####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_BIF-n _publ_requested_journal 'Chem. Mater.' loop_ _publ_author_name 'Tao Wu' 'Jian Zhang' 'Xianhui Bu' 'Pingyun Feng' _publ_contact_author_name 'Pingyun Feng' _publ_contact_author_address ; Department of Chemistry University of California Riverside, CA 92521 UNITED STATES OF AMERICA ; _publ_contact_author_email 'pingyun.feng@ucr.edu' _publ_section_title ; Variable Lithium Coordination Modes in Two- and Three-Dimensional Lithium Boron Imidazolate Frameworks ; # Attachment 'BIF-n.cif' data_BIF-10 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H39 B2 Li2 N13 O' _chemical_formula_weight 597.21 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 Cc 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 13.6623(5) _cell_length_b 13.9688(6) _cell_length_c 18.0454(9) _cell_angle_alpha 90.00 _cell_angle_beta 111.235(3) _cell_angle_gamma 90.00 _cell_volume 3210.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.236 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1264 _exptl_absorpt_coefficient_mu 0.080 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6225 _diffrn_reflns_av_R_equivalents 0.0543 _diffrn_reflns_av_sigmaI/netI 0.0824 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 22.49 _reflns_number_total 3204 _reflns_number_gt 2487 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+5.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00 _refine_ls_number_reflns 3204 _refine_ls_number_parameters 422 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1180 _refine_ls_R_factor_gt 0.0960 _refine_ls_wR_factor_ref 0.2889 _refine_ls_wR_factor_gt 0.2684 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.017 _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 0.4514(3) 0.9071(3) 0.7602(2) 0.0397(12) Uani 1 1 d . . . H101 H 0.528(2) 0.978(2) 0.7626(17) 0.026(8) Uiso 1 1 d . . . B2 B 0.3308(3) 0.3440(3) 0.6048(3) 0.0428(12) Uani 1 1 d . . . H102 H 0.2817(17) 0.3066(17) 0.6030(14) 0.006(6) Uiso 1 1 d . . . Li1 Li 0.2842(4) 0.8400(5) 0.4303(3) 0.0494(19) Uani 1 1 d . . . Li2 Li 0.1913(5) 0.6343(5) 0.7697(4) 0.060(2) Uani 1 1 d . . . N1 N 0.5222(3) 0.6304(2) 0.5065(2) 0.0670(13) Uani 1 1 d . . . O1 O 0.3894(2) 0.7289(2) 0.43495(19) 0.0734(11) Uani 1 1 d . . . C1 C 0.5521(5) 0.6000(6) 0.4471(4) 0.151(3) Uani 1 1 d . . . H1A H 0.6269 0.6061 0.4629 0.226 Uiso 1 1 calc R . . H1B H 0.5183 0.6381 0.4006 0.226 Uiso 1 1 calc R . . H1C H 0.5324 0.5341 0.4355 0.226 Uiso 1 1 calc R . . C2 C 0.5820(7) 0.6000(8) 0.5912(5) 0.272(4) Uani 1 1 d . . . H2A H 0.5979 0.5329 0.5925 0.409 Uiso 1 1 calc R . . H2B H 0.5400 0.6120 0.6229 0.409 Uiso 1 1 calc R . . H2C H 0.6462 0.6358 0.6121 0.409 Uiso 1 1 calc R . . C3 C 0.4412(4) 0.6932(4) 0.4978(4) 0.0943(18) Uani 1 1 d . . . H3 H 0.4257 0.7089 0.5424 0.113 Uiso 1 1 calc R . . N11 N 0.5112(2) 0.81349(19) 0.79066(17) 0.0424(9) Uani 1 1 d . . . N12 N 0.6376(2) 0.7119(2) 0.8608(2) 0.0489(10) Uani 1 1 d . . . C11 C 0.5996(3) 0.8015(3) 0.8555(2) 0.0458(12) Uani 1 1 d . . . C12 C 0.4894(3) 0.7226(3) 0.7548(2) 0.0525(12) Uani 1 1 d . . . H12 H 0.4314 0.7076 0.7099 0.063 Uiso 1 1 calc R . . C13 C 0.5651(3) 0.6609(3) 0.7954(2) 0.0516(13) Uani 1 1 d . . . H13 H 0.5694 0.5968 0.7831 0.062 Uiso 1 1 calc R . . C14 C 0.6481(4) 0.8751(4) 0.9141(3) 0.0789(17) Uani 1 1 d . . . H14A H 0.5955 0.9200 0.9154 0.118 Uiso 1 1 calc R . . H14B H 0.7007 0.9078 0.9001 0.118 Uiso 1 1 calc R . . H14C H 0.6800 0.8462 0.9655 0.118 Uiso 1 1 calc R . . N21 N 0.3972(2) 0.94154(19) 0.81718(17) 0.0414(8) Uani 1 1 d . . . N22 N 0.3222(2) 1.0396(2) 0.88008(18) 0.0507(10) Uani 1 1 d . . . C21 C 0.3602(3) 1.0305(3) 0.8227(2) 0.0480(12) Uani 1 1 d . . . C22 C 0.3781(3) 0.8886(3) 0.8764(2) 0.0481(11) Uani 1 1 d . . . H22 H 0.3909 0.8237 0.8873 0.058 Uiso 1 1 calc R . . C23 C 0.3372(3) 0.9514(3) 0.9146(2) 0.0514(12) Uani 1 1 d . . . H23 H 0.3212 0.9361 0.9591 0.062 Uiso 1 1 calc R . . C24 C 0.3610(3) 1.1123(3) 0.7680(3) 0.0680(15) Uani 1 1 d . . . H24A H 0.3347 1.0903 0.7139 0.102 Uiso 1 1 calc R . . H24B H 0.4315 1.1353 0.7813 0.102 Uiso 1 1 calc R . . H24C H 0.3172 1.1632 0.7740 0.102 Uiso 1 1 calc R . . N31 N 0.3715(2) 0.89128(19) 0.67604(16) 0.0388(8) Uani 1 1 d . . . N32 N 0.3047(2) 0.8653(2) 0.54503(18) 0.0498(10) Uani 1 1 d . . . C31 C 0.3882(2) 0.8877(2) 0.6069(2) 0.0399(10) Uani 1 1 d . . . C32 C 0.2639(3) 0.8728(3) 0.6550(2) 0.0514(12) Uani 1 1 d . . . H32 H 0.2250 0.8720 0.6879 0.062 Uiso 1 1 calc R . . C33 C 0.2302(3) 0.8565(3) 0.5763(2) 0.0508(12) Uani 1 1 d . . . H33 H 0.1610 0.8405 0.5463 0.061 Uiso 1 1 calc R . . C34 C 0.4921(3) 0.9005(3) 0.6005(3) 0.0584(12) Uani 1 1 d . . . H34A H 0.5287 0.8404 0.6101 0.088 Uiso 1 1 calc R . . H34B H 0.5319 0.9466 0.6392 0.088 Uiso 1 1 calc R . . H34C H 0.4832 0.9228 0.5482 0.088 Uiso 1 1 calc R . . N41 N 0.4427(2) 0.3198(2) 0.66104(17) 0.0475(9) Uani 1 1 d . . . N42 N 0.5869(2) 0.2341(2) 0.72710(18) 0.0539(10) Uani 1 1 d . . . C41 C 0.4944(3) 0.2370(3) 0.6668(2) 0.0580(13) Uani 1 1 d . . . C42 C 0.5098(3) 0.3763(3) 0.7258(2) 0.0435(11) Uani 1 1 d . . . H42 H 0.4970 0.4384 0.7384 0.052 Uiso 1 1 calc R . . C43 C 0.5945(2) 0.3231(3) 0.7649(2) 0.0530(12) Uani 1 1 d . . . H43 H 0.6499 0.3422 0.8103 0.064 Uiso 1 1 calc R . . C44 C 0.4546(5) 0.1610(3) 0.6050(3) 0.0796(18) Uani 1 1 d . . . H44A H 0.4101 0.1894 0.5559 0.119 Uiso 1 1 calc R . . H44B H 0.4153 0.1148 0.6221 0.119 Uiso 1 1 calc R . . H44C H 0.5129 0.1301 0.5972 0.119 Uiso 1 1 calc R . . N51 N 0.3284(2) 0.3569(2) 0.51848(17) 0.0449(9) Uani 1 1 d . . . N52 N 0.2696(3) 0.3731(3) 0.3883(2) 0.0625(12) Uani 1 1 d . . . C51 C 0.2490(3) 0.3574(3) 0.4514(2) 0.0479(11) Uani 1 1 d . . . C52 C 0.4156(3) 0.3727(3) 0.4965(2) 0.0487(12) Uani 1 1 d . . . H52 H 0.4857 0.3751 0.5300 0.058 Uiso 1 1 calc R . . C53 C 0.3763(3) 0.3839(3) 0.4156(2) 0.0613(13) Uani 1 1 d . . . H53 H 0.4158 0.3967 0.3842 0.074 Uiso 1 1 calc R . . C54 C 0.1332(3) 0.3521(3) 0.4484(3) 0.0632(14) Uani 1 1 d . . . H54A H 0.0874 0.3355 0.3956 0.095 Uiso 1 1 calc R . . H54B H 0.1130 0.4132 0.4627 0.095 Uiso 1 1 calc R . . H54C H 0.1281 0.3044 0.4851 0.095 Uiso 1 1 calc R . . N61 N 0.2960(2) 0.4419(2) 0.63275(18) 0.0438(9) Uani 1 1 d . . . N62 N 0.2379(2) 0.5489(2) 0.6972(2) 0.0531(10) Uani 1 1 d . . . C61 C 0.2637(3) 0.4582(3) 0.6937(2) 0.0494(12) Uani 1 1 d . . . C62 C 0.2879(3) 0.5284(3) 0.5943(2) 0.0522(12) Uani 1 1 d . . . H62 H 0.3041 0.5404 0.5494 0.063 Uiso 1 1 calc R . . C63 C 0.2527(3) 0.5912(3) 0.6336(2) 0.0546(12) Uani 1 1 d . . . H63 H 0.2397 0.6554 0.6199 0.065 Uiso 1 1 calc R . . C64 C 0.2608(3) 0.3782(4) 0.7491(3) 0.0704(14) Uani 1 1 d . . . H64A H 0.2206 0.3981 0.7804 0.106 Uiso 1 1 calc R . . H64B H 0.3311 0.3630 0.7837 0.106 Uiso 1 1 calc R . . H64C H 0.2289 0.3227 0.7186 0.106 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 0.0457(18) 0.0216(18) 0.050(2) -0.0021(17) 0.0158(16) 0.0016(16) B2 0.0352(15) 0.040(2) 0.059(2) 0.0082(18) 0.0243(14) -0.0002(16) Li1 0.040(3) 0.069(4) 0.035(3) 0.007(3) 0.009(2) -0.015(3) Li2 0.049(3) 0.069(4) 0.060(4) -0.012(3) 0.017(3) 0.017(3) N1 0.0727(19) 0.0450(18) 0.079(2) -0.0023(17) 0.0220(17) 0.0162(16) O1 0.0579(14) 0.081(2) 0.0759(19) 0.0022(16) 0.0177(13) 0.0097(14) C1 0.199(4) 0.144(5) 0.165(4) -0.018(4) 0.134(3) -0.058(4) C2 0.333(6) 0.391(8) 0.102(5) 0.063(5) 0.089(5) 0.284(5) C3 0.081(2) 0.108(4) 0.114(3) -0.032(3) 0.0598(19) -0.004(3) N11 0.0417(13) 0.0357(14) 0.0512(15) -0.0053(13) 0.0185(11) 0.0015(12) N12 0.0489(14) 0.0341(15) 0.0607(18) -0.0019(14) 0.0162(13) 0.0129(13) C11 0.0401(17) 0.055(2) 0.0358(18) -0.0028(16) 0.0066(14) 0.0069(16) C12 0.0426(17) 0.053(2) 0.059(2) -0.0225(17) 0.0152(15) -0.0039(16) C13 0.0417(17) 0.040(2) 0.068(2) 0.0066(17) 0.0144(16) 0.0050(16) C14 0.064(2) 0.111(3) 0.049(2) -0.036(2) 0.005(2) 0.006(2) N21 0.0471(13) 0.0383(15) 0.0438(15) 0.0055(13) 0.0224(10) 0.0018(12) N22 0.0585(15) 0.0476(17) 0.0455(16) -0.0014(13) 0.0183(12) 0.0267(13) C21 0.0575(19) 0.0424(19) 0.0429(19) -0.0036(16) 0.0167(15) 0.0092(16) C22 0.0570(17) 0.041(2) 0.0522(19) 0.0015(16) 0.0269(14) -0.0047(16) C23 0.0568(17) 0.059(2) 0.0440(18) 0.0123(17) 0.0246(13) 0.0012(17) C24 0.084(2) 0.040(2) 0.088(3) 0.0204(19) 0.0398(19) 0.0089(19) N31 0.0433(13) 0.0344(15) 0.0397(14) 0.0029(12) 0.0161(11) 0.0077(12) N32 0.0555(16) 0.0559(18) 0.0359(15) -0.0016(14) 0.0140(12) 0.0110(14) C31 0.0363(15) 0.0444(19) 0.0407(17) -0.0052(15) 0.0160(12) 0.0052(14) C32 0.0387(16) 0.069(2) 0.0497(19) 0.0011(19) 0.0196(13) 0.0013(17) C33 0.0376(16) 0.071(2) 0.040(2) 0.0053(18) 0.0105(14) -0.0082(17) C34 0.0534(17) 0.069(2) 0.059(2) -0.0063(19) 0.0281(14) -0.0259(17) N41 0.0420(13) 0.0591(18) 0.0398(15) -0.0056(14) 0.0127(11) 0.0158(13) N42 0.0436(14) 0.072(2) 0.0458(16) -0.0024(15) 0.0160(12) 0.0170(14) C41 0.074(2) 0.052(2) 0.051(2) -0.0058(18) 0.0254(17) 0.0111(18) C42 0.0407(15) 0.0403(19) 0.0538(19) -0.0018(16) 0.0223(13) 0.0026(14) C43 0.0367(15) 0.080(3) 0.0502(19) -0.0121(19) 0.0255(13) 0.0013(17) C44 0.134(4) 0.028(2) 0.068(3) -0.0089(19) 0.026(3) 0.015(2) N51 0.0469(14) 0.0500(17) 0.0354(15) -0.0017(13) 0.0121(11) 0.0117(13) N52 0.0691(18) 0.067(2) 0.0494(18) -0.0032(16) 0.0194(14) -0.0037(17) C51 0.0587(18) 0.048(2) 0.0365(18) 0.0003(16) 0.0167(14) -0.0168(17) C52 0.0396(16) 0.055(2) 0.056(2) 0.0036(17) 0.0237(14) 0.0064(15) C53 0.0536(16) 0.079(3) 0.069(2) -0.009(2) 0.0432(13) -0.0120(18) C54 0.0433(18) 0.073(3) 0.072(3) -0.006(2) 0.0193(17) -0.0133(18) N61 0.0509(14) 0.0342(15) 0.0447(16) -0.0015(13) 0.0155(12) 0.0021(13) N62 0.0626(16) 0.0274(14) 0.0680(19) -0.0080(14) 0.0219(14) 0.0148(13) C61 0.0364(15) 0.080(3) 0.0321(17) 0.0162(18) 0.0128(12) 0.0098(17) C62 0.0580(18) 0.043(2) 0.060(2) 0.0154(17) 0.0260(15) 0.0061(16) C63 0.0608(19) 0.0402(19) 0.061(2) 0.0009(18) 0.0203(16) 0.0185(17) C64 0.079(2) 0.091(3) 0.057(2) 0.014(2) 0.0441(15) 0.011(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 N31 1.531(4) . ? B1 N11 1.535(4) . ? B1 N21 1.546(6) . ? B1 H101 1.42(3) . ? B2 N41 1.536(4) . ? B2 N51 1.556(6) . ? B2 N61 1.588(5) . ? B2 H102 0.84(2) . ? Li1 N32 2.016(7) . ? Li1 N22 2.065(7) 2_574 ? Li1 N12 2.071(6) 4_464 ? Li1 O1 2.096(7) . ? Li2 N42 1.944(7) 3_455 ? Li2 N52 2.019(8) 2_565 ? Li2 N62 2.034(8) . ? N1 C1 1.346(9) . ? N1 C3 1.376(6) . ? N1 C2 1.510(9) . ? O1 C3 1.206(6) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 H3 0.9300 . ? N11 C11 1.354(4) . ? N11 C12 1.407(5) . ? N12 C11 1.344(5) . ? N12 C13 1.427(5) . ? N12 Li1 2.071(6) 4_565 ? C11 C14 1.451(6) . ? C12 C13 1.341(5) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? N21 C21 1.358(5) . ? N21 C22 1.400(5) . ? N22 C21 1.322(6) . ? N22 C23 1.362(5) . ? N22 Li1 2.065(7) 2_575 ? C21 C24 1.513(6) . ? C22 C23 1.355(6) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? N31 C31 1.348(5) . ? N31 C32 1.403(4) . ? N32 C31 1.313(4) . ? N32 C33 1.337(6) . ? C31 C34 1.476(5) . ? C32 C33 1.345(6) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? N41 C41 1.339(5) . ? N41 C42 1.433(4) . ? N42 C41 1.337(4) . ? N42 C43 1.403(5) . ? N42 Li2 1.944(7) 3_545 ? C41 C44 1.492(6) . ? C42 C43 1.341(5) . ? C42 H42 0.9300 . ? C43 H43 0.9300 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? N51 C51 1.300(4) . ? N51 C52 1.402(5) . ? N52 C51 1.287(6) . ? N52 C53 1.368(5) . ? N52 Li2 2.019(8) 2_564 ? C51 C54 1.565(6) . ? C52 C53 1.371(6) . ? C52 H52 0.9300 . ? C53 H53 0.9300 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? N61 C61 1.346(5) . ? N61 C62 1.378(5) . ? N62 C61 1.323(5) . ? N62 C63 1.369(6) . ? C61 C64 1.509(6) . ? C62 C63 1.322(6) . ? C62 H62 0.9300 . ? C63 H63 0.9300 . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N31 B1 N11 109.1(3) . . ? N31 B1 N21 111.3(3) . . ? N11 B1 N21 110.3(3) . . ? N31 B1 H101 112.5(12) . . ? N11 B1 H101 106.9(11) . . ? N21 B1 H101 106.6(13) . . ? N41 B2 N51 110.0(3) . . ? N41 B2 N61 108.6(3) . . ? N51 B2 N61 108.5(3) . . ? N41 B2 H102 118.5(15) . . ? N51 B2 H102 107.8(17) . . ? N61 B2 H102 102.8(18) . . ? N32 Li1 N22 110.1(3) . 2_574 ? N32 Li1 N12 115.3(3) . 4_464 ? N22 Li1 N12 111.1(3) 2_574 4_464 ? N32 Li1 O1 104.5(3) . . ? N22 Li1 O1 110.0(3) 2_574 . ? N12 Li1 O1 105.3(3) 4_464 . ? N42 Li2 N52 119.1(4) 3_455 2_565 ? N42 Li2 N62 121.5(4) 3_455 . ? N52 Li2 N62 118.9(3) 2_565 . ? C1 N1 C3 125.0(5) . . ? C1 N1 C2 120.6(5) . . ? C3 N1 C2 114.4(6) . . ? C3 O1 Li1 120.2(4) . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? O1 C3 N1 123.0(6) . . ? O1 C3 H3 118.5 . . ? N1 C3 H3 118.5 . . ? C11 N11 C12 105.0(3) . . ? C11 N11 B1 127.5(3) . . ? C12 N11 B1 127.4(3) . . ? C11 N12 C13 105.7(3) . . ? C11 N12 Li1 129.2(3) . 4_565 ? C13 N12 Li1 123.8(3) . 4_565 ? N12 C11 N11 112.2(3) . . ? N12 C11 C14 123.0(3) . . ? N11 C11 C14 124.8(4) . . ? C13 C12 N11 109.6(3) . . ? C13 C12 H12 125.2 . . ? N11 C12 H12 125.2 . . ? C12 C13 N12 107.4(3) . . ? C12 C13 H13 126.3 . . ? N12 C13 H13 126.3 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C21 N21 C22 104.5(3) . . ? C21 N21 B1 127.9(3) . . ? C22 N21 B1 127.6(3) . . ? C21 N22 C23 103.6(3) . . ? C21 N22 Li1 130.9(3) . 2_575 ? C23 N22 Li1 123.8(3) . 2_575 ? N22 C21 N21 114.1(3) . . ? N22 C21 C24 122.4(3) . . ? N21 C21 C24 123.5(4) . . ? C23 C22 N21 105.8(3) . . ? C23 C22 H22 127.1 . . ? N21 C22 H22 127.1 . . ? C22 C23 N22 112.0(4) . . ? C22 C23 H23 124.0 . . ? N22 C23 H23 124.0 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C31 N31 C32 104.8(3) . . ? C31 N31 B1 128.6(3) . . ? C32 N31 B1 126.5(3) . . ? C31 N32 C33 102.9(3) . . ? C31 N32 Li1 132.0(3) . . ? C33 N32 Li1 125.0(3) . . ? N32 C31 N31 114.2(3) . . ? N32 C31 C34 121.8(4) . . ? N31 C31 C34 123.8(3) . . ? C33 C32 N31 104.0(4) . . ? C33 C32 H32 128.0 . . ? N31 C32 H32 128.0 . . ? N32 C33 C32 114.1(3) . . ? N32 C33 H33 123.0 . . ? C32 C33 H33 123.0 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C41 N41 C42 104.4(3) . . ? C41 N41 B2 127.7(3) . . ? C42 N41 B2 127.5(3) . . ? C41 N42 C43 104.5(3) . . ? C41 N42 Li2 133.3(3) . 3_545 ? C43 N42 Li2 121.9(3) . 3_545 ? N41 C41 N42 114.0(3) . . ? N41 C41 C44 121.2(3) . . ? N42 C41 C44 124.6(4) . . ? C43 C42 N41 107.5(3) . . ? C43 C42 H42 126.3 . . ? N41 C42 H42 126.3 . . ? C42 C43 N42 109.7(3) . . ? C42 C43 H43 125.2 . . ? N42 C43 H43 125.2 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C51 N51 C52 104.1(3) . . ? C51 N51 B2 129.8(3) . . ? C52 N51 B2 126.1(3) . . ? C51 N52 C53 104.3(3) . . ? C51 N52 Li2 136.7(4) . 2_564 ? C53 N52 Li2 118.2(4) . 2_564 ? N52 C51 N51 116.7(4) . . ? N52 C51 C54 121.3(3) . . ? N51 C51 C54 121.6(4) . . ? C53 C52 N51 105.9(3) . . ? C53 C52 H52 127.1 . . ? N51 C52 H52 127.1 . . ? N52 C53 C52 109.0(4) . . ? N52 C53 H53 125.5 . . ? C52 C53 H53 125.5 . . ? C51 C54 H54A 109.5 . . ? C51 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C51 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C61 N61 C62 105.8(3) . . ? C61 N61 B2 129.1(3) . . ? C62 N61 B2 125.1(3) . . ? C61 N62 C63 104.6(4) . . ? C61 N62 Li2 137.9(4) . . ? C63 N62 Li2 117.5(3) . . ? N62 C61 N61 111.9(4) . . ? N62 C61 C64 127.4(4) . . ? N61 C61 C64 120.8(4) . . ? C63 C62 N61 106.9(4) . . ? C63 C62 H62 126.5 . . ? N61 C62 H62 126.5 . . ? C62 C63 N62 110.9(4) . . ? C62 C63 H63 124.6 . . ? N62 C63 H63 124.6 . . ? C61 C64 H64A 109.5 . . ? C61 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C61 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 22.49 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.414 _refine_diff_density_min -0.291 _refine_diff_density_rms 0.083 ================================================== data_BIF-11 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H28 B Li N8' _chemical_formula_weight 398.25 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' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M P-43n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y+1/2, x+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' 'x+1/2, z+1/2, y+1/2' '-x+1/2, z+1/2, -y+1/2' '-x+1/2, -z+1/2, y+1/2' 'x+1/2, -z+1/2, -y+1/2' 'z+1/2, y+1/2, x+1/2' 'z+1/2, -y+1/2, -x+1/2' '-z+1/2, y+1/2, -x+1/2' '-z+1/2, -y+1/2, x+1/2' _cell_length_a 16.31380(10) _cell_length_b 16.31380(10) _cell_length_c 16.31380(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4341.76(5) _cell_formula_units_Z 6 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.914 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1272 _exptl_absorpt_coefficient_mu 0.057 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30236 _diffrn_reflns_av_R_equivalents 0.0318 _diffrn_reflns_av_sigmaI/netI 0.0173 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 30.91 _reflns_number_total 2128 _reflns_number_gt 1925 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1481P)^2^+2.4931P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0(4) _refine_ls_number_reflns 2128 _refine_ls_number_parameters 70 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0752 _refine_ls_R_factor_gt 0.0691 _refine_ls_wR_factor_ref 0.2121 _refine_ls_wR_factor_gt 0.2063 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _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 Li1 Li 0.7500 0.5000 0.0000 0.0190(13) Uani 1 4 d S . . B1 B 0.5000 0.2500 0.0000 0.0127(7) Uani 1 4 d S . . N1 N 0.56931(10) 0.30674(10) 0.03208(10) 0.0139(3) Uani 1 1 d . . . N2 N 0.66309(10) 0.40727(10) 0.04062(10) 0.0170(4) Uani 1 1 d . . . C1 C 0.60828(11) 0.36999(11) -0.00710(11) 0.0152(4) Uani 1 1 d . . . C2 C 0.65718(13) 0.36827(12) 0.11595(12) 0.0192(4) Uani 1 1 d . . . C3 C 0.60031(12) 0.30744(12) 0.11120(12) 0.0171(4) Uani 1 1 d . . . H3 H 0.5846 0.2718 0.1545 0.021 Uiso 1 1 calc R . . C4 C 0.58817(15) 0.39848(13) -0.09212(13) 0.0229(4) Uani 1 1 d . . . H4A H 0.5372 0.4302 -0.0911 0.034 Uiso 1 1 calc R . . H4B H 0.5814 0.3509 -0.1281 0.034 Uiso 1 1 calc R . . H4C H 0.6328 0.4330 -0.1128 0.034 Uiso 1 1 calc R . . C5 C 0.70702(17) 0.39252(17) 0.18839(15) 0.0353(6) Uani 1 1 d . . . H5A H 0.6800 0.3735 0.2386 0.053 Uiso 1 1 calc R . . H5B H 0.7123 0.4523 0.1899 0.053 Uiso 1 1 calc R . . H5C H 0.7616 0.3677 0.1844 0.053 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 Li1 0.021(3) 0.0178(19) 0.0178(19) 0.000 0.000 0.000 B1 0.0130(10) 0.0120(16) 0.0130(10) 0.000 0.000 0.000 N1 0.0154(7) 0.0125(7) 0.0137(7) 0.0005(5) -0.0005(5) -0.0013(5) N2 0.0175(8) 0.0171(8) 0.0163(7) 0.0010(6) -0.0015(6) -0.0028(6) C1 0.0175(8) 0.0141(8) 0.0140(8) 0.0005(6) 0.0009(6) -0.0016(6) C2 0.0198(9) 0.0209(9) 0.0170(9) 0.0028(7) -0.0043(7) -0.0047(7) C3 0.0187(9) 0.0180(9) 0.0147(8) 0.0036(6) -0.0035(6) -0.0026(7) C4 0.0313(11) 0.0213(9) 0.0161(8) 0.0035(7) -0.0038(8) -0.0065(8) C5 0.0395(14) 0.0432(15) 0.0233(11) 0.0079(10) -0.0152(10) -0.0219(11) _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 Li1 N2 2.1767(16) 19_654 ? Li1 N2 2.1767(16) 18_655 ? Li1 N2 2.1767(16) 4_565 ? Li1 N2 2.1767(16) . ? B1 N1 1.5522(16) 22 ? B1 N1 1.5522(16) . ? B1 N1 1.5522(16) 3_655 ? B1 N1 1.5522(16) 24_554 ? N1 C1 1.370(2) . ? N1 C3 1.386(2) . ? N2 C1 1.332(2) . ? N2 C2 1.387(2) . ? C1 C4 1.499(3) . ? C2 C3 1.361(3) . ? C2 C5 1.488(3) . ? C3 H3 0.9500 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Li1 N2 98.71(9) 19_654 18_655 ? N2 Li1 N2 115.11(5) 19_654 4_565 ? N2 Li1 N2 115.11(5) 18_655 4_565 ? N2 Li1 N2 115.11(5) 19_654 . ? N2 Li1 N2 115.11(5) 18_655 . ? N2 Li1 N2 98.71(9) 4_565 . ? N1 B1 N1 110.83(6) 22 . ? N1 B1 N1 110.83(6) 22 3_655 ? N1 B1 N1 106.78(12) . 3_655 ? N1 B1 N1 106.78(12) 22 24_554 ? N1 B1 N1 110.83(6) . 24_554 ? N1 B1 N1 110.83(6) 3_655 24_554 ? C1 N1 C3 105.00(16) . . ? C1 N1 B1 129.04(14) . . ? C3 N1 B1 125.77(14) . . ? C1 N2 C2 105.16(16) . . ? C1 N2 Li1 125.20(13) . . ? C2 N2 Li1 129.33(13) . . ? N2 C1 N1 112.49(16) . . ? N2 C1 C4 123.08(17) . . ? N1 C1 C4 124.30(17) . . ? C3 C2 N2 109.36(16) . . ? C3 C2 C5 127.71(18) . . ? N2 C2 C5 122.93(18) . . ? C2 C3 N1 107.92(16) . . ? C2 C3 H3 126.0 . . ? N1 C3 H3 126.0 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 30.91 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 1.087 _refine_diff_density_min -0.384 _refine_diff_density_rms 0.191 ========================================================= data_BIF-12 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H31 B Li N9 O' _chemical_formula_weight 575.41 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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.4369(3) _cell_length_b 13.4869(3) _cell_length_c 17.8943(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.7090(10) _cell_angle_gamma 90.00 _cell_volume 3001.27(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.273 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1208 _exptl_absorpt_coefficient_mu 0.081 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15140 _diffrn_reflns_av_R_equivalents 0.0307 _diffrn_reflns_av_sigmaI/netI 0.0540 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 25.06 _reflns_number_total 4820 _reflns_number_gt 2935 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0809P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0058(10) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4820 _refine_ls_number_parameters 403 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1006 _refine_ls_R_factor_gt 0.0548 _refine_ls_wR_factor_ref 0.1596 _refine_ls_wR_factor_gt 0.1356 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _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 -0.2216(2) 0.8669(2) 0.87822(16) 0.0365(8) Uani 1 1 d . . . C1 C -0.2479(3) 1.1601(2) 1.12997(17) 0.0672(9) Uani 1 1 d . . . H1A H -0.3051 1.1700 1.0934 0.081 Uiso 1 1 calc R . . H1B H -0.1829 1.1444 1.1030 0.081 Uiso 1 1 calc R . . C2 C -0.2307(4) 1.2546(3) 1.1716(2) 0.0992(13) Uani 1 1 d . . . H2 H -0.2024 1.3006 1.1344 0.119 Uiso 1 1 calc R . . C3 C -0.3241(4) 1.3013(3) 1.1982(3) 0.1238(16) Uani 1 1 d . . . H3A H -0.3012 1.3532 1.2324 0.149 Uiso 1 1 calc R . . H3B H -0.3630 1.2528 1.2274 0.149 Uiso 1 1 calc R . . C4 C -0.4021(3) 1.3463(3) 1.1441(3) 0.1341(18) Uani 1 1 d . . . H4A H -0.3676 1.3990 1.1175 0.201 Uiso 1 1 calc R . . H4B H -0.4625 1.3722 1.1707 0.201 Uiso 1 1 calc R . . H4C H -0.4264 1.2967 1.1094 0.201 Uiso 1 1 calc R . . O1 O -0.27482(19) 1.07837(15) 1.17572(12) 0.0566(6) Uani 1 1 d . . . H101 H -0.340(3) 1.070(2) 1.1752(18) 0.082(13) Uiso 1 1 d . . . N11 N -0.18362(16) 0.86362(14) 0.96059(11) 0.0371(6) Uani 1 1 d . . . N12 N -0.17801(18) 0.89217(16) 1.08536(11) 0.0459(6) Uani 1 1 d . . . C11 C -0.2264(2) 0.90948(19) 1.02114(15) 0.0422(7) Uani 1 1 d . . . H11 H -0.2862 0.9506 1.0172 0.051 Uiso 1 1 calc R . . C12 C -0.0952(2) 0.82764(19) 1.06708(14) 0.0394(7) Uani 1 1 d . . . C13 C -0.0164(2) 0.7849(2) 1.11310(15) 0.0494(8) Uani 1 1 d . . . H13 H -0.0145 0.7970 1.1643 0.059 Uiso 1 1 calc R . . C14 C 0.0577(2) 0.7247(2) 1.08036(17) 0.0537(8) Uani 1 1 d . . . H14 H 0.1106 0.6952 1.1100 0.064 Uiso 1 1 calc R . . C15 C 0.0562(2) 0.7064(2) 1.00392(16) 0.0536(8) Uani 1 1 d . . . H15 H 0.1084 0.6655 0.9836 0.064 Uiso 1 1 calc R . . C16 C -0.0214(2) 0.74759(19) 0.95760(15) 0.0480(8) Uani 1 1 d . . . H16 H -0.0227 0.7349 0.9065 0.058 Uiso 1 1 calc R . . C17 C -0.0973(2) 0.80882(19) 0.99038(14) 0.0386(7) Uani 1 1 d . . . N21 N -0.23425(16) 0.75826(15) 0.85057(11) 0.0359(5) Uani 1 1 d . . . N22 N -0.21903(18) 0.62252(16) 0.77696(12) 0.0434(6) Uani 1 1 d . . . C21 C -0.1968(2) 0.7162(2) 0.78645(14) 0.0397(7) Uani 1 1 d . . . H21 H -0.1578 0.7522 0.7517 0.048 Uiso 1 1 calc R . . C22 C -0.2853(2) 0.67995(19) 0.88686(14) 0.0359(7) Uani 1 1 d . . . C23 C -0.3381(2) 0.6743(2) 0.95449(15) 0.0483(8) Uani 1 1 d . . . H23 H -0.3462 0.7296 0.9850 0.058 Uiso 1 1 calc R . . C24 C -0.3781(2) 0.5829(2) 0.97435(16) 0.0533(8) Uani 1 1 d . . . H24 H -0.4145 0.5767 1.0192 0.064 Uiso 1 1 calc R . . C25 C -0.3658(2) 0.4997(2) 0.92973(18) 0.0565(8) Uani 1 1 d . . . H25 H -0.3924 0.4390 0.9458 0.068 Uiso 1 1 calc R . . C26 C -0.3154(2) 0.5053(2) 0.86270(17) 0.0524(8) Uani 1 1 d . . . H26 H -0.3080 0.4497 0.8324 0.063 Uiso 1 1 calc R . . C27 C -0.2756(2) 0.59661(19) 0.84127(14) 0.0389(7) Uani 1 1 d . . . N31 N -0.13694(17) 0.92164(14) 0.83139(10) 0.0372(6) Uani 1 1 d . . . N32 N 0.02314(17) 0.98985(15) 0.80035(12) 0.0410(6) Uani 1 1 d . . . C31 C -0.0374(2) 0.95357(18) 0.85308(15) 0.0397(7) Uani 1 1 d . . . H31 H -0.0138 0.9498 0.9025 0.048 Uiso 1 1 calc R . . C32 C -0.0413(2) 0.98154(17) 0.73604(14) 0.0384(7) Uani 1 1 d . . . C33 C -0.0177(2) 1.00409(18) 0.66229(15) 0.0496(8) Uani 1 1 d . . . H33 H 0.0483 1.0314 0.6496 0.059 Uiso 1 1 calc R . . C34 C -0.0946(3) 0.9849(2) 0.60888(16) 0.0618(9) Uani 1 1 d . . . H34 H -0.0800 0.9978 0.5590 0.074 Uiso 1 1 calc R . . C35 C -0.1938(3) 0.9465(2) 0.62794(17) 0.0657(10) Uani 1 1 d . . . H35 H -0.2444 0.9346 0.5903 0.079 Uiso 1 1 calc R . . C36 C -0.2201(2) 0.9254(2) 0.70019(16) 0.0565(9) Uani 1 1 d . . . H36 H -0.2878 0.9017 0.7125 0.068 Uiso 1 1 calc R . . C37 C -0.1406(2) 0.94117(18) 0.75449(14) 0.0390(7) Uani 1 1 d . . . N41 N -0.33027(16) 0.92034(15) 0.87046(11) 0.0399(6) Uani 1 1 d . . . N42 N -0.50575(19) 0.94269(19) 0.84085(14) 0.0613(7) Uani 1 1 d . . . C41 C -0.4253(2) 0.8809(2) 0.84614(15) 0.0502(8) Uani 1 1 d . . . H41 H -0.4323 0.8141 0.8341 0.060 Uiso 1 1 calc R . . C42 C -0.3537(2) 1.0208(2) 0.88135(14) 0.0443(7) Uani 1 1 d . . . C43 C -0.2909(2) 1.1007(2) 0.90592(15) 0.0557(8) Uani 1 1 d . . . H43 H -0.2182 1.0934 0.9174 0.067 Uiso 1 1 calc R . . C44 C -0.3422(3) 1.1910(2) 0.91229(18) 0.0711(10) Uani 1 1 d . . . H44 H -0.3032 1.2457 0.9290 0.085 Uiso 1 1 calc R . . C45 C -0.4500(3) 1.2024(3) 0.8946(2) 0.0756(10) Uani 1 1 d . . . H45 H -0.4812 1.2647 0.8996 0.091 Uiso 1 1 calc R . . C46 C -0.5121(3) 1.1257(2) 0.87005(18) 0.0692(9) Uani 1 1 d . . . H46 H -0.5845 1.1343 0.8582 0.083 Uiso 1 1 calc R . . C47 C -0.4625(2) 1.0339(2) 0.86362(15) 0.0513(8) Uani 1 1 d . . . Li1 Li -0.1802(3) 0.9651(3) 1.1872(2) 0.0435(11) Uani 1 1 d . . . N1 N -0.1442(3) 1.2437(2) 1.22616(19) 0.1318(14) Uani 1 1 d . . . H1C H -0.1415 1.2974 1.2550 0.198 Uiso 1 1 d R . . H1D H -0.0825 1.2374 1.2019 0.198 Uiso 1 1 d 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 0.0297(18) 0.0437(19) 0.0362(17) -0.0019(14) 0.0006(15) -0.0038(15) C1 0.071(2) 0.060(2) 0.071(2) 0.0023(18) -0.0018(19) 0.0024(18) C2 0.091(3) 0.081(3) 0.125(3) -0.024(2) -0.028(3) 0.017(2) C3 0.116(4) 0.125(4) 0.131(4) -0.039(3) -0.004(3) 0.017(3) C4 0.086(3) 0.111(3) 0.204(5) 0.045(3) -0.051(3) 0.004(3) O1 0.0363(13) 0.0591(15) 0.0743(15) 0.0111(11) 0.0004(12) 0.0011(11) N11 0.0304(13) 0.0469(13) 0.0341(12) -0.0060(10) 0.0027(11) 0.0007(11) N12 0.0418(14) 0.0600(16) 0.0360(13) -0.0041(11) 0.0013(12) 0.0046(12) C11 0.0342(16) 0.0491(17) 0.0433(17) -0.0060(13) 0.0032(15) 0.0021(13) C12 0.0353(16) 0.0446(17) 0.0382(16) -0.0027(12) 0.0000(14) -0.0031(14) C13 0.0491(19) 0.0565(19) 0.0425(17) 0.0025(14) -0.0015(16) -0.0027(16) C14 0.0479(19) 0.0531(19) 0.060(2) 0.0067(15) -0.0042(17) 0.0024(16) C15 0.0482(19) 0.0542(19) 0.058(2) -0.0003(15) 0.0034(17) 0.0100(15) C16 0.0454(18) 0.0515(18) 0.0471(17) -0.0054(14) 0.0010(16) 0.0009(16) C17 0.0322(16) 0.0422(16) 0.0416(16) -0.0026(13) 0.0028(14) -0.0029(14) N21 0.0339(13) 0.0427(14) 0.0311(12) -0.0023(10) 0.0036(11) -0.0030(11) N22 0.0478(15) 0.0396(14) 0.0430(14) -0.0029(11) 0.0063(12) -0.0006(12) C21 0.0390(17) 0.0447(18) 0.0356(16) 0.0016(13) 0.0041(14) 0.0000(14) C22 0.0285(15) 0.0469(17) 0.0325(15) 0.0006(13) 0.0003(13) -0.0016(13) C23 0.0432(18) 0.065(2) 0.0370(17) -0.0035(14) 0.0037(15) -0.0064(16) C24 0.0430(19) 0.074(2) 0.0428(17) 0.0103(17) 0.0080(15) -0.0114(17) C25 0.054(2) 0.051(2) 0.064(2) 0.0117(17) 0.0082(19) -0.0073(16) C26 0.056(2) 0.0432(19) 0.059(2) 0.0016(15) 0.0100(18) -0.0027(15) C27 0.0362(16) 0.0437(18) 0.0368(16) 0.0037(13) 0.0035(14) -0.0011(14) N31 0.0335(13) 0.0446(13) 0.0335(12) 0.0019(10) -0.0009(11) -0.0044(11) N32 0.0346(13) 0.0482(14) 0.0401(13) 0.0015(11) 0.0003(12) -0.0055(11) C31 0.0320(16) 0.0465(17) 0.0406(16) -0.0024(13) -0.0036(15) -0.0024(14) C32 0.0393(17) 0.0376(16) 0.0382(16) 0.0032(12) 0.0014(14) -0.0024(13) C33 0.053(2) 0.0481(18) 0.0474(18) 0.0060(13) 0.0016(17) -0.0047(15) C34 0.081(3) 0.061(2) 0.0428(18) 0.0084(15) -0.004(2) -0.0007(19) C35 0.076(3) 0.074(2) 0.046(2) 0.0090(16) -0.0234(19) -0.009(2) C36 0.0494(19) 0.067(2) 0.0524(19) 0.0091(15) -0.0157(17) -0.0111(16) C37 0.0388(17) 0.0386(16) 0.0396(16) 0.0043(12) -0.0030(14) -0.0027(13) N41 0.0312(13) 0.0400(14) 0.0483(14) -0.0033(10) -0.0021(11) -0.0037(11) N42 0.0337(15) 0.0623(17) 0.0876(19) -0.0029(14) -0.0066(14) 0.0016(13) C41 0.0335(17) 0.0513(19) 0.066(2) -0.0022(15) -0.0061(16) -0.0033(15) C42 0.0393(18) 0.0457(18) 0.0480(17) -0.0019(13) 0.0015(15) -0.0001(15) C43 0.0448(19) 0.055(2) 0.068(2) -0.0079(15) -0.0005(17) -0.0027(16) C44 0.070(3) 0.046(2) 0.097(3) -0.0120(17) 0.001(2) -0.0005(19) C45 0.062(2) 0.054(2) 0.111(3) -0.0067(19) 0.014(2) 0.015(2) C46 0.044(2) 0.062(2) 0.102(3) 0.0008(19) 0.0027(19) 0.0089(18) C47 0.0351(17) 0.054(2) 0.065(2) 0.0000(15) 0.0022(16) 0.0002(16) Li1 0.041(3) 0.048(3) 0.042(3) 0.002(2) 0.000(2) -0.004(2) N1 0.110(3) 0.131(3) 0.153(3) -0.039(2) -0.075(3) 0.006(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 N41 1.536(3) . ? B1 N31 1.543(4) . ? B1 N11 1.543(3) . ? B1 N21 1.553(3) . ? C1 O1 1.416(3) . ? C1 C2 1.490(4) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.409(5) . ? C2 N1 1.451(4) . ? C2 H2 0.9800 . ? C3 C4 1.491(5) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? O1 Li1 1.937(5) . ? O1 H101 0.82(3) . ? N11 C11 1.361(3) . ? N11 C17 1.403(3) . ? N12 C11 1.311(3) . ? N12 C12 1.391(3) . ? N12 Li1 2.072(5) . ? C11 H11 0.9300 . ? C12 C17 1.396(3) . ? C12 C13 1.396(3) . ? C13 C14 1.365(4) . ? C13 H13 0.9300 . ? C14 C15 1.390(4) . ? C14 H14 0.9300 . ? C15 C16 1.380(3) . ? C15 H15 0.9300 . ? C16 C17 1.389(3) . ? C16 H16 0.9300 . ? N21 C21 1.367(3) . ? N21 C22 1.396(3) . ? N22 C21 1.304(3) . ? N22 C27 1.400(3) . ? N22 Li1 2.056(5) 4_575 ? C21 H21 0.9300 . ? C22 C23 1.386(3) . ? C22 C27 1.395(3) . ? C23 C24 1.378(4) . ? C23 H23 0.9300 . ? C24 C25 1.386(4) . ? C24 H24 0.9300 . ? C25 C26 1.362(4) . ? C25 H25 0.9300 . ? C26 C27 1.384(3) . ? C26 H26 0.9300 . ? N31 C31 1.363(3) . ? N31 C37 1.401(3) . ? N32 C31 1.309(3) . ? N32 C32 1.399(3) . ? N32 Li1 2.055(5) 3_577 ? C31 H31 0.9300 . ? C32 C33 1.389(3) . ? C32 C37 1.392(3) . ? C33 C34 1.368(4) . ? C33 H33 0.9300 . ? C34 C35 1.385(4) . ? C34 H34 0.9300 . ? C35 C36 1.367(4) . ? C35 H35 0.9300 . ? C36 C37 1.394(3) . ? C36 H36 0.9300 . ? N41 C41 1.362(3) . ? N41 C42 1.400(3) . ? N42 C41 1.305(3) . ? N42 C47 1.401(3) . ? C41 H41 0.9300 . ? C42 C47 1.397(4) . ? C42 C43 1.398(4) . ? C43 C44 1.380(4) . ? C43 H43 0.9300 . ? C44 C45 1.382(4) . ? C44 H44 0.9300 . ? C45 C46 1.361(4) . ? C45 H45 0.9300 . ? C46 C47 1.388(4) . ? C46 H46 0.9300 . ? Li1 N32 2.055(5) 3_577 ? Li1 N22 2.056(5) 4_576 ? N1 H1C 0.8900 . ? N1 H1D 0.8899 . ? 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 N41 B1 N31 109.4(2) . . ? N41 B1 N11 111.0(2) . . ? N31 B1 N11 109.2(2) . . ? N41 B1 N21 109.2(2) . . ? N31 B1 N21 110.2(2) . . ? N11 B1 N21 107.8(2) . . ? O1 C1 C2 114.2(3) . . ? O1 C1 H1A 108.7 . . ? C2 C1 H1A 108.7 . . ? O1 C1 H1B 108.7 . . ? C2 C1 H1B 108.7 . . ? H1A C1 H1B 107.6 . . ? C3 C2 N1 115.2(4) . . ? C3 C2 C1 115.9(4) . . ? N1 C2 C1 110.5(3) . . ? C3 C2 H2 104.6 . . ? N1 C2 H2 104.6 . . ? C1 C2 H2 104.6 . . ? C2 C3 C4 119.7(4) . . ? C2 C3 H3A 107.4 . . ? C4 C3 H3A 107.4 . . ? C2 C3 H3B 107.4 . . ? C4 C3 H3B 107.4 . . ? H3A C3 H3B 106.9 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C1 O1 Li1 121.9(2) . . ? C1 O1 H101 110(2) . . ? Li1 O1 H101 120(2) . . ? C11 N11 C17 104.0(2) . . ? C11 N11 B1 129.0(2) . . ? C17 N11 B1 127.0(2) . . ? C11 N12 C12 103.8(2) . . ? C11 N12 Li1 132.5(2) . . ? C12 N12 Li1 121.5(2) . . ? N12 C11 N11 115.9(2) . . ? N12 C11 H11 122.0 . . ? N11 C11 H11 122.0 . . ? N12 C12 C17 109.9(2) . . ? N12 C12 C13 129.5(2) . . ? C17 C12 C13 120.6(3) . . ? C14 C13 C12 117.7(3) . . ? C14 C13 H13 121.2 . . ? C12 C13 H13 121.2 . . ? C13 C14 C15 121.8(3) . . ? C13 C14 H14 119.1 . . ? C15 C14 H14 119.1 . . ? C16 C15 C14 121.3(3) . . ? C16 C15 H15 119.3 . . ? C14 C15 H15 119.3 . . ? C15 C16 C17 117.3(3) . . ? C15 C16 H16 121.3 . . ? C17 C16 H16 121.3 . . ? C16 C17 C12 121.2(2) . . ? C16 C17 N11 132.3(2) . . ? C12 C17 N11 106.4(2) . . ? C21 N21 C22 103.8(2) . . ? C21 N21 B1 128.7(2) . . ? C22 N21 B1 127.6(2) . . ? C21 N22 C27 104.0(2) . . ? C21 N22 Li1 127.4(2) . 4_575 ? C27 N22 Li1 128.6(2) . 4_575 ? N22 C21 N21 116.0(2) . . ? N22 C21 H21 122.0 . . ? N21 C21 H21 122.0 . . ? C23 C22 C27 120.8(3) . . ? C23 C22 N21 132.1(2) . . ? C27 C22 N21 107.1(2) . . ? C24 C23 C22 116.8(3) . . ? C24 C23 H23 121.6 . . ? C22 C23 H23 121.6 . . ? C23 C24 C25 122.2(3) . . ? C23 C24 H24 118.9 . . ? C25 C24 H24 118.9 . . ? C26 C25 C24 121.2(3) . . ? C26 C25 H25 119.4 . . ? C24 C25 H25 119.4 . . ? C25 C26 C27 117.6(3) . . ? C25 C26 H26 121.2 . . ? C27 C26 H26 121.2 . . ? C26 C27 C22 121.4(3) . . ? C26 C27 N22 129.4(3) . . ? C22 C27 N22 109.1(2) . . ? C31 N31 C37 103.8(2) . . ? C31 N31 B1 128.4(2) . . ? C37 N31 B1 127.6(2) . . ? C31 N32 C32 103.5(2) . . ? C31 N32 Li1 125.9(2) . 3_577 ? C32 N32 Li1 130.3(2) . 3_577 ? N32 C31 N31 116.2(2) . . ? N32 C31 H31 121.9 . . ? N31 C31 H31 121.9 . . ? C33 C32 C37 120.6(2) . . ? C33 C32 N32 129.6(3) . . ? C37 C32 N32 109.7(2) . . ? C34 C33 C32 117.9(3) . . ? C34 C33 H33 121.1 . . ? C32 C33 H33 121.1 . . ? C33 C34 C35 121.1(3) . . ? C33 C34 H34 119.5 . . ? C35 C34 H34 119.5 . . ? C36 C35 C34 122.3(3) . . ? C36 C35 H35 118.8 . . ? C34 C35 H35 118.8 . . ? C35 C36 C37 116.9(3) . . ? C35 C36 H36 121.6 . . ? C37 C36 H36 121.6 . . ? C32 C37 C36 121.2(2) . . ? C32 C37 N31 106.8(2) . . ? C36 C37 N31 132.0(3) . . ? C41 N41 C42 104.0(2) . . ? C41 N41 B1 127.1(2) . . ? C42 N41 B1 128.7(2) . . ? C41 N42 C47 104.4(2) . . ? N42 C41 N41 115.8(3) . . ? N42 C41 H41 122.1 . . ? N41 C41 H41 122.1 . . ? C47 C42 C43 120.6(3) . . ? C47 C42 N41 107.0(2) . . ? C43 C42 N41 132.3(3) . . ? C44 C43 C42 116.7(3) . . ? C44 C43 H43 121.7 . . ? C42 C43 H43 121.7 . . ? C43 C44 C45 121.8(3) . . ? C43 C44 H44 119.1 . . ? C45 C44 H44 119.1 . . ? C46 C45 C44 122.3(3) . . ? C46 C45 H45 118.8 . . ? C44 C45 H45 118.8 . . ? C45 C46 C47 116.9(3) . . ? C45 C46 H46 121.5 . . ? C47 C46 H46 121.5 . . ? C46 C47 C42 121.6(3) . . ? C46 C47 N42 129.6(3) . . ? C42 C47 N42 108.8(3) . . ? O1 Li1 N32 110.7(2) . 3_577 ? O1 Li1 N22 112.8(2) . 4_576 ? N32 Li1 N22 108.5(2) 3_577 4_576 ? O1 Li1 N12 107.2(2) . . ? N32 Li1 N12 102.3(2) 3_577 . ? N22 Li1 N12 114.8(2) 4_576 . ? C2 N1 H1C 109.3 . . ? C2 N1 H1D 108.6 . . ? H1C N1 H1D 109.5 . . ? _diffrn_measured_fraction_theta_max 0.905 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.905 _refine_diff_density_max 0.340 _refine_diff_density_min -0.320 _refine_diff_density_rms 0.045