# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and The Centre National de la Recherche Scientifique, 2010 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Chivers, Tristram' _publ_contact_author_email CHIVERS@UCALGARY.CA _publ_section_title ; Syntheses and structures of new alkali-metal boraamidinates and ferrocenyl aminoboranes ; _publ_author_name T.Chivers # Attachment '- Newbams_revised.cif' data_Compound1a _database_code_depnum_ccdc_archive 'CCDC 773247' #TrackingRef '- Newbams_revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H29 B Fe N2' _chemical_formula_sum 'C18 H29 B Fe N2' _chemical_formula_weight 340.09 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 17.365(4) _cell_length_b 5.9559(12) _cell_length_c 35.480(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3669.6(13) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 22275 _cell_measurement_theta_min 3.28 _cell_measurement_theta_max 25.02 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.231 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1456 _exptl_absorpt_coefficient_mu 0.820 _exptl_absorpt_correction_type Integration _exptl_absorpt_correction_T_min 0.8029 _exptl_absorpt_correction_T_max 0.9679 _exptl_absorpt_process_details 'HKL Scalepack (Otwinowski and Minor 1997)' _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 'Nonius Kappa CCD' _diffrn_measurement_method 'phi\omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5629 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0479 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 3.28 _diffrn_reflns_theta_max 25.02 _reflns_number_total 5629 _reflns_number_gt 4927 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NOnius COLLECT' _computing_cell_refinement 'Nonius DENZO' _computing_data_reduction 'Nonius DENZO' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0498P)^2^+2.7062P] 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 constr _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 0.50(2) _refine_ls_number_reflns 5629 _refine_ls_number_parameters 397 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0570 _refine_ls_R_factor_gt 0.0428 _refine_ls_wR_factor_ref 0.1121 _refine_ls_wR_factor_gt 0.0981 _refine_ls_goodness_of_fit_ref 1.126 _refine_ls_restrained_S_all 1.126 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.5963(3) 0.5916(7) 0.61287(16) 0.0251(11) Uani 1 1 d . . . N1 N 0.66751(19) 0.5083(5) 0.62678(13) 0.0286(9) Uani 1 1 d . . . H1A H 0.6766 0.5422 0.6505 0.034 Uiso 1 1 calc R . . N2 N 0.5745(2) 0.5714(6) 0.57462(13) 0.0312(9) Uani 1 1 d . . . H2A H 0.6112 0.5175 0.5601 0.037 Uiso 1 1 calc R . . Fe1 Fe 0.56496(3) 0.82254(9) 0.697192(19) 0.02654(16) Uani 1 1 d . . . C1 C 0.5405(3) 0.6930(7) 0.64423(14) 0.0247(10) Uani 1 1 d . . . C2 C 0.5096(3) 0.9138(7) 0.64892(15) 0.0298(11) Uani 1 1 d . . . H2B H 0.5229 1.0469 0.6330 0.036 Uiso 1 1 calc R . . C3 C 0.4579(3) 0.9159(9) 0.67968(17) 0.0394(13) Uani 1 1 d . . . H3A H 0.4278 1.0480 0.6889 0.047 Uiso 1 1 calc R . . C4 C 0.4562(3) 0.6961(9) 0.69481(19) 0.0397(12) Uani 1 1 d . . . H4A H 0.4246 0.6454 0.7168 0.048 Uiso 1 1 calc R . . C5 C 0.5069(3) 0.5596(7) 0.67318(17) 0.0358(13) Uani 1 1 d . . . H5A H 0.5177 0.3969 0.6778 0.043 Uiso 1 1 calc R . . C6 C 0.6813(3) 0.8631(8) 0.70403(17) 0.0369(13) Uani 1 1 d . . . H6A H 0.7213 0.8336 0.6844 0.044 Uiso 1 1 calc R . . C7 C 0.6420(3) 1.0698(8) 0.70952(17) 0.0398(13) Uani 1 1 d . . . H7A H 0.6501 1.2111 0.6949 0.048 Uiso 1 1 calc R . . C8 C 0.5901(3) 1.0405(8) 0.73986(17) 0.0424(14) Uani 1 1 d . . . H8A H 0.5548 1.1572 0.7505 0.051 Uiso 1 1 calc R . . C9 C 0.5969(4) 0.8136(9) 0.75234(17) 0.0436(13) Uani 1 1 d . . . H9A H 0.5675 0.7424 0.7734 0.052 Uiso 1 1 calc R . . C10 C 0.6535(3) 0.7076(8) 0.72947(18) 0.0414(13) Uani 1 1 d . . . H10A H 0.6704 0.5477 0.7315 0.050 Uiso 1 1 calc R . . C11 C 0.7291(2) 0.3753(7) 0.60874(14) 0.0276(10) Uani 1 1 d . . . C12 C 0.7646(3) 0.4966(8) 0.57508(19) 0.0457(14) Uani 1 1 d . . . H12A H 0.7252 0.5192 0.5557 0.069 Uiso 1 1 calc R . . H12B H 0.8067 0.4060 0.5647 0.069 Uiso 1 1 calc R . . H12C H 0.7847 0.6426 0.5832 0.069 Uiso 1 1 calc R . . C13 C 0.7916(3) 0.3414(10) 0.63902(19) 0.0486(15) Uani 1 1 d . . . H13A H 0.7694 0.2635 0.6608 0.073 Uiso 1 1 calc R . . H13B H 0.8116 0.4878 0.6470 0.073 Uiso 1 1 calc R . . H13C H 0.8337 0.2512 0.6286 0.073 Uiso 1 1 calc R . . C14 C 0.6986(3) 0.1450(7) 0.59741(16) 0.0384(12) Uani 1 1 d . . . H14A H 0.6586 0.1627 0.5782 0.058 Uiso 1 1 calc R . . H14B H 0.6768 0.0700 0.6195 0.058 Uiso 1 1 calc R . . H14C H 0.7409 0.0543 0.5873 0.058 Uiso 1 1 calc R . . C15 C 0.5031(3) 0.6220(8) 0.55420(16) 0.0317(11) Uani 1 1 d . . . C16 C 0.4936(3) 0.8760(8) 0.54878(19) 0.0449(14) Uani 1 1 d . . . H16A H 0.5387 0.9359 0.5355 0.067 Uiso 1 1 calc R . . H16B H 0.4889 0.9488 0.5734 0.067 Uiso 1 1 calc R . . H16C H 0.4472 0.9055 0.5339 0.067 Uiso 1 1 calc R . . C17 C 0.4334(3) 0.5252(9) 0.57477(17) 0.0401(12) Uani 1 1 d . . . H17A H 0.4402 0.3630 0.5780 0.060 Uiso 1 1 calc R . . H17B H 0.3868 0.5538 0.5600 0.060 Uiso 1 1 calc R . . H17C H 0.4286 0.5967 0.5995 0.060 Uiso 1 1 calc R . . C18 C 0.5096(3) 0.5125(9) 0.51553(18) 0.0479(14) Uani 1 1 d . . . H18A H 0.5156 0.3498 0.5185 0.072 Uiso 1 1 calc R . . H18B H 0.5544 0.5735 0.5022 0.072 Uiso 1 1 calc R . . H18C H 0.4628 0.5436 0.5010 0.072 Uiso 1 1 calc R . . B2 B 0.8493(3) 0.4427(7) 0.89689(15) 0.0236(11) Uani 1 1 d . . . N3 N 0.9194(2) 0.5302(6) 0.88115(13) 0.0299(9) Uani 1 1 d . . . H3B H 0.9253 0.5038 0.8569 0.036 Uiso 1 1 calc R . . N4 N 0.8317(2) 0.4528(6) 0.93519(12) 0.0298(9) Uani 1 1 d . . . H4B H 0.8701 0.5014 0.9492 0.036 Uiso 1 1 calc R . . Fe2 Fe 0.80948(3) 0.22042(9) 0.81247(2) 0.02719(16) Uani 1 1 d . . . C19 C 0.7906(3) 0.3456(7) 0.86619(14) 0.0262(10) Uani 1 1 d . . . C20 C 0.7538(3) 0.4810(8) 0.83815(16) 0.0312(11) Uani 1 1 d . . . H20A H 0.7644 0.6438 0.8336 0.037 Uiso 1 1 calc R . . C21 C 0.7009(3) 0.3463(8) 0.81706(18) 0.0376(12) Uani 1 1 d . . . H21A H 0.6673 0.3982 0.7959 0.045 Uiso 1 1 calc R . . C22 C 0.7050(3) 0.1251(9) 0.83188(16) 0.0365(12) Uani 1 1 d . . . H22A H 0.6746 -0.0072 0.8229 0.044 Uiso 1 1 calc R . . C23 C 0.7595(3) 0.1250(7) 0.86217(15) 0.0296(11) Uani 1 1 d . . . H23A H 0.7744 -0.0088 0.8775 0.035 Uiso 1 1 calc R . . C24 C 0.9247(3) 0.1831(8) 0.80168(19) 0.0410(14) Uani 1 1 d . . . H24A H 0.9675 0.2171 0.8196 0.049 Uiso 1 1 calc R . . C25 C 0.8922(3) 0.3344(9) 0.77585(18) 0.0447(14) Uani 1 1 d . . . H25A H 0.9079 0.4944 0.7721 0.054 Uiso 1 1 calc R . . C26 C 0.8330(4) 0.2171(10) 0.75560(18) 0.0472(14) Uani 1 1 d . . . H26A H 0.7998 0.2812 0.7353 0.057 Uiso 1 1 calc R . . C27 C 0.8293(3) -0.0042(9) 0.77000(18) 0.0431(14) Uani 1 1 d . . . H27A H 0.7932 -0.1247 0.7614 0.052 Uiso 1 1 calc R . . C28 C 0.8859(3) -0.0258(8) 0.79824(15) 0.0357(12) Uani 1 1 d . . . H28A H 0.8970 -0.1644 0.8132 0.043 Uiso 1 1 calc R . . C29 C 0.9833(3) 0.6570(7) 0.89862(16) 0.0314(11) Uani 1 1 d . . . C30 C 1.0233(3) 0.5167(9) 0.9288(2) 0.0600(19) Uani 1 1 d . . . H30A H 0.9869 0.4844 0.9492 0.090 Uiso 1 1 calc R . . H30B H 1.0674 0.6001 0.9389 0.090 Uiso 1 1 calc R . . H30C H 1.0412 0.3754 0.9177 0.090 Uiso 1 1 calc R . . C31 C 1.0408(3) 0.7066(11) 0.8669(2) 0.0582(18) Uani 1 1 d . . . H31A H 1.0156 0.7969 0.8474 0.087 Uiso 1 1 calc R . . H31B H 1.0587 0.5649 0.8559 0.087 Uiso 1 1 calc R . . H31C H 1.0848 0.7895 0.8771 0.087 Uiso 1 1 calc R . . C32 C 0.9544(3) 0.8761(8) 0.91418(19) 0.0434(14) Uani 1 1 d . . . H32A H 0.9176 0.8468 0.9345 0.065 Uiso 1 1 calc R . . H32B H 0.9289 0.9613 0.8941 0.065 Uiso 1 1 calc R . . H32C H 0.9979 0.9631 0.9240 0.065 Uiso 1 1 calc R . . C33 C 0.7617(3) 0.3983(7) 0.95684(17) 0.0338(12) Uani 1 1 d . . . C34 C 0.7706(3) 0.5088(9) 0.99569(18) 0.0476(14) Uani 1 1 d . . . H34A H 0.8163 0.4481 1.0083 0.071 Uiso 1 1 calc R . . H34B H 0.7248 0.4773 1.0110 0.071 Uiso 1 1 calc R . . H34C H 0.7763 0.6714 0.9926 0.071 Uiso 1 1 calc R . . C35 C 0.7543(3) 0.1451(8) 0.96251(18) 0.0431(13) Uani 1 1 d . . . H35A H 0.7486 0.0715 0.9380 0.065 Uiso 1 1 calc R . . H35B H 0.7090 0.1132 0.9781 0.065 Uiso 1 1 calc R . . H35C H 0.8006 0.0881 0.9751 0.065 Uiso 1 1 calc R . . C36 C 0.6907(3) 0.4912(9) 0.93685(18) 0.0452(14) Uani 1 1 d . . . H36A H 0.6855 0.4198 0.9121 0.068 Uiso 1 1 calc R . . H36B H 0.6962 0.6538 0.9336 0.068 Uiso 1 1 calc R . . H36C H 0.6447 0.4595 0.9520 0.068 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 B1 0.027(3) 0.021(2) 0.027(3) -0.001(2) 0.000(2) -0.0040(18) N1 0.0238(19) 0.0270(18) 0.035(3) -0.0066(16) 0.0002(18) 0.0042(14) N2 0.026(2) 0.044(2) 0.024(3) -0.0041(17) 0.0014(17) 0.0043(15) Fe1 0.0275(3) 0.0307(3) 0.0214(4) -0.0034(3) -0.0018(3) 0.0007(2) C1 0.025(2) 0.033(2) 0.016(3) -0.0049(18) -0.003(2) -0.0012(17) C2 0.032(3) 0.030(2) 0.027(3) -0.0036(19) -0.011(2) 0.0057(18) C3 0.025(2) 0.046(3) 0.048(4) -0.015(2) -0.004(2) 0.007(2) C4 0.031(2) 0.061(3) 0.027(3) -0.009(3) 0.007(3) -0.010(2) C5 0.031(3) 0.029(2) 0.047(4) -0.006(2) 0.002(2) -0.0070(18) C6 0.031(2) 0.039(3) 0.041(4) -0.014(2) -0.015(2) 0.0027(18) C7 0.035(3) 0.036(3) 0.048(4) -0.013(2) -0.007(2) -0.0021(19) C8 0.039(3) 0.048(3) 0.040(4) -0.022(2) -0.005(3) 0.004(2) C9 0.051(3) 0.068(4) 0.012(3) -0.004(2) -0.001(3) -0.005(3) C10 0.048(3) 0.039(3) 0.037(4) -0.004(2) -0.017(3) 0.000(2) C11 0.024(2) 0.033(2) 0.025(3) -0.0035(19) -0.001(2) 0.0030(17) C12 0.034(3) 0.042(3) 0.062(5) 0.003(3) 0.016(3) 0.003(2) C13 0.037(3) 0.069(4) 0.041(4) -0.010(3) -0.006(3) 0.016(2) C14 0.046(3) 0.030(2) 0.040(4) -0.005(2) 0.005(3) 0.006(2) C15 0.028(2) 0.038(3) 0.029(3) -0.002(2) -0.003(2) 0.0047(18) C16 0.051(3) 0.041(3) 0.043(4) 0.000(2) -0.005(3) 0.005(2) C17 0.031(3) 0.053(3) 0.036(4) 0.000(2) -0.005(2) -0.004(2) C18 0.047(3) 0.062(3) 0.034(4) -0.010(3) -0.005(3) 0.006(3) B2 0.031(3) 0.022(2) 0.018(3) -0.0022(19) 0.001(2) 0.0008(18) N3 0.030(2) 0.034(2) 0.026(3) -0.0073(16) 0.0045(17) -0.0068(15) N4 0.028(2) 0.046(2) 0.016(3) -0.0050(16) 0.0000(17) -0.0053(16) Fe2 0.0273(3) 0.0331(3) 0.0212(4) -0.0037(3) 0.0010(3) -0.0025(2) C19 0.025(2) 0.035(2) 0.019(3) -0.0058(19) 0.004(2) -0.0019(18) C20 0.030(2) 0.032(2) 0.032(3) -0.004(2) 0.005(2) 0.0022(18) C21 0.024(2) 0.058(3) 0.031(4) -0.003(3) -0.002(2) 0.0053(18) C22 0.026(2) 0.051(3) 0.033(3) -0.006(2) 0.003(2) -0.014(2) C23 0.033(3) 0.035(2) 0.021(3) -0.0028(19) 0.007(2) -0.0120(19) C24 0.025(3) 0.049(3) 0.049(4) -0.015(2) 0.009(2) -0.0020(19) C25 0.052(3) 0.046(3) 0.036(4) -0.002(2) 0.017(3) -0.002(2) C26 0.046(3) 0.081(4) 0.015(3) -0.002(3) 0.003(3) 0.008(3) C27 0.038(3) 0.050(3) 0.042(4) -0.016(2) 0.004(3) -0.004(2) C28 0.038(3) 0.036(3) 0.034(3) -0.011(2) 0.001(2) -0.0003(19) C29 0.024(2) 0.031(2) 0.039(3) -0.006(2) -0.003(2) -0.0037(18) C30 0.039(3) 0.050(3) 0.091(6) 0.017(3) -0.023(3) -0.012(2) C31 0.035(3) 0.077(4) 0.063(5) -0.020(3) 0.013(3) -0.019(3) C32 0.036(3) 0.037(3) 0.058(5) -0.013(2) 0.000(3) -0.006(2) C33 0.032(3) 0.033(2) 0.036(4) -0.004(2) 0.000(2) -0.0021(19) C34 0.053(3) 0.056(3) 0.033(4) -0.008(2) 0.004(3) -0.007(3) C35 0.053(3) 0.039(3) 0.037(4) 0.003(2) 0.005(3) -0.006(2) C36 0.039(3) 0.056(3) 0.041(4) 0.004(2) 0.014(3) 0.008(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 B1 N2 1.414(7) . ? B1 N1 1.421(6) . ? B1 C1 1.595(7) . ? N1 C11 1.477(6) . ? N2 C15 1.467(6) . ? Fe1 C9 2.035(6) . ? Fe1 C4 2.036(5) . ? Fe1 C10 2.035(5) . ? Fe1 C7 2.037(5) . ? Fe1 C3 2.037(5) . ? Fe1 C2 2.038(5) . ? Fe1 C8 2.041(5) . ? Fe1 C5 2.048(5) . ? Fe1 C6 2.049(4) . ? Fe1 C1 2.076(5) . ? C1 C5 1.423(7) . ? C1 C2 1.430(6) . ? C2 C3 1.413(8) . ? C3 C4 1.415(8) . ? C4 C5 1.424(7) . ? C6 C10 1.380(9) . ? C6 C7 1.421(7) . ? C7 C8 1.415(8) . ? C8 C9 1.427(8) . ? C9 C10 1.422(9) . ? C11 C14 1.524(6) . ? C11 C12 1.526(7) . ? C11 C13 1.541(7) . ? C15 C18 1.523(8) . ? C15 C17 1.526(7) . ? C15 C16 1.534(7) . ? B2 N4 1.394(7) . ? B2 N3 1.437(6) . ? B2 C19 1.600(7) . ? N3 C29 1.479(6) . ? N4 C33 1.474(7) . ? Fe2 C22 2.022(5) . ? Fe2 C21 2.036(5) . ? Fe2 C28 2.041(5) . ? Fe2 C27 2.044(5) . ? Fe2 C20 2.043(5) . ? Fe2 C23 2.046(5) . ? Fe2 C24 2.050(5) . ? Fe2 C25 2.053(6) . ? Fe2 C26 2.059(6) . ? Fe2 C19 2.073(5) . ? C19 C23 1.427(6) . ? C19 C20 1.431(7) . ? C20 C21 1.431(7) . ? C21 C22 1.421(8) . ? C22 C23 1.431(7) . ? C24 C25 1.404(9) . ? C24 C28 1.420(7) . ? C25 C26 1.436(9) . ? C26 C27 1.415(8) . ? C27 C28 1.410(8) . ? C29 C32 1.503(7) . ? C29 C30 1.526(8) . ? C29 C31 1.533(9) . ? C33 C35 1.527(7) . ? C33 C36 1.527(7) . ? C33 C34 1.535(8) . ? 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 N2 B1 N1 122.5(4) . . ? N2 B1 C1 122.6(4) . . ? N1 B1 C1 114.8(4) . . ? B1 N1 C11 131.8(4) . . ? B1 N2 C15 133.0(4) . . ? C9 Fe1 C4 106.4(3) . . ? C9 Fe1 C10 40.9(2) . . ? C4 Fe1 C10 126.9(2) . . ? C9 Fe1 C7 68.5(2) . . ? C4 Fe1 C7 152.4(2) . . ? C10 Fe1 C7 68.1(2) . . ? C9 Fe1 C3 123.3(2) . . ? C4 Fe1 C3 40.7(2) . . ? C10 Fe1 C3 162.3(3) . . ? C7 Fe1 C3 117.9(2) . . ? C9 Fe1 C2 160.7(2) . . ? C4 Fe1 C2 68.0(2) . . ? C10 Fe1 C2 156.8(2) . . ? C7 Fe1 C2 107.3(2) . . ? C3 Fe1 C2 40.6(2) . . ? C9 Fe1 C8 41.0(2) . . ? C4 Fe1 C8 117.7(2) . . ? C10 Fe1 C8 68.6(2) . . ? C7 Fe1 C8 40.6(2) . . ? C3 Fe1 C8 104.3(2) . . ? C2 Fe1 C8 123.7(2) . . ? C9 Fe1 C5 120.9(2) . . ? C4 Fe1 C5 40.8(2) . . ? C10 Fe1 C5 110.4(2) . . ? C7 Fe1 C5 164.9(2) . . ? C3 Fe1 C5 68.5(2) . . ? C2 Fe1 C5 67.8(2) . . ? C8 Fe1 C5 154.1(2) . . ? C9 Fe1 C6 67.7(2) . . ? C4 Fe1 C6 164.5(2) . . ? C10 Fe1 C6 39.5(2) . . ? C7 Fe1 C6 40.70(19) . . ? C3 Fe1 C6 154.6(2) . . ? C2 Fe1 C6 122.2(2) . . ? C8 Fe1 C6 68.1(2) . . ? C5 Fe1 C6 128.66(19) . . ? C9 Fe1 C1 156.5(2) . . ? C4 Fe1 C1 68.6(2) . . ? C10 Fe1 C1 122.6(2) . . ? C7 Fe1 C1 126.7(2) . . ? C3 Fe1 C1 68.8(2) . . ? C2 Fe1 C1 40.68(18) . . ? C8 Fe1 C1 162.1(2) . . ? C5 Fe1 C1 40.4(2) . . ? C6 Fe1 C1 110.7(2) . . ? C5 C1 C2 106.0(4) . . ? C5 C1 B1 122.8(4) . . ? C2 C1 B1 131.1(4) . . ? C5 C1 Fe1 68.8(3) . . ? C2 C1 Fe1 68.3(3) . . ? B1 C1 Fe1 130.4(3) . . ? C3 C2 C1 109.6(4) . . ? C3 C2 Fe1 69.7(3) . . ? C1 C2 Fe1 71.1(3) . . ? C4 C3 C2 107.4(4) . . ? C4 C3 Fe1 69.6(3) . . ? C2 C3 Fe1 69.7(3) . . ? C3 C4 C5 108.1(5) . . ? C3 C4 Fe1 69.7(3) . . ? C5 C4 Fe1 70.1(3) . . ? C1 C5 C4 108.9(4) . . ? C1 C5 Fe1 70.8(2) . . ? C4 C5 Fe1 69.1(3) . . ? C10 C6 C7 108.9(5) . . ? C10 C6 Fe1 69.7(3) . . ? C7 C6 Fe1 69.2(3) . . ? C8 C7 C6 107.7(5) . . ? C8 C7 Fe1 69.9(3) . . ? C6 C7 Fe1 70.1(3) . . ? C7 C8 C9 107.5(4) . . ? C7 C8 Fe1 69.5(3) . . ? C9 C8 Fe1 69.3(3) . . ? C10 C9 C8 107.5(5) . . ? C10 C9 Fe1 69.6(3) . . ? C8 C9 Fe1 69.8(3) . . ? C6 C10 C9 108.5(5) . . ? C6 C10 Fe1 70.8(3) . . ? C9 C10 Fe1 69.5(3) . . ? N1 C11 C14 110.2(4) . . ? N1 C11 C12 112.2(4) . . ? C14 C11 C12 111.1(4) . . ? N1 C11 C13 106.2(4) . . ? C14 C11 C13 108.1(4) . . ? C12 C11 C13 108.8(4) . . ? N2 C15 C18 107.1(4) . . ? N2 C15 C17 110.9(5) . . ? C18 C15 C17 109.1(4) . . ? N2 C15 C16 110.8(4) . . ? C18 C15 C16 108.5(4) . . ? C17 C15 C16 110.3(4) . . ? N4 B2 N3 123.2(4) . . ? N4 B2 C19 122.7(4) . . ? N3 B2 C19 114.0(4) . . ? B2 N3 C29 131.2(4) . . ? B2 N4 C33 132.7(4) . . ? C22 Fe2 C21 41.0(2) . . ? C22 Fe2 C28 117.8(2) . . ? C21 Fe2 C28 152.45(19) . . ? C22 Fe2 C27 102.6(2) . . ? C21 Fe2 C27 117.1(2) . . ? C28 Fe2 C27 40.4(2) . . ? C22 Fe2 C20 68.7(2) . . ? C21 Fe2 C20 41.1(2) . . ? C28 Fe2 C20 164.5(2) . . ? C27 Fe2 C20 154.9(2) . . ? C22 Fe2 C23 41.2(2) . . ? C21 Fe2 C23 68.9(2) . . ? C28 Fe2 C23 106.8(2) . . ? C27 Fe2 C23 121.7(2) . . ? C20 Fe2 C23 68.0(2) . . ? C22 Fe2 C24 155.4(2) . . ? C21 Fe2 C24 163.6(2) . . ? C28 Fe2 C24 40.62(19) . . ? C27 Fe2 C24 68.1(2) . . ? C20 Fe2 C24 128.89(19) . . ? C23 Fe2 C24 123.0(2) . . ? C22 Fe2 C25 159.5(3) . . ? C21 Fe2 C25 125.3(2) . . ? C28 Fe2 C25 68.0(2) . . ? C27 Fe2 C25 68.4(2) . . ? C20 Fe2 C25 111.2(2) . . ? C23 Fe2 C25 159.1(2) . . ? C24 Fe2 C25 40.0(2) . . ? C22 Fe2 C26 120.6(2) . . ? C21 Fe2 C26 105.4(3) . . ? C28 Fe2 C26 67.8(2) . . ? C27 Fe2 C26 40.4(2) . . ? C20 Fe2 C26 122.6(2) . . ? C23 Fe2 C26 157.9(2) . . ? C24 Fe2 C26 67.8(3) . . ? C25 Fe2 C26 40.9(3) . . ? C22 Fe2 C19 69.3(2) . . ? C21 Fe2 C19 69.4(2) . . ? C28 Fe2 C19 126.1(2) . . ? C27 Fe2 C19 160.0(2) . . ? C20 Fe2 C19 40.7(2) . . ? C23 Fe2 C19 40.55(18) . . ? C24 Fe2 C19 111.4(2) . . ? C25 Fe2 C19 125.0(2) . . ? C26 Fe2 C19 159.4(2) . . ? C23 C19 C20 106.3(4) . . ? C23 C19 B2 129.9(4) . . ? C20 C19 B2 123.6(4) . . ? C23 C19 Fe2 68.7(3) . . ? C20 C19 Fe2 68.5(3) . . ? B2 C19 Fe2 130.9(3) . . ? C21 C20 C19 109.5(4) . . ? C21 C20 Fe2 69.2(3) . . ? C19 C20 Fe2 70.8(3) . . ? C22 C21 C20 107.1(5) . . ? C22 C21 Fe2 69.0(3) . . ? C20 C21 Fe2 69.7(3) . . ? C21 C22 C23 108.2(4) . . ? C21 C22 Fe2 70.1(3) . . ? C23 C22 Fe2 70.3(3) . . ? C19 C23 C22 109.0(4) . . ? C19 C23 Fe2 70.7(3) . . ? C22 C23 Fe2 68.5(3) . . ? C25 C24 C28 108.4(5) . . ? C25 C24 Fe2 70.1(3) . . ? C28 C24 Fe2 69.4(3) . . ? C24 C25 C26 107.6(5) . . ? C24 C25 Fe2 69.9(3) . . ? C26 C25 Fe2 69.8(3) . . ? C27 C26 C25 107.8(5) . . ? C27 C26 Fe2 69.3(4) . . ? C25 C26 Fe2 69.3(4) . . ? C28 C27 C26 108.0(5) . . ? C28 C27 Fe2 69.7(3) . . ? C26 C27 Fe2 70.4(3) . . ? C27 C28 C24 108.2(5) . . ? C27 C28 Fe2 69.9(3) . . ? C24 C28 Fe2 70.0(3) . . ? N3 C29 C32 110.3(4) . . ? N3 C29 C30 110.9(4) . . ? C32 C29 C30 111.7(5) . . ? N3 C29 C31 106.2(5) . . ? C32 C29 C31 108.7(4) . . ? C30 C29 C31 108.9(5) . . ? N4 C33 C35 110.8(4) . . ? N4 C33 C36 110.2(5) . . ? C35 C33 C36 110.6(4) . . ? N4 C33 C34 106.9(4) . . ? C35 C33 C34 108.2(5) . . ? C36 C33 C34 110.1(4) . . ? _diffrn_measured_fraction_theta_max 0.943 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.943 _refine_diff_density_max 0.289 _refine_diff_density_min -0.365 _refine_diff_density_rms 0.072 #===END data_Compound1b _database_code_depnum_ccdc_archive 'CCDC 773248' #TrackingRef '- Newbams_revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H45 B Fe N2' _chemical_formula_sum 'C34 H45 B Fe N2' _chemical_formula_weight 548.38 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.451(4) _cell_length_b 10.016(2) _cell_length_c 28.699(6) _cell_angle_alpha 90.00 _cell_angle_beta 99.88(3) _cell_angle_gamma 90.00 _cell_volume 6075(2) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 30049 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 27.46 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.199 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2352 _exptl_absorpt_coefficient_mu 0.521 _exptl_absorpt_correction_type Integration _exptl_absorpt_correction_T_min 0.9030 _exptl_absorpt_correction_T_max 0.9795 _exptl_absorpt_process_details 'HKL Scalepack (Otwinowski and Minor 1997)' _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 'Nonius Kappa CCD' _diffrn_measurement_method 'phi\omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30049 _diffrn_reflns_av_R_equivalents 0.0583 _diffrn_reflns_av_sigmaI/netI 0.0785 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 27.46 _reflns_number_total 6921 _reflns_number_gt 4350 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Nonius DENZO' _computing_data_reduction 'Nonius DENZO' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0585P)^2^+2.6635P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6921 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1062 _refine_ls_R_factor_gt 0.0525 _refine_ls_wR_factor_ref 0.1380 _refine_ls_wR_factor_gt 0.1189 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _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 B1 B 0.32076(13) 0.4042(3) -0.11059(9) 0.0254(6) Uani 1 1 d . . . N1 N 0.25897(9) 0.3499(2) -0.11487(7) 0.0261(5) Uani 1 1 d . . . H1A H 0.2525 0.2918 -0.0932 0.031 Uiso 1 1 calc R . . N2 N 0.33181(9) 0.5083(2) -0.14171(7) 0.0287(5) Uani 1 1 d . . . H2A H 0.2976 0.5465 -0.1574 0.034 Uiso 1 1 calc R . . Fe1 Fe 0.383748(18) 0.36774(4) 0.000315(12) 0.03265(13) Uani 1 1 d . . . C1 C 0.37485(12) 0.3461(3) -0.07213(8) 0.0279(6) Uani 1 1 d . . . C2 C 0.43401(12) 0.4071(3) -0.05254(8) 0.0330(6) Uani 1 1 d . . . H2B H 0.4484 0.4974 -0.0610 0.040 Uiso 1 1 calc R . . C3 C 0.46850(13) 0.3195(3) -0.01857(9) 0.0417(7) Uani 1 1 d . . . H3A H 0.5113 0.3371 0.0005 0.050 Uiso 1 1 calc R . . C4 C 0.43176(14) 0.2036(3) -0.01642(10) 0.0437(7) Uani 1 1 d . . . H4A H 0.4439 0.1245 0.0044 0.052 Uiso 1 1 calc R . . C5 C 0.37437(13) 0.2193(3) -0.04888(9) 0.0346(6) Uani 1 1 d . . . H5A H 0.3391 0.1528 -0.0545 0.041 Uiso 1 1 calc R . . C6 C 0.31020(17) 0.4782(5) 0.01458(11) 0.0667(12) Uani 1 1 d . . . H6A H 0.2746 0.5143 -0.0092 0.080 Uiso 1 1 calc R . . C7 C 0.31137(17) 0.3537(5) 0.03740(11) 0.0681(12) Uani 1 1 d . . . H7A H 0.2768 0.2854 0.0324 0.082 Uiso 1 1 calc R . . C8 C 0.36966(16) 0.3419(4) 0.06863(10) 0.0524(9) Uani 1 1 d . . . H8A H 0.3839 0.2641 0.0896 0.063 Uiso 1 1 calc R . . C9 C 0.40350(15) 0.4601(3) 0.06495(10) 0.0461(8) Uani 1 1 d . . . H9A H 0.4468 0.4806 0.0827 0.055 Uiso 1 1 calc R . . C10 C 0.36722(18) 0.5435(4) 0.03167(11) 0.0557(9) Uani 1 1 d . . . H10A H 0.3797 0.6342 0.0220 0.067 Uiso 1 1 calc R . . C11 C 0.20581(11) 0.3804(3) -0.15115(8) 0.0264(5) Uani 1 1 d . . . C12 C 0.16895(12) 0.4936(3) -0.14683(9) 0.0332(6) Uani 1 1 d . . . C13 C 0.11624(13) 0.5168(3) -0.18191(11) 0.0424(7) Uani 1 1 d . . . H13A H 0.0903 0.5924 -0.1793 0.051 Uiso 1 1 calc R . . C14 C 0.10093(13) 0.4329(3) -0.22011(10) 0.0424(7) Uani 1 1 d . . . H14A H 0.0647 0.4505 -0.2433 0.051 Uiso 1 1 calc R . . C15 C 0.13798(13) 0.3243(3) -0.22456(10) 0.0381(7) Uani 1 1 d . . . H15A H 0.1273 0.2672 -0.2512 0.046 Uiso 1 1 calc R . . C16 C 0.19151(12) 0.2953(3) -0.19055(9) 0.0289(6) Uani 1 1 d . . . C17 C 0.18408(15) 0.5882(3) -0.10471(10) 0.0416(7) Uani 1 1 d . . . H17A H 0.2293 0.5734 -0.0900 0.050 Uiso 1 1 calc R . . C18 C 0.1433(2) 0.5563(4) -0.06735(12) 0.0646(10) Uani 1 1 d . . . H18A H 0.1538 0.6181 -0.0407 0.097 Uiso 1 1 calc R . . H18B H 0.1515 0.4645 -0.0562 0.097 Uiso 1 1 calc R . . H18C H 0.0985 0.5659 -0.0813 0.097 Uiso 1 1 calc R . . C19 C 0.17710(17) 0.7339(3) -0.11963(13) 0.0562(9) Uani 1 1 d . . . H19A H 0.2036 0.7519 -0.1435 0.084 Uiso 1 1 calc R . . H19B H 0.1904 0.7912 -0.0920 0.084 Uiso 1 1 calc R . . H19C H 0.1328 0.7524 -0.1329 0.084 Uiso 1 1 calc R . . C20 C 0.23021(13) 0.1714(3) -0.19549(9) 0.0354(6) Uani 1 1 d . . . H20A H 0.2733 0.1857 -0.1765 0.043 Uiso 1 1 calc R . . C21 C 0.20096(19) 0.0513(3) -0.17455(14) 0.0653(10) Uani 1 1 d . . . H21A H 0.1960 0.0714 -0.1419 0.098 Uiso 1 1 calc R . . H21B H 0.2286 -0.0264 -0.1748 0.098 Uiso 1 1 calc R . . H21C H 0.1594 0.0320 -0.1935 0.098 Uiso 1 1 calc R . . C22 C 0.23814(17) 0.1418(4) -0.24619(11) 0.0594(10) Uani 1 1 d . . . H22A H 0.2569 0.2194 -0.2593 0.089 Uiso 1 1 calc R . . H22B H 0.1967 0.1227 -0.2653 0.089 Uiso 1 1 calc R . . H22C H 0.2659 0.0643 -0.2466 0.089 Uiso 1 1 calc R . . C23 C 0.39048(12) 0.5604(3) -0.15139(8) 0.0279(6) Uani 1 1 d . . . C24 C 0.43271(12) 0.4757(3) -0.16937(9) 0.0317(6) Uani 1 1 d . . . C25 C 0.48819(13) 0.5306(3) -0.18013(9) 0.0396(7) Uani 1 1 d . . . H25A H 0.5173 0.4745 -0.1923 0.048 Uiso 1 1 calc R . . C26 C 0.50176(14) 0.6644(3) -0.17357(10) 0.0444(8) Uani 1 1 d . . . H26A H 0.5398 0.6998 -0.1812 0.053 Uiso 1 1 calc R . . C27 C 0.46017(14) 0.7464(3) -0.15595(10) 0.0414(7) Uani 1 1 d . . . H27A H 0.4700 0.8384 -0.1513 0.050 Uiso 1 1 calc R . . C28 C 0.40361(13) 0.6974(3) -0.14476(9) 0.0334(6) Uani 1 1 d . . . C29 C 0.41922(14) 0.3282(3) -0.17958(10) 0.0368(6) Uani 1 1 d . . . H29A H 0.3827 0.3026 -0.1640 0.044 Uiso 1 1 calc R . . C30 C 0.47480(17) 0.2395(4) -0.15915(15) 0.0646(10) Uani 1 1 d . . . H30A H 0.4640 0.1460 -0.1666 0.097 Uiso 1 1 calc R . . H30B H 0.4843 0.2511 -0.1247 0.097 Uiso 1 1 calc R . . H30C H 0.5119 0.2643 -0.1729 0.097 Uiso 1 1 calc R . . C31 C 0.3991(2) 0.3060(4) -0.23247(12) 0.0731(12) Uani 1 1 d . . . H31A H 0.3906 0.2109 -0.2386 0.110 Uiso 1 1 calc R . . H31B H 0.4331 0.3350 -0.2490 0.110 Uiso 1 1 calc R . . H31C H 0.3607 0.3577 -0.2439 0.110 Uiso 1 1 calc R . . C32 C 0.35771(15) 0.7890(3) -0.12534(10) 0.0418(7) Uani 1 1 d . . . H32A H 0.3140 0.7608 -0.1398 0.050 Uiso 1 1 calc R . . C33 C 0.36349(18) 0.7735(4) -0.07202(12) 0.0615(10) Uani 1 1 d . . . H33A H 0.3593 0.6790 -0.0642 0.092 Uiso 1 1 calc R . . H33C H 0.3300 0.8250 -0.0610 0.092 Uiso 1 1 calc R . . H33D H 0.4049 0.8064 -0.0565 0.092 Uiso 1 1 calc R . . C34 C 0.3643(2) 0.9365(3) -0.13726(13) 0.0648(10) Uani 1 1 d . . . H34C H 0.3606 0.9470 -0.1716 0.097 Uiso 1 1 calc R . . H34D H 0.4058 0.9693 -0.1217 0.097 Uiso 1 1 calc R . . H34A H 0.3309 0.9879 -0.1261 0.097 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 B1 0.0296(15) 0.0268(14) 0.0214(13) -0.0035(11) 0.0090(11) 0.0029(12) N1 0.0276(11) 0.0279(11) 0.0227(10) 0.0037(9) 0.0042(8) -0.0012(9) N2 0.0245(11) 0.0325(12) 0.0299(11) 0.0055(10) 0.0067(9) -0.0001(9) Fe1 0.0348(2) 0.0415(2) 0.02141(19) 0.00001(17) 0.00410(14) -0.00588(19) C1 0.0318(14) 0.0304(14) 0.0219(11) -0.0034(11) 0.0059(10) -0.0015(11) C2 0.0312(14) 0.0435(16) 0.0247(12) -0.0007(12) 0.0057(10) -0.0043(12) C3 0.0327(15) 0.061(2) 0.0294(14) 0.0015(14) -0.0010(11) 0.0015(14) C4 0.0460(18) 0.0468(18) 0.0353(15) 0.0059(14) -0.0010(13) 0.0065(15) C5 0.0370(15) 0.0352(15) 0.0302(13) -0.0001(12) 0.0020(11) -0.0007(12) C6 0.052(2) 0.121(4) 0.0274(15) -0.011(2) 0.0085(14) 0.027(2) C7 0.052(2) 0.123(4) 0.0328(16) -0.015(2) 0.0175(15) -0.037(2) C8 0.070(2) 0.065(2) 0.0237(13) -0.0005(14) 0.0103(14) -0.0180(18) C9 0.0493(19) 0.061(2) 0.0294(14) -0.0109(15) 0.0105(13) -0.0127(16) C10 0.082(3) 0.054(2) 0.0369(16) -0.0052(16) 0.0263(17) 0.0076(19) C11 0.0240(12) 0.0296(14) 0.0264(12) 0.0050(11) 0.0063(9) -0.0020(11) C12 0.0319(15) 0.0344(15) 0.0351(14) 0.0030(12) 0.0112(11) 0.0034(12) C13 0.0326(15) 0.0423(17) 0.0536(18) 0.0115(15) 0.0110(13) 0.0105(13) C14 0.0290(15) 0.0517(19) 0.0432(16) 0.0123(15) -0.0028(12) 0.0017(14) C15 0.0345(15) 0.0460(17) 0.0322(14) 0.0018(13) 0.0011(11) -0.0066(13) C16 0.0285(13) 0.0313(14) 0.0275(12) 0.0023(11) 0.0069(10) -0.0030(11) C17 0.0444(17) 0.0373(16) 0.0456(16) -0.0024(14) 0.0144(13) 0.0072(13) C18 0.094(3) 0.054(2) 0.054(2) -0.0057(18) 0.035(2) 0.001(2) C19 0.063(2) 0.0364(17) 0.072(2) -0.0051(17) 0.0199(18) 0.0034(16) C20 0.0395(16) 0.0358(15) 0.0303(13) -0.0061(12) 0.0041(11) -0.0003(12) C21 0.085(3) 0.0327(18) 0.084(3) -0.0004(18) 0.030(2) -0.0020(17) C22 0.059(2) 0.077(3) 0.0425(17) -0.0150(18) 0.0115(15) 0.0147(19) C23 0.0264(13) 0.0333(14) 0.0239(12) 0.0069(11) 0.0041(10) -0.0019(11) C24 0.0313(15) 0.0385(16) 0.0259(12) 0.0035(12) 0.0066(10) -0.0015(12) C25 0.0346(15) 0.0529(18) 0.0339(14) 0.0028(14) 0.0132(12) -0.0012(14) C26 0.0336(16) 0.058(2) 0.0426(16) 0.0110(15) 0.0080(13) -0.0129(14) C27 0.0433(17) 0.0394(17) 0.0404(16) 0.0063(13) 0.0041(13) -0.0124(14) C28 0.0375(15) 0.0328(15) 0.0289(13) 0.0048(12) 0.0030(11) -0.0045(12) C29 0.0389(16) 0.0374(16) 0.0373(15) -0.0029(13) 0.0157(12) -0.0006(13) C30 0.057(2) 0.050(2) 0.088(3) 0.011(2) 0.0145(19) 0.0119(17) C31 0.117(3) 0.055(2) 0.0435(19) -0.0112(18) 0.004(2) -0.011(2) C32 0.0472(18) 0.0337(16) 0.0434(16) -0.0009(14) 0.0043(13) 0.0025(13) C33 0.083(3) 0.056(2) 0.0487(19) -0.0009(17) 0.0193(18) 0.0132(19) C34 0.091(3) 0.042(2) 0.060(2) 0.0053(18) 0.011(2) 0.0075(19) _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 B1 N1 1.418(4) . ? B1 N2 1.419(3) . ? B1 C1 1.569(4) . ? N1 C11 1.439(3) . ? N2 C23 1.433(3) . ? Fe1 C6 2.025(3) . ? Fe1 C7 2.032(3) . ? Fe1 C10 2.036(3) . ? Fe1 C5 2.037(3) . ? Fe1 C4 2.041(3) . ? Fe1 C3 2.042(3) . ? Fe1 C2 2.044(3) . ? Fe1 C9 2.051(3) . ? Fe1 C8 2.051(3) . ? Fe1 C1 2.066(2) . ? C1 C2 1.433(4) . ? C1 C5 1.436(4) . ? C2 C3 1.421(4) . ? C3 C4 1.411(4) . ? C4 C5 1.419(4) . ? C6 C10 1.400(5) . ? C6 C7 1.406(6) . ? C7 C8 1.413(5) . ? C8 C9 1.402(4) . ? C9 C10 1.401(5) . ? C11 C12 1.400(4) . ? C11 C16 1.408(4) . ? C12 C13 1.398(4) . ? C12 C17 1.526(4) . ? C13 C14 1.376(4) . ? C14 C15 1.366(4) . ? C15 C16 1.404(4) . ? C16 C20 1.513(4) . ? C17 C19 1.521(4) . ? C17 C18 1.529(4) . ? C20 C22 1.523(4) . ? C20 C21 1.527(4) . ? C23 C24 1.403(4) . ? C23 C28 1.407(4) . ? C24 C25 1.393(4) . ? C24 C29 1.524(4) . ? C25 C26 1.377(4) . ? C26 C27 1.372(4) . ? C27 C28 1.396(4) . ? C28 C32 1.520(4) . ? C29 C31 1.521(4) . ? C29 C30 1.521(4) . ? C32 C33 1.522(4) . ? C32 C34 1.529(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 N1 B1 N2 118.8(2) . . ? N1 B1 C1 119.1(2) . . ? N2 B1 C1 122.1(2) . . ? B1 N1 C11 126.5(2) . . ? B1 N2 C23 129.5(2) . . ? C6 Fe1 C7 40.56(16) . . ? C6 Fe1 C10 40.32(15) . . ? C7 Fe1 C10 67.77(16) . . ? C6 Fe1 C5 123.46(13) . . ? C7 Fe1 C5 108.61(14) . . ? C10 Fe1 C5 159.05(13) . . ? C6 Fe1 C4 158.39(16) . . ? C7 Fe1 C4 121.96(16) . . ? C10 Fe1 C4 159.07(14) . . ? C5 Fe1 C4 40.74(11) . . ? C6 Fe1 C3 160.51(16) . . ? C7 Fe1 C3 156.57(16) . . ? C10 Fe1 C3 123.53(14) . . ? C5 Fe1 C3 68.27(12) . . ? C4 Fe1 C3 40.42(12) . . ? C6 Fe1 C2 124.96(14) . . ? C7 Fe1 C2 161.70(13) . . ? C10 Fe1 C2 108.38(13) . . ? C5 Fe1 C2 68.18(11) . . ? C4 Fe1 C2 68.22(12) . . ? C3 Fe1 C2 40.70(11) . . ? C6 Fe1 C9 67.55(13) . . ? C7 Fe1 C9 67.38(13) . . ? C10 Fe1 C9 40.09(13) . . ? C5 Fe1 C9 159.51(12) . . ? C4 Fe1 C9 122.81(13) . . ? C3 Fe1 C9 106.95(12) . . ? C2 Fe1 C9 122.06(11) . . ? C6 Fe1 C8 68.16(15) . . ? C7 Fe1 C8 40.49(13) . . ? C10 Fe1 C8 67.74(14) . . ? C5 Fe1 C8 123.87(12) . . ? C4 Fe1 C8 106.64(14) . . ? C3 Fe1 C8 120.52(13) . . ? C2 Fe1 C8 156.44(12) . . ? C9 Fe1 C8 39.97(12) . . ? C6 Fe1 C1 108.66(12) . . ? C7 Fe1 C1 124.94(12) . . ? C10 Fe1 C1 122.84(12) . . ? C5 Fe1 C1 40.96(10) . . ? C4 Fe1 C1 69.02(11) . . ? C3 Fe1 C1 68.95(10) . . ? C2 Fe1 C1 40.81(10) . . ? C9 Fe1 C1 157.89(12) . . ? C8 Fe1 C1 160.97(11) . . ? C2 C1 C5 105.7(2) . . ? C2 C1 B1 128.0(2) . . ? C5 C1 B1 126.2(2) . . ? C2 C1 Fe1 68.77(14) . . ? C5 C1 Fe1 68.41(14) . . ? B1 C1 Fe1 126.74(17) . . ? C3 C2 C1 109.1(2) . . ? C3 C2 Fe1 69.57(15) . . ? C1 C2 Fe1 70.42(14) . . ? C4 C3 C2 108.0(2) . . ? C4 C3 Fe1 69.73(17) . . ? C2 C3 Fe1 69.73(16) . . ? C3 C4 C5 108.0(3) . . ? C3 C4 Fe1 69.85(18) . . ? C5 C4 Fe1 69.48(17) . . ? C4 C5 C1 109.2(2) . . ? C4 C5 Fe1 69.78(17) . . ? C1 C5 Fe1 70.62(15) . . ? C10 C6 C7 107.9(3) . . ? C10 C6 Fe1 70.25(19) . . ? C7 C6 Fe1 70.0(2) . . ? C6 C7 C8 108.2(3) . . ? C6 C7 Fe1 69.45(19) . . ? C8 C7 Fe1 70.46(18) . . ? C9 C8 C7 107.1(3) . . ? C9 C8 Fe1 70.01(16) . . ? C7 C8 Fe1 69.06(17) . . ? C10 C9 C8 108.7(3) . . ? C10 C9 Fe1 69.39(17) . . ? C8 C9 Fe1 70.01(16) . . ? C6 C10 C9 108.0(3) . . ? C6 C10 Fe1 69.4(2) . . ? C9 C10 Fe1 70.52(19) . . ? C12 C11 C16 120.9(2) . . ? C12 C11 N1 119.8(2) . . ? C16 C11 N1 119.3(2) . . ? C13 C12 C11 118.1(3) . . ? C13 C12 C17 120.2(3) . . ? C11 C12 C17 121.8(2) . . ? C14 C13 C12 121.7(3) . . ? C15 C14 C13 119.9(3) . . ? C14 C15 C16 121.3(3) . . ? C15 C16 C11 118.2(2) . . ? C15 C16 C20 120.1(2) . . ? C11 C16 C20 121.6(2) . . ? C19 C17 C12 112.0(3) . . ? C19 C17 C18 110.9(3) . . ? C12 C17 C18 110.9(3) . . ? C16 C20 C22 113.7(2) . . ? C16 C20 C21 109.9(2) . . ? C22 C20 C21 110.1(3) . . ? C24 C23 C28 120.8(2) . . ? C24 C23 N2 119.7(2) . . ? C28 C23 N2 119.4(2) . . ? C25 C24 C23 118.2(3) . . ? C25 C24 C29 118.8(3) . . ? C23 C24 C29 122.9(2) . . ? C26 C25 C24 121.5(3) . . ? C27 C26 C25 119.8(3) . . ? C26 C27 C28 121.3(3) . . ? C27 C28 C23 118.3(3) . . ? C27 C28 C32 121.0(3) . . ? C23 C28 C32 120.7(2) . . ? C31 C29 C30 111.6(3) . . ? C31 C29 C24 110.2(2) . . ? C30 C29 C24 112.4(3) . . ? C28 C32 C33 111.1(2) . . ? C28 C32 C34 114.2(3) . . ? C33 C32 C34 109.2(3) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.417 _refine_diff_density_min -0.408 _refine_diff_density_rms 0.083 #===END data_Compound2 _database_code_depnum_ccdc_archive 'CCDC 773249' #TrackingRef '- Newbams_revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H48 B2 Fe N4' _chemical_formula_sum 'C26 H48 B2 Fe N4' _chemical_formula_weight 494.15 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' Fe Fe 0.3463 0.8444 '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 10.265(2) _cell_length_b 12.189(2) _cell_length_c 13.101(3) _cell_angle_alpha 109.70(3) _cell_angle_beta 102.12(3) _cell_angle_gamma 103.19(3) _cell_volume 1427.2(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 24390 _cell_measurement_theta_min 2.97 _cell_measurement_theta_max 25.03 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.150 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 536 _exptl_absorpt_coefficient_mu 0.548 _exptl_absorpt_correction_type Integration _exptl_absorpt_correction_T_min 0.8106 _exptl_absorpt_correction_T_max 0.8442 _exptl_absorpt_process_details 'HKL Scalepack (Otwinowski and Minor 1997)' _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 'Nonius Kappa CCD' _diffrn_measurement_method 'Phi\omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24390 _diffrn_reflns_av_R_equivalents 0.0200 _diffrn_reflns_av_sigmaI/netI 0.0286 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 25.03 _reflns_number_total 5021 _reflns_number_gt 4265 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Nonius DENZO' _computing_data_reduction 'Nonius DENZO' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0464P)^2^+0.8008P] 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 5021 _refine_ls_number_parameters 314 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0462 _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_ref 0.0966 _refine_ls_wR_factor_gt 0.0907 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 C1 C 0.25927(18) 0.13742(17) 0.89139(15) 0.0237(4) Uani 1 1 d . . . C2 C 0.2359(2) 0.01568(17) 0.88716(17) 0.0288(4) Uani 1 1 d . . . H2A H 0.2532 -0.0057 0.9550 0.035 Uiso 1 1 calc R . . C3 C 0.1846(2) -0.07057(18) 0.77095(19) 0.0346(5) Uani 1 1 d . . . H3A H 0.1584 -0.1622 0.7435 0.042 Uiso 1 1 calc R . . C4 C 0.1766(2) -0.0038(2) 0.70138(17) 0.0338(5) Uani 1 1 d . . . H4A H 0.1436 -0.0396 0.6160 0.041 Uiso 1 1 calc R . . C5 C 0.22242(19) 0.12345(19) 0.77491(16) 0.0278(4) Uani 1 1 d . . . H5A H 0.2290 0.1925 0.7493 0.033 Uiso 1 1 calc R . . Fe1 Fe 0.37950(3) 0.04867(2) 0.80427(2) 0.02296(10) Uani 1 1 d . . . C6 C 0.50120(18) -0.03618(17) 0.71506(16) 0.0244(4) Uani 1 1 d . . . C7 C 0.5240(2) 0.08745(17) 0.72413(17) 0.0281(4) Uani 1 1 d . . . H7A H 0.5076 0.1124 0.6585 0.034 Uiso 1 1 calc R . . C8 C 0.57424(19) 0.16928(17) 0.84173(18) 0.0306(5) Uani 1 1 d . . . H8A H 0.6004 0.2611 0.8725 0.037 Uiso 1 1 calc R . . C9 C 0.5815(2) 0.09829(18) 0.90718(17) 0.0306(5) Uani 1 1 d . . . H9A H 0.6136 0.1306 0.9924 0.037 Uiso 1 1 calc R . . C10 C 0.53604(19) -0.02819(18) 0.82951(16) 0.0273(4) Uani 1 1 d . . . H10A H 0.5288 -0.0997 0.8517 0.033 Uiso 1 1 calc R . . B1 B 0.3044(2) 0.26040(19) 1.00341(18) 0.0242(4) Uani 1 1 d . . . N1 N 0.45016(17) 0.31593(15) 1.06387(14) 0.0286(4) Uani 1 1 d . . . H1 H 0.502(2) 0.280(2) 1.0321(19) 0.030(6) Uiso 1 1 d . . . N2 N 0.20297(18) 0.30977(17) 1.04139(15) 0.0342(4) Uani 1 1 d . . . H2 H 0.236(3) 0.377(2) 1.095(2) 0.045(7) Uiso 1 1 d . . . C11 C 0.5310(2) 0.42612(19) 1.17062(17) 0.0312(5) Uani 1 1 d . . . C12 C 0.4844(2) 0.4133(2) 1.27023(17) 0.0386(5) Uani 1 1 d . . . H12A H 0.4963 0.3384 1.2776 0.058 Uiso 1 1 calc R . . H12B H 0.3851 0.4078 1.2564 0.058 Uiso 1 1 calc R . . H12C H 0.5420 0.4852 1.3408 0.058 Uiso 1 1 calc R . . C13 C 0.5122(3) 0.5427(2) 1.15866(19) 0.0468(6) Uani 1 1 d . . . H13A H 0.4128 0.5372 1.1447 0.070 Uiso 1 1 calc R . . H13B H 0.5421 0.5508 1.0945 0.070 Uiso 1 1 calc R . . H13C H 0.5696 0.6149 1.2291 0.070 Uiso 1 1 calc R . . C14 C 0.6856(2) 0.4352(3) 1.1937(2) 0.0662(9) Uani 1 1 d . . . H14A H 0.6976 0.3606 1.2014 0.099 Uiso 1 1 calc R . . H14B H 0.7423 0.5073 1.2644 0.099 Uiso 1 1 calc R . . H14C H 0.7166 0.4437 1.1301 0.099 Uiso 1 1 calc R . . C15 C 0.0484(2) 0.27167(19) 0.99556(18) 0.0334(5) Uani 1 1 d . . . C16 C -0.0189(2) 0.1352(2) 0.9613(3) 0.0545(7) Uani 1 1 d . . . H16A H 0.0066 0.1154 1.0278 0.082 Uiso 1 1 calc R . . H16B H 0.0145 0.0885 0.9014 0.082 Uiso 1 1 calc R . . H16C H -0.1216 0.1133 0.9327 0.082 Uiso 1 1 calc R . . C17 C 0.0056(3) 0.3020(3) 0.8928(3) 0.0710(9) Uani 1 1 d . . . H17A H 0.0483 0.3905 0.9147 0.107 Uiso 1 1 calc R . . H17B H -0.0972 0.2796 0.8655 0.107 Uiso 1 1 calc R . . H17C H 0.0380 0.2556 0.8320 0.107 Uiso 1 1 calc R . . C18 C -0.0044(3) 0.3408(3) 1.0895(3) 0.0771(11) Uani 1 1 d . . . H18A H 0.0235 0.3206 1.1555 0.116 Uiso 1 1 calc R . . H18B H -0.1074 0.3167 1.0614 0.116 Uiso 1 1 calc R . . H18C H 0.0365 0.4296 1.1123 0.116 Uiso 1 1 calc R . . B2 B 0.4569(2) -0.15733(19) 0.60147(18) 0.0246(4) Uani 1 1 d . . . N3 N 0.31116(17) -0.22354(15) 0.55106(15) 0.0310(4) Uani 1 1 d . . . H3 H 0.264(2) -0.192(2) 0.5901(19) 0.030(6) Uiso 1 1 d . . . N4 N 0.55863(17) -0.19592(16) 0.55397(15) 0.0310(4) Uani 1 1 d . . . H4 H 0.532(2) -0.262(2) 0.500(2) 0.037(7) Uiso 1 1 d . . . C19 C 0.2273(2) -0.33603(18) 0.44800(17) 0.0317(5) Uani 1 1 d . . . C20 C 0.0729(2) -0.3479(3) 0.4314(2) 0.0618(8) Uani 1 1 d . . . H20A H 0.0563 -0.2750 0.4226 0.093 Uiso 1 1 calc R . . H20B H 0.0486 -0.3544 0.4980 0.093 Uiso 1 1 calc R . . H20C H 0.0143 -0.4218 0.3629 0.093 Uiso 1 1 calc R . . C21 C 0.2624(3) -0.3268(2) 0.34245(18) 0.0428(6) Uani 1 1 d . . . H21A H 0.2451 -0.2542 0.3337 0.064 Uiso 1 1 calc R . . H21B H 0.2027 -0.4010 0.2745 0.064 Uiso 1 1 calc R . . H21C H 0.3616 -0.3194 0.3517 0.064 Uiso 1 1 calc R . . C22 C 0.2540(3) -0.4490(2) 0.4618(2) 0.0436(5) Uani 1 1 d . . . H22A H 0.2312 -0.4549 0.5292 0.065 Uiso 1 1 calc R . . H22B H 0.3533 -0.4416 0.4714 0.065 Uiso 1 1 calc R . . H22C H 0.1945 -0.5232 0.3939 0.065 Uiso 1 1 calc R . . C23 C 0.7146(2) -0.14628(18) 0.59082(17) 0.0306(4) Uani 1 1 d . . . C24 C 0.7625(2) -0.2188(2) 0.4946(2) 0.0527(7) Uani 1 1 d . . . H24A H 0.7312 -0.3062 0.4805 0.079 Uiso 1 1 calc R . . H24B H 0.8655 -0.1882 0.5162 0.079 Uiso 1 1 calc R . . H24C H 0.7216 -0.2085 0.4251 0.079 Uiso 1 1 calc R . . C25 C 0.7782(2) -0.1630(2) 0.6980(2) 0.0473(6) Uani 1 1 d . . . H25A H 0.7454 -0.2505 0.6838 0.071 Uiso 1 1 calc R . . H25B H 0.7491 -0.1155 0.7606 0.071 Uiso 1 1 calc R . . H25C H 0.8812 -0.1339 0.7187 0.071 Uiso 1 1 calc R . . C26 C 0.7651(2) -0.0107(2) 0.6108(2) 0.0457(6) Uani 1 1 d . . . H26A H 0.7235 -0.0012 0.5411 0.069 Uiso 1 1 calc R . . H26B H 0.8680 0.0185 0.6311 0.069 Uiso 1 1 calc R . . H26C H 0.7363 0.0378 0.6732 0.069 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 C1 0.0182(9) 0.0245(9) 0.0254(10) 0.0056(8) 0.0077(7) 0.0076(8) C2 0.0249(10) 0.0259(10) 0.0368(11) 0.0101(9) 0.0152(8) 0.0094(8) C3 0.0227(10) 0.0233(10) 0.0455(12) -0.0004(9) 0.0151(9) 0.0030(8) C4 0.0195(10) 0.0407(12) 0.0253(10) -0.0029(9) 0.0049(8) 0.0081(9) C5 0.0211(9) 0.0347(11) 0.0255(10) 0.0086(8) 0.0068(8) 0.0114(8) Fe1 0.01802(15) 0.02130(16) 0.02344(16) 0.00243(11) 0.00672(11) 0.00526(11) C6 0.0174(9) 0.0251(10) 0.0260(10) 0.0040(8) 0.0083(7) 0.0070(8) C7 0.0251(10) 0.0251(10) 0.0331(11) 0.0082(8) 0.0140(8) 0.0071(8) C8 0.0195(9) 0.0214(10) 0.0405(12) 0.0007(9) 0.0118(8) 0.0040(8) C9 0.0199(9) 0.0317(11) 0.0279(10) -0.0010(8) 0.0043(8) 0.0094(8) C10 0.0238(10) 0.0278(10) 0.0270(10) 0.0053(8) 0.0077(8) 0.0112(8) B1 0.0249(11) 0.0213(10) 0.0238(11) 0.0066(9) 0.0069(8) 0.0070(9) N1 0.0223(8) 0.0276(9) 0.0260(9) -0.0005(7) 0.0082(7) 0.0070(7) N2 0.0243(9) 0.0283(9) 0.0319(10) -0.0058(8) 0.0020(7) 0.0095(8) C11 0.0245(10) 0.0298(11) 0.0249(10) -0.0002(8) 0.0053(8) 0.0018(8) C12 0.0427(13) 0.0367(12) 0.0267(11) 0.0083(9) 0.0050(9) 0.0079(10) C13 0.0640(16) 0.0273(11) 0.0304(11) 0.0047(9) 0.0093(11) -0.0029(11) C14 0.0254(12) 0.0739(19) 0.0528(16) -0.0150(14) 0.0019(11) 0.0034(12) C15 0.0231(10) 0.0318(11) 0.0358(11) 0.0020(9) 0.0058(8) 0.0127(9) C16 0.0285(12) 0.0404(14) 0.087(2) 0.0152(13) 0.0221(13) 0.0101(11) C17 0.0424(15) 0.098(2) 0.087(2) 0.057(2) 0.0077(15) 0.0284(16) C18 0.0331(14) 0.085(2) 0.0657(19) -0.0253(16) 0.0081(13) 0.0253(14) B2 0.0226(10) 0.0227(10) 0.0240(11) 0.0053(9) 0.0070(8) 0.0062(9) N3 0.0222(8) 0.0292(9) 0.0302(9) -0.0014(7) 0.0091(7) 0.0076(7) N4 0.0216(8) 0.0264(9) 0.0280(9) -0.0052(8) 0.0063(7) 0.0033(7) C19 0.0235(10) 0.0262(10) 0.0320(11) 0.0013(9) 0.0035(8) 0.0043(8) C20 0.0239(12) 0.0553(16) 0.0659(18) -0.0106(13) 0.0030(11) 0.0035(11) C21 0.0476(14) 0.0349(12) 0.0283(11) 0.0047(10) 0.0000(10) 0.0049(10) C22 0.0489(14) 0.0295(11) 0.0389(12) 0.0075(10) 0.0066(10) 0.0045(10) C23 0.0223(10) 0.0287(10) 0.0314(11) 0.0016(8) 0.0095(8) 0.0064(8) C24 0.0304(12) 0.0517(15) 0.0524(15) -0.0071(12) 0.0188(11) 0.0086(11) C25 0.0277(11) 0.0591(15) 0.0516(15) 0.0219(12) 0.0082(10) 0.0124(11) C26 0.0294(11) 0.0363(12) 0.0682(16) 0.0159(12) 0.0205(11) 0.0081(10) _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 C1 C2 1.428(3) . ? C1 C5 1.433(3) . ? C1 B1 1.591(3) . ? C1 Fe1 2.0891(19) . ? C2 C3 1.426(3) . ? C2 Fe1 2.052(2) . ? C3 C4 1.414(3) . ? C3 Fe1 2.045(2) . ? C4 C5 1.423(3) . ? C4 Fe1 2.048(2) . ? C5 Fe1 2.056(2) . ? Fe1 C8 2.039(2) . ? Fe1 C9 2.046(2) . ? Fe1 C7 2.048(2) . ? Fe1 C10 2.0595(19) . ? Fe1 C6 2.0938(18) . ? C6 C10 1.430(3) . ? C6 C7 1.430(3) . ? C6 B2 1.591(3) . ? C7 C8 1.425(3) . ? C8 C9 1.412(3) . ? C9 C10 1.430(3) . ? B1 N2 1.413(3) . ? B1 N1 1.415(3) . ? N1 C11 1.479(3) . ? N2 C15 1.473(3) . ? C11 C14 1.523(3) . ? C11 C12 1.523(3) . ? C11 C13 1.531(3) . ? C15 C16 1.513(3) . ? C15 C17 1.518(4) . ? C15 C18 1.520(3) . ? B2 N4 1.414(3) . ? B2 N3 1.414(3) . ? N3 C19 1.473(3) . ? N4 C23 1.483(3) . ? C19 C20 1.520(3) . ? C19 C22 1.524(3) . ? C19 C21 1.533(3) . ? C23 C25 1.519(3) . ? C23 C24 1.523(3) . ? C23 C26 1.526(3) . ? 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 C2 C1 C5 105.80(17) . . ? C2 C1 B1 126.05(17) . . ? C5 C1 B1 127.97(17) . . ? C2 C1 Fe1 68.42(10) . . ? C5 C1 Fe1 68.52(10) . . ? B1 C1 Fe1 131.23(13) . . ? C3 C2 C1 109.25(19) . . ? C3 C2 Fe1 69.40(12) . . ? C1 C2 Fe1 71.24(11) . . ? C4 C3 C2 107.95(18) . . ? C4 C3 Fe1 69.91(12) . . ? C2 C3 Fe1 69.87(12) . . ? C3 C4 C5 107.54(18) . . ? C3 C4 Fe1 69.69(12) . . ? C5 C4 Fe1 69.98(11) . . ? C4 C5 C1 109.46(18) . . ? C4 C5 Fe1 69.44(12) . . ? C1 C5 Fe1 71.04(11) . . ? C8 Fe1 C3 178.56(8) . . ? C8 Fe1 C9 40.42(9) . . ? C3 Fe1 C9 138.73(10) . . ? C8 Fe1 C7 40.81(8) . . ? C3 Fe1 C7 140.62(9) . . ? C9 Fe1 C7 68.23(9) . . ? C8 Fe1 C4 140.46(10) . . ? C3 Fe1 C4 40.40(9) . . ? C9 Fe1 C4 179.04(9) . . ? C7 Fe1 C4 112.22(9) . . ? C8 Fe1 C2 137.85(8) . . ? C3 Fe1 C2 40.72(8) . . ? C9 Fe1 C2 111.46(9) . . ? C7 Fe1 C2 178.19(8) . . ? C4 Fe1 C2 68.12(9) . . ? C8 Fe1 C5 112.14(8) . . ? C3 Fe1 C5 67.83(9) . . ? C9 Fe1 C5 140.20(8) . . ? C7 Fe1 C5 111.51(8) . . ? C4 Fe1 C5 40.58(8) . . ? C2 Fe1 C5 67.50(8) . . ? C8 Fe1 C10 68.02(8) . . ? C3 Fe1 C10 112.05(9) . . ? C9 Fe1 C10 40.76(8) . . ? C7 Fe1 C10 67.65(8) . . ? C4 Fe1 C10 138.48(8) . . ? C2 Fe1 C10 113.37(8) . . ? C5 Fe1 C10 178.62(7) . . ? C8 Fe1 C1 110.50(8) . . ? C3 Fe1 C1 68.48(8) . . ? C9 Fe1 C1 111.68(8) . . ? C7 Fe1 C1 137.95(8) . . ? C4 Fe1 C1 68.61(8) . . ? C2 Fe1 C1 40.33(8) . . ? C5 Fe1 C1 40.45(8) . . ? C10 Fe1 C1 140.90(8) . . ? C8 Fe1 C6 68.46(8) . . ? C3 Fe1 C6 112.58(8) . . ? C9 Fe1 C6 68.51(8) . . ? C7 Fe1 C6 40.39(8) . . ? C4 Fe1 C6 111.23(8) . . ? C2 Fe1 C6 141.33(8) . . ? C5 Fe1 C6 138.38(8) . . ? C10 Fe1 C6 40.28(8) . . ? C1 Fe1 C6 178.28(8) . . ? C10 C6 C7 106.10(17) . . ? C10 C6 B2 126.62(17) . . ? C7 C6 B2 127.15(17) . . ? C10 C6 Fe1 68.57(10) . . ? C7 C6 Fe1 68.07(10) . . ? B2 C6 Fe1 131.11(13) . . ? C8 C7 C6 109.05(18) . . ? C8 C7 Fe1 69.28(11) . . ? C6 C7 Fe1 71.53(11) . . ? C9 C8 C7 108.11(17) . . ? C9 C8 Fe1 70.06(11) . . ? C7 C8 Fe1 69.91(11) . . ? C8 C9 C10 107.58(17) . . ? C8 C9 Fe1 69.52(11) . . ? C10 C9 Fe1 70.11(11) . . ? C9 C10 C6 109.15(18) . . ? C9 C10 Fe1 69.13(11) . . ? C6 C10 Fe1 71.15(11) . . ? N2 B1 N1 121.97(18) . . ? N2 B1 C1 121.25(17) . . ? N1 B1 C1 116.77(17) . . ? B1 N1 C11 132.60(17) . . ? B1 N2 C15 132.87(17) . . ? N1 C11 C14 107.40(17) . . ? N1 C11 C12 110.54(17) . . ? C14 C11 C12 108.9(2) . . ? N1 C11 C13 110.83(17) . . ? C14 C11 C13 109.5(2) . . ? C12 C11 C13 109.63(18) . . ? N2 C15 C16 111.60(18) . . ? N2 C15 C17 110.5(2) . . ? C16 C15 C17 109.1(2) . . ? N2 C15 C18 107.76(18) . . ? C16 C15 C18 107.9(2) . . ? C17 C15 C18 110.0(2) . . ? N4 B2 N3 122.17(18) . . ? N4 B2 C6 121.33(17) . . ? N3 B2 C6 116.50(17) . . ? B2 N3 C19 133.86(17) . . ? B2 N4 C23 132.69(17) . . ? N3 C19 C20 107.59(17) . . ? N3 C19 C22 110.62(17) . . ? C20 C19 C22 109.7(2) . . ? N3 C19 C21 110.82(17) . . ? C20 C19 C21 108.4(2) . . ? C22 C19 C21 109.60(18) . . ? N4 C23 C25 110.60(18) . . ? N4 C23 C24 107.35(17) . . ? C25 C23 C24 109.1(2) . . ? N4 C23 C26 111.21(17) . . ? C25 C23 C26 110.33(19) . . ? C24 C23 C26 108.19(19) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.729 _refine_diff_density_min -0.372 _refine_diff_density_rms 0.045 #===END data_Compound4.6THF _database_code_depnum_ccdc_archive 'CCDC 773250' #TrackingRef '- Newbams_revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H88 B2 Li4 N4 O6' _chemical_formula_sum 'C46 H88 B2 Li4 N4 O6' _chemical_formula_weight 842.58 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' Li Li -0.0003 0.0001 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.003(2) _cell_length_b 14.712(3) _cell_length_c 19.859(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.29(3) _cell_angle_gamma 90.00 _cell_volume 2921.8(10) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 32486 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 25.03 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.958 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 924 _exptl_absorpt_coefficient_mu 0.060 _exptl_absorpt_correction_type Integration _exptl_absorpt_correction_T_min 0.9881 _exptl_absorpt_correction_T_max 0.9881 _exptl_absorpt_process_details 'HKL Scalepack (Otwinowski and Minor 1997)' _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 'Nonius Kappa CCD' _diffrn_measurement_method 'phi\omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32486 _diffrn_reflns_av_R_equivalents 0.0188 _diffrn_reflns_av_sigmaI/netI 0.0304 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 25.03 _reflns_number_total 5107 _reflns_number_gt 3773 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Nonius DENZO' _computing_data_reduction 'Nonius DENZO' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1374P)^2^+0.7009P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5107 _refine_ls_number_parameters 286 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0877 _refine_ls_R_factor_gt 0.0679 _refine_ls_wR_factor_ref 0.2254 _refine_ls_wR_factor_gt 0.2070 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.000 _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 B1 B 0.3738(2) 0.39053(16) 0.11342(11) 0.0370(5) Uani 1 1 d . . . C1 C 0.43998(19) 0.44756(14) 0.05350(10) 0.0380(5) Uani 1 1 d . . . C2 C 0.37036(19) 0.47114(15) -0.00584(10) 0.0407(5) Uani 1 1 d . . . H2A H 0.2800 0.4521 -0.0113 0.061 Uiso 1 1 calc R . . C3 C 0.57288(19) 0.47900(15) 0.05709(10) 0.0409(5) Uani 1 1 d . . . H3A H 0.6257 0.4655 0.0962 0.061 Uiso 1 1 calc R . . N1 N 0.31050(16) 0.42891(11) 0.17110(8) 0.0386(4) Uani 1 1 d . . . C4 C 0.3013(2) 0.52442(15) 0.18966(11) 0.0458(5) Uani 1 1 d . . . C5 C 0.4372(3) 0.56306(17) 0.21184(15) 0.0640(7) Uani 1 1 d . . . H5A H 0.4756 0.5254 0.2481 0.096 Uiso 1 1 calc R . . H5B H 0.4258 0.6254 0.2281 0.096 Uiso 1 1 calc R . . H5C H 0.4973 0.5631 0.1735 0.096 Uiso 1 1 calc R . . C6 C 0.2074(3) 0.53158(19) 0.24921(14) 0.0728(8) Uani 1 1 d . . . H6A H 0.2436 0.4959 0.2871 0.109 Uiso 1 1 calc R . . H6B H 0.1190 0.5081 0.2359 0.109 Uiso 1 1 calc R . . H6C H 0.1994 0.5954 0.2628 0.109 Uiso 1 1 calc R . . C7 C 0.2435(3) 0.58574(17) 0.13344(13) 0.0584(6) Uani 1 1 d . . . H7A H 0.1565 0.5620 0.1181 0.088 Uiso 1 1 calc R . . H7B H 0.3048 0.5867 0.0956 0.088 Uiso 1 1 calc R . . H7C H 0.2324 0.6476 0.1508 0.088 Uiso 1 1 calc R . . N2 N 0.37070(16) 0.29265(11) 0.11739(8) 0.0386(4) Uani 1 1 d . . . C8 C 0.4207(2) 0.22735(16) 0.06926(11) 0.0468(5) Uani 1 1 d . . . C9 C 0.5697(3) 0.2390(2) 0.05569(18) 0.0825(10) Uani 1 1 d . . . H9A H 0.6208 0.2352 0.0983 0.124 Uiso 1 1 calc R . . H9B H 0.5847 0.2983 0.0348 0.124 Uiso 1 1 calc R . . H9C H 0.5989 0.1908 0.0253 0.124 Uiso 1 1 calc R . . C10 C 0.3998(3) 0.13176(17) 0.09763(13) 0.0608(7) Uani 1 1 d . . . H10A H 0.4494 0.1257 0.1405 0.091 Uiso 1 1 calc R . . H10B H 0.4323 0.0866 0.0656 0.091 Uiso 1 1 calc R . . H10C H 0.3044 0.1218 0.1050 0.091 Uiso 1 1 calc R . . C11 C 0.3436(3) 0.2313(2) 0.00130(12) 0.0660(7) Uani 1 1 d . . . H11A H 0.2474 0.2275 0.0091 0.099 Uiso 1 1 calc R . . H11B H 0.3708 0.1802 -0.0270 0.099 Uiso 1 1 calc R . . H11C H 0.3637 0.2886 -0.0215 0.099 Uiso 1 1 calc R . . O1 O 0.00684(16) 0.30802(12) 0.13674(9) 0.0586(5) Uani 1 1 d . . . C12 C -0.0383(3) 0.2321(2) 0.09775(16) 0.0745(8) Uani 1 1 d . . . H12A H -0.1209 0.2067 0.1168 0.089 Uiso 1 1 calc R . . H12B H 0.0309 0.1840 0.0980 0.089 Uiso 1 1 calc R . . C13 C -0.0649(3) 0.2646(3) 0.02750(15) 0.0879(10) Uani 1 1 d . . . H13A H -0.1584 0.2516 0.0131 0.105 Uiso 1 1 calc R . . H13B H -0.0038 0.2350 -0.0043 0.105 Uiso 1 1 calc R . . C14 C -0.0402(4) 0.3652(3) 0.03038(19) 0.1033(13) Uani 1 1 d . . . H14A H -0.1093 0.3988 0.0040 0.124 Uiso 1 1 calc R . . H14B H 0.0490 0.3804 0.0130 0.124 Uiso 1 1 calc R . . C15 C -0.0480(3) 0.3869(2) 0.1043(2) 0.0868(10) Uani 1 1 d . . . H15A H 0.0052 0.4417 0.1158 0.104 Uiso 1 1 calc R . . H15B H -0.1417 0.3970 0.1175 0.104 Uiso 1 1 calc R . . O2 O 0.55855(16) 0.31805(12) 0.27421(8) 0.0548(5) Uani 1 1 d . . . C16 C 0.6839(3) 0.3428(2) 0.24880(15) 0.0759(9) Uani 1 1 d . . . H16A H 0.6727 0.3774 0.2063 0.091 Uiso 1 1 calc R . . H16B H 0.7388 0.2882 0.2402 0.091 Uiso 1 1 calc R . . C17 C 0.7487(4) 0.4012(3) 0.3029(3) 0.1097(14) Uani 1 1 d . . . H17A H 0.8474 0.3961 0.3020 0.132 Uiso 1 1 calc R . . H17B H 0.7231 0.4657 0.2971 0.132 Uiso 1 1 calc R . . C18 C 0.6975(4) 0.3647(3) 0.3653(2) 0.1041(13) Uani 1 1 d . . . H18A H 0.6944 0.4123 0.4005 0.125 Uiso 1 1 calc R . . H18B H 0.7534 0.3136 0.3820 0.125 Uiso 1 1 calc R . . C19 C 0.5598(3) 0.3330(2) 0.34574(13) 0.0784(9) Uani 1 1 d . . . H19A H 0.5384 0.2760 0.3697 0.094 Uiso 1 1 calc R . . H19B H 0.4928 0.3796 0.3575 0.094 Uiso 1 1 calc R . . O3 O 0.22900(16) 0.25528(11) 0.25539(8) 0.0547(5) Uani 1 1 d . . . C20 C 0.2201(3) 0.15740(18) 0.25812(15) 0.0681(7) Uani 1 1 d . . . H20A H 0.3088 0.1294 0.2515 0.082 Uiso 1 1 calc R . . H20B H 0.1570 0.1344 0.2230 0.082 Uiso 1 1 calc R . . C21 C 0.1707(4) 0.1367(3) 0.32660(18) 0.0945(11) Uani 1 1 d . . . H21A H 0.1141 0.0815 0.3260 0.113 Uiso 1 1 calc R . . H21B H 0.2461 0.1277 0.3591 0.113 Uiso 1 1 calc R . . C22 C 0.0914(5) 0.2183(3) 0.3442(2) 0.1087(14) Uani 1 1 d . . . H22A H -0.0024 0.2119 0.3278 0.130 Uiso 1 1 calc R . . H22B H 0.0920 0.2277 0.3935 0.130 Uiso 1 1 calc R . . C23 C 0.1569(3) 0.2940(2) 0.31047(15) 0.0768(9) Uani 1 1 d . . . H23A H 0.0897 0.3383 0.2935 0.092 Uiso 1 1 calc R . . H23B H 0.2191 0.3256 0.3421 0.092 Uiso 1 1 calc R . . Li2 Li 0.4025(4) 0.3214(2) 0.21431(17) 0.0450(8) Uani 1 1 d . . . Li1 Li 0.1970(3) 0.3202(2) 0.16002(17) 0.0438(8) Uani 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 B1 0.0333(10) 0.0394(13) 0.0382(11) 0.0086(9) -0.0008(9) -0.0049(9) C1 0.0386(10) 0.0392(11) 0.0364(10) 0.0055(8) 0.0057(8) -0.0033(8) C2 0.0345(10) 0.0468(12) 0.0409(11) 0.0097(9) 0.0021(8) -0.0076(8) C3 0.0400(10) 0.0458(12) 0.0367(10) 0.0098(9) -0.0009(8) -0.0038(9) N1 0.0451(9) 0.0324(9) 0.0386(8) 0.0043(7) 0.0057(7) -0.0025(7) C4 0.0566(12) 0.0352(12) 0.0459(12) 0.0027(9) 0.0061(10) 0.0010(9) C5 0.0719(16) 0.0425(14) 0.0771(17) -0.0119(12) -0.0097(13) -0.0042(12) C6 0.108(2) 0.0452(15) 0.0664(16) -0.0017(12) 0.0304(15) 0.0092(14) C7 0.0711(15) 0.0399(13) 0.0643(15) 0.0088(11) 0.0052(12) 0.0083(11) N2 0.0418(9) 0.0375(10) 0.0368(9) 0.0026(7) 0.0069(7) -0.0017(7) C8 0.0495(12) 0.0468(13) 0.0447(11) -0.0013(9) 0.0122(9) -0.0022(10) C9 0.0559(15) 0.074(2) 0.119(3) -0.0334(19) 0.0318(16) -0.0016(14) C10 0.0842(17) 0.0410(13) 0.0575(14) -0.0030(11) 0.0086(13) 0.0055(12) C11 0.0933(19) 0.0617(17) 0.0432(13) -0.0040(11) 0.0054(12) 0.0000(14) O1 0.0472(9) 0.0652(11) 0.0632(10) 0.0030(8) -0.0009(7) -0.0047(7) C12 0.0639(16) 0.0680(19) 0.091(2) -0.0004(16) -0.0092(15) -0.0156(14) C13 0.0671(18) 0.127(3) 0.0694(18) -0.0115(19) 0.0049(14) -0.0085(18) C14 0.091(2) 0.130(4) 0.089(2) 0.039(2) -0.0071(19) 0.007(2) C15 0.0637(17) 0.068(2) 0.128(3) -0.0073(19) -0.0133(18) 0.0203(14) O2 0.0581(9) 0.0647(11) 0.0414(8) 0.0090(7) -0.0002(7) -0.0005(8) C16 0.0584(15) 0.096(2) 0.0732(18) 0.0205(16) 0.0038(13) -0.0002(14) C17 0.086(2) 0.079(3) 0.162(4) 0.007(3) -0.035(3) -0.0139(19) C18 0.142(3) 0.071(2) 0.097(3) -0.018(2) -0.051(3) 0.005(2) C19 0.103(2) 0.086(2) 0.0455(14) 0.0013(14) 0.0001(14) 0.0198(17) O3 0.0684(10) 0.0450(10) 0.0515(9) 0.0149(7) 0.0225(7) 0.0033(7) C20 0.0775(18) 0.0478(15) 0.0797(18) 0.0202(13) 0.0150(14) 0.0044(12) C21 0.116(3) 0.079(2) 0.090(2) 0.0390(19) 0.028(2) -0.009(2) C22 0.133(3) 0.094(3) 0.102(3) 0.003(2) 0.070(2) -0.025(2) C23 0.095(2) 0.074(2) 0.0627(16) 0.0069(14) 0.0355(15) 0.0037(16) Li2 0.0491(19) 0.044(2) 0.0422(18) 0.0080(15) 0.0006(15) -0.0035(15) Li1 0.0424(17) 0.045(2) 0.0447(18) 0.0053(15) 0.0054(14) -0.0050(15) _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 B1 N1 1.437(3) . ? B1 N2 1.442(3) . ? B1 C1 1.610(3) . ? B1 Li2 2.260(4) . ? B1 Li1 2.265(4) . ? C1 C2 1.399(3) . ? C1 C3 1.408(3) . ? C2 C3 1.386(3) 3_665 ? C3 C2 1.386(3) 3_665 ? N1 C4 1.456(3) . ? N1 Li1 1.970(4) . ? N1 Li2 2.013(4) . ? C4 C5 1.529(3) . ? C4 C6 1.530(3) . ? C4 C7 1.538(3) . ? N2 C8 1.452(3) . ? N2 Li2 1.989(4) . ? N2 Li1 1.992(4) . ? C8 C9 1.530(3) . ? C8 C10 1.531(3) . ? C8 C11 1.540(3) . ? O1 C12 1.426(3) . ? O1 C15 1.431(4) . ? O1 Li1 1.956(4) . ? C12 C13 1.493(4) . ? C13 C14 1.501(6) . ? C14 C15 1.507(5) . ? O2 C16 1.410(3) . ? O2 C19 1.437(3) . ? O2 Li2 1.942(4) . ? C16 C17 1.509(5) . ? C17 C18 1.454(6) . ? C18 C19 1.497(5) . ? O3 C23 1.441(3) . ? O3 C20 1.444(3) . ? O3 Li1 2.139(4) . ? O3 Li2 2.165(4) . ? C20 C21 1.489(4) . ? C21 C22 1.485(5) . ? C22 C23 1.462(4) . ? Li2 Li1 2.300(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 N1 B1 N2 109.77(16) . . ? N1 B1 C1 125.46(19) . . ? N2 B1 C1 124.77(19) . . ? N1 B1 Li2 61.28(14) . . ? N2 B1 Li2 60.31(13) . . ? C1 B1 Li2 147.53(16) . . ? N1 B1 Li1 59.43(13) . . ? N2 B1 Li1 60.24(14) . . ? C1 B1 Li1 151.36(16) . . ? Li2 B1 Li1 61.11(14) . . ? C2 C1 C3 114.38(17) . . ? C2 C1 B1 123.13(16) . . ? C3 C1 B1 122.48(17) . . ? C3 C2 C1 123.04(17) 3_665 . ? C2 C3 C1 122.58(18) 3_665 . ? B1 N1 C4 127.78(17) . . ? B1 N1 Li1 81.68(16) . . ? C4 N1 Li1 140.49(17) . . ? B1 N1 Li2 79.95(15) . . ? C4 N1 Li2 132.97(17) . . ? Li1 N1 Li2 70.53(16) . . ? N1 C4 C5 111.74(18) . . ? N1 C4 C6 107.79(18) . . ? C5 C4 C6 108.0(2) . . ? N1 C4 C7 114.03(18) . . ? C5 C4 C7 108.0(2) . . ? C6 C4 C7 107.1(2) . . ? B1 N2 C8 128.05(17) . . ? B1 N2 Li2 80.65(15) . . ? C8 N2 Li2 136.69(17) . . ? B1 N2 Li1 80.80(16) . . ? C8 N2 Li1 136.98(17) . . ? Li2 N2 Li1 70.58(16) . . ? N2 C8 C9 113.15(19) . . ? N2 C8 C10 108.29(17) . . ? C9 C8 C10 108.0(2) . . ? N2 C8 C11 112.28(19) . . ? C9 C8 C11 108.2(2) . . ? C10 C8 C11 106.7(2) . . ? C12 O1 C15 106.1(2) . . ? C12 O1 Li1 119.62(19) . . ? C15 O1 Li1 113.1(2) . . ? O1 C12 C13 107.7(3) . . ? C12 C13 C14 104.7(3) . . ? C13 C14 C15 103.5(3) . . ? O1 C15 C14 103.8(3) . . ? C16 O2 C19 109.0(2) . . ? C16 O2 Li2 118.91(18) . . ? C19 O2 Li2 126.2(2) . . ? O2 C16 C17 105.3(3) . . ? C18 C17 C16 104.1(3) . . ? C17 C18 C19 103.5(3) . . ? O2 C19 C18 106.9(3) . . ? C23 O3 C20 109.47(19) . . ? C23 O3 Li1 115.35(19) . . ? C20 O3 Li1 118.07(18) . . ? C23 O3 Li2 121.84(19) . . ? C20 O3 Li2 120.85(18) . . ? Li1 O3 Li2 64.59(14) . . ? O3 C20 C21 105.1(2) . . ? C22 C21 C20 103.9(3) . . ? C23 C22 C21 105.1(3) . . ? O3 C23 C22 106.5(3) . . ? O2 Li2 N2 134.1(2) . . ? O2 Li2 N1 129.4(2) . . ? N2 Li2 N1 72.11(13) . . ? O2 Li2 O3 113.45(17) . . ? N2 Li2 O3 99.03(16) . . ? N1 Li2 O3 98.69(16) . . ? O2 Li2 B1 129.71(19) . . ? N2 Li2 B1 39.04(10) . . ? N1 Li2 B1 38.77(10) . . ? O3 Li2 B1 116.71(16) . . ? O2 Li2 Li1 170.0(2) . . ? N2 Li2 Li1 54.76(13) . . ? N1 Li2 Li1 53.88(13) . . ? O3 Li2 Li1 57.16(13) . . ? B1 Li2 Li1 59.55(13) . . ? O1 Li1 N1 131.0(2) . . ? O1 Li1 N2 137.2(2) . . ? N1 Li1 N2 72.95(13) . . ? O1 Li1 O3 107.08(17) . . ? N1 Li1 O3 100.91(16) . . ? N2 Li1 O3 99.83(16) . . ? O1 Li1 B1 135.22(19) . . ? N1 Li1 B1 38.89(10) . . ? N2 Li1 B1 38.96(10) . . ? O3 Li1 B1 117.59(17) . . ? O1 Li1 Li2 165.0(2) . . ? N1 Li1 Li2 55.59(13) . . ? N2 Li1 Li2 54.66(13) . . ? O3 Li1 Li2 58.25(13) . . ? B1 Li1 Li2 59.34(13) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.430 _refine_diff_density_min -0.246 _refine_diff_density_rms 0.053 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 0.000 177.9 13.4 2 0.000 0.500 0.500 177.8 13.4 _platon_squeeze_details ; Electron density in two regions were attributed to a disordered diethyl ether molecule for which no suitable model could be found. These regions of electron density were removed from the reflections data using the program SQUEEZE (PLATON), leaving a void of 355.7 angstroms cubed ; #===END data_Compound5.2THF _database_code_depnum_ccdc_archive 'CCDC 773251' #TrackingRef '- Newbams.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H56 B Li N2 O2' _chemical_formula_sum 'C38 H56 B Li N2 O2' _chemical_formula_weight 590.60 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' Li Li -0.0003 0.0001 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.028(3) _cell_length_b 16.356(3) _cell_length_c 16.606(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.66(3) _cell_angle_gamma 90.00 _cell_volume 3702.4(13) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 56077 _cell_measurement_theta_min 2.79 _cell_measurement_theta_max 25.03 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.060 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1288 _exptl_absorpt_coefficient_mu 0.063 _exptl_absorpt_correction_type Integration _exptl_absorpt_correction_T_min 0.9912 _exptl_absorpt_correction_T_max 0.9925 _exptl_absorpt_process_details 'HKL Scalepack (Otwinowski and Minor 1997)' _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 'Nonius Kappa CCD' _diffrn_measurement_method 'phi\omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 56077 _diffrn_reflns_av_R_equivalents 0.0666 _diffrn_reflns_av_sigmaI/netI 0.0432 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 25.03 _reflns_number_total 6541 _reflns_number_gt 4342 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Nonius DENZO' _computing_data_reduction 'Nonius DENZO' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0644P)^2^+3.0061P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6541 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1165 _refine_ls_R_factor_gt 0.0740 _refine_ls_wR_factor_ref 0.1958 _refine_ls_wR_factor_gt 0.1684 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.000 _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 N1 N 0.70967(14) 0.23850(13) -0.09644(13) 0.0381(5) Uani 1 1 d . . . B1 B 0.6742(2) 0.26310(17) -0.02847(18) 0.0350(7) Uani 1 1 d . . . N2 N 0.73469(14) 0.25810(13) 0.05508(13) 0.0384(5) Uani 1 1 d . . . H2A H 0.7919 0.2342 0.0595 0.046 Uiso 1 1 calc R . . C1 C 0.56503(18) 0.29689(16) -0.04362(17) 0.0398(6) Uani 1 1 d . . . C2 C 0.53744(19) 0.36564(16) -0.00466(18) 0.0436(7) Uani 1 1 d . . . H2B H 0.5861 0.3947 0.0344 0.052 Uiso 1 1 calc R . . C3 C 0.4411(2) 0.39278(18) -0.0213(2) 0.0543(8) Uani 1 1 d . . . H3A H 0.4248 0.4403 0.0055 0.065 Uiso 1 1 calc R . . C4 C 0.3692(2) 0.3510(2) -0.0766(2) 0.0651(9) Uani 1 1 d . . . H4A H 0.3030 0.3689 -0.0873 0.078 Uiso 1 1 calc R . . C5 C 0.3934(2) 0.2831(2) -0.1164(2) 0.0701(10) Uani 1 1 d . . . H5A H 0.3441 0.2543 -0.1550 0.084 Uiso 1 1 calc R . . C6 C 0.4900(2) 0.25687(19) -0.1000(2) 0.0566(8) Uani 1 1 d . . . H6A H 0.5058 0.2100 -0.1280 0.068 Uiso 1 1 calc R . . C7 C 0.80290(18) 0.20293(16) -0.08413(15) 0.0390(6) Uani 1 1 d . . . C8 C 0.81558(19) 0.11796(17) -0.06857(17) 0.0462(7) Uani 1 1 d . . . C9 C 0.9078(2) 0.0831(2) -0.06316(19) 0.0590(8) Uani 1 1 d . . . H9A H 0.9164 0.0262 -0.0528 0.071 Uiso 1 1 calc R . . C10 C 0.9862(2) 0.1291(2) -0.0724(2) 0.0655(9) Uani 1 1 d . . . H10A H 1.0478 0.1039 -0.0699 0.079 Uiso 1 1 calc R . . C11 C 0.9751(2) 0.2119(2) -0.08530(18) 0.0573(8) Uani 1 1 d . . . H11A H 1.0299 0.2435 -0.0912 0.069 Uiso 1 1 calc R . . C12 C 0.88546(18) 0.25083(18) -0.08993(16) 0.0439(7) Uani 1 1 d . . . C13 C 0.7302(2) 0.06509(18) -0.0593(2) 0.0575(8) Uani 1 1 d . . . H13A H 0.6804 0.1038 -0.0469 0.069 Uiso 1 1 calc R . . C14 C 0.6811(5) 0.0236(4) -0.1371(3) 0.168(3) Uani 1 1 d . . . H14A H 0.6265 -0.0094 -0.1276 0.253 Uiso 1 1 calc R . . H14B H 0.7282 -0.0119 -0.1554 0.253 Uiso 1 1 calc R . . H14C H 0.6560 0.0646 -0.1799 0.253 Uiso 1 1 calc R . . C15 C 0.7510(3) 0.0068(4) 0.0105(3) 0.131(2) Uani 1 1 d . . . H15A H 0.6912 -0.0236 0.0118 0.196 Uiso 1 1 calc R . . H15B H 0.7735 0.0368 0.0626 0.196 Uiso 1 1 calc R . . H15C H 0.8022 -0.0315 0.0034 0.196 Uiso 1 1 calc R . . C16 C 0.8754(2) 0.34224(19) -0.10284(18) 0.0527(7) Uani 1 1 d . . . H16A H 0.8159 0.3598 -0.0840 0.063 Uiso 1 1 calc R . . C17 C 0.9624(2) 0.3908(2) -0.0525(2) 0.0750(10) Uani 1 1 d . . . H17A H 0.9731 0.3763 0.0062 0.112 Uiso 1 1 calc R . . H17B H 0.9485 0.4495 -0.0594 0.112 Uiso 1 1 calc R . . H17C H 1.0213 0.3778 -0.0720 0.112 Uiso 1 1 calc R . . C18 C 0.8592(3) 0.3655(2) -0.1936(2) 0.0781(11) Uani 1 1 d . . . H18A H 0.8037 0.3343 -0.2263 0.117 Uiso 1 1 calc R . . H18B H 0.9184 0.3531 -0.2129 0.117 Uiso 1 1 calc R . . H18C H 0.8449 0.4241 -0.2001 0.117 Uiso 1 1 calc R . . C19 C 0.71632(19) 0.28572(16) 0.13099(16) 0.0418(6) Uani 1 1 d . . . C20 C 0.6425(2) 0.24901(19) 0.16275(19) 0.0536(8) Uani 1 1 d . . . C21 C 0.6235(3) 0.2797(2) 0.2351(2) 0.0720(11) Uani 1 1 d . . . H21A H 0.5725 0.2562 0.2562 0.086 Uiso 1 1 calc R . . C22 C 0.6765(3) 0.3431(3) 0.2768(2) 0.0825(13) Uani 1 1 d . . . H22A H 0.6621 0.3631 0.3263 0.099 Uiso 1 1 calc R . . C23 C 0.7510(3) 0.3782(2) 0.2469(2) 0.0697(10) Uani 1 1 d . . . H23A H 0.7882 0.4218 0.2766 0.084 Uiso 1 1 calc R . . C24 C 0.7723(2) 0.35033(17) 0.17374(17) 0.0492(7) Uani 1 1 d . . . C25 C 0.5862(2) 0.1752(2) 0.1220(2) 0.0659(9) Uani 1 1 d . . . H25A H 0.6039 0.1663 0.0677 0.079 Uiso 1 1 calc R . . C26 C 0.6171(3) 0.0988(2) 0.1753(3) 0.1021(15) Uani 1 1 d . . . H26A H 0.6883 0.0917 0.1854 0.153 Uiso 1 1 calc R . . H26B H 0.5841 0.0507 0.1462 0.153 Uiso 1 1 calc R . . H26C H 0.5986 0.1051 0.2283 0.153 Uiso 1 1 calc R . . C27 C 0.4745(3) 0.1860(3) 0.1044(3) 0.0947(14) Uani 1 1 d . . . H27A H 0.4552 0.2345 0.0697 0.142 Uiso 1 1 calc R . . H27B H 0.4548 0.1927 0.1568 0.142 Uiso 1 1 calc R . . H27C H 0.4422 0.1376 0.0753 0.142 Uiso 1 1 calc R . . C28 C 0.8501(2) 0.39224(19) 0.1385(2) 0.0572(8) Uani 1 1 d . . . H28A H 0.8635 0.3560 0.0939 0.069 Uiso 1 1 calc R . . C29 C 0.8121(3) 0.4724(2) 0.0984(3) 0.0954(14) Uani 1 1 d . . . H29A H 0.7502 0.4631 0.0575 0.143 Uiso 1 1 calc R . . H29B H 0.8603 0.4956 0.0707 0.143 Uiso 1 1 calc R . . H29C H 0.8012 0.5105 0.1409 0.143 Uiso 1 1 calc R . . C30 C 0.9470(3) 0.4050(2) 0.2015(2) 0.0833(12) Uani 1 1 d . . . H30A H 0.9938 0.4317 0.1746 0.125 Uiso 1 1 calc R . . H30B H 0.9733 0.3519 0.2237 0.125 Uiso 1 1 calc R . . H30C H 0.9364 0.4395 0.2468 0.125 Uiso 1 1 calc R . . Li1 Li 0.6424(4) 0.2702(3) -0.2056(3) 0.0621(14) Uani 1 1 d . . . O1 O 0.67360(19) 0.22114(16) -0.30182(14) 0.0780(7) Uani 1 1 d . . . C31 C 0.6483(3) 0.2564(3) -0.3833(2) 0.0936(13) Uani 1 1 d . . . H31A H 0.6575 0.3165 -0.3803 0.112 Uiso 1 1 calc R . . H31B H 0.5791 0.2445 -0.4107 0.112 Uiso 1 1 calc R . . C32 C 0.7157(3) 0.2181(4) -0.4301(3) 0.1169(19) Uani 1 1 d . . . H32A H 0.6787 0.2006 -0.4858 0.140 Uiso 1 1 calc R . . H32B H 0.7670 0.2574 -0.4367 0.140 Uiso 1 1 calc R . . C33 C 0.7600(5) 0.1476(4) -0.3815(3) 0.144(2) Uani 1 1 d . . . H33A H 0.7295 0.0963 -0.4070 0.173 Uiso 1 1 calc R . . H33B H 0.8312 0.1454 -0.3785 0.173 Uiso 1 1 calc R . . C34 C 0.7432(4) 0.1574(3) -0.3009(3) 0.1173(18) Uani 1 1 d . . . H34A H 0.8056 0.1711 -0.2611 0.141 Uiso 1 1 calc R . . H34B H 0.7181 0.1057 -0.2829 0.141 Uiso 1 1 calc R . . O2 O 0.57418(19) 0.36903(18) -0.24682(16) 0.0850(8) Uani 1 1 d . . . C35 C 0.6016(3) 0.4454(3) -0.2050(3) 0.0928(13) Uani 1 1 d . . . H35A H 0.6524 0.4729 -0.2278 0.111 Uiso 1 1 calc R . . H35B H 0.6285 0.4359 -0.1451 0.111 Uiso 1 1 calc R . . C36 C 0.5137(4) 0.4960(4) -0.2180(3) 0.126(2) Uani 1 1 d . . . H36A H 0.4966 0.5066 -0.1644 0.151 Uiso 1 1 calc R . . H36B H 0.5254 0.5492 -0.2425 0.151 Uiso 1 1 calc R . . C37 C 0.4359(4) 0.4537(3) -0.2724(4) 0.1204(18) Uani 1 1 d . . . H37A H 0.4081 0.4879 -0.3215 0.144 Uiso 1 1 calc R . . H37B H 0.3831 0.4415 -0.2438 0.144 Uiso 1 1 calc R . . C38 C 0.4756(3) 0.3764(3) -0.2985(3) 0.1065(16) Uani 1 1 d . . . H38A H 0.4349 0.3292 -0.2899 0.128 Uiso 1 1 calc R . . H38B H 0.4770 0.3788 -0.3578 0.128 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 N1 0.0343(11) 0.0392(12) 0.0392(13) -0.0005(10) 0.0058(9) 0.0017(9) B1 0.0355(14) 0.0283(14) 0.0415(18) 0.0030(12) 0.0094(13) -0.0015(11) N2 0.0354(11) 0.0405(12) 0.0415(13) 0.0009(10) 0.0135(9) 0.0072(9) C1 0.0361(13) 0.0378(14) 0.0459(16) 0.0058(12) 0.0103(11) -0.0023(11) C2 0.0404(14) 0.0381(15) 0.0537(18) 0.0047(13) 0.0136(12) 0.0012(11) C3 0.0457(16) 0.0455(17) 0.075(2) 0.0072(15) 0.0213(15) 0.0101(13) C4 0.0347(15) 0.062(2) 0.097(3) 0.0107(19) 0.0119(16) 0.0090(15) C5 0.0359(16) 0.067(2) 0.099(3) -0.008(2) 0.0004(16) -0.0040(15) C6 0.0426(16) 0.0489(17) 0.076(2) -0.0068(16) 0.0092(15) -0.0006(13) C7 0.0398(14) 0.0466(15) 0.0291(14) -0.0056(12) 0.0050(11) 0.0067(12) C8 0.0474(16) 0.0494(17) 0.0381(16) -0.0067(13) 0.0030(12) 0.0117(13) C9 0.064(2) 0.0582(19) 0.0511(19) -0.0062(15) 0.0070(15) 0.0198(16) C10 0.0501(18) 0.084(3) 0.063(2) -0.0038(18) 0.0146(16) 0.0266(18) C11 0.0384(15) 0.087(3) 0.0478(18) -0.0023(17) 0.0134(13) 0.0037(16) C12 0.0382(14) 0.0600(18) 0.0331(15) -0.0059(13) 0.0078(11) -0.0008(13) C13 0.0615(19) 0.0386(16) 0.067(2) -0.0017(15) 0.0051(16) 0.0044(14) C14 0.216(6) 0.200(6) 0.079(3) -0.018(4) 0.015(4) -0.147(6) C15 0.107(4) 0.183(6) 0.093(4) 0.063(4) 0.005(3) -0.037(4) C16 0.0437(15) 0.0615(19) 0.0545(19) 0.0017(15) 0.0151(13) -0.0102(14) C17 0.066(2) 0.080(2) 0.078(3) -0.005(2) 0.0154(18) -0.0277(19) C18 0.091(3) 0.081(3) 0.060(2) 0.0132(19) 0.0127(19) -0.008(2) C19 0.0466(15) 0.0435(15) 0.0372(15) 0.0080(12) 0.0135(12) 0.0141(12) C20 0.0555(17) 0.0548(18) 0.0570(19) 0.0231(15) 0.0263(15) 0.0221(14) C21 0.083(2) 0.078(3) 0.068(2) 0.025(2) 0.045(2) 0.033(2) C22 0.108(3) 0.097(3) 0.054(2) 0.014(2) 0.043(2) 0.052(3) C23 0.093(3) 0.064(2) 0.051(2) -0.0094(16) 0.0142(18) 0.0248(19) C24 0.0610(18) 0.0467(16) 0.0397(16) 0.0008(13) 0.0116(13) 0.0142(14) C25 0.0575(19) 0.057(2) 0.092(3) 0.0324(18) 0.0351(18) 0.0050(15) C26 0.099(3) 0.072(3) 0.141(4) 0.048(3) 0.039(3) 0.012(2) C27 0.062(2) 0.097(3) 0.135(4) 0.043(3) 0.042(2) -0.001(2) C28 0.0615(19) 0.0496(18) 0.057(2) -0.0090(15) 0.0059(15) -0.0040(15) C29 0.065(2) 0.086(3) 0.124(4) 0.041(3) -0.002(2) -0.009(2) C30 0.066(2) 0.087(3) 0.085(3) -0.012(2) -0.0072(19) 0.012(2) Li1 0.064(3) 0.069(3) 0.046(3) 0.004(3) -0.002(2) 0.007(3) O1 0.0995(18) 0.0860(18) 0.0447(14) -0.0056(12) 0.0097(12) -0.0058(15) C31 0.106(3) 0.124(4) 0.044(2) 0.001(2) 0.003(2) -0.005(3) C32 0.061(2) 0.224(6) 0.065(3) 0.026(3) 0.013(2) 0.008(3) C33 0.201(6) 0.156(5) 0.097(4) 0.009(4) 0.079(4) 0.041(5) C34 0.176(5) 0.107(4) 0.069(3) -0.006(3) 0.031(3) 0.043(4) O2 0.0815(17) 0.097(2) 0.0689(17) 0.0183(15) 0.0021(13) 0.0309(15) C35 0.091(3) 0.083(3) 0.104(3) 0.019(3) 0.022(2) 0.014(2) C36 0.117(4) 0.148(5) 0.096(4) -0.005(3) -0.006(3) 0.068(4) C37 0.092(3) 0.097(4) 0.158(5) 0.030(3) 0.003(3) 0.036(3) C38 0.090(3) 0.134(4) 0.080(3) 0.019(3) -0.011(2) 0.040(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 B1 1.396(4) . ? N1 C7 1.402(3) . ? N1 Li1 1.908(5) . ? B1 N2 1.448(4) . ? B1 C1 1.591(4) . ? N2 C19 1.419(3) . ? C1 C6 1.395(4) . ? C1 C2 1.397(4) . ? C2 C3 1.387(4) . ? C3 C4 1.375(4) . ? C4 C5 1.375(5) . ? C5 C6 1.386(4) . ? C7 C8 1.417(4) . ? C7 C12 1.420(4) . ? C8 C9 1.397(4) . ? C8 C13 1.514(4) . ? C9 C10 1.370(5) . ? C10 C11 1.375(5) . ? C11 C12 1.395(4) . ? C12 C16 1.512(4) . ? C13 C15 1.476(5) . ? C13 C14 1.478(5) . ? C16 C18 1.519(4) . ? C16 C17 1.529(4) . ? C19 C20 1.403(4) . ? C19 C24 1.405(4) . ? C20 C21 1.385(5) . ? C20 C25 1.512(5) . ? C21 C22 1.365(6) . ? C22 C23 1.383(5) . ? C23 C24 1.394(4) . ? C24 C28 1.519(4) . ? C25 C26 1.533(5) . ? C25 C27 1.535(4) . ? C28 C29 1.509(5) . ? C28 C30 1.522(4) . ? Li1 O2 1.920(6) . ? Li1 O1 1.928(6) . ? O1 C34 1.425(5) . ? O1 C31 1.437(4) . ? C31 C32 1.496(6) . ? C32 C33 1.460(7) . ? C33 C34 1.421(6) . ? O2 C35 1.436(5) . ? O2 C38 1.450(4) . ? C35 C36 1.459(5) . ? C36 C37 1.422(7) . ? C37 C38 1.488(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 B1 N1 C7 120.0(2) . . ? B1 N1 Li1 120.0(2) . . ? C7 N1 Li1 119.1(2) . . ? N1 B1 N2 121.2(2) . . ? N1 B1 C1 119.1(2) . . ? N2 B1 C1 119.7(2) . . ? C19 N2 B1 130.2(2) . . ? C6 C1 C2 116.2(2) . . ? C6 C1 B1 119.2(2) . . ? C2 C1 B1 124.6(2) . . ? C3 C2 C1 121.9(3) . . ? C4 C3 C2 120.0(3) . . ? C5 C4 C3 119.8(3) . . ? C4 C5 C6 119.8(3) . . ? C5 C6 C1 122.3(3) . . ? N1 C7 C8 120.4(2) . . ? N1 C7 C12 120.6(2) . . ? C8 C7 C12 119.0(2) . . ? C9 C8 C7 119.1(3) . . ? C9 C8 C13 120.2(3) . . ? C7 C8 C13 120.7(2) . . ? C10 C9 C8 121.6(3) . . ? C9 C10 C11 119.6(3) . . ? C10 C11 C12 121.7(3) . . ? C11 C12 C7 118.9(3) . . ? C11 C12 C16 120.7(3) . . ? C7 C12 C16 120.3(2) . . ? C15 C13 C14 110.8(4) . . ? C15 C13 C8 115.7(3) . . ? C14 C13 C8 113.0(3) . . ? C12 C16 C18 112.0(3) . . ? C12 C16 C17 113.6(3) . . ? C18 C16 C17 109.0(3) . . ? C20 C19 C24 120.4(3) . . ? C20 C19 N2 120.2(3) . . ? C24 C19 N2 119.4(2) . . ? C21 C20 C19 118.8(3) . . ? C21 C20 C25 119.4(3) . . ? C19 C20 C25 121.8(3) . . ? C22 C21 C20 121.5(3) . . ? C21 C22 C23 120.0(3) . . ? C22 C23 C24 120.8(4) . . ? C23 C24 C19 118.5(3) . . ? C23 C24 C28 120.6(3) . . ? C19 C24 C28 120.8(2) . . ? C20 C25 C26 110.2(3) . . ? C20 C25 C27 113.3(3) . . ? C26 C25 C27 109.9(3) . . ? C29 C28 C24 110.5(3) . . ? C29 C28 C30 110.5(3) . . ? C24 C28 C30 113.8(3) . . ? N1 Li1 O2 131.3(3) . . ? N1 Li1 O1 121.1(3) . . ? O2 Li1 O1 104.3(3) . . ? C34 O1 C31 108.6(3) . . ? C34 O1 Li1 125.8(3) . . ? C31 O1 Li1 124.0(3) . . ? O1 C31 C32 106.0(4) . . ? C33 C32 C31 106.3(4) . . ? C34 C33 C32 106.8(5) . . ? C33 C34 O1 109.8(4) . . ? C35 O2 C38 108.9(3) . . ? C35 O2 Li1 120.4(3) . . ? C38 O2 Li1 127.3(3) . . ? O2 C35 C36 107.6(4) . . ? C37 C36 C35 108.2(4) . . ? C36 C37 C38 108.4(4) . . ? O2 C38 C37 105.6(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.405 _refine_diff_density_min -0.288 _refine_diff_density_rms 0.043 #===END data_Compound7.3THF _database_code_depnum_ccdc_archive 'CCDC 773252' #TrackingRef '- Newbams.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H63 B K2 N2 O3' _chemical_formula_sum 'C42 H63 B K2 N2 O3' _chemical_formula_weight 732.95 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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.456(2) _cell_length_b 15.323(3) _cell_length_c 27.854(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.91(3) _cell_angle_gamma 90.00 _cell_volume 4462.0(16) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 37588 _cell_measurement_theta_min 2.57 _cell_measurement_theta_max 25.03 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.091 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1584 _exptl_absorpt_coefficient_mu 0.248 _exptl_absorpt_correction_type Integration _exptl_absorpt_correction_T_min 0.9521 _exptl_absorpt_correction_T_max 0.9804 _exptl_absorpt_process_details 'HKL Scalepack (Otwinowski and Minor 1997)' _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 'Nonius Kappa CCD' _diffrn_measurement_method 'phi\omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37588 _diffrn_reflns_av_R_equivalents 0.0417 _diffrn_reflns_av_sigmaI/netI 0.0499 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 25.03 _reflns_number_total 7805 _reflns_number_gt 5465 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Nonius DENZO' _computing_data_reduction 'Nonius DENZO' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0618P)^2^+8.1699P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7805 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1202 _refine_ls_R_factor_gt 0.0859 _refine_ls_wR_factor_ref 0.2078 _refine_ls_wR_factor_gt 0.1908 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.093 _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 B1 B 0.0212(4) 0.1780(3) 0.30419(16) 0.0368(10) Uani 1 1 d . . . N1 N 0.0405(3) 0.0875(2) 0.30840(11) 0.0382(7) Uani 1 1 d . . . N2 N 0.0603(3) 0.2407(2) 0.33911(11) 0.0388(8) Uani 1 1 d . . . C1 C -0.0440(4) 0.2113(2) 0.25481(13) 0.0372(9) Uani 1 1 d . . . C2 C -0.0169(4) 0.2918(3) 0.23354(15) 0.0463(10) Uani 1 1 d . . . H2A H 0.0454 0.3283 0.2485 0.056 Uiso 1 1 calc R . . C3 C -0.0766(5) 0.3209(3) 0.19176(16) 0.0571(12) Uani 1 1 d . . . H3A H -0.0547 0.3761 0.1787 0.069 Uiso 1 1 calc R . . C4 C -0.1676(5) 0.2698(3) 0.16924(17) 0.0666(14) Uani 1 1 d . . . H4A H -0.2088 0.2891 0.1405 0.080 Uiso 1 1 calc R . . C5 C -0.1980(5) 0.1905(3) 0.18895(17) 0.0631(13) Uani 1 1 d . . . H5A H -0.2611 0.1550 0.1737 0.076 Uiso 1 1 calc R . . C6 C -0.1385(4) 0.1614(3) 0.23069(15) 0.0465(10) Uani 1 1 d . . . H6A H -0.1618 0.1063 0.2434 0.056 Uiso 1 1 calc R . . C7 C 0.0827(4) 0.0504(2) 0.35049(14) 0.0393(9) Uani 1 1 d . . . C8 C 0.2154(4) 0.0321(3) 0.35950(15) 0.0462(10) Uani 1 1 d . . . C9 C 0.2538(5) -0.0058(3) 0.40292(17) 0.0601(12) Uani 1 1 d . . . H9A H 0.3467 -0.0180 0.4089 0.072 Uiso 1 1 calc R . . C10 C 0.1672(5) -0.0257(3) 0.43830(17) 0.0642(14) Uani 1 1 d . . . H10A H 0.1970 -0.0520 0.4694 0.077 Uiso 1 1 calc R . . C11 C 0.0393(5) -0.0105(3) 0.42982(16) 0.0580(12) Uani 1 1 d . . . H11A H -0.0233 -0.0272 0.4550 0.070 Uiso 1 1 calc R . . C12 C -0.0064(4) 0.0259(3) 0.38722(14) 0.0450(10) Uani 1 1 d . . . C13 C 0.3149(4) 0.0529(3) 0.32208(17) 0.0537(11) Uani 1 1 d . . . H13A H 0.2690 0.0785 0.2936 0.064 Uiso 1 1 calc R . . C14 C 0.3840(5) -0.0296(4) 0.3051(2) 0.0803(16) Uani 1 1 d . . . H14A H 0.3208 -0.0725 0.2938 0.120 Uiso 1 1 calc R . . H14B H 0.4342 -0.0544 0.3318 0.120 Uiso 1 1 calc R . . H14C H 0.4411 -0.0146 0.2787 0.120 Uiso 1 1 calc R . . C15 C 0.4133(5) 0.1195(4) 0.3393(2) 0.0765(15) Uani 1 1 d . . . H15A H 0.3696 0.1727 0.3497 0.115 Uiso 1 1 calc R . . H15B H 0.4711 0.1335 0.3130 0.115 Uiso 1 1 calc R . . H15C H 0.4628 0.0952 0.3663 0.115 Uiso 1 1 calc R . . C16 C -0.1476(4) 0.0390(3) 0.37770(16) 0.0525(11) Uani 1 1 d . . . H16A H -0.1576 0.0951 0.3597 0.063 Uiso 1 1 calc R . . C17 C -0.2285(5) 0.0460(4) 0.42304(19) 0.0762(15) Uani 1 1 d . . . H17A H -0.1943 0.0925 0.4437 0.114 Uiso 1 1 calc R . . H17B H -0.2258 -0.0096 0.4404 0.114 Uiso 1 1 calc R . . H17C H -0.3172 0.0596 0.4139 0.114 Uiso 1 1 calc R . . C18 C -0.2002(5) -0.0332(4) 0.3455(2) 0.0733(15) Uani 1 1 d . . . H18A H -0.1483 -0.0375 0.3166 0.110 Uiso 1 1 calc R . . H18B H -0.2889 -0.0197 0.3363 0.110 Uiso 1 1 calc R . . H18C H -0.1975 -0.0888 0.3629 0.110 Uiso 1 1 calc R . . C19 C 0.0272(4) 0.3239(2) 0.34833(13) 0.0371(9) Uani 1 1 d . . . C20 C -0.1025(4) 0.3521(2) 0.35762(13) 0.0380(9) Uani 1 1 d . . . C21 C -0.1259(4) 0.4353(3) 0.37487(13) 0.0403(9) Uani 1 1 d . . . H21A H -0.2113 0.4508 0.3823 0.048 Uiso 1 1 calc R . . C22 C -0.0303(4) 0.4969(3) 0.38181(14) 0.0459(10) Uani 1 1 d . . . H22A H -0.0491 0.5534 0.3938 0.055 Uiso 1 1 calc R . . C23 C 0.0937(4) 0.4732(3) 0.37060(14) 0.0450(10) Uani 1 1 d . . . H23A H 0.1602 0.5149 0.3747 0.054 Uiso 1 1 calc R . . C24 C 0.1242(4) 0.3907(3) 0.35363(14) 0.0403(9) Uani 1 1 d . . . C25 C -0.2146(4) 0.2899(3) 0.35066(15) 0.0429(9) Uani 1 1 d . . . H25A H -0.1794 0.2325 0.3401 0.051 Uiso 1 1 calc R . . C26 C -0.3083(4) 0.3212(3) 0.31175(16) 0.0544(11) Uani 1 1 d . . . H26A H -0.2625 0.3305 0.2818 0.082 Uiso 1 1 calc R . . H26B H -0.3477 0.3761 0.3218 0.082 Uiso 1 1 calc R . . H26C H -0.3750 0.2771 0.3067 0.082 Uiso 1 1 calc R . . C27 C -0.2855(5) 0.2746(3) 0.39772(17) 0.0629(13) Uani 1 1 d . . . H27A H -0.2249 0.2542 0.4225 0.094 Uiso 1 1 calc R . . H27B H -0.3522 0.2304 0.3926 0.094 Uiso 1 1 calc R . . H27C H -0.3248 0.3293 0.4082 0.094 Uiso 1 1 calc R . . C28 C 0.2613(4) 0.3689(3) 0.34125(16) 0.0485(11) Uani 1 1 d . . . H28A H 0.2628 0.3063 0.3312 0.058 Uiso 1 1 calc R . . C29 C 0.3522(5) 0.3779(5) 0.3838(2) 0.0896(19) Uani 1 1 d . . . H29A H 0.3208 0.3429 0.4107 0.134 Uiso 1 1 calc R . . H29B H 0.3574 0.4393 0.3935 0.134 Uiso 1 1 calc R . . H29C H 0.4373 0.3572 0.3749 0.134 Uiso 1 1 calc R . . C30 C 0.3088(5) 0.4221(4) 0.29916(19) 0.0703(14) Uani 1 1 d . . . H30A H 0.2498 0.4149 0.2717 0.106 Uiso 1 1 calc R . . H30B H 0.3941 0.4018 0.2904 0.106 Uiso 1 1 calc R . . H30C H 0.3130 0.4838 0.3082 0.106 Uiso 1 1 calc R . . K1 K 0.08076(10) 0.00328(7) 0.22598(3) 0.0528(3) Uani 1 1 d . . . K2 K 0.14214(11) 0.18711(7) 0.42707(4) 0.0605(3) Uani 1 1 d . . . O1 O 0.2801(4) 0.1015(3) 0.18983(16) 0.0872(12) Uani 1 1 d . . . C31 C 0.2435(9) 0.1847(6) 0.1822(5) 0.184(6) Uani 1 1 d . . . H31A H 0.2309 0.1948 0.1473 0.221 Uiso 1 1 calc R . . H31B H 0.1612 0.1956 0.1982 0.221 Uiso 1 1 calc R . . C32 C 0.3306(15) 0.2382(7) 0.1992(5) 0.204(6) Uani 1 1 d . . . H32A H 0.3153 0.2512 0.2334 0.245 Uiso 1 1 calc R . . H32B H 0.3296 0.2937 0.1809 0.245 Uiso 1 1 calc R . . C33 C 0.4475(9) 0.1952(10) 0.1938(5) 0.233(8) Uani 1 1 d . . . H33A H 0.4976 0.1947 0.2243 0.279 Uiso 1 1 calc R . . H33B H 0.4992 0.2226 0.1684 0.279 Uiso 1 1 calc R . . C34 C 0.4048(8) 0.1022(5) 0.1794(4) 0.154(4) Uani 1 1 d . . . H34A H 0.4178 0.0918 0.1447 0.184 Uiso 1 1 calc R . . H34B H 0.4522 0.0575 0.1981 0.184 Uiso 1 1 calc R . . O2 O 0.3407(4) 0.2005(4) 0.49002(15) 0.1098(16) Uani 1 1 d . . . C35 C 0.4593(8) 0.1675(10) 0.4814(3) 0.200(6) Uani 1 1 d . . . H35A H 0.4504 0.1111 0.4644 0.240 Uiso 1 1 calc R . . H35B H 0.5058 0.2081 0.4602 0.240 Uiso 1 1 calc R . . C36 C 0.5253(10) 0.1559(10) 0.5204(4) 0.205(6) Uani 1 1 d . . . H36A H 0.6065 0.1889 0.5186 0.246 Uiso 1 1 calc R . . H36B H 0.5464 0.0933 0.5240 0.246 Uiso 1 1 calc R . . C37 C 0.4575(9) 0.1838(9) 0.5598(3) 0.185(5) Uani 1 1 d . . . H37A H 0.5019 0.2326 0.5763 0.222 Uiso 1 1 calc R . . H37B H 0.4455 0.1355 0.5830 0.222 Uiso 1 1 calc R . . C38 C 0.3316(7) 0.2129(6) 0.5387(2) 0.113(2) Uani 1 1 d . . . H38A H 0.2607 0.1778 0.5518 0.136 Uiso 1 1 calc R . . H38B H 0.3161 0.2752 0.5461 0.136 Uiso 1 1 calc R . . O3 O 0.0352(4) 0.2702(2) 0.49981(13) 0.0780(11) Uani 1 1 d . . . C39 C -0.0288(7) 0.2568(4) 0.5439(2) 0.103(2) Uani 1 1 d . . . H39A H 0.0293 0.2695 0.5715 0.123 Uiso 1 1 calc R . . H39B H -0.0584 0.1957 0.5465 0.123 Uiso 1 1 calc R . . C40 C -0.1384(6) 0.3170(4) 0.5437(2) 0.0794(16) Uani 1 1 d . . . H40A H -0.1530 0.3407 0.5762 0.095 Uiso 1 1 calc R . . H40B H -0.2171 0.2873 0.5322 0.095 Uiso 1 1 calc R . . C41 C -0.1004(5) 0.3893(3) 0.50929(18) 0.0680(14) Uani 1 1 d . . . H41A H -0.1623 0.3939 0.4821 0.082 Uiso 1 1 calc R . . H41B H -0.0952 0.4462 0.5260 0.082 Uiso 1 1 calc R . . C42 C 0.0279(6) 0.3614(3) 0.49234(19) 0.0719(15) Uani 1 1 d . . . H42A H 0.0373 0.3753 0.4579 0.086 Uiso 1 1 calc R . . H42B H 0.0964 0.3916 0.5108 0.086 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 B1 0.035(2) 0.039(3) 0.036(2) -0.0002(19) 0.0029(18) 0.0002(19) N1 0.0472(19) 0.0324(17) 0.0350(18) -0.0022(14) -0.0035(14) 0.0000(14) N2 0.0417(18) 0.0338(18) 0.0406(19) -0.0034(14) -0.0068(14) 0.0027(14) C1 0.042(2) 0.036(2) 0.034(2) -0.0025(17) 0.0034(16) 0.0073(17) C2 0.050(2) 0.042(2) 0.048(2) 0.0045(19) 0.0072(19) 0.0051(19) C3 0.081(3) 0.044(3) 0.046(3) 0.010(2) 0.005(2) 0.018(2) C4 0.097(4) 0.061(3) 0.042(3) -0.002(2) -0.017(3) 0.032(3) C5 0.074(3) 0.057(3) 0.057(3) -0.011(2) -0.025(2) 0.018(3) C6 0.053(2) 0.038(2) 0.048(3) -0.0048(19) -0.008(2) 0.0095(19) C7 0.053(2) 0.028(2) 0.036(2) -0.0053(16) -0.0048(18) 0.0003(17) C8 0.054(3) 0.040(2) 0.043(2) -0.0056(19) -0.0066(19) 0.002(2) C9 0.059(3) 0.063(3) 0.058(3) 0.000(2) -0.015(2) 0.013(2) C10 0.086(4) 0.061(3) 0.045(3) 0.010(2) -0.016(3) 0.018(3) C11 0.078(3) 0.052(3) 0.044(3) 0.008(2) 0.001(2) 0.008(2) C12 0.061(3) 0.035(2) 0.038(2) 0.0005(17) -0.0054(19) 0.0046(19) C13 0.049(3) 0.056(3) 0.056(3) -0.005(2) -0.010(2) 0.003(2) C14 0.082(4) 0.066(3) 0.094(4) -0.014(3) 0.024(3) -0.001(3) C15 0.077(4) 0.063(3) 0.089(4) -0.008(3) -0.002(3) -0.010(3) C16 0.057(3) 0.050(3) 0.051(3) 0.005(2) 0.008(2) 0.008(2) C17 0.076(3) 0.083(4) 0.071(4) 0.011(3) 0.019(3) 0.012(3) C18 0.062(3) 0.079(4) 0.078(4) -0.003(3) -0.002(3) -0.006(3) C19 0.043(2) 0.037(2) 0.031(2) 0.0029(16) -0.0028(16) 0.0007(17) C20 0.049(2) 0.035(2) 0.030(2) 0.0010(16) -0.0002(17) -0.0005(18) C21 0.044(2) 0.046(2) 0.031(2) 0.0033(17) 0.0008(16) 0.0052(19) C22 0.067(3) 0.034(2) 0.037(2) -0.0042(18) -0.0034(19) 0.000(2) C23 0.052(2) 0.042(2) 0.041(2) -0.0008(18) -0.0078(19) -0.011(2) C24 0.045(2) 0.036(2) 0.040(2) 0.0015(17) -0.0058(17) -0.0055(18) C25 0.039(2) 0.043(2) 0.047(2) -0.0041(19) 0.0013(18) -0.0016(18) C26 0.043(2) 0.064(3) 0.057(3) -0.005(2) -0.005(2) -0.005(2) C27 0.061(3) 0.066(3) 0.062(3) 0.000(3) 0.009(2) -0.013(2) C28 0.038(2) 0.041(2) 0.066(3) 0.000(2) -0.005(2) -0.0042(19) C29 0.054(3) 0.139(6) 0.076(4) 0.010(4) -0.010(3) 0.006(3) C30 0.050(3) 0.086(4) 0.075(4) 0.010(3) 0.009(2) -0.003(3) K1 0.0624(6) 0.0574(6) 0.0388(5) -0.0104(4) 0.0038(4) -0.0048(5) K2 0.0778(7) 0.0578(6) 0.0454(6) -0.0128(5) -0.0152(5) 0.0101(5) O1 0.063(2) 0.078(3) 0.122(3) 0.007(2) 0.012(2) -0.006(2) C31 0.109(7) 0.101(7) 0.347(18) 0.042(9) 0.105(9) 0.028(6) C32 0.264(16) 0.087(7) 0.258(14) -0.061(8) -0.101(13) 0.013(9) C33 0.089(6) 0.265(15) 0.342(18) 0.181(14) -0.078(9) -0.093(8) C34 0.124(7) 0.102(6) 0.239(11) 0.034(7) 0.099(7) 0.031(5) O2 0.076(3) 0.186(5) 0.067(3) -0.022(3) -0.018(2) 0.024(3) C35 0.085(5) 0.42(2) 0.101(7) -0.073(9) -0.017(5) 0.078(9) C36 0.146(9) 0.348(18) 0.122(8) 0.030(10) -0.005(7) 0.134(10) C37 0.127(7) 0.347(17) 0.078(6) 0.019(8) -0.028(5) 0.081(9) C38 0.108(5) 0.161(7) 0.069(4) 0.003(4) -0.002(4) 0.030(5) O3 0.119(3) 0.055(2) 0.060(2) 0.0030(17) 0.019(2) 0.015(2) C39 0.147(6) 0.066(4) 0.096(5) 0.024(3) 0.042(4) 0.017(4) C40 0.086(4) 0.077(4) 0.076(4) 0.000(3) 0.012(3) -0.008(3) C41 0.096(4) 0.057(3) 0.051(3) -0.002(2) -0.011(3) 0.004(3) C42 0.100(4) 0.058(3) 0.058(3) 0.007(3) 0.012(3) 0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 N1 1.407(5) . ? B1 N2 1.422(5) . ? B1 C1 1.608(6) . ? B1 K1 3.514(5) . ? N1 C7 1.370(5) . ? N1 K1 2.673(3) . ? N2 C19 1.347(5) . ? N2 K2 2.709(3) . ? C1 C2 1.399(5) . ? C1 C6 1.411(5) . ? C2 C3 1.385(6) . ? C2 K1 3.499(4) 2 ? C3 C4 1.377(7) . ? C4 C5 1.372(7) . ? C5 C6 1.384(6) . ? C6 K1 3.339(4) . ? C7 C8 1.433(6) . ? C7 C12 1.444(6) . ? C7 K2 3.047(4) . ? C8 C9 1.395(6) . ? C8 C13 1.519(6) . ? C8 K2 3.133(4) . ? C9 C10 1.383(7) . ? C9 K2 3.253(5) . ? C10 C11 1.374(7) . ? C10 K2 3.285(5) . ? C11 C12 1.389(6) . ? C11 K2 3.214(5) . ? C12 C16 1.509(6) . ? C12 K2 3.113(4) . ? C13 C15 1.521(6) . ? C13 C14 1.535(7) . ? C16 C18 1.521(7) . ? C16 C17 1.535(6) . ? C19 C24 1.447(5) . ? C19 C20 1.450(5) . ? C19 K2 3.250(4) . ? C20 C21 1.386(5) . ? C20 C25 1.521(5) . ? C20 K1 3.295(4) 2 ? C21 C22 1.386(6) . ? C21 K1 3.040(4) 2 ? C22 C23 1.388(6) . ? C22 K1 3.042(4) 2 ? C23 C24 1.388(6) . ? C23 K1 3.259(4) 2 ? C24 C28 1.517(6) . ? C24 K1 3.512(4) 2 ? C25 C26 1.527(6) . ? C25 C27 1.534(6) . ? C28 C29 1.515(6) . ? C28 C30 1.517(6) . ? K1 O1 2.773(4) . ? K1 C21 3.040(4) 2_545 ? K1 C22 3.042(4) 2_545 ? K1 C23 3.259(4) 2_545 ? K1 C20 3.295(4) 2_545 ? K1 C31 3.489(9) . ? K1 C2 3.499(4) 2_545 ? K1 C24 3.512(4) 2_545 ? K2 O3 2.655(4) . ? K2 O2 2.704(4) . ? K2 C42 3.454(5) . ? O1 C34 1.340(8) . ? O1 C31 1.347(9) . ? C31 C32 1.308(13) . ? C32 C33 1.399(15) . ? C33 C34 1.545(15) . ? O2 C35 1.364(8) . ? O2 C38 1.375(7) . ? C35 C36 1.290(11) . ? C36 C37 1.383(11) . ? C37 C38 1.500(10) . ? O3 C42 1.415(6) . ? O3 C39 1.423(6) . ? C39 C40 1.471(8) . ? C40 C41 1.521(7) . ? C41 C42 1.491(7) . ? 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 N1 B1 N2 124.7(4) . . ? N1 B1 C1 116.3(3) . . ? N2 B1 C1 119.0(3) . . ? N1 B1 K1 43.40(19) . . ? N2 B1 K1 152.5(3) . . ? C1 B1 K1 77.8(2) . . ? C7 N1 B1 121.6(3) . . ? C7 N1 K1 118.8(2) . . ? B1 N1 K1 115.4(2) . . ? C19 N2 B1 134.2(3) . . ? C19 N2 K2 101.1(2) . . ? B1 N2 K2 119.8(2) . . ? C2 C1 C6 114.9(4) . . ? C2 C1 B1 123.8(4) . . ? C6 C1 B1 121.3(3) . . ? C3 C2 C1 123.3(4) . . ? C3 C2 K1 83.5(3) . 2 ? C1 C2 K1 129.7(3) . 2 ? C4 C3 C2 119.9(4) . . ? C5 C4 C3 119.0(4) . . ? C4 C5 C6 121.2(5) . . ? C5 C6 C1 121.8(4) . . ? C5 C6 K1 120.1(3) . . ? C1 C6 K1 86.3(2) . . ? N1 C7 C8 121.9(4) . . ? N1 C7 C12 120.7(4) . . ? C8 C7 C12 117.3(4) . . ? N1 C7 K2 111.9(2) . . ? C8 C7 K2 80.0(2) . . ? C12 C7 K2 79.0(2) . . ? C9 C8 C7 119.9(4) . . ? C9 C8 C13 119.4(4) . . ? C7 C8 C13 120.7(4) . . ? C9 C8 K2 82.2(3) . . ? C7 C8 K2 73.3(2) . . ? C13 C8 K2 115.5(3) . . ? C10 C9 C8 121.7(4) . . ? C10 C9 K2 79.1(3) . . ? C8 C9 K2 72.6(3) . . ? C11 C10 C9 119.2(4) . . ? C11 C10 K2 74.9(3) . . ? C9 C10 K2 76.5(3) . . ? C10 C11 C12 122.4(5) . . ? C10 C11 K2 80.7(3) . . ? C12 C11 K2 73.3(3) . . ? C11 C12 C7 119.5(4) . . ? C11 C12 C16 121.7(4) . . ? C7 C12 C16 118.8(4) . . ? C11 C12 K2 81.4(3) . . ? C7 C12 K2 73.9(2) . . ? C16 C12 K2 116.0(3) . . ? C8 C13 C15 113.1(4) . . ? C8 C13 C14 111.7(4) . . ? C15 C13 C14 109.3(4) . . ? C12 C16 C18 110.6(4) . . ? C12 C16 C17 114.5(4) . . ? C18 C16 C17 109.7(4) . . ? N2 C19 C24 120.5(3) . . ? N2 C19 C20 124.1(3) . . ? C24 C19 C20 115.3(3) . . ? N2 C19 K2 54.88(19) . . ? C24 C19 K2 97.8(2) . . ? C20 C19 K2 114.1(2) . . ? C21 C20 C19 120.5(4) . . ? C21 C20 C25 118.7(4) . . ? C19 C20 C25 120.8(3) . . ? C21 C20 K1 67.2(2) . 2 ? C19 C20 K1 90.5(2) . 2 ? C25 C20 K1 114.3(2) . 2 ? C20 C21 C22 123.0(4) . . ? C20 C21 K1 87.9(2) . 2 ? C22 C21 K1 76.9(2) . 2 ? C21 C22 C23 117.7(4) . . ? C21 C22 K1 76.8(2) . 2 ? C23 C22 K1 86.2(2) . 2 ? C22 C23 C24 122.4(4) . . ? C22 C23 K1 68.6(2) . 2 ? C24 C23 K1 88.6(2) . 2 ? C23 C24 C19 121.0(4) . . ? C23 C24 C28 120.0(4) . . ? C19 C24 C28 119.0(3) . . ? C23 C24 K1 68.1(2) . 2 ? C19 C24 K1 82.2(2) . 2 ? C28 C24 K1 122.3(3) . 2 ? C20 C25 C26 112.3(3) . . ? C20 C25 C27 111.7(3) . . ? C26 C25 C27 109.9(3) . . ? C29 C28 C24 112.7(4) . . ? C29 C28 C30 110.3(4) . . ? C24 C28 C30 112.3(4) . . ? N1 K1 O1 100.35(12) . . ? N1 K1 C21 171.15(11) . 2_545 ? O1 K1 C21 73.84(12) . 2_545 ? N1 K1 C22 146.74(11) . 2_545 ? O1 K1 C22 77.20(13) . 2_545 ? C21 K1 C22 26.35(10) 2_545 2_545 ? N1 K1 C23 133.13(11) . 2_545 ? O1 K1 C23 101.03(12) . 2_545 ? C21 K1 C23 44.10(11) 2_545 2_545 ? C22 K1 C23 25.14(11) 2_545 2_545 ? N1 K1 C20 163.72(10) . 2_545 ? O1 K1 C20 93.69(12) . 2_545 ? C21 K1 C20 24.86(10) 2_545 2_545 ? C22 K1 C20 44.99(10) 2_545 2_545 ? C23 K1 C20 50.29(10) 2_545 2_545 ? N1 K1 C6 59.90(10) . . ? O1 K1 C6 98.10(12) . . ? C21 K1 C6 113.69(11) 2_545 . ? C22 K1 C6 87.35(11) 2_545 . ? C23 K1 C6 76.09(10) 2_545 . ? C20 K1 C6 126.37(10) 2_545 . ? N1 K1 C31 90.0(2) . . ? O1 K1 C31 21.14(14) . . ? C21 K1 C31 82.3(3) 2_545 . ? C22 K1 C31 76.0(3) 2_545 . ? C23 K1 C31 95.4(3) 2_545 . ? C20 K1 C31 105.9(2) 2_545 . ? C6 K1 C31 76.97(15) . . ? N1 K1 C2 97.85(10) . 2_545 ? O1 K1 C2 140.17(12) . 2_545 ? C21 K1 C2 90.78(10) 2_545 2_545 ? C22 K1 C2 104.92(11) 2_545 2_545 ? C23 K1 C2 91.59(10) 2_545 2_545 ? C20 K1 C2 65.93(10) 2_545 2_545 ? C6 K1 C2 121.65(11) . 2_545 ? C31 K1 C2 161.27(16) . 2_545 ? N1 K1 C24 132.58(10) . 2_545 ? O1 K1 C24 119.47(12) . 2_545 ? C21 K1 C24 49.49(10) 2_545 2_545 ? C22 K1 C24 42.83(11) 2_545 2_545 ? C23 K1 C24 23.28(10) 2_545 2_545 ? C20 K1 C24 41.98(9) 2_545 2_545 ? C6 K1 C24 88.22(10) . 2_545 ? C31 K1 C24 117.8(3) . 2_545 ? C2 K1 C24 68.34(10) 2_545 2_545 ? N1 K1 B1 21.21(10) . . ? O1 K1 B1 87.32(12) . . ? C21 K1 B1 149.96(11) 2_545 . ? C22 K1 B1 127.36(11) 2_545 . ? C23 K1 B1 121.15(11) 2_545 . ? C20 K1 B1 171.41(10) 2_545 . ? C6 K1 B1 45.10(10) . . ? C31 K1 B1 72.7(2) . . ? C2 K1 B1 117.99(10) 2_545 . ? C24 K1 B1 130.80(10) 2_545 . ? O3 K2 O2 78.30(13) . . ? O3 K2 N2 114.46(11) . . ? O2 K2 N2 142.32(14) . . ? O3 K2 C7 141.29(13) . . ? O2 K2 C7 130.69(14) . . ? N2 K2 C7 61.15(10) . . ? O3 K2 C12 116.02(13) . . ? O2 K2 C12 131.68(15) . . ? N2 K2 C12 76.68(10) . . ? C7 K2 C12 27.10(11) . . ? O3 K2 C8 158.73(12) . . ? O2 K2 C8 104.75(13) . . ? N2 K2 C8 76.31(10) . . ? C7 K2 C8 26.77(10) . . ? C12 K2 C8 46.34(11) . . ? O3 K2 C11 106.75(12) . . ? O2 K2 C11 108.05(15) . . ? N2 K2 C11 101.89(11) . . ? C7 K2 C11 45.92(11) . . ? C12 K2 C11 25.29(11) . . ? C8 K2 C11 52.07(12) . . ? O3 K2 C19 92.87(11) . . ? O2 K2 C19 131.34(15) . . ? N2 K2 C19 23.99(9) . . ? C7 K2 C19 84.37(10) . . ? C12 K2 C19 95.39(10) . . ? C8 K2 C19 100.07(11) . . ? C11 K2 C19 120.21(11) . . ? O3 K2 C9 138.64(12) . . ? O2 K2 C9 85.90(14) . . ? N2 K2 C9 101.40(11) . . ? C7 K2 C9 45.58(11) . . ? C12 K2 C9 51.96(12) . . ? C8 K2 C9 25.15(11) . . ? C11 K2 C9 43.13(13) . . ? C19 K2 C9 125.22(11) . . ? O3 K2 C10 115.91(13) . . ? O2 K2 C10 87.39(15) . . ? N2 K2 C10 114.23(11) . . ? C7 K2 C10 53.08(11) . . ? C12 K2 C10 44.36(11) . . ? C8 K2 C10 44.35(12) . . ? C11 K2 C10 24.38(12) . . ? C19 K2 C10 137.07(11) . . ? C9 K2 C10 24.42(12) . . ? O3 K2 C42 22.22(11) . . ? O2 K2 C42 82.45(14) . . ? N2 K2 C42 97.74(12) . . ? C7 K2 C42 146.27(13) . . ? C12 K2 C42 128.77(13) . . ? C8 K2 C42 172.79(13) . . ? C11 K2 C42 126.65(13) . . ? C19 K2 C42 74.29(11) . . ? C9 K2 C42 160.00(13) . . ? C10 K2 C42 138.14(13) . . ? C34 O1 C31 103.5(6) . . ? C34 O1 K1 145.4(4) . . ? C31 O1 K1 110.9(4) . . ? C32 C31 O1 110.0(10) . . ? C32 C31 K1 135.5(12) . . ? O1 C31 K1 47.9(3) . . ? C31 C32 C33 105.7(9) . . ? C32 C33 C34 102.3(7) . . ? O1 C34 C33 103.3(7) . . ? C35 O2 C38 107.6(5) . . ? C35 O2 K2 123.3(4) . . ? C38 O2 K2 125.9(4) . . ? C36 C35 O2 112.2(8) . . ? C35 C36 C37 110.6(8) . . ? C36 C37 C38 103.8(7) . . ? O2 C38 C37 105.7(6) . . ? C42 O3 C39 104.1(4) . . ? C42 O3 K2 112.6(3) . . ? C39 O3 K2 143.1(3) . . ? O3 C39 C40 106.4(5) . . ? C39 C40 C41 104.4(5) . . ? C42 C41 C40 103.7(4) . . ? O3 C42 C41 106.4(4) . . ? O3 C42 K2 45.2(2) . . ? C41 C42 K2 135.1(4) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.407 _refine_diff_density_min -0.390 _refine_diff_density_rms 0.057 _platon_squeeze_details ; Electron density in two regions were attributed to a disordered hexane molecule for which no suitable model could be found. These regions of electron density were removed from the reflections data using the program SQUEEZE (PLATON), leaving a void of 327.4 angstroms cubed ;