 1 calc R . . C203 C 0.08823(17) 0.47095(12) 0.10270(19) 0.0321(8) Uani 1 1 d . . . H20D H 0.0323 0.4843 0.0817 0.038 Uiso 1 1 calc R . . C204 C 0.09738(18) 0.42096(12) 0.09042(18) 0.0315(7) Uani 1 1 d . . . H20C H 0.0484 0.4009 0.0624 0.038 Uiso 1 1 calc R . . C205 C 0.17149(17) 0.40153(11) 0.11663(17) 0.0259(7) Uani 1 1 d . . . H20E H 0.1795 0.3672 0.1087 0.031 Uiso 1 1 calc R . . C206 C 0.23631(16) 0.43189(10) 0.15531(17) 0.0222(6) Uani 1 1 d . . . H20A H 0.2920 0.4183 0.1757 0.027 Uiso 1 1 calc R . . O211 O 0.36441(10) 0.49074(6) 0.23221(11) 0.0200(4) Uani 1 1 d . . . C212 C 0.30015(16) 0.51425(10) 0.20778(16) 0.0180(6) Uani 1 1 d . . . C213 C 0.29605(16) 0.56567(10) 0.21934(17) 0.0223(6) Uani 1 1 d . . . H21A H 0.2410 0.5803 0.1978 0.027 Uiso 1 1 calc R . . C214 C 0.36209(16) 0.59627(10) 0.25774(16) 0.0184(6) Uani 1 1 d . . . O215 O 0.43088(10) 0.58143(6) 0.27555(11) 0.0211(4) Uani 1 1 d . . . C221 C 0.35549(16) 0.64902(10) 0.28306(17) 0.0199(6) Uani 1 1 d . . . C222 C 0.28481(17) 0.67044(10) 0.27161(18) 0.0270(7) Uani 1 1 d . . . H22B H 0.2327 0.6533 0.2426 0.032 Uiso 1 1 calc R . . C223 C 0.28316(19) 0.71828(11) 0.3009(2) 0.0333(8) Uani 1 1 d . . . H22D H 0.2292 0.7322 0.2893 0.040 Uiso 1 1 calc R . . C224 C 0.35133(19) 0.74540(11) 0.3435(2) 0.0354(8) Uani 1 1 d . . . H22E H 0.3485 0.7772 0.3644 0.043 Uiso 1 1 calc R . . C225 C 0.42177(18) 0.72480(10) 0.3543(2) 0.0334(8) Uani 1 1 d . . . H22C H 0.4737 0.7421 0.3836 0.040 Uiso 1 1 calc R . . C226 C 0.42336(17) 0.67749(10) 0.32363(18) 0.0272(7) Uani 1 1 d . . . H22A H 0.4772 0.6646 0.3325 0.033 Uiso 1 1 calc R . . C231 C 0.62746(16) 0.62516(10) 0.20207(16) 0.0187(6) Uani 1 1 d . . . C232 C 0.68563(17) 0.63671(10) 0.17735(17) 0.0251(7) Uani 1 1 d . . . H23E H 0.7288 0.6130 0.1850 0.030 Uiso 1 1 calc R . . C233 C 0.68532(19) 0.68260(11) 0.14049(19) 0.0320(7) Uani 1 1 d . . . H23C H 0.7292 0.6887 0.1257 0.038 Uiso 1 1 calc R . . C234 C 0.62699(19) 0.71714(11) 0.12578(19) 0.0325(7) Uani 1 1 d . . . H23B H 0.6265 0.7477 0.1002 0.039 Uiso 1 1 calc R . . C235 C 0.56891(18) 0.70616(11) 0.14933(18) 0.0296(7) Uani 1 1 d . . . H23D H 0.5250 0.7297 0.1401 0.036 Uiso 1 1 calc R . . C236 C 0.56982(16) 0.66095(10) 0.18751(17) 0.0223(6) Uani 1 1 d . . . H23A H 0.5269 0.6557 0.2038 0.027 Uiso 1 1 calc R . . O241 O 0.56925(10) 0.57276(6) 0.26452(11) 0.0189(4) Uani 1 1 d . . . C242 C 0.62353(15) 0.57611(9) 0.24186(15) 0.0161(6) Uani 1 1 d . . . C243 C 0.67428(15) 0.53674(9) 0.24911(16) 0.0187(6) Uani 1 1 d . . . H24A H 0.7189 0.5417 0.2349 0.022 Uiso 1 1 calc R . . C244 C 0.66677(15) 0.48867(10) 0.27604(16) 0.0179(6) Uani 1 1 d . . . O245 O 0.61305(11) 0.47638(7) 0.29559(12) 0.0223(4) Uani 1 1 d . . . C251 C 0.71977(15) 0.44660(10) 0.27895(16) 0.0179(6) Uani 1 1 d . . . C252 C 0.78893(17) 0.45336(11) 0.27207(18) 0.0267(7) Uani 1 1 d . . . H25A H 0.8077 0.4859 0.2673 0.032 Uiso 1 1 calc R . . C253 C 0.83305(18) 0.41219(11) 0.27204(19) 0.0311(7) Uani 1 1 d . . . H25D H 0.8842 0.4167 0.2676 0.037 Uiso 1 1 calc R . . C254 C 0.80932(17) 0.36440(11) 0.27794(18) 0.0284(7) Uani 1 1 d . . . H25C H 0.8430 0.3368 0.2773 0.034 Uiso 1 1 calc R . . C255 C 0.74063(17) 0.35733(11) 0.28444(19) 0.0308(7) Uani 1 1 d . . . H25E H 0.7218 0.3246 0.2884 0.037 Uiso 1 1 calc R . . C256 C 0.69675(17) 0.39809(10) 0.28532(18) 0.0259(7) Uani 1 1 d . . . H25B H 0.6463 0.3933 0.2907 0.031 Uiso 1 1 calc R . . N261 N 0.56056(13) 0.53181(8) 0.43009(14) 0.0201(5) Uani 1 1 d . . . C262 C 0.58841(15) 0.49610(10) 0.49094(17) 0.0195(6) Uani 1 1 d . . . C263 C 0.62656(17) 0.50801(11) 0.57661(17) 0.0244(6) Uani 1 1 d . . . H26A H 0.6446 0.4817 0.6140 0.029 Uiso 1 1 calc R . . C264 C 0.63549(17) 0.55740(11) 0.60118(18) 0.0257(7) Uani 1 1 d . . . H26D H 0.6583 0.5664 0.6548 0.031 Uiso 1 1 calc R . . C265 C 0.60769(16) 0.59392(11) 0.53960(17) 0.0247(7) Uani 1 1 d . . . H26C H 0.6127 0.6284 0.5529 0.030 Uiso 1 1 calc R . . C266 C 0.57132(16) 0.57959(10) 0.45571(18) 0.0239(6) Uani 1 1 d . . . H26B H 0.5547 0.6056 0.4179 0.029 Uiso 1 1 calc R . . N271 N 0.52316(13) 0.38508(8) 0.36760(14) 0.0226(5) Uani 1 1 d . . . N272 N 0.52424(13) 0.43564(8) 0.37836(14) 0.0188(5) Uani 1 1 d . . . C273 C 0.57399(16) 0.44434(10) 0.46003(17) 0.0207(6) Uani 1 1 d . . . C274 C 0.60452(17) 0.39965(11) 0.50293(18) 0.0274(7) Uani 1 1 d . . . H274 H 0.6383 0.3950 0.5575 0.033 Uiso 1 1 calc R . . C275 C 0.57104(17) 0.36360(10) 0.44225(18) 0.0267(7) Uani 1 1 d . . . H275 H 0.5799 0.3286 0.4509 0.032 Uiso 1 1 calc R . . N281 N 0.46950(13) 0.37882(8) 0.20636(14) 0.0218(5) Uani 1 1 d . . . N282 N 0.46046(13) 0.42812(8) 0.18528(14) 0.0195(5) Uani 1 1 d . . . C283 C 0.44544(15) 0.43122(10) 0.10389(17) 0.0207(6) Uani 1 1 d . . . C284 C 0.44428(17) 0.38357(10) 0.07054(19) 0.0274(7) Uani 1 1 d . . . H284 H 0.4359 0.3748 0.0196 0.033 Uiso 1 1 calc R . . C285 C 0.45970(17) 0.35234(11) 0.13745(19) 0.0290(7) Uani 1 1 d . . . H285 H 0.4631 0.3169 0.1359 0.035 Uiso 1 1 calc R . . N291 N 0.44653(13) 0.51996(8) 0.11697(14) 0.0192(5) Uani 1 1 d . . . C292 C 0.43269(16) 0.48053(10) 0.06381(17) 0.0206(6) Uani 1 1 d . . . C293 C 0.40768(16) 0.48698(11) -0.02256(17) 0.0253(7) Uani 1 1 d . . . H29C H 0.3983 0.4583 -0.0547 0.030 Uiso 1 1 calc R . . C294 C 0.39832(16) 0.53478(11) -0.05530(18) 0.0270(7) Uani 1 1 d . . . H294 H 0.3836 0.5401 -0.1089 0.032 Uiso 1 1 calc R . . C295 C 0.41281(16) 0.57500(11) -0.00141(17) 0.0243(7) Uani 1 1 d . . . H29E H 0.4077 0.6085 -0.0197 0.029 Uiso 1 1 calc R . . C296 C 0.43600(15) 0.56598(10) 0.08349(17) 0.0222(6) Uani 1 1 d . . . H29D H 0.4438 0.5944 0.1158 0.027 Uiso 1 1 calc R . . Cl1 Cl 0.00675(6) 0.48693(3) 0.42353(6) 0.0514(2) Uani 1 1 d . . . C300 C 0.0465(4) 0.5284(2) 0.5177(4) 0.0389(17) Uani 0.50 1 d P . . H30A H 0.1085 0.5236 0.5494 0.047 Uiso 0.50 1 calc PR . . H30B H 0.0364 0.5640 0.5024 0.047 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 Tb1 0.01143(6) 0.01203(6) 0.02073(8) -0.00044(5) 0.00643(5) -0.00030(5) Tb2 0.01008(6) 0.01357(6) 0.02241(8) 0.00036(5) 0.00743(5) 0.00013(5) B1 0.0204(16) 0.0143(15) 0.040(2) -0.0075(15) 0.0136(15) -0.0034(13) C101 0.0110(12) 0.0162(13) 0.0278(17) 0.0022(12) 0.0108(12) -0.0008(10) C102 0.0140(12) 0.0197(14) 0.0304(18) 0.0003(12) 0.0092(12) 0.0003(11) C103 0.0173(13) 0.0160(14) 0.044(2) 0.0015(13) 0.0158(14) 0.0022(11) C104 0.0119(12) 0.0238(16) 0.041(2) 0.0105(14) 0.0094(13) 0.0051(11) C105 0.0147(13) 0.0261(16) 0.0329(18) 0.0024(14) 0.0056(13) -0.0029(12) C106 0.0136(12) 0.0175(14) 0.0346(18) 0.0005(13) 0.0095(13) -0.0004(11) O111 0.0110(8) 0.0155(9) 0.0305(12) -0.0016(8) 0.0058(8) 0.0000(7) C112 0.0110(12) 0.0187(14) 0.0231(16) 0.0000(12) 0.0078(11) 0.0014(10) C113 0.0128(12) 0.0152(14) 0.0289(17) -0.0008(12) 0.0061(12) 0.0003(10) C114 0.0140(12) 0.0162(13) 0.0228(16) -0.0017(11) 0.0111(12) -0.0019(10) O115 0.0113(8) 0.0163(10) 0.0285(12) -0.0012(8) 0.0059(8) 0.0002(7) C121 0.0154(12) 0.0156(13) 0.0253(17) -0.0007(12) 0.0118(12) -0.0004(10) C122 0.0133(13) 0.0193(14) 0.0371(19) 0.0017(13) 0.0084(13) -0.0001(11) C123 0.0198(14) 0.0182(15) 0.054(2) 0.0054(14) 0.0173(15) 0.0031(12) C124 0.0265(15) 0.0117(14) 0.051(2) -0.0038(13) 0.0256(16) -0.0028(12) C125 0.0211(14) 0.0211(15) 0.0342(19) -0.0055(13) 0.0129(13) -0.0067(12) C126 0.0154(13) 0.0210(15) 0.0280(18) -0.0008(13) 0.0080(12) -0.0010(11) C131 0.0110(12) 0.0166(14) 0.0292(17) 0.0017(12) 0.0086(12) 0.0012(10) C132 0.0173(13) 0.0214(15) 0.0314(19) -0.0004(13) 0.0063(13) -0.0018(11) C133 0.0217(14) 0.0286(17) 0.0312(19) 0.0099(14) 0.0064(13) 0.0029(13) C134 0.0201(14) 0.0170(15) 0.051(2) 0.0066(14) 0.0141(15) 0.0030(12) C135 0.0214(14) 0.0172(15) 0.043(2) -0.0050(14) 0.0104(14) -0.0009(12) C136 0.0149(13) 0.0211(15) 0.0310(18) 0.0024(13) 0.0062(13) 0.0012(11) O141 0.0126(8) 0.0164(10) 0.0273(12) -0.0005(8) 0.0051(8) -0.0004(7) C142 0.0127(12) 0.0169(14) 0.0252(16) 0.0022(12) 0.0094(12) 0.0021(10) C143 0.0160(13) 0.0192(14) 0.0267(17) 0.0004(12) 0.0056(12) 0.0009(11) C144 0.0133(12) 0.0212(14) 0.0247(17) -0.0027(12) 0.0087(12) -0.0021(11) O145 0.0123(9) 0.0160(10) 0.0329(12) -0.0005(8) 0.0073(9) -0.0001(7) C151 0.0132(12) 0.0206(15) 0.0306(17) -0.0046(12) 0.0105(12) -0.0014(11) C152 0.0238(15) 0.0229(16) 0.0344(19) -0.0027(14) 0.0073(14) -0.0065(12) C153 0.0289(16) 0.0369(19) 0.034(2) -0.0080(16) 0.0045(15) -0.0089(15) C154 0.0208(15) 0.0269(17) 0.047(2) -0.0154(15) 0.0118(15) -0.0095(13) C155 0.0168(14) 0.0173(15) 0.054(2) -0.0058(14) 0.0153(15) -0.0024(12) C156 0.0122(12) 0.0218(15) 0.0360(19) -0.0033(13) 0.0080(13) -0.0010(11) N161 0.0091(10) 0.0191(12) 0.0268(14) -0.0009(10) 0.0072(10) -0.0006(9) C162 0.0090(11) 0.0222(15) 0.0223(16) 0.0000(12) 0.0044(11) -0.0043(10) C163 0.0165(13) 0.0255(15) 0.0299(18) 0.0028(13) 0.0109(13) -0.0022(12) C164 0.0161(13) 0.0361(18) 0.0300(18) -0.0055(14) 0.0124(13) -0.0022(12) C165 0.0147(13) 0.0251(16) 0.0325(18) -0.0065(13) 0.0104(13) 0.0003(11) C166 0.0139(12) 0.0198(14) 0.0267(17) 0.0005(12) 0.0068(12) 0.0023(11) N171 0.0130(10) 0.0125(11) 0.0289(15) -0.0008(10) 0.0075(10) -0.0026(9) N172 0.0098(10) 0.0149(11) 0.0291(14) -0.0003(10) 0.0072(10) -0.0019(9) C173 0.0119(12) 0.0213(14) 0.0231(16) 0.0013(12) 0.0057(12) -0.0046(11) C174 0.0239(14) 0.0256(16) 0.0247(17) 0.0034(13) 0.0098(13) -0.0036(12) C175 0.0195(14) 0.0165(14) 0.0333(19) 0.0028(13) 0.0072(13) -0.0012(11) N181 0.0216(12) 0.0105(11) 0.0324(15) -0.0027(10) 0.0138(11) 0.0001(9) N182 0.0146(11) 0.0135(11) 0.0301(14) -0.0015(10) 0.0098(10) -0.0007(9) C183 0.0183(13) 0.0180(14) 0.0295(17) -0.0037(12) 0.0141(13) -0.0003(11) C184 0.0247(15) 0.0201(15) 0.051(2) -0.0013(14) 0.0241(15) 0.0028(12) C185 0.0273(15) 0.0154(14) 0.050(2) -0.0005(14) 0.0229(15) 0.0080(12) N191 0.0149(11) 0.0172(12) 0.0299(15) -0.0007(10) 0.0105(10) 0.0005(9) C192 0.0153(12) 0.0191(14) 0.0247(17) -0.0031(12) 0.0082(12) -0.0020(11) C193 0.0175(13) 0.0242(15) 0.0379(19) -0.0007(13) 0.0158(13) -0.0004(12) C194 0.0211(14) 0.0267(16) 0.039(2) -0.0002(14) 0.0177(14) -0.0052(12) C195 0.0262(15) 0.0190(15) 0.038(2) 0.0028(13) 0.0156(14) -0.0035(12) C196 0.0223(14) 0.0183(14) 0.0328(18) 0.0021(13) 0.0150(13) 0.0002(11) B2 0.0213(16) 0.0175(16) 0.038(2) 0.0020(15) 0.0138(16) -0.0007(13) C201 0.0120(12) 0.0200(14) 0.0206(16) 0.0002(11) 0.0075(11) -0.0010(10) C202 0.0149(13) 0.0202(15) 0.0376(19) 0.0029(13) 0.0109(13) 0.0012(11) C203 0.0124(13) 0.0370(18) 0.042(2) 0.0046(15) 0.0080(14) -0.0003(13) C204 0.0179(14) 0.0365(19) 0.035(2) -0.0007(15) 0.0074(14) -0.0107(13) C205 0.0231(14) 0.0230(15) 0.0323(19) -0.0022(13) 0.0131(14) -0.0042(12) C206 0.0153(13) 0.0235(15) 0.0277(18) 0.0000(12) 0.0096(12) -0.0020(11) O211 0.0106(8) 0.0156(9) 0.0347(12) 0.0008(8) 0.0111(8) 0.0013(7) C212 0.0140(12) 0.0208(14) 0.0197(16) 0.0019(12) 0.0082(11) 0.0013(11) C213 0.0107(12) 0.0184(14) 0.0335(18) 0.0009(12) 0.0063(12) 0.0027(11) C214 0.0167(13) 0.0154(13) 0.0231(16) 0.0033(12) 0.0089(12) 0.0025(11) O215 0.0092(8) 0.0174(10) 0.0370(13) -0.0013(9) 0.0107(9) 0.0006(7) C221 0.0183(13) 0.0160(14) 0.0270(17) 0.0018(12) 0.0118(12) 0.0008(11) C222 0.0177(13) 0.0230(15) 0.042(2) -0.0017(14) 0.0146(14) 0.0004(12) C223 0.0253(15) 0.0232(16) 0.057(2) -0.0004(15) 0.0239(16) 0.0052(13) C224 0.0359(18) 0.0170(15) 0.058(2) -0.0065(15) 0.0249(18) 0.0004(13) C225 0.0237(15) 0.0187(16) 0.053(2) -0.0020(14) 0.0131(16) -0.0040(12) C226 0.0174(13) 0.0197(15) 0.040(2) 0.0003(13) 0.0086(13) 0.0016(12) C231 0.0170(13) 0.0164(14) 0.0212(16) -0.0034(12) 0.0073(12) -0.0032(11) C232 0.0197(14) 0.0227(15) 0.0365(19) 0.0008(13) 0.0159(14) -0.0016(12) C233 0.0302(16) 0.0275(17) 0.047(2) 0.0044(15) 0.0256(16) -0.0039(13) C234 0.0370(17) 0.0190(16) 0.044(2) 0.0038(14) 0.0202(16) -0.0044(13) C235 0.0257(15) 0.0187(15) 0.043(2) -0.0007(14) 0.0138(15) 0.0009(12) C236 0.0163(13) 0.0180(14) 0.0317(18) -0.0020(12) 0.0102(13) -0.0021(11) O241 0.0111(8) 0.0177(10) 0.0301(12) -0.0007(8) 0.0112(8) -0.0005(7) C242 0.0107(12) 0.0167(13) 0.0178(15) -0.0046(11) 0.0036(11) -0.0045(10) C243 0.0113(12) 0.0189(14) 0.0267(17) 0.0010(12) 0.0094(12) -0.0005(10) C244 0.0120(12) 0.0212(14) 0.0183(15) -0.0018(12) 0.0050(11) 0.0001(11) O245 0.0123(9) 0.0185(10) 0.0398(13) 0.0048(9) 0.0150(9) 0.0012(7) C251 0.0115(12) 0.0213(14) 0.0201(16) 0.0016(12) 0.0064(11) 0.0024(10) C252 0.0166(13) 0.0227(15) 0.042(2) 0.0048(14) 0.0146(14) 0.0022(12) C253 0.0186(14) 0.0307(17) 0.049(2) 0.0042(15) 0.0194(15) 0.0062(13) C254 0.0208(14) 0.0266(16) 0.040(2) 0.0047(14) 0.0155(14) 0.0103(12) C255 0.0247(15) 0.0195(15) 0.050(2) 0.0023(14) 0.0184(15) 0.0018(12) C256 0.0167(13) 0.0226(15) 0.040(2) 0.0027(14) 0.0144(13) 0.0019(12) N261 0.0104(10) 0.0207(12) 0.0283(15) 0.0001(10) 0.0081(10) -0.0024(9) C262 0.0092(11) 0.0241(15) 0.0280(17) 0.0017(12) 0.0109(11) -0.0007(11) C263 0.0180(13) 0.0258(16) 0.0285(18) 0.0062(13) 0.0096(13) -0.0008(12) C264 0.0171(13) 0.0325(17) 0.0276(18) -0.0018(14) 0.0103(13) -0.0046(12) C265 0.0164(13) 0.0238(15) 0.0344(19) -0.0035(13) 0.0120(13) -0.0043(12) C266 0.0175(13) 0.0201(15) 0.0325(19) 0.0011(13) 0.0097(13) -0.0015(11) N271 0.0157(11) 0.0139(12) 0.0407(16) 0.0032(11) 0.0149(11) -0.0001(9) N272 0.0110(10) 0.0136(11) 0.0348(15) 0.0008(10) 0.0129(10) -0.0005(9) C273 0.0121(12) 0.0241(15) 0.0284(18) 0.0047(13) 0.0113(12) 0.0009(11) C274 0.0202(14) 0.0290(17) 0.0319(19) 0.0095(14) 0.0107(13) 0.0038(12) C275 0.0209(14) 0.0177(15) 0.042(2) 0.0107(14) 0.0149(14) 0.0043(12) N281 0.0163(11) 0.0101(11) 0.0396(16) -0.0016(10) 0.0131(11) -0.0004(9) N282 0.0105(10) 0.0139(11) 0.0339(15) 0.0005(10) 0.0097(10) -0.0004(9) C283 0.0097(12) 0.0229(15) 0.0289(18) -0.0042(12) 0.0083(12) -0.0013(11) C284 0.0272(15) 0.0218(15) 0.038(2) -0.0088(14) 0.0193(15) -0.0047(12) C285 0.0222(14) 0.0166(15) 0.051(2) -0.0093(14) 0.0187(15) -0.0044(12) N291 0.0091(10) 0.0195(12) 0.0280(14) -0.0001(10) 0.0074(10) -0.0009(9) C292 0.0116(12) 0.0219(15) 0.0291(17) -0.0027(12) 0.0098(12) -0.0003(11) C293 0.0156(13) 0.0284(16) 0.0300(18) -0.0078(13) 0.0085(13) -0.0015(12) C294 0.0168(13) 0.0366(18) 0.0248(18) 0.0033(14) 0.0068(13) 0.0032(13) C295 0.0151(13) 0.0238(15) 0.0317(18) 0.0076(13) 0.0086(13) 0.0048(11) C296 0.0132(13) 0.0187(14) 0.0318(18) -0.0024(12) 0.0076(12) -0.0021(11) Cl1 0.0409(5) 0.0438(5) 0.0773(7) 0.0019(5) 0.0336(5) 0.0082(4) C300 0.025(3) 0.030(4) 0.067(5) 0.003(3) 0.024(3) 0.001(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 Tb1 O111 2.305(2) . ? Tb1 O145 2.317(2) . ? Tb1 O141 2.3224(18) . ? Tb1 O115 2.3316(18) . ? Tb1 N182 2.490(2) . ? Tb1 N172 2.558(2) . ? Tb1 N191 2.563(2) . ? Tb1 N161 2.617(2) . ? Tb2 O211 2.0876(17) . ? Tb2 O245 2.1155(17) . ? Tb2 O241 2.2832(17) . ? Tb2 O215 2.2920(17) . ? Tb2 N272 2.605(2) . ? Tb2 N282 2.607(2) . ? Tb2 N261 2.734(2) . ? Tb2 N291 2.792(2) . ? B1 N181 1.483(4) . ? B1 N171 1.649(4) . ? C101 C102 1.412(4) . ? C101 C106 1.454(4) . ? C101 C112 1.496(4) . ? C102 C103 1.375(4) . ? C103 C104 1.449(4) . ? C104 C105 1.399(4) . ? C105 C106 1.390(4) . ? O111 C112 1.253(3) . ? C112 C113 1.398(3) . ? C113 C114 1.387(4) . ? C114 O115 1.237(3) . ? C114 C121 1.495(3) . ? C121 C126 1.358(4) . ? C121 C122 1.373(4) . ? C122 C123 1.385(4) . ? C123 C124 1.345(4) . ? C124 C125 1.357(4) . ? C125 C126 1.390(4) . ? C131 C136 1.461(4) . ? C131 C132 1.491(4) . ? C131 C142 1.506(3) . ? C132 C133 1.390(4) . ? C133 C134 1.448(4) . ? C134 C135 1.478(4) . ? C135 C136 1.386(4) . ? O141 C142 1.304(3) . ? C142 C143 1.419(4) . ? C143 C144 1.397(4) . ? C144 O145 1.294(3) . ? C144 C151 1.501(4) . ? C151 C156 1.411(4) . ? C151 C152 1.471(4) . ? C152 C153 1.398(4) . ? C153 C154 1.398(4) . ? C154 C155 1.469(4) . ? C155 C156 1.389(4) . ? N161 C166 1.335(3) . ? N161 C162 1.407(3) . ? C162 C173 1.465(4) . ? C162 C163 1.482(4) . ? C163 C164 1.370(4) . ? C164 C165 1.435(4) . ? C165 C166 1.463(4) . ? N171 N172 1.337(3) . ? N171 C175 1.446(4) . ? N172 C173 1.449(3) . ? C173 C174 1.428(4) . ? C174 C175 1.408(4) . ? N181 C185 1.249(3) . ? N181 N182 1.364(3) . ? N182 C183 1.276(3) . ? C183 C184 1.338(4) . ? C183 C192 1.473(4) . ? C184 C185 1.366(4) . ? N191 C192 1.303(3) . ? N191 C196 1.357(3) . ? C192 C193 1.366(4) . ? C193 C194 1.385(4) . ? C194 C195 1.332(4) . ? C195 C196 1.363(4) . ? B2 N271 1.595(4) . ? B2 N281 1.665(4) . ? C201 C202 1.294(3) . ? C201 C206 1.394(4) . ? C201 C212 1.427(3) . ? C202 C203 1.326(4) . ? C203 C204 1.378(4) . ? C204 C205 1.279(4) . ? C205 C206 1.322(4) . ? O211 C212 1.191(3) . ? C212 C213 1.399(4) . ? C213 C214 1.339(4) . ? C214 O215 1.170(3) . ? C214 C221 1.512(4) . ? C221 C222 1.296(3) . ? C221 C226 1.332(4) . ? C222 C223 1.402(4) . ? C223 C224 1.323(4) . ? C224 C225 1.287(4) . ? C225 C226 1.400(4) . ? C231 C236 1.330(3) . ? C231 C232 1.345(3) . ? C231 C242 1.534(4) . ? C232 C233 1.414(4) . ? C233 C234 1.314(4) . ? C234 C235 1.325(4) . ? C235 C236 1.409(4) . ? O241 C242 1.220(3) . ? C242 C243 1.347(3) . ? C243 C244 1.413(4) . ? C244 O245 1.210(3) . ? C244 C251 1.447(3) . ? C251 C252 1.297(3) . ? C251 C256 1.380(4) . ? C252 C253 1.347(4) . ? C253 C254 1.364(4) . ? C254 C255 1.286(4) . ? C255 C256 1.340(4) . ? N261 C266 1.350(3) . ? N261 C262 1.413(3) . ? C262 C273 1.481(4) . ? C262 C263 1.502(4) . ? C263 C264 1.386(4) . ? C264 C265 1.437(4) . ? C265 C266 1.488(4) . ? N271 N272 1.366(3) . ? N271 C275 1.414(4) . ? N272 C273 1.427(4) . ? C273 C274 1.411(4) . ? C274 C275 1.418(4) . ? N281 N282 1.366(3) . ? N281 C285 1.439(4) . ? N282 C283 1.463(4) . ? C283 C284 1.421(4) . ? C283 C292 1.490(4) . ? C284 C285 1.450(4) . ? N291 C296 1.361(3) . ? N291 C292 1.409(3) . ? C292 C293 1.519(4) . ? C293 C294 1.400(4) . ? C294 C295 1.432(4) . ? C295 C296 1.508(4) . ? Cl1 C300 1.809(6) 3_566 ? Cl1 C300 1.959(7) . ? C300 Cl1 1.809(6) 3_566 ? 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 O111 Tb1 O145 145.70(6) . . ? O111 Tb1 O141 142.40(6) . . ? O145 Tb1 O141 71.90(6) . . ? O111 Tb1 O115 70.66(6) . . ? O145 Tb1 O115 143.59(6) . . ? O141 Tb1 O115 71.77(7) . . ? O111 Tb1 N182 80.26(7) . . ? O145 Tb1 N182 73.15(7) . . ? O141 Tb1 N182 126.71(7) . . ? O115 Tb1 N182 129.57(6) . . ? O111 Tb1 N172 65.61(6) . . ? O145 Tb1 N172 87.64(7) . . ? O141 Tb1 N172 137.97(6) . . ? O115 Tb1 N172 121.87(7) . . ? N182 Tb1 N172 78.00(7) . . ? O111 Tb1 N191 100.13(7) . . ? O145 Tb1 N191 87.93(7) . . ? O141 Tb1 N191 74.93(7) . . ? O115 Tb1 N191 80.54(7) . . ? N182 Tb1 N191 64.85(7) . . ? N172 Tb1 N191 142.23(7) . . ? O111 Tb1 N161 77.49(7) . . ? O145 Tb1 N161 110.14(7) . . ? O141 Tb1 N161 89.70(7) . . ? O115 Tb1 N161 71.94(6) . . ? N182 Tb1 N161 140.23(7) . . ? N172 Tb1 N161 62.88(7) . . ? N191 Tb1 N161 151.61(7) . . ? O211 Tb2 O245 144.44(7) . . ? O211 Tb2 O241 134.07(6) . . ? O245 Tb2 O241 74.88(6) . . ? O211 Tb2 O215 74.52(6) . . ? O245 Tb2 O215 140.60(6) . . ? O241 Tb2 O215 67.80(6) . . ? O211 Tb2 N272 88.33(7) . . ? O245 Tb2 N272 74.93(7) . . ? O241 Tb2 N272 134.79(7) . . ? O215 Tb2 N272 124.70(7) . . ? O211 Tb2 N282 72.32(7) . . ? O245 Tb2 N282 74.00(7) . . ? O241 Tb2 N282 121.83(7) . . ? O215 Tb2 N282 137.50(7) . . ? N272 Tb2 N282 80.12(7) . . ? O211 Tb2 N261 109.86(7) . . ? O245 Tb2 N261 89.54(8) . . ? O241 Tb2 N261 85.66(7) . . ? O215 Tb2 N261 75.78(7) . . ? N272 Tb2 N261 61.31(7) . . ? N282 Tb2 N261 140.98(7) . . ? O211 Tb2 N291 81.74(7) . . ? O245 Tb2 N291 91.74(7) . . ? O241 Tb2 N291 72.39(7) . . ? O215 Tb2 N291 88.81(7) . . ? N272 Tb2 N291 140.97(7) . . ? N282 Tb2 N291 60.89(7) . . ? N261 Tb2 N291 156.83(6) . . ? N181 B1 N171 110.6(2) . . ? C102 C101 C106 120.9(2) . . ? C102 C101 C112 114.8(2) . . ? C106 C101 C112 124.2(2) . . ? C103 C102 C101 117.5(3) . . ? C102 C103 C104 121.3(3) . . ? C105 C104 C103 122.0(3) . . ? C106 C105 C104 116.8(3) . . ? C105 C106 C101 121.4(3) . . ? C112 O111 Tb1 138.69(17) . . ? O111 C112 C113 123.7(2) . . ? O111 C112 C101 115.1(2) . . ? C113 C112 C101 121.2(2) . . ? C114 C113 C112 124.0(2) . . ? O115 C114 C113 122.4(2) . . ? O115 C114 C121 115.2(2) . . ? C113 C114 C121 122.4(2) . . ? C114 O115 Tb1 139.18(17) . . ? C126 C121 C122 117.3(3) . . ? C126 C121 C114 123.5(2) . . ? C122 C121 C114 119.2(2) . . ? C121 C122 C123 121.6(3) . . ? C124 C123 C122 120.4(3) . . ? C123 C124 C125 118.7(3) . . ? C124 C125 C126 121.2(3) . . ? C121 C126 C125 120.7(3) . . ? C136 C131 C132 122.4(2) . . ? C136 C131 C142 115.3(2) . . ? C132 C131 C142 122.3(2) . . ? C133 C132 C131 119.5(3) . . ? C132 C133 C134 117.3(3) . . ? C133 C134 C135 123.9(3) . . ? C136 C135 C134 118.9(3) . . ? C135 C136 C131 118.0(3) . . ? C142 O141 Tb1 136.42(16) . . ? O141 C142 C143 125.2(2) . . ? O141 C142 C131 116.2(2) . . ? C143 C142 C131 118.7(2) . . ? C144 C143 C142 122.3(3) . . ? O145 C144 C143 123.8(2) . . ? O145 C144 C151 116.7(2) . . ? C143 C144 C151 119.5(2) . . ? C144 O145 Tb1 139.13(17) . . ? C156 C151 C152 120.9(3) . . ? C156 C151 C144 115.2(3) . . ? C152 C151 C144 123.9(2) . . ? C153 C152 C151 122.1(3) . . ? C152 C153 C154 116.3(3) . . ? C153 C154 C155 122.2(3) . . ? C156 C155 C154 121.4(3) . . ? C155 C156 C151 117.1(3) . . ? C166 N161 C162 114.8(2) . . ? C166 N161 Tb1 121.35(18) . . ? C162 N161 Tb1 122.78(16) . . ? N161 C162 C173 112.3(2) . . ? N161 C162 C163 125.4(2) . . ? C173 C162 C163 122.2(2) . . ? C164 C163 C162 118.3(3) . . ? C163 C164 C165 116.5(3) . . ? C164 C165 C166 122.2(3) . . ? N161 C166 C165 122.7(3) . . ? N172 N171 C175 108.0(2) . . ? N172 N171 B1 119.6(2) . . ? C175 N171 B1 132.2(2) . . ? N171 N172 C173 104.8(2) . . ? N171 N172 Tb1 129.86(16) . . ? C173 N172 Tb1 119.13(16) . . ? C174 C173 N172 114.7(2) . . ? C174 C173 C162 126.5(3) . . ? N172 C173 C162 118.7(2) . . ? C175 C174 C173 98.9(2) . . ? C174 C175 N171 113.5(2) . . ? C185 N181 N182 109.1(2) . . ? C185 N181 B1 124.5(2) . . ? N182 N181 B1 126.1(2) . . ? C183 N182 N181 109.4(2) . . ? C183 N182 Tb1 114.82(17) . . ? N181 N182 Tb1 125.88(16) . . ? N182 C183 C184 106.1(2) . . ? N182 C183 C192 120.5(2) . . ? C184 C183 C192 133.4(2) . . ? C183 C184 C185 108.6(2) . . ? N181 C185 C184 106.7(3) . . ? C192 N191 C196 118.4(2) . . ? C192 N191 Tb1 116.21(18) . . ? C196 N191 Tb1 124.90(17) . . ? N191 C192 C193 120.0(3) . . ? N191 C192 C183 116.0(2) . . ? C193 C192 C183 124.1(2) . . ? C192 C193 C194 120.8(3) . . ? C195 C194 C193 119.9(3) . . ? C194 C195 C196 116.5(3) . . ? N191 C196 C195 124.5(3) . . ? N271 B2 N281 118.4(2) . . ? C202 C201 C206 119.0(3) . . ? C202 C201 C212 118.8(3) . . ? C206 C201 C212 122.2(2) . . ? C201 C202 C203 116.3(3) . . ? C202 C203 C204 124.0(3) . . ? C205 C204 C203 120.3(3) . . ? C204 C205 C206 116.2(3) . . ? C205 C206 C201 124.2(3) . . ? C212 O211 Tb2 136.51(18) . . ? O211 C212 C213 124.3(2) . . ? O211 C212 C201 110.8(2) . . ? C213 C212 C201 124.8(2) . . ? C214 C213 C212 126.4(2) . . ? O215 C214 C213 118.8(3) . . ? O215 C214 C221 116.2(2) . . ? C213 C214 C221 124.9(2) . . ? C214 O215 Tb2 137.25(18) . . ? C222 C221 C226 112.8(3) . . ? C222 C221 C214 124.4(3) . . ? C226 C221 C214 122.7(2) . . ? C221 C222 C223 121.8(3) . . ? C224 C223 C222 124.7(3) . . ? C225 C224 C223 114.0(3) . . ? C224 C225 C226 121.3(3) . . ? C221 C226 C225 125.3(3) . . ? C236 C231 C232 113.1(3) . . ? C236 C231 C242 121.2(2) . . ? C232 C231 C242 125.7(2) . . ? C231 C232 C233 122.9(3) . . ? C234 C233 C232 122.9(3) . . ? C233 C234 C235 114.9(3) . . ? C234 C235 C236 122.5(3) . . ? C231 C236 C235 123.7(3) . . ? C242 O241 Tb2 132.33(17) . . ? O241 C242 C243 119.8(2) . . ? O241 C242 C231 117.3(2) . . ? C243 C242 C231 122.8(2) . . ? C242 C243 C244 125.5(2) . . ? O245 C244 C243 125.1(2) . . ? O245 C244 C251 111.0(2) . . ? C243 C244 C251 123.7(2) . . ? C244 O245 Tb2 133.84(18) . . ? C252 C251 C256 117.9(3) . . ? C252 C251 C244 120.5(3) . . ? C256 C251 C244 121.5(2) . . ? C251 C252 C253 117.1(3) . . ? C252 C253 C254 124.4(3) . . ? C255 C254 C253 118.9(3) . . ? C254 C255 C256 117.1(3) . . ? C255 C256 C251 124.6(3) . . ? C266 N261 C262 113.5(2) . . ? C266 N261 Tb2 123.39(18) . . ? C262 N261 Tb2 123.10(17) . . ? N261 C262 C273 111.6(2) . . ? N261 C262 C263 125.3(2) . . ? C273 C262 C263 123.2(2) . . ? C264 C263 C262 120.0(3) . . ? C263 C264 C265 115.0(3) . . ? C264 C265 C266 122.3(3) . . ? N261 C266 C265 123.9(3) . . ? N272 N271 C275 106.7(2) . . ? N272 N271 B2 123.5(2) . . ? C275 N271 B2 129.2(2) . . ? N271 N272 C273 106.7(2) . . ? N271 N272 Tb2 128.27(18) . . ? C273 N272 Tb2 121.78(16) . . ? C274 C273 N272 112.7(2) . . ? C274 C273 C262 127.3(3) . . ? N272 C273 C262 120.1(2) . . ? C273 C274 C275 100.9(3) . . ? N271 C275 C274 113.1(2) . . ? N282 N281 C285 104.6(2) . . ? N282 N281 B2 122.9(2) . . ? C285 N281 B2 130.4(2) . . ? N281 N282 C283 108.1(2) . . ? N281 N282 Tb2 127.99(18) . . ? C283 N282 Tb2 122.77(16) . . ? C284 C283 N282 112.9(2) . . ? C284 C283 C292 126.3(3) . . ? N282 C283 C292 120.8(2) . . ? C283 C284 C285 99.1(3) . . ? N281 C285 C284 115.2(2) . . ? C296 N291 C292 113.1(2) . . ? C296 N291 Tb2 122.81(18) . . ? C292 N291 Tb2 124.08(17) . . ? N291 C292 C283 110.6(2) . . ? N291 C292 C293 125.1(2) . . ? C283 C292 C293 124.4(2) . . ? C294 C293 C292 120.7(3) . . ? C293 C294 C295 114.5(3) . . ? C294 C295 C296 122.1(3) . . ? N291 C296 C295 124.5(3) . . ? C300 Cl1 C300 67.9(3) 3_566 . ? Cl1 C300 Cl1 112.1(3) 3_566 . ? _diffrn_measured_fraction_theta_max 0.939 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.939 _refine_diff_density_max 1.313 _refine_diff_density_min -0.447 _refine_diff_density_rms 0.084 #=END