# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'M Beckett' 'Peter N Horton' 'Mike Hursthouse' 'David A. Knox' 'James L. Timmis' _publ_contact_author_name 'M Beckett' _publ_contact_author_email M.A.BECKETT@BANGOR.AC.UK _publ_section_title ; Structural(XRD) and thermal (DSC, TGA) and BET analysis of materials derived from non-metal- cation pentaborate salts ; # Attachment 'pentaborates.CIF' data_1a #TrackingRef 'pentaborates.CIF' _database_code_depnum_ccdc_archive 'CCDC 764920' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H16 B5 N O11' _chemical_formula_weight 308.23 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 0.0000 '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 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 9.0867(2) _cell_length_b 9.4434(3) _cell_length_c 9.7789(3) _cell_angle_alpha 73.734(2) _cell_angle_beta 74.7480(10) _cell_angle_gamma 62.056(2) _cell_volume 702.96(3) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 3143 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description Slab _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.456 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 320 _exptl_absorpt_coefficient_mu 0.133 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9689 _exptl_absorpt_correction_T_max 0.9921 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2003)' _exptl_special_details ; SADABS was used to perform the Absorption correction Parameter refinement on 12894 reflections reduced R(int) from 0.1000 to 0.0407 Ratio of minimum to maximum apparent transmission: 0.915209 The given Tmin and Tmax were generated using the SHELX SIZE command ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12667 _diffrn_reflns_av_R_equivalents 0.0387 _diffrn_reflns_av_sigmaI/netI 0.0346 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 27.47 _reflns_number_total 3197 _reflns_number_gt 2984 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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^)+(0.0570P)^2^+0.6783P] 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 ? _refine_ls_number_reflns 3197 _refine_ls_number_parameters 395 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0525 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_ref 0.1230 _refine_ls_wR_factor_gt 0.1183 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 0.1769(5) 0.8618(5) 0.6585(4) 0.0143(8) Uani 1 1 d . . . B2 B 0.3937(5) 0.5749(5) 0.6474(5) 0.0176(8) Uani 1 1 d . . . B3 B 0.3913(5) 0.7801(5) 0.4403(5) 0.0173(8) Uani 1 1 d . . . B4 B -0.1215(5) 1.0584(5) 0.6773(4) 0.0150(8) Uani 1 1 d . . . B5 B 0.0641(5) 1.0946(5) 0.7827(5) 0.0164(8) Uani 1 1 d . . . O1 O 0.2591(3) 0.6859(3) 0.7188(3) 0.0145(5) Uani 1 1 d . . . O2 O 0.4647(4) 0.6200(3) 0.5085(3) 0.0220(6) Uani 1 1 d . . . O3 O 0.2640(3) 0.8956(3) 0.5105(3) 0.0163(5) Uani 1 1 d . . . O4 O 0.0014(3) 0.9099(3) 0.6532(3) 0.0161(5) Uani 1 1 d . . . O5 O -0.0885(3) 1.1567(3) 0.7362(3) 0.0183(6) Uani 1 1 d . . . O6 O 0.1940(3) 0.9527(3) 0.7496(3) 0.0164(5) Uani 1 1 d . . . O7 O 0.4670(3) 0.4142(3) 0.7083(3) 0.0213(6) Uani 1 1 d . . . H7 H 0.4122 0.3978 0.7901 0.032 Uiso 1 1 calc R . . O8 O 0.4561(4) 0.8164(3) 0.2990(3) 0.0223(6) Uani 1 1 d . . . H8 H 0.4032 0.9162 0.2673 0.034 Uiso 1 1 calc R . . O9 O -0.2771(3) 1.1098(3) 0.6458(3) 0.0213(6) Uani 1 1 d . . . H9 H -0.3419 1.1990 0.6729 0.032 Uiso 1 1 calc R . . O10 O 0.0762(3) 1.1832(3) 0.8641(3) 0.0230(6) Uani 1 1 d . . . H10 H 0.1769 1.1457 0.8760 0.034 Uiso 1 1 calc R . . B11 B 0.3953(5) 0.1698(5) 0.0368(4) 0.0128(8) Uani 1 1 d . . . B12 B 0.6956(5) -0.0310(5) 0.0144(4) 0.0146(8) Uani 1 1 d . . . B13 B 0.5048(5) -0.0640(5) -0.0871(5) 0.0170(8) Uani 1 1 d . . . B14 B 0.1925(5) 0.4581(5) 0.0552(4) 0.0148(8) Uani 1 1 d . . . B15 B 0.1988(5) 0.2502(5) 0.2623(5) 0.0159(8) Uani 1 1 d . . . O11 O 0.5739(3) 0.1189(3) 0.0389(3) 0.0155(5) Uani 1 1 d . . . O12 O 0.6601(3) -0.1274(3) -0.0437(3) 0.0180(5) Uani 1 1 d . . . O13 O 0.3779(3) 0.0783(3) -0.0531(3) 0.0142(5) Uani 1 1 d . . . O14 O 0.3163(3) 0.3440(3) -0.0223(3) 0.0145(5) Uani 1 1 d . . . O15 O 0.1380(3) 0.4140(3) 0.1986(3) 0.0184(5) Uani 1 1 d . . . O16 O 0.3132(3) 0.1333(3) 0.1855(3) 0.0149(5) Uani 1 1 d . . . O17 O 0.8507(3) -0.0793(3) 0.0452(3) 0.0218(6) Uani 1 1 d . . . H17 H 0.9098 -0.1776 0.0380 0.033 Uiso 1 1 calc R . . O18 O 0.4855(3) -0.1552(3) -0.1614(3) 0.0241(6) Uani 1 1 d . . . H18 H 0.3940 -0.1013 -0.1942 0.036 Uiso 1 1 calc R . . O19 O 0.1213(3) 0.6181(3) -0.0058(3) 0.0202(6) Uani 1 1 d . . . H19 H 0.1621 0.6304 -0.0936 0.030 Uiso 1 1 calc R . . O20 O 0.1388(4) 0.2155(3) 0.4039(3) 0.0225(6) Uani 1 1 d . . . H20 H 0.1789 0.1140 0.4319 0.034 Uiso 1 1 calc R . . C21 C 0.8787(5) 0.5874(5) 0.6890(4) 0.0235(8) Uani 1 1 d . . . H21A H 0.9743 0.4825 0.7173 0.028 Uiso 1 1 calc R . . H21B H 0.8825 0.6722 0.7270 0.028 Uiso 1 1 calc R . . C22 C 0.8957(5) 0.6312(5) 0.5276(5) 0.0222(8) Uani 1 1 d . . . C23 C 0.7666(6) 0.7991(5) 0.4713(5) 0.0316(10) Uani 1 1 d . . . H23A H 0.6528 0.8076 0.5129 0.047 Uiso 1 1 calc R . . H23B H 0.7805 0.8160 0.3660 0.047 Uiso 1 1 calc R . . H23C H 0.7831 0.8823 0.4986 0.047 Uiso 1 1 calc R . . C24 C 1.0726(6) 0.6137(6) 0.4590(6) 0.0360(11) Uani 1 1 d . . . H24A H 1.0818 0.6353 0.3538 0.054 Uiso 1 1 calc R . . H24B H 1.1546 0.5027 0.4912 0.054 Uiso 1 1 calc R . . H24C H 1.0956 0.6920 0.4877 0.054 Uiso 1 1 calc R . . N21 N 0.8645(4) 0.5058(4) 0.4798(3) 0.0235(7) Uani 1 1 d . . . H21C H 0.7695 0.4981 0.5343 0.035 Uiso 1 1 calc R . . H21D H 0.9541 0.4066 0.4919 0.035 Uiso 1 1 calc R . . H21E H 0.8514 0.5388 0.3853 0.035 Uiso 1 1 calc R . . O21 O 0.7229(3) 0.5738(3) 0.7503(3) 0.0247(6) Uani 1 1 d . . . H21 H 0.6463 0.6657 0.7643 0.037 Uiso 1 1 calc R . . C31 C 0.7833(5) 0.4960(5) 0.1023(4) 0.0200(7) Uani 1 1 d . . . H31A H 0.9058 0.4322 0.0744 0.024 Uiso 1 1 calc R . . H31B H 0.7406 0.5829 0.0191 0.024 Uiso 1 1 calc R . . C32 C 0.6947(5) 0.3849(5) 0.1384(5) 0.0229(8) Uani 1 1 d . . . C33 C 0.5049(6) 0.4754(8) 0.1739(7) 0.0493(16) Uani 1 1 d . . . H33A H 0.4545 0.3977 0.2009 0.074 Uiso 1 1 calc R . . H33B H 0.4607 0.5560 0.0893 0.074 Uiso 1 1 calc R . . H33C H 0.4768 0.5310 0.2544 0.074 Uiso 1 1 calc R . . C34 C 0.7713(10) 0.2372(7) 0.2506(6) 0.0522(17) Uani 1 1 d . . . H34A H 0.8919 0.1784 0.2169 0.078 Uiso 1 1 calc R . . H34B H 0.7156 0.1653 0.2670 0.078 Uiso 1 1 calc R . . H34C H 0.7562 0.2717 0.3410 0.078 Uiso 1 1 calc R . . N31 N 0.7335(4) 0.3219(4) -0.0004(3) 0.0199(6) Uani 1 1 d . . . H31C H 0.8452 0.2542 -0.0169 0.030 Uiso 1 1 calc R . . H31D H 0.7072 0.4076 -0.0754 0.030 Uiso 1 1 calc R . . H31E H 0.6714 0.2664 0.0083 0.030 Uiso 1 1 calc R . . O31 O 0.7568(4) 0.5682(4) 0.2208(3) 0.0262(6) Uani 1 1 d . . . H31 H 0.6612 0.6474 0.2257 0.039 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 0.0164(18) 0.0096(17) 0.014(2) -0.0014(15) -0.0011(15) -0.0043(15) B2 0.0186(19) 0.0126(19) 0.014(2) -0.0016(16) 0.0019(16) -0.0036(16) B3 0.0187(19) 0.0137(19) 0.0140(19) -0.0042(15) -0.0006(15) -0.0025(15) B4 0.0170(19) 0.0126(19) 0.0130(19) -0.0014(15) -0.0003(15) -0.0060(16) B5 0.0163(19) 0.0149(19) 0.0152(19) -0.0047(16) -0.0016(15) -0.0037(16) O1 0.0139(11) 0.0091(12) 0.0139(12) -0.0021(9) -0.0002(9) -0.0006(10) O2 0.0246(14) 0.0109(12) 0.0162(13) -0.0014(10) 0.0074(10) -0.0020(10) O3 0.0181(12) 0.0103(12) 0.0129(12) -0.0024(10) 0.0012(10) -0.0018(10) O4 0.0138(12) 0.0119(12) 0.0207(13) -0.0068(10) -0.0022(10) -0.0021(10) O5 0.0172(13) 0.0113(12) 0.0223(14) -0.0066(11) -0.0063(11) 0.0009(10) O6 0.0160(12) 0.0127(12) 0.0169(12) -0.0048(10) -0.0035(10) -0.0015(10) O7 0.0208(13) 0.0111(12) 0.0167(14) -0.0017(10) 0.0077(11) -0.0005(11) O8 0.0259(15) 0.0110(13) 0.0157(14) -0.0018(10) 0.0051(11) -0.0008(11) O9 0.0161(12) 0.0164(14) 0.0284(16) -0.0101(11) -0.0061(11) 0.0001(11) O10 0.0155(13) 0.0218(14) 0.0299(16) -0.0136(12) -0.0053(11) -0.0007(11) B11 0.0136(18) 0.0085(17) 0.0132(19) -0.0039(15) -0.0009(15) -0.0018(14) B12 0.0130(18) 0.0144(19) 0.0131(19) -0.0032(15) 0.0022(14) -0.0050(15) B13 0.0177(19) 0.0119(19) 0.017(2) -0.0049(16) -0.0028(16) -0.0017(16) B14 0.0142(18) 0.0124(18) 0.016(2) -0.0041(15) -0.0006(15) -0.0040(15) B15 0.0158(18) 0.0124(18) 0.017(2) -0.0026(15) -0.0008(15) -0.0048(15) O11 0.0141(12) 0.0116(12) 0.0200(13) -0.0049(10) -0.0023(10) -0.0040(10) O12 0.0165(12) 0.0145(12) 0.0214(14) -0.0078(10) -0.0043(11) -0.0022(10) O13 0.0135(11) 0.0131(12) 0.0152(12) -0.0067(10) -0.0021(9) -0.0029(10) O14 0.0186(12) 0.0092(12) 0.0106(12) 0.0000(10) -0.0006(10) -0.0036(10) O15 0.0218(13) 0.0111(12) 0.0142(12) -0.0010(10) 0.0017(10) -0.0035(10) O16 0.0179(12) 0.0108(12) 0.0114(12) -0.0008(9) -0.0001(10) -0.0042(10) O17 0.0165(13) 0.0149(13) 0.0330(17) -0.0100(12) -0.0039(11) -0.0027(11) O18 0.0173(13) 0.0191(14) 0.0356(17) -0.0150(12) -0.0117(12) 0.0018(11) O19 0.0228(14) 0.0120(13) 0.0144(13) 0.0012(10) 0.0034(11) -0.0033(11) O20 0.0294(15) 0.0103(12) 0.0147(13) -0.0004(10) 0.0055(11) -0.0036(11) C21 0.0262(18) 0.0202(18) 0.0231(18) -0.0054(14) -0.0065(15) -0.0071(15) C22 0.0250(19) 0.0151(18) 0.028(2) -0.0023(15) -0.0069(15) -0.0088(15) C23 0.043(3) 0.021(2) 0.031(2) -0.0049(17) -0.0156(19) -0.0091(18) C24 0.032(2) 0.044(3) 0.042(3) -0.022(2) 0.0012(19) -0.020(2) N21 0.0251(16) 0.0208(16) 0.0174(15) -0.0065(12) -0.0004(13) -0.0040(13) O21 0.0280(14) 0.0202(12) 0.0219(13) -0.0083(10) 0.0025(11) -0.0078(11) C31 0.0215(17) 0.0212(16) 0.0203(17) -0.0096(14) 0.0006(13) -0.0104(14) C32 0.0214(18) 0.0232(19) 0.0250(19) -0.0058(15) -0.0020(15) -0.0105(15) C33 0.022(2) 0.072(4) 0.075(4) -0.059(3) 0.012(2) -0.021(2) C34 0.109(5) 0.030(3) 0.035(3) 0.010(2) -0.035(3) -0.040(3) N31 0.0217(15) 0.0185(14) 0.0211(15) -0.0081(12) 0.0002(12) -0.0093(12) O31 0.0238(14) 0.0261(14) 0.0243(14) -0.0120(11) -0.0051(11) -0.0023(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 B1 O4 1.450(5) . ? B1 O6 1.477(5) . ? B1 O1 1.478(4) . ? B1 O3 1.483(5) . ? B2 O1 1.357(5) . ? B2 O7 1.363(5) . ? B2 O2 1.384(5) . ? B3 O3 1.348(5) . ? B3 O8 1.367(5) . ? B3 O2 1.378(5) . ? B4 O9 1.354(5) . ? B4 O4 1.359(5) . ? B4 O5 1.391(5) . ? B5 O10 1.361(5) . ? B5 O6 1.361(5) . ? B5 O5 1.376(5) . ? O7 H7 0.8400 . ? O8 H8 0.8400 . ? O9 H9 0.8400 . ? O10 H10 0.8400 . ? B11 O14 1.461(4) . ? B11 O11 1.466(5) . ? B11 O13 1.473(5) . ? B11 O16 1.476(5) . ? B12 O17 1.352(5) . ? B12 O11 1.366(5) . ? B12 O12 1.384(5) . ? B13 O13 1.357(5) . ? B13 O18 1.363(5) . ? B13 O12 1.383(5) . ? B14 O19 1.357(5) . ? B14 O14 1.369(5) . ? B14 O15 1.373(5) . ? B15 O20 1.356(5) . ? B15 O16 1.357(5) . ? B15 O15 1.388(5) . ? O17 H17 0.8400 . ? O18 H18 0.8400 . ? O19 H19 0.8400 . ? O20 H20 0.8400 . ? C21 O21 1.435(5) . ? C21 C22 1.501(6) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.517(6) . ? C22 C24 1.520(6) . ? C22 N21 1.547(5) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? N21 H21C 0.9100 . ? N21 H21D 0.9100 . ? N21 H21E 0.9100 . ? O21 H21 0.8400 . ? C31 O31 1.416(4) . ? C31 C32 1.519(5) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C34 1.506(6) . ? C32 C33 1.515(6) . ? C32 N31 1.524(5) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? N31 H31C 0.9100 . ? N31 H31D 0.9100 . ? N31 H31E 0.9100 . ? O31 H31 0.8400 . ? 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 O4 B1 O6 111.5(3) . . ? O4 B1 O1 110.0(3) . . ? O6 B1 O1 108.1(3) . . ? O4 B1 O3 109.1(3) . . ? O6 B1 O3 108.5(3) . . ? O1 B1 O3 109.5(3) . . ? O1 B2 O7 122.2(3) . . ? O1 B2 O2 121.4(3) . . ? O7 B2 O2 116.4(3) . . ? O3 B3 O8 121.8(4) . . ? O3 B3 O2 121.5(4) . . ? O8 B3 O2 116.7(3) . . ? O9 B4 O4 119.9(3) . . ? O9 B4 O5 119.9(3) . . ? O4 B4 O5 120.2(3) . . ? O10 B5 O6 122.4(4) . . ? O10 B5 O5 115.8(3) . . ? O6 B5 O5 121.8(3) . . ? B2 O1 B1 124.2(3) . . ? B3 O2 B2 118.7(3) . . ? B3 O3 B1 124.3(3) . . ? B4 O4 B1 122.0(3) . . ? B5 O5 B4 118.8(3) . . ? B5 O6 B1 120.7(3) . . ? B2 O7 H7 109.5 . . ? B3 O8 H8 109.5 . . ? B4 O9 H9 109.5 . . ? B5 O10 H10 109.5 . . ? O14 B11 O11 109.6(3) . . ? O14 B11 O13 109.2(3) . . ? O11 B11 O13 110.2(3) . . ? O14 B11 O16 110.8(3) . . ? O11 B11 O16 108.6(3) . . ? O13 B11 O16 108.5(3) . . ? O17 B12 O11 118.1(3) . . ? O17 B12 O12 121.7(3) . . ? O11 B12 O12 120.2(3) . . ? O13 B13 O18 122.4(4) . . ? O13 B13 O12 121.5(3) . . ? O18 B13 O12 116.1(3) . . ? O19 B14 O14 121.4(3) . . ? O19 B14 O15 117.8(3) . . ? O14 B14 O15 120.8(3) . . ? O20 B15 O16 122.8(3) . . ? O20 B15 O15 116.2(3) . . ? O16 B15 O15 121.0(4) . . ? B12 O11 B11 122.4(3) . . ? B13 O12 B12 118.8(3) . . ? B13 O13 B11 122.1(3) . . ? B14 O14 B11 123.9(3) . . ? B14 O15 B15 119.4(3) . . ? B15 O16 B11 123.4(3) . . ? B12 O17 H17 109.5 . . ? B13 O18 H18 109.5 . . ? B14 O19 H19 109.5 . . ? B15 O20 H20 109.5 . . ? O21 C21 C22 110.8(3) . . ? O21 C21 H21A 109.5 . . ? C22 C21 H21A 109.5 . . ? O21 C21 H21B 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 108.1 . . ? C21 C22 C23 114.1(4) . . ? C21 C22 C24 111.6(3) . . ? C23 C22 C24 110.1(4) . . ? C21 C22 N21 105.8(3) . . ? C23 C22 N21 107.1(3) . . ? C24 C22 N21 107.9(3) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 N21 H21C 109.5 . . ? C22 N21 H21D 109.5 . . ? H21C N21 H21D 109.5 . . ? C22 N21 H21E 109.5 . . ? H21C N21 H21E 109.5 . . ? H21D N21 H21E 109.5 . . ? C21 O21 H21 109.5 . . ? O31 C31 C32 111.6(3) . . ? O31 C31 H31A 109.3 . . ? C32 C31 H31A 109.3 . . ? O31 C31 H31B 109.3 . . ? C32 C31 H31B 109.3 . . ? H31A C31 H31B 108.0 . . ? C34 C32 C33 113.6(5) . . ? C34 C32 C31 111.7(4) . . ? C33 C32 C31 112.7(4) . . ? C34 C32 N31 106.1(4) . . ? C33 C32 N31 107.7(3) . . ? C31 C32 N31 104.3(3) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C32 N31 H31C 109.5 . . ? C32 N31 H31D 109.5 . . ? H31C N31 H31D 109.5 . . ? C32 N31 H31E 109.5 . . ? H31C N31 H31E 109.5 . . ? H31D N31 H31E 109.5 . . ? C31 O31 H31 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O7 H7 O14 0.84 1.85 2.689(4) 173.0 1_556 O8 H8 O16 0.84 1.83 2.670(4) 172.8 1_565 O9 H9 O7 0.84 2.01 2.831(4) 166.1 1_465 O10 H10 O13 0.84 1.88 2.706(4) 165.8 1_566 O17 H17 O19 0.84 2.04 2.833(4) 157.9 1_645 O18 H18 O6 0.84 1.83 2.646(4) 161.9 1_544 O19 H19 O1 0.84 1.86 2.691(4) 169.9 1_554 O20 H20 O3 0.84 1.84 2.674(4) 174.5 1_545 N21 H21C O2 0.91 2.50 3.224(5) 136.3 . N21 H21D O20 0.91 2.02 2.836(4) 148.2 1_655 N21 H21E O31 0.91 1.91 2.765(4) 155.3 . O21 H21 O18 0.84 1.83 2.652(4) 166.6 1_566 N31 H31C O10 0.91 2.01 2.854(4) 153.5 1_644 N31 H31D O21 0.91 1.99 2.876(4) 163.0 1_554 N31 H31E O11 0.91 1.90 2.798(4) 170.2 . O31 H31 O8 0.84 1.92 2.729(4) 161.4 . _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.612 _refine_diff_density_min -0.264 _refine_diff_density_rms 0.064 #===END data_1b #TrackingRef 'pentaborates.CIF' _database_code_depnum_ccdc_archive 'CCDC 764921' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H14 B5 N O11' _chemical_formula_weight 306.21 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' 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7992(3) _cell_length_b 9.0108(2) _cell_length_c 9.3873(3) _cell_angle_alpha 73.957(2) _cell_angle_beta 78.099(2) _cell_angle_gamma 63.845(2) _cell_volume 638.99(3) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 2878 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.592 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 316 _exptl_absorpt_coefficient_mu 0.146 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9687 _exptl_absorpt_correction_T_max 0.9942 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2003)' _exptl_special_details ; SADABS was used to perform the Absorption correction Parameter refinement on 11082 reflections reduced R(int) from 0.1327 to 0.0361 Ratio of minimum to maximum apparent transmission: 0.925823 The given Tmin and Tmax were generated using the SHELX SIZE command ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11693 _diffrn_reflns_av_R_equivalents 0.0354 _diffrn_reflns_av_sigmaI/netI 0.0326 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2921 _reflns_number_gt 2573 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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^)+(0.0188P)^2^+0.4666P] 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 2921 _refine_ls_number_parameters 194 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0457 _refine_ls_R_factor_gt 0.0385 _refine_ls_wR_factor_ref 0.0865 _refine_ls_wR_factor_gt 0.0817 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _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 0.34157(19) 0.88849(19) 0.30547(17) 0.0128(3) Uani 1 1 d . . . B2 B 0.58518(19) 0.76730(19) 0.45705(17) 0.0141(3) Uani 1 1 d . . . B3 B 0.5440(2) 0.5896(2) 0.33670(17) 0.0142(3) Uani 1 1 d . . . B4 B 0.2812(2) 1.1455(2) 0.10697(17) 0.0146(3) Uani 1 1 d . . . B5 B 0.07361(19) 1.1401(2) 0.31371(17) 0.0138(3) Uani 1 1 d . . . O1 O 0.44465(12) 0.90081(12) 0.40466(11) 0.0156(2) Uani 1 1 d . . . O2 O 0.64529(12) 0.61493(12) 0.41426(11) 0.0157(2) Uani 1 1 d . . . O3 O 0.38646(12) 0.71196(11) 0.30520(11) 0.0137(2) Uani 1 1 d . . . O4 O 0.37251(12) 0.97630(12) 0.15408(10) 0.0150(2) Uani 1 1 d . . . O5 O 0.13706(12) 1.23173(12) 0.19442(11) 0.0154(2) Uani 1 1 d . . . O6 O 0.16218(12) 0.96992(12) 0.36179(10) 0.0137(2) Uani 1 1 d . . . O7 O 0.67708(13) 0.77714(12) 0.55237(12) 0.0186(2) Uani 1 1 d . . . H7 H 0.6340 0.8756 0.5680 0.028 Uiso 1 1 calc R . . O8 O 0.59696(12) 0.44033(12) 0.29548(11) 0.0172(2) Uani 1 1 d . . . H8 H 0.6967 0.3781 0.3178 0.026 Uiso 1 1 calc R . . O9 O 0.33204(13) 1.23496(12) -0.01936(11) 0.0192(2) Uani 1 1 d . . . H9 H 0.4242 1.1708 -0.0581 0.029 Uiso 1 1 calc R . . O10 O -0.08250(12) 1.22276(12) 0.38288(11) 0.0187(2) Uani 1 1 d . . . H10 H -0.1016 1.1574 0.4605 0.028 Uiso 1 1 calc R . . C11 C 1.06422(19) 0.18499(19) 0.79628(17) 0.0220(3) Uani 1 1 d . . . H11A H 1.0187 0.1209 0.7599 0.026 Uiso 1 1 calc R . . H11B H 1.1895 0.1354 0.7747 0.026 Uiso 1 1 calc R . . C12 C 0.99283(18) 0.36805(19) 0.71432(18) 0.0218(3) Uani 1 1 d . . . H12A H 1.0452 0.4311 0.7436 0.026 Uiso 1 1 calc R . . H12B H 1.0193 0.3748 0.6056 0.026 Uiso 1 1 calc R . . C13 C 0.7608(2) 0.42146(19) 0.91684(17) 0.0234(3) Uani 1 1 d . . . H13A H 0.6357 0.4650 0.9402 0.028 Uiso 1 1 calc R . . H13B H 0.8031 0.4851 0.9573 0.028 Uiso 1 1 calc R . . C14 C 0.8422(2) 0.23459(19) 0.98658(17) 0.0224(3) Uani 1 1 d . . . H14A H 0.8149 0.2177 1.0960 0.027 Uiso 1 1 calc R . . H14B H 0.7953 0.1725 0.9491 0.027 Uiso 1 1 calc R . . N11 N 0.80494(15) 0.44430(15) 0.75201(14) 0.0183(3) Uani 1 1 d . . . H11C H 0.7556 0.3942 0.7139 0.022 Uiso 1 1 calc R . . H11D H 0.7622 0.5578 0.7090 0.022 Uiso 1 1 calc R . . O11 O 1.02213(14) 0.16900(13) 0.95186(12) 0.0227(2) 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 0.0115(7) 0.0113(7) 0.0137(7) -0.0021(5) -0.0013(5) -0.0033(6) B2 0.0131(7) 0.0136(7) 0.0140(7) -0.0021(6) -0.0004(6) -0.0049(6) B3 0.0143(7) 0.0142(7) 0.0127(7) -0.0016(6) 0.0012(6) -0.0064(6) B4 0.0146(7) 0.0139(7) 0.0156(7) -0.0042(6) -0.0015(6) -0.0055(6) B5 0.0127(7) 0.0144(7) 0.0136(7) -0.0038(6) -0.0026(6) -0.0039(6) O1 0.0153(5) 0.0122(5) 0.0186(5) -0.0040(4) -0.0059(4) -0.0027(4) O2 0.0132(5) 0.0128(5) 0.0190(5) -0.0045(4) -0.0039(4) -0.0016(4) O3 0.0133(5) 0.0106(5) 0.0158(5) -0.0028(4) -0.0019(4) -0.0035(4) O4 0.0142(5) 0.0128(5) 0.0142(5) -0.0019(4) 0.0009(4) -0.0037(4) O5 0.0162(5) 0.0116(5) 0.0147(5) -0.0023(4) 0.0011(4) -0.0037(4) O6 0.0115(5) 0.0123(5) 0.0137(5) -0.0015(4) -0.0003(4) -0.0028(4) O7 0.0185(5) 0.0135(5) 0.0231(5) -0.0056(4) -0.0079(4) -0.0025(4) O8 0.0137(5) 0.0123(5) 0.0234(5) -0.0056(4) -0.0039(4) -0.0016(4) O9 0.0189(5) 0.0137(5) 0.0182(5) -0.0027(4) 0.0048(4) -0.0038(4) O10 0.0148(5) 0.0150(5) 0.0170(5) 0.0009(4) 0.0020(4) -0.0019(4) C11 0.0184(7) 0.0200(7) 0.0248(8) -0.0048(6) -0.0036(6) -0.0047(6) C12 0.0153(7) 0.0222(8) 0.0241(8) -0.0016(6) -0.0009(6) -0.0067(6) C13 0.0244(8) 0.0196(7) 0.0233(8) -0.0071(6) 0.0023(6) -0.0070(6) C14 0.0254(8) 0.0211(8) 0.0197(7) -0.0024(6) -0.0022(6) -0.0096(6) N11 0.0169(6) 0.0137(6) 0.0233(7) -0.0015(5) -0.0048(5) -0.0056(5) O11 0.0221(6) 0.0220(6) 0.0229(6) -0.0012(4) -0.0089(4) -0.0071(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 O4 1.4590(18) . ? B1 O3 1.4609(17) . ? B1 O6 1.4693(17) . ? B1 O1 1.4820(18) . ? B2 O1 1.3530(18) . ? B2 O7 1.3667(18) . ? B2 O2 1.3796(18) . ? B3 O8 1.3553(18) . ? B3 O3 1.3660(18) . ? B3 O2 1.3840(18) . ? B4 O9 1.3517(18) . ? B4 O4 1.3635(18) . ? B4 O5 1.3933(18) . ? B5 O10 1.3641(18) . ? B5 O6 1.3678(18) . ? B5 O5 1.3731(18) . ? O7 H7 0.8400 . ? O8 H8 0.8400 . ? O9 H9 0.8400 . ? O10 H10 0.8400 . ? C11 O11 1.4137(19) . ? C11 C12 1.514(2) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 N11 1.4908(18) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 N11 1.4946(19) . ? C13 C14 1.516(2) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 O11 1.4250(18) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? N11 H11C 0.9200 . ? N11 H11D 0.9200 . ? 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 O4 B1 O3 108.96(11) . . ? O4 B1 O6 110.29(11) . . ? O3 B1 O6 110.35(11) . . ? O4 B1 O1 109.24(11) . . ? O3 B1 O1 110.87(11) . . ? O6 B1 O1 107.12(11) . . ? O1 B2 O7 121.92(13) . . ? O1 B2 O2 121.58(13) . . ? O7 B2 O2 116.49(12) . . ? O8 B3 O3 118.80(13) . . ? O8 B3 O2 120.47(13) . . ? O3 B3 O2 120.69(12) . . ? O9 B4 O4 121.65(13) . . ? O9 B4 O5 118.47(13) . . ? O4 B4 O5 119.78(13) . . ? O10 B5 O6 120.30(13) . . ? O10 B5 O5 118.22(13) . . ? O6 B5 O5 121.48(13) . . ? B2 O1 B1 121.93(11) . . ? B2 O2 B3 118.69(11) . . ? B3 O3 B1 121.09(11) . . ? B4 O4 B1 121.32(11) . . ? B5 O5 B4 118.81(11) . . ? B5 O6 B1 119.58(11) . . ? B2 O7 H7 109.5 . . ? B3 O8 H8 109.5 . . ? B4 O9 H9 109.5 . . ? B5 O10 H10 109.5 . . ? O11 C11 C12 111.73(12) . . ? O11 C11 H11A 109.3 . . ? C12 C11 H11A 109.3 . . ? O11 C11 H11B 109.3 . . ? C12 C11 H11B 109.3 . . ? H11A C11 H11B 107.9 . . ? N11 C12 C11 109.11(12) . . ? N11 C12 H12A 109.9 . . ? C11 C12 H12A 109.9 . . ? N11 C12 H12B 109.9 . . ? C11 C12 H12B 109.9 . . ? H12A C12 H12B 108.3 . . ? N11 C13 C14 108.62(12) . . ? N11 C13 H13A 110.0 . . ? C14 C13 H13A 110.0 . . ? N11 C13 H13B 110.0 . . ? C14 C13 H13B 110.0 . . ? H13A C13 H13B 108.3 . . ? O11 C14 C13 110.73(12) . . ? O11 C14 H14A 109.5 . . ? C13 C14 H14A 109.5 . . ? O11 C14 H14B 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? C12 N11 C13 111.00(12) . . ? C12 N11 H11C 109.4 . . ? C13 N11 H11C 109.4 . . ? C12 N11 H11D 109.4 . . ? C13 N11 H11D 109.4 . . ? H11C N11 H11D 108.0 . . ? C11 O11 C14 110.48(11) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O7 H7 O1 0.84 1.89 2.7313(14) 174.9 2_676 O8 H8 O10 0.84 1.93 2.7681(14) 174.9 1_645 O9 H9 O4 0.84 1.92 2.7556(14) 176.9 2_675 O10 H10 O6 0.84 1.87 2.7076(14) 174.5 2_576 N11 H11C O3 0.92 1.94 2.8264(15) 162.1 2_666 N11 H11D O7 0.92 2.04 2.9259(16) 160.6 . _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.276 _refine_diff_density_min -0.235 _refine_diff_density_rms 0.052 #===END data_1c #TrackingRef 'pentaborates.CIF' _database_code_depnum_ccdc_archive 'CCDC 764922' #Structure solved in P1, due to the disordered cations not exhibiting #an inversion centre, which can be found for the borate anion framework. #The is also a partial water molecule inside the cavity _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H16.33 B5 N O12.16' _chemical_formula_weight 327.20 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 0.0000 '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 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 9.0614(2) _cell_length_b 9.3967(2) _cell_length_c 9.8368(2) _cell_angle_alpha 73.555(2) _cell_angle_beta 74.6210(10) _cell_angle_gamma 62.0930(10) _cell_volume 701.14(3) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 3157 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description 'Cut Shard' _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.550 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 339 _exptl_absorpt_coefficient_mu 0.144 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9829 _exptl_absorpt_correction_T_max 0.9971 _exptl_absorpt_process_details 'SADABS 2007/2 (Sheldrick, G.M., 2007)' _exptl_special_details ; SADABS was used to perform the Absorption correction Parameter refinement on 13883 reflections reduced R(int) from 0.0748 to 0.0275 Ratio of minimum to maximum apparent transmission: 0.933410 The given Tmin and Tmax were generated using the SHELX SIZE command ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius APEX II CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14142 _diffrn_reflns_av_R_equivalents 0.0276 _diffrn_reflns_av_sigmaI/netI 0.0244 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3199 _reflns_number_gt 2956 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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^)+(0.0470P)^2^+0.4811P] 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 ? _refine_ls_number_reflns 3199 _refine_ls_number_parameters 676 _refine_ls_number_restraints 1588 _refine_ls_R_factor_all 0.0461 _refine_ls_R_factor_gt 0.0409 _refine_ls_wR_factor_ref 0.1046 _refine_ls_wR_factor_gt 0.0994 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 0.918 _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 0.3011(5) 0.0247(4) 0.2973(4) 0.0174(7) Uani 1 1 d . . . B2 B 0.0904(5) 0.1060(5) 0.5150(4) 0.0262(8) Uani 1 1 d . . . B3 B 0.0857(5) 0.3140(4) 0.3081(4) 0.0194(7) Uani 1 1 d . . . B4 B 0.4152(5) -0.2104(5) 0.1738(4) 0.0216(7) Uani 1 1 d . . . B5 B 0.6022(5) -0.1730(4) 0.2784(4) 0.0195(7) Uani 1 1 d . . . O1 O 0.2145(3) -0.0104(3) 0.4439(2) 0.0206(5) Uani 1 1 d . . . O2 O 0.0200(4) 0.2683(3) 0.4480(3) 0.0338(6) Uani 1 1 d . . . O3 O 0.2206(3) 0.2004(3) 0.2370(2) 0.0190(5) Uani 1 1 d . . . O4 O 0.2856(3) -0.0674(3) 0.2065(2) 0.0207(5) Uani 1 1 d . . . O5 O 0.5696(3) -0.2731(3) 0.2192(3) 0.0239(5) Uani 1 1 d . . . O6 O 0.4784(3) -0.0248(3) 0.3034(2) 0.0208(5) Uani 1 1 d . . . O7 O 0.0282(4) 0.0718(3) 0.6573(3) 0.0370(7) Uani 1 1 d . . . H7 H 0.0754 -0.0296 0.6880 0.055 Uiso 1 1 calc R . . O8 O 0.0130(3) 0.4737(3) 0.2462(3) 0.0258(5) Uani 1 1 d . . . H8 H 0.0618 0.4874 0.1614 0.039 Uiso 1 1 calc R . . O9 O 0.4031(3) -0.3000(3) 0.0945(3) 0.0310(6) Uani 1 1 d . . . H9 H 0.3015 -0.2649 0.0856 0.047 Uiso 1 1 calc R . . O10 O 0.7569(3) -0.2241(3) 0.3108(3) 0.0272(6) Uani 1 1 d . . . H10 H 0.8188 -0.3192 0.2940 0.041 Uiso 1 1 calc R . . B11 B 0.0835(5) 0.7187(4) 0.9181(4) 0.0179(7) Uani 1 1 d . . . B12 B -0.0277(5) 0.9497(5) 1.0446(4) 0.0233(8) Uani 1 1 d . . . B13 B -0.2170(5) 0.9186(5) 0.9416(4) 0.0202(7) Uani 1 1 d . . . B14 B 0.2821(5) 0.6358(5) 0.6948(4) 0.0192(7) Uani 1 1 d . . . B15 B 0.2869(4) 0.4290(4) 0.9028(4) 0.0176(7) Uani 1 1 d . . . O11 O 0.1011(3) 0.8096(3) 1.0070(2) 0.0188(4) Uani 1 1 d . . . O12 O -0.1829(3) 1.0130(3) 1.0018(3) 0.0244(5) Uani 1 1 d . . . O13 O -0.0958(3) 0.7695(3) 0.9159(2) 0.0200(5) Uani 1 1 d . . . O14 O 0.1660(3) 0.7533(3) 0.7701(2) 0.0202(5) Uani 1 1 d . . . O15 O 0.3442(3) 0.4720(3) 0.7601(2) 0.0242(5) Uani 1 1 d . . . O16 O 0.1619(3) 0.5426(3) 0.9781(2) 0.0187(5) Uani 1 1 d . . . O17 O -0.0103(3) 1.0380(3) 1.1228(3) 0.0343(7) Uani 1 1 d . . . H17 H 0.0776 0.9805 1.1607 0.051 Uiso 1 1 calc R . . O18 O -0.3744(3) 0.9696(3) 0.9103(3) 0.0261(5) Uani 1 1 d . . . H18 H -0.4378 1.0625 0.9315 0.039 Uiso 1 1 calc R . . O19 O 0.3395(3) 0.6697(3) 0.5534(3) 0.0281(6) Uani 1 1 d . . . H19 H 0.2967 0.7716 0.5242 0.042 Uiso 1 1 calc R . . O20 O 0.3636(3) 0.2684(3) 0.9649(2) 0.0239(5) Uani 1 1 d . . . H20 H 0.3043 0.2496 1.0432 0.036 Uiso 1 1 calc R . . C121 C 0.7798(15) 0.5120(15) 0.8146(13) 0.022(2) Uani 0.397(3) 1 d PDU A 1 C122 C 0.6878(18) 0.4033(17) 0.8463(19) 0.020(2) Uani 0.397(3) 1 d PDU A 1 H12A H 0.7120 0.3273 0.9390 0.024 Uiso 0.397(3) 1 calc PR A 1 H12B H 0.5644 0.4725 0.8555 0.024 Uiso 0.397(3) 1 calc PR A 1 C123 C 0.9651(14) 0.4395(14) 0.7638(12) 0.023(2) Uani 0.397(3) 1 d PDU A 1 H12C H 0.9902 0.3901 0.6791 0.028 Uiso 0.397(3) 1 calc PR A 1 H12D H 1.0068 0.5257 0.7354 0.028 Uiso 0.397(3) 1 calc PR A 1 C124 C 0.6879(18) 0.6672(15) 0.7101(16) 0.036(3) Uani 0.397(3) 1 d PDU A 1 H12E H 0.7447 0.7398 0.6873 0.054 Uiso 0.397(3) 1 calc PR A 1 H12F H 0.5705 0.7239 0.7544 0.054 Uiso 0.397(3) 1 calc PR A 1 H12G H 0.6898 0.6373 0.6218 0.054 Uiso 0.397(3) 1 calc PR A 1 N121 N 0.747(2) 0.5691(19) 0.9529(12) 0.020(3) Uani 0.397(3) 1 d PDU A 1 H12H H 0.8191 0.4889 1.0126 0.030 Uiso 0.397(3) 1 calc PR A 1 H12I H 0.6387 0.5919 0.9957 0.030 Uiso 0.397(3) 1 calc PR A 1 H12J H 0.7651 0.6610 0.9337 0.030 Uiso 0.397(3) 1 calc PR A 1 O122 O 0.738(3) 0.310(3) 0.735(3) 0.020(2) Uani 0.397(3) 1 d PDU A 1 H122 H 0.8404 0.2439 0.7333 0.031 Uiso 0.397(3) 1 calc PR A 1 O123 O 1.0482(9) 0.3152(9) 0.8789(8) 0.057(2) Uani 0.397(3) 1 d PDU A 1 H123 H 1.1068 0.2256 0.8504 0.086 Uiso 0.397(3) 1 calc PR A 1 C221 C 0.7915(13) 0.4930(14) 0.8196(12) 0.022(2) Uani 0.396(5) 1 d PDU B 2 C222 C 0.7076(17) 0.3773(16) 0.8529(18) 0.016(2) Uani 0.396(5) 1 d PDU B 2 H22A H 0.7648 0.2799 0.9239 0.019 Uiso 0.396(5) 1 calc PR B 2 H22B H 0.5880 0.4331 0.8961 0.019 Uiso 0.396(5) 1 calc PR B 2 C223 C 0.7457(13) 0.6333(15) 0.6977(14) 0.042(3) Uani 0.396(5) 1 d PDU B 2 H22C H 0.8124 0.6957 0.6861 0.050 Uiso 0.396(5) 1 calc PR B 2 H22D H 0.7720 0.5923 0.6079 0.050 Uiso 0.396(5) 1 calc PR B 2 C224 C 0.9835(11) 0.3903(14) 0.7984(13) 0.028(2) Uani 0.396(5) 1 d PDU B 2 H22E H 1.0165 0.3311 0.7199 0.041 Uiso 0.396(5) 1 calc PR B 2 H22F H 1.0160 0.3115 0.8870 0.041 Uiso 0.396(5) 1 calc PR B 2 H22G H 1.0407 0.4626 0.7748 0.041 Uiso 0.396(5) 1 calc PR B 2 N221 N 0.7470(19) 0.559(2) 0.9551(14) 0.021(3) Uani 0.396(5) 1 d PDU B 2 H22H H 0.8156 0.6069 0.9510 0.032 Uiso 0.396(5) 1 calc PR B 2 H22I H 0.7613 0.4754 1.0321 0.032 Uiso 0.396(5) 1 calc PR B 2 H22J H 0.6374 0.6346 0.9639 0.032 Uiso 0.396(5) 1 calc PR B 2 O222 O 0.715(3) 0.325(3) 0.726(3) 0.020(2) Uani 0.396(5) 1 d PDU B 2 H222 H 0.8159 0.2803 0.6879 0.031 Uiso 0.396(5) 1 calc PR B 2 O223 O 0.5673(12) 0.7389(11) 0.7250(11) 0.061(2) Uani 0.396(5) 1 d PDU B 2 H223 H 0.5542 0.8237 0.7487 0.091 Uiso 0.396(5) 1 calc PR B 2 C321 C 0.7917(17) 0.4908(16) 0.7795(12) 0.027(3) Uani 0.206(4) 1 d PDU C 3 C322 C 0.7820(15) 0.451(2) 0.9419(11) 0.026(3) Uani 0.206(4) 1 d PDU C 3 H32A H 0.8828 0.3503 0.9693 0.031 Uiso 0.206(4) 1 calc PR C 3 H32B H 0.7809 0.5419 0.9749 0.031 Uiso 0.206(4) 1 calc PR C 3 C323 C 0.675(2) 0.654(2) 0.711(2) 0.031(4) Uani 0.206(4) 1 d PDU C 3 H32C H 0.7077 0.7384 0.7177 0.037 Uiso 0.206(4) 1 calc PR C 3 H32D H 0.6865 0.6548 0.6075 0.037 Uiso 0.206(4) 1 calc PR C 3 C324 C 0.9751(18) 0.461(3) 0.7113(18) 0.034(4) Uani 0.206(4) 1 d PDU C 3 H32E H 0.9820 0.4962 0.6069 0.050 Uiso 0.206(4) 1 calc PR C 3 H32F H 1.0497 0.3445 0.7345 0.050 Uiso 0.206(4) 1 calc PR C 3 H32G H 1.0103 0.5248 0.7491 0.050 Uiso 0.206(4) 1 calc PR C 3 N321 N 0.7640(19) 0.3606(17) 0.7416(14) 0.022(3) Uani 0.206(4) 1 d PDU C 3 H32H H 0.7395 0.3935 0.6507 0.033 Uiso 0.206(4) 1 calc PR C 3 H32I H 0.6763 0.3452 0.8042 0.033 Uiso 0.206(4) 1 calc PR C 3 H32J H 0.8593 0.2649 0.7473 0.033 Uiso 0.206(4) 1 calc PR C 3 O322 O 0.6308(14) 0.4277(15) 1.0098(11) 0.029(3) Uani 0.206(4) 1 d PDU C 3 H322 H 0.5696 0.4974 1.0626 0.044 Uiso 0.206(4) 1 calc PR C 3 O323 O 0.5021(18) 0.695(2) 0.776(2) 0.058(4) Uani 0.206(4) 1 d PDU C 3 H323 H 0.4384 0.7592 0.7154 0.088 Uiso 0.206(4) 1 calc PR C 3 C131 C 0.5739(11) 0.2597(13) 0.4266(10) 0.0263(17) Uani 0.454(3) 1 d PDU D 1 C132 C 0.6025(15) 0.290(2) 0.2632(9) 0.0232(12) Uani 0.454(3) 1 d PDU D 1 H13A H 0.6140 0.1947 0.2307 0.028 Uiso 0.454(3) 1 calc PR D 1 H13B H 0.5034 0.3874 0.2273 0.028 Uiso 0.454(3) 1 calc PR D 1 C133 C 0.6685(11) 0.0916(13) 0.5044(13) 0.035(2) Uani 0.454(3) 1 d PDU D 1 H13C H 0.6565 0.0949 0.6066 0.042 Uiso 0.454(3) 1 calc PR D 1 H13D H 0.6187 0.0194 0.4999 0.042 Uiso 0.454(3) 1 calc PR D 1 C134 C 0.3843(10) 0.3098(14) 0.4804(11) 0.0354(14) Uani 0.454(3) 1 d PDU D 1 H13E H 0.3466 0.2465 0.4452 0.053 Uiso 0.454(3) 1 calc PR D 1 H13F H 0.3212 0.4270 0.4448 0.053 Uiso 0.454(3) 1 calc PR D 1 H13G H 0.3640 0.2880 0.5855 0.053 Uiso 0.454(3) 1 calc PR D 1 N131 N 0.6188(19) 0.3767(16) 0.4672(18) 0.0213(13) Uani 0.454(3) 1 d PDU D 1 H13H H 0.6101 0.3583 0.5643 0.032 Uiso 0.454(3) 1 calc PR D 1 H13I H 0.5466 0.4817 0.4356 0.032 Uiso 0.454(3) 1 calc PR D 1 H13J H 0.7267 0.3605 0.4260 0.032 Uiso 0.454(3) 1 calc PR D 1 O132 O 0.7528(14) 0.318(2) 0.2049(10) 0.0199(15) Uani 0.454(3) 1 d PDU D 1 H132 H 0.7548 0.3817 0.2489 0.030 Uiso 0.454(3) 1 calc PR D 1 O133 O 0.8451(10) 0.0237(12) 0.4451(10) 0.078(3) Uani 0.454(3) 1 d PDU D 1 H133 H 0.8740 -0.0695 0.4286 0.116 Uiso 0.454(3) 1 calc PR D 1 C231 C 0.603(2) 0.2475(17) 0.4423(17) 0.024(2) Uani 0.193(7) 1 d PDU E 2 C232 C 0.580(2) 0.313(3) 0.2856(17) 0.0232(12) Uani 0.193(7) 1 d PDU E 2 H23A H 0.5428 0.2454 0.2538 0.028 Uiso 0.193(7) 1 calc PR E 2 H23B H 0.4906 0.4270 0.2748 0.028 Uiso 0.193(7) 1 calc PR E 2 C233 C 0.749(2) 0.0868(19) 0.479(3) 0.028(3) Uani 0.193(7) 1 d PDU E 2 H23C H 0.8450 0.0709 0.3990 0.033 Uiso 0.193(7) 1 calc PR E 2 H23D H 0.7862 0.0822 0.5664 0.033 Uiso 0.193(7) 1 calc PR E 2 C234 C 0.443(2) 0.231(3) 0.532(2) 0.0354(14) Uani 0.193(7) 1 d PDU E 2 H23E H 0.4184 0.1599 0.4934 0.053 Uiso 0.193(7) 1 calc PR E 2 H23F H 0.3471 0.3391 0.5282 0.053 Uiso 0.193(7) 1 calc PR E 2 H23G H 0.4608 0.1821 0.6319 0.053 Uiso 0.193(7) 1 calc PR E 2 N231 N 0.619(4) 0.377(3) 0.492(3) 0.0213(13) Uani 0.193(7) 1 d PDU E 2 H23H H 0.6650 0.3316 0.5744 0.032 Uiso 0.193(7) 1 calc PR E 2 H23I H 0.5144 0.4596 0.5093 0.032 Uiso 0.193(7) 1 calc PR E 2 H23J H 0.6861 0.4168 0.4232 0.032 Uiso 0.193(7) 1 calc PR E 2 O232 O 0.736(4) 0.310(5) 0.197(2) 0.0199(15) Uani 0.193(7) 1 d PDU E 2 H232 H 0.8128 0.2139 0.2098 0.030 Uiso 0.193(7) 1 calc PR E 2 O233 O 0.6891(19) -0.0375(14) 0.5020(16) 0.050(4) Uani 0.193(7) 1 d PDU E 2 H233 H 0.6792 -0.0470 0.4229 0.075 Uiso 0.193(7) 1 calc PR E 2 C331 C 0.6079(16) 0.2310(16) 0.4001(13) 0.026(2) Uani 0.210(4) 1 d PDU F 3 C332 C 0.4276(17) 0.2588(16) 0.4705(19) 0.0354(14) Uani 0.210(4) 1 d PDU F 3 H33A H 0.3885 0.3274 0.5441 0.042 Uiso 0.210(4) 1 calc PR F 3 H33B H 0.3512 0.3165 0.3976 0.042 Uiso 0.210(4) 1 calc PR F 3 C333 C 0.6754(19) 0.3563(18) 0.3654(13) 0.027(2) Uani 0.210(4) 1 d PDU F 3 H33C H 0.7972 0.3064 0.3259 0.032 Uiso 0.210(4) 1 calc PR F 3 H33D H 0.6166 0.4472 0.2906 0.032 Uiso 0.210(4) 1 calc PR F 3 C334 C 0.726(3) 0.078(2) 0.493(2) 0.036(5) Uani 0.210(4) 1 d PDU F 3 H33E H 0.8258 0.0924 0.4951 0.054 Uiso 0.210(4) 1 calc PR F 3 H33F H 0.7620 -0.0188 0.4513 0.054 Uiso 0.210(4) 1 calc PR F 3 H33G H 0.6660 0.0630 0.5905 0.054 Uiso 0.210(4) 1 calc PR F 3 N331 N 0.6362(18) 0.1774(18) 0.2597(14) 0.033(3) Uani 0.210(4) 1 d PDU F 3 H33H H 0.6011 0.2674 0.1894 0.050 Uiso 0.210(4) 1 calc PR F 3 H33I H 0.5762 0.1187 0.2705 0.050 Uiso 0.210(4) 1 calc PR F 3 H33J H 0.7481 0.1140 0.2353 0.050 Uiso 0.210(4) 1 calc PR F 3 O332 O 0.4242(16) 0.0999(17) 0.5371(11) 0.051(3) Uani 0.210(4) 1 d PDU F 3 H332 H 0.5211 0.0307 0.5545 0.076 Uiso 0.210(4) 1 calc PR F 3 O333 O 0.6539(19) 0.4205(18) 0.4886(15) 0.033(3) Uani 0.210(4) 1 d PDU F 3 H333 H 0.5788 0.5173 0.4810 0.049 Uiso 0.210(4) 1 calc PR F 3 C431 C 0.584(3) 0.265(4) 0.436(3) 0.027(3) Uani 0.143(7) 1 d PDU G 4 C432 C 0.614(4) 0.291(7) 0.273(3) 0.0232(12) Uani 0.143(7) 1 d PDU G 4 H43A H 0.6095 0.2017 0.2425 0.028 Uiso 0.143(7) 1 calc PR G 4 H43B H 0.5248 0.3962 0.2341 0.028 Uiso 0.143(7) 1 calc PR G 4 C433 C 0.418(3) 0.272(3) 0.517(3) 0.0354(14) Uani 0.143(7) 1 d PDU G 4 H43C H 0.4092 0.1703 0.5185 0.042 Uiso 0.143(7) 1 calc PR G 4 H43D H 0.4073 0.2806 0.6178 0.042 Uiso 0.143(7) 1 calc PR G 4 C434 C 0.724(3) 0.099(4) 0.491(5) 0.032(5) Uani 0.143(7) 1 d PDU G 4 H43E H 0.6987 0.0725 0.5961 0.048 Uiso 0.143(7) 1 calc PR G 4 H43F H 0.8329 0.1054 0.4634 0.048 Uiso 0.143(7) 1 calc PR G 4 H43G H 0.7281 0.0137 0.4496 0.048 Uiso 0.143(7) 1 calc PR G 4 N431 N 0.617(6) 0.393(5) 0.472(6) 0.0213(13) Uani 0.143(7) 1 d PDU G 4 H43H H 0.5183 0.4849 0.4804 0.032 Uiso 0.143(7) 1 calc PR G 4 H43I H 0.6936 0.4177 0.4016 0.032 Uiso 0.143(7) 1 calc PR G 4 H43J H 0.6577 0.3530 0.5570 0.032 Uiso 0.143(7) 1 calc PR G 4 O432 O 0.778(3) 0.293(4) 0.216(3) 0.0199(15) Uani 0.143(7) 1 d PDU G 4 H432 H 0.7873 0.3216 0.1261 0.030 Uiso 0.143(7) 1 calc PR G 4 O433 O 0.285(2) 0.412(3) 0.450(3) 0.059(5) Uani 0.143(7) 1 d PDU G 4 H433 H 0.2110 0.3848 0.4446 0.089 Uiso 0.143(7) 1 calc PR G 4 O101 O 0.3220(9) 0.0221(8) 0.8048(9) 0.0400(16) Uani 0.33 1 d PD . . H101 H 0.3296 0.0269 0.7159 0.060 Uiso 0.33 1 d PRD . . H102 H 0.3554 0.0898 0.8128 0.060 Uiso 0.33 1 d PRD . . 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 0.0189(16) 0.0124(16) 0.0124(16) -0.0036(13) 0.0000(13) -0.0004(13) B2 0.0284(19) 0.0164(18) 0.0165(17) -0.0024(14) 0.0046(14) -0.0001(15) B3 0.0187(16) 0.0127(17) 0.0165(17) -0.0021(13) 0.0002(13) -0.0003(14) B4 0.0210(17) 0.0173(17) 0.0190(17) -0.0047(13) -0.0008(14) -0.0026(14) B5 0.0204(17) 0.0125(16) 0.0200(18) -0.0012(13) 0.0014(13) -0.0058(14) O1 0.0237(11) 0.0111(10) 0.0148(10) -0.0011(8) 0.0026(9) -0.0013(9) O2 0.0393(14) 0.0123(11) 0.0218(12) 0.0010(9) 0.0128(10) 0.0003(10) O3 0.0218(11) 0.0112(10) 0.0154(10) -0.0012(8) 0.0003(8) -0.0024(9) O4 0.0208(11) 0.0165(11) 0.0194(11) -0.0045(9) -0.0003(9) -0.0045(9) O5 0.0232(12) 0.0166(11) 0.0251(12) -0.0082(9) -0.0065(9) 0.0009(9) O6 0.0193(11) 0.0139(11) 0.0242(12) -0.0056(9) -0.0015(9) -0.0028(9) O7 0.0461(17) 0.0183(13) 0.0175(12) 0.0020(10) 0.0120(11) -0.0020(12) O8 0.0242(12) 0.0150(12) 0.0211(12) -0.0014(9) 0.0058(9) -0.0004(10) O9 0.0227(12) 0.0279(13) 0.0398(15) -0.0182(11) -0.0052(11) -0.0019(10) O10 0.0214(12) 0.0202(13) 0.0336(14) -0.0078(11) -0.0051(11) -0.0017(10) B11 0.0200(17) 0.0115(16) 0.0179(17) -0.0012(13) -0.0004(14) -0.0054(14) B12 0.0250(19) 0.0156(17) 0.0255(19) -0.0083(14) -0.0029(15) -0.0037(15) B13 0.0201(17) 0.0194(18) 0.0162(17) -0.0031(13) -0.0002(13) -0.0061(15) B14 0.0212(16) 0.0154(17) 0.0179(17) -0.0022(13) 0.0006(13) -0.0076(14) B15 0.0165(15) 0.0159(17) 0.0180(17) -0.0035(13) 0.0000(12) -0.0061(14) O11 0.0181(10) 0.0145(11) 0.0193(10) -0.0077(9) -0.0010(8) -0.0019(9) O12 0.0209(11) 0.0172(12) 0.0310(13) -0.0103(10) -0.0042(10) -0.0014(9) O13 0.0188(11) 0.0148(11) 0.0236(12) -0.0057(9) -0.0010(9) -0.0050(9) O14 0.0242(12) 0.0139(11) 0.0155(11) -0.0019(8) 0.0019(9) -0.0054(9) O15 0.0276(12) 0.0139(10) 0.0174(11) -0.0037(9) 0.0058(9) -0.0021(9) O16 0.0196(11) 0.0137(11) 0.0152(10) -0.0027(8) 0.0031(8) -0.0039(9) O17 0.0238(13) 0.0277(14) 0.0504(17) -0.0274(13) -0.0131(12) 0.0049(10) O18 0.0195(11) 0.0196(13) 0.0355(14) -0.0109(11) -0.0023(10) -0.0032(10) O19 0.0353(13) 0.0107(11) 0.0191(12) -0.0039(9) 0.0060(10) 0.0011(10) O20 0.0254(12) 0.0121(11) 0.0164(11) 0.0011(9) 0.0052(9) 0.0000(10) C121 0.023(3) 0.022(4) 0.023(3) -0.009(3) 0.002(3) -0.013(3) C122 0.025(4) 0.018(4) 0.018(4) -0.007(3) -0.002(3) -0.008(3) C123 0.027(4) 0.017(5) 0.028(5) -0.009(4) -0.007(3) -0.005(3) C124 0.054(6) 0.008(4) 0.029(5) -0.006(3) -0.020(5) 0.009(4) N121 0.034(7) 0.015(5) 0.011(4) 0.004(3) -0.009(4) -0.011(4) O122 0.015(6) 0.023(4) 0.022(3) -0.009(3) -0.010(3) -0.001(4) O123 0.042(4) 0.051(4) 0.059(5) -0.022(4) -0.017(3) 0.007(3) C221 0.025(3) 0.020(3) 0.022(3) -0.008(3) -0.003(3) -0.009(3) C222 0.019(4) 0.012(4) 0.021(4) -0.011(3) 0.002(3) -0.008(3) C223 0.053(5) 0.028(5) 0.040(4) 0.005(4) -0.004(4) -0.022(4) C224 0.015(4) 0.033(6) 0.036(6) -0.025(4) 0.012(4) -0.008(4) N221 0.017(6) 0.031(7) 0.028(5) -0.022(5) 0.011(4) -0.017(5) O222 0.015(6) 0.023(4) 0.022(3) -0.009(3) -0.010(3) -0.001(4) O223 0.068(6) 0.039(4) 0.070(6) 0.012(4) -0.026(5) -0.023(4) C321 0.033(4) 0.024(4) 0.025(4) -0.009(4) -0.004(4) -0.010(4) C322 0.023(5) 0.025(5) 0.022(4) -0.013(4) 0.001(4) -0.002(4) C323 0.043(6) 0.020(5) 0.032(6) -0.006(5) -0.011(5) -0.011(5) C324 0.034(6) 0.050(10) 0.032(8) -0.027(8) -0.002(6) -0.020(6) N321 0.029(7) 0.018(6) 0.013(6) -0.007(5) 0.005(5) -0.008(5) O322 0.031(6) 0.018(6) 0.023(5) -0.005(4) 0.001(4) 0.000(5) O323 0.045(6) 0.062(9) 0.044(8) -0.018(7) -0.009(6) 0.002(6) C131 0.030(3) 0.029(3) 0.028(3) -0.011(3) -0.002(2) -0.017(2) C132 0.025(2) 0.024(2) 0.022(2) -0.0182(19) -0.0031(17) -0.004(2) C133 0.038(4) 0.030(3) 0.030(4) -0.010(3) -0.003(4) -0.008(4) C134 0.028(3) 0.046(3) 0.041(3) -0.027(3) -0.003(2) -0.013(2) N131 0.0210(18) 0.027(3) 0.017(3) -0.015(2) -0.003(2) -0.0044(18) O132 0.022(3) 0.016(3) 0.022(2) -0.0085(17) -0.009(2) -0.002(2) O133 0.055(4) 0.068(5) 0.071(6) -0.009(4) -0.008(4) 0.002(4) C231 0.026(4) 0.034(4) 0.022(4) -0.019(3) -0.002(3) -0.013(3) C232 0.025(2) 0.024(2) 0.022(2) -0.0182(19) -0.0031(17) -0.004(2) C233 0.031(5) 0.028(5) 0.021(5) -0.017(5) 0.002(5) -0.006(4) C234 0.028(3) 0.046(3) 0.041(3) -0.027(3) -0.003(2) -0.013(2) N231 0.0210(18) 0.027(3) 0.017(3) -0.015(2) -0.003(2) -0.0044(18) O232 0.022(3) 0.016(3) 0.022(2) -0.0085(17) -0.009(2) -0.002(2) O233 0.063(8) 0.032(5) 0.054(7) -0.015(5) -0.013(6) -0.014(5) C331 0.022(4) 0.029(4) 0.031(4) -0.017(4) 0.005(4) -0.013(3) C332 0.028(3) 0.046(3) 0.041(3) -0.027(3) -0.003(2) -0.013(2) C333 0.028(4) 0.027(4) 0.025(4) -0.011(4) -0.002(4) -0.009(4) C334 0.038(7) 0.023(6) 0.037(7) -0.015(6) 0.005(7) -0.006(7) N331 0.026(6) 0.024(7) 0.049(6) -0.025(6) 0.004(5) -0.005(5) O332 0.061(7) 0.101(8) 0.033(5) -0.047(5) 0.029(5) -0.069(6) O333 0.031(7) 0.024(7) 0.035(7) -0.022(5) 0.001(5) 0.000(5) C431 0.029(4) 0.031(4) 0.025(4) -0.017(4) -0.003(4) -0.011(3) C432 0.025(2) 0.024(2) 0.022(2) -0.0182(19) -0.0031(17) -0.004(2) C433 0.028(3) 0.046(3) 0.041(3) -0.027(3) -0.003(2) -0.013(2) C434 0.034(7) 0.025(6) 0.035(8) -0.001(7) -0.003(8) -0.014(7) N431 0.0210(18) 0.027(3) 0.017(3) -0.015(2) -0.003(2) -0.0044(18) O432 0.022(3) 0.016(3) 0.022(2) -0.0085(17) -0.009(2) -0.002(2) O433 0.041(7) 0.054(10) 0.077(12) -0.016(8) -0.013(8) -0.012(7) O101 0.041(4) 0.026(3) 0.054(4) -0.003(3) -0.022(3) -0.010(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 O6 1.461(4) . ? B1 O3 1.469(4) . ? B1 O1 1.476(4) . ? B1 O4 1.477(4) . ? B2 O1 1.347(4) . ? B2 O7 1.370(5) . ? B2 O2 1.382(5) . ? B3 O8 1.352(4) . ? B3 O3 1.367(4) . ? B3 O2 1.379(4) . ? B4 O9 1.354(5) . ? B4 O4 1.362(4) . ? B4 O5 1.384(4) . ? B5 O10 1.348(4) . ? B5 O6 1.358(4) . ? B5 O5 1.404(5) . ? O7 H7 0.8400 . ? O8 H8 0.8400 . ? O9 H9 0.8400 . ? O10 H10 0.8400 . ? B11 O11 1.464(4) . ? B11 O13 1.468(4) . ? B11 O16 1.470(4) . ? B11 O14 1.472(4) . ? B12 O11 1.357(4) . ? B12 O17 1.362(4) . ? B12 O12 1.377(5) . ? B13 O13 1.359(4) . ? B13 O18 1.367(4) . ? B13 O12 1.372(5) . ? B14 O19 1.352(4) . ? B14 O14 1.355(4) . ? B14 O15 1.385(4) . ? B15 O16 1.358(4) . ? B15 O20 1.362(4) . ? B15 O15 1.375(4) . ? O17 H17 0.8400 . ? O18 H18 0.8400 . ? O19 H19 0.8400 . ? O20 H20 0.8400 . ? C121 C123 1.487(10) . ? C121 N121 1.509(6) . ? C121 C122 1.521(7) . ? C121 C124 1.532(10) . ? C122 O122 1.438(6) . ? C122 H12A 0.9900 . ? C122 H12B 0.9900 . ? C123 O123 1.447(7) . ? C123 H12C 0.9900 . ? C123 H12D 0.9900 . ? C124 H12E 0.9800 . ? C124 H12F 0.9800 . ? C124 H12G 0.9800 . ? N121 H12H 0.9100 . ? N121 H12I 0.9100 . ? N121 H12J 0.9100 . ? O122 H122 0.8400 . ? O123 H123 0.8400 . ? C221 C223 1.484(9) . ? C221 N221 1.507(6) . ? C221 C222 1.519(7) . ? C221 C224 1.533(9) . ? C222 O222 1.439(6) . ? C222 H22A 0.9900 . ? C222 H22B 0.9900 . ? C223 O223 1.445(7) . ? C223 H22C 0.9900 . ? C223 H22D 0.9900 . ? C224 H22E 0.9800 . ? C224 H22F 0.9800 . ? C224 H22G 0.9800 . ? N221 H22H 0.9100 . ? N221 H22I 0.9100 . ? N221 H22J 0.9100 . ? O222 H222 0.8400 . ? O223 H223 0.8400 . ? C321 C323 1.484(10) . ? C321 N321 1.515(8) . ? C321 C322 1.523(7) . ? C321 C324 1.540(10) . ? C322 O322 1.445(7) . ? C322 H32A 0.9900 . ? C322 H32B 0.9900 . ? C323 O323 1.436(9) . ? C323 H32C 0.9900 . ? C323 H32D 0.9900 . ? C324 H32E 0.9800 . ? C324 H32F 0.9800 . ? C324 H32G 0.9800 . ? N321 H32H 0.9100 . ? N321 H32I 0.9100 . ? N321 H32J 0.9100 . ? O322 H322 0.8400 . ? O323 H323 0.8400 . ? C131 C133 1.487(9) . ? C131 N131 1.513(7) . ? C131 C132 1.523(6) . ? C131 C134 1.535(8) . ? C132 O132 1.443(6) . ? C132 H13A 0.9900 . ? C132 H13B 0.9900 . ? C133 O133 1.438(7) . ? C133 H13C 0.9900 . ? C133 H13D 0.9900 . ? C134 H13E 0.9800 . ? C134 H13F 0.9800 . ? C134 H13G 0.9800 . ? N131 H13H 0.9100 . ? N131 H13I 0.9100 . ? N131 H13J 0.9100 . ? O132 H132 0.8400 . ? O133 H133 0.8400 . ? C231 C233 1.495(10) . ? C231 N231 1.508(7) . ? C231 C232 1.521(7) . ? C231 C234 1.537(10) . ? C232 O232 1.445(7) . ? C232 H23A 0.9900 . ? C232 H23B 0.9900 . ? C233 O233 1.444(8) . ? C233 H23C 0.9900 . ? C233 H23D 0.9900 . ? C234 H23E 0.9800 . ? C234 H23F 0.9800 . ? C234 H23G 0.9800 . ? N231 H23H 0.9100 . ? N231 H23I 0.9100 . ? N231 H23J 0.9100 . ? O232 H232 0.8400 . ? O233 H233 0.8400 . ? C331 C333 1.487(10) . ? C331 C332 1.522(8) . ? C331 N331 1.521(8) . ? C331 C334 1.543(10) . ? C332 O332 1.462(7) . ? C332 H33A 0.9900 . ? C332 H33B 0.9900 . ? C333 O333 1.432(7) . ? C333 H33C 0.9900 . ? C333 H33D 0.9900 . ? C334 H33E 0.9800 . ? C334 H33F 0.9800 . ? C334 H33G 0.9800 . ? N331 H33H 0.9100 . ? N331 H33I 0.9100 . ? N331 H33J 0.9100 . ? O332 H332 0.8400 . ? O333 H333 0.8400 . ? C431 C433 1.489(11) . ? C431 N431 1.512(8) . ? C431 C432 1.523(8) . ? C431 C434 1.537(11) . ? C432 O432 1.445(7) . ? C432 H43A 0.9900 . ? C432 H43B 0.9900 . ? C433 O433 1.437(8) . ? C433 H43C 0.9900 . ? C433 H43D 0.9900 . ? C434 H43E 0.9800 . ? C434 H43F 0.9800 . ? C434 H43G 0.9800 . ? N431 H43H 0.9100 . ? N431 H43I 0.9100 . ? N431 H43J 0.9100 . ? O432 H432 0.8400 . ? O433 H433 0.8400 . ? O101 H101 0.8488 . ? O101 H102 0.8499 . ? 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 O6 B1 O3 110.0(3) . . ? O6 B1 O1 108.7(3) . . ? O3 B1 O1 110.2(3) . . ? O6 B1 O4 111.1(3) . . ? O3 B1 O4 108.5(3) . . ? O1 B1 O4 108.4(3) . . ? O1 B2 O7 122.4(3) . . ? O1 B2 O2 121.4(3) . . ? O7 B2 O2 116.1(3) . . ? O8 B3 O3 122.1(3) . . ? O8 B3 O2 117.5(3) . . ? O3 B3 O2 120.4(3) . . ? O9 B4 O4 122.8(3) . . ? O9 B4 O5 115.5(3) . . ? O4 B4 O5 121.7(3) . . ? O10 B5 O6 119.7(3) . . ? O10 B5 O5 120.0(3) . . ? O6 B5 O5 120.3(3) . . ? B2 O1 B1 123.9(3) . . ? B3 O2 B2 119.3(3) . . ? B3 O3 B1 124.4(3) . . ? B4 O4 B1 121.5(3) . . ? B4 O5 B5 118.5(3) . . ? B5 O6 B1 122.5(3) . . ? B2 O7 H7 109.5 . . ? B3 O8 H8 109.5 . . ? B4 O9 H9 109.5 . . ? B5 O10 H10 109.5 . . ? O11 B11 O13 110.4(3) . . ? O11 B11 O16 109.0(3) . . ? O13 B11 O16 109.1(3) . . ? O11 B11 O14 109.3(3) . . ? O13 B11 O14 108.5(3) . . ? O16 B11 O14 110.5(3) . . ? O11 B12 O17 122.3(3) . . ? O11 B12 O12 121.5(3) . . ? O17 B12 O12 116.2(3) . . ? O13 B13 O18 118.4(3) . . ? O13 B13 O12 120.5(3) . . ? O18 B13 O12 121.0(3) . . ? O19 B14 O14 122.7(3) . . ? O19 B14 O15 116.6(3) . . ? O14 B14 O15 120.7(3) . . ? O16 B15 O20 121.9(3) . . ? O16 B15 O15 121.2(3) . . ? O20 B15 O15 116.9(3) . . ? B12 O11 B11 122.0(3) . . ? B13 O12 B12 118.9(3) . . ? B13 O13 B11 122.1(3) . . ? B14 O14 B11 123.9(3) . . ? B15 O15 B14 119.4(3) . . ? B15 O16 B11 123.8(3) . . ? B12 O17 H17 109.5 . . ? B13 O18 H18 109.5 . . ? B14 O19 H19 109.5 . . ? B15 O20 H20 109.5 . . ? C123 C121 N121 108.6(8) . . ? C123 C121 C122 118.0(8) . . ? N121 C121 C122 105.7(7) . . ? C123 C121 C124 111.1(7) . . ? N121 C121 C124 104.9(8) . . ? C122 C121 C124 107.5(9) . . ? O122 C122 C121 111.9(8) . . ? O122 C122 H12A 109.2 . . ? C121 C122 H12A 109.2 . . ? O122 C122 H12B 109.2 . . ? C121 C122 H12B 109.2 . . ? H12A C122 H12B 107.9 . . ? O123 C123 C121 108.6(8) . . ? O123 C123 H12C 110.0 . . ? C121 C123 H12C 110.0 . . ? O123 C123 H12D 110.0 . . ? C121 C123 H12D 110.0 . . ? H12C C123 H12D 108.4 . . ? C121 C124 H12E 109.5 . . ? C121 C124 H12F 109.5 . . ? H12E C124 H12F 109.5 . . ? C121 C124 H12G 109.5 . . ? H12E C124 H12G 109.5 . . ? H12F C124 H12G 109.5 . . ? C121 N121 H12H 109.5 . . ? C121 N121 H12I 109.5 . . ? H12H N121 H12I 109.5 . . ? C121 N121 H12J 109.5 . . ? H12H N121 H12J 109.5 . . ? H12I N121 H12J 109.5 . . ? C122 O122 H122 109.5 . . ? C123 O123 H123 109.5 . . ? C223 C221 N221 108.6(9) . . ? C223 C221 C222 118.4(8) . . ? N221 C221 C222 105.3(6) . . ? C223 C221 C224 109.6(7) . . ? N221 C221 C224 106.4(8) . . ? C222 C221 C224 107.9(8) . . ? O222 C222 C221 111.8(8) . . ? O222 C222 H22A 109.3 . . ? C221 C222 H22A 109.3 . . ? O222 C222 H22B 109.3 . . ? C221 C222 H22B 109.3 . . ? H22A C222 H22B 107.9 . . ? O223 C223 C221 109.5(7) . . ? O223 C223 H22C 109.8 . . ? C221 C223 H22C 109.8 . . ? O223 C223 H22D 109.8 . . ? C221 C223 H22D 109.8 . . ? H22C C223 H22D 108.2 . . ? C221 C224 H22E 109.5 . . ? C221 C224 H22F 109.5 . . ? H22E C224 H22F 109.5 . . ? C221 C224 H22G 109.5 . . ? H22E C224 H22G 109.5 . . ? H22F C224 H22G 109.5 . . ? C221 N221 H22H 109.5 . . ? C221 N221 H22I 109.5 . . ? H22H N221 H22I 109.5 . . ? C221 N221 H22J 109.5 . . ? H22H N221 H22J 109.5 . . ? H22I N221 H22J 109.5 . . ? C222 O222 H222 109.5 . . ? C223 O223 H223 109.5 . . ? C323 C321 N321 108.5(10) . . ? C323 C321 C322 119.3(10) . . ? N321 C321 C322 105.9(7) . . ? C323 C321 C324 109.0(8) . . ? N321 C321 C324 105.1(9) . . ? C322 C321 C324 108.1(9) . . ? O322 C322 C321 110.0(8) . . ? O322 C322 H32A 109.7 . . ? C321 C322 H32A 109.7 . . ? O322 C322 H32B 109.7 . . ? C321 C322 H32B 109.7 . . ? H32A C322 H32B 108.2 . . ? O323 C323 C321 112.1(10) . . ? O323 C323 H32C 109.2 . . ? C321 C323 H32C 109.2 . . ? O323 C323 H32D 109.2 . . ? C321 C323 H32D 109.2 . . ? H32C C323 H32D 107.9 . . ? C321 C324 H32E 109.5 . . ? C321 C324 H32F 109.5 . . ? H32E C324 H32F 109.5 . . ? C321 C324 H32G 109.5 . . ? H32E C324 H32G 109.5 . . ? H32F C324 H32G 109.5 . . ? C321 N321 H32H 109.5 . . ? C321 N321 H32I 109.5 . . ? H32H N321 H32I 109.5 . . ? C321 N321 H32J 109.5 . . ? H32H N321 H32J 109.5 . . ? H32I N321 H32J 109.5 . . ? C322 O322 H322 109.5 . . ? C323 O323 H323 109.5 . . ? C133 C131 N131 108.4(7) . . ? C133 C131 C132 118.2(7) . . ? N131 C131 C132 106.2(5) . . ? C133 C131 C134 108.3(6) . . ? N131 C131 C134 106.8(6) . . ? C132 C131 C134 108.4(7) . . ? O132 C132 C131 110.8(6) . . ? O132 C132 H13A 109.5 . . ? C131 C132 H13A 109.5 . . ? O132 C132 H13B 109.5 . . ? C131 C132 H13B 109.5 . . ? H13A C132 H13B 108.1 . . ? O133 C133 C131 112.2(7) . . ? O133 C133 H13C 109.2 . . ? C131 C133 H13C 109.2 . . ? O133 C133 H13D 109.2 . . ? C131 C133 H13D 109.2 . . ? H13C C133 H13D 107.9 . . ? C131 C134 H13E 109.5 . . ? C131 C134 H13F 109.5 . . ? H13E C134 H13F 109.5 . . ? C131 C134 H13G 109.5 . . ? H13E C134 H13G 109.5 . . ? H13F C134 H13G 109.5 . . ? C131 N131 H13H 109.5 . . ? C131 N131 H13I 109.5 . . ? H13H N131 H13I 109.5 . . ? C131 N131 H13J 109.5 . . ? H13H N131 H13J 109.5 . . ? H13I N131 H13J 109.5 . . ? C132 O132 H132 109.5 . . ? C133 O133 H133 109.5 . . ? C233 C231 N231 108.6(10) . . ? C233 C231 C232 118.0(10) . . ? N231 C231 C232 106.4(8) . . ? C233 C231 C234 106.6(8) . . ? N231 C231 C234 107.0(9) . . ? C232 C231 C234 109.8(9) . . ? O232 C232 C231 110.4(10) . . ? O232 C232 H23A 109.6 . . ? C231 C232 H23A 109.6 . . ? O232 C232 H23B 109.6 . . ? C231 C232 H23B 109.6 . . ? H23A C232 H23B 108.1 . . ? O233 C233 C231 106.2(9) . . ? O233 C233 H23C 110.5 . . ? C231 C233 H23C 110.5 . . ? O233 C233 H23D 110.5 . . ? C231 C233 H23D 110.5 . . ? H23C C233 H23D 108.7 . . ? C231 C234 H23E 109.5 . . ? C231 C234 H23F 109.5 . . ? H23E C234 H23F 109.5 . . ? C231 C234 H23G 109.5 . . ? H23E C234 H23G 109.5 . . ? H23F C234 H23G 109.5 . . ? C231 N231 H23H 109.5 . . ? C231 N231 H23I 109.5 . . ? H23H N231 H23I 109.5 . . ? C231 N231 H23J 109.5 . . ? H23H N231 H23J 109.5 . . ? H23I N231 H23J 109.5 . . ? C232 O232 H232 109.5 . . ? C233 O233 H233 109.5 . . ? C333 C331 C332 124.7(9) . . ? C333 C331 N331 106.1(8) . . ? C332 C331 N331 106.2(8) . . ? C333 C331 C334 107.1(9) . . ? C332 C331 C334 106.8(10) . . ? N331 C331 C334 104.3(10) . . ? O332 C332 C331 108.8(8) . . ? O332 C332 H33A 109.9 . . ? C331 C332 H33A 109.9 . . ? O332 C332 H33B 109.9 . . ? C331 C332 H33B 109.9 . . ? H33A C332 H33B 108.3 . . ? O333 C333 C331 112.2(9) . . ? O333 C333 H33C 109.2 . . ? C331 C333 H33C 109.2 . . ? O333 C333 H33D 109.2 . . ? C331 C333 H33D 109.2 . . ? H33C C333 H33D 107.9 . . ? C331 C334 H33E 109.5 . . ? C331 C334 H33F 109.5 . . ? H33E C334 H33F 109.5 . . ? C331 C334 H33G 109.5 . . ? H33E C334 H33G 109.5 . . ? H33F C334 H33G 109.5 . . ? C331 N331 H33H 109.5 . . ? C331 N331 H33I 109.5 . . ? H33H N331 H33I 109.5 . . ? C331 N331 H33J 109.5 . . ? H33H N331 H33J 109.5 . . ? H33I N331 H33J 109.5 . . ? C332 O332 H332 109.5 . . ? C333 O333 H333 109.5 . . ? C433 C431 N431 108.7(11) . . ? C433 C431 C432 119.6(11) . . ? N431 C431 C432 106.0(9) . . ? C433 C431 C434 108.4(10) . . ? N431 C431 C434 105.5(11) . . ? C432 C431 C434 107.8(11) . . ? O432 C432 C431 110.2(10) . . ? O432 C432 H43A 109.6 . . ? C431 C432 H43A 109.6 . . ? O432 C432 H43B 109.6 . . ? C431 C432 H43B 109.6 . . ? H43A C432 H43B 108.1 . . ? O433 C433 C431 109.0(11) . . ? O433 C433 H43C 109.9 . . ? C431 C433 H43C 109.9 . . ? O433 C433 H43D 109.9 . . ? C431 C433 H43D 109.9 . . ? H43C C433 H43D 108.3 . . ? C431 C434 H43E 109.5 . . ? C431 C434 H43F 109.5 . . ? H43E C434 H43F 109.5 . . ? C431 C434 H43G 109.5 . . ? H43E C434 H43G 109.5 . . ? H43F C434 H43G 109.5 . . ? C431 N431 H43H 109.5 . . ? C431 N431 H43I 109.5 . . ? H43H N431 H43I 109.5 . . ? C431 N431 H43J 109.5 . . ? H43H N431 H43J 109.5 . . ? H43I N431 H43J 109.5 . . ? C432 O432 H432 109.5 . . ? C433 O433 H433 109.5 . . ? H101 O101 H102 107.6 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O7 H7 O14 0.84 1.83 2.665(3) 174.9 1_545 O8 H8 O16 0.84 1.84 2.676(3) 173.1 1_554 O9 H9 O11 0.84 1.91 2.721(3) 162.8 1_544 O10 H10 O8 0.84 1.99 2.815(3) 165.2 1_645 O17 H17 O4 0.84 1.87 2.659(3) 155.7 1_566 O18 H18 O20 0.84 1.97 2.783(3) 163.0 1_465 O19 H19 O1 0.84 1.83 2.665(3) 174.6 1_565 O20 H20 O3 0.84 1.87 2.687(3) 164.8 1_556 N121 H12J O13 0.91 1.91 2.745(18) 152.0 1_655 N121 H12H O132 0.91 2.26 2.891(19) 126.3 1_556 N121 H12I O9 0.91 1.99 2.875(16) 163.4 1_566 O122 H122 O7 0.84 1.87 2.63(2) 149.2 1_655 O123 H123 O101 0.84 2.05 2.838(10) 156.6 1_655 N221 H22I O232 0.91 1.95 2.85(3) 166.5 1_556 N221 H22J O9 0.91 2.08 2.872(14) 145.2 1_566 N221 H22H O13 0.91 1.95 2.829(18) 162.0 1_655 O222 H222 O7 0.84 2.03 2.79(3) 149.0 1_655 O223 H223 O101 0.84 2.12 2.713(12) 127.1 1_565 N321 H32H O333 0.91 1.86 2.74(2) 162.4 . N321 H32I O322 0.91 2.24 2.712(16) 111.9 . N321 H32J O7 0.91 2.00 2.815(14) 147.9 1_655 O322 H322 O9 0.84 1.84 2.618(12) 152.5 1_566 O323 H323 O14 0.84 2.41 2.846(18) 113.3 . N131 H13I O19 0.91 2.21 2.893(15) 131.2 . N131 H13H O122 0.91 2.12 2.91(3) 144.6 . N131 H13J O2 0.91 2.43 3.251(14) 150.1 1_655 N231 H23H O222 0.91 1.65 2.51(3) 157.9 . N231 H23I O19 0.91 1.95 2.82(3) 160.3 . O232 H232 O17 0.84 1.90 2.65(4) 146.8 1_644 O233 H233 O10 0.84 2.00 2.689(14) 138.5 . N331 H33H O322 0.91 2.02 2.87(2) 155.6 1_554 N331 H33I O6 0.91 1.85 2.755(14) 172.2 . N331 H33J O17 0.91 2.06 2.928(14) 160.3 1_644 O333 H333 O19 0.84 2.03 2.765(14) 146.1 . N431 H43H O19 0.91 1.90 2.78(5) 160.8 . N431 H43I O432 0.91 2.22 2.73(4) 115.4 . O101 H101 O332 0.85 1.83 2.564(13) 143.1 . O101 H102 O20 0.85 2.58 3.342(8) 149.7 . _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.403 _refine_diff_density_min -0.262 _refine_diff_density_rms 0.049 #===END data_1d #TrackingRef 'pentaborates.CIF' _database_code_depnum_ccdc_archive 'CCDC 764923' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C7 H14 B5 N O11' _chemical_formula_weight 342.24 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' _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 9.3330(3) _cell_length_b 15.9080(5) _cell_length_c 9.8979(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.291(2) _cell_angle_gamma 90.00 _cell_volume 1469.52(8) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 3418 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.547 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 0.136 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9839 _exptl_absorpt_correction_T_max 0.9973 _exptl_absorpt_process_details 'SADABS 2007/2 (Sheldrick, G.M., 2007)' _exptl_special_details ; SADABS was used to perform the Absorption correction Parameter refinement on 15793 reflections reduced R(int) from 0.0966 to 0.0403 Ratio of minimum to maximum apparent transmission: 0.886277 The given Tmin and Tmax were generated using the SHELX SIZE command ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius APEX II CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18472 _diffrn_reflns_av_R_equivalents 0.0433 _diffrn_reflns_av_sigmaI/netI 0.0337 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.26 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3359 _reflns_number_gt 2600 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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^)+(0.0220P)^2^+2.1876P] 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 3359 _refine_ls_number_parameters 245 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0797 _refine_ls_R_factor_gt 0.0568 _refine_ls_wR_factor_ref 0.1230 _refine_ls_wR_factor_gt 0.1091 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 1.100 _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 0.2869(2) 0.13601(15) 0.8950(2) 0.0184(5) Uani 1 1 d . . . B2 B 0.0318(2) 0.08979(15) 0.9005(2) 0.0178(5) Uani 1 1 d . . . B3 B 0.1112(3) 0.19022(15) 1.0630(2) 0.0196(5) Uani 1 1 d . . . B4 B 0.5460(3) 0.10059(16) 0.8886(3) 0.0220(5) Uani 1 1 d . . . B5 B 0.4590(3) 0.2092(2) 0.7446(3) 0.0326(6) Uani 1 1 d . . . O1 O 0.16702(15) 0.08278(9) 0.85068(15) 0.0195(3) Uani 1 1 d . . . O2 O 0.00002(15) 0.14730(9) 1.00059(15) 0.0202(3) Uani 1 1 d . . . O3 O 0.24807(15) 0.18290(10) 1.01691(15) 0.0213(3) Uani 1 1 d . . . O4 O 0.41015(15) 0.08159(9) 0.92690(15) 0.0199(3) Uani 1 1 d . . . O5 O 0.57346(17) 0.16564(12) 0.80153(18) 0.0337(4) Uani 1 1 d . . . O6 O 0.32314(15) 0.19478(10) 0.78631(15) 0.0223(3) Uani 1 1 d . . . O7 O -0.06965(15) 0.03841(10) 0.84770(15) 0.0226(3) Uani 1 1 d . . . H7 H -0.1494 0.0496 0.8823 0.034 Uiso 1 1 calc R . . O8 O 0.07814(16) 0.23855(11) 1.17106(17) 0.0286(4) Uani 1 1 d . . . H8 H 0.1536 0.2588 1.2043 0.043 Uiso 1 1 calc R . . O9 O 0.65967(16) 0.05459(11) 0.93313(18) 0.0284(4) Uani 1 1 d . . . H9 H 0.6301 0.0138 0.9790 0.043 Uiso 1 1 calc R . . O10 O 0.4904(2) 0.26740(19) 0.6498(3) 0.0773(10) Uani 1 1 d . . . H10 H 0.4143 0.2845 0.6135 0.116 Uiso 1 1 calc R . . C11 C 0.7994(3) 0.02639(15) 0.4743(2) 0.0288(5) Uani 1 1 d D . . C12 C 0.7874(3) 0.09705(17) 0.5547(3) 0.0393(7) Uani 1 1 d . . . H12 H 0.7798 0.0912 0.6500 0.047 Uiso 1 1 calc R . . C13 C 0.7863(3) 0.17575(17) 0.4974(3) 0.0359(6) Uani 1 1 d . . . H13 H 0.7764 0.2241 0.5531 0.043 Uiso 1 1 calc R . . C14 C 0.7994(3) 0.18484(16) 0.3599(3) 0.0338(6) Uani 1 1 d . . . H14 H 0.8012 0.2391 0.3197 0.041 Uiso 1 1 calc R . . C15 C 0.8099(3) 0.11369(16) 0.2821(3) 0.0319(5) Uani 1 1 d . . . H15 H 0.8181 0.1183 0.1867 0.038 Uiso 1 1 calc R . . N11 N 0.8087(2) 0.03789(12) 0.34041(19) 0.0244(4) Uani 1 1 d . . . H11 H 0.8142 -0.0068 0.2882 0.029 Uiso 1 1 calc R . . C16 C 0.8120(10) -0.0607(11) 0.531(3) 0.0294(11) Uani 0.319(3) 1 d PD . . H16A H 0.8993 -0.0641 0.5881 0.035 Uiso 0.319(3) 1 calc PR . . H16B H 0.8229 -0.1011 0.4559 0.035 Uiso 0.319(3) 1 calc PR . . C17 C 0.6834(10) -0.0858(6) 0.6150(9) 0.0325(14) Uani 0.319(3) 1 d PD . . H17A H 0.6966 -0.1439 0.6489 0.039 Uiso 0.319(3) 1 calc PR . . H17B H 0.6755 -0.0479 0.6939 0.039 Uiso 0.319(3) 1 calc PR . . O11 O 0.5530(7) -0.0813(5) 0.5354(8) 0.0433(9) Uani 0.319(3) 1 d PD . . H11A H 0.4818 -0.0871 0.5862 0.065 Uiso 0.319(3) 1 calc PR . . C116 C 0.7710(10) -0.0634(8) 0.5197(18) 0.0294(11) Uani 0.342(3) 1 d PD . . H11B H 0.8219 -0.1007 0.4559 0.035 Uiso 0.342(3) 1 calc PR . . H11C H 0.8185 -0.0704 0.6087 0.035 Uiso 0.342(3) 1 calc PR . . C117 C 0.6201(11) -0.0980(6) 0.5337(9) 0.0325(14) Uani 0.342(3) 1 d PD . . H11D H 0.5658 -0.0879 0.4491 0.039 Uiso 0.342(3) 1 calc PR . . H11E H 0.6244 -0.1595 0.5490 0.039 Uiso 0.342(3) 1 calc PR . . O111 O 0.5472(6) -0.0582(4) 0.6454(6) 0.0433(9) Uani 0.342(3) 1 d PD . . H111 H 0.6056 -0.0285 0.6892 0.065 Uiso 0.342(3) 1 calc PR . . C216 C 0.8146(11) -0.0615(10) 0.526(3) 0.0294(11) Uani 0.339(4) 1 d PD . . H21A H 0.8767 -0.0631 0.6076 0.035 Uiso 0.339(4) 1 calc PR . . H21B H 0.8559 -0.0988 0.4565 0.035 Uiso 0.339(4) 1 calc PR . . C217 C 0.6631(10) -0.0878(6) 0.5602(11) 0.0325(14) Uani 0.339(4) 1 d PD . . H21C H 0.6637 -0.1465 0.5938 0.039 Uiso 0.339(4) 1 calc PR . . H21D H 0.6259 -0.0514 0.6331 0.039 Uiso 0.339(4) 1 calc PR . . O211 O 0.5694(6) -0.0818(4) 0.4430(7) 0.0433(9) Uani 0.339(4) 1 d PD . . H211 H 0.5426 -0.0318 0.4331 0.065 Uiso 0.339(4) 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B1 0.0144(10) 0.0199(12) 0.0209(11) -0.0001(9) 0.0008(9) -0.0012(9) B2 0.0159(10) 0.0190(11) 0.0186(11) 0.0025(9) 0.0006(9) 0.0022(9) B3 0.0181(11) 0.0201(12) 0.0206(11) 0.0011(10) -0.0005(9) 0.0009(9) B4 0.0166(11) 0.0255(13) 0.0240(12) 0.0017(10) 0.0017(9) -0.0009(10) B5 0.0183(12) 0.0423(17) 0.0373(15) 0.0182(13) -0.0015(11) -0.0032(11) O1 0.0157(7) 0.0217(8) 0.0213(7) -0.0033(6) 0.0017(6) -0.0003(6) O2 0.0150(7) 0.0221(8) 0.0236(8) -0.0035(6) -0.0001(6) 0.0006(6) O3 0.0155(7) 0.0238(8) 0.0245(8) -0.0052(6) 0.0010(6) -0.0004(6) O4 0.0151(7) 0.0192(7) 0.0254(8) 0.0024(6) 0.0015(6) 0.0009(6) O5 0.0163(8) 0.0447(11) 0.0402(10) 0.0224(9) 0.0014(7) -0.0010(7) O6 0.0168(7) 0.0244(8) 0.0257(8) 0.0063(6) 0.0003(6) 0.0006(6) O7 0.0159(7) 0.0266(8) 0.0253(8) -0.0052(7) 0.0023(6) -0.0022(6) O8 0.0196(8) 0.0350(10) 0.0312(9) -0.0130(7) 0.0014(7) -0.0022(7) O9 0.0156(7) 0.0318(9) 0.0379(10) 0.0140(8) 0.0033(7) 0.0011(7) O10 0.0200(10) 0.117(2) 0.0953(19) 0.0861(18) 0.0006(11) 0.0007(12) C11 0.0334(13) 0.0267(12) 0.0261(12) -0.0032(10) -0.0065(10) 0.0040(10) C12 0.0564(17) 0.0356(15) 0.0259(13) -0.0060(11) -0.0099(12) 0.0096(13) C13 0.0407(15) 0.0281(13) 0.0388(14) -0.0125(11) -0.0050(12) 0.0025(11) C14 0.0352(14) 0.0236(12) 0.0427(15) 0.0005(11) 0.0075(11) -0.0010(10) C15 0.0363(13) 0.0312(13) 0.0283(12) 0.0015(11) 0.0085(10) -0.0019(11) N11 0.0238(9) 0.0222(10) 0.0273(10) -0.0070(8) 0.0029(8) -0.0003(8) C16 0.025(3) 0.0294(14) 0.034(2) 0.0033(13) -0.011(3) 0.009(2) C17 0.047(4) 0.022(2) 0.029(4) 0.001(3) -0.006(3) -0.006(2) O11 0.0330(17) 0.0391(19) 0.058(2) 0.004(2) 0.000(2) -0.0030(15) C116 0.025(3) 0.0294(14) 0.034(2) 0.0033(13) -0.011(3) 0.009(2) C117 0.047(4) 0.022(2) 0.029(4) 0.001(3) -0.006(3) -0.006(2) O111 0.0330(17) 0.0391(19) 0.058(2) 0.004(2) 0.000(2) -0.0030(15) C216 0.025(3) 0.0294(14) 0.034(2) 0.0033(13) -0.011(3) 0.009(2) C217 0.047(4) 0.022(2) 0.029(4) 0.001(3) -0.006(3) -0.006(2) O211 0.0330(17) 0.0391(19) 0.058(2) 0.004(2) 0.000(2) -0.0030(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 O3 1.466(3) . ? B1 O6 1.466(3) . ? B1 O1 1.468(3) . ? B1 O4 1.473(3) . ? B2 O7 1.354(3) . ? B2 O1 1.362(3) . ? B2 O2 1.382(3) . ? B3 O8 1.354(3) . ? B3 O3 1.363(3) . ? B3 O2 1.385(3) . ? B4 O4 1.359(3) . ? B4 O9 1.360(3) . ? B4 O5 1.372(3) . ? B5 O10 1.352(3) . ? B5 O6 1.355(3) . ? B5 O5 1.390(3) . ? O7 H7 0.8400 . ? O8 H8 0.8400 . ? O9 H9 0.8400 . ? O10 H10 0.8400 . ? C11 N11 1.341(3) . ? C11 C12 1.382(3) . ? C11 C216 1.497(12) . ? C11 C16 1.500(12) . ? C11 C116 1.522(11) . ? C12 C13 1.375(4) . ? C12 H12 0.9500 . ? C13 C14 1.375(4) . ? C13 H13 0.9500 . ? C14 C15 1.373(4) . ? C14 H14 0.9500 . ? C15 N11 1.337(3) . ? C15 H15 0.9500 . ? N11 H11 0.8800 . ? C16 C17 1.516(9) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 O11 1.448(8) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? O11 H11A 0.8400 . ? C116 C117 1.519(9) . ? C116 H11B 0.9900 . ? C116 H11C 0.9900 . ? C117 O111 1.447(8) . ? C117 H11D 0.9900 . ? C117 H11E 0.9900 . ? O111 H111 0.8400 . ? C216 C217 1.514(8) . ? C216 H21A 0.9900 . ? C216 H21B 0.9900 . ? C217 O211 1.452(9) . ? C217 H21C 0.9900 . ? C217 H21D 0.9900 . ? O211 H211 0.8400 . ? 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 O3 B1 O6 109.78(18) . . ? O3 B1 O1 110.37(17) . . ? O6 B1 O1 109.08(17) . . ? O3 B1 O4 108.59(17) . . ? O6 B1 O4 110.46(17) . . ? O1 B1 O4 108.56(17) . . ? O7 B2 O1 117.3(2) . . ? O7 B2 O2 121.62(19) . . ? O1 B2 O2 121.08(19) . . ? O8 B3 O3 122.1(2) . . ? O8 B3 O2 117.29(19) . . ? O3 B3 O2 120.7(2) . . ? O4 B4 O9 121.1(2) . . ? O4 B4 O5 121.4(2) . . ? O9 B4 O5 117.5(2) . . ? O10 B5 O6 122.3(2) . . ? O10 B5 O5 117.0(2) . . ? O6 B5 O5 120.7(2) . . ? B2 O1 B1 123.43(17) . . ? B2 O2 B3 118.89(17) . . ? B3 O3 B1 123.71(17) . . ? B4 O4 B1 122.55(18) . . ? B4 O5 B5 119.00(19) . . ? B5 O6 B1 123.43(18) . . ? B2 O7 H7 109.5 . . ? B3 O8 H8 109.5 . . ? B4 O9 H9 109.5 . . ? B5 O10 H10 109.5 . . ? N11 C11 C12 117.6(2) . . ? N11 C11 C216 117.4(11) . . ? C12 C11 C216 124.7(11) . . ? N11 C11 C16 119.4(12) . . ? C12 C11 C16 122.8(12) . . ? N11 C11 C116 115.6(7) . . ? C12 C11 C116 125.4(7) . . ? C13 C12 C11 120.2(2) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C12 C13 C14 120.3(2) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? C15 C14 C13 118.4(2) . . ? C15 C14 H14 120.8 . . ? C13 C14 H14 120.8 . . ? N11 C15 C14 120.0(2) . . ? N11 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C15 N11 C11 123.4(2) . . ? C15 N11 H11 118.3 . . ? C11 N11 H11 118.3 . . ? C11 C16 C17 112.8(10) . . ? C11 C16 H16A 109.0 . . ? C17 C16 H16A 109.0 . . ? C11 C16 H16B 109.0 . . ? C17 C16 H16B 109.0 . . ? H16A C16 H16B 107.8 . . ? O11 C17 C16 110.8(9) . . ? O11 C17 H17A 109.5 . . ? C16 C17 H17A 109.5 . . ? O11 C17 H17B 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 108.1 . . ? C17 O11 H11A 109.5 . . ? C117 C116 C11 122.0(8) . . ? C117 C116 H11B 106.8 . . ? C11 C116 H11B 106.8 . . ? C117 C116 H11C 106.8 . . ? C11 C116 H11C 106.8 . . ? H11B C116 H11C 106.7 . . ? O111 C117 C116 110.6(9) . . ? O111 C117 H11D 109.5 . . ? C116 C117 H11D 109.5 . . ? O111 C117 H11E 109.5 . . ? C116 C117 H11E 109.5 . . ? H11D C117 H11E 108.1 . . ? C117 O111 H111 109.5 . . ? C11 C216 C217 104.4(8) . . ? C11 C216 H21A 110.9 . . ? C217 C216 H21A 110.9 . . ? C11 C216 H21B 110.9 . . ? C217 C216 H21B 110.9 . . ? H21A C216 H21B 108.9 . . ? O211 C217 C216 111.3(10) . . ? O211 C217 H21C 109.4 . . ? C216 C217 H21C 109.4 . . ? O211 C217 H21D 109.4 . . ? C216 C217 H21D 109.4 . . ? H21C C217 H21D 108.0 . . ? C217 O211 H211 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O7 H7 O9 0.84 1.86 2.681(2) 166.8 1_455 O8 H8 O6 0.84 1.92 2.762(2) 178.1 4_566 O9 H9 O4 0.84 1.82 2.654(2) 172.0 3_657 O10 H10 O3 0.84 1.89 2.728(2) 174.5 4_565 N11 H11 O1 0.88 1.84 2.705(2) 167.2 3_656 O211 H211 O111 0.84 1.83 2.628(9) 157.9 3_656 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.705 _refine_diff_density_min -0.662 _refine_diff_density_rms 0.061 #===END data_1e #TrackingRef 'pentaborates.CIF' _database_code_depnum_ccdc_archive 'CCDC 764924' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H18 B5 N O11' _chemical_formula_weight 334.26 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' _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 9.0191(2) _cell_length_b 17.8062(5) _cell_length_c 9.4544(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.373(2) _cell_angle_gamma 90.00 _cell_volume 1498.07(7) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 3508 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.482 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 696 _exptl_absorpt_coefficient_mu 0.131 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9693 _exptl_absorpt_correction_T_max 0.9974 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2003)' _exptl_special_details ; SADABS was used to perform the Absorption correction Parameter refinement on 19791 reflections reduced R(int) from 0.1690 to 0.0887 Ratio of minimum to maximum apparent transmission: 0.705970 The given Tmin and Tmax were generated using the SHELX SIZE command ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type ; Bruker-Nonius APEX II CCD camera on \k-goniostat ; _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16175 _diffrn_reflns_av_R_equivalents 0.0488 _diffrn_reflns_av_sigmaI/netI 0.0392 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3425 _reflns_number_gt 2844 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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^)+(0.0010P)^2^+1.7042P] 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 3425 _refine_ls_number_parameters 213 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0627 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_ref 0.0984 _refine_ls_wR_factor_gt 0.0910 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _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 0.3016(2) 0.13726(12) 0.3835(2) 0.0153(4) Uani 1 1 d . . . B2 B 0.1416(2) 0.17166(11) 0.5651(2) 0.0157(4) Uani 1 1 d . . . B3 B 0.0395(2) 0.09021(12) 0.3728(2) 0.0164(4) Uani 1 1 d . . . B4 B 0.5616(2) 0.08865(12) 0.3876(2) 0.0167(4) Uani 1 1 d . . . B5 B 0.4842(2) 0.19598(12) 0.2449(2) 0.0169(4) Uani 1 1 d . . . O1 O 0.27205(13) 0.17731(7) 0.51181(13) 0.0169(3) Uani 1 1 d . . . O2 O 0.02518(13) 0.12678(7) 0.49882(13) 0.0198(3) Uani 1 1 d . . . O3 O 0.16814(13) 0.09611(7) 0.31506(12) 0.0167(3) Uani 1 1 d . . . O4 O 0.42361(13) 0.08252(7) 0.42683(13) 0.0163(3) Uani 1 1 d . . . O5 O 0.59632(13) 0.14659(7) 0.30256(14) 0.0212(3) Uani 1 1 d . . . O6 O 0.34430(13) 0.19143(7) 0.28043(13) 0.0172(3) Uani 1 1 d . . . O7 O 0.11794(14) 0.21016(7) 0.68281(13) 0.0201(3) Uani 1 1 d . . . H7 H 0.1924 0.2378 0.7111 0.030 Uiso 1 1 calc R . . O8 O -0.07427(14) 0.04839(8) 0.30111(14) 0.0225(3) Uani 1 1 d . . . H8 H -0.1461 0.0475 0.3476 0.034 Uiso 1 1 calc R . . O9 O 0.67141(13) 0.03654(7) 0.42816(14) 0.0209(3) Uani 1 1 d . . . H9 H 0.6385 0.0029 0.4771 0.031 Uiso 1 1 calc R . . O10 O 0.52016(14) 0.24785(8) 0.15080(15) 0.0233(3) Uani 1 1 d . . . H10 H 0.4417 0.2696 0.1110 0.035 Uiso 1 1 calc R . . C11 C -0.2671(2) 0.14811(12) -0.0003(2) 0.0240(4) Uani 1 1 d . . . H11A H -0.2697 0.2028 -0.0197 0.029 Uiso 1 1 calc R . . H11B H -0.2525 0.1399 0.1046 0.029 Uiso 1 1 calc R . . C12 C -0.4106(2) 0.11034(13) -0.0739(2) 0.0310(5) Uani 1 1 d . . . H12A H -0.4938 0.1471 -0.0925 0.037 Uiso 1 1 calc R . . H12B H -0.4404 0.0694 -0.0135 0.037 Uiso 1 1 calc R . . C13 C -0.3735(2) 0.07883(12) -0.2158(2) 0.0303(5) Uani 1 1 d . . . H13A H -0.3822 0.0234 -0.2178 0.036 Uiso 1 1 calc R . . H13B H -0.4427 0.0997 -0.2984 0.036 Uiso 1 1 calc R . . C14 C -0.2127(2) 0.10275(12) -0.2210(2) 0.0274(4) Uani 1 1 d . . . H14A H -0.1590 0.0641 -0.2687 0.033 Uiso 1 1 calc R . . H14B H -0.2099 0.1510 -0.2724 0.033 Uiso 1 1 calc R . . C15 C -0.0004(2) 0.15254(11) -0.0370(2) 0.0209(4) Uani 1 1 d . . . H15A H 0.0157 0.1713 0.0629 0.025 Uiso 1 1 calc R . . H15B H -0.0064 0.1966 -0.1016 0.025 Uiso 1 1 calc R . . C16 C 0.1322(2) 0.10445(11) -0.0594(2) 0.0221(4) Uani 1 1 d . . . H16A H 0.1141 0.0835 -0.1576 0.027 Uiso 1 1 calc R . . H16B H 0.2236 0.1360 -0.0497 0.027 Uiso 1 1 calc R . . N11 N -0.14484(17) 0.11071(9) -0.06523(16) 0.0190(3) Uani 1 1 d . . . H11 H -0.1293 0.0629 -0.0259 0.023 Uiso 1 1 calc R . . O11 O 0.15612(15) 0.04457(7) 0.04168(14) 0.0230(3) Uani 1 1 d . . . H11C H 0.1649 0.0621 0.1252 0.035 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 0.0143(9) 0.0167(10) 0.0153(9) 0.0009(7) 0.0036(7) -0.0009(7) B2 0.0168(9) 0.0145(10) 0.0162(9) 0.0026(7) 0.0043(7) 0.0019(7) B3 0.0164(9) 0.0148(10) 0.0186(9) 0.0009(7) 0.0042(7) 0.0027(7) B4 0.0145(9) 0.0198(11) 0.0161(9) -0.0010(8) 0.0030(7) -0.0013(7) B5 0.0167(9) 0.0183(10) 0.0165(9) -0.0007(7) 0.0046(7) -0.0006(8) O1 0.0159(6) 0.0184(7) 0.0170(6) -0.0030(5) 0.0050(5) -0.0015(5) O2 0.0166(6) 0.0243(7) 0.0201(6) -0.0038(5) 0.0078(5) -0.0036(5) O3 0.0145(6) 0.0200(7) 0.0159(6) -0.0021(5) 0.0033(4) -0.0011(5) O4 0.0156(6) 0.0160(7) 0.0180(6) 0.0030(5) 0.0046(5) 0.0009(5) O5 0.0155(6) 0.0228(7) 0.0266(7) 0.0083(5) 0.0073(5) 0.0023(5) O6 0.0148(6) 0.0191(7) 0.0187(6) 0.0033(5) 0.0053(5) 0.0014(5) O7 0.0196(6) 0.0224(7) 0.0193(6) -0.0031(5) 0.0065(5) -0.0034(5) O8 0.0159(6) 0.0276(8) 0.0251(7) -0.0070(6) 0.0063(5) -0.0042(5) O9 0.0156(6) 0.0212(7) 0.0273(7) 0.0076(5) 0.0074(5) 0.0023(5) O10 0.0182(6) 0.0238(8) 0.0293(7) 0.0107(6) 0.0086(5) 0.0031(5) C11 0.0238(9) 0.0259(11) 0.0230(9) -0.0049(8) 0.0058(7) 0.0023(8) C12 0.0259(10) 0.0345(13) 0.0320(11) -0.0033(9) 0.0029(8) -0.0032(9) C13 0.0279(10) 0.0284(12) 0.0306(11) -0.0071(9) -0.0075(8) 0.0063(9) C14 0.0354(11) 0.0295(11) 0.0160(9) -0.0040(8) 0.0002(8) 0.0036(9) C15 0.0254(9) 0.0169(10) 0.0210(9) -0.0003(7) 0.0056(7) -0.0022(7) C16 0.0250(9) 0.0225(10) 0.0201(9) 0.0017(7) 0.0074(7) -0.0004(8) N11 0.0236(8) 0.0175(8) 0.0160(7) 0.0002(6) 0.0037(6) 0.0007(6) O11 0.0312(7) 0.0199(7) 0.0173(6) -0.0001(5) 0.0017(5) 0.0009(6) _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 O3 1.466(2) . ? B1 O6 1.466(2) . ? B1 O1 1.469(2) . ? B1 O4 1.477(2) . ? B2 O7 1.354(2) . ? B2 O1 1.357(2) . ? B2 O2 1.385(2) . ? B3 O8 1.356(2) . ? B3 O3 1.364(2) . ? B3 O2 1.382(2) . ? B4 O4 1.359(2) . ? B4 O9 1.366(2) . ? B4 O5 1.375(2) . ? B5 O10 1.358(2) . ? B5 O6 1.360(2) . ? B5 O5 1.383(2) . ? O7 H7 0.8400 . ? O8 H8 0.8400 . ? O9 H9 0.8400 . ? O10 H10 0.8400 . ? C11 N11 1.502(2) . ? C11 C12 1.523(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.540(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.520(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 N11 1.507(2) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 N11 1.487(2) . ? C15 C16 1.513(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 O11 1.424(2) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? N11 H11 0.9300 . ? O11 H11C 0.8400 . ? 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 O3 B1 O6 108.75(14) . . ? O3 B1 O1 111.16(14) . . ? O6 B1 O1 109.39(15) . . ? O3 B1 O4 108.28(15) . . ? O6 B1 O4 110.72(14) . . ? O1 B1 O4 108.55(14) . . ? O7 B2 O1 121.99(17) . . ? O7 B2 O2 117.06(15) . . ? O1 B2 O2 120.94(16) . . ? O8 B3 O3 117.78(16) . . ? O8 B3 O2 121.32(16) . . ? O3 B3 O2 120.89(16) . . ? O4 B4 O9 121.55(17) . . ? O4 B4 O5 121.70(17) . . ? O9 B4 O5 116.73(16) . . ? O10 B5 O6 122.16(17) . . ? O10 B5 O5 116.97(16) . . ? O6 B5 O5 120.86(16) . . ? B2 O1 B1 123.73(14) . . ? B3 O2 B2 119.42(14) . . ? B3 O3 B1 123.54(14) . . ? B4 O4 B1 123.03(14) . . ? B4 O5 B5 119.07(14) . . ? B5 O6 B1 123.92(14) . . ? B2 O7 H7 109.5 . . ? B3 O8 H8 109.5 . . ? B4 O9 H9 109.5 . . ? B5 O10 H10 109.5 . . ? N11 C11 C12 104.11(15) . . ? N11 C11 H11A 110.9 . . ? C12 C11 H11A 110.9 . . ? N11 C11 H11B 110.9 . . ? C12 C11 H11B 110.9 . . ? H11A C11 H11B 109.0 . . ? C11 C12 C13 105.62(16) . . ? C11 C12 H12A 110.6 . . ? C13 C12 H12A 110.6 . . ? C11 C12 H12B 110.6 . . ? C13 C12 H12B 110.6 . . ? H12A C12 H12B 108.7 . . ? C14 C13 C12 105.69(16) . . ? C14 C13 H13A 110.6 . . ? C12 C13 H13A 110.6 . . ? C14 C13 H13B 110.6 . . ? C12 C13 H13B 110.6 . . ? H13A C13 H13B 108.7 . . ? N11 C14 C13 103.41(15) . . ? N11 C14 H14A 111.1 . . ? C13 C14 H14A 111.1 . . ? N11 C14 H14B 111.1 . . ? C13 C14 H14B 111.1 . . ? H14A C14 H14B 109.0 . . ? N11 C15 C16 112.39(15) . . ? N11 C15 H15A 109.1 . . ? C16 C15 H15A 109.1 . . ? N11 C15 H15B 109.1 . . ? C16 C15 H15B 109.1 . . ? H15A C15 H15B 107.9 . . ? O11 C16 C15 111.52(15) . . ? O11 C16 H16A 109.3 . . ? C15 C16 H16A 109.3 . . ? O11 C16 H16B 109.3 . . ? C15 C16 H16B 109.3 . . ? H16A C16 H16B 108.0 . . ? C15 N11 C11 112.63(14) . . ? C15 N11 C14 115.27(14) . . ? C11 N11 C14 103.47(14) . . ? C15 N11 H11 108.4 . . ? C11 N11 H11 108.4 . . ? C14 N11 H11 108.4 . . ? C16 O11 H11C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O7 H7 O6 0.84 1.90 2.7343(17) 173.3 4_566 O8 H8 O9 0.84 1.93 2.7651(17) 170.6 1_455 O9 H9 O4 0.84 1.90 2.7370(17) 172.4 3_656 O10 H10 O1 0.84 1.91 2.7481(17) 175.8 4_565 N11 H11 O11 0.93 1.93 2.777(2) 150.1 3 O11 H11C O3 0.84 1.89 2.7282(17) 174.5 . _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.229 _refine_diff_density_min -0.246 _refine_diff_density_rms 0.055 #===END data_1f #TrackingRef 'pentaborates.CIF' _database_code_depnum_ccdc_archive 'CCDC 764925' #The structure was solved in C2, as there was only a pseudo mirror #plane which the borate anion almost fitted, but the disordered #cation would not. _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C7 H20 B5 N O11' _chemical_formula_weight 348.29 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 0.0000 '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 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0000 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 14.7118(3) _cell_length_b 11.4599(3) _cell_length_c 9.8194(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.911(2) _cell_angle_gamma 90.00 _cell_volume 1606.95(7) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 3593 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description Plate _exptl_crystal_colour 'Light Yellow' _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.440 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 728 _exptl_absorpt_coefficient_mu 0.125 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9286 _exptl_absorpt_correction_T_max 0.9802 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2003)' _exptl_special_details ; SADABS was used to perform the Absorption correction Parameter refinement on 11787 reflections reduced R(int) from 0.1703 to 0.0383 Ratio of minimum to maximum apparent transmission: 0.888353 The given Tmin and Tmax were generated using the SHELX SIZE command ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13456 _diffrn_reflns_av_R_equivalents 0.0430 _diffrn_reflns_av_sigmaI/netI 0.0293 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 27.48 _reflns_number_total 1932 _reflns_number_gt 1589 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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^)+(0.0854P)^2^+2.9712P] 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 ? _refine_ls_number_reflns 1932 _refine_ls_number_parameters 473 _refine_ls_number_restraints 1371 _refine_ls_R_factor_all 0.0721 _refine_ls_R_factor_gt 0.0599 _refine_ls_wR_factor_ref 0.1702 _refine_ls_wR_factor_gt 0.1566 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 0.878 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.19001(18) 0.6216(7) 0.4134(3) 0.0247(6) Uani 1 1 d U . . B2 B 0.2987(5) 0.5179(6) 0.6102(6) 0.0309(12) Uani 1 1 d U . . B3 B 0.2984(5) 0.7253(7) 0.6071(7) 0.0373(14) Uani 1 1 d U . . B4 B 0.12292(19) 0.6214(8) 0.1551(3) 0.0299(6) Uani 1 1 d U . . B5 B 0.0182(2) 0.6208(10) 0.3078(3) 0.0419(9) Uani 1 1 d U . . O1 O 0.2340(2) 0.5143(3) 0.4836(4) 0.0285(8) Uani 1 1 d U . . O2 O 0.32967(15) 0.6187(5) 0.6742(2) 0.0424(5) Uani 1 1 d U . . O3 O 0.2360(3) 0.7247(3) 0.4828(3) 0.0279(8) Uani 1 1 d U . . O4 O 0.19733(11) 0.6202(5) 0.26696(17) 0.0268(4) Uani 1 1 d U . . O5 O 0.03235(12) 0.6192(7) 0.17295(19) 0.0458(6) Uani 1 1 d U . . O6 O 0.09107(11) 0.6201(5) 0.42025(17) 0.0280(4) Uani 1 1 d U . . O7 O 0.3361(4) 0.4159(4) 0.6722(5) 0.0576(16) Uani 1 1 d U . . H7 H 0.3180 0.3600 0.6170 0.086 Uiso 1 1 calc R . . O8 O 0.3340(4) 0.8224(4) 0.6752(5) 0.0518(14) Uani 1 1 d U . . H8 H 0.3008 0.8799 0.6412 0.078 Uiso 1 1 calc R . . O9 O 0.13881(12) 0.6201(6) 0.02546(18) 0.0404(5) Uani 1 1 d U . . H9 H 0.0896 0.6389 -0.0337 0.061 Uiso 1 1 calc R . . O10 O -0.07180(15) 0.6196(11) 0.3158(2) 0.0876(14) Uani 1 1 d U . . H10 H -0.0762 0.6506 0.3915 0.131 Uiso 1 1 calc R . . N11 N 0.3632(14) 0.6211(18) 0.1289(19) 0.050(4) Uani 0.225(3) 1 d PDU A 1 H11 H 0.3132 0.6074 0.1694 0.059 Uiso 0.225(3) 1 calc PR A 1 C12 C 0.4538(17) 0.625(2) 0.242(2) 0.051(5) Uani 0.225(3) 1 d PDU A 1 H12A H 0.4639 0.5494 0.2931 0.061 Uiso 0.225(3) 1 calc PR A 1 H12B H 0.5075 0.6386 0.1996 0.061 Uiso 0.225(3) 1 calc PR A 1 C13 C 0.446(2) 0.721(2) 0.3399(17) 0.066(5) Uani 0.225(3) 1 d PDU A 1 H13A H 0.4012 0.6965 0.3958 0.079 Uiso 0.225(3) 1 calc PR A 1 H13B H 0.5074 0.7320 0.4061 0.079 Uiso 0.225(3) 1 calc PR A 1 C14 C 0.415(3) 0.835(2) 0.278(3) 0.079(6) Uani 0.225(3) 1 d PDU A 1 H14A H 0.4706 0.8772 0.2643 0.094 Uiso 0.225(3) 1 calc PR A 1 H14B H 0.3899 0.8801 0.3472 0.094 Uiso 0.225(3) 1 calc PR A 1 C15 C 0.341(2) 0.837(2) 0.139(3) 0.070(5) Uani 0.225(3) 1 d PDU A 1 H15A H 0.2777 0.8376 0.1579 0.084 Uiso 0.225(3) 1 calc PR A 1 H15B H 0.3478 0.9097 0.0877 0.084 Uiso 0.225(3) 1 calc PR A 1 C16 C 0.349(2) 0.7360(19) 0.050(2) 0.057(4) Uani 0.225(3) 1 d PDU A 1 H16A H 0.4018 0.7489 0.0060 0.069 Uiso 0.225(3) 1 calc PR A 1 H16B H 0.2910 0.7306 -0.0266 0.069 Uiso 0.225(3) 1 calc PR A 1 C17 C 0.3643(18) 0.5304(17) 0.019(2) 0.052(4) Uani 0.225(3) 1 d PDU A 1 H17A H 0.2995 0.5161 -0.0363 0.062 Uiso 0.225(3) 1 calc PR A 1 H17B H 0.4009 0.5600 -0.0465 0.062 Uiso 0.225(3) 1 calc PR A 1 C18 C 0.405(2) 0.4205(19) 0.081(3) 0.062(5) Uani 0.225(3) 1 d PDU A 1 H18A H 0.4706 0.4324 0.1349 0.075 Uiso 0.225(3) 1 calc PR A 1 H18B H 0.4048 0.3614 0.0070 0.075 Uiso 0.225(3) 1 calc PR A 1 O19 O 0.3420(12) 0.3819(13) 0.1783(17) 0.041(3) Uani 0.225(3) 1 d PDU A 1 H19 H 0.2868 0.3733 0.1306 0.061 Uiso 0.225(3) 1 calc PR A 1 N21 N 0.3551(19) 0.6455(15) 0.152(2) 0.049(4) Uani 0.221(7) 1 d PDU B 2 H21 H 0.3052 0.6262 0.1907 0.059 Uiso 0.221(7) 1 calc PR B 2 C22 C 0.4438(19) 0.625(2) 0.265(3) 0.046(5) Uani 0.221(7) 1 d PDU B 2 H22A H 0.4502 0.6850 0.3390 0.056 Uiso 0.221(7) 1 calc PR B 2 H22B H 0.4990 0.6297 0.2241 0.056 Uiso 0.221(7) 1 calc PR B 2 C23 C 0.4379(19) 0.505(2) 0.326(2) 0.058(5) Uani 0.221(7) 1 d PDU B 2 H23A H 0.5009 0.4693 0.3476 0.070 Uiso 0.221(7) 1 calc PR B 2 H23B H 0.4189 0.5136 0.4158 0.070 Uiso 0.221(7) 1 calc PR B 2 C24 C 0.371(2) 0.426(2) 0.233(3) 0.075(5) Uani 0.221(7) 1 d PDU B 2 H24A H 0.3082 0.4385 0.2491 0.090 Uiso 0.221(7) 1 calc PR B 2 H24B H 0.3898 0.3443 0.2597 0.090 Uiso 0.221(7) 1 calc PR B 2 C25 C 0.367(3) 0.4424(19) 0.077(3) 0.064(5) Uani 0.221(7) 1 d PDU B 2 H25A H 0.4264 0.4149 0.0579 0.076 Uiso 0.221(7) 1 calc PR B 2 H25B H 0.3158 0.3933 0.0218 0.076 Uiso 0.221(7) 1 calc PR B 2 C26 C 0.351(3) 0.5647(19) 0.030(2) 0.055(5) Uani 0.221(7) 1 d PDU B 2 H26A H 0.2887 0.5714 -0.0368 0.066 Uiso 0.221(7) 1 calc PR B 2 H26B H 0.3990 0.5880 -0.0204 0.066 Uiso 0.221(7) 1 calc PR B 2 C27 C 0.3408(17) 0.7692(16) 0.103(2) 0.053(5) Uani 0.221(7) 1 d PDU B 2 H27A H 0.3279 0.7711 -0.0011 0.063 Uiso 0.221(7) 1 calc PR B 2 H27B H 0.2858 0.8023 0.1305 0.063 Uiso 0.221(7) 1 calc PR B 2 C28 C 0.423(2) 0.840(3) 0.162(3) 0.068(5) Uani 0.221(7) 1 d PDU B 2 H28A H 0.4141 0.9194 0.1202 0.082 Uiso 0.221(7) 1 calc PR B 2 H28B H 0.4785 0.8052 0.1370 0.082 Uiso 0.221(7) 1 calc PR B 2 O29 O 0.441(2) 0.850(3) 0.323(3) 0.135(10) Uani 0.221(7) 1 d PDU B 2 H29 H 0.4988 0.8574 0.3581 0.203 Uiso 0.221(7) 1 calc PR B 2 N31 N 0.3552(14) 0.5912(11) 0.1603(18) 0.035(3) Uani 0.250(6) 1 d PDU C 3 H31 H 0.2988 0.6117 0.1811 0.043 Uiso 0.250(6) 1 calc PR C 3 C32 C 0.356(2) 0.6589(16) 0.0276(18) 0.048(4) Uani 0.250(6) 1 d PDU C 3 H32A H 0.4174 0.6478 0.0038 0.058 Uiso 0.250(6) 1 calc PR C 3 H32B H 0.3067 0.6289 -0.0513 0.058 Uiso 0.250(6) 1 calc PR C 3 C33 C 0.341(2) 0.7864(17) 0.048(2) 0.062(5) Uani 0.250(6) 1 d PDU C 3 H33A H 0.3881 0.8307 0.0134 0.074 Uiso 0.250(6) 1 calc PR C 3 H33B H 0.2786 0.8075 -0.0116 0.074 Uiso 0.250(6) 1 calc PR C 3 C34 C 0.3439(19) 0.8266(19) 0.191(2) 0.060(5) Uani 0.250(6) 1 d PDU C 3 H34A H 0.2823 0.8131 0.2121 0.072 Uiso 0.250(6) 1 calc PR C 3 H34B H 0.3567 0.9114 0.1971 0.072 Uiso 0.250(6) 1 calc PR C 3 C35 C 0.4198(19) 0.7623(17) 0.298(2) 0.058(5) Uani 0.250(6) 1 d PDU C 3 H35A H 0.4808 0.7985 0.2977 0.069 Uiso 0.250(6) 1 calc PR C 3 H35B H 0.4083 0.7759 0.3921 0.069 Uiso 0.250(6) 1 calc PR C 3 C36 C 0.4284(18) 0.6364(17) 0.280(2) 0.055(4) Uani 0.250(6) 1 d PDU C 3 H36A H 0.4234 0.5961 0.3671 0.065 Uiso 0.250(6) 1 calc PR C 3 H36B H 0.4910 0.6190 0.2641 0.065 Uiso 0.250(6) 1 calc PR C 3 C37 C 0.3497(13) 0.4640(14) 0.142(3) 0.063(4) Uani 0.250(6) 1 d PDU C 3 H37A H 0.3033 0.4322 0.1900 0.075 Uiso 0.250(6) 1 calc PR C 3 H37B H 0.3279 0.4457 0.0406 0.075 Uiso 0.250(6) 1 calc PR C 3 C38 C 0.4395(15) 0.408(2) 0.197(3) 0.067(5) Uani 0.250(6) 1 d PDU C 3 H38A H 0.4320 0.3225 0.1902 0.080 Uiso 0.250(6) 1 calc PR C 3 H38B H 0.4628 0.4289 0.2973 0.080 Uiso 0.250(6) 1 calc PR C 3 O39 O 0.5105(12) 0.447(2) 0.1155(19) 0.100(6) Uani 0.250(6) 1 d PDU C 3 H39 H 0.5427 0.3898 0.1021 0.149 Uiso 0.250(6) 1 calc PR C 3 N41 N 0.3715(10) 0.6448(11) 0.1885(14) 0.052(3) Uani 0.304(7) 1 d PDU D 4 H41 H 0.3118 0.6453 0.2046 0.062 Uiso 0.304(7) 1 calc PR D 4 C42 C 0.3652(15) 0.6029(15) 0.0390(14) 0.054(3) Uani 0.304(7) 1 d PDU D 4 H42A H 0.3159 0.6467 -0.0279 0.065 Uiso 0.304(7) 1 calc PR D 4 H42B H 0.4256 0.6158 0.0136 0.065 Uiso 0.304(7) 1 calc PR D 4 C43 C 0.3419(16) 0.4745(16) 0.033(2) 0.064(5) Uani 0.304(7) 1 d PDU D 4 H43A H 0.2781 0.4644 0.0479 0.077 Uiso 0.304(7) 1 calc PR D 4 H43B H 0.3411 0.4449 -0.0620 0.077 Uiso 0.304(7) 1 calc PR D 4 C44 C 0.4080(16) 0.4032(18) 0.138(2) 0.072(5) Uani 0.304(7) 1 d PDU D 4 H44A H 0.4721 0.4106 0.1229 0.087 Uiso 0.304(7) 1 calc PR D 4 H44B H 0.3895 0.3200 0.1274 0.087 Uiso 0.304(7) 1 calc PR D 4 C45 C 0.4060(17) 0.4475(15) 0.2863(18) 0.068(5) Uani 0.304(7) 1 d PDU D 4 H45A H 0.3422 0.4390 0.3014 0.081 Uiso 0.304(7) 1 calc PR D 4 H45B H 0.4497 0.4011 0.3585 0.081 Uiso 0.304(7) 1 calc PR D 4 C46 C 0.4339(14) 0.5710(14) 0.2977(19) 0.065(4) Uani 0.304(7) 1 d PDU D 4 H46A H 0.4992 0.5778 0.2879 0.079 Uiso 0.304(7) 1 calc PR D 4 H46B H 0.4322 0.6003 0.3918 0.079 Uiso 0.304(7) 1 calc PR D 4 C47 C 0.4092(16) 0.7657(14) 0.2026(17) 0.079(4) Uani 0.304(7) 1 d PDU D 4 H47A H 0.3808 0.8064 0.2712 0.094 Uiso 0.304(7) 1 calc PR D 4 H47B H 0.4772 0.7600 0.2456 0.094 Uiso 0.304(7) 1 calc PR D 4 C48 C 0.3983(18) 0.8391(16) 0.0851(18) 0.063(4) Uani 0.304(7) 1 d PDU D 4 H48A H 0.4282 0.9145 0.1187 0.076 Uiso 0.304(7) 1 calc PR D 4 H48B H 0.3305 0.8545 0.0505 0.076 Uiso 0.304(7) 1 calc PR D 4 O49 O 0.4346(9) 0.8030(14) -0.0398(11) 0.080(4) Uani 0.304(7) 1 d PDU D 4 H49 H 0.3893 0.7928 -0.1094 0.120 Uiso 0.304(7) 1 calc PR D 4 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 0.0194(11) 0.0343(14) 0.0188(11) 0.000(3) 0.0011(9) -0.006(3) B2 0.029(3) 0.033(3) 0.022(3) 0.003(2) -0.010(2) 0.006(2) B3 0.031(3) 0.041(3) 0.035(3) 0.004(3) -0.003(2) 0.006(3) B4 0.0212(12) 0.0466(17) 0.0206(12) 0.003(3) 0.0020(10) -0.003(3) B5 0.0196(13) 0.085(3) 0.0195(14) 0.010(4) 0.0010(11) -0.009(4) O1 0.0222(18) 0.033(2) 0.0235(17) 0.0011(17) -0.0070(13) 0.0037(15) O2 0.0446(11) 0.0386(11) 0.0304(10) 0.003(2) -0.0178(8) 0.001(2) O3 0.029(2) 0.035(2) 0.0178(16) 0.0004(17) 0.0015(13) 0.0031(16) O4 0.0183(8) 0.0409(10) 0.0194(8) 0.0043(19) 0.0009(6) -0.0032(19) O5 0.0186(9) 0.1029(19) 0.0145(8) -0.002(3) 0.0010(6) 0.001(3) O6 0.0186(8) 0.0484(11) 0.0157(8) -0.003(2) 0.0016(6) 0.001(2) O7 0.062(4) 0.041(2) 0.046(3) 0.005(2) -0.034(2) 0.002(2) O8 0.064(3) 0.036(2) 0.037(3) 0.0046(19) -0.022(2) -0.005(2) O9 0.0209(8) 0.0816(16) 0.0168(8) -0.001(3) 0.0009(6) 0.004(3) O10 0.0199(10) 0.224(4) 0.0173(10) -0.006(5) 0.0018(8) -0.003(5) N11 0.035(6) 0.068(7) 0.045(7) -0.008(8) 0.010(6) 0.001(8) C12 0.039(7) 0.074(8) 0.038(7) -0.005(8) 0.007(6) 0.006(9) C13 0.054(10) 0.073(10) 0.073(10) -0.003(9) 0.021(8) 0.003(9) C14 0.071(11) 0.082(10) 0.073(10) -0.003(10) -0.001(10) -0.001(10) C15 0.066(9) 0.086(9) 0.055(10) 0.012(9) 0.010(9) -0.015(9) C16 0.048(8) 0.075(8) 0.048(8) 0.015(7) 0.010(7) -0.019(8) C17 0.044(8) 0.063(9) 0.054(8) 0.000(7) 0.021(7) -0.011(8) C18 0.055(10) 0.068(9) 0.061(10) 0.010(9) 0.008(9) -0.014(9) O19 0.039(5) 0.036(5) 0.046(5) 0.006(4) 0.009(4) -0.002(4) N21 0.043(5) 0.058(5) 0.046(5) -0.001(4) 0.013(4) -0.004(4) C22 0.030(8) 0.073(8) 0.036(7) 0.006(8) 0.007(7) 0.003(8) C23 0.044(9) 0.072(10) 0.066(9) 0.007(9) 0.027(8) 0.002(9) C24 0.058(11) 0.087(10) 0.073(11) -0.010(10) 0.000(10) 0.024(9) C25 0.058(10) 0.074(9) 0.055(9) 0.002(9) 0.006(9) 0.007(9) C26 0.051(6) 0.060(6) 0.055(5) -0.003(4) 0.015(4) 0.000(4) C27 0.053(8) 0.065(8) 0.035(8) -0.007(7) 0.001(8) 0.000(7) C28 0.062(9) 0.085(9) 0.055(9) 0.015(9) 0.009(9) -0.023(8) O29 0.113(18) 0.135(18) 0.134(16) -0.030(16) -0.015(15) -0.005(16) N31 0.026(4) 0.046(5) 0.037(5) -0.002(4) 0.013(3) 0.004(4) C32 0.047(5) 0.054(5) 0.044(5) 0.003(4) 0.013(4) 0.003(4) C33 0.062(9) 0.072(9) 0.044(9) 0.016(8) -0.002(8) -0.006(9) C34 0.051(8) 0.079(9) 0.043(9) 0.012(8) -0.001(8) -0.017(8) C35 0.053(9) 0.073(9) 0.044(8) 0.007(8) 0.006(8) -0.013(9) C36 0.042(7) 0.074(8) 0.048(7) 0.002(7) 0.012(7) 0.005(8) C37 0.054(8) 0.068(8) 0.069(9) -0.004(8) 0.019(7) 0.008(7) C38 0.060(9) 0.081(9) 0.060(10) -0.020(8) 0.013(8) 0.018(8) O39 0.079(10) 0.127(16) 0.094(13) -0.024(12) 0.022(10) 0.024(11) N41 0.028(5) 0.081(7) 0.052(6) -0.015(6) 0.021(5) -0.010(5) C42 0.064(7) 0.071(8) 0.040(6) -0.004(7) 0.038(5) -0.001(8) C43 0.045(8) 0.075(9) 0.068(9) -0.003(8) 0.004(8) 0.005(8) C44 0.040(8) 0.089(9) 0.064(10) -0.004(8) -0.032(8) 0.023(7) C45 0.047(9) 0.090(9) 0.053(8) -0.034(8) -0.015(7) 0.019(8) C46 0.034(7) 0.087(9) 0.066(8) -0.009(8) -0.006(7) 0.007(9) C47 0.069(7) 0.088(7) 0.072(7) -0.004(7) 0.002(7) 0.001(7) C48 0.080(9) 0.071(8) 0.035(7) -0.005(7) 0.008(7) -0.005(8) O49 0.095(10) 0.089(10) 0.042(6) 0.009(6) -0.010(6) -0.017(8) _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 O3 1.447(7) . ? B1 O4 1.468(3) . ? B1 O6 1.473(3) . ? B1 O1 1.480(8) . ? B2 O2 1.341(9) . ? B2 O1 1.374(6) . ? B2 O7 1.370(8) . ? B3 O8 1.338(9) . ? B3 O3 1.339(7) . ? B3 O2 1.412(9) . ? B4 O9 1.348(3) . ? B4 O4 1.352(3) . ? B4 O5 1.385(3) . ? B5 O6 1.341(3) . ? B5 O10 1.345(4) . ? B5 O5 1.390(4) . ? O7 H7 0.8400 . ? O8 H8 0.8400 . ? O9 H9 0.8400 . ? O10 H10 0.8400 . ? N11 C17 1.505(14) . ? N11 C12 1.517(14) . ? N11 C16 1.517(16) . ? N11 H11 0.9300 . ? C12 C13 1.494(16) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.462(16) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.528(16) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.473(16) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.464(16) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 O19 1.553(17) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? O19 H19 0.8400 . ? N21 C27 1.498(14) . ? N21 C26 1.508(16) . ? N21 C22 1.512(14) . ? N21 H21 0.9300 . ? C22 C23 1.510(16) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.477(16) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.532(17) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.478(16) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.458(16) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 O29 1.547(17) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? O29 H29 0.8400 . ? N31 C37 1.469(13) . ? N31 C36 1.484(15) . ? N31 C32 1.520(14) . ? N31 H31 0.9300 . ? C32 C33 1.502(15) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.460(16) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.529(16) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.463(15) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.451(15) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 O39 1.528(17) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? O39 H39 0.8400 . ? N41 C47 1.486(14) . ? N41 C46 1.495(14) . ? N41 C42 1.526(12) . ? N41 H41 0.9300 . ? C42 C43 1.510(15) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.479(15) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.553(16) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.470(16) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.405(15) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 O49 1.508(15) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? O49 H49 0.8400 . ? 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 O3 B1 O4 109.5(4) . . ? O3 B1 O6 110.0(5) . . ? O4 B1 O6 110.52(18) . . ? O3 B1 O1 110.92(19) . . ? O4 B1 O1 108.6(4) . . ? O6 B1 O1 107.2(4) . . ? O2 B2 O1 122.2(5) . . ? O2 B2 O7 118.2(4) . . ? O1 B2 O7 119.6(6) . . ? O8 B3 O3 124.1(6) . . ? O8 B3 O2 116.2(5) . . ? O3 B3 O2 119.8(6) . . ? O9 B4 O4 118.5(2) . . ? O9 B4 O5 120.7(2) . . ? O4 B4 O5 120.8(2) . . ? O6 B5 O10 123.7(3) . . ? O6 B5 O5 120.8(2) . . ? O10 B5 O5 115.5(2) . . ? B2 O1 B1 121.8(4) . . ? B2 O2 B3 119.4(2) . . ? B3 O3 B1 125.0(5) . . ? B4 O4 B1 124.1(2) . . ? B4 O5 B5 119.3(2) . . ? B5 O6 B1 124.4(2) . . ? B2 O7 H7 109.5 . . ? B3 O8 H8 109.5 . . ? B4 O9 H9 109.5 . . ? B5 O10 H10 109.5 . . ? C17 N11 C12 112.6(13) . . ? C17 N11 C16 104.8(13) . . ? C12 N11 C16 110.1(14) . . ? C17 N11 H11 109.8 . . ? C12 N11 H11 109.8 . . ? C16 N11 H11 109.8 . . ? C13 C12 N11 107.3(13) . . ? C13 C12 H12A 110.3 . . ? N11 C12 H12A 110.3 . . ? C13 C12 H12B 110.3 . . ? N11 C12 H12B 110.3 . . ? H12A C12 H12B 108.5 . . ? C14 C13 C12 117.4(15) . . ? C14 C13 H13A 108.0 . . ? C12 C13 H13A 108.0 . . ? C14 C13 H13B 108.0 . . ? C12 C13 H13B 108.0 . . ? H13A C13 H13B 107.2 . . ? C13 C14 C15 117.9(16) . . ? C13 C14 H14A 107.8 . . ? C15 C14 H14A 107.8 . . ? C13 C14 H14B 107.8 . . ? C15 C14 H14B 107.8 . . ? H14A C14 H14B 107.2 . . ? C16 C15 C14 112.3(16) . . ? C16 C15 H15A 109.1 . . ? C14 C15 H15A 109.1 . . ? C16 C15 H15B 109.1 . . ? C14 C15 H15B 109.1 . . ? H15A C15 H15B 107.9 . . ? C15 C16 N11 113.6(15) . . ? C15 C16 H16A 108.9 . . ? N11 C16 H16A 108.9 . . ? C15 C16 H16B 108.9 . . ? N11 C16 H16B 108.9 . . ? H16A C16 H16B 107.7 . . ? C18 C17 N11 111.7(14) . . ? C18 C17 H17A 109.3 . . ? N11 C17 H17A 109.3 . . ? C18 C17 H17B 109.3 . . ? N11 C17 H17B 109.3 . . ? H17A C17 H17B 107.9 . . ? C17 C18 O19 104.7(15) . . ? C17 C18 H18A 110.8 . . ? O19 C18 H18A 110.8 . . ? C17 C18 H18B 110.8 . . ? O19 C18 H18B 110.8 . . ? H18A C18 H18B 108.9 . . ? C27 N21 C26 110.2(15) . . ? C27 N21 C22 114.5(14) . . ? C26 N21 C22 110.6(15) . . ? C27 N21 H21 107.1 . . ? C26 N21 H21 107.1 . . ? C22 N21 H21 107.1 . . ? N21 C22 C23 108.2(13) . . ? N21 C22 H22A 110.1 . . ? C23 C22 H22A 110.1 . . ? N21 C22 H22B 110.1 . . ? C23 C22 H22B 110.1 . . ? H22A C22 H22B 108.4 . . ? C24 C23 C22 113.9(13) . . ? C24 C23 H23A 108.8 . . ? C22 C23 H23A 108.8 . . ? C24 C23 H23B 108.8 . . ? C22 C23 H23B 108.8 . . ? H23A C23 H23B 107.7 . . ? C23 C24 C25 113.9(16) . . ? C23 C24 H24A 108.8 . . ? C25 C24 H24A 108.8 . . ? C23 C24 H24B 108.8 . . ? C25 C24 H24B 108.8 . . ? H24A C24 H24B 107.7 . . ? C26 C25 C24 113.5(15) . . ? C26 C25 H25A 108.9 . . ? C24 C25 H25A 108.9 . . ? C26 C25 H25B 108.9 . . ? C24 C25 H25B 108.9 . . ? H25A C25 H25B 107.7 . . ? C25 C26 N21 110.9(13) . . ? C25 C26 H26A 109.5 . . ? N21 C26 H26A 109.5 . . ? C25 C26 H26B 109.4 . . ? N21 C26 H26B 109.5 . . ? H26A C26 H26B 108.0 . . ? C28 C27 N21 111.1(15) . . ? C28 C27 H27A 109.4 . . ? N21 C27 H27A 109.4 . . ? C28 C27 H27B 109.4 . . ? N21 C27 H27B 109.4 . . ? H27A C27 H27B 108.0 . . ? C27 C28 O29 111.6(16) . . ? C27 C28 H28A 109.3 . . ? O29 C28 H28A 109.3 . . ? C27 C28 H28B 109.3 . . ? O29 C28 H28B 109.3 . . ? H28A C28 H28B 108.0 . . ? C28 O29 H29 109.5 . . ? C37 N31 C36 116.9(13) . . ? C37 N31 C32 114.3(14) . . ? C36 N31 C32 110.2(13) . . ? C37 N31 H31 104.7 . . ? C36 N31 H31 104.7 . . ? C32 N31 H31 104.7 . . ? C33 C32 N31 110.3(12) . . ? C33 C32 H32A 109.6 . . ? N31 C32 H32A 109.6 . . ? C33 C32 H32B 109.6 . . ? N31 C32 H32B 109.6 . . ? H32A C32 H32B 108.1 . . ? C34 C33 C32 117.8(13) . . ? C34 C33 H33A 107.9 . . ? C32 C33 H33A 107.9 . . ? C34 C33 H33B 107.9 . . ? C32 C33 H33B 107.9 . . ? H33A C33 H33B 107.2 . . ? C33 C34 C35 111.0(15) . . ? C33 C34 H34A 109.4 . . ? C35 C34 H34A 109.4 . . ? C33 C34 H34B 109.4 . . ? C35 C34 H34B 109.4 . . ? H34A C34 H34B 108.0 . . ? C36 C35 C34 117.5(14) . . ? C36 C35 H35A 107.9 . . ? C34 C35 H35A 107.9 . . ? C36 C35 H35B 107.9 . . ? C34 C35 H35B 107.9 . . ? H35A C35 H35B 107.2 . . ? C35 C36 N31 111.9(12) . . ? C35 C36 H36A 109.2 . . ? N31 C36 H36A 109.2 . . ? C35 C36 H36B 109.2 . . ? N31 C36 H36B 109.2 . . ? H36A C36 H36B 107.9 . . ? C38 C37 N31 111.9(14) . . ? C38 C37 H37A 109.2 . . ? N31 C37 H37A 109.2 . . ? C38 C37 H37B 109.2 . . ? N31 C37 H37B 109.2 . . ? H37A C37 H37B 107.9 . . ? C37 C38 O39 110.5(15) . . ? C37 C38 H38A 109.5 . . ? O39 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? O39 C38 H38B 109.5 . . ? H38A C38 H38B 108.1 . . ? C47 N41 C46 108.0(12) . . ? C47 N41 C42 108.5(11) . . ? C46 N41 C42 113.4(12) . . ? C47 N41 H41 108.9 . . ? C46 N41 H41 108.9 . . ? C42 N41 H41 108.9 . . ? C43 C42 N41 107.8(11) . . ? C43 C42 H42A 110.2 . . ? N41 C42 H42A 110.2 . . ? C43 C42 H42B 110.2 . . ? N41 C42 H42B 110.2 . . ? H42A C42 H42B 108.5 . . ? C44 C43 C42 113.9(15) . . ? C44 C43 H43A 108.8 . . ? C42 C43 H43A 108.8 . . ? C44 C43 H43B 108.8 . . ? C42 C43 H43B 108.8 . . ? H43A C43 H43B 107.7 . . ? C43 C44 C45 108.3(14) . . ? C43 C44 H44A 110.0 . . ? C45 C44 H44A 110.0 . . ? C43 C44 H44B 110.0 . . ? C45 C44 H44B 110.0 . . ? H44A C44 H44B 108.4 . . ? C46 C45 C44 108.5(14) . . ? C46 C45 H45A 110.0 . . ? C44 C45 H45A 110.0 . . ? C46 C45 H45B 110.0 . . ? C44 C45 H45B 110.0 . . ? H45A C45 H45B 108.4 . . ? C45 C46 N41 112.2(12) . . ? C45 C46 H46A 109.2 . . ? N41 C46 H46A 109.2 . . ? C45 C46 H46B 109.2 . . ? N41 C46 H46B 109.2 . . ? H46A C46 H46B 107.9 . . ? C48 C47 N41 121.0(14) . . ? C48 C47 H47A 107.1 . . ? N41 C47 H47A 107.1 . . ? C48 C47 H47B 107.1 . . ? N41 C47 H47B 107.1 . . ? H47A C47 H47B 106.8 . . ? C47 C48 O49 120.7(15) . . ? C47 C48 H48A 107.1 . . ? O49 C48 H48A 107.1 . . ? C47 C48 H48B 107.1 . . ? O49 C48 H48B 107.1 . . ? H48A C48 H48B 106.8 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O7 H7 O3 0.84 1.90 2.732(6) 169.2 4_546 O8 H8 O1 0.84 1.96 2.742(6) 154.9 4_556 O9 H9 O5 0.84 1.99 2.789(3) 158.6 2 O10 H10 O6 0.84 1.94 2.674(3) 144.6 2_556 N11 H11 O4 0.93 2.15 3.06(2) 166.3 . N21 H21 O4 0.93 1.91 2.83(3) 168.3 . O29 H29 O8 0.84 2.59 3.32(4) 145.9 2_656 N31 H31 O4 0.93 1.89 2.79(2) 162.6 . N41 H41 O4 0.93 1.95 2.862(15) 167.7 . O49 H49 O8 0.84 2.10 2.842(11) 146.7 1_554 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.375 _refine_diff_density_min -0.280 _refine_diff_density_rms 0.057 #===END data_1h #TrackingRef 'pentaborates.CIF' _database_code_depnum_ccdc_archive 'CCDC 764926' #The cations are disordered in cavities created by borate anion #framework. Only the major components are modelled. _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C7 H22 B5 N O11' _chemical_formula_weight 350.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 11.7329(3) _cell_length_b 15.3306(5) _cell_length_c 18.0615(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.906(2) _cell_angle_gamma 90.00 _cell_volume 3200.33(16) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 7467 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.454 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 0.126 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9752 _exptl_absorpt_correction_T_max 0.9925 _exptl_absorpt_process_details 'SADABS 2007/2 (Sheldrick, G.M., 2007)' _exptl_special_details ; SADABS was used to perform the Absorption correction Parameter refinement on 25922 reflections reduced R(int) from 0.1001 to 0.0474 Ratio of minimum to maximum apparent transmission: 0.824325 The given Tmin and Tmax were generated using the SHELX SIZE command ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius APEX II CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31495 _diffrn_reflns_av_R_equivalents 0.0498 _diffrn_reflns_av_sigmaI/netI 0.0469 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7287 _reflns_number_gt 5224 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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^)+(0.0571P)^2^+6.4888P] 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 7287 _refine_ls_number_parameters 694 _refine_ls_number_restraints 1407 _refine_ls_R_factor_all 0.1188 _refine_ls_R_factor_gt 0.0861 _refine_ls_wR_factor_ref 0.2109 _refine_ls_wR_factor_gt 0.1885 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.049 _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 0.5681(3) 0.3789(2) 0.14447(19) 0.0256(6) Uani 1 1 d U . . B2 B 0.6648(3) 0.2353(2) 0.13674(17) 0.0236(6) Uani 1 1 d U . . B3 B 0.4637(3) 0.2383(2) 0.14291(18) 0.0244(6) Uani 1 1 d U . . B4 B 0.5610(3) 0.5348(2) 0.1081(2) 0.0342(8) Uani 1 1 d U . . B5 B 0.6051(3) 0.4979(2) 0.2379(2) 0.0327(7) Uani 1 1 d U . . O1 O 0.66601(15) 0.32320(12) 0.13012(11) 0.0256(4) Uani 1 1 d U . . O2 O 0.56446(16) 0.19166(12) 0.14487(12) 0.0290(4) Uani 1 1 d U . . O3 O 0.46154(16) 0.32585(12) 0.13665(11) 0.0275(4) Uani 1 1 d U . . O4 O 0.55041(16) 0.44888(12) 0.08874(11) 0.0280(4) Uani 1 1 d U . . O5 O 0.5887(2) 0.56045(14) 0.18213(13) 0.0409(6) Uani 1 1 d U . . O6 O 0.59515(18) 0.41225(13) 0.22071(12) 0.0330(5) Uani 1 1 d U . . O7 O 0.76010(17) 0.18499(13) 0.13651(12) 0.0316(5) Uani 1 1 d U . . H7 H 0.8182 0.2171 0.1370 0.047 Uiso 1 1 calc R . . O8 O 0.36628(17) 0.19087(13) 0.14663(13) 0.0335(5) Uani 1 1 d U . . H8 H 0.3086 0.2242 0.1407 0.050 Uiso 1 1 calc R . . O9 O 0.5423(3) 0.59925(14) 0.05604(15) 0.0515(7) Uani 1 1 d U . . H9 H 0.5228 0.5773 0.0131 0.077 Uiso 1 1 calc R . . O10 O 0.6293(2) 0.52118(15) 0.31139(13) 0.0406(6) Uani 1 1 d U . . H10 H 0.6301 0.5758 0.3149 0.061 Uiso 1 1 calc R . . B11 B 0.0700(3) 0.2244(2) 0.1544(2) 0.0310(7) Uani 1 1 d U . . B12 B -0.0370(3) 0.3654(2) 0.13884(18) 0.0273(7) Uani 1 1 d U . . B13 B 0.1649(3) 0.3667(2) 0.13368(19) 0.0279(7) Uani 1 1 d U . . B14 B 0.0637(3) 0.0676(2) 0.1252(2) 0.0338(8) Uani 1 1 d U . . B15 B 0.1025(3) 0.1105(2) 0.2534(2) 0.0322(7) Uani 1 1 d U . . O11 O -0.03752(16) 0.27762(13) 0.14321(12) 0.0320(5) Uani 1 1 d U . . O12 O 0.06293(17) 0.41118(13) 0.13471(13) 0.0347(5) Uani 1 1 d U . . O13 O 0.16834(17) 0.27864(13) 0.13956(13) 0.0363(5) Uani 1 1 d U . . O14 O 0.05480(18) 0.15139(14) 0.10249(12) 0.0334(5) Uani 1 1 d U . . O15 O 0.08675(19) 0.04548(14) 0.20043(12) 0.0363(5) Uani 1 1 d U . . O16 O 0.09402(18) 0.19592(13) 0.23293(12) 0.0344(5) Uani 1 1 d U . . O17 O -0.13474(17) 0.41424(13) 0.13600(13) 0.0325(5) Uani 1 1 d U . . H17 H -0.1917 0.3812 0.1365 0.049 Uiso 1 1 calc R . . O18 O 0.25865(18) 0.41555(14) 0.12675(14) 0.0389(5) Uani 1 1 d U . . H18 H 0.3166 0.3830 0.1285 0.058 Uiso 1 1 calc R . . O19 O 0.0484(2) 0.00115(17) 0.07450(16) 0.0494(6) Uani 1 1 d U . . H19A H -0.0127 0.0094 0.0436 0.074 Uiso 0.43(6) 1 calc PR A 1 H19B H 0.0523 -0.0467 0.0974 0.074 Uiso 0.57(6) 1 d PR A 2 O20 O 0.1243(2) 0.09129(15) 0.32797(13) 0.0426(6) Uani 1 1 d U . . H20 H 0.1256 0.0369 0.3337 0.064 Uiso 1 1 calc R . . C21 C 0.6178(5) 0.9699(4) 0.1476(4) 0.0480(16) Uani 0.580(6) 1 d PDU B 1 H21A H 0.6137 0.9443 0.1974 0.058 Uiso 0.580(6) 1 calc PR B 1 H21B H 0.6391 1.0321 0.1551 0.058 Uiso 0.580(6) 1 calc PR B 1 C22 C 0.7109(6) 0.9226(6) 0.1131(4) 0.041(2) Uani 0.580(6) 1 d PDU B 1 C23 C 0.7196(7) 0.9680(6) 0.0384(4) 0.057(2) Uani 0.580(6) 1 d PDU B 1 H23A H 0.7752 0.9368 0.0134 0.085 Uiso 0.580(6) 1 calc PR B 1 H23B H 0.7458 1.0283 0.0484 0.085 Uiso 0.580(6) 1 calc PR B 1 H23C H 0.6436 0.9680 0.0060 0.085 Uiso 0.580(6) 1 calc PR B 1 C24 C 0.8253(5) 0.9276(5) 0.1685(4) 0.0531(19) Uani 0.580(6) 1 d PDU B 1 H24A H 0.8170 0.8977 0.2152 0.080 Uiso 0.580(6) 1 calc PR B 1 H24B H 0.8454 0.9889 0.1794 0.080 Uiso 0.580(6) 1 calc PR B 1 H24C H 0.8865 0.8996 0.1464 0.080 Uiso 0.580(6) 1 calc PR B 1 C25 C 0.5671(11) 0.8184(9) 0.0390(8) 0.109(6) Uani 0.580(6) 1 d PDU B 1 H25A H 0.5855 0.8329 -0.0105 0.164 Uiso 0.580(6) 1 calc PR B 1 H25B H 0.5083 0.8589 0.0511 0.164 Uiso 0.580(6) 1 calc PR B 1 H25C H 0.5373 0.7586 0.0382 0.164 Uiso 0.580(6) 1 calc PR B 1 C26 C 0.7663(12) 0.7734(7) 0.0681(7) 0.115(5) Uani 0.580(6) 1 d PDU B 1 H26A H 0.7378 0.7140 0.0568 0.172 Uiso 0.580(6) 1 calc PR B 1 H26B H 0.8370 0.7715 0.1059 0.172 Uiso 0.580(6) 1 calc PR B 1 H26C H 0.7831 0.8008 0.0221 0.172 Uiso 0.580(6) 1 calc PR B 1 C27 C 0.6519(10) 0.7805(5) 0.1677(6) 0.054(3) Uani 0.580(6) 1 d PDU B 1 H27A H 0.5867 0.8089 0.1854 0.081 Uiso 0.580(6) 1 calc PR B 1 H27B H 0.7207 0.7838 0.2069 0.081 Uiso 0.580(6) 1 calc PR B 1 H27C H 0.6328 0.7192 0.1562 0.081 Uiso 0.580(6) 1 calc PR B 1 N21 N 0.6754(7) 0.8258(5) 0.0979(4) 0.048(2) Uani 0.580(6) 1 d PDU B 1 O21 O 0.5075(4) 0.9634(4) 0.1007(3) 0.0689(17) Uani 0.580(6) 1 d PDU B 1 H21 H 0.4555 0.9741 0.1261 0.103 Uiso 0.580(6) 1 calc PR B 1 C121 C 0.7742(9) 0.7794(7) 0.0949(6) 0.051(3) Uani 0.420(6) 1 d PDU B 2 H12A H 0.7535 0.7170 0.0967 0.061 Uiso 0.420(6) 1 calc PR B 2 H12B H 0.7967 0.7913 0.0455 0.061 Uiso 0.420(6) 1 calc PR B 2 C122 C 0.6697(10) 0.8361(7) 0.1044(6) 0.045(3) Uani 0.420(6) 1 d PDU B 2 C123 C 0.5796(11) 0.8170(6) 0.0338(7) 0.041(3) Uani 0.420(6) 1 d PDU B 2 H12C H 0.5022 0.8315 0.0436 0.062 Uiso 0.420(6) 1 calc PR B 2 H12D H 0.5825 0.7550 0.0210 0.062 Uiso 0.420(6) 1 calc PR B 2 H12E H 0.5966 0.8523 -0.0082 0.062 Uiso 0.420(6) 1 calc PR B 2 C124 C 0.6290(14) 0.8110(8) 0.1776(7) 0.053(3) Uani 0.420(6) 1 d PDU B 2 H12F H 0.6953 0.8104 0.2188 0.079 Uiso 0.420(6) 1 calc PR B 2 H12G H 0.5936 0.7529 0.1723 0.079 Uiso 0.420(6) 1 calc PR B 2 H12H H 0.5719 0.8536 0.1887 0.079 Uiso 0.420(6) 1 calc PR B 2 C125 C 0.5914(8) 0.9922(6) 0.0849(7) 0.066(3) Uani 0.420(6) 1 d PDU B 2 H12I H 0.5545 0.9970 0.1295 0.100 Uiso 0.420(6) 1 calc PR B 2 H12J H 0.5369 0.9663 0.0436 0.100 Uiso 0.420(6) 1 calc PR B 2 H12K H 0.6140 1.0503 0.0702 0.100 Uiso 0.420(6) 1 calc PR B 2 C126 C 0.7681(9) 0.9558(9) 0.0424(6) 0.055(3) Uani 0.420(6) 1 d PDU B 2 H12L H 0.7895 1.0177 0.0452 0.082 Uiso 0.420(6) 1 calc PR B 2 H12M H 0.7223 0.9432 -0.0071 0.082 Uiso 0.420(6) 1 calc PR B 2 H12N H 0.8384 0.9200 0.0500 0.082 Uiso 0.420(6) 1 calc PR B 2 C127 C 0.7639(13) 0.9664(7) 0.1765(6) 0.088(4) Uani 0.420(6) 1 d PDU B 2 H12O H 0.7855 1.0276 0.1719 0.132 Uiso 0.420(6) 1 calc PR B 2 H12P H 0.8339 0.9310 0.1903 0.132 Uiso 0.420(6) 1 calc PR B 2 H12Q H 0.7156 0.9609 0.2155 0.132 Uiso 0.420(6) 1 calc PR B 2 N121 N 0.6974(8) 0.9351(6) 0.1028(5) 0.041(2) Uani 0.420(6) 1 d PDU B 2 O121 O 0.8681(6) 0.7984(5) 0.1531(5) 0.082(3) Uani 0.420(6) 1 d PDU B 2 H121 H 0.8794 0.7559 0.1828 0.124 Uiso 0.420(6) 1 calc PR B 2 C31 C 0.2911(7) 0.8168(6) 0.1090(5) 0.066(2) Uani 0.442(3) 1 d PDU C 1 H31A H 0.3210 0.8053 0.0619 0.079 Uiso 0.442(3) 1 calc PR C 1 H31B H 0.2744 0.8799 0.1113 0.079 Uiso 0.442(3) 1 calc PR C 1 C32 C 0.1795(7) 0.7638(5) 0.1097(4) 0.046(2) Uani 0.442(3) 1 d PDU C 1 C33 C 0.0983(10) 0.7926(7) 0.0370(4) 0.084(3) Uani 0.442(3) 1 d PDU C 1 H33A H 0.1424 0.7965 -0.0043 0.125 Uiso 0.442(3) 1 calc PR C 1 H33B H 0.0650 0.8498 0.0449 0.125 Uiso 0.442(3) 1 calc PR C 1 H33C H 0.0360 0.7498 0.0243 0.125 Uiso 0.442(3) 1 calc PR C 1 C34 C 0.1324(12) 0.7897(8) 0.1809(6) 0.045(3) Uani 0.442(3) 1 d PDU C 1 H34A H 0.0572 0.7617 0.1805 0.068 Uiso 0.442(3) 1 calc PR C 1 H34B H 0.1232 0.8532 0.1822 0.068 Uiso 0.442(3) 1 calc PR C 1 H34C H 0.1867 0.7708 0.2254 0.068 Uiso 0.442(3) 1 calc PR C 1 C35 C 0.0922(8) 0.6140(6) 0.0737(6) 0.064(3) Uani 0.442(3) 1 d PDU C 1 H35A H 0.1021 0.5521 0.0871 0.096 Uiso 0.442(3) 1 calc PR C 1 H35B H 0.0802 0.6201 0.0189 0.096 Uiso 0.442(3) 1 calc PR C 1 H35C H 0.0250 0.6372 0.0926 0.096 Uiso 0.442(3) 1 calc PR C 1 C36 C 0.2384(12) 0.6255(7) 0.1855(5) 0.072(3) Uani 0.442(3) 1 d PDU C 1 H36A H 0.2720 0.5677 0.1807 0.109 Uiso 0.442(3) 1 calc PR C 1 H36B H 0.1718 0.6202 0.2113 0.109 Uiso 0.442(3) 1 calc PR C 1 H36C H 0.2965 0.6637 0.2145 0.109 Uiso 0.442(3) 1 calc PR C 1 C37 C 0.2909(9) 0.6386(7) 0.0630(6) 0.067(3) Uani 0.442(3) 1 d PDU C 1 H37A H 0.3601 0.6744 0.0785 0.100 Uiso 0.442(3) 1 calc PR C 1 H37B H 0.2615 0.6480 0.0094 0.100 Uiso 0.442(3) 1 calc PR C 1 H37C H 0.3107 0.5769 0.0717 0.100 Uiso 0.442(3) 1 calc PR C 1 N31 N 0.1993(7) 0.6639(5) 0.1082(4) 0.041(2) Uani 0.442(3) 1 d PDU C 1 O31 O 0.3749(6) 0.7925(6) 0.1715(4) 0.079(2) Uani 0.442(3) 1 d PDU C 1 H31 H 0.3761 0.8297 0.2058 0.119 Uiso 0.442(3) 1 calc PR C 1 C131 C 0.1597(11) 0.8040(10) 0.1686(6) 0.046(3) Uani 0.366(5) 1 d PDU D 2 H13A H 0.1308 0.7661 0.2057 0.055 Uiso 0.366(5) 1 calc PR D 2 H13B H 0.2118 0.8483 0.1964 0.055 Uiso 0.366(5) 1 calc PR D 2 C132 C 0.2264(7) 0.7492(5) 0.1196(5) 0.040(2) Uani 0.366(5) 1 d PDU D 2 C133 C 0.3470(7) 0.7321(7) 0.1649(6) 0.050(3) Uani 0.366(5) 1 d PDU D 2 H13C H 0.3617 0.7725 0.2076 0.075 Uiso 0.366(5) 1 calc PR D 2 H13D H 0.4052 0.7409 0.1327 0.075 Uiso 0.366(5) 1 calc PR D 2 H13E H 0.3513 0.6719 0.1836 0.075 Uiso 0.366(5) 1 calc PR D 2 C134 C 0.2299(16) 0.8011(8) 0.0469(6) 0.071(4) Uani 0.366(5) 1 d PDU D 2 H13F H 0.2667 0.7656 0.0125 0.106 Uiso 0.366(5) 1 calc PR D 2 H13G H 0.2745 0.8548 0.0591 0.106 Uiso 0.366(5) 1 calc PR D 2 H13H H 0.1509 0.8158 0.0229 0.106 Uiso 0.366(5) 1 calc PR D 2 C135 C 0.0423(7) 0.6681(7) 0.0620(6) 0.048(2) Uani 0.366(5) 1 d PDU D 2 H13I H 0.0369 0.7076 0.0189 0.072 Uiso 0.366(5) 1 calc PR D 2 H13J H -0.0032 0.6916 0.0981 0.072 Uiso 0.366(5) 1 calc PR D 2 H13K H 0.0122 0.6106 0.0448 0.072 Uiso 0.366(5) 1 calc PR D 2 C136 C 0.1685(12) 0.6031(8) 0.1676(7) 0.043(3) Uani 0.366(5) 1 d PDU D 2 H13L H 0.0913 0.5783 0.1669 0.064 Uiso 0.366(5) 1 calc PR D 2 H13M H 0.1903 0.6384 0.2131 0.064 Uiso 0.366(5) 1 calc PR D 2 H13N H 0.2247 0.5558 0.1674 0.064 Uiso 0.366(5) 1 calc PR D 2 C137 C 0.2273(12) 0.6101(9) 0.0448(7) 0.052(3) Uani 0.366(5) 1 d PDU D 2 H13O H 0.2117 0.6385 -0.0045 0.078 Uiso 0.366(5) 1 calc PR D 2 H13P H 0.1982 0.5500 0.0402 0.078 Uiso 0.366(5) 1 calc PR D 2 H13Q H 0.3108 0.6095 0.0634 0.078 Uiso 0.366(5) 1 calc PR D 2 N131 N 0.1673(7) 0.6596(5) 0.0993(5) 0.045(2) Uani 0.366(5) 1 d PDU D 2 O131 O 0.0646(6) 0.8462(5) 0.1222(4) 0.056(2) Uani 0.366(5) 1 d PDU D 2 H131 H 0.0028 0.8331 0.1371 0.084 Uiso 0.366(5) 1 calc PR D 2 C231 C 0.223(2) 0.6232(13) 0.0523(11) 0.053(5) Uani 0.193(4) 1 d PDU E 3 H23D H 0.2712 0.5700 0.0628 0.064 Uiso 0.193(4) 1 calc PR E 3 H23E H 0.1427 0.6054 0.0330 0.064 Uiso 0.193(4) 1 calc PR E 3 C232 C 0.2286(13) 0.6772(10) 0.1247(9) 0.052(4) Uani 0.193(4) 1 d PDU E 3 C233 C 0.3580(13) 0.6924(14) 0.1534(13) 0.066(6) Uani 0.193(4) 1 d PDU E 3 H23F H 0.3897 0.7299 0.1179 0.100 Uiso 0.193(4) 1 calc PR E 3 H23G H 0.3986 0.6363 0.1579 0.100 Uiso 0.193(4) 1 calc PR E 3 H23H H 0.3681 0.7208 0.2027 0.100 Uiso 0.193(4) 1 calc PR E 3 C234 C 0.170(2) 0.6254(14) 0.1804(12) 0.051(6) Uani 0.193(4) 1 d PDU E 3 H23I H 0.2133 0.6327 0.2313 0.076 Uiso 0.193(4) 1 calc PR E 3 H23J H 0.1673 0.5634 0.1668 0.076 Uiso 0.193(4) 1 calc PR E 3 H23K H 0.0905 0.6470 0.1785 0.076 Uiso 0.193(4) 1 calc PR E 3 C235 C 0.2312(19) 0.8280(13) 0.0636(12) 0.056(6) Uani 0.193(4) 1 d PDU E 3 H23L H 0.2959 0.8549 0.0975 0.084 Uiso 0.193(4) 1 calc PR E 3 H23M H 0.1782 0.8736 0.0404 0.084 Uiso 0.193(4) 1 calc PR E 3 H23N H 0.2609 0.7954 0.0243 0.084 Uiso 0.193(4) 1 calc PR E 3 C236 C 0.0473(12) 0.7562(11) 0.0618(10) 0.048(4) Uani 0.193(4) 1 d PDU E 3 H23O H 0.0020 0.7164 0.0877 0.072 Uiso 0.193(4) 1 calc PR E 3 H23P H 0.0533 0.7323 0.0123 0.072 Uiso 0.193(4) 1 calc PR E 3 H23Q H 0.0090 0.8132 0.0557 0.072 Uiso 0.193(4) 1 calc PR E 3 C237 C 0.155(3) 0.8140(18) 0.1790(11) 0.052(7) Uani 0.193(4) 1 d PDU E 3 H23R H 0.0728 0.8231 0.1806 0.077 Uiso 0.193(4) 1 calc PR E 3 H23S H 0.1943 0.8705 0.1804 0.077 Uiso 0.193(4) 1 calc PR E 3 H23T H 0.1899 0.7790 0.2225 0.077 Uiso 0.193(4) 1 calc PR E 3 N231 N 0.1673(12) 0.7665(10) 0.1077(8) 0.047(3) Uani 0.193(4) 1 d PDU E 3 O231 O 0.266(4) 0.676(2) -0.0018(13) 0.164(8) Uani 0.193(4) 1 d PDU E 3 H231 H 0.2626 0.6476 -0.0421 0.246 Uiso 0.193(4) 1 calc PR E 3 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 0.0216(14) 0.0190(14) 0.0360(17) 0.0005(12) 0.0043(12) 0.0005(11) B2 0.0253(15) 0.0229(15) 0.0228(14) -0.0020(11) 0.0048(12) 0.0019(12) B3 0.0242(15) 0.0205(14) 0.0288(15) 0.0034(12) 0.0055(12) 0.0019(12) B4 0.0323(17) 0.0208(16) 0.048(2) 0.0020(14) 0.0023(15) 0.0009(13) B5 0.0235(15) 0.0305(17) 0.0437(19) -0.0050(15) 0.0047(14) 0.0036(13) O1 0.0208(9) 0.0202(9) 0.0364(11) 0.0016(8) 0.0063(8) 0.0013(7) O2 0.0244(10) 0.0185(9) 0.0438(12) 0.0022(8) 0.0052(8) 0.0016(8) O3 0.0214(9) 0.0204(10) 0.0416(11) 0.0045(8) 0.0077(8) 0.0006(7) O4 0.0253(10) 0.0194(9) 0.0388(11) 0.0024(8) 0.0039(8) -0.0008(8) O5 0.0498(14) 0.0217(11) 0.0480(13) -0.0026(10) -0.0008(11) 0.0021(10) O6 0.0360(11) 0.0241(10) 0.0383(12) -0.0023(9) 0.0047(9) 0.0015(9) O7 0.0250(10) 0.0239(10) 0.0460(12) -0.0011(9) 0.0064(9) 0.0024(8) O8 0.0247(10) 0.0227(10) 0.0536(13) 0.0093(9) 0.0077(10) -0.0001(8) O9 0.0750(18) 0.0192(11) 0.0533(15) 0.0036(10) -0.0087(14) -0.0021(11) O10 0.0446(13) 0.0310(12) 0.0453(13) -0.0091(10) 0.0051(10) 0.0064(10) B11 0.0256(15) 0.0227(16) 0.0452(19) 0.0037(14) 0.0073(14) -0.0007(12) B12 0.0231(15) 0.0303(17) 0.0281(16) -0.0036(13) 0.0034(12) 0.0002(12) B13 0.0233(15) 0.0260(16) 0.0340(17) 0.0037(13) 0.0040(13) -0.0006(12) B14 0.0274(16) 0.0319(18) 0.044(2) -0.0001(15) 0.0121(15) 0.0005(14) B15 0.0241(15) 0.0297(17) 0.0422(19) 0.0042(14) 0.0043(14) -0.0072(13) O11 0.0229(10) 0.0269(11) 0.0476(13) 0.0016(9) 0.0101(9) 0.0010(8) O12 0.0240(10) 0.0239(10) 0.0566(14) -0.0001(10) 0.0080(9) 0.0020(8) O13 0.0250(10) 0.0256(11) 0.0600(14) 0.0088(10) 0.0125(10) 0.0026(8) O14 0.0321(11) 0.0291(11) 0.0393(12) 0.0021(9) 0.0069(9) 0.0048(9) O15 0.0404(12) 0.0259(11) 0.0431(12) 0.0052(9) 0.0090(10) -0.0009(9) O16 0.0360(11) 0.0261(11) 0.0399(12) 0.0014(9) 0.0031(9) -0.0061(9) O17 0.0235(10) 0.0270(11) 0.0469(13) -0.0037(9) 0.0059(9) -0.0010(8) O18 0.0261(11) 0.0250(11) 0.0676(16) 0.0045(10) 0.0134(11) 0.0019(8) O19 0.0558(16) 0.0394(14) 0.0541(15) -0.0111(12) 0.0121(13) 0.0049(12) O20 0.0486(14) 0.0333(12) 0.0428(13) 0.0054(10) -0.0007(11) -0.0097(11) C21 0.057(4) 0.034(3) 0.053(4) -0.010(3) 0.010(3) 0.004(3) C22 0.048(4) 0.039(4) 0.039(4) 0.003(3) 0.013(3) -0.009(3) C23 0.049(5) 0.072(6) 0.050(4) 0.019(4) 0.011(4) -0.014(5) C24 0.042(4) 0.066(5) 0.049(4) -0.002(4) 0.002(3) -0.012(3) C25 0.113(9) 0.134(11) 0.068(9) 0.021(8) -0.023(8) -0.066(8) C26 0.182(11) 0.079(8) 0.091(10) 0.001(7) 0.047(8) 0.056(8) C27 0.072(6) 0.026(4) 0.061(5) 0.011(4) 0.000(4) -0.005(4) N21 0.065(4) 0.027(3) 0.049(4) 0.001(3) 0.000(3) 0.000(3) O21 0.059(3) 0.081(4) 0.069(3) -0.017(3) 0.019(3) 0.011(3) C121 0.074(6) 0.039(5) 0.038(6) 0.012(4) 0.002(4) 0.000(5) C122 0.063(6) 0.034(5) 0.036(5) 0.001(4) -0.002(5) -0.009(5) C123 0.065(7) 0.013(4) 0.037(6) -0.002(4) -0.015(5) -0.007(4) C124 0.073(8) 0.042(7) 0.046(5) 0.012(6) 0.017(5) -0.017(6) C125 0.084(7) 0.047(5) 0.078(7) -0.004(5) 0.039(6) 0.006(5) C126 0.036(6) 0.063(7) 0.062(6) 0.031(5) 0.000(5) -0.018(5) C127 0.139(12) 0.048(7) 0.061(6) -0.001(5) -0.031(7) -0.028(7) N121 0.054(5) 0.027(4) 0.039(4) 0.005(4) -0.001(4) -0.014(4) O121 0.058(4) 0.084(6) 0.099(6) 0.052(5) -0.004(4) 0.007(4) C31 0.073(6) 0.064(5) 0.061(5) -0.013(5) 0.013(5) -0.009(5) C32 0.065(5) 0.034(4) 0.041(4) -0.003(4) 0.016(4) 0.001(4) C33 0.150(9) 0.073(7) 0.020(4) 0.016(4) -0.003(5) -0.038(7) C34 0.064(7) 0.034(6) 0.042(5) 0.007(4) 0.024(5) 0.025(5) C35 0.070(6) 0.051(6) 0.071(6) 0.001(5) 0.010(5) -0.029(5) C36 0.129(10) 0.041(5) 0.039(5) -0.001(4) -0.010(6) 0.009(7) C37 0.077(7) 0.061(7) 0.066(6) -0.008(5) 0.025(6) 0.013(6) N31 0.055(5) 0.034(4) 0.035(4) -0.003(3) 0.017(4) -0.001(3) O31 0.072(5) 0.078(6) 0.080(5) -0.020(4) -0.008(4) 0.018(4) C131 0.069(7) 0.032(6) 0.035(6) 0.008(5) 0.004(5) 0.001(6) C132 0.055(5) 0.030(4) 0.035(4) 0.005(3) 0.008(4) -0.005(4) C133 0.046(5) 0.032(6) 0.072(7) -0.037(5) 0.011(5) -0.022(4) C134 0.129(10) 0.043(6) 0.041(7) 0.008(5) 0.017(7) -0.021(7) C135 0.041(5) 0.048(6) 0.051(6) -0.003(5) -0.002(4) -0.005(4) C136 0.057(7) 0.024(6) 0.051(7) 0.006(5) 0.017(5) -0.013(5) C137 0.060(7) 0.063(8) 0.034(6) -0.015(5) 0.012(5) -0.005(6) N131 0.053(5) 0.031(4) 0.047(5) -0.005(4) 0.000(4) -0.011(4) O131 0.057(4) 0.041(4) 0.073(5) 0.002(3) 0.015(4) 0.012(3) C231 0.059(9) 0.045(8) 0.053(8) -0.025(7) 0.001(8) -0.001(8) C232 0.062(7) 0.036(6) 0.053(7) -0.004(6) -0.005(6) 0.007(6) C233 0.063(10) 0.056(14) 0.068(12) -0.036(11) -0.022(9) -0.005(9) C234 0.071(12) 0.024(11) 0.046(10) -0.002(9) -0.021(9) -0.012(10) C235 0.068(10) 0.076(12) 0.020(8) 0.004(9) -0.003(8) -0.033(10) C236 0.054(9) 0.039(9) 0.050(9) 0.013(8) 0.005(8) -0.010(7) C237 0.060(13) 0.050(13) 0.046(11) 0.000(10) 0.010(10) 0.018(11) N231 0.062(6) 0.036(6) 0.043(6) 0.000(5) 0.010(6) -0.002(6) O231 0.196(19) 0.167(18) 0.133(14) 0.009(14) 0.039(16) -0.014(17) _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 O6 1.452(4) . ? B1 O4 1.462(4) . ? B1 O3 1.478(4) . ? B1 O1 1.489(4) . ? B2 O1 1.353(4) . ? B2 O7 1.360(4) . ? B2 O2 1.384(4) . ? B3 O3 1.346(4) . ? B3 O8 1.367(4) . ? B3 O2 1.377(4) . ? B4 O9 1.356(4) . ? B4 O4 1.362(4) . ? B4 O5 1.379(4) . ? B5 O6 1.350(4) . ? B5 O10 1.357(4) . ? B5 O5 1.380(4) . ? O7 H7 0.8400 . ? O8 H8 0.8400 . ? O9 H9 0.8400 . ? O10 H10 0.8400 . ? B11 O14 1.452(4) . ? B11 O16 1.464(4) . ? B11 O13 1.483(4) . ? B11 O11 1.487(4) . ? B12 O11 1.348(4) . ? B12 O17 1.363(4) . ? B12 O12 1.379(4) . ? B13 O13 1.354(4) . ? B13 O18 1.355(4) . ? B13 O12 1.380(4) . ? B14 O14 1.346(4) . ? B14 O19 1.362(4) . ? B14 O15 1.381(4) . ? B15 O16 1.359(4) . ? B15 O20 1.359(4) . ? B15 O15 1.373(4) . ? O17 H17 0.8400 . ? O18 H18 0.8400 . ? O19 H19A 0.8400 . ? O19 H19B 0.8400 . ? O20 H20 0.8400 . ? C21 O21 1.423(7) . ? C21 C22 1.530(8) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C24 1.532(7) . ? C22 C23 1.537(7) . ? C22 N21 1.553(6) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 N21 1.515(7) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 N21 1.507(7) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 N21 1.505(6) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? O21 H21 0.8400 . ? C121 O121 1.416(9) . ? C121 C122 1.537(10) . ? C121 H12A 0.9900 . ? C121 H12B 0.9900 . ? C122 C124 1.531(8) . ? C122 C123 1.538(7) . ? C122 N121 1.553(7) . ? C123 H12C 0.9800 . ? C123 H12D 0.9800 . ? C123 H12E 0.9800 . ? C124 H12F 0.9800 . ? C124 H12G 0.9800 . ? C124 H12H 0.9800 . ? C125 N121 1.510(7) . ? C125 H12I 0.9800 . ? C125 H12J 0.9800 . ? C125 H12K 0.9800 . ? C126 N121 1.513(7) . ? C126 H12L 0.9800 . ? C126 H12M 0.9800 . ? C126 H12N 0.9800 . ? C127 N121 1.502(7) . ? C127 H12O 0.9800 . ? C127 H12P 0.9800 . ? C127 H12Q 0.9800 . ? O121 H121 0.8400 . ? C31 O31 1.413(8) . ? C31 C32 1.542(9) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C34 1.537(7) . ? C32 N31 1.550(7) . ? C32 C33 1.548(7) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 N31 1.512(7) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 N31 1.511(7) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 N31 1.508(7) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? O31 H31 0.8400 . ? C131 O131 1.430(9) . ? C131 C132 1.529(10) . ? C131 H13A 0.9900 . ? C131 H13B 0.9900 . ? C132 C133 1.531(7) . ? C132 C134 1.541(7) . ? C132 N131 1.555(7) . ? C133 H13C 0.9800 . ? C133 H13D 0.9800 . ? C133 H13E 0.9800 . ? C134 H13F 0.9800 . ? C134 H13G 0.9800 . ? C134 H13H 0.9800 . ? C135 N131 1.510(7) . ? C135 H13I 0.9800 . ? C135 H13J 0.9800 . ? C135 H13K 0.9800 . ? C136 N131 1.506(7) . ? C136 H13L 0.9800 . ? C136 H13M 0.9800 . ? C136 H13N 0.9800 . ? C137 N131 1.509(7) . ? C137 H13O 0.9800 . ? C137 H13P 0.9800 . ? C137 H13Q 0.9800 . ? O131 H131 0.8400 . ? C231 O231 1.423(10) . ? C231 C232 1.539(10) . ? C231 H23D 0.9900 . ? C231 H23E 0.9900 . ? C232 C234 1.537(8) . ? C232 C233 1.535(8) . ? C232 N231 1.553(8) . ? C233 H23F 0.9800 . ? C233 H23G 0.9800 . ? C233 H23H 0.9800 . ? C234 H23I 0.9800 . ? C234 H23J 0.9800 . ? C234 H23K 0.9800 . ? C235 N231 1.513(8) . ? C235 H23L 0.9800 . ? C235 H23M 0.9800 . ? C235 H23N 0.9800 . ? C236 N231 1.514(7) . ? C236 H23O 0.9800 . ? C236 H23P 0.9800 . ? C236 H23Q 0.9800 . ? C237 N231 1.508(8) . ? C237 H23R 0.9800 . ? C237 H23S 0.9800 . ? C237 H23T 0.9800 . ? O231 H231 0.8400 . ? 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 O6 B1 O4 112.1(2) . . ? O6 B1 O3 109.1(2) . . ? O4 B1 O3 108.7(2) . . ? O6 B1 O1 108.5(2) . . ? O4 B1 O1 108.9(2) . . ? O3 B1 O1 109.5(2) . . ? O1 B2 O7 122.9(3) . . ? O1 B2 O2 120.9(2) . . ? O7 B2 O2 116.2(3) . . ? O3 B3 O8 122.0(3) . . ? O3 B3 O2 121.6(3) . . ? O8 B3 O2 116.4(2) . . ? O9 B4 O4 122.0(3) . . ? O9 B4 O5 116.6(3) . . ? O4 B4 O5 121.4(3) . . ? O6 B5 O10 118.4(3) . . ? O6 B5 O5 120.9(3) . . ? O10 B5 O5 120.7(3) . . ? B2 O1 B1 122.4(2) . . ? B3 O2 B2 119.2(2) . . ? B3 O3 B1 122.4(2) . . ? B4 O4 B1 122.5(3) . . ? B4 O5 B5 119.3(3) . . ? B5 O6 B1 123.8(3) . . ? B2 O7 H7 109.5 . . ? B3 O8 H8 109.5 . . ? B4 O9 H9 109.5 . . ? B5 O10 H10 109.5 . . ? O14 B11 O16 112.2(2) . . ? O14 B11 O13 109.2(3) . . ? O16 B11 O13 108.5(2) . . ? O14 B11 O11 109.1(2) . . ? O16 B11 O11 108.2(3) . . ? O13 B11 O11 109.7(2) . . ? O11 B12 O17 122.6(3) . . ? O11 B12 O12 121.6(3) . . ? O17 B12 O12 115.8(3) . . ? O13 B13 O18 123.0(3) . . ? O13 B13 O12 120.4(3) . . ? O18 B13 O12 116.6(3) . . ? O14 B14 O19 121.0(3) . . ? O14 B14 O15 121.8(3) . . ? O19 B14 O15 117.3(3) . . ? O16 B15 O20 118.1(3) . . ? O16 B15 O15 121.0(3) . . ? O20 B15 O15 120.9(3) . . ? B12 O11 B11 122.9(2) . . ? B12 O12 B13 119.7(2) . . ? B13 O13 B11 124.0(2) . . ? B14 O14 B11 123.0(3) . . ? B15 O15 B14 119.2(3) . . ? B15 O16 B11 123.0(3) . . ? B12 O17 H17 109.5 . . ? B13 O18 H18 109.5 . . ? B14 O19 H19A 109.5 . . ? B14 O19 H19B 109.5 . . ? B15 O20 H20 109.5 . . ? O21 C21 C22 111.4(5) . . ? O21 C21 H21A 109.4 . . ? C22 C21 H21A 109.4 . . ? O21 C21 H21B 109.4 . . ? C22 C21 H21B 109.4 . . ? H21A C21 H21B 108.0 . . ? C24 C22 C21 108.5(5) . . ? C24 C22 C23 111.5(7) . . ? C21 C22 C23 107.6(6) . . ? C24 C22 N21 110.0(5) . . ? C21 C22 N21 109.7(5) . . ? C23 C22 N21 109.6(5) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N21 C25 H25A 109.5 . . ? N21 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N21 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N21 C26 H26A 109.5 . . ? N21 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N21 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N21 C27 H27A 109.5 . . ? N21 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N21 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C27 N21 C26 107.3(7) . . ? C27 N21 C25 107.5(8) . . ? C26 N21 C25 105.6(8) . . ? C27 N21 C22 112.1(5) . . ? C26 N21 C22 112.8(5) . . ? C25 N21 C22 111.3(5) . . ? O121 C121 C122 109.6(7) . . ? O121 C121 H12A 109.7 . . ? C122 C121 H12A 109.7 . . ? O121 C121 H12B 109.7 . . ? C122 C121 H12B 109.7 . . ? H12A C121 H12B 108.2 . . ? C124 C122 C123 113.3(9) . . ? C124 C122 C121 109.1(8) . . ? C123 C122 C121 104.4(7) . . ? C124 C122 N121 111.1(7) . . ? C123 C122 N121 106.7(6) . . ? C121 C122 N121 112.1(7) . . ? C122 C123 H12C 109.5 . . ? C122 C123 H12D 109.5 . . ? H12C C123 H12D 109.5 . . ? C122 C123 H12E 109.5 . . ? H12C C123 H12E 109.5 . . ? H12D C123 H12E 109.5 . . ? C122 C124 H12F 109.5 . . ? C122 C124 H12G 109.5 . . ? H12F C124 H12G 109.5 . . ? C122 C124 H12H 109.5 . . ? H12F C124 H12H 109.5 . . ? H12G C124 H12H 109.5 . . ? N121 C125 H12I 109.5 . . ? N121 C125 H12J 109.5 . . ? H12I C125 H12J 109.5 . . ? N121 C125 H12K 109.5 . . ? H12I C125 H12K 109.5 . . ? H12J C125 H12K 109.5 . . ? N121 C126 H12L 109.5 . . ? N121 C126 H12M 109.5 . . ? H12L C126 H12M 109.5 . . ? N121 C126 H12N 109.5 . . ? H12L C126 H12N 109.5 . . ? H12M C126 H12N 109.5 . . ? N121 C127 H12O 109.5 . . ? N121 C127 H12P 109.5 . . ? H12O C127 H12P 109.5 . . ? N121 C127 H12Q 109.5 . . ? H12O C127 H12Q 109.5 . . ? H12P C127 H12Q 109.5 . . ? C127 N121 C125 106.7(8) . . ? C127 N121 C126 107.9(8) . . ? C125 N121 C126 105.0(7) . . ? C127 N121 C122 111.9(7) . . ? C125 N121 C122 113.7(7) . . ? C126 N121 C122 111.2(7) . . ? C121 O121 H121 109.5 . . ? O31 C31 C32 109.3(7) . . ? O31 C31 H31A 109.8 . . ? C32 C31 H31A 109.8 . . ? O31 C31 H31B 109.8 . . ? C32 C31 H31B 109.8 . . ? H31A C31 H31B 108.3 . . ? C34 C32 C31 107.4(7) . . ? C34 C32 N31 110.2(6) . . ? C31 C32 N31 113.0(7) . . ? C34 C32 C33 112.2(8) . . ? C31 C32 C33 104.1(7) . . ? N31 C32 C33 109.8(6) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N31 C35 H35A 109.5 . . ? N31 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N31 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N31 C36 H36A 109.5 . . ? N31 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N31 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N31 C37 H37A 109.5 . . ? N31 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? N31 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C37 N31 C35 105.4(7) . . ? C37 N31 C36 105.6(7) . . ? C35 N31 C36 106.4(7) . . ? C37 N31 C32 112.8(6) . . ? C35 N31 C32 113.0(6) . . ? C36 N31 C32 113.1(6) . . ? O131 C131 C132 109.5(7) . . ? O131 C131 H13A 109.8 . . ? C132 C131 H13A 109.8 . . ? O131 C131 H13B 109.8 . . ? C132 C131 H13B 109.8 . . ? H13A C131 H13B 108.2 . . ? C133 C132 C131 107.6(7) . . ? C133 C132 C134 112.7(8) . . ? C131 C132 C134 107.6(7) . . ? C133 C132 N131 107.9(6) . . ? C131 C132 N131 111.7(8) . . ? C134 C132 N131 109.4(7) . . ? C132 C133 H13C 109.5 . . ? C132 C133 H13D 109.5 . . ? H13C C133 H13D 109.5 . . ? C132 C133 H13E 109.5 . . ? H13C C133 H13E 109.5 . . ? H13D C133 H13E 109.5 . . ? C132 C134 H13F 109.5 . . ? C132 C134 H13G 109.5 . . ? H13F C134 H13G 109.5 . . ? C132 C134 H13H 109.5 . . ? H13F C134 H13H 109.5 . . ? H13G C134 H13H 109.5 . . ? N131 C135 H13I 109.5 . . ? N131 C135 H13J 109.5 . . ? H13I C135 H13J 109.5 . . ? N131 C135 H13K 109.5 . . ? H13I C135 H13K 109.5 . . ? H13J C135 H13K 109.5 . . ? N131 C136 H13L 109.5 . . ? N131 C136 H13M 109.5 . . ? H13L C136 H13M 109.5 . . ? N131 C136 H13N 109.5 . . ? H13L C136 H13N 109.5 . . ? H13M C136 H13N 109.5 . . ? N131 C137 H13O 109.5 . . ? N131 C137 H13P 109.5 . . ? H13O C137 H13P 109.5 . . ? N131 C137 H13Q 109.5 . . ? H13O C137 H13Q 109.5 . . ? H13P C137 H13Q 109.5 . . ? C136 N131 C135 106.7(8) . . ? C136 N131 C137 107.8(7) . . ? C135 N131 C137 106.1(8) . . ? C136 N131 C132 112.0(7) . . ? C135 N131 C132 112.8(6) . . ? C137 N131 C132 111.1(7) . . ? C131 O131 H131 109.5 . . ? O231 C231 C232 108.2(11) . . ? O231 C231 H23D 110.1 . . ? C232 C231 H23D 110.1 . . ? O231 C231 H23E 110.1 . . ? C232 C231 H23E 110.1 . . ? H23D C231 H23E 108.4 . . ? C234 C232 C233 112.8(11) . . ? C234 C232 C231 108.7(10) . . ? C233 C232 C231 105.1(9) . . ? C234 C232 N231 109.9(9) . . ? C233 C232 N231 109.3(9) . . ? C231 C232 N231 111.0(10) . . ? C232 C233 H23F 109.5 . . ? C232 C233 H23G 109.5 . . ? H23F C233 H23G 109.5 . . ? C232 C233 H23H 109.5 . . ? H23F C233 H23H 109.5 . . ? H23G C233 H23H 109.5 . . ? C232 C234 H23I 109.5 . . ? C232 C234 H23J 109.5 . . ? H23I C234 H23J 109.5 . . ? C232 C234 H23K 109.5 . . ? H23I C234 H23K 109.5 . . ? H23J C234 H23K 109.5 . . ? N231 C235 H23L 109.5 . . ? N231 C235 H23M 109.5 . . ? H23L C235 H23M 109.5 . . ? N231 C235 H23N 109.5 . . ? H23L C235 H23N 109.5 . . ? H23M C235 H23N 109.5 . . ? N231 C236 H23O 109.5 . . ? N231 C236 H23P 109.5 . . ? H23O C236 H23P 109.5 . . ? N231 C236 H23Q 109.5 . . ? H23O C236 H23Q 109.5 . . ? H23P C236 H23Q 109.5 . . ? N231 C237 H23R 109.5 . . ? N231 C237 H23S 109.5 . . ? H23R C237 H23S 109.5 . . ? N231 C237 H23T 109.5 . . ? H23R C237 H23T 109.5 . . ? H23S C237 H23T 109.5 . . ? C237 N231 C236 107.6(10) . . ? C237 N231 C235 106.2(10) . . ? C236 N231 C235 106.0(10) . . ? C237 N231 C232 111.4(10) . . ? C236 N231 C232 111.8(9) . . ? C235 N231 C232 113.5(9) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O7 H7 O11 0.84 1.92 2.751(3) 172.6 1_655 O8 H8 O13 0.84 1.84 2.668(3) 167.4 . O9 H9 O4 0.84 1.93 2.754(3) 165.2 3_665 O10 H10 O8 0.84 1.89 2.708(3) 162.9 2_655 O17 H17 O1 0.84 1.88 2.709(3) 170.3 1_455 O18 H18 O3 0.84 1.90 2.728(3) 170.8 . O19 H19A O19 0.84 2.11 2.735(6) 131.3 3 O19 H19B O131 0.84 1.70 2.522(8) 165.4 1_545 O20 H20 O17 0.84 1.96 2.789(3) 170.9 2_545 O21 H21 O10 0.84 1.78 2.599(6) 164.2 2_655 O121 H121 O16 0.84 1.76 2.567(7) 160.6 2_655 O31 H31 O6 0.84 1.82 2.655(8) 170.2 2_655 O131 H131 O121 0.84 1.74 2.570(11) 170.4 1_455 O231 H231 O1 0.84 1.97 2.58(2) 128.0 3_665 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.861 _refine_diff_density_min -0.512 _refine_diff_density_rms 0.067 #===END data_1i #TrackingRef 'pentaborates.CIF' _database_code_depnum_ccdc_archive 'CCDC 764927' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H18 B5 N O11' _chemical_formula_weight 334.26 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' _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 9.4232(2) _cell_length_b 16.6235(3) _cell_length_c 9.5934(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.6780(10) _cell_angle_gamma 90.00 _cell_volume 1492.58(5) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 3493 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.488 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 696 _exptl_absorpt_coefficient_mu 0.131 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9717 _exptl_absorpt_correction_T_max 0.9935 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2003)' _exptl_special_details ; SADABS was used to perform the Absorption correction Parameter refinement on 13815 reflections reduced R(int) from 0.0702 to 0.0383 Ratio of minimum to maximum apparent transmission: 0.906795 The given Tmin and Tmax were generated using the SHELX SIZE command ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14757 _diffrn_reflns_av_R_equivalents 0.0370 _diffrn_reflns_av_sigmaI/netI 0.0299 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.25 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3410 _reflns_number_gt 2915 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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^)+(0.0201P)^2^+1.1900P] 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 3410 _refine_ls_number_parameters 214 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0509 _refine_ls_R_factor_gt 0.0422 _refine_ls_wR_factor_ref 0.0953 _refine_ls_wR_factor_gt 0.0892 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _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 0.78840(16) 0.12539(10) 0.35942(16) 0.0155(3) Uani 1 1 d . . . B2 B 0.53663(17) 0.08377(10) 0.36288(17) 0.0169(3) Uani 1 1 d . . . B3 B 0.62649(17) 0.18995(10) 0.51466(17) 0.0180(3) Uani 1 1 d . . . B4 B 1.04424(17) 0.08586(10) 0.36543(17) 0.0168(3) Uani 1 1 d . . . B5 B 0.95314(17) 0.18381(10) 0.19900(17) 0.0170(3) Uani 1 1 d . . . O1 O 0.66686(10) 0.07335(6) 0.31887(10) 0.0176(2) Uani 1 1 d . . . O2 O 0.51271(10) 0.14335(6) 0.45830(11) 0.0204(2) Uani 1 1 d . . . O3 O 0.75810(10) 0.18136(6) 0.47214(10) 0.0177(2) Uani 1 1 d . . . O4 O 0.91436(10) 0.07704(6) 0.41176(10) 0.0166(2) Uani 1 1 d . . . O5 O 1.06881(10) 0.14344(6) 0.26715(11) 0.0193(2) Uani 1 1 d . . . O6 O 0.82008(10) 0.17364(6) 0.23699(10) 0.0179(2) Uani 1 1 d . . . O7 O 0.42760(11) 0.03492(7) 0.31003(11) 0.0226(2) Uani 1 1 d . . . H7 H 0.3540 0.0460 0.3479 0.034 Uiso 1 1 calc R . . O8 O 0.59891(11) 0.24492(7) 0.61260(12) 0.0251(3) Uani 1 1 d . . . H8 H 0.6750 0.2685 0.6433 0.038 Uiso 1 1 calc R . . O9 O 1.15914(10) 0.04016(6) 0.41550(11) 0.0200(2) Uani 1 1 d . . . H9 H 1.1340 0.0059 0.4721 0.030 Uiso 1 1 calc R . . O10 O 0.98095(11) 0.23333(7) 0.09298(11) 0.0243(2) Uani 1 1 d . . . H10 H 0.9054 0.2567 0.0601 0.036 Uiso 1 1 calc R . . C11 C 0.31953(19) 0.45120(10) 0.45165(17) 0.0286(4) Uani 1 1 d . . . H11A H 0.3840 0.4480 0.5406 0.034 Uiso 1 1 calc R . . H11B H 0.3573 0.4929 0.3921 0.034 Uiso 1 1 calc R . . C12 C 0.1725(2) 0.47495(12) 0.4825(2) 0.0376(4) Uani 1 1 d . . . H12A H 0.1381 0.4359 0.5489 0.045 Uiso 1 1 calc R . . H12B H 0.1766 0.5286 0.5277 0.045 Uiso 1 1 calc R . . C13 C 0.0646(2) 0.40095(12) 0.2921(2) 0.0400(5) Uani 1 1 d . . . H13A H -0.0059 0.4033 0.2073 0.048 Uiso 1 1 calc R . . H13B H 0.0307 0.3609 0.3572 0.048 Uiso 1 1 calc R . . C14 C 0.2063(2) 0.37516(11) 0.25194(18) 0.0342(4) Uani 1 1 d . . . H14A H 0.2375 0.4136 0.1828 0.041 Uiso 1 1 calc R . . H14B H 0.1967 0.3215 0.2070 0.041 Uiso 1 1 calc R . . C15 C 0.28859(19) 0.30355(11) 0.4735(2) 0.0334(4) Uani 1 1 d . . . H15A H 0.2872 0.2526 0.4220 0.050 Uiso 1 1 calc R . . H15B H 0.1958 0.3119 0.5080 0.050 Uiso 1 1 calc R . . H15C H 0.3638 0.3018 0.5531 0.050 Uiso 1 1 calc R . . C16 C 0.4607(2) 0.35820(12) 0.3290(2) 0.0419(5) Uani 1 1 d . . . H16A H 0.4598 0.3077 0.2762 0.063 Uiso 1 1 calc R . . H16B H 0.5337 0.3553 0.4104 0.063 Uiso 1 1 calc R . . H16C H 0.4824 0.4030 0.2685 0.063 Uiso 1 1 calc R . . N11 N 0.31758(14) 0.37131(8) 0.37783(14) 0.0257(3) Uani 1 1 d . . . O11 O 0.07484(14) 0.47733(8) 0.35758(14) 0.0396(3) 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 0.0138(7) 0.0165(7) 0.0166(7) 0.0002(6) 0.0030(6) -0.0001(6) B2 0.0157(7) 0.0176(7) 0.0171(7) 0.0009(6) 0.0016(6) 0.0008(6) B3 0.0150(7) 0.0203(8) 0.0190(8) -0.0003(6) 0.0034(6) 0.0006(6) B4 0.0147(7) 0.0188(8) 0.0171(7) -0.0003(6) 0.0027(6) -0.0010(6) B5 0.0162(7) 0.0175(7) 0.0176(7) -0.0001(6) 0.0031(6) 0.0007(6) O1 0.0136(5) 0.0198(5) 0.0198(5) -0.0031(4) 0.0040(4) -0.0010(4) O2 0.0136(5) 0.0240(5) 0.0241(5) -0.0073(4) 0.0044(4) -0.0016(4) O3 0.0138(5) 0.0200(5) 0.0199(5) -0.0037(4) 0.0039(4) -0.0015(4) O4 0.0134(5) 0.0190(5) 0.0179(5) 0.0026(4) 0.0034(4) 0.0015(4) O5 0.0136(5) 0.0218(5) 0.0229(5) 0.0060(4) 0.0043(4) 0.0009(4) O6 0.0138(5) 0.0215(5) 0.0189(5) 0.0043(4) 0.0035(4) 0.0019(4) O7 0.0142(5) 0.0264(6) 0.0279(6) -0.0083(5) 0.0056(4) -0.0023(4) O8 0.0149(5) 0.0317(6) 0.0296(6) -0.0139(5) 0.0059(4) -0.0036(4) O9 0.0136(5) 0.0233(5) 0.0236(5) 0.0076(4) 0.0047(4) 0.0016(4) O10 0.0168(5) 0.0300(6) 0.0270(6) 0.0119(5) 0.0067(4) 0.0047(4) C11 0.0338(9) 0.0290(8) 0.0234(8) 0.0016(7) 0.0053(7) -0.0020(7) C12 0.0478(11) 0.0350(10) 0.0325(9) 0.0022(8) 0.0155(8) 0.0098(8) C13 0.0325(10) 0.0417(11) 0.0434(11) 0.0158(9) -0.0052(8) -0.0001(8) C14 0.0441(11) 0.0331(9) 0.0248(8) 0.0009(7) 0.0014(7) -0.0036(8) C15 0.0271(9) 0.0320(9) 0.0433(10) 0.0163(8) 0.0132(7) 0.0059(7) C16 0.0378(10) 0.0404(11) 0.0528(12) 0.0161(9) 0.0286(9) 0.0117(8) N11 0.0260(7) 0.0257(7) 0.0269(7) 0.0048(6) 0.0093(6) 0.0030(5) O11 0.0359(7) 0.0413(8) 0.0432(8) 0.0156(6) 0.0115(6) 0.0144(6) _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 O1 1.4518(18) . ? B1 O4 1.4725(18) . ? B1 O3 1.4793(18) . ? B1 O6 1.4811(18) . ? B2 O1 1.3545(18) . ? B2 O7 1.3605(19) . ? B2 O2 1.3849(19) . ? B3 O8 1.3572(19) . ? B3 O3 1.3574(18) . ? B3 O2 1.3811(19) . ? B4 O4 1.3578(18) . ? B4 O9 1.3635(19) . ? B4 O5 1.3819(19) . ? B5 O6 1.3564(18) . ? B5 O10 1.3574(19) . ? B5 O5 1.3784(18) . ? O7 H7 0.8400 . ? O8 H8 0.8400 . ? O9 H9 0.8400 . ? O10 H10 0.8400 . ? C11 C12 1.503(2) . ? C11 N11 1.504(2) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 O11 1.424(2) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 O11 1.415(3) . ? C13 C14 1.495(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 N11 1.506(2) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 N11 1.498(2) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 N11 1.494(2) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 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 O1 B1 O4 110.22(12) . . ? O1 B1 O3 110.94(11) . . ? O4 B1 O3 108.09(11) . . ? O1 B1 O6 109.61(11) . . ? O4 B1 O6 109.70(11) . . ? O3 B1 O6 108.24(11) . . ? O1 B2 O7 118.68(13) . . ? O1 B2 O2 121.37(13) . . ? O7 B2 O2 119.95(13) . . ? O8 B3 O3 122.28(14) . . ? O8 B3 O2 116.50(13) . . ? O3 B3 O2 121.21(13) . . ? O4 B4 O9 122.25(13) . . ? O4 B4 O5 121.80(13) . . ? O9 B4 O5 115.92(12) . . ? O6 B5 O10 122.81(13) . . ? O6 B5 O5 121.10(13) . . ? O10 B5 O5 116.09(13) . . ? B2 O1 B1 123.74(12) . . ? B3 O2 B2 118.77(12) . . ? B3 O3 B1 123.14(12) . . ? B4 O4 B1 123.44(11) . . ? B5 O5 B4 118.35(12) . . ? B5 O6 B1 123.95(11) . . ? B2 O7 H7 109.5 . . ? B3 O8 H8 109.5 . . ? B4 O9 H9 109.5 . . ? B5 O10 H10 109.5 . . ? C12 C11 N11 111.32(14) . . ? C12 C11 H11A 109.4 . . ? N11 C11 H11A 109.4 . . ? C12 C11 H11B 109.4 . . ? N11 C11 H11B 109.4 . . ? H11A C11 H11B 108.0 . . ? O11 C12 C11 111.20(14) . . ? O11 C12 H12A 109.4 . . ? C11 C12 H12A 109.4 . . ? O11 C12 H12B 109.4 . . ? C11 C12 H12B 109.4 . . ? H12A C12 H12B 108.0 . . ? O11 C13 C14 110.81(16) . . ? O11 C13 H13A 109.5 . . ? C14 C13 H13A 109.5 . . ? O11 C13 H13B 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? C13 C14 N11 111.39(14) . . ? C13 C14 H14A 109.3 . . ? N11 C14 H14A 109.3 . . ? C13 C14 H14B 109.3 . . ? N11 C14 H14B 109.3 . . ? H14A C14 H14B 108.0 . . ? N11 C15 H15A 109.5 . . ? N11 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N11 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N11 C16 H16A 109.5 . . ? N11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C16 N11 C15 108.53(13) . . ? C16 N11 C11 108.31(14) . . ? C15 N11 C11 111.63(13) . . ? C16 N11 C14 108.94(14) . . ? C15 N11 C14 111.33(14) . . ? C11 N11 C14 108.02(13) . . ? C13 O11 C12 110.64(14) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O7 H7 O9 0.84 2.02 2.8331(14) 162.8 1_455 O8 H8 O6 0.84 1.82 2.6499(14) 168.8 4_566 O9 H9 O4 0.84 1.86 2.6998(14) 174.8 3_756 O10 H10 O3 0.84 1.85 2.6831(14) 170.7 4_565 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.277 _refine_diff_density_min -0.240 _refine_diff_density_rms 0.047 #===END data_1g #TrackingRef 'pentaborates.CIF' #For reference _database_code_depnum_ccdc_archive 'CCDC 764928' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H11 B5 N2 O10' _chemical_formula_weight 301.20 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' _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 8.5734(4) _cell_length_b 11.3879(8) _cell_length_c 13.5143(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.058(3) _cell_angle_gamma 90.00 _cell_volume 1319.44(13) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 2704 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description 'Cut Block' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.516 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 616 _exptl_absorpt_coefficient_mu 0.136 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9785 _exptl_absorpt_correction_T_max 0.9919 _exptl_absorpt_process_details 'SADABS 2007/2 (Sheldrick, G.M., 2007)' _exptl_special_details ; SADABS was used to perform the Absorption correction Estimated minimum and maximum transmission: 0.6427 0.7456 The given Tmin and Tmax were generated using the SHELX SIZE command ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius APEX II CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9523 _diffrn_reflns_av_R_equivalents 0.0398 _diffrn_reflns_av_sigmaI/netI 0.0430 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 27.47 _reflns_number_total 2973 _reflns_number_gt 2341 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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^)+(0.0305P)^2^+2.0187P] 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 2973 _refine_ls_number_parameters 195 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0775 _refine_ls_R_factor_gt 0.0590 _refine_ls_wR_factor_ref 0.1341 _refine_ls_wR_factor_gt 0.1216 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _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 1.1249(3) 0.5419(2) 0.7091(2) 0.0233(5) Uani 1 1 d . . . B2 B 0.9251(3) 0.6425(2) 0.8131(2) 0.0249(5) Uani 1 1 d . . . B3 B 0.9555(3) 0.4363(2) 0.8305(2) 0.0250(5) Uani 1 1 d . . . B4 B 1.2247(3) 0.5029(2) 0.5402(2) 0.0253(6) Uani 1 1 d . . . B5 B 1.4047(3) 0.5503(2) 0.66901(19) 0.0234(5) Uani 1 1 d . . . O1 O 1.03060(18) 0.64461(14) 0.73875(12) 0.0252(4) Uani 1 1 d . . . O2 O 0.8896(2) 0.53964(14) 0.86258(12) 0.0293(4) Uani 1 1 d . . . O3 O 1.06695(18) 0.43493(14) 0.75973(12) 0.0243(4) Uani 1 1 d . . . O4 O 1.10330(17) 0.52453(14) 0.60198(11) 0.0233(4) Uani 1 1 d . . . O5 O 1.37602(19) 0.51556(17) 0.57268(12) 0.0333(4) Uani 1 1 d . . . O6 O 1.28720(18) 0.56127(14) 0.73501(11) 0.0253(4) Uani 1 1 d . . . O7 O 0.8486(2) 0.74059(15) 0.84341(13) 0.0335(4) Uani 1 1 d . . . H7 H 0.8811 0.7989 0.8114 0.050 Uiso 1 1 calc R . . O8 O 0.9032(2) 0.33550(15) 0.87361(13) 0.0333(4) Uani 1 1 d . . . H8 H 0.9317 0.2775 0.8398 0.050 Uiso 1 1 calc R . . O9 O 1.20440(19) 0.46910(17) 0.44455(12) 0.0323(4) Uani 1 1 d . . . H9 H 1.1086 0.4633 0.4323 0.048 Uiso 1 1 calc R . . O10 O 1.55439(18) 0.57188(16) 0.69827(12) 0.0296(4) Uani 1 1 d . . . H10 H 1.6150 0.5617 0.6502 0.044 Uiso 1 1 calc R . . C1 C 0.5384(3) 0.2950(2) 1.03249(19) 0.0325(6) Uani 1 1 d . . . C2 C 0.5018(4) 0.3974(3) 0.8964(2) 0.0462(7) Uani 1 1 d . . . H2 H 0.5222 0.4393 0.8371 0.055 Uiso 1 1 calc R . . C3 C 0.3636(4) 0.3804(3) 0.9385(2) 0.0483(8) Uani 1 1 d . . . H3 H 0.2658 0.4070 0.9142 0.058 Uiso 1 1 calc R . . C4 C 0.6113(4) 0.2303(3) 1.1155(2) 0.0515(8) Uani 1 1 d . . . H4A H 0.7234 0.2471 1.1172 0.077 Uiso 1 1 calc R . . H4B H 0.5951 0.1458 1.1063 0.077 Uiso 1 1 calc R . . H4C H 0.5636 0.2551 1.1780 0.077 Uiso 1 1 calc R . . N1 N 0.6099(3) 0.3417(2) 0.95630(16) 0.0368(5) Uani 1 1 d . . . H1 H 0.7108 0.3382 0.9450 0.044 Uiso 1 1 calc R . . N2 N 0.3886(3) 0.3168(2) 1.02425(18) 0.0401(6) Uani 1 1 d . . . H2A H 0.3161 0.2946 1.0663 0.048 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 0.0229(12) 0.0185(13) 0.0287(13) -0.0017(10) 0.0092(10) 0.0001(10) B2 0.0250(12) 0.0191(13) 0.0306(13) -0.0003(10) 0.0105(10) -0.0007(10) B3 0.0240(12) 0.0209(13) 0.0300(13) 0.0000(10) 0.0093(10) 0.0000(10) B4 0.0232(12) 0.0243(13) 0.0285(13) -0.0001(11) 0.0080(10) -0.0008(11) B5 0.0242(12) 0.0202(13) 0.0257(13) -0.0003(10) 0.0085(10) -0.0019(10) O1 0.0278(8) 0.0163(8) 0.0313(9) 0.0003(7) 0.0142(7) 0.0002(7) O2 0.0335(9) 0.0196(8) 0.0347(9) 0.0006(7) 0.0206(7) 0.0000(7) O3 0.0250(8) 0.0176(8) 0.0304(9) -0.0008(6) 0.0121(7) 0.0006(6) O4 0.0212(8) 0.0220(8) 0.0268(8) -0.0015(6) 0.0080(6) 0.0009(6) O5 0.0206(8) 0.0518(12) 0.0276(9) -0.0088(8) 0.0077(7) 0.0001(8) O6 0.0232(8) 0.0260(9) 0.0268(8) -0.0039(7) 0.0079(6) -0.0032(7) O7 0.0385(10) 0.0178(8) 0.0444(11) 0.0007(7) 0.0256(8) 0.0008(7) O8 0.0383(10) 0.0173(8) 0.0442(11) 0.0002(7) 0.0239(8) 0.0012(7) O9 0.0196(8) 0.0488(11) 0.0286(9) -0.0075(8) 0.0063(7) 0.0002(8) O10 0.0233(8) 0.0371(10) 0.0285(9) -0.0041(7) 0.0078(7) -0.0031(7) C1 0.0380(14) 0.0241(13) 0.0356(13) -0.0047(10) 0.0099(11) -0.0027(11) C2 0.0617(19) 0.0429(17) 0.0342(15) 0.0061(13) 0.0059(13) 0.0015(15) C3 0.0380(15) 0.0508(19) 0.0560(19) 0.0100(15) -0.0058(13) 0.0049(14) C4 0.081(2) 0.0280(15) 0.0453(17) -0.0012(13) -0.0201(16) 0.0009(15) N1 0.0303(11) 0.0372(13) 0.0430(13) -0.0037(10) 0.0157(10) -0.0032(10) N2 0.0342(12) 0.0396(13) 0.0466(14) -0.0007(11) 0.0203(10) -0.0034(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 B1 O6 1.451(3) . ? B1 O4 1.472(3) . ? B1 O1 1.478(3) . ? B1 O3 1.483(3) . ? B2 O1 1.352(3) . ? B2 O7 1.359(3) . ? B2 O2 1.383(3) . ? B3 O3 1.352(3) . ? B3 O8 1.364(3) . ? B3 O2 1.376(3) . ? B4 O4 1.357(3) . ? B4 O9 1.360(3) . ? B4 O5 1.377(3) . ? B5 O6 1.352(3) . ? B5 O10 1.365(3) . ? B5 O5 1.383(3) . ? O7 H7 0.8400 . ? O8 H8 0.8400 . ? O9 H9 0.8400 . ? O10 H10 0.8400 . ? C1 N1 1.311(3) . ? C1 N2 1.313(3) . ? C1 C4 1.481(4) . ? C2 C3 1.328(4) . ? C2 N1 1.383(4) . ? C2 H2 0.9500 . ? C3 N2 1.383(4) . ? C3 H3 0.9500 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? N1 H1 0.8800 . ? N2 H2A 0.8800 . ? 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 O6 B1 O4 112.18(18) . . ? O6 B1 O1 109.78(19) . . ? O4 B1 O1 107.73(19) . . ? O6 B1 O3 109.58(19) . . ? O4 B1 O3 107.57(19) . . ? O1 B1 O3 109.95(17) . . ? O1 B2 O7 122.2(2) . . ? O1 B2 O2 121.5(2) . . ? O7 B2 O2 116.3(2) . . ? O3 B3 O8 121.7(2) . . ? O3 B3 O2 121.6(2) . . ? O8 B3 O2 116.7(2) . . ? O4 B4 O9 122.6(2) . . ? O4 B4 O5 120.5(2) . . ? O9 B4 O5 116.9(2) . . ? O6 B5 O10 119.6(2) . . ? O6 B5 O5 121.1(2) . . ? O10 B5 O5 119.4(2) . . ? B2 O1 B1 123.63(19) . . ? B3 O2 B2 118.75(18) . . ? B3 O3 B1 123.65(18) . . ? B4 O4 B1 122.22(19) . . ? B4 O5 B5 119.77(19) . . ? B5 O6 B1 122.77(19) . . ? B2 O7 H7 109.5 . . ? B3 O8 H8 109.5 . . ? B4 O9 H9 109.5 . . ? B5 O10 H10 109.5 . . ? N1 C1 N2 108.3(2) . . ? N1 C1 C4 126.9(3) . . ? N2 C1 C4 124.8(3) . . ? C3 C2 N1 106.3(3) . . ? C3 C2 H2 126.9 . . ? N1 C2 H2 126.9 . . ? C2 C3 N2 107.3(3) . . ? C2 C3 H3 126.4 . . ? N2 C3 H3 126.4 . . ? 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 . . ? C1 N1 C2 109.4(2) . . ? C1 N1 H1 125.3 . . ? C2 N1 H1 125.3 . . ? C1 N2 C3 108.7(2) . . ? C1 N2 H2A 125.6 . . ? C3 N2 H2A 125.6 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O7 H7 O3 0.84 1.88 2.714(2) 174.2 2_756 O8 H8 O1 0.84 1.88 2.712(2) 173.0 2_746 O9 H9 O4 0.84 1.88 2.712(2) 170.7 3_766 O10 H10 O9 0.84 2.04 2.868(2) 168.2 3_866 N1 H1 O8 0.88 1.91 2.754(3) 159.6 . N2 H2A O7 0.88 1.91 2.787(3) 175.2 3_667 _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.535 _refine_diff_density_min -0.330 _refine_diff_density_rms 0.060 #===END