# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 #=============================================================================== _audit_creation_date 2011-08-05 # 1. SUBMISSION DETAILS _publ_contact_author_name 'Francois Nief' _publ_contact_author_address ;Laboratoire DCPH Ecole Polytechnique Route de Saclay F91128 Palaiseau France ; _publ_contact_author_email francois.nief@polytechnique.edu _publ_contact_author_phone 330169334401 _publ_contact_author_fax 330169334440 _publ_contact_letter ; Please consider this CIF submission for publication as a new structure paper in CHEMICAL COMMUNICATIONS. The figures, chemical structure diagram (scheme), Transfert of Copyright Agreement form and structure factors will be sent on receipt of your acknowledgement letter ; #=============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #=============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis and structure of divalent thulium borohydrides, and their application in 'epsilon'-caprolactone polymerisation ; _publ_author_address ; a) Ecole Polytechnique, CNRS, Laboratoire Heteroelements et Coordination, Palaiseau, France. b) Universite de Lille Nord de France, Ecole Nationale Superieure de Chimie de Lille, CNRS, Unite de Catalyse et Chimie du Solide, Villeneuve d'Ascq, France. c) Universite de Toulouse, Institut National des Sciences Appliquees, CNRS, Laboratoire de Physique et Chimie de Nano-Objets, Toulouse, France. d) University of Alberta, Department of Chemistry, Edmonton, Alberta, Canada. ; #=============================================================================== # 4. TEXT _publ_section_abstract ; ? ; _publ_section_comment ; ; _publ_section_exptl_prep ;All structures were solved using SIR97 (Altomare et al.) and refined with SHELXL97 (Sheldrick). Figures were drawn with Platon (Spek, 1990). ; _publ_section_references ;Altomare, A., Cascarano, G., Giacovazzo, C. & Guagliardi, A. (1993) J. Appl. Cryst. 26, 343-350. Sheldrick, G.M. SHELXL97. Program for crystal structure refinement. University of G\\"ottingen, Germany, 1997. Sluis, P. v.d., Spek, A.L. (1990). Acta Cryst. A46, 194-201. Spek, A.L. (1990). Acta Cryst. A46, C-34. Spek, A. L. J. Appl. Crystallogr. 2003, 36, 7 ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; loop_ _publ_author_name A.Momin F.Bonnet M.Visseaux L.Maron J.Takats M.J.Ferguson ; X.F.Le Goff ; F.Nief #=============================================================================== # If more than one structure is reported, sections 5-10 should be filled in # per structure. For each data set, replace the ? in the data_? line below # by a unique identifier. #=============================================================================== #compound 1 data_amx530 _database_code_depnum_ccdc_archive 'CCDC 837318' #TrackingRef '2011_momin_chem_comm.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H28 B2 O4 Tm' _chemical_formula_sum 'C8 H28 B2 O4 Tm' _chemical_formula_weight 378.85 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tm Tm -0.3139 5.2483 '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 ' _symmetry_space_group_name_Hall '-P 2ybc ' 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 8.734(1) _cell_length_b 12.631(1) _cell_length_c 14.616(1) _cell_angle_alpha 90.00 _cell_angle_beta 102.472(1) _cell_angle_gamma 90.00 _cell_volume 1574.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 3401 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description Block _exptl_crystal_colour Black _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.598 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 748 _exptl_absorpt_coefficient_mu 5.628 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3017 _exptl_absorpt_correction_T_max 0.3990 _exptl_absorpt_process_details 'Denzo/Scalepack (Otwinowski & Minor, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Kappa APEXII CCD' _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 9931 _diffrn_reflns_av_R_equivalents 0.0303 _diffrn_reflns_av_sigmaI/netI 0.0336 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.23 _diffrn_reflns_theta_max 30.03 _reflns_number_total 4549 _reflns_number_gt 4128 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+5.0314P] 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 SHELXL _refine_ls_extinction_coef 0.0004(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4549 _refine_ls_number_parameters 165 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0320 _refine_ls_R_factor_gt 0.0276 _refine_ls_wR_factor_ref 0.0628 _refine_ls_wR_factor_gt 0.0599 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _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 Tm1 Tm 0.150588(17) 0.181013(11) 0.695566(10) 0.02301(6) Uani 1 1 d . . . O1 O 0.3627(3) 0.1242(2) 0.6163(2) 0.0365(6) Uani 1 1 d . . . O2 O 0.1098(3) 0.0052(2) 0.62034(18) 0.0309(5) Uani 1 1 d . . . O3 O 0.2714(3) 0.0596(2) 0.82958(18) 0.0330(6) Uani 1 1 d . . . O4 O -0.0228(3) 0.1424(2) 0.80610(18) 0.0293(5) Uani 1 1 d . . . C1 C 0.4637(6) 0.1943(4) 0.5796(4) 0.0505(12) Uani 1 1 d . . . H1A H 0.5676 0.1619 0.5868 0.076 Uiso 1 1 calc R . . H1B H 0.4730 0.2615 0.6139 0.076 Uiso 1 1 calc R . . H1C H 0.4195 0.2073 0.5130 0.076 Uiso 1 1 calc R . . C2 C 0.3436(5) 0.0260(3) 0.5661(3) 0.0393(9) Uani 1 1 d . . . H2A H 0.4476 -0.0051 0.5659 0.047 Uiso 1 1 calc R . . H2B H 0.2884 0.0382 0.5004 0.047 Uiso 1 1 calc R . . C3 C 0.2510(5) -0.0481(3) 0.6124(3) 0.0370(8) Uani 1 1 d . . . H3A H 0.2258 -0.1133 0.5745 0.044 Uiso 1 1 calc R . . H3B H 0.3120 -0.0681 0.6752 0.044 Uiso 1 1 calc R . . C4 C -0.0012(5) -0.0663(3) 0.6453(3) 0.0377(8) Uani 1 1 d . . . H4A H -0.0280 -0.1212 0.5971 0.057 Uiso 1 1 calc R . . H4B H -0.0961 -0.0274 0.6503 0.057 Uiso 1 1 calc R . . H4C H 0.0444 -0.0994 0.7057 0.057 Uiso 1 1 calc R . . C5 C 0.4367(5) 0.0464(4) 0.8572(3) 0.0485(11) Uani 1 1 d . . . H5A H 0.4823 0.1070 0.8955 0.073 Uiso 1 1 calc R . . H5B H 0.4815 0.0420 0.8014 0.073 Uiso 1 1 calc R . . H5C H 0.4601 -0.0188 0.8939 0.073 Uiso 1 1 calc R . . C6 C 0.2003(5) 0.0685(3) 0.9088(3) 0.0386(9) Uani 1 1 d . . . H6A H 0.2310 0.1364 0.9415 0.046 Uiso 1 1 calc R . . H6B H 0.2370 0.0101 0.9534 0.046 Uiso 1 1 calc R . . C7 C 0.0270(5) 0.0637(3) 0.8769(3) 0.0346(8) Uani 1 1 d . . . H7A H -0.0048 -0.0075 0.8513 0.041 Uiso 1 1 calc R . . H7B H -0.0231 0.0766 0.9305 0.041 Uiso 1 1 calc R . . C8 C -0.1898(5) 0.1569(4) 0.7884(3) 0.0392(9) Uani 1 1 d . . . H8A H -0.2422 0.0895 0.7688 0.059 Uiso 1 1 calc R . . H8B H -0.2215 0.2096 0.7387 0.059 Uiso 1 1 calc R . . H8C H -0.2196 0.1816 0.8457 0.059 Uiso 1 1 calc R . . B1 B -0.0881(5) 0.2598(3) 0.5732(3) 0.0314(8) Uani 1 1 d . . . H1B1 H -0.050(5) 0.308(3) 0.642(3) 0.038 Uiso 1 1 d . . . H2B1 H -0.114(5) 0.171(3) 0.590(3) 0.038 Uiso 1 1 d . . . H3B1 H -0.186(6) 0.296(3) 0.523(3) 0.038 Uiso 1 1 d . . . H4B1 H 0.024(5) 0.260(3) 0.546(3) 0.038 Uiso 1 1 d . . . B2 B 0.3306(6) 0.3391(4) 0.7765(4) 0.0407(11) Uani 1 1 d . . . H1B2 H 0.417(6) 0.276(4) 0.775(3) 0.049 Uiso 1 1 d . . . H2B2 H 0.251(6) 0.303(4) 0.817(4) 0.049 Uiso 1 1 d . . . H3B2 H 0.384(6) 0.413(4) 0.808(3) 0.049 Uiso 1 1 d . . . H4B2 H 0.268(6) 0.353(4) 0.698(4) 0.049 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 Tm1 0.02322(9) 0.02292(9) 0.02387(9) -0.00034(5) 0.00727(5) -0.00027(5) O1 0.0325(14) 0.0435(15) 0.0382(15) 0.0010(12) 0.0181(12) -0.0002(12) O2 0.0310(13) 0.0279(12) 0.0338(14) -0.0034(10) 0.0073(11) 0.0052(10) O3 0.0330(14) 0.0376(14) 0.0280(13) 0.0009(11) 0.0053(10) 0.0076(11) O4 0.0291(13) 0.0302(12) 0.0304(13) 0.0031(10) 0.0106(10) -0.0016(10) C1 0.041(2) 0.068(3) 0.048(3) 0.011(2) 0.023(2) -0.005(2) C2 0.041(2) 0.050(2) 0.0295(18) -0.0005(17) 0.0134(16) 0.0171(18) C3 0.037(2) 0.038(2) 0.0343(19) -0.0073(16) 0.0054(16) 0.0138(17) C4 0.043(2) 0.0300(18) 0.040(2) -0.0047(15) 0.0088(17) 0.0001(16) C5 0.037(2) 0.067(3) 0.038(2) 0.003(2) 0.0016(18) 0.015(2) C6 0.052(2) 0.038(2) 0.0272(18) 0.0025(15) 0.0114(17) 0.0049(18) C7 0.049(2) 0.0301(17) 0.0283(17) 0.0045(14) 0.0156(16) -0.0015(16) C8 0.0275(18) 0.051(2) 0.043(2) -0.0036(19) 0.0184(17) -0.0046(17) B1 0.035(2) 0.0294(19) 0.0278(19) 0.0035(15) 0.0033(16) 0.0052(16) B2 0.029(2) 0.040(2) 0.053(3) -0.011(2) 0.007(2) -0.0114(18) _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 Tm1 O2 2.470(2) . ? Tm1 O4 2.490(2) . ? Tm1 O1 2.494(3) . ? Tm1 O3 2.532(3) . ? Tm1 B1 2.632(4) . ? Tm1 B2 2.656(5) . ? Tm1 H1B1 2.38(4) . ? Tm1 H2B1 2.49(5) . ? Tm1 H4B1 2.44(4) . ? Tm1 H2B2 2.37(5) . ? Tm1 H4B2 2.40(5) . ? O1 C1 1.432(5) . ? O1 C2 1.432(5) . ? O2 C4 1.429(5) . ? O2 C3 1.431(4) . ? O3 C5 1.422(5) . ? O3 C6 1.432(5) . ? O4 C7 1.434(4) . ? O4 C8 1.437(5) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.491(6) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.486(6) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? B1 H1B1 1.16(5) . ? B1 H2B1 1.18(4) . ? B1 H3B1 1.10(5) . ? B1 H4B1 1.14(4) . ? B2 H1B2 1.10(5) . ? B2 H2B2 1.11(5) . ? B2 H3B2 1.10(5) . ? B2 H4B2 1.18(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Tm1 O4 93.62(9) . . ? O2 Tm1 O1 65.46(9) . . ? O4 Tm1 O1 149.59(9) . . ? O2 Tm1 O3 78.20(9) . . ? O4 Tm1 O3 65.77(9) . . ? O1 Tm1 O3 87.59(9) . . ? O2 Tm1 B1 91.19(11) . . ? O4 Tm1 B1 90.65(12) . . ? O1 Tm1 B1 110.62(12) . . ? O3 Tm1 B1 153.07(12) . . ? O2 Tm1 B2 152.74(13) . . ? O4 Tm1 B2 104.05(13) . . ? O1 Tm1 B2 89.75(13) . . ? O3 Tm1 B2 90.17(15) . . ? B1 Tm1 B2 108.91(16) . . ? O2 Tm1 H1B1 115.7(11) . . ? O4 Tm1 H1B1 80.6(11) . . ? O1 Tm1 H1B1 127.6(11) . . ? O3 Tm1 H1B1 144.7(11) . . ? B1 Tm1 H1B1 26.2(11) . . ? B2 Tm1 H1B1 87.9(11) . . ? O2 Tm1 H2B1 69.7(10) . . ? O4 Tm1 H2B1 77.2(10) . . ? O1 Tm1 H2B1 112.4(10) . . ? O3 Tm1 H2B1 128.6(10) . . ? B1 Tm1 H2B1 26.5(10) . . ? B2 Tm1 H2B1 134.1(10) . . ? H1B1 Tm1 H2B1 46.5(14) . . ? O2 Tm1 H4B1 88.6(10) . . ? O4 Tm1 H4B1 116.2(11) . . ? O1 Tm1 H4B1 86.5(11) . . ? O3 Tm1 H4B1 166.8(10) . . ? B1 Tm1 H4B1 25.5(11) . . ? B2 Tm1 H4B1 101.6(10) . . ? H1B1 Tm1 H4B1 43.3(15) . . ? H2B1 Tm1 H4B1 44.5(14) . . ? O2 Tm1 H2B2 155.8(12) . . ? O4 Tm1 H2B2 79.5(12) . . ? O1 Tm1 H2B2 110.2(13) . . ? O3 Tm1 H2B2 77.9(12) . . ? B1 Tm1 H2B2 111.9(12) . . ? B2 Tm1 H2B2 24.6(12) . . ? H1B1 Tm1 H2B2 86.2(16) . . ? H2B1 Tm1 H2B2 129.8(16) . . ? H4B1 Tm1 H2B2 115.3(15) . . ? O2 Tm1 H4B2 147.2(12) . . ? O4 Tm1 H4B2 119.1(12) . . ? O1 Tm1 H4B2 84.8(12) . . ? O3 Tm1 H4B2 115.7(12) . . ? B1 Tm1 H4B2 86.5(12) . . ? B2 Tm1 H4B2 26.3(12) . . ? H1B1 Tm1 H4B2 71.1(16) . . ? H2B1 Tm1 H4B2 113.0(16) . . ? H4B1 Tm1 H4B2 75.5(16) . . ? H2B2 Tm1 H4B2 46.8(16) . . ? C1 O1 C2 110.9(3) . . ? C1 O1 Tm1 125.1(3) . . ? C2 O1 Tm1 118.1(2) . . ? C4 O2 C3 111.6(3) . . ? C4 O2 Tm1 119.7(2) . . ? C3 O2 Tm1 114.5(2) . . ? C5 O3 C6 111.7(3) . . ? C5 O3 Tm1 121.2(3) . . ? C6 O3 Tm1 113.4(2) . . ? C7 O4 C8 110.9(3) . . ? C7 O4 Tm1 118.2(2) . . ? C8 O4 Tm1 126.5(2) . . ? O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 109.1(3) . . ? O1 C2 H2A 109.9 . . ? C3 C2 H2A 109.9 . . ? O1 C2 H2B 109.9 . . ? C3 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? O2 C3 C2 107.6(3) . . ? O2 C3 H3A 110.2 . . ? C2 C3 H3A 110.2 . . ? O2 C3 H3B 110.2 . . ? C2 C3 H3B 110.2 . . ? H3A C3 H3B 108.5 . . ? O2 C4 H4A 109.5 . . ? O2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? O2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O3 C5 H5A 109.5 . . ? O3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? O3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O3 C6 C7 109.5(3) . . ? O3 C6 H6A 109.8 . . ? C7 C6 H6A 109.8 . . ? O3 C6 H6B 109.8 . . ? C7 C6 H6B 109.8 . . ? H6A C6 H6B 108.2 . . ? O4 C7 C6 109.1(3) . . ? O4 C7 H7A 109.9 . . ? C6 C7 H7A 109.9 . . ? O4 C7 H7B 109.9 . . ? C6 C7 H7B 109.9 . . ? H7A C7 H7B 108.3 . . ? O4 C8 H8A 109.5 . . ? O4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Tm1 B1 H1B1 65(2) . . ? Tm1 B1 H2B1 70(2) . . ? H1B1 B1 H2B1 110(3) . . ? Tm1 B1 H3B1 178(2) . . ? H1B1 B1 H3B1 113(3) . . ? H2B1 B1 H3B1 112(3) . . ? Tm1 B1 H4B1 68(2) . . ? H1B1 B1 H4B1 101(3) . . ? H2B1 B1 H4B1 107(3) . . ? H3B1 B1 H4B1 112(3) . . ? Tm1 B2 H1B2 78(3) . . ? Tm1 B2 H2B2 63(3) . . ? H1B2 B2 H2B2 103(4) . . ? Tm1 B2 H3B2 169(3) . . ? H1B2 B2 H3B2 113(4) . . ? H2B2 B2 H3B2 112(4) . . ? Tm1 B2 H4B2 65(2) . . ? H1B2 B2 H4B2 106(3) . . ? H2B2 B2 H4B2 112(4) . . ? H3B2 B2 H4B2 110(3) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.081 _refine_diff_density_min -0.861 _refine_diff_density_rms 0.125 #===END #compound 2 data_tak1108 _database_code_depnum_ccdc_archive 'CCDC 837319' #TrackingRef '2011_momin_chem_comm.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H52 B2 N6 O Tm' _chemical_formula_sum 'C28 H52 B2 N6 O Tm' _chemical_formula_weight 679.31 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' Tm Tm -0.3139 5.2483 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 12.2792(8) _cell_length_b 15.4471(10) _cell_length_c 17.2852(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3278.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9238 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 27.44 _exptl_crystal_description fragment _exptl_crystal_colour green _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.376 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1396 _exptl_absorpt_coefficient_mu 2.735 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.4335 _exptl_absorpt_correction_T_max 0.7090 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _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 'Bruker APEX-II CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 29076 _diffrn_reflns_av_R_equivalents 0.0402 _diffrn_reflns_av_sigmaI/netI 0.0335 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 27.52 _reflns_number_total 7536 _reflns_number_gt 7216 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0278P)^2^+0.3746P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.017(8) _refine_ls_number_reflns 7536 _refine_ls_number_parameters 361 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0239 _refine_ls_R_factor_gt 0.0224 _refine_ls_wR_factor_ref 0.0567 _refine_ls_wR_factor_gt 0.0560 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 Tm Tm 0.170742(10) 0.611009(8) 0.167745(7) 0.02978(4) Uani 1 1 d . . . O41 O 0.1720(2) 0.51500(14) 0.28144(12) 0.0393(5) Uani 1 1 d . . . N11 N -0.0410(2) 0.49889(17) 0.11999(16) 0.0319(6) Uani 1 1 d . . . N12 N -0.0234(2) 0.56644(16) 0.17080(16) 0.0316(5) Uani 1 1 d . . . N21 N 0.1334(2) 0.43979(17) 0.05444(16) 0.0314(6) Uani 1 1 d . . . N22 N 0.2176(2) 0.47402(17) 0.09733(15) 0.0307(5) Uani 1 1 d . . . N31 N 0.0410(2) 0.57491(16) 0.00173(16) 0.0301(5) Uani 1 1 d . . . N32 N 0.1023(2) 0.64077(16) 0.03212(15) 0.0287(5) Uani 1 1 d . . . C13 C -0.1022(3) 0.5619(2) 0.2235(2) 0.0337(7) Uani 1 1 d . . . C14 C -0.1694(3) 0.4905(2) 0.2093(2) 0.0403(7) Uani 1 1 d . . . H14 H -0.2302 0.4719 0.2390 0.048 Uiso 1 1 calc R . . C15 C -0.1288(3) 0.4528(2) 0.1431(2) 0.0380(7) Uani 1 1 d . . . C16 C -0.1717(4) 0.3746(2) 0.1013(2) 0.0502(9) Uani 1 1 d . . . H16A H -0.2247 0.3448 0.1342 0.060 Uiso 1 1 calc R . . H16B H -0.1113 0.3354 0.0894 0.060 Uiso 1 1 calc R . . H16C H -0.2069 0.3928 0.0531 0.060 Uiso 1 1 calc R . . C17 C -0.1141(3) 0.6271(2) 0.2894(2) 0.0391(8) Uani 1 1 d . . . C18 C -0.0258(4) 0.6959(3) 0.2860(3) 0.0584(11) Uani 1 1 d . . . H18A H -0.0314 0.7276 0.2370 0.070 Uiso 1 1 calc R . . H18B H 0.0459 0.6683 0.2895 0.070 Uiso 1 1 calc R . . H18C H -0.0349 0.7363 0.3292 0.070 Uiso 1 1 calc R . . C19 C -0.2253(4) 0.6707(3) 0.2831(3) 0.0696(14) Uani 1 1 d . . . H19A H -0.2826 0.6265 0.2850 0.084 Uiso 1 1 calc R . . H19B H -0.2299 0.7022 0.2340 0.084 Uiso 1 1 calc R . . H19C H -0.2348 0.7112 0.3262 0.084 Uiso 1 1 calc R . . C20 C -0.1080(4) 0.5805(3) 0.3673(2) 0.0623(12) Uani 1 1 d . . . H20A H -0.1624 0.5341 0.3687 0.075 Uiso 1 1 calc R . . H20B H -0.1226 0.6218 0.4090 0.075 Uiso 1 1 calc R . . H20C H -0.0351 0.5558 0.3740 0.075 Uiso 1 1 calc R . . C23 C 0.3006(3) 0.4186(2) 0.09125(18) 0.0330(7) Uani 1 1 d . . . C24 C 0.2711(3) 0.3491(2) 0.0435(2) 0.0426(8) Uani 1 1 d . . . H24 H 0.3154 0.3013 0.0293 0.051 Uiso 1 1 calc R . . C25 C 0.1656(3) 0.36412(19) 0.02157(19) 0.0381(7) Uani 1 1 d . . . C26 C 0.0966(4) 0.3099(3) -0.0306(3) 0.0552(11) Uani 1 1 d . . . H26A H 0.0300 0.2929 -0.0034 0.066 Uiso 1 1 calc R . . H26B H 0.1371 0.2580 -0.0460 0.066 Uiso 1 1 calc R . . H26C H 0.0774 0.3434 -0.0768 0.066 Uiso 1 1 calc R . . C27 C 0.4099(3) 0.4319(3) 0.1310(2) 0.0405(8) Uani 1 1 d . . . C28 C 0.5004(3) 0.4303(3) 0.0700(2) 0.0507(10) Uani 1 1 d . . . H28A H 0.5713 0.4363 0.0955 0.061 Uiso 1 1 calc R . . H28B H 0.4899 0.4783 0.0337 0.061 Uiso 1 1 calc R . . H28C H 0.4979 0.3753 0.0418 0.061 Uiso 1 1 calc R . . C29 C 0.4147(3) 0.5202(3) 0.1728(3) 0.0569(11) Uani 1 1 d . . . H29A H 0.3598 0.5217 0.2140 0.068 Uiso 1 1 calc R . . H29B H 0.4001 0.5667 0.1356 0.068 Uiso 1 1 calc R . . H29C H 0.4872 0.5284 0.1954 0.068 Uiso 1 1 calc R . . C30 C 0.4274(4) 0.3579(3) 0.1880(3) 0.0653(13) Uani 1 1 d . . . H30A H 0.3696 0.3588 0.2271 0.078 Uiso 1 1 calc R . . H30B H 0.4983 0.3647 0.2133 0.078 Uiso 1 1 calc R . . H30C H 0.4255 0.3027 0.1602 0.078 Uiso 1 1 calc R . . C33 C 0.1017(2) 0.7045(2) -0.02061(19) 0.0332(7) Uani 1 1 d . . . C34 C 0.0399(3) 0.6792(2) -0.0854(2) 0.0400(8) Uani 1 1 d . . . H34 H 0.0263 0.7120 -0.1309 0.048 Uiso 1 1 calc R . . C35 C 0.0036(3) 0.5973(2) -0.06901(19) 0.0360(7) Uani 1 1 d . . . C36 C -0.0674(3) 0.5406(3) -0.1183(2) 0.0532(10) Uani 1 1 d . . . H36A H -0.1337 0.5256 -0.0896 0.064 Uiso 1 1 calc R . . H36B H -0.0279 0.4875 -0.1317 0.064 Uiso 1 1 calc R . . H36C H -0.0872 0.5715 -0.1657 0.064 Uiso 1 1 calc R . . C37 C 0.1572(3) 0.7908(2) -0.0074(2) 0.0445(8) Uani 1 1 d . . . C38 C 0.2786(3) 0.7788(3) 0.0052(3) 0.0643(13) Uani 1 1 d . . . H38A H 0.3110 0.7518 -0.0407 0.077 Uiso 1 1 calc R . . H38B H 0.2906 0.7415 0.0503 0.077 Uiso 1 1 calc R . . H38C H 0.3127 0.8352 0.0142 0.077 Uiso 1 1 calc R . . C39 C 0.1047(5) 0.8350(3) 0.0596(4) 0.096(2) Uani 1 1 d . . . H39A H 0.0263 0.8400 0.0503 0.115 Uiso 1 1 calc R . . H39B H 0.1361 0.8930 0.0658 0.115 Uiso 1 1 calc R . . H39C H 0.1173 0.8012 0.1067 0.115 Uiso 1 1 calc R . . C40 C 0.1456(6) 0.8459(4) -0.0795(4) 0.104(2) Uani 1 1 d . . . H40A H 0.1763 0.8149 -0.1239 0.125 Uiso 1 1 calc R . . H40B H 0.1847 0.9006 -0.0723 0.125 Uiso 1 1 calc R . . H40C H 0.0684 0.8579 -0.0890 0.125 Uiso 1 1 calc R . . C42 C 0.1245(3) 0.4278(2) 0.2762(2) 0.0392(8) Uani 1 1 d . . . H42A H 0.1456 0.3993 0.2272 0.047 Uiso 1 1 calc R . . H42B H 0.0440 0.4304 0.2791 0.047 Uiso 1 1 calc R . . C43 C 0.1712(3) 0.3789(2) 0.34568(19) 0.0433(7) Uani 1 1 d . . . H43A H 0.1203 0.3337 0.3640 0.052 Uiso 1 1 calc R . . H43B H 0.2420 0.3519 0.3329 0.052 Uiso 1 1 calc R . . C44 C 0.1843(4) 0.4497(3) 0.4048(2) 0.0458(8) Uani 1 1 d . . . H44A H 0.2391 0.4339 0.4443 0.055 Uiso 1 1 calc R . . H44B H 0.1143 0.4626 0.4308 0.055 Uiso 1 1 calc R . . C45 C 0.2222(3) 0.5255(3) 0.3568(2) 0.0493(9) Uani 1 1 d . . . H45A H 0.1992 0.5808 0.3807 0.059 Uiso 1 1 calc R . . H45B H 0.3026 0.5254 0.3521 0.059 Uiso 1 1 calc R . . B1 B 0.0224(3) 0.4871(2) 0.0433(2) 0.0303(7) Uani 1 1 d . . . H1B H -0.0234 0.4503 0.0085 0.036 Uiso 1 1 calc R . . B2 B 0.2886(5) 0.7343(3) 0.2344(3) 0.0594(14) Uani 1 1 d D . . H2BA H 0.325(3) 0.711(2) 0.1834(15) 0.071 Uiso 1 1 d D . . H2BB H 0.210(2) 0.757(2) 0.2215(19) 0.071 Uiso 1 1 d D . . H2BC H 0.282(3) 0.6835(18) 0.2742(17) 0.071 Uiso 1 1 d D . . H2BD H 0.336(3) 0.7841(18) 0.2574(18) 0.071 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tm 0.03011(6) 0.02788(6) 0.03135(6) -0.00340(5) -0.00074(6) -0.00267(5) O41 0.0487(13) 0.0353(11) 0.0339(11) 0.0022(9) -0.0070(12) -0.0101(12) N11 0.0299(13) 0.0283(13) 0.0376(14) -0.0008(11) -0.0005(11) -0.0030(10) N12 0.0309(12) 0.0281(12) 0.0357(13) -0.0029(12) 0.0003(12) -0.0022(9) N21 0.0346(13) 0.0244(13) 0.0351(14) -0.0015(11) -0.0015(11) -0.0007(10) N22 0.0318(13) 0.0296(13) 0.0308(13) -0.0016(11) -0.0007(10) 0.0046(10) N31 0.0292(12) 0.0274(11) 0.0338(13) -0.0009(11) -0.0033(11) 0.0008(9) N32 0.0283(12) 0.0248(11) 0.0331(13) -0.0015(10) -0.0004(10) 0.0021(9) C13 0.0315(15) 0.0282(15) 0.0415(18) 0.0039(13) 0.0014(13) 0.0025(12) C14 0.0333(15) 0.0418(17) 0.0457(18) 0.0027(14) 0.0036(17) -0.0058(16) C15 0.0305(15) 0.0346(17) 0.049(2) 0.0029(14) -0.0020(14) -0.0038(13) C16 0.0462(19) 0.044(2) 0.061(2) -0.0048(17) 0.0025(19) -0.015(2) C17 0.0385(17) 0.0363(19) 0.0425(18) 0.0008(15) 0.0044(14) 0.0032(14) C18 0.064(3) 0.054(2) 0.058(3) -0.017(2) 0.012(2) -0.009(2) C19 0.058(3) 0.066(3) 0.085(4) -0.023(3) -0.001(2) 0.023(2) C20 0.087(3) 0.056(3) 0.044(2) 0.0020(19) 0.008(2) 0.013(2) C23 0.0345(16) 0.0344(15) 0.0301(15) 0.0038(12) 0.0058(12) 0.0083(12) C24 0.051(2) 0.0259(16) 0.051(2) -0.0014(15) 0.0076(16) 0.0093(14) C25 0.0491(18) 0.0228(13) 0.0424(17) -0.0032(11) 0.0071(17) -0.0033(14) C26 0.058(2) 0.045(2) 0.063(3) -0.024(2) 0.003(2) -0.0065(18) C27 0.0335(17) 0.046(2) 0.0417(19) 0.0042(16) 0.0047(15) 0.0122(15) C28 0.039(2) 0.063(2) 0.051(2) -0.0066(19) 0.0118(17) 0.0093(18) C29 0.0355(17) 0.083(3) 0.052(2) -0.016(3) -0.0046(19) 0.0091(18) C30 0.046(2) 0.087(3) 0.062(3) 0.031(2) -0.0059(19) 0.012(2) C33 0.0280(14) 0.0318(15) 0.0399(18) 0.0039(13) 0.0072(12) 0.0070(12) C34 0.0352(17) 0.044(2) 0.0405(19) 0.0124(16) 0.0016(14) 0.0086(15) C35 0.0302(14) 0.0428(19) 0.0349(15) 0.0009(14) -0.0021(12) 0.0039(14) C36 0.052(2) 0.066(3) 0.042(2) 0.005(2) -0.0138(18) -0.008(2) C37 0.046(2) 0.0281(15) 0.060(2) 0.0042(15) 0.0116(19) 0.0025(15) C38 0.043(2) 0.051(2) 0.099(4) -0.023(3) 0.003(2) -0.0110(18) C39 0.107(5) 0.047(3) 0.133(5) -0.031(3) 0.067(4) -0.011(3) C40 0.135(6) 0.057(3) 0.121(5) 0.046(3) -0.038(4) -0.037(4) C42 0.0439(19) 0.0338(17) 0.0399(19) 0.0041(15) -0.0048(15) -0.0071(15) C43 0.0476(17) 0.0416(17) 0.0408(18) 0.0060(14) -0.0023(16) 0.0021(18) C44 0.052(2) 0.054(2) 0.0323(16) 0.0049(15) -0.0053(16) 0.0098(18) C45 0.054(2) 0.055(2) 0.0392(19) 0.0025(17) -0.0138(16) -0.0112(18) B1 0.0306(16) 0.0259(16) 0.0344(18) -0.0033(13) -0.0015(14) -0.0032(13) B2 0.081(4) 0.050(3) 0.048(3) -0.011(2) 0.002(2) -0.029(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 Tm O41 2.462(2) . ? Tm N12 2.482(2) . ? Tm N22 2.508(3) . ? Tm N32 2.532(3) . ? Tm B2 2.656(4) . ? Tm H2BA 2.46(3) . ? Tm H2BB 2.49(3) . ? Tm H2BC 2.55(3) . ? O41 C45 1.450(4) . ? O41 C42 1.471(4) . ? N11 C15 1.352(4) . ? N11 N12 1.381(4) . ? N11 B1 1.548(4) . ? N12 C13 1.331(4) . ? N21 C25 1.359(4) . ? N21 N22 1.378(4) . ? N21 B1 1.559(4) . ? N22 C23 1.335(4) . ? N31 C35 1.351(4) . ? N31 N32 1.370(4) . ? N31 B1 1.553(4) . ? N32 C33 1.342(4) . ? C13 C14 1.400(5) . ? C13 C17 1.528(5) . ? C14 C15 1.378(5) . ? C15 C16 1.502(5) . ? C17 C18 1.520(5) . ? C17 C19 1.526(5) . ? C17 C20 1.527(6) . ? C23 C24 1.401(5) . ? C23 C27 1.522(5) . ? C24 C25 1.370(5) . ? C25 C26 1.494(5) . ? C27 C30 1.524(6) . ? C27 C28 1.533(5) . ? C27 C29 1.545(6) . ? C33 C34 1.409(5) . ? C33 C37 1.514(5) . ? C34 C35 1.372(5) . ? C35 C36 1.502(5) . ? C37 C39 1.492(6) . ? C37 C40 1.516(6) . ? C37 C38 1.518(6) . ? C42 C43 1.529(5) . ? C43 C44 1.506(5) . ? C44 C45 1.509(5) . ? B2 H2BA 1.05(2) . ? B2 H2BB 1.06(2) . ? B2 H2BC 1.05(2) . ? B2 H2BD 1.04(2) . ? 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 O41 Tm N12 79.73(9) . . ? O41 Tm N22 82.98(8) . . ? N12 Tm N22 89.81(8) . . ? O41 Tm N32 148.24(8) . . ? N12 Tm N32 75.60(9) . . ? N22 Tm N32 77.29(8) . . ? O41 Tm H2BC 71.6(5) . . ? N12 Tm H2BC 128.3(7) . . ? N22 Tm H2BC 126.8(7) . . ? N32 Tm H2BC 140.0(5) . . ? O41 Tm B2 94.72(13) . . ? N12 Tm B2 135.50(14) . . ? N22 Tm B2 133.69(15) . . ? N32 Tm B2 116.91(13) . . ? H2BC Tm B2 23.1(5) . . ? O41 Tm H2BA 106.7(7) . . ? N12 Tm H2BA 155.6(6) . . ? N22 Tm H2BA 114.1(6) . . ? N32 Tm H2BA 104.1(7) . . ? H2BC Tm H2BA 39.9(9) . . ? B2 Tm H2BA 23.3(5) . . ? O41 Tm H2BB 104.3(7) . . ? N12 Tm H2BB 115.4(6) . . ? N22 Tm H2BB 154.5(6) . . ? N32 Tm H2BB 104.2(7) . . ? H2BC Tm H2BB 39.5(8) . . ? B2 Tm H2BB 23.4(5) . . ? H2BA Tm H2BB 40.5(9) . . ? C45 O41 C42 109.0(3) . . ? C45 O41 Tm 130.7(2) . . ? C42 O41 Tm 120.05(19) . . ? C15 N11 N12 109.6(3) . . ? C15 N11 B1 126.2(3) . . ? N12 N11 B1 123.7(2) . . ? C13 N12 N11 106.4(2) . . ? C13 N12 Tm 136.7(2) . . ? N11 N12 Tm 110.27(18) . . ? C25 N21 N22 109.7(3) . . ? C25 N21 B1 127.3(3) . . ? N22 N21 B1 122.9(2) . . ? C23 N22 N21 106.5(3) . . ? C23 N22 Tm 139.0(2) . . ? N21 N22 Tm 114.38(18) . . ? C35 N31 N32 110.1(3) . . ? C35 N31 B1 126.3(3) . . ? N32 N31 B1 123.5(3) . . ? C33 N32 N31 106.3(3) . . ? C33 N32 Tm 139.8(2) . . ? N31 N32 Tm 113.73(18) . . ? N12 C13 C14 110.5(3) . . ? N12 C13 C17 123.1(3) . . ? C14 C13 C17 126.5(3) . . ? C15 C14 C13 105.4(3) . . ? N11 C15 C14 108.1(3) . . ? N11 C15 C16 124.1(3) . . ? C14 C15 C16 127.7(3) . . ? C18 C17 C19 109.1(3) . . ? C18 C17 C20 109.2(4) . . ? C19 C17 C20 108.3(4) . . ? C18 C17 C13 111.3(3) . . ? C19 C17 C13 108.8(3) . . ? C20 C17 C13 110.0(3) . . ? N22 C23 C24 109.9(3) . . ? N22 C23 C27 123.4(3) . . ? C24 C23 C27 126.7(3) . . ? C25 C24 C23 106.1(3) . . ? N21 C25 C24 107.8(3) . . ? N21 C25 C26 124.7(4) . . ? C24 C25 C26 127.5(3) . . ? C23 C27 C30 108.3(3) . . ? C23 C27 C28 109.1(3) . . ? C30 C27 C28 109.3(3) . . ? C23 C27 C29 111.3(3) . . ? C30 C27 C29 110.8(4) . . ? C28 C27 C29 108.0(3) . . ? N32 C33 C34 109.9(3) . . ? N32 C33 C37 122.8(3) . . ? C34 C33 C37 127.3(3) . . ? C35 C34 C33 105.4(3) . . ? N31 C35 C34 108.3(3) . . ? N31 C35 C36 124.2(3) . . ? C34 C35 C36 127.6(3) . . ? C39 C37 C33 109.0(3) . . ? C39 C37 C40 109.9(4) . . ? C33 C37 C40 109.2(4) . . ? C39 C37 C38 111.6(4) . . ? C33 C37 C38 110.9(3) . . ? C40 C37 C38 106.2(4) . . ? O41 C42 C43 104.8(3) . . ? C44 C43 C42 102.4(3) . . ? C43 C44 C45 102.9(3) . . ? O41 C45 C44 106.0(3) . . ? N11 B1 N31 111.5(3) . . ? N11 B1 N21 112.9(3) . . ? N31 B1 N21 109.7(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N12 Tm O41 C45 -136.0(3) . . . . ? N22 Tm O41 C45 132.9(3) . . . . ? N32 Tm O41 C45 -175.4(3) . . . . ? B2 Tm O41 C45 -0.6(3) . . . . ? N12 Tm O41 C42 50.3(2) . . . . ? N22 Tm O41 C42 -40.8(2) . . . . ? N32 Tm O41 C42 10.9(3) . . . . ? B2 Tm O41 C42 -174.3(3) . . . . ? C15 N11 N12 C13 -1.3(3) . . . . ? B1 N11 N12 C13 171.4(3) . . . . ? C15 N11 N12 Tm 155.1(2) . . . . ? B1 N11 N12 Tm -32.1(3) . . . . ? O41 Tm N12 C13 48.9(3) . . . . ? N22 Tm N12 C13 131.8(3) . . . . ? N32 Tm N12 C13 -151.3(3) . . . . ? B2 Tm N12 C13 -37.4(4) . . . . ? O41 Tm N12 N11 -97.17(19) . . . . ? N22 Tm N12 N11 -14.3(2) . . . . ? N32 Tm N12 N11 62.65(19) . . . . ? B2 Tm N12 N11 176.6(2) . . . . ? C25 N21 N22 C23 -0.7(3) . . . . ? B1 N21 N22 C23 -177.1(3) . . . . ? C25 N21 N22 Tm -177.3(2) . . . . ? B1 N21 N22 Tm 6.3(4) . . . . ? O41 Tm N22 C23 -68.8(3) . . . . ? N12 Tm N22 C23 -148.5(3) . . . . ? N32 Tm N22 C23 136.3(3) . . . . ? B2 Tm N22 C23 21.0(4) . . . . ? O41 Tm N22 N21 106.3(2) . . . . ? N12 Tm N22 N21 26.6(2) . . . . ? N32 Tm N22 N21 -48.7(2) . . . . ? B2 Tm N22 N21 -163.9(2) . . . . ? C35 N31 N32 C33 0.4(3) . . . . ? B1 N31 N32 C33 178.6(3) . . . . ? C35 N31 N32 Tm 177.21(19) . . . . ? B1 N31 N32 Tm -4.6(3) . . . . ? O41 Tm N32 C33 170.3(3) . . . . ? N12 Tm N32 C33 130.1(3) . . . . ? N22 Tm N32 C33 -136.8(3) . . . . ? B2 Tm N32 C33 -4.0(4) . . . . ? O41 Tm N32 N31 -5.0(3) . . . . ? N12 Tm N32 N31 -45.16(18) . . . . ? N22 Tm N32 N31 47.96(18) . . . . ? B2 Tm N32 N31 -179.2(2) . . . . ? N11 N12 C13 C14 1.9(4) . . . . ? Tm N12 C13 C14 -145.0(3) . . . . ? N11 N12 C13 C17 -178.3(3) . . . . ? Tm N12 C13 C17 34.8(5) . . . . ? N12 C13 C14 C15 -1.7(4) . . . . ? C17 C13 C14 C15 178.4(3) . . . . ? N12 N11 C15 C14 0.3(4) . . . . ? B1 N11 C15 C14 -172.3(3) . . . . ? N12 N11 C15 C16 179.9(3) . . . . ? B1 N11 C15 C16 7.4(5) . . . . ? C13 C14 C15 N11 0.9(4) . . . . ? C13 C14 C15 C16 -178.8(4) . . . . ? N12 C13 C17 C18 0.2(5) . . . . ? C14 C13 C17 C18 -180.0(4) . . . . ? N12 C13 C17 C19 120.5(4) . . . . ? C14 C13 C17 C19 -59.7(5) . . . . ? N12 C13 C17 C20 -121.0(4) . . . . ? C14 C13 C17 C20 58.8(5) . . . . ? N21 N22 C23 C24 0.9(4) . . . . ? Tm N22 C23 C24 176.2(2) . . . . ? N21 N22 C23 C27 -179.4(3) . . . . ? Tm N22 C23 C27 -4.1(5) . . . . ? N22 C23 C24 C25 -0.8(4) . . . . ? C27 C23 C24 C25 179.5(3) . . . . ? N22 N21 C25 C24 0.2(4) . . . . ? B1 N21 C25 C24 176.4(3) . . . . ? N22 N21 C25 C26 -178.3(3) . . . . ? B1 N21 C25 C26 -2.1(5) . . . . ? C23 C24 C25 N21 0.4(4) . . . . ? C23 C24 C25 C26 178.9(4) . . . . ? N22 C23 C27 C30 117.4(4) . . . . ? C24 C23 C27 C30 -63.0(5) . . . . ? N22 C23 C27 C28 -123.7(4) . . . . ? C24 C23 C27 C28 55.9(5) . . . . ? N22 C23 C27 C29 -4.7(5) . . . . ? C24 C23 C27 C29 174.9(4) . . . . ? N31 N32 C33 C34 -0.2(3) . . . . ? Tm N32 C33 C34 -175.7(2) . . . . ? N31 N32 C33 C37 177.6(3) . . . . ? Tm N32 C33 C37 2.1(5) . . . . ? N32 C33 C34 C35 0.0(4) . . . . ? C37 C33 C34 C35 -177.7(3) . . . . ? N32 N31 C35 C34 -0.4(4) . . . . ? B1 N31 C35 C34 -178.5(3) . . . . ? N32 N31 C35 C36 -179.2(3) . . . . ? B1 N31 C35 C36 2.7(5) . . . . ? C33 C34 C35 N31 0.3(4) . . . . ? C33 C34 C35 C36 179.0(4) . . . . ? N32 C33 C37 C39 -62.6(5) . . . . ? C34 C33 C37 C39 114.8(5) . . . . ? N32 C33 C37 C40 177.3(4) . . . . ? C34 C33 C37 C40 -5.3(6) . . . . ? N32 C33 C37 C38 60.6(5) . . . . ? C34 C33 C37 C38 -122.0(4) . . . . ? C45 O41 C42 C43 -12.5(4) . . . . ? Tm O41 C42 C43 162.5(2) . . . . ? O41 C42 C43 C44 31.6(4) . . . . ? C42 C43 C44 C45 -38.3(4) . . . . ? C42 O41 C45 C44 -11.8(4) . . . . ? Tm O41 C45 C44 174.0(2) . . . . ? C43 C44 C45 O41 31.6(4) . . . . ? C15 N11 B1 N31 131.6(3) . . . . ? N12 N11 B1 N31 -39.9(4) . . . . ? C15 N11 B1 N21 -104.3(4) . . . . ? N12 N11 B1 N21 84.2(3) . . . . ? C35 N31 B1 N11 -118.4(3) . . . . ? N32 N31 B1 N11 63.8(4) . . . . ? C35 N31 B1 N21 115.7(3) . . . . ? N32 N31 B1 N21 -62.1(4) . . . . ? C25 N21 B1 N11 120.3(3) . . . . ? N22 N21 B1 N11 -63.9(4) . . . . ? C25 N21 B1 N31 -114.5(3) . . . . ? N22 N21 B1 N31 61.2(4) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.927 _refine_diff_density_min -0.409 _refine_diff_density_rms 0.067 #===END