Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global # *** Added by check_cif _publ_contact_author ; Prof. Mike Ward School of Chemistry Cantock's Close BRISTOL BS8 1TS ; _publ_contact_author_fax '0117 9287655' _publ_contact_author_email mike.ward@bristol.ac.uk _publ_contact_letter ; This CIF file contains details of the three crystal structures in the paper Synthesis and near-IR luminescence properties...' by A. Beeby et al, submitted to Dalton Transactions for publication. ; #======================================================== data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Faulkner, Stephen' 'Beeby, A.' 'Burton-Pye, Benjamin P.' 'Jeffery, J.' 'McCleverty, J. A.' 'Motson, Graham R.' 'Ward, Mike' _publ_contact_author_name 'Dr Stephen Faulkner' _publ_contact_author_address ; Department of Chemistry University of Manchester Oxford Road Manchester M13 9PL UNITED KINGDOM ; _publ_contact_author_email 'STEPHEN.FAULKNER@MAN.AC.UK' _publ_section_title ; Synthesis and near-IR luminescence properties of neodymium(III) and ytterbium(III) complexes with poly(pyrazolyl)borate ligands ; data_squeeze _database_code_CSD 177766 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H29 B N11 Nd O7' _chemical_formula_weight 786.67 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 10.4274(11) _cell_length_b 13.4278(14) _cell_length_c 14.5271(15) _cell_angle_alpha 113.062(2) _cell_angle_beta 95.236(2) _cell_angle_gamma 105.849(2) _cell_volume 1754.6(3) _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 'Pale purple' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.489 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 790 _exptl_absorpt_coefficient_mu 1.538 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6555 _exptl_absorpt_correction_T_max 0.7485 _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 15113 _diffrn_reflns_av_R_equivalents 0.0438 _diffrn_reflns_av_sigmaI/netI 0.0427 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6170 _reflns_number_gt 5386 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995b)' _computing_cell_refinement 'SAINT (Siemens, 1995b)' _computing_data_reduction 'SAINT (Siemens, 1995b)' _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^)+(0.1133P)^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 6170 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0618 _refine_ls_R_factor_gt 0.0543 _refine_ls_wR_factor_ref 0.1456 _refine_ls_wR_factor_gt 0.1404 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.78946(3) 0.85212(2) 0.66718(2) 0.02452(14) Uani 1 1 d . . . B1 B 0.5143(6) 0.8266(6) 0.8180(5) 0.0287(13) Uani 1 1 d . . . H1 H 0.4415 0.8188 0.8575 0.034 Uiso 1 1 calc R . . N1 N 1.0233(5) 0.7801(4) 0.7158(4) 0.0324(11) Uani 1 1 d . . . O2 O 1.1117(4) 0.7396(4) 0.7299(3) 0.0405(10) Uani 1 1 d . . . O3 O 1.0229(4) 0.8229(3) 0.6514(3) 0.0320(9) Uani 1 1 d . . . O4 O 0.9274(4) 0.7792(3) 0.7635(3) 0.0318(9) Uani 1 1 d . . . N5 N 0.7238(5) 0.8033(4) 0.4451(4) 0.0335(11) Uani 1 1 d . . . O6 O 0.8462(4) 0.8354(3) 0.4946(3) 0.0332(9) Uani 1 1 d . . . O7 O 0.6295(4) 0.7803(3) 0.4912(3) 0.0345(9) Uani 1 1 d . . . O8 O 0.6965(6) 0.7940(5) 0.3581(4) 0.0578(14) Uani 1 1 d . . . N11 N 0.5813(5) 0.9165(4) 0.6998(4) 0.0270(10) Uani 1 1 d . . . N12 N 0.4824(4) 0.8835(4) 0.7475(4) 0.0285(10) Uani 1 1 d . . . C13 C 0.3903(6) 0.9372(5) 0.7469(4) 0.0344(13) Uani 1 1 d . . . H13A H 0.3117 0.9285 0.7753 0.041 Uiso 1 1 calc R . . C14 C 0.4289(6) 1.0064(5) 0.6984(5) 0.0355(13) Uani 1 1 d . . . H14A H 0.3833 1.0535 0.6853 0.043 Uiso 1 1 calc R . . C15 C 0.5507(5) 0.9919(5) 0.6728(4) 0.0277(12) Uani 1 1 d . . . N21 N 0.7670(5) 1.0287(4) 0.6259(4) 0.0286(10) Uani 1 1 d . . . C22 C 0.6489(6) 1.0517(5) 0.6282(4) 0.0302(12) Uani 1 1 d . . . C23 C 0.6216(7) 1.1274(6) 0.5933(5) 0.0394(14) Uani 1 1 d . . . H23A H 0.5377 1.1422 0.5965 0.047 Uiso 1 1 calc R . . C24 C 0.7185(8) 1.1811(6) 0.5536(6) 0.0511(18) Uani 1 1 d . . . H24A H 0.7018 1.2331 0.5286 0.061 Uiso 1 1 calc R . . C25 C 0.8403(7) 1.1584(6) 0.5506(6) 0.0435(15) Uani 1 1 d . . . H25A H 0.9084 1.1938 0.5233 0.052 Uiso 1 1 calc R . . C26 C 0.8599(6) 1.0836(5) 0.5880(5) 0.0346(13) Uani 1 1 d . . . H26A H 0.9443 1.0694 0.5872 0.042 Uiso 1 1 calc R . . N31 N 0.6096(5) 0.6981(4) 0.6877(4) 0.0281(10) Uani 1 1 d . . . N32 N 0.5251(5) 0.7092(4) 0.7548(4) 0.0296(10) Uani 1 1 d . . . C33 C 0.4668(6) 0.6090(5) 0.7568(5) 0.0361(13) Uani 1 1 d . . . H33A H 0.4064 0.5963 0.7994 0.043 Uiso 1 1 calc R . . C34 C 0.5084(6) 0.5259(5) 0.6868(5) 0.0392(14) Uani 1 1 d . . . H34A H 0.4815 0.4462 0.6701 0.047 Uiso 1 1 calc R . . C35 C 0.5987(6) 0.5864(5) 0.6464(4) 0.0303(12) Uani 1 1 d . . . N41 N 0.7638(4) 0.6301(4) 0.5524(3) 0.0279(10) Uani 1 1 d . . . C42 C 0.6777(6) 0.5471(5) 0.5699(4) 0.0287(12) Uani 1 1 d . . . C43 C 0.6639(6) 0.4307(5) 0.5167(5) 0.0328(13) Uani 1 1 d . . . H43A H 0.6010 0.3740 0.5294 0.039 Uiso 1 1 calc R . . C44 C 0.7412(6) 0.3993(5) 0.4470(5) 0.0388(14) Uani 1 1 d . . . H44A H 0.7334 0.3209 0.4115 0.047 Uiso 1 1 calc R . . C45 C 0.8313(6) 0.4827(5) 0.4282(5) 0.0364(13) Uani 1 1 d . . . H45A H 0.8862 0.4627 0.3798 0.044 Uiso 1 1 calc R . . C46 C 0.8391(6) 0.5969(5) 0.4824(5) 0.0319(12) Uani 1 1 d . . . H46A H 0.9003 0.6542 0.4694 0.038 Uiso 1 1 calc R . . N51 N 0.7656(5) 0.9343(4) 0.8540(4) 0.0293(10) Uani 1 1 d . . . N52 N 0.6532(5) 0.9093(4) 0.8922(4) 0.0309(10) Uani 1 1 d . . . C53 C 0.6788(6) 0.9860(6) 0.9923(5) 0.0376(14) Uani 1 1 d . . . H53A H 0.6167 0.9865 1.0363 0.045 Uiso 1 1 calc R . . C54 C 0.8087(6) 1.0622(5) 1.0191(4) 0.0372(14) Uani 1 1 d . . . H54A H 0.8546 1.1251 1.0839 0.045 Uiso 1 1 calc R . . C55 C 0.8588(6) 1.0272(5) 0.9305(4) 0.0309(12) Uani 1 1 d . . . N61 N 0.9967(5) 1.0368(4) 0.8088(4) 0.0308(10) Uani 1 1 d . . . C62 C 0.9901(6) 1.0800(5) 0.9088(4) 0.0302(12) Uani 1 1 d . . . C63 C 1.0966(6) 1.1700(5) 0.9867(5) 0.0398(14) Uani 1 1 d . . . H63A H 1.0880 1.1992 1.0560 0.048 Uiso 1 1 calc R . . C64 C 1.2141(7) 1.2151(6) 0.9604(5) 0.0460(16) Uani 1 1 d . . . H64A H 1.2891 1.2756 1.0120 0.055 Uiso 1 1 calc R . . C65 C 1.2240(7) 1.1730(6) 0.8592(6) 0.0435(16) Uani 1 1 d . . . H65A H 1.3045 1.2044 0.8400 0.052 Uiso 1 1 calc R . . C66 C 1.1149(6) 1.0848(5) 0.7873(5) 0.0364(13) Uani 1 1 d . . . H66A H 1.1226 1.0554 0.7177 0.044 Uiso 1 1 calc R . . C100 C 0.136(3) 0.3880(14) 0.7969(15) 0.199(11) Uani 1 1 d . . . H10A H 0.0727 0.3152 0.7425 0.298 Uiso 1 1 calc R . . H10B H 0.1743 0.3743 0.8530 0.298 Uiso 1 1 calc R . . H10C H 0.2096 0.4207 0.7692 0.298 Uiso 1 1 calc R . . C101 C 0.054(4) 0.476(3) 0.839(3) 0.31(2) Uani 1 1 d . . . H10I H -0.0095 0.4572 0.8812 0.367 Uiso 1 1 calc R . . H10J H 0.0109 0.4938 0.7869 0.367 Uiso 1 1 calc R . . O100 O 0.212(5) 0.572(3) 0.908(4) 0.57(4) Uani 1 1 d . . . C102 C 0.223(6) 0.702(3) 0.999(4) 0.46(4) Uani 1 1 d . . . H10G H 0.2279 0.7565 0.9680 0.553 Uiso 1 1 calc R . . H10H H 0.1418 0.6954 1.0291 0.553 Uiso 1 1 calc R . . C103 C 0.341(3) 0.741(3) 1.0740(18) 0.29(2) Uani 1 1 d . . . H10D H 0.3501 0.8161 1.1280 0.436 Uiso 1 1 calc R . . H10E H 0.4212 0.7477 1.0433 0.436 Uiso 1 1 calc R . . H10F H 0.3356 0.6861 1.1038 0.436 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 0.02482(19) 0.02261(19) 0.02305(19) 0.00374(13) 0.01035(12) 0.01108(13) B1 0.027(3) 0.032(3) 0.027(3) 0.010(3) 0.013(3) 0.011(3) N1 0.032(3) 0.025(2) 0.029(3) -0.001(2) 0.007(2) 0.012(2) O2 0.034(2) 0.043(2) 0.043(3) 0.009(2) 0.0119(19) 0.025(2) O3 0.032(2) 0.032(2) 0.030(2) 0.0089(18) 0.0125(17) 0.0132(17) O4 0.032(2) 0.032(2) 0.029(2) 0.0069(17) 0.0142(17) 0.0136(17) N5 0.042(3) 0.034(3) 0.028(3) 0.009(2) 0.014(2) 0.023(2) O6 0.038(2) 0.032(2) 0.031(2) 0.0085(18) 0.0176(18) 0.0167(18) O7 0.031(2) 0.033(2) 0.037(2) 0.0116(19) 0.0093(18) 0.0123(18) O8 0.081(4) 0.078(4) 0.030(3) 0.025(3) 0.020(2) 0.045(3) N11 0.028(2) 0.031(2) 0.025(2) 0.010(2) 0.0141(19) 0.015(2) N12 0.025(2) 0.028(2) 0.029(3) 0.006(2) 0.0131(19) 0.0112(19) C13 0.026(3) 0.042(3) 0.030(3) 0.006(3) 0.010(2) 0.016(3) C14 0.036(3) 0.044(3) 0.035(3) 0.016(3) 0.015(3) 0.025(3) C15 0.026(3) 0.028(3) 0.024(3) 0.005(2) 0.007(2) 0.010(2) N21 0.029(2) 0.026(2) 0.028(2) 0.006(2) 0.0118(19) 0.013(2) C22 0.034(3) 0.029(3) 0.026(3) 0.007(2) 0.011(2) 0.014(2) C23 0.042(3) 0.043(4) 0.049(4) 0.024(3) 0.023(3) 0.028(3) C24 0.062(4) 0.049(4) 0.065(5) 0.036(4) 0.027(4) 0.031(4) C25 0.044(4) 0.041(4) 0.054(4) 0.024(3) 0.026(3) 0.017(3) C26 0.035(3) 0.030(3) 0.042(3) 0.014(3) 0.018(3) 0.014(3) N31 0.030(2) 0.025(2) 0.026(2) 0.005(2) 0.0109(19) 0.012(2) N32 0.029(2) 0.031(3) 0.026(2) 0.009(2) 0.0136(19) 0.009(2) C33 0.037(3) 0.037(3) 0.038(3) 0.018(3) 0.017(3) 0.012(3) C34 0.039(3) 0.032(3) 0.046(4) 0.018(3) 0.011(3) 0.007(3) C35 0.032(3) 0.026(3) 0.028(3) 0.006(2) 0.006(2) 0.012(2) N41 0.027(2) 0.027(2) 0.026(2) 0.005(2) 0.0074(19) 0.011(2) C42 0.030(3) 0.026(3) 0.027(3) 0.006(2) 0.008(2) 0.014(2) C43 0.038(3) 0.023(3) 0.035(3) 0.010(2) 0.006(3) 0.011(2) C44 0.048(4) 0.026(3) 0.041(4) 0.008(3) 0.010(3) 0.021(3) C45 0.041(3) 0.027(3) 0.036(3) 0.003(3) 0.014(3) 0.016(3) C46 0.037(3) 0.027(3) 0.032(3) 0.008(2) 0.016(2) 0.015(2) N51 0.027(2) 0.031(2) 0.023(2) 0.003(2) 0.0096(19) 0.011(2) N52 0.029(2) 0.032(3) 0.027(3) 0.005(2) 0.0124(19) 0.013(2) C53 0.041(3) 0.047(4) 0.023(3) 0.008(3) 0.016(2) 0.021(3) C54 0.037(3) 0.042(3) 0.021(3) 0.001(3) 0.006(2) 0.014(3) C55 0.029(3) 0.033(3) 0.028(3) 0.007(2) 0.008(2) 0.015(2) N61 0.033(2) 0.026(2) 0.028(3) 0.004(2) 0.011(2) 0.013(2) C62 0.033(3) 0.029(3) 0.029(3) 0.010(2) 0.010(2) 0.015(2) C63 0.039(3) 0.036(3) 0.029(3) 0.002(3) 0.004(3) 0.009(3) C64 0.040(3) 0.035(3) 0.045(4) 0.008(3) 0.006(3) 0.001(3) C65 0.036(3) 0.037(3) 0.046(4) 0.008(3) 0.017(3) 0.009(3) C66 0.031(3) 0.034(3) 0.034(3) 0.006(3) 0.010(3) 0.009(3) C100 0.30(3) 0.096(12) 0.137(15) -0.004(10) -0.042(16) 0.085(16) C101 0.32(5) 0.16(3) 0.34(5) 0.09(3) -0.06(4) 0.03(3) O100 0.93(8) 0.52(5) 0.97(9) 0.63(6) 0.86(8) 0.64(6) C102 0.76(11) 0.32(5) 0.62(9) 0.33(6) 0.33(8) 0.42(7) C103 0.160(19) 0.34(4) 0.139(18) -0.07(2) -0.087(16) 0.04(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 Nd1 N31 2.520(5) . ? Nd1 O4 2.541(4) . ? Nd1 N11 2.563(4) . ? Nd1 N51 2.564(5) . ? Nd1 O6 2.567(4) . ? Nd1 O7 2.581(4) . ? Nd1 O3 2.586(4) . ? Nd1 N61 2.705(5) . ? Nd1 N41 2.707(4) . ? Nd1 N21 2.726(5) . ? B1 N32 1.524(8) . ? B1 N52 1.547(8) . ? B1 N12 1.560(8) . ? N1 O2 1.230(6) . ? N1 O4 1.267(6) . ? N1 O3 1.275(6) . ? N5 O8 1.218(6) . ? N5 O6 1.273(6) . ? N5 O7 1.276(6) . ? N11 C15 1.322(7) . ? N11 N12 1.364(6) . ? N12 C13 1.351(7) . ? C13 C14 1.371(9) . ? C14 C15 1.398(8) . ? C15 C22 1.481(8) . ? N21 C26 1.345(7) . ? N21 C22 1.349(7) . ? C22 C23 1.381(8) . ? C23 C24 1.382(10) . ? C24 C25 1.386(10) . ? C25 C26 1.366(9) . ? N31 C35 1.346(7) . ? N31 N32 1.365(6) . ? N32 C33 1.330(8) . ? C33 C34 1.387(9) . ? C34 C35 1.396(9) . ? C35 C42 1.461(8) . ? N41 C42 1.353(7) . ? N41 C46 1.353(7) . ? C42 C43 1.404(8) . ? C43 C44 1.361(9) . ? C44 C45 1.387(9) . ? C45 C46 1.398(8) . ? N51 C55 1.338(7) . ? N51 N52 1.358(6) . ? N52 C53 1.361(8) . ? C53 C54 1.366(9) . ? C54 C55 1.391(8) . ? C55 C62 1.484(8) . ? N61 C66 1.352(8) . ? N61 C62 1.353(7) . ? C62 C63 1.393(9) . ? C63 C64 1.370(9) . ? C64 C65 1.378(10) . ? C65 C66 1.366(9) . ? C100 C101 1.60(4) . ? C101 O100 1.70(6) . ? O100 C102 1.69(6) . ? C102 C103 1.39(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 N31 Nd1 O4 76.43(13) . . ? N31 Nd1 N11 71.36(14) . . ? O4 Nd1 N11 131.32(13) . . ? N31 Nd1 N51 72.34(15) . . ? O4 Nd1 N51 72.39(13) . . ? N11 Nd1 N51 63.67(14) . . ? N31 Nd1 O6 124.08(14) . . ? O4 Nd1 O6 115.16(12) . . ? N11 Nd1 O6 113.01(14) . . ? N51 Nd1 O6 162.46(15) . . ? N31 Nd1 O7 84.93(14) . . ? O4 Nd1 O7 139.70(13) . . ? N11 Nd1 O7 72.33(14) . . ? N51 Nd1 O7 134.84(14) . . ? O6 Nd1 O7 49.80(13) . . ? N31 Nd1 O3 116.35(13) . . ? O4 Nd1 O3 50.07(13) . . ? N11 Nd1 O3 170.53(13) . . ? N51 Nd1 O3 112.27(14) . . ? O6 Nd1 O3 68.05(13) . . ? O7 Nd1 O3 112.75(13) . . ? N31 Nd1 N61 130.27(15) . . ? O4 Nd1 N61 72.67(13) . . ? N11 Nd1 N61 102.11(14) . . ? N51 Nd1 N61 61.71(15) . . ? O6 Nd1 N61 104.21(14) . . ? O7 Nd1 N61 141.72(13) . . ? O3 Nd1 N61 68.84(13) . . ? N31 Nd1 N41 61.91(14) . . ? O4 Nd1 N41 68.26(13) . . ? N11 Nd1 N41 122.12(14) . . ? N51 Nd1 N41 124.69(15) . . ? O6 Nd1 N41 72.31(13) . . ? O7 Nd1 N41 71.45(13) . . ? O3 Nd1 N41 67.34(13) . . ? N61 Nd1 N41 133.71(13) . . ? N31 Nd1 N21 130.07(14) . . ? O4 Nd1 N21 148.58(13) . . ? N11 Nd1 N21 61.01(14) . . ? N51 Nd1 N21 97.74(14) . . ? O6 Nd1 N21 67.39(13) . . ? O7 Nd1 N21 67.80(13) . . ? O3 Nd1 N21 112.66(13) . . ? N61 Nd1 N21 76.40(14) . . ? N41 Nd1 N21 135.10(14) . . ? N32 B1 N52 110.1(5) . . ? N32 B1 N12 110.8(5) . . ? N52 B1 N12 105.6(4) . . ? O2 N1 O4 121.3(5) . . ? O2 N1 O3 121.5(5) . . ? O4 N1 O3 117.2(4) . . ? N1 O3 Nd1 95.0(3) . . ? N1 O4 Nd1 97.4(3) . . ? O8 N5 O6 122.6(5) . . ? O8 N5 O7 121.0(5) . . ? O6 N5 O7 116.5(5) . . ? N5 O6 Nd1 96.9(3) . . ? N5 O7 Nd1 96.2(3) . . ? C15 N11 N12 106.2(4) . . ? C15 N11 Nd1 124.9(4) . . ? N12 N11 Nd1 128.9(3) . . ? C13 N12 N11 109.5(5) . . ? C13 N12 B1 129.7(5) . . ? N11 N12 B1 117.7(4) . . ? N12 C13 C14 108.7(5) . . ? C13 C14 C15 104.1(5) . . ? N11 C15 C14 111.4(5) . . ? N11 C15 C22 118.2(5) . . ? C14 C15 C22 130.3(5) . . ? C26 N21 C22 117.1(5) . . ? C26 N21 Nd1 123.0(4) . . ? C22 N21 Nd1 119.1(4) . . ? N21 C22 C23 122.6(5) . . ? N21 C22 C15 115.5(5) . . ? C23 C22 C15 121.8(5) . . ? C22 C23 C24 118.7(6) . . ? C23 C24 C25 119.3(6) . . ? C26 C25 C24 118.2(6) . . ? N21 C26 C25 124.0(6) . . ? C35 N31 N32 105.7(4) . . ? C35 N31 Nd1 123.9(4) . . ? N32 N31 Nd1 129.2(3) . . ? C33 N32 N31 110.4(5) . . ? C33 N32 B1 129.5(5) . . ? N31 N32 B1 120.1(4) . . ? N32 C33 C34 109.0(5) . . ? C33 C34 C35 104.0(5) . . ? N31 C35 C34 110.9(5) . . ? N31 C35 C42 118.6(5) . . ? C34 C35 C42 130.5(5) . . ? C42 N41 C46 117.2(5) . . ? C42 N41 Nd1 118.8(3) . . ? C46 N41 Nd1 123.8(4) . . ? N41 C42 C43 122.0(5) . . ? N41 C42 C35 115.6(5) . . ? C43 C42 C35 122.4(5) . . ? C44 C43 C42 119.7(6) . . ? C43 C44 C45 119.5(5) . . ? C44 C45 C46 118.1(6) . . ? N41 C46 C45 123.4(6) . . ? C55 N51 N52 106.2(4) . . ? C55 N51 Nd1 124.1(4) . . ? N52 N51 Nd1 128.7(3) . . ? N51 N52 C53 109.3(5) . . ? N51 N52 B1 119.7(4) . . ? C53 N52 B1 129.0(5) . . ? N52 C53 C54 108.7(5) . . ? C53 C54 C55 104.7(5) . . ? N51 C55 C54 111.0(5) . . ? N51 C55 C62 118.4(5) . . ? C54 C55 C62 130.4(6) . . ? C66 N61 C62 116.2(5) . . ? C66 N61 Nd1 123.5(4) . . ? C62 N61 Nd1 120.0(4) . . ? N61 C62 C63 123.2(5) . . ? N61 C62 C55 115.3(5) . . ? C63 C62 C55 121.5(5) . . ? C64 C63 C62 118.0(6) . . ? C63 C64 C65 120.2(6) . . ? C66 C65 C64 118.2(6) . . ? N61 C66 C65 124.1(6) . . ? C100 C101 O100 84(2) . . ? C102 O100 C101 118(3) . . ? C103 C102 O100 108(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 3.513 _refine_diff_density_min -2.506 _refine_diff_density_rms 0.169 #=END data_sad _database_code_CSD 177767 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C75.61 H66.43 B3 N18 Nd O' _chemical_formula_weight 1419.86 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' 'Nd' 'Nd' -0.1943 3.0179 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 12.0803(14) _cell_length_b 24.827(3) _cell_length_c 22.673(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.707(2) _cell_angle_gamma 90.00 _cell_volume 6738.5(13) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 364 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.400 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2916 _exptl_absorpt_coefficient_mu 0.832 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7320 _exptl_absorpt_correction_T_max 0.8513 _exptl_absorpt_process_details ? _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 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_% none _diffrn_reflns_number 43400 _diffrn_reflns_av_R_equivalents 0.0437 _diffrn_reflns_av_sigmaI/netI 0.0601 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 27.51 _reflns_number_total 15407 _reflns_number_gt 7940 _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^)+(0.0416P)^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 15407 _refine_ls_number_parameters 918 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0933 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0919 _refine_ls_wR_factor_gt 0.0753 _refine_ls_goodness_of_fit_ref 0.955 _refine_ls_restrained_S_all 0.956 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.0000 0.5000 1.0000 0.02333(6) Uani 1 2 d S . . B1 B 0.1205(3) 0.46679(15) 1.16376(17) 0.0323(9) Uani 1 1 d . . . H1 H 0.1510 0.4584 1.2060 0.039 Uiso 1 1 calc R . . Nd2 Nd 0.0000 0.5000 0.5000 0.02496(6) Uani 1 2 d S . . B2 B 0.0405(3) 0.41725(14) 0.64710(16) 0.0281(8) Uani 1 1 d . . . H2 H 0.0508 0.3958 0.6848 0.034 Uiso 1 1 calc R . . N11 N 0.2120(2) 0.45755(10) 1.12361(11) 0.0287(6) Uani 1 1 d . . . N12 N 0.1926(2) 0.46640(10) 1.06391(11) 0.0258(6) Uani 1 1 d . . . C13 C 0.2880(2) 0.45476(12) 1.04326(14) 0.0281(7) Uani 1 1 d . . . C14 C 0.3695(3) 0.43841(14) 1.08946(15) 0.0399(9) Uani 1 1 d . . . H14 H 0.4443 0.4280 1.0867 0.048 Uiso 1 1 calc R . . C15 C 0.3180(3) 0.44063(13) 1.13915(16) 0.0393(9) Uani 1 1 d . . . H15 H 0.3511 0.4317 1.1783 0.047 Uiso 1 1 calc R . . N21 N 0.2035(2) 0.47679(10) 0.94464(12) 0.0283(6) Uani 1 1 d . . . C22 C 0.2966(3) 0.46094(12) 0.98029(15) 0.0303(7) Uani 1 1 d . . . C23 C 0.3975(3) 0.45203(15) 0.95816(17) 0.0472(10) Uani 1 1 d . . . H23 H 0.4614 0.4406 0.9842 0.057 Uiso 1 1 calc R . . C24 C 0.4044(3) 0.45985(17) 0.89848(17) 0.0557(11) Uani 1 1 d . . . H24 H 0.4726 0.4541 0.8829 0.067 Uiso 1 1 calc R . . C25 C 0.3093(3) 0.47625(15) 0.86195(17) 0.0459(9) Uani 1 1 d . . . H25 H 0.3108 0.4820 0.8206 0.055 Uiso 1 1 calc R . . C26 C 0.2128(3) 0.48405(12) 0.88665(15) 0.0337(8) Uani 1 1 d . . . H26 H 0.1482 0.4953 0.8611 0.040 Uiso 1 1 calc R . . N31 N -0.0209(2) 0.56948(10) 0.85606(11) 0.0284(6) Uani 1 1 d . . . N32 N 0.0363(2) 0.56612(9) 0.91208(11) 0.0266(6) Uani 1 1 d . . . C33 C 0.1187(2) 0.60279(12) 0.91372(14) 0.0269(7) Uani 1 1 d . . . C34 C 0.1147(3) 0.62935(13) 0.85902(14) 0.0344(8) Uani 1 1 d . . . H34 H 0.1632 0.6568 0.8484 0.041 Uiso 1 1 calc R . . C35 C 0.0254(3) 0.60706(12) 0.82429(14) 0.0337(8) Uani 1 1 d . . . H35 H 0.0001 0.6165 0.7841 0.040 Uiso 1 1 calc R . . N41 N 0.1814(2) 0.57882(10) 1.01479(11) 0.0275(6) Uani 1 1 d . . . C42 C 0.1943(2) 0.61100(12) 0.96916(14) 0.0288(7) Uani 1 1 d . . . C43 C 0.2734(3) 0.65236(13) 0.97277(16) 0.0429(9) Uani 1 1 d . . . H43 H 0.2806 0.6743 0.9392 0.051 Uiso 1 1 calc R . . C44 C 0.3404(3) 0.66058(15) 1.02581(17) 0.0508(11) Uani 1 1 d . . . H44 H 0.3943 0.6886 1.0294 0.061 Uiso 1 1 calc R . . C45 C 0.3291(3) 0.62787(13) 1.07390(16) 0.0408(9) Uani 1 1 d . . . H45 H 0.3742 0.6329 1.1112 0.049 Uiso 1 1 calc R . . C46 C 0.2492(3) 0.58742(12) 1.06571(15) 0.0325(8) Uani 1 1 d . . . H46 H 0.2421 0.5643 1.0984 0.039 Uiso 1 1 calc R . . N51 N 0.0826(2) 0.52542(11) 1.15904(11) 0.0295(6) Uani 1 1 d . . . N52 N 0.0361(2) 0.54773(10) 1.10685(11) 0.0258(6) Uani 1 1 d . . . C53 C 0.0156(3) 0.59907(13) 1.11898(15) 0.0308(8) Uani 1 1 d . . . C54 C 0.0489(3) 0.61023(14) 1.17918(15) 0.0428(9) Uani 1 1 d . . . H54 H 0.0440 0.6436 1.1992 0.051 Uiso 1 1 calc R . . C55 C 0.0900(3) 0.56251(14) 1.20271(15) 0.0398(9) Uani 1 1 d . . . H55 H 0.1190 0.5565 1.2432 0.048 Uiso 1 1 calc R . . N61 N 0.0567(2) 0.38614(10) 0.98334(11) 0.0284(6) Uani 1 1 d . . . C62 C 0.0315(3) 0.36445(12) 0.92913(15) 0.0318(8) Uani 1 1 d . . . C63 C 0.0463(3) 0.30959(13) 0.91761(18) 0.0457(10) Uani 1 1 d . . . H63 H 0.0272 0.2955 0.8786 0.055 Uiso 1 1 calc R . . C64 C 0.0893(3) 0.27644(14) 0.96389(19) 0.0509(11) Uani 1 1 d . . . H64 H 0.1004 0.2392 0.9573 0.061 Uiso 1 1 calc R . . C65 C 0.1157(3) 0.29825(13) 1.01980(18) 0.0424(9) Uani 1 1 d . . . H65 H 0.1454 0.2763 1.0525 0.051 Uiso 1 1 calc R . . C66 C 0.0982(3) 0.35263(13) 1.02742(16) 0.0360(8) Uani 1 1 d . . . H66 H 0.1167 0.3673 1.0662 0.043 Uiso 1 1 calc R . . N111 N 0.1081(2) 0.39149(9) 0.60143(11) 0.0266(6) Uani 1 1 d . . . N112 N 0.1056(2) 0.41240(9) 0.54593(11) 0.0267(6) Uani 1 1 d . . . C113 C 0.1734(2) 0.38132(11) 0.51804(14) 0.0256(7) Uani 1 1 d . . . C114 C 0.2200(3) 0.34014(12) 0.55660(14) 0.0300(7) Uani 1 1 d . . . H114 H 0.2709 0.3128 0.5484 0.036 Uiso 1 1 calc R . . C115 C 0.1761(2) 0.34818(12) 0.60804(14) 0.0303(8) Uani 1 1 d . . . H115 H 0.1909 0.3268 0.6430 0.036 Uiso 1 1 calc R . . N121 N 0.1383(2) 0.43655(10) 0.43121(11) 0.0283(6) Uani 1 1 d . . . C122 C 0.1897(2) 0.39238(12) 0.45695(14) 0.0277(7) Uani 1 1 d . . . C123 C 0.2546(3) 0.35902(14) 0.42685(16) 0.0465(10) Uani 1 1 d . . . H123 H 0.2883 0.3279 0.4459 0.056 Uiso 1 1 calc R . . C124 C 0.2707(3) 0.37078(16) 0.36943(18) 0.0593(12) Uani 1 1 d . . . H124 H 0.3154 0.3482 0.3483 0.071 Uiso 1 1 calc R . . C125 C 0.2199(3) 0.41638(14) 0.34312(15) 0.0419(9) Uani 1 1 d . . . H125 H 0.2294 0.4260 0.3036 0.050 Uiso 1 1 calc R . . C126 C 0.1558(3) 0.44724(12) 0.37530(14) 0.0309(8) Uani 1 1 d . . . H126 H 0.1213 0.4784 0.3567 0.037 Uiso 1 1 calc R . . N131 N 0.0836(2) 0.47491(10) 0.65975(11) 0.0269(6) Uani 1 1 d . . . N132 N 0.0800(2) 0.51242(9) 0.61590(11) 0.0259(6) Uani 1 1 d . . . C133 C 0.1227(3) 0.55793(12) 0.64232(13) 0.0276(7) Uani 1 1 d . . . C134 C 0.1532(3) 0.54914(13) 0.70350(14) 0.0337(8) Uani 1 1 d . . . H134 H 0.1854 0.5743 0.7324 0.040 Uiso 1 1 calc R . . C135 C 0.1265(3) 0.49637(13) 0.71273(14) 0.0332(7) Uani 1 1 d . . . H135 H 0.1364 0.4781 0.7499 0.040 Uiso 1 1 calc R . . N141 N 0.0928(2) 0.60399(10) 0.54895(11) 0.0287(6) Uani 1 1 d . . . C142 C 0.1326(3) 0.60673(12) 0.60795(14) 0.0298(7) Uani 1 1 d . . . C143 C 0.1816(3) 0.65297(13) 0.63406(16) 0.0457(10) Uani 1 1 d . . . H143 H 0.2086 0.6536 0.6754 0.055 Uiso 1 1 calc R . . C144 C 0.1904(3) 0.69790(14) 0.59935(16) 0.0515(11) Uani 1 1 d . . . H144 H 0.2238 0.7299 0.6165 0.062 Uiso 1 1 calc R . . C145 C 0.1504(3) 0.69612(13) 0.53937(16) 0.0403(9) Uani 1 1 d . . . H145 H 0.1555 0.7265 0.5144 0.048 Uiso 1 1 calc R . . C146 C 0.1030(3) 0.64883(12) 0.51708(15) 0.0334(8) Uani 1 1 d . . . H146 H 0.0751 0.6478 0.4759 0.040 Uiso 1 1 calc R . . N151 N 0.0831(2) 0.58115(9) 0.37810(11) 0.0251(6) Uani 1 1 d . . . N152 N 0.1198(2) 0.55649(9) 0.43071(11) 0.0268(6) Uani 1 1 d . . . C153 C 0.2319(3) 0.56249(12) 0.43823(14) 0.0277(7) Uani 1 1 d . . . C154 C 0.2667(3) 0.58959(12) 0.39018(14) 0.0306(7) Uani 1 1 d . . . H154 H 0.3409 0.5983 0.3842 0.037 Uiso 1 1 calc R . . C155 C 0.1701(3) 0.60097(12) 0.35358(14) 0.0300(7) Uani 1 1 d . . . H155 H 0.1652 0.6198 0.3168 0.036 Uiso 1 1 calc R . . N161 N 0.2463(2) 0.51081(9) 0.52819(12) 0.0284(6) Uani 1 1 d . . . C162 C 0.2981(3) 0.54314(12) 0.49326(14) 0.0297(7) Uani 1 1 d . . . C163 C 0.4084(3) 0.55923(13) 0.50769(15) 0.0357(8) Uani 1 1 d . . . H163 H 0.4410 0.5834 0.4824 0.043 Uiso 1 1 calc R . . C164 C 0.4706(3) 0.54000(13) 0.55884(16) 0.0393(8) Uani 1 1 d . . . H164 H 0.5463 0.5505 0.5695 0.047 Uiso 1 1 calc R . . C165 C 0.4198(3) 0.50522(13) 0.59387(15) 0.0372(8) Uani 1 1 d . . . H165 H 0.4605 0.4905 0.6289 0.045 Uiso 1 1 calc R . . C166 C 0.3086(3) 0.49186(12) 0.57744(14) 0.0319(8) Uani 1 1 d . . . H166 H 0.2744 0.4680 0.6024 0.038 Uiso 1 1 calc R . . B200 B 0.3900(3) 0.73900(14) 1.32563(17) 0.0324(9) Uani 1 1 d . . . C211 C 0.4202(3) 0.78731(15) 1.28099(17) 0.0439(9) Uani 1 1 d . . . C212 C 0.4547(4) 0.77779(18) 1.2255(2) 0.0631(12) Uani 1 1 d . . . H212 H 0.4669 0.7417 1.2142 0.076 Uiso 1 1 calc R . . C213 C 0.4721(4) 0.8190(2) 1.1862(2) 0.0860(17) Uani 1 1 d . . . H213 H 0.4929 0.8107 1.1482 0.103 Uiso 1 1 calc R . . C214 C 0.4590(4) 0.8721(2) 1.2025(3) 0.0896(19) Uani 1 1 d . . . H214 H 0.4739 0.9005 1.1766 0.107 Uiso 1 1 calc R . . C215 C 0.4240(3) 0.88370(17) 1.2566(2) 0.0692(14) Uani 1 1 d . . . H215 H 0.4137 0.9200 1.2679 0.083 Uiso 1 1 calc R . . C216 C 0.4042(3) 0.84195(14) 1.29427(19) 0.0485(10) Uani 1 1 d . . . H216 H 0.3784 0.8506 1.3309 0.058 Uiso 1 1 calc R . . C221 C 0.2536(3) 0.74099(11) 1.32383(15) 0.0305(8) Uani 1 1 d . . . C222 C 0.1839(3) 0.75089(12) 1.26925(15) 0.0392(8) Uani 1 1 d . . . H222 H 0.2179 0.7580 1.2346 0.047 Uiso 1 1 calc R . . C223 C 0.0685(3) 0.75052(14) 1.26455(17) 0.0461(9) Uani 1 1 d . . . H223 H 0.0254 0.7568 1.2270 0.055 Uiso 1 1 calc R . . C224 C 0.0156(3) 0.74126(14) 1.3134(2) 0.0551(11) Uani 1 1 d . . . H224 H -0.0637 0.7408 1.3098 0.066 Uiso 1 1 calc R . . C225 C 0.0790(3) 0.73260(14) 1.36756(19) 0.0466(10) Uani 1 1 d . . . H225 H 0.0435 0.7265 1.4019 0.056 Uiso 1 1 calc R . . C226 C 0.1946(3) 0.73269(12) 1.37228(16) 0.0338(8) Uani 1 1 d . . . H226 H 0.2361 0.7268 1.4104 0.041 Uiso 1 1 calc R . . C231 C 0.4569(3) 0.74728(12) 1.39334(15) 0.0331(7) Uani 1 1 d . . . C232 C 0.4442(3) 0.71003(13) 1.43922(15) 0.0371(8) Uani 1 1 d . . . H232 H 0.3941 0.6807 1.4304 0.044 Uiso 1 1 calc R . . C233 C 0.5010(3) 0.71408(14) 1.49617(16) 0.0437(9) Uani 1 1 d . . . H233 H 0.4892 0.6880 1.5253 0.052 Uiso 1 1 calc R . . C234 C 0.5748(3) 0.75588(14) 1.51082(19) 0.0497(11) Uani 1 1 d . . . H234 H 0.6135 0.7592 1.5500 0.060 Uiso 1 1 calc R . . C235 C 0.5910(3) 0.79238(15) 1.46763(19) 0.0496(10) Uani 1 1 d . . . H235 H 0.6426 0.8210 1.4768 0.060 Uiso 1 1 calc R . . C236 C 0.5336(3) 0.78833(13) 1.41084(17) 0.0406(9) Uani 1 1 d . . . H236 H 0.5469 0.8147 1.3823 0.049 Uiso 1 1 calc R . . C241 C 0.4263(3) 0.67979(13) 1.30082(14) 0.0301(7) Uani 1 1 d . . . C242 C 0.3571(3) 0.64820(13) 1.25997(14) 0.0358(8) Uani 1 1 d . . . H242 H 0.2848 0.6615 1.2455 0.043 Uiso 1 1 calc R . . C243 C 0.3886(3) 0.59862(14) 1.23955(15) 0.0386(8) Uani 1 1 d . . . H243 H 0.3382 0.5788 1.2119 0.046 Uiso 1 1 calc R . . C244 C 0.4935(3) 0.57792(14) 1.25944(14) 0.0406(9) Uani 1 1 d . . . H244 H 0.5158 0.5439 1.2460 0.049 Uiso 1 1 calc R . . C245 C 0.5646(3) 0.60792(14) 1.29915(16) 0.0414(9) Uani 1 1 d . . . H245 H 0.6372 0.5947 1.3130 0.050 Uiso 1 1 calc R . . C246 C 0.5310(3) 0.65725(14) 1.31905(15) 0.0374(8) Uani 1 1 d . . . H246 H 0.5820 0.6768 1.3466 0.045 Uiso 1 1 calc R . . C311 C 0.7344(11) 0.8267(6) 1.6868(8) 0.143(3) Uani 0.608(4) 1 d PD A 1 H31F H 0.6615 0.8406 1.6942 0.215 Uiso 0.608(4) 1 calc PR A 1 H31G H 0.7471 0.8362 1.6463 0.215 Uiso 0.608(4) 1 calc PR A 1 H31H H 0.7933 0.8426 1.7155 0.215 Uiso 0.608(4) 1 calc PR A 1 C312 C 0.7360(14) 0.7703(6) 1.6931(8) 0.143(3) Uani 0.608(4) 1 d PD A 1 H31L H 0.6650 0.7538 1.6749 0.172 Uiso 0.608(4) 1 calc PR A 1 H31M H 0.7990 0.7539 1.6757 0.172 Uiso 0.608(4) 1 calc PR A 1 O313 O 0.7500(4) 0.7660(3) 1.7536(3) 0.099(2) Uani 0.608(4) 1 d PD A 1 C314 C 0.7421(9) 0.7094(5) 1.7623(6) 0.143(3) Uani 0.608(4) 1 d PD A 1 H31A H 0.6682 0.6959 1.7440 0.172 Uiso 0.608(4) 1 calc PR A 1 H31E H 0.8007 0.6903 1.7438 0.172 Uiso 0.608(4) 1 calc PR A 1 C315 C 0.7559(8) 0.7009(5) 1.8218(5) 0.143(3) Uani 0.608(4) 1 d PD A 1 H31B H 0.7383 0.6633 1.8299 0.215 Uiso 0.608(4) 1 calc PR A 1 H31C H 0.7058 0.7248 1.8403 0.215 Uiso 0.608(4) 1 calc PR A 1 H31D H 0.8335 0.7086 1.8382 0.215 Uiso 0.608(4) 1 calc PR A 1 O300 O 0.7397(10) 0.7572(4) 1.6545(6) 0.105(4) Uani 0.392(4) 1 d P A 2 C300 C 0.7052(9) 0.8030(6) 1.6729(6) 0.069(4) Uani 0.392(4) 1 d PD A 2 C301 C 0.6022(11) 0.8258(5) 1.6504(5) 0.079(4) Uani 0.392(4) 1 d PD A 2 H30A H 0.6130 0.8520 1.6193 0.119 Uiso 0.392(4) 1 calc PR A 2 H30B H 0.5703 0.8439 1.6826 0.119 Uiso 0.392(4) 1 calc PR A 2 H30C H 0.5511 0.7974 1.6334 0.119 Uiso 0.392(4) 1 calc PR A 2 C302 C 0.7833(10) 0.8401(6) 1.7078(7) 0.080(5) Uani 0.392(4) 1 d PD A 2 H30D H 0.8215 0.8212 1.7426 0.119 Uiso 0.392(4) 1 calc PR A 2 H30E H 0.7418 0.8708 1.7208 0.119 Uiso 0.392(4) 1 calc PR A 2 H30F H 0.8385 0.8530 1.6831 0.119 Uiso 0.392(4) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.02472(12) 0.02332(12) 0.02112(13) 0.00179(12) -0.00001(10) -0.00240(11) B1 0.039(2) 0.034(2) 0.021(2) 0.0062(17) -0.0037(17) -0.0037(18) Nd2 0.03251(14) 0.02173(12) 0.02007(13) -0.00016(12) 0.00146(10) 0.00512(11) B2 0.038(2) 0.0264(19) 0.0194(19) 0.0033(16) 0.0040(16) 0.0006(16) N11 0.0317(15) 0.0290(14) 0.0239(15) 0.0043(12) -0.0021(12) -0.0026(11) N12 0.0267(14) 0.0255(14) 0.0241(14) 0.0014(11) -0.0007(11) -0.0019(11) C13 0.0257(17) 0.0266(17) 0.0314(19) 0.0005(14) 0.0014(14) 0.0000(13) C14 0.0271(18) 0.050(2) 0.041(2) 0.0042(18) -0.0009(16) 0.0076(16) C15 0.0310(19) 0.046(2) 0.037(2) 0.0081(17) -0.0073(16) 0.0058(16) N21 0.0291(15) 0.0262(14) 0.0291(16) 0.0005(12) 0.0023(12) -0.0007(11) C22 0.0257(17) 0.0305(18) 0.035(2) -0.0012(15) 0.0063(15) -0.0023(14) C23 0.029(2) 0.066(3) 0.046(2) 0.002(2) 0.0041(17) 0.0067(18) C24 0.033(2) 0.090(3) 0.047(3) -0.006(2) 0.0120(19) 0.007(2) C25 0.040(2) 0.064(2) 0.036(2) -0.0006(19) 0.0105(18) 0.0012(19) C26 0.0327(19) 0.0336(19) 0.035(2) -0.0009(15) 0.0037(16) 0.0008(14) N31 0.0343(15) 0.0273(14) 0.0231(15) 0.0010(12) 0.0022(12) -0.0027(12) N32 0.0285(14) 0.0250(14) 0.0251(15) 0.0048(11) -0.0006(12) -0.0022(11) C33 0.0288(17) 0.0228(16) 0.0295(18) 0.0025(14) 0.0059(14) -0.0021(13) C34 0.040(2) 0.0310(18) 0.035(2) 0.0064(15) 0.0121(16) -0.0053(15) C35 0.043(2) 0.0320(18) 0.0265(18) 0.0086(15) 0.0063(16) 0.0009(15) N41 0.0289(14) 0.0275(14) 0.0256(15) 0.0002(12) 0.0017(12) -0.0023(11) C42 0.0263(17) 0.0258(17) 0.0344(19) 0.0040(15) 0.0045(15) -0.0007(13) C43 0.041(2) 0.040(2) 0.046(2) 0.0149(18) -0.0010(18) -0.0130(17) C44 0.047(2) 0.048(2) 0.054(3) 0.011(2) -0.007(2) -0.0269(18) C45 0.035(2) 0.044(2) 0.039(2) 0.0003(17) -0.0080(16) -0.0125(16) C46 0.0304(18) 0.0316(18) 0.035(2) 0.0039(15) 0.0024(15) -0.0010(14) N51 0.0318(16) 0.0335(15) 0.0220(15) -0.0009(13) -0.0008(12) -0.0047(13) N52 0.0255(14) 0.0265(14) 0.0250(15) -0.0016(12) 0.0022(11) -0.0041(11) C53 0.0291(18) 0.0291(18) 0.034(2) -0.0039(15) 0.0039(15) -0.0058(14) C54 0.053(2) 0.040(2) 0.034(2) -0.0116(17) -0.0002(18) -0.0036(18) C55 0.050(2) 0.043(2) 0.0239(19) -0.0085(17) -0.0029(16) -0.0070(17) N61 0.0249(14) 0.0290(14) 0.0307(16) 0.0023(12) 0.0017(12) -0.0015(11) C62 0.0292(18) 0.0237(16) 0.043(2) -0.0023(15) 0.0046(15) -0.0042(14) C63 0.051(2) 0.0299(19) 0.056(3) -0.0091(18) 0.0034(19) -0.0024(17) C64 0.050(2) 0.0229(19) 0.079(3) -0.002(2) 0.008(2) 0.0034(17) C65 0.038(2) 0.032(2) 0.057(3) 0.0069(18) 0.0025(19) 0.0020(16) C66 0.0318(19) 0.035(2) 0.041(2) 0.0058(17) 0.0031(16) -0.0004(15) N111 0.0325(15) 0.0235(14) 0.0227(15) 0.0020(11) -0.0005(12) 0.0044(11) N112 0.0341(15) 0.0230(14) 0.0218(14) -0.0004(11) 0.0001(12) 0.0022(11) C113 0.0281(17) 0.0189(16) 0.0286(18) 0.0000(13) -0.0010(14) 0.0003(13) C114 0.0316(18) 0.0240(17) 0.034(2) 0.0011(14) 0.0023(15) 0.0057(14) C115 0.0305(18) 0.0271(17) 0.032(2) 0.0069(15) -0.0019(15) 0.0040(14) N121 0.0334(15) 0.0248(14) 0.0261(15) -0.0016(12) 0.0013(12) 0.0034(11) C122 0.0270(17) 0.0233(16) 0.0326(19) -0.0025(14) 0.0037(14) 0.0024(13) C123 0.060(2) 0.039(2) 0.044(2) 0.0050(18) 0.020(2) 0.0216(19) C124 0.080(3) 0.057(3) 0.049(3) 0.008(2) 0.034(2) 0.035(2) C125 0.051(2) 0.046(2) 0.030(2) 0.0027(17) 0.0116(17) 0.0154(18) C126 0.0366(19) 0.0290(18) 0.0260(18) 0.0019(15) 0.0002(15) 0.0063(14) N131 0.0330(15) 0.0253(14) 0.0218(15) 0.0004(12) 0.0013(12) 0.0018(12) N132 0.0339(15) 0.0224(14) 0.0205(14) -0.0023(10) -0.0003(11) 0.0019(10) C133 0.0330(18) 0.0245(17) 0.0248(18) -0.0012(14) 0.0026(14) 0.0043(14) C134 0.040(2) 0.0348(19) 0.0255(18) -0.0084(15) 0.0001(15) -0.0046(15) C135 0.0388(18) 0.0392(19) 0.0203(15) -0.0037(17) -0.0009(13) -0.0023(16) N141 0.0346(15) 0.0261(14) 0.0249(15) -0.0018(12) 0.0026(12) 0.0047(12) C142 0.0338(18) 0.0276(17) 0.0276(19) -0.0040(15) 0.0029(15) 0.0038(14) C143 0.071(3) 0.0284(19) 0.035(2) -0.0061(17) -0.0031(19) -0.0107(18) C144 0.081(3) 0.028(2) 0.042(2) -0.0063(18) -0.004(2) -0.0125(19) C145 0.057(2) 0.0254(18) 0.037(2) 0.0005(16) 0.0027(18) -0.0004(16) C146 0.042(2) 0.0291(19) 0.0292(19) -0.0018(15) 0.0032(16) 0.0046(15) N151 0.0317(15) 0.0225(13) 0.0209(14) -0.0011(11) 0.0027(12) 0.0004(11) N152 0.0351(16) 0.0225(13) 0.0218(14) 0.0004(11) -0.0002(12) 0.0021(11) C153 0.0350(19) 0.0229(16) 0.0250(17) -0.0031(14) 0.0028(14) 0.0022(14) C154 0.0340(18) 0.0270(17) 0.0316(19) -0.0036(15) 0.0077(15) -0.0047(14) C155 0.040(2) 0.0222(16) 0.0274(18) -0.0011(14) 0.0021(15) -0.0001(14) N161 0.0345(15) 0.0230(15) 0.0273(15) -0.0033(11) 0.0025(12) 0.0045(11) C162 0.0339(19) 0.0258(17) 0.0291(19) -0.0051(14) 0.0033(15) 0.0028(14) C163 0.036(2) 0.0346(19) 0.035(2) 0.0010(16) 0.0017(16) 0.0012(15) C164 0.0323(19) 0.043(2) 0.041(2) -0.0035(18) 0.0008(16) 0.0001(16) C165 0.0384(19) 0.038(2) 0.0324(18) -0.0036(17) -0.0050(15) 0.0084(16) C166 0.0403(19) 0.0297(19) 0.0248(17) 0.0014(14) 0.0013(14) 0.0043(14) B200 0.038(2) 0.030(2) 0.030(2) 0.0041(16) 0.0072(17) 0.0017(16) C211 0.039(2) 0.046(2) 0.048(2) 0.0161(19) 0.0126(18) 0.0042(17) C212 0.070(3) 0.064(3) 0.061(3) 0.027(2) 0.026(2) 0.011(2) C213 0.090(4) 0.094(4) 0.083(4) 0.050(3) 0.044(3) 0.024(3) C214 0.073(3) 0.086(4) 0.116(5) 0.070(4) 0.034(3) 0.018(3) C215 0.045(3) 0.047(3) 0.116(4) 0.039(3) 0.009(3) 0.002(2) C216 0.038(2) 0.037(2) 0.071(3) 0.019(2) 0.010(2) 0.0018(17) C221 0.0344(18) 0.0224(18) 0.0342(19) 0.0015(14) 0.0028(15) 0.0026(13) C222 0.052(2) 0.0319(18) 0.0331(19) -0.0017(17) 0.0043(16) 0.0030(18) C223 0.045(2) 0.041(2) 0.047(2) -0.004(2) -0.0138(18) 0.0001(19) C224 0.034(2) 0.045(3) 0.085(3) 0.009(2) 0.000(2) -0.0123(17) C225 0.046(2) 0.0348(19) 0.062(3) 0.0094(19) 0.017(2) -0.0042(17) C226 0.041(2) 0.0250(16) 0.035(2) 0.0034(14) 0.0034(16) -0.0004(14) C231 0.0347(17) 0.0279(17) 0.0365(19) -0.0049(17) 0.0047(14) 0.0021(16) C232 0.041(2) 0.0313(18) 0.037(2) -0.0019(16) -0.0014(16) 0.0045(15) C233 0.055(2) 0.0386(19) 0.035(2) -0.0054(18) -0.0012(17) 0.0195(19) C234 0.050(2) 0.041(2) 0.052(3) -0.020(2) -0.0131(19) 0.0219(19) C235 0.039(2) 0.040(2) 0.068(3) -0.018(2) -0.004(2) 0.0027(17) C236 0.037(2) 0.0329(19) 0.052(2) -0.0029(17) 0.0063(18) -0.0005(16) C241 0.0349(19) 0.0330(18) 0.0231(18) 0.0054(14) 0.0070(15) -0.0002(15) C242 0.0362(19) 0.046(2) 0.0262(19) -0.0009(16) 0.0071(15) 0.0036(16) C243 0.046(2) 0.040(2) 0.029(2) -0.0025(16) 0.0047(16) -0.0036(17) C244 0.055(2) 0.037(2) 0.033(2) 0.0019(16) 0.0146(19) 0.0056(18) C245 0.039(2) 0.042(2) 0.043(2) 0.0057(18) 0.0062(18) 0.0107(17) C246 0.039(2) 0.039(2) 0.033(2) 0.0020(16) 0.0023(16) 0.0019(16) C311 0.083(4) 0.142(6) 0.209(10) -0.071(8) 0.034(6) -0.025(4) C312 0.083(4) 0.142(6) 0.209(10) -0.071(8) 0.034(6) -0.025(4) O313 0.052(3) 0.185(7) 0.059(4) 0.027(4) 0.000(3) -0.004(4) C314 0.083(4) 0.142(6) 0.209(10) -0.071(8) 0.034(6) -0.025(4) C315 0.083(4) 0.142(6) 0.209(10) -0.071(8) 0.034(6) -0.025(4) O300 0.133(10) 0.064(6) 0.127(10) -0.024(6) 0.047(8) -0.019(6) C300 0.045(8) 0.087(10) 0.076(9) -0.064(8) 0.009(6) -0.033(7) C301 0.101(11) 0.066(8) 0.074(9) -0.005(7) 0.024(8) 0.020(7) C302 0.035(7) 0.107(11) 0.097(11) -0.056(9) 0.011(7) 0.001(7) _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 2.664(2) 3_567 ? Nd1 N32 2.664(2) . ? Nd1 N52 2.680(2) . ? Nd1 N52 2.680(2) 3_567 ? Nd1 N12 2.702(2) . ? Nd1 N12 2.702(2) 3_567 ? Nd1 N41 2.924(2) 3_567 ? Nd1 N41 2.924(2) . ? Nd1 N61 2.945(2) . ? Nd1 N61 2.945(2) 3_567 ? Nd1 N21 2.963(3) 3_567 ? Nd1 N21 2.963(3) . ? B1 N31 1.522(4) 3_567 ? B1 N51 1.525(5) . ? B1 N11 1.540(5) . ? Nd2 N112 2.662(2) . ? Nd2 N112 2.662(2) 3_566 ? Nd2 N152 2.672(3) 3_566 ? Nd2 N152 2.672(3) . ? Nd2 N132 2.693(2) . ? Nd2 N132 2.693(2) 3_566 ? Nd2 N121 2.899(2) 3_566 ? Nd2 N121 2.899(3) . ? Nd2 N141 2.970(2) 3_566 ? Nd2 N141 2.970(2) . ? Nd2 N161 2.970(3) . ? Nd2 N161 2.970(3) 3_566 ? B2 N151 1.526(4) 3_566 ? B2 N131 1.537(4) . ? B2 N111 1.540(4) . ? N11 C15 1.349(4) . ? N11 N12 1.360(3) . ? N12 C13 1.333(4) . ? C13 C14 1.398(4) . ? C13 C22 1.453(4) . ? C14 C15 1.359(5) . ? N21 C26 1.346(4) . ? N21 C22 1.352(4) . ? C22 C23 1.397(4) . ? C23 C24 1.380(5) . ? C24 C25 1.384(5) . ? C25 C26 1.373(4) . ? N31 C35 1.346(4) . ? N31 N32 1.365(3) . ? N31 B1 1.522(4) 3_567 ? N32 C33 1.346(4) . ? C33 C34 1.400(4) . ? C33 C42 1.465(4) . ? C34 C35 1.364(4) . ? N41 C42 1.332(4) . ? N41 C46 1.340(4) . ? C42 C43 1.398(4) . ? C43 C44 1.372(5) . ? C44 C45 1.381(5) . ? C45 C46 1.388(4) . ? N51 C55 1.346(4) . ? N51 N52 1.358(3) . ? N52 C53 1.334(4) . ? C53 C54 1.398(4) . ? C53 C62 1.472(4) 3_567 ? C54 C55 1.365(5) . ? N61 C62 1.339(4) . ? N61 C66 1.345(4) . ? C62 C63 1.403(4) . ? C62 C53 1.472(4) 3_567 ? C63 C64 1.379(5) . ? C64 C65 1.376(5) . ? C65 C66 1.381(4) . ? N111 C115 1.350(4) . ? N111 N112 1.358(3) . ? N112 C113 1.343(4) . ? C113 C114 1.413(4) . ? C113 C122 1.451(4) . ? C114 C115 1.359(4) . ? N121 C126 1.339(4) . ? N121 C122 1.354(4) . ? C122 C123 1.382(4) . ? C123 C124 1.373(5) . ? C124 C125 1.384(5) . ? C125 C126 1.368(4) . ? N131 C135 1.352(4) . ? N131 N132 1.359(3) . ? N132 C133 1.348(4) . ? C133 C134 1.404(4) . ? C133 C142 1.454(4) . ? C134 C135 1.372(4) . ? N141 C146 1.342(4) . ? N141 C142 1.361(4) . ? C142 C143 1.387(4) . ? C143 C144 1.378(5) . ? C144 C145 1.382(5) . ? C145 C146 1.373(4) . ? N151 C155 1.347(4) . ? N151 N152 1.361(3) . ? N151 B2 1.526(4) 3_566 ? N152 C153 1.351(4) . ? C153 C154 1.392(4) . ? C153 C162 1.470(4) . ? C154 C155 1.367(4) . ? N161 C162 1.341(4) . ? N161 C166 1.345(4) . ? C162 C163 1.388(4) . ? C163 C164 1.380(4) . ? C164 C165 1.372(4) . ? C165 C166 1.386(4) . ? B200 C211 1.641(5) . ? B200 C221 1.644(5) . ? B200 C231 1.649(5) . ? B200 C241 1.654(5) . ? C211 C212 1.397(5) . ? C211 C216 1.409(5) . ? C212 C213 1.393(5) . ? C213 C214 1.385(7) . ? C214 C215 1.380(6) . ? C215 C216 1.384(5) . ? C221 C226 1.403(5) . ? C221 C222 1.421(5) . ? C222 C223 1.384(5) . ? C223 C224 1.370(5) . ? C224 C225 1.375(5) . ? C225 C226 1.386(5) . ? C231 C236 1.399(4) . ? C231 C232 1.416(4) . ? C232 C233 1.382(4) . ? C233 C234 1.379(5) . ? C234 C235 1.367(5) . ? C235 C236 1.382(5) . ? C241 C246 1.394(4) . ? C241 C242 1.401(4) . ? C242 C243 1.386(4) . ? C243 C244 1.386(4) . ? C244 C245 1.377(5) . ? C245 C246 1.384(4) . ? C311 C312 1.407(16) . ? C312 O313 1.363(16) . ? O313 C314 1.424(12) . ? C314 C315 1.353(13) . ? O300 C300 1.298(15) . ? C300 C301 1.401(13) . ? C300 C302 1.471(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N32 Nd1 N32 180.000(1) 3_567 . ? N32 Nd1 N52 67.61(7) 3_567 . ? N32 Nd1 N52 112.39(7) . . ? N32 Nd1 N52 112.39(7) 3_567 3_567 ? N32 Nd1 N52 67.61(7) . 3_567 ? N52 Nd1 N52 180.000(1) . 3_567 ? N32 Nd1 N12 67.95(7) 3_567 . ? N32 Nd1 N12 112.05(7) . . ? N52 Nd1 N12 68.14(7) . . ? N52 Nd1 N12 111.86(7) 3_567 . ? N32 Nd1 N12 112.05(7) 3_567 3_567 ? N32 Nd1 N12 67.95(7) . 3_567 ? N52 Nd1 N12 111.86(7) . 3_567 ? N52 Nd1 N12 68.14(7) 3_567 3_567 ? N12 Nd1 N12 180.0 . 3_567 ? N32 Nd1 N41 58.49(7) 3_567 3_567 ? N32 Nd1 N41 121.51(7) . 3_567 ? N52 Nd1 N41 115.36(7) . 3_567 ? N52 Nd1 N41 64.64(7) 3_567 3_567 ? N12 Nd1 N41 115.66(7) . 3_567 ? N12 Nd1 N41 64.34(7) 3_567 3_567 ? N32 Nd1 N41 121.51(7) 3_567 . ? N32 Nd1 N41 58.49(7) . . ? N52 Nd1 N41 64.64(7) . . ? N52 Nd1 N41 115.36(7) 3_567 . ? N12 Nd1 N41 64.34(7) . . ? N12 Nd1 N41 115.66(7) 3_567 . ? N41 Nd1 N41 180.00(7) 3_567 . ? N32 Nd1 N61 64.46(7) 3_567 . ? N32 Nd1 N61 115.54(7) . . ? N52 Nd1 N61 121.87(7) . . ? N52 Nd1 N61 58.13(7) 3_567 . ? N12 Nd1 N61 64.79(7) . . ? N12 Nd1 N61 115.21(7) 3_567 . ? N41 Nd1 N61 61.74(7) 3_567 . ? N41 Nd1 N61 118.26(7) . . ? N32 Nd1 N61 115.54(7) 3_567 3_567 ? N32 Nd1 N61 64.46(7) . 3_567 ? N52 Nd1 N61 58.13(7) . 3_567 ? N52 Nd1 N61 121.87(7) 3_567 3_567 ? N12 Nd1 N61 115.21(7) . 3_567 ? N12 Nd1 N61 64.79(7) 3_567 3_567 ? N41 Nd1 N61 118.26(7) 3_567 3_567 ? N41 Nd1 N61 61.74(7) . 3_567 ? N61 Nd1 N61 180.000(1) . 3_567 ? N32 Nd1 N21 64.77(7) 3_567 3_567 ? N32 Nd1 N21 115.23(7) . 3_567 ? N52 Nd1 N21 64.83(7) . 3_567 ? N52 Nd1 N21 115.17(7) 3_567 3_567 ? N12 Nd1 N21 122.44(7) . 3_567 ? N12 Nd1 N21 57.56(7) 3_567 3_567 ? N41 Nd1 N21 61.76(7) 3_567 3_567 ? N41 Nd1 N21 118.24(7) . 3_567 ? N61 Nd1 N21 117.48(7) . 3_567 ? N61 Nd1 N21 62.52(7) 3_567 3_567 ? N32 Nd1 N21 115.23(7) 3_567 . ? N32 Nd1 N21 64.77(7) . . ? N52 Nd1 N21 115.17(7) . . ? N52 Nd1 N21 64.83(7) 3_567 . ? N12 Nd1 N21 57.56(7) . . ? N12 Nd1 N21 122.44(7) 3_567 . ? N41 Nd1 N21 118.24(7) 3_567 . ? N41 Nd1 N21 61.76(7) . . ? N61 Nd1 N21 62.52(7) . . ? N61 Nd1 N21 117.48(7) 3_567 . ? N21 Nd1 N21 180.0 3_567 . ? N31 B1 N51 109.0(3) 3_567 . ? N31 B1 N11 109.8(3) 3_567 . ? N51 B1 N11 109.5(3) . . ? N112 Nd2 N112 180.00(10) . 3_566 ? N112 Nd2 N152 67.05(8) . 3_566 ? N112 Nd2 N152 112.95(8) 3_566 3_566 ? N112 Nd2 N152 112.95(8) . . ? N112 Nd2 N152 67.05(8) 3_566 . ? N152 Nd2 N152 180.00(8) 3_566 . ? N112 Nd2 N132 67.75(7) . . ? N112 Nd2 N132 112.25(7) 3_566 . ? N152 Nd2 N132 68.79(7) 3_566 . ? N152 Nd2 N132 111.21(7) . . ? N112 Nd2 N132 112.25(7) . 3_566 ? N112 Nd2 N132 67.75(7) 3_566 3_566 ? N152 Nd2 N132 111.21(7) 3_566 3_566 ? N152 Nd2 N132 68.79(7) . 3_566 ? N132 Nd2 N132 180.0 . 3_566 ? N112 Nd2 N121 120.93(7) . 3_566 ? N112 Nd2 N121 59.07(7) 3_566 3_566 ? N152 Nd2 N121 64.68(7) 3_566 3_566 ? N152 Nd2 N121 115.32(7) . 3_566 ? N132 Nd2 N121 64.54(7) . 3_566 ? N132 Nd2 N121 115.46(7) 3_566 3_566 ? N112 Nd2 N121 59.07(7) . . ? N112 Nd2 N121 120.93(7) 3_566 . ? N152 Nd2 N121 115.32(7) 3_566 . ? N152 Nd2 N121 64.68(7) . . ? N132 Nd2 N121 115.46(7) . . ? N132 Nd2 N121 64.54(7) 3_566 . ? N121 Nd2 N121 180.00(8) 3_566 . ? N112 Nd2 N141 64.73(7) . 3_566 ? N112 Nd2 N141 115.27(7) 3_566 3_566 ? N152 Nd2 N141 63.66(7) 3_566 3_566 ? N152 Nd2 N141 116.34(7) . 3_566 ? N132 Nd2 N141 122.16(7) . 3_566 ? N132 Nd2 N141 57.84(7) 3_566 3_566 ? N121 Nd2 N141 117.23(7) 3_566 3_566 ? N121 Nd2 N141 62.77(7) . 3_566 ? N112 Nd2 N141 115.27(7) . . ? N112 Nd2 N141 64.73(7) 3_566 . ? N152 Nd2 N141 116.34(7) 3_566 . ? N152 Nd2 N141 63.66(7) . . ? N132 Nd2 N141 57.84(7) . . ? N132 Nd2 N141 122.16(7) 3_566 . ? N121 Nd2 N141 62.77(7) 3_566 . ? N121 Nd2 N141 117.23(7) . . ? N141 Nd2 N141 180.00(5) 3_566 . ? N112 Nd2 N161 64.91(7) . . ? N112 Nd2 N161 115.09(7) 3_566 . ? N152 Nd2 N161 121.78(7) 3_566 . ? N152 Nd2 N161 58.22(7) . . ? N132 Nd2 N161 64.00(7) . . ? N132 Nd2 N161 116.00(7) 3_566 . ? N121 Nd2 N161 117.90(7) 3_566 . ? N121 Nd2 N161 62.10(7) . . ? N141 Nd2 N161 118.43(6) 3_566 . ? N141 Nd2 N161 61.57(6) . . ? N112 Nd2 N161 115.09(7) . 3_566 ? N112 Nd2 N161 64.91(7) 3_566 3_566 ? N152 Nd2 N161 58.22(7) 3_566 3_566 ? N152 Nd2 N161 121.78(7) . 3_566 ? N132 Nd2 N161 116.00(7) . 3_566 ? N132 Nd2 N161 64.00(7) 3_566 3_566 ? N121 Nd2 N161 62.10(7) 3_566 3_566 ? N121 Nd2 N161 117.90(7) . 3_566 ? N141 Nd2 N161 61.57(6) 3_566 3_566 ? N141 Nd2 N161 118.43(6) . 3_566 ? N161 Nd2 N161 180.000(1) . 3_566 ? N151 B2 N131 109.6(3) 3_566 . ? N151 B2 N111 109.8(3) 3_566 . ? N131 B2 N111 108.4(3) . . ? C15 N11 N12 110.0(3) . . ? C15 N11 B1 128.5(3) . . ? N12 N11 B1 121.5(2) . . ? C13 N12 N11 105.8(2) . . ? C13 N12 Nd1 127.0(2) . . ? N11 N12 Nd1 127.21(18) . . ? N12 C13 C14 110.8(3) . . ? N12 C13 C22 120.1(3) . . ? C14 C13 C22 129.1(3) . . ? C15 C14 C13 104.8(3) . . ? N11 C15 C14 108.7(3) . . ? C26 N21 C22 116.8(3) . . ? C26 N21 Nd1 124.7(2) . . ? C22 N21 Nd1 118.3(2) . . ? N21 C22 C23 121.8(3) . . ? N21 C22 C13 117.1(3) . . ? C23 C22 C13 121.1(3) . . ? C24 C23 C22 120.0(3) . . ? C23 C24 C25 118.3(3) . . ? C26 C25 C24 118.6(4) . . ? N21 C26 C25 124.4(3) . . ? C35 N31 N32 110.2(3) . . ? C35 N31 B1 128.4(3) . 3_567 ? N32 N31 B1 121.4(3) . 3_567 ? C33 N32 N31 105.4(2) . . ? C33 N32 Nd1 126.27(19) . . ? N31 N32 Nd1 128.36(18) . . ? N32 C33 C34 110.9(3) . . ? N32 C33 C42 119.4(3) . . ? C34 C33 C42 129.7(3) . . ? C35 C34 C33 104.5(3) . . ? N31 C35 C34 109.0(3) . . ? C42 N41 C46 116.9(3) . . ? C42 N41 Nd1 118.40(19) . . ? C46 N41 Nd1 124.6(2) . . ? N41 C42 C43 123.0(3) . . ? N41 C42 C33 117.3(3) . . ? C43 C42 C33 119.6(3) . . ? C44 C43 C42 118.6(3) . . ? C43 C44 C45 119.7(3) . . ? C44 C45 C46 117.4(3) . . ? N41 C46 C45 124.3(3) . . ? C55 N51 N52 109.9(3) . . ? C55 N51 B1 127.7(3) . . ? N52 N51 B1 122.4(3) . . ? C53 N52 N51 106.1(2) . . ? C53 N52 Nd1 126.6(2) . . ? N51 N52 Nd1 127.26(18) . . ? N52 C53 C54 110.7(3) . . ? N52 C53 C62 119.9(3) . 3_567 ? C54 C53 C62 129.3(3) . 3_567 ? C55 C54 C53 104.6(3) . . ? N51 C55 C54 108.7(3) . . ? C62 N61 C66 116.7(3) . . ? C62 N61 Nd1 118.39(19) . . ? C66 N61 Nd1 124.6(2) . . ? N61 C62 C63 122.8(3) . . ? N61 C62 C53 116.8(3) . 3_567 ? C63 C62 C53 120.4(3) . 3_567 ? C64 C63 C62 118.8(4) . . ? C65 C64 C63 118.9(3) . . ? C64 C65 C66 118.6(3) . . ? N61 C66 C65 124.1(3) . . ? C115 N111 N112 110.2(3) . . ? C115 N111 B2 128.7(3) . . ? N112 N111 B2 121.1(2) . . ? C113 N112 N111 106.1(2) . . ? C113 N112 Nd2 125.14(19) . . ? N111 N112 Nd2 128.65(18) . . ? N112 C113 C114 110.0(3) . . ? N112 C113 C122 120.7(3) . . ? C114 C113 C122 129.3(3) . . ? C115 C114 C113 104.8(3) . . ? N111 C115 C114 108.9(3) . . ? C126 N121 C122 116.5(3) . . ? C126 N121 Nd2 125.25(19) . . ? C122 N121 Nd2 118.2(2) . . ? N121 C122 C123 122.1(3) . . ? N121 C122 C113 116.8(3) . . ? C123 C122 C113 121.1(3) . . ? C124 C123 C122 120.2(3) . . ? C123 C124 C125 118.2(3) . . ? C126 C125 C124 118.6(3) . . ? N121 C126 C125 124.5(3) . . ? C135 N131 N132 110.5(2) . . ? C135 N131 B2 127.8(3) . . ? N132 N131 B2 121.7(2) . . ? C133 N132 N131 106.1(2) . . ? C133 N132 Nd2 126.53(19) . . ? N131 N132 Nd2 127.40(17) . . ? N132 C133 C134 110.0(3) . . ? N132 C133 C142 120.9(3) . . ? C134 C133 C142 129.0(3) . . ? C135 C134 C133 105.3(3) . . ? N131 C135 C134 108.1(3) . . ? C146 N141 C142 116.2(3) . . ? C146 N141 Nd2 125.3(2) . . ? C142 N141 Nd2 118.5(2) . . ? N141 C142 C143 122.3(3) . . ? N141 C142 C133 116.2(3) . . ? C143 C142 C133 121.5(3) . . ? C144 C143 C142 119.2(3) . . ? C143 C144 C145 119.5(3) . . ? C146 C145 C144 117.6(3) . . ? N141 C146 C145 125.1(3) . . ? C155 N151 N152 110.2(2) . . ? C155 N151 B2 127.9(3) . 3_566 ? N152 N151 B2 121.8(2) . 3_566 ? C153 N152 N151 105.3(2) . . ? C153 N152 Nd2 126.64(19) . . ? N151 N152 Nd2 127.83(18) . . ? N152 C153 C154 110.9(3) . . ? N152 C153 C162 119.6(3) . . ? C154 C153 C162 129.5(3) . . ? C155 C154 C153 104.7(3) . . ? N151 C155 C154 108.9(3) . . ? C162 N161 C166 116.5(3) . . ? C162 N161 Nd2 117.45(19) . . ? C166 N161 Nd2 125.4(2) . . ? N161 C162 C163 122.9(3) . . ? N161 C162 C153 116.9(3) . . ? C163 C162 C153 120.1(3) . . ? C164 C163 C162 119.7(3) . . ? C165 C164 C163 118.0(3) . . ? C164 C165 C166 119.2(3) . . ? N161 C166 C165 123.6(3) . . ? C211 B200 C221 105.5(3) . . ? C211 B200 C231 111.2(3) . . ? C221 B200 C231 112.6(3) . . ? C211 B200 C241 110.4(3) . . ? C221 B200 C241 109.2(3) . . ? C231 B200 C241 108.0(3) . . ? C212 C211 C216 114.9(4) . . ? C212 C211 B200 123.3(3) . . ? C216 C211 B200 121.6(3) . . ? C213 C212 C211 122.8(4) . . ? C214 C213 C212 119.7(5) . . ? C215 C214 C213 119.7(4) . . ? C214 C215 C216 119.4(4) . . ? C215 C216 C211 123.3(4) . . ? C226 C221 C222 113.8(3) . . ? C226 C221 B200 126.1(3) . . ? C222 C221 B200 120.1(3) . . ? C223 C222 C221 122.6(3) . . ? C224 C223 C222 120.9(3) . . ? C223 C224 C225 118.9(4) . . ? C224 C225 C226 120.2(4) . . ? C225 C226 C221 123.5(3) . . ? C236 C231 C232 113.6(3) . . ? C236 C231 B200 125.3(3) . . ? C232 C231 B200 121.0(3) . . ? C233 C232 C231 123.4(3) . . ? C234 C233 C232 120.2(4) . . ? C235 C234 C233 118.4(4) . . ? C234 C235 C236 121.1(4) . . ? C235 C236 C231 123.2(4) . . ? C246 C241 C242 114.1(3) . . ? C246 C241 B200 121.8(3) . . ? C242 C241 B200 124.1(3) . . ? C243 C242 C241 123.5(3) . . ? C244 C243 C242 120.0(3) . . ? C245 C244 C243 118.4(3) . . ? C244 C245 C246 120.5(3) . . ? C245 C246 C241 123.5(3) . . ? O313 C312 C311 100.3(13) . . ? C312 O313 C314 102.4(10) . . ? C315 C314 O313 106.8(11) . . ? O300 C300 C301 123.0(10) . . ? O300 C300 C302 120.7(12) . . ? C301 C300 C302 114.6(13) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.553 _refine_diff_density_min -1.018 _refine_diff_density_rms 0.068 #=END data_push _database_code_CSD 177768 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H42 B2 N15 Nd O5' _chemical_formula_weight 954.73 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' '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 10.3989(12) _cell_length_b 14.3209(15) _cell_length_c 15.8589(15) _cell_angle_alpha 112.795(11) _cell_angle_beta 91.777(7) _cell_angle_gamma 98.120(8) _cell_volume 2145.9(4) _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 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.478 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 970 _exptl_absorpt_coefficient_mu 1.271 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7852 _exptl_absorpt_correction_T_max 0.8835 _exptl_absorpt_process_details ? _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 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 11976 _diffrn_reflns_av_R_equivalents 0.0334 _diffrn_reflns_av_sigmaI/netI 0.0969 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9184 _reflns_number_gt 6705 _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^)+(0.0298P)^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 9184 _refine_ls_number_parameters 584 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0792 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.0845 _refine_ls_wR_factor_gt 0.0754 _refine_ls_goodness_of_fit_ref 0.961 _refine_ls_restrained_S_all 0.961 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.16971(2) 0.63191(2) 0.301000(17) 0.02256(7) Uani 1 1 d . . . N1 N -0.0647(4) 0.4591(3) 0.2332(2) 0.0321(9) Uani 1 1 d . . . O1 O 0.0500(3) 0.4398(2) 0.2362(2) 0.0386(8) Uani 1 1 d . . . O2 O -0.0749(3) 0.5520(2) 0.2578(2) 0.0423(8) Uani 1 1 d . . . O3 O -0.1605(3) 0.3903(2) 0.2086(2) 0.0455(9) Uani 1 1 d . . . B1 B -0.0552(5) 0.8150(4) 0.2649(4) 0.0390(14) Uani 1 1 d . . . H1A H -0.1160 0.7679 0.2831 0.047 Uiso 1 1 calc R . . H1B H -0.1046 0.8646 0.2549 0.047 Uiso 1 1 calc R . . N11 N 0.1399(3) 0.8225(3) 0.3689(2) 0.0276(8) Uani 1 1 d . . . C12 C 0.2182(4) 0.8950(3) 0.4401(3) 0.0260(9) Uani 1 1 d . . . C13 C 0.1847(5) 0.9908(4) 0.4591(4) 0.0426(13) Uani 1 1 d . . . H13 H 0.2240 1.0546 0.5059 0.051 Uiso 1 1 calc R . . C14 C 0.0824(5) 0.9732(4) 0.3957(3) 0.0402(12) Uani 1 1 d . . . H14 H 0.0373 1.0243 0.3907 0.048 Uiso 1 1 calc R . . N15 N 0.0556(3) 0.8729(3) 0.3419(3) 0.0300(9) Uani 1 1 d . . . N21 N 0.3295(3) 0.7635(3) 0.4506(2) 0.0252(8) Uani 1 1 d . . . C22 C 0.3210(4) 0.8651(3) 0.4856(3) 0.0284(10) Uani 1 1 d . . . C23 C 0.4044(5) 0.9366(4) 0.5598(3) 0.0414(12) Uani 1 1 d . . . H23 H 0.3972 1.0073 0.5819 0.050 Uiso 1 1 calc R . . C24 C 0.4976(5) 0.9042(4) 0.6010(3) 0.0460(13) Uani 1 1 d . . . H24 H 0.5551 0.9519 0.6518 0.055 Uiso 1 1 calc R . . C25 C 0.5050(4) 0.8020(4) 0.5671(3) 0.0341(11) Uani 1 1 d . . . H25 H 0.5676 0.7775 0.5946 0.041 Uiso 1 1 calc R . . C26 C 0.4216(4) 0.7347(3) 0.4931(3) 0.0287(10) Uani 1 1 d . . . H26 H 0.4290 0.6640 0.4704 0.034 Uiso 1 1 calc R . . N31 N 0.0716(3) 0.6783(3) 0.1706(2) 0.0310(9) Uani 1 1 d . . . C32 C 0.1070(4) 0.6396(4) 0.0844(3) 0.0340(11) Uani 1 1 d . . . C33 C 0.0574(6) 0.6891(4) 0.0329(4) 0.0517(15) Uani 1 1 d . . . H33 H 0.0674 0.6767 -0.0297 0.062 Uiso 1 1 calc R . . C34 C -0.0083(5) 0.7588(4) 0.0922(4) 0.0494(14) Uani 1 1 d . . . H34 H -0.0537 0.8044 0.0775 0.059 Uiso 1 1 calc R . . N35 N 0.0009(4) 0.7532(3) 0.1753(3) 0.0354(9) Uani 1 1 d . . . N41 N 0.2085(4) 0.5223(3) 0.1238(2) 0.0331(9) Uani 1 1 d . . . C42 C 0.1838(5) 0.5576(4) 0.0584(3) 0.0371(11) Uani 1 1 d . . . C43 C 0.2318(6) 0.5177(5) -0.0276(4) 0.0624(17) Uani 1 1 d . . . H43 H 0.2149 0.5446 -0.0722 0.075 Uiso 1 1 calc R . . C44 C 0.3025(7) 0.4404(5) -0.0472(4) 0.076(2) Uani 1 1 d . . . H44 H 0.3373 0.4143 -0.1049 0.091 Uiso 1 1 calc R . . C45 C 0.3234(6) 0.4004(4) 0.0166(4) 0.0595(16) Uani 1 1 d . . . H45 H 0.3701 0.3447 0.0034 0.071 Uiso 1 1 calc R . . C46 C 0.2749(5) 0.4428(4) 0.1004(3) 0.0406(12) Uani 1 1 d . . . H46 H 0.2890 0.4145 0.1444 0.049 Uiso 1 1 calc R . . B2 B 0.3544(5) 0.4206(4) 0.3278(4) 0.0322(12) Uani 1 1 d . . . H2A H 0.4066 0.3733 0.3393 0.039 Uiso 1 1 calc R . . H2B H 0.2866 0.3796 0.2765 0.039 Uiso 1 1 calc R . . N51 N 0.2034(3) 0.5424(3) 0.4144(2) 0.0246(8) Uani 1 1 d . . . C52 C 0.1622(4) 0.5774(3) 0.4992(3) 0.0262(9) Uani 1 1 d . . . C53 C 0.2203(4) 0.5372(3) 0.5548(3) 0.0303(10) Uani 1 1 d . . . H53 H 0.2071 0.5488 0.6169 0.036 Uiso 1 1 calc R . . C54 C 0.3017(4) 0.4766(3) 0.4993(3) 0.0299(10) Uani 1 1 d . . . H54 H 0.3571 0.4388 0.5173 0.036 Uiso 1 1 calc R . . N55 N 0.2898(3) 0.4796(3) 0.4154(2) 0.0265(8) Uani 1 1 d . . . N61 N 0.0306(3) 0.6744(3) 0.4508(2) 0.0271(8) Uani 1 1 d . . . C62 C 0.0638(4) 0.6447(3) 0.5187(3) 0.0276(10) Uani 1 1 d . . . C63 C 0.0073(4) 0.6736(3) 0.6013(3) 0.0323(11) Uani 1 1 d . . . H63 H 0.0355 0.6532 0.6482 0.039 Uiso 1 1 calc R . . C64 C -0.0904(5) 0.7323(3) 0.6142(3) 0.0395(12) Uani 1 1 d . . . H64 H -0.1309 0.7529 0.6699 0.047 Uiso 1 1 calc R . . C65 C -0.1281(4) 0.7606(3) 0.5444(3) 0.0386(12) Uani 1 1 d . . . H65 H -0.1964 0.7998 0.5509 0.046 Uiso 1 1 calc R . . C66 C -0.0651(4) 0.7312(3) 0.4652(3) 0.0367(11) Uani 1 1 d . . . H66 H -0.0909 0.7522 0.4182 0.044 Uiso 1 1 calc R . . N71 N 0.3973(3) 0.5785(3) 0.2892(2) 0.0249(8) Uani 1 1 d . . . C72 C 0.5005(4) 0.6329(3) 0.2703(3) 0.0258(10) Uani 1 1 d . . . C73 C 0.6126(4) 0.5913(4) 0.2717(3) 0.0333(11) Uani 1 1 d . . . H73 H 0.6981 0.6153 0.2612 0.040 Uiso 1 1 calc R . . C74 C 0.5715(4) 0.5075(4) 0.2919(3) 0.0325(11) Uani 1 1 d . . . H74 H 0.6254 0.4614 0.2972 0.039 Uiso 1 1 calc R . . N75 N 0.4436(3) 0.5006(3) 0.3029(2) 0.0257(8) Uani 1 1 d . . . N81 N 0.3593(3) 0.7430(3) 0.2485(2) 0.0269(8) Uani 1 1 d . . . C82 C 0.4815(4) 0.7208(3) 0.2474(3) 0.0257(9) Uani 1 1 d . . . C83 C 0.5856(4) 0.7756(4) 0.2225(3) 0.0371(11) Uani 1 1 d . . . H83 H 0.6712 0.7599 0.2244 0.044 Uiso 1 1 calc R . . C84 C 0.5616(5) 0.8525(4) 0.1952(3) 0.0402(12) Uani 1 1 d . . . H84 H 0.6302 0.8896 0.1768 0.048 Uiso 1 1 calc R . . C85 C 0.4379(4) 0.8749(3) 0.1951(3) 0.0345(11) Uani 1 1 d . . . H85 H 0.4192 0.9274 0.1764 0.041 Uiso 1 1 calc R . . C86 C 0.3411(4) 0.8198(3) 0.2225(3) 0.0299(10) Uani 1 1 d . . . H86 H 0.2560 0.8369 0.2231 0.036 Uiso 1 1 calc R . . C101 C 0.6590(9) 0.0511(8) 0.0490(7) 0.118(4) Uani 1 1 d . . . H101 H 0.6552 0.0402 -0.0141 0.142 Uiso 1 1 calc R . . N101 N 0.6286(6) 0.1405(5) 0.1067(4) 0.0841(19) Uani 1 1 d . . . O101 O 0.6916(6) -0.0190(5) 0.0679(4) 0.128(2) Uani 1 1 d . . . C102 C 0.6332(9) 0.1619(6) 0.2037(5) 0.122(3) Uani 1 1 d . . . H10D H 0.5441 0.1565 0.2219 0.183 Uiso 1 1 calc R . . H10E H 0.6806 0.2315 0.2388 0.183 Uiso 1 1 calc R . . H10F H 0.6780 0.1121 0.2162 0.183 Uiso 1 1 calc R . . C103 C 0.5870(8) 0.2142(6) 0.0736(5) 0.099(3) Uani 1 1 d . . . H10A H 0.5864 0.1874 0.0066 0.148 Uiso 1 1 calc R . . H10B H 0.6476 0.2794 0.1011 0.148 Uiso 1 1 calc R . . H10C H 0.4990 0.2254 0.0909 0.148 Uiso 1 1 calc R . . N111 N 0.1099(6) 0.1079(4) 0.1487(3) 0.0643(14) Uani 1 1 d . . . O111 O 0.2860(7) 0.0683(5) 0.2038(4) 0.131(2) Uani 1 1 d . . . C111 C 0.2385(13) 0.1189(9) 0.1671(7) 0.073(4) Uani 0.662(18) 1 d P A 1 H111 H 0.2948 0.1668 0.1515 0.088 Uiso 0.662(18) 1 calc PR A 1 C112 C 0.0175(15) 0.0438(9) 0.1772(8) 0.094(6) Uani 0.662(18) 1 d P A 1 H11D H 0.0644 0.0105 0.2093 0.141 Uiso 0.662(18) 1 calc PR A 1 H11E H -0.0357 -0.0088 0.1232 0.141 Uiso 0.662(18) 1 calc PR A 1 H11F H -0.0391 0.0859 0.2187 0.141 Uiso 0.662(18) 1 calc PR A 1 C113 C 0.0524(14) 0.1702(9) 0.1086(9) 0.073(4) Uani 0.662(18) 1 d P A 1 H11A H 0.1216 0.2096 0.0893 0.110 Uiso 0.662(18) 1 calc PR A 1 H11B H 0.0053 0.2176 0.1543 0.110 Uiso 0.662(18) 1 calc PR A 1 H11C H -0.0084 0.1254 0.0551 0.110 Uiso 0.662(18) 1 calc PR A 1 C121 C 0.153(4) 0.044(2) 0.183(2) 0.120(13) Uani 0.338(18) 1 d P A 2 H121 H 0.0991 -0.0101 0.1918 0.143 Uiso 0.338(18) 1 calc PR A 2 C122 C 0.178(4) 0.165(2) 0.1078(18) 0.141(18) Uani 0.338(18) 1 d P A 2 H12A H 0.2636 0.1965 0.1417 0.212 Uiso 0.338(18) 1 calc PR A 2 H12B H 0.1294 0.2197 0.1083 0.212 Uiso 0.338(18) 1 calc PR A 2 H12C H 0.1880 0.1213 0.0442 0.212 Uiso 0.338(18) 1 calc PR A 2 C123 C -0.042(3) 0.095(4) 0.133(3) 0.23(3) Uani 0.338(18) 1 d P A 2 H12D H -0.0822 0.0474 0.1593 0.348 Uiso 0.338(18) 1 calc PR A 2 H12E H -0.0686 0.0676 0.0673 0.348 Uiso 0.338(18) 1 calc PR A 2 H12F H -0.0693 0.1619 0.1636 0.348 Uiso 0.338(18) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.02274(12) 0.02587(12) 0.02209(12) 0.01289(9) 0.00032(8) 0.00398(8) N1 0.037(2) 0.041(2) 0.0180(19) 0.0143(18) -0.0026(17) -0.0040(19) O1 0.0360(19) 0.0327(18) 0.047(2) 0.0154(16) -0.0011(16) 0.0065(15) O2 0.0333(19) 0.0322(19) 0.059(2) 0.0155(17) 0.0008(17) 0.0049(15) O3 0.0350(19) 0.045(2) 0.047(2) 0.0165(19) -0.0052(16) -0.0160(17) B1 0.028(3) 0.044(3) 0.060(4) 0.036(3) 0.000(3) 0.008(3) N11 0.028(2) 0.032(2) 0.028(2) 0.0169(18) 0.0049(16) 0.0067(16) C12 0.030(2) 0.025(2) 0.024(2) 0.011(2) 0.0051(19) 0.0058(19) C13 0.056(3) 0.023(3) 0.047(3) 0.011(2) 0.004(3) 0.011(2) C14 0.047(3) 0.036(3) 0.047(3) 0.023(3) 0.005(3) 0.017(2) N15 0.029(2) 0.032(2) 0.039(2) 0.0231(19) 0.0032(18) 0.0104(17) N21 0.029(2) 0.026(2) 0.0208(19) 0.0088(16) 0.0040(16) 0.0040(16) C22 0.029(2) 0.029(3) 0.026(2) 0.011(2) 0.000(2) 0.0005(19) C23 0.051(3) 0.027(3) 0.039(3) 0.007(2) -0.005(3) 0.004(2) C24 0.048(3) 0.045(3) 0.035(3) 0.009(3) -0.012(2) -0.001(3) C25 0.034(3) 0.038(3) 0.029(3) 0.014(2) -0.005(2) 0.005(2) C26 0.029(2) 0.032(3) 0.026(2) 0.013(2) 0.000(2) 0.006(2) N31 0.030(2) 0.036(2) 0.031(2) 0.0195(19) -0.0081(17) 0.0013(17) C32 0.043(3) 0.037(3) 0.024(2) 0.018(2) -0.008(2) -0.004(2) C33 0.086(4) 0.045(3) 0.032(3) 0.024(3) -0.007(3) 0.015(3) C34 0.064(4) 0.048(3) 0.048(3) 0.032(3) -0.013(3) 0.008(3) N35 0.033(2) 0.037(2) 0.042(3) 0.025(2) -0.0070(19) 0.0004(18) N41 0.045(2) 0.033(2) 0.021(2) 0.0131(18) -0.0050(17) 0.0005(18) C42 0.050(3) 0.036(3) 0.024(3) 0.014(2) -0.006(2) -0.002(2) C43 0.107(5) 0.065(4) 0.030(3) 0.029(3) 0.011(3) 0.029(4) C44 0.136(6) 0.075(5) 0.031(3) 0.026(3) 0.029(4) 0.046(4) C45 0.088(5) 0.060(4) 0.033(3) 0.015(3) 0.012(3) 0.030(3) C46 0.055(3) 0.038(3) 0.025(3) 0.010(2) -0.001(2) 0.007(2) B2 0.043(3) 0.030(3) 0.030(3) 0.017(2) 0.000(3) 0.009(2) N51 0.028(2) 0.028(2) 0.0232(19) 0.0148(16) 0.0013(16) 0.0061(16) C52 0.028(2) 0.030(2) 0.023(2) 0.014(2) 0.0038(19) 0.0019(19) C53 0.036(3) 0.039(3) 0.022(2) 0.018(2) 0.001(2) 0.007(2) C54 0.035(3) 0.035(3) 0.026(2) 0.019(2) -0.001(2) 0.006(2) N55 0.030(2) 0.029(2) 0.027(2) 0.0178(17) 0.0027(16) 0.0070(16) N61 0.0258(19) 0.029(2) 0.032(2) 0.0184(17) 0.0040(16) 0.0046(16) C62 0.030(2) 0.026(2) 0.027(2) 0.013(2) 0.0002(19) -0.0006(19) C63 0.041(3) 0.030(3) 0.027(3) 0.013(2) 0.008(2) 0.004(2) C64 0.049(3) 0.032(3) 0.038(3) 0.013(2) 0.020(2) 0.008(2) C65 0.037(3) 0.034(3) 0.053(3) 0.023(3) 0.015(2) 0.011(2) C66 0.035(3) 0.037(3) 0.048(3) 0.026(2) 0.010(2) 0.010(2) N71 0.031(2) 0.0247(19) 0.0217(19) 0.0112(16) 0.0008(16) 0.0080(16) C72 0.022(2) 0.032(2) 0.022(2) 0.011(2) 0.0020(18) 0.0038(19) C73 0.025(2) 0.052(3) 0.030(3) 0.022(2) 0.005(2) 0.012(2) C74 0.031(3) 0.047(3) 0.023(2) 0.014(2) 0.002(2) 0.018(2) N75 0.031(2) 0.028(2) 0.0233(19) 0.0132(16) 0.0026(16) 0.0123(16) N81 0.029(2) 0.029(2) 0.0228(19) 0.0120(17) 0.0001(16) 0.0036(16) C82 0.024(2) 0.029(2) 0.022(2) 0.0086(19) 0.0016(18) 0.0022(19) C83 0.030(3) 0.038(3) 0.044(3) 0.018(2) 0.005(2) 0.001(2) C84 0.040(3) 0.037(3) 0.044(3) 0.019(3) 0.010(2) -0.004(2) C85 0.040(3) 0.029(3) 0.037(3) 0.017(2) 0.005(2) 0.003(2) C86 0.030(2) 0.033(3) 0.032(3) 0.017(2) 0.001(2) 0.007(2) C101 0.151(9) 0.101(8) 0.091(7) 0.050(7) -0.008(6) -0.044(7) N101 0.097(5) 0.081(5) 0.056(4) 0.025(4) -0.008(3) -0.030(4) O101 0.160(6) 0.108(5) 0.116(5) 0.058(4) 0.007(4) -0.016(4) C102 0.163(8) 0.127(7) 0.062(5) 0.044(5) 0.007(5) -0.036(6) C103 0.124(7) 0.087(6) 0.070(5) 0.027(5) -0.020(5) -0.011(5) N111 0.093(5) 0.055(3) 0.052(3) 0.027(3) 0.008(3) 0.020(3) O111 0.147(6) 0.119(5) 0.133(5) 0.036(4) -0.010(5) 0.087(5) C111 0.092(10) 0.066(8) 0.069(8) 0.024(6) 0.017(7) 0.042(7) C112 0.134(15) 0.076(8) 0.085(9) 0.056(7) -0.013(9) -0.011(8) C113 0.084(10) 0.075(8) 0.072(8) 0.048(7) -0.009(7) 0.002(7) C121 0.15(3) 0.10(2) 0.16(3) 0.09(2) 0.06(2) 0.09(2) C122 0.25(5) 0.10(2) 0.070(18) 0.041(17) 0.02(3) -0.02(3) C123 0.10(3) 0.35(8) 0.17(4) 0.01(5) -0.04(3) 0.08(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 N71 2.578(3) . ? Nd1 N11 2.586(3) . ? Nd1 O2 2.590(3) . ? Nd1 N51 2.622(3) . ? Nd1 N31 2.624(3) . ? Nd1 O1 2.633(3) . ? Nd1 N21 2.711(4) . ? Nd1 N81 2.711(3) . ? Nd1 N41 2.712(4) . ? Nd1 N61 2.729(3) . ? N1 O3 1.232(4) . ? N1 O2 1.254(4) . ? N1 O1 1.265(4) . ? B1 N35 1.538(7) . ? B1 N15 1.538(7) . ? N11 C12 1.346(5) . ? N11 N15 1.366(4) . ? C12 C13 1.384(6) . ? C12 C22 1.472(6) . ? C13 C14 1.366(7) . ? C14 N15 1.339(6) . ? N21 C26 1.352(5) . ? N21 C22 1.358(5) . ? C22 C23 1.393(6) . ? C23 C24 1.380(6) . ? C24 C25 1.365(6) . ? C25 C26 1.372(6) . ? N31 C32 1.347(5) . ? N31 N35 1.363(5) . ? C32 C33 1.400(6) . ? C32 C42 1.448(6) . ? C33 C34 1.361(7) . ? C34 N35 1.352(6) . ? N41 C46 1.348(6) . ? N41 C42 1.352(5) . ? C42 C43 1.398(7) . ? C43 C44 1.356(8) . ? C44 C45 1.368(7) . ? C45 C46 1.375(7) . ? B2 N75 1.549(6) . ? B2 N55 1.550(6) . ? N51 C52 1.349(5) . ? N51 N55 1.362(4) . ? C52 C53 1.391(5) . ? C52 C62 1.463(6) . ? C53 C54 1.380(6) . ? C54 N55 1.351(5) . ? N61 C66 1.343(5) . ? N61 C62 1.353(5) . ? C62 C63 1.388(6) . ? C63 C64 1.379(6) . ? C64 C65 1.381(6) . ? C65 C66 1.380(6) . ? N71 C72 1.347(5) . ? N71 N75 1.363(4) . ? C72 C73 1.385(6) . ? C72 C82 1.475(5) . ? C73 C74 1.375(6) . ? C74 N75 1.342(5) . ? N81 C86 1.350(5) . ? N81 C82 1.352(5) . ? C82 C83 1.403(5) . ? C83 C84 1.380(6) . ? C84 C85 1.369(6) . ? C85 C86 1.376(6) . ? C101 O101 1.240(10) . ? C101 N101 1.342(11) . ? N101 C102 1.446(8) . ? N101 C103 1.457(8) . ? N111 C111 1.334(12) . ? N111 C121 1.35(2) . ? N111 C122 1.37(3) . ? N111 C112 1.440(12) . ? N111 C113 1.457(11) . ? N111 C123 1.56(3) . ? O111 C111 1.233(11) . ? O111 C121 1.37(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 N71 Nd1 N11 121.99(11) . . ? N71 Nd1 O2 140.56(10) . . ? N11 Nd1 O2 97.40(10) . . ? N71 Nd1 N51 70.57(10) . . ? N11 Nd1 N51 118.41(10) . . ? O2 Nd1 N51 93.81(10) . . ? N71 Nd1 N31 119.07(11) . . ? N11 Nd1 N31 70.61(11) . . ? O2 Nd1 N31 69.34(10) . . ? N51 Nd1 N31 162.38(10) . . ? N71 Nd1 O1 92.55(10) . . ? N11 Nd1 O1 145.35(10) . . ? O2 Nd1 O1 48.32(10) . . ? N51 Nd1 O1 67.53(10) . . ? N31 Nd1 O1 96.34(10) . . ? N71 Nd1 N21 71.05(10) . . ? N11 Nd1 N21 61.94(11) . . ? O2 Nd1 N21 138.84(10) . . ? N51 Nd1 N21 70.38(10) . . ? N31 Nd1 N21 125.71(10) . . ? O1 Nd1 N21 137.84(10) . . ? N71 Nd1 N81 62.49(10) . . ? N11 Nd1 N81 70.97(10) . . ? O2 Nd1 N81 139.58(10) . . ? N51 Nd1 N81 126.10(10) . . ? N31 Nd1 N81 70.29(10) . . ? O1 Nd1 N81 136.17(10) . . ? N21 Nd1 N81 70.58(10) . . ? N71 Nd1 N41 68.94(11) . . ? N11 Nd1 N41 125.52(10) . . ? O2 Nd1 N41 87.39(11) . . ? N51 Nd1 N41 115.31(11) . . ? N31 Nd1 N41 60.61(11) . . ? O1 Nd1 N41 66.29(10) . . ? N21 Nd1 N41 133.77(10) . . ? N81 Nd1 N41 71.03(10) . . ? N71 Nd1 N61 125.91(10) . . ? N11 Nd1 N61 68.77(10) . . ? O2 Nd1 N61 67.44(11) . . ? N51 Nd1 N61 60.67(10) . . ? N31 Nd1 N61 114.33(11) . . ? O1 Nd1 N61 89.60(10) . . ? N21 Nd1 N61 71.77(10) . . ? N81 Nd1 N61 134.17(10) . . ? N41 Nd1 N61 153.41(11) . . ? O3 N1 O2 122.3(4) . . ? O3 N1 O1 121.5(4) . . ? O2 N1 O1 116.2(4) . . ? N1 O1 Nd1 96.5(2) . . ? N1 O2 Nd1 99.0(2) . . ? N35 B1 N15 110.2(4) . . ? C12 N11 N15 105.9(3) . . ? C12 N11 Nd1 122.8(3) . . ? N15 N11 Nd1 131.2(3) . . ? N11 C12 C13 110.7(4) . . ? N11 C12 C22 119.4(4) . . ? C13 C12 C22 129.9(4) . . ? C14 C13 C12 104.6(4) . . ? N15 C14 C13 109.5(4) . . ? C14 N15 N11 109.2(4) . . ? C14 N15 B1 129.0(4) . . ? N11 N15 B1 121.7(4) . . ? C26 N21 C22 116.5(4) . . ? C26 N21 Nd1 123.7(3) . . ? C22 N21 Nd1 119.8(3) . . ? N21 C22 C23 122.1(4) . . ? N21 C22 C12 115.9(4) . . ? C23 C22 C12 122.0(4) . . ? C24 C23 C22 119.6(4) . . ? C25 C24 C23 118.4(5) . . ? C24 C25 C26 119.7(4) . . ? N21 C26 C25 123.6(4) . . ? C32 N31 N35 106.7(3) . . ? C32 N31 Nd1 121.7(3) . . ? N35 N31 Nd1 130.6(3) . . ? N31 C32 C33 110.0(4) . . ? N31 C32 C42 119.5(4) . . ? C33 C32 C42 130.5(4) . . ? C34 C33 C32 104.8(4) . . ? N35 C34 C33 109.6(4) . . ? C34 N35 N31 108.9(4) . . ? C34 N35 B1 130.1(4) . . ? N31 N35 B1 121.0(3) . . ? C46 N41 C42 116.8(4) . . ? C46 N41 Nd1 121.8(3) . . ? C42 N41 Nd1 120.2(3) . . ? N41 C42 C43 121.4(5) . . ? N41 C42 C32 115.4(4) . . ? C43 C42 C32 123.2(4) . . ? C44 C43 C42 119.9(5) . . ? C43 C44 C45 119.6(5) . . ? C44 C45 C46 118.3(5) . . ? N41 C46 C45 123.9(5) . . ? N75 B2 N55 108.0(4) . . ? C52 N51 N55 105.9(3) . . ? C52 N51 Nd1 121.6(3) . . ? N55 N51 Nd1 129.8(2) . . ? N51 C52 C53 111.2(4) . . ? N51 C52 C62 118.9(3) . . ? C53 C52 C62 129.9(4) . . ? C54 C53 C52 104.2(4) . . ? N55 C54 C53 109.0(4) . . ? C54 N55 N51 109.6(3) . . ? C54 N55 B2 129.1(4) . . ? N51 N55 B2 121.2(3) . . ? C66 N61 C62 116.6(4) . . ? C66 N61 Nd1 123.2(3) . . ? C62 N61 Nd1 120.0(3) . . ? N61 C62 C63 123.1(4) . . ? N61 C62 C52 115.7(4) . . ? C63 C62 C52 121.2(4) . . ? C64 C63 C62 118.9(4) . . ? C63 C64 C65 118.7(4) . . ? C66 C65 C64 119.0(4) . . ? N61 C66 C65 123.6(4) . . ? C72 N71 N75 105.8(3) . . ? C72 N71 Nd1 122.3(3) . . ? N75 N71 Nd1 131.9(2) . . ? N71 C72 C73 111.3(4) . . ? N71 C72 C82 119.4(3) . . ? C73 C72 C82 129.3(4) . . ? C74 C73 C72 103.9(4) . . ? N75 C74 C73 109.7(4) . . ? C74 N75 N71 109.3(3) . . ? C74 N75 B2 128.7(4) . . ? N71 N75 B2 122.0(3) . . ? C86 N81 C82 116.6(3) . . ? C86 N81 Nd1 124.7(3) . . ? C82 N81 Nd1 118.7(2) . . ? N81 C82 C83 122.3(4) . . ? N81 C82 C72 116.9(3) . . ? C83 C82 C72 120.8(4) . . ? C84 C83 C82 118.9(4) . . ? C85 C84 C83 119.3(4) . . ? C84 C85 C86 118.7(4) . . ? N81 C86 C85 124.2(4) . . ? O101 C101 N101 127.9(9) . . ? C101 N101 C102 118.7(8) . . ? C101 N101 C103 121.7(7) . . ? C102 N101 C103 119.6(7) . . ? C111 N111 C121 62.8(16) . . ? C111 N111 C122 68.2(18) . . ? C121 N111 C122 129(2) . . ? C111 N111 C112 122.6(8) . . ? C121 N111 C112 60.6(14) . . ? C122 N111 C112 168.2(18) . . ? C111 N111 C113 122.0(8) . . ? C121 N111 C113 174.9(19) . . ? C122 N111 C113 55.3(16) . . ? C112 N111 C113 114.9(9) . . ? C111 N111 C123 176.4(19) . . ? C121 N111 C123 115(3) . . ? C122 N111 C123 115(2) . . ? C112 N111 C123 55(2) . . ? C113 N111 C123 60.5(19) . . ? C111 O111 C121 64.6(11) . . ? O111 C111 N111 121.6(11) . . ? N111 C121 O111 111(2) . . ? _diffrn_measured_fraction_theta_max 0.932 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.932 _refine_diff_density_max 0.576 _refine_diff_density_min -0.852 _refine_diff_density_rms 0.107 #=END