# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email m.a.beckett@bangor.ac.uk _publ_contact_author_name 'Michael A. Beckett' loop_ _publ_author_name M.Beckett P.Horton M.Hursthouse J.Timmis.K.Varma data_1 _database_code_depnum_ccdc_archive 'CCDC 846310' #TrackingRef 'web_deposit_cif_file_0_PeterNHorton_1317124519.borates1.cif' #Dr. M. Beckett/ James Timmis _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C3 H12 B5 N O10' _chemical_formula_weight 276.19 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 8.0079(2) _cell_length_b 8.8634(3) _cell_length_c 8.8643(2) _cell_angle_alpha 67.429(2) _cell_angle_beta 88.975(2) _cell_angle_gamma 75.9650(10) _cell_volume 561.64(3) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 2522 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description Slab _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.62 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.633 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 284 _exptl_absorpt_coefficient_mu 0.149 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9131 _exptl_absorpt_correction_T_max 0.9794 _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: 0.6932 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 graphite _diffrn_measurement_device_type 'Bruker-Nonius Roper 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 12353 _diffrn_reflns_av_R_equivalents 0.0274 _diffrn_reflns_av_sigmaI/netI 0.0232 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2571 _reflns_number_gt 2284 _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, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0383P)^2^+0.1789P] 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 2571 _refine_ls_number_parameters 177 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0361 _refine_ls_R_factor_gt 0.0317 _refine_ls_wR_factor_ref 0.0821 _refine_ls_wR_factor_gt 0.0792 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _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 0.26952(15) 0.36925(15) 0.28296(14) 0.0116(2) Uani 1 1 d . . . B2 B 0.04071(16) 0.26914(15) 0.19142(15) 0.0141(2) Uani 1 1 d . . . B3 B 0.26009(15) 0.06857(15) 0.39451(15) 0.0125(2) Uani 1 1 d . . . B4 B 0.46353(15) 0.56396(15) 0.19625(15) 0.0125(2) Uani 1 1 d . . . B5 B 0.28217(15) 0.57572(15) 0.40878(15) 0.0128(2) Uani 1 1 d . . . O1 O 0.11912(10) 0.39461(9) 0.17607(9) 0.01426(17) Uani 1 1 d . . . O2 O 0.10398(10) 0.10788(10) 0.30862(10) 0.01609(18) Uani 1 1 d . . . O3 O 0.34556(9) 0.18877(9) 0.37801(9) 0.01269(17) Uani 1 1 d . . . O4 O 0.39715(9) 0.44367(9) 0.17843(9) 0.01237(17) Uani 1 1 d . . . O5 O 0.41242(10) 0.62744(9) 0.31457(9) 0.01453(18) Uani 1 1 d . . . O6 O 0.21384(10) 0.45401(9) 0.39543(9) 0.01341(17) Uani 1 1 d . . . O7 O -0.09579(11) 0.29593(10) 0.08845(11) 0.0210(2) Uani 1 1 d . . . H7 H -0.1164 0.3947 0.0166 0.032 Uiso 1 1 calc R . . O8 O 0.32840(10) -0.09597(9) 0.49333(10) 0.01643(18) Uani 1 1 d . . . H8 H 0.4298 -0.1085 0.5282 0.025 Uiso 1 1 calc R . . O9 O 0.58239(10) 0.62971(10) 0.09798(9) 0.01547(18) Uani 1 1 d . . . H9 H 0.5946 0.5946 0.0219 0.023 Uiso 1 1 calc R . . O10 O 0.21149(11) 0.64428(10) 0.51472(10) 0.01793(18) Uani 1 1 d . . . H10 H 0.2530 0.7253 0.5065 0.027 Uiso 1 1 calc R . . C1 C 0.84374(15) 0.86675(14) 0.20610(14) 0.0184(2) Uani 1 1 d . . . H1 H 0.9397 0.8985 0.2477 0.022 Uiso 1 1 calc R . . C2 C 0.66946(17) 0.98607(16) 0.17460(16) 0.0239(3) Uani 1 1 d . . . H2A H 0.6576 1.0889 0.1974 0.029 Uiso 1 1 calc R . . H2B H 0.5680 0.9378 0.1964 0.029 Uiso 1 1 calc R . . C3 C 0.77014(17) 0.97321(16) 0.03425(15) 0.0241(3) Uani 1 1 d . . . H3A H 0.7308 0.9169 -0.0305 0.029 Uiso 1 1 calc R . . H3B H 0.8204 1.0681 -0.0295 0.029 Uiso 1 1 calc R . . N1 N 0.85032(12) 0.68556(12) 0.26883(12) 0.0163(2) Uani 1 1 d . . . H1A H 0.8388 0.6468 0.3785 0.024 Uiso 1 1 calc R . . H1B H 0.9534 0.6278 0.2498 0.024 Uiso 1 1 calc R . . H1C H 0.7629 0.6700 0.2169 0.024 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 0.0127(5) 0.0106(5) 0.0121(5) -0.0042(4) 0.0001(4) -0.0043(4) B2 0.0135(6) 0.0134(6) 0.0158(6) -0.0056(5) -0.0002(4) -0.0046(4) B3 0.0132(5) 0.0123(6) 0.0132(5) -0.0060(4) 0.0013(4) -0.0039(4) B4 0.0122(5) 0.0121(5) 0.0125(5) -0.0037(4) -0.0017(4) -0.0033(4) B5 0.0123(5) 0.0116(5) 0.0135(6) -0.0036(4) -0.0008(4) -0.0034(4) O1 0.0142(4) 0.0119(4) 0.0150(4) -0.0024(3) -0.0038(3) -0.0046(3) O2 0.0152(4) 0.0121(4) 0.0196(4) -0.0033(3) -0.0041(3) -0.0057(3) O3 0.0127(4) 0.0101(4) 0.0147(4) -0.0034(3) -0.0025(3) -0.0039(3) O4 0.0140(4) 0.0131(4) 0.0120(4) -0.0054(3) 0.0024(3) -0.0064(3) O5 0.0172(4) 0.0150(4) 0.0154(4) -0.0075(3) 0.0038(3) -0.0089(3) O6 0.0145(4) 0.0131(4) 0.0163(4) -0.0077(3) 0.0042(3) -0.0071(3) O7 0.0204(4) 0.0145(4) 0.0248(4) -0.0028(3) -0.0101(3) -0.0059(3) O8 0.0151(4) 0.0113(4) 0.0216(4) -0.0040(3) -0.0051(3) -0.0047(3) O9 0.0183(4) 0.0188(4) 0.0144(4) -0.0085(3) 0.0047(3) -0.0107(3) O10 0.0215(4) 0.0165(4) 0.0231(4) -0.0122(3) 0.0090(3) -0.0111(3) C1 0.0191(6) 0.0164(5) 0.0184(6) -0.0033(4) -0.0012(4) -0.0079(4) C2 0.0270(6) 0.0193(6) 0.0223(6) -0.0081(5) 0.0015(5) -0.0003(5) C3 0.0292(7) 0.0208(6) 0.0170(6) -0.0026(5) 0.0020(5) -0.0049(5) N1 0.0143(4) 0.0163(5) 0.0174(5) -0.0048(4) 0.0010(4) -0.0056(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 O1 1.4645(13) . ? B1 O3 1.4666(13) . ? B1 O6 1.4676(13) . ? B1 O4 1.4704(13) . ? B2 O7 1.3519(14) . ? B2 O1 1.3671(14) . ? B2 O2 1.3808(14) . ? B3 O8 1.3576(14) . ? B3 O3 1.3621(14) . ? B3 O2 1.3722(14) . ? B4 O4 1.3607(14) . ? B4 O9 1.3617(14) . ? B4 O5 1.3820(14) . ? B5 O10 1.3505(14) . ? B5 O6 1.3652(14) . ? B5 O5 1.3792(14) . ? O7 H7 0.8400 . ? O8 H8 0.8400 . ? O9 H9 0.8400 . ? O10 H10 0.8400 . ? C1 N1 1.4716(15) . ? C1 C2 1.4884(17) . ? C1 C3 1.4891(16) . ? C1 H1 1.0000 . ? C2 C3 1.4964(17) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? N1 H1A 0.9100 . ? N1 H1B 0.9100 . ? N1 H1C 0.9100 . ? 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 O3 110.86(8) . . ? O1 B1 O6 108.55(8) . . ? O3 B1 O6 109.39(9) . . ? O1 B1 O4 107.81(8) . . ? O3 B1 O4 109.64(8) . . ? O6 B1 O4 110.57(8) . . ? O7 B2 O1 121.52(10) . . ? O7 B2 O2 117.66(10) . . ? O1 B2 O2 120.75(10) . . ? O8 B3 O3 121.23(10) . . ? O8 B3 O2 117.29(10) . . ? O3 B3 O2 121.45(10) . . ? O4 B4 O9 122.08(10) . . ? O4 B4 O5 121.66(10) . . ? O9 B4 O5 116.26(9) . . ? O10 B5 O6 116.20(10) . . ? O10 B5 O5 122.79(10) . . ? O6 B5 O5 120.98(10) . . ? B2 O1 B1 123.05(9) . . ? B3 O2 B2 119.04(9) . . ? B3 O3 B1 122.58(9) . . ? B4 O4 B1 123.50(8) . . ? B5 O5 B4 118.80(9) . . ? B5 O6 B1 124.10(8) . . ? B2 O7 H7 109.5 . . ? B3 O8 H8 109.5 . . ? B4 O9 H9 109.5 . . ? B5 O10 H10 109.5 . . ? N1 C1 C2 116.77(10) . . ? N1 C1 C3 117.71(10) . . ? C2 C1 C3 60.34(8) . . ? N1 C1 H1 116.7 . . ? C2 C1 H1 116.7 . . ? C3 C1 H1 116.7 . . ? C1 C2 C3 59.85(8) . . ? C1 C2 H2A 117.8 . . ? C3 C2 H2A 117.8 . . ? C1 C2 H2B 117.8 . . ? C3 C2 H2B 117.8 . . ? H2A C2 H2B 114.9 . . ? C1 C3 C2 59.81(8) . . ? C1 C3 H3A 117.8 . . ? C2 C3 H3A 117.8 . . ? C1 C3 H3B 117.8 . . ? C2 C3 H3B 117.8 . . ? H3A C3 H3B 114.9 . . ? C1 N1 H1A 109.5 . . ? C1 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? C1 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 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 O1 0.84 1.98 2.8082(11) 166.7 2_565 O8 H8 O3 0.84 1.85 2.6719(11) 166.7 2_656 O9 H9 O4 0.84 1.93 2.7586(11) 169.5 2_665 O10 H10 O8 0.84 1.79 2.6299(11) 176.2 1_565 N1 H1A O6 0.91 1.94 2.8423(12) 170.3 2_666 N1 H1B O6 0.91 2.32 3.0654(12) 138.5 1_655 N1 H1B O1 0.91 2.48 3.2912(12) 149.1 1_655 N1 H1C O9 0.91 1.98 2.8895(12) 176.8 . _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.165 _refine_diff_density_min -0.288 _refine_diff_density_rms 0.050 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 846311' #TrackingRef 'web_deposit_cif_file_0_PeterNHorton_1317124519.borates1.cif' #Dr. M. Beckett/ James Timmis _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'B5 H4 O10, C5 H12 N' _chemical_formula_sum 'C5 H16 B5 N O10' _chemical_formula_weight 304.24 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 9.4446(4) _cell_length_b 13.9129(7) _cell_length_c 10.3330(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.517(3) _cell_angle_gamma 90.00 _cell_volume 1356.46(10) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 3154 _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 0.42 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.490 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 632 _exptl_absorpt_coefficient_mu 0.131 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9469 _exptl_absorpt_correction_T_max 0.9768 _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: 0.6419 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 graphite _diffrn_measurement_device_type 'Bruker-Nonius Roper 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 15990 _diffrn_reflns_av_R_equivalents 0.0500 _diffrn_reflns_av_sigmaI/netI 0.0447 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3110 _reflns_number_gt 2319 _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, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0627P)^2^+0.2571P] 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 3110 _refine_ls_number_parameters 215 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0665 _refine_ls_R_factor_gt 0.0447 _refine_ls_wR_factor_ref 0.1204 _refine_ls_wR_factor_gt 0.1078 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.029 _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 0.77962(16) 0.12458(14) 0.12862(15) 0.0173(4) Uani 1 1 d . . . B2 B 0.52885(18) 0.07624(13) 0.11978(15) 0.0180(4) Uani 1 1 d . . . B3 B 0.60536(18) 0.19021(14) -0.03373(16) 0.0197(4) Uani 1 1 d . . . B4 B 1.03908(17) 0.09963(13) 0.13504(15) 0.0178(4) Uani 1 1 d . . . B5 B 0.94297(18) 0.21472(14) 0.27745(15) 0.0189(4) Uani 1 1 d . . . O1 O 0.66619(10) 0.05871(8) 0.15903(9) 0.0178(3) Uani 1 1 d . . . O2 O 0.49579(10) 0.14768(8) 0.03025(9) 0.0203(3) Uani 1 1 d . . . O3 O 0.74168(10) 0.18018(8) 0.01045(9) 0.0190(3) Uani 1 1 d . . . O4 O 0.90652(10) 0.06810(8) 0.10102(9) 0.0184(3) Uani 1 1 d . . . O5 O 1.05916(10) 0.17296(8) 0.22305(10) 0.0219(3) Uani 1 1 d . . . O6 O 0.80916(10) 0.19007(8) 0.23814(9) 0.0191(3) Uani 1 1 d . . . O7 O 0.42670(11) 0.02006(9) 0.16686(11) 0.0253(3) Uani 1 1 d . . . H7 H 0.3469 0.0396 0.1389 0.038 Uiso 1 1 calc R . . O8 O 0.56678(11) 0.24067(9) -0.14211(10) 0.0253(3) Uani 1 1 d . . . H8 H 0.6396 0.2619 -0.1763 0.038 Uiso 1 1 calc R . . O9 O 1.15528(11) 0.06005(9) 0.08402(10) 0.0239(3) Uani 1 1 d . . . H9 H 1.1300 0.0194 0.0275 0.036 Uiso 1 1 calc R . . O10 O 0.97380(11) 0.28146(9) 0.37054(10) 0.0247(3) Uani 1 1 d . . . H10 H 0.8993 0.2970 0.4068 0.037 Uiso 1 1 calc R . . C1 C 0.2586(4) 0.1578(4) 0.6626(5) 0.0223(7) Uani 0.741(3) 1 d PD A 1 H1 H 0.2472 0.2275 0.6409 0.027 Uiso 0.741(3) 1 calc PR A 1 C2 C 0.1304(5) 0.0996(3) 0.6056(5) 0.0336(10) Uani 0.741(3) 1 d PD A 1 H2A H 0.0899 0.0587 0.6731 0.040 Uiso 0.741(3) 1 calc PR A 1 H2B H 0.0555 0.1434 0.5704 0.040 Uiso 0.741(3) 1 calc PR A 1 C3 C 0.1887(5) 0.0373(3) 0.4970(3) 0.0461(9) Uani 0.741(3) 1 d PD A 1 H3A H 0.2019 -0.0299 0.5263 0.055 Uiso 0.741(3) 1 calc PR A 1 H3B H 0.1232 0.0380 0.4195 0.055 Uiso 0.741(3) 1 calc PR A 1 C4 C 0.3274(3) 0.0816(2) 0.4673(2) 0.0463(7) Uani 0.741(3) 1 d PD A 1 H4A H 0.3138 0.1360 0.4062 0.056 Uiso 0.741(3) 1 calc PR A 1 H4B H 0.3908 0.0337 0.4291 0.056 Uiso 0.741(3) 1 calc PR A 1 C5 C 0.3887(5) 0.1165(5) 0.5984(7) 0.0332(8) Uani 0.741(3) 1 d PD A 1 H5A H 0.4618 0.1666 0.5875 0.040 Uiso 0.741(3) 1 calc PR A 1 H5B H 0.4307 0.0627 0.6497 0.040 Uiso 0.741(3) 1 calc PR A 1 N1 N 0.2727(9) 0.1443(9) 0.8069(5) 0.0238(8) Uani 0.741(3) 1 d PD A 1 H1A H 0.2827 0.0807 0.8255 0.036 Uiso 0.741(3) 1 calc PR A 1 H1B H 0.1938 0.1673 0.8438 0.036 Uiso 0.741(3) 1 calc PR A 1 H1C H 0.3501 0.1769 0.8389 0.036 Uiso 0.741(3) 1 calc PR A 1 C21 C 0.2852(16) 0.1548(14) 0.6450(16) 0.0223(7) Uani 0.259(3) 1 d PD A 2 H21 H 0.2953 0.2248 0.6253 0.027 Uiso 0.259(3) 1 calc PR A 2 C22 C 0.1399(17) 0.1209(12) 0.5883(17) 0.0336(10) Uani 0.259(3) 1 d PD A 2 H22A H 0.0700 0.1149 0.6565 0.040 Uiso 0.259(3) 1 calc PR A 2 H22B H 0.1023 0.1652 0.5201 0.040 Uiso 0.259(3) 1 calc PR A 2 C23 C 0.1765(14) 0.0234(11) 0.5324(12) 0.0461(9) Uani 0.259(3) 1 d PD A 2 H23A H 0.1382 -0.0281 0.5870 0.055 Uiso 0.259(3) 1 calc PR A 2 H23B H 0.1322 0.0171 0.4442 0.055 Uiso 0.259(3) 1 calc PR A 2 C24 C 0.3278(9) 0.0126(6) 0.5270(7) 0.0463(7) Uani 0.259(3) 1 d PD A 2 H24A H 0.3540 0.0028 0.4362 0.056 Uiso 0.259(3) 1 calc PR A 2 H24B H 0.3597 -0.0441 0.5783 0.056 Uiso 0.259(3) 1 calc PR A 2 C25 C 0.3987(17) 0.1026(16) 0.581(2) 0.0332(8) Uani 0.259(3) 1 d PD A 2 H25A H 0.4766 0.0860 0.6448 0.040 Uiso 0.259(3) 1 calc PR A 2 H25B H 0.4376 0.1418 0.5114 0.040 Uiso 0.259(3) 1 calc PR A 2 N21 N 0.288(3) 0.143(3) 0.7880(16) 0.0238(8) Uani 0.259(3) 1 d PD A 2 H21A H 0.2874 0.0795 0.8081 0.036 Uiso 0.259(3) 1 calc PR A 2 H21B H 0.2095 0.1716 0.8197 0.036 Uiso 0.259(3) 1 calc PR A 2 H21C H 0.3670 0.1712 0.8238 0.036 Uiso 0.259(3) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B1 0.0130(8) 0.0227(10) 0.0162(8) -0.0010(7) 0.0007(6) -0.0007(7) B2 0.0155(8) 0.0208(9) 0.0176(8) -0.0019(7) 0.0001(6) 0.0002(7) B3 0.0168(8) 0.0237(10) 0.0185(8) -0.0029(7) 0.0006(6) 0.0019(7) B4 0.0141(8) 0.0213(9) 0.0179(8) 0.0004(7) -0.0008(6) -0.0001(7) B5 0.0170(8) 0.0231(10) 0.0168(8) -0.0005(7) 0.0012(6) -0.0007(7) O1 0.0124(5) 0.0213(6) 0.0197(5) 0.0011(4) 0.0008(4) -0.0002(4) O2 0.0131(5) 0.0270(6) 0.0208(5) 0.0033(4) 0.0001(4) 0.0021(4) O3 0.0140(5) 0.0253(6) 0.0178(5) 0.0026(4) 0.0005(4) -0.0003(4) O4 0.0123(5) 0.0222(6) 0.0208(5) -0.0038(4) 0.0005(4) 0.0004(4) O5 0.0132(5) 0.0272(7) 0.0253(5) -0.0078(5) 0.0009(4) -0.0022(5) O6 0.0144(5) 0.0253(6) 0.0175(5) -0.0034(4) 0.0006(4) -0.0006(5) O7 0.0131(5) 0.0286(7) 0.0340(6) 0.0079(5) -0.0013(4) -0.0013(5) O8 0.0174(6) 0.0352(7) 0.0232(6) 0.0083(5) 0.0004(4) 0.0023(5) O9 0.0130(5) 0.0303(7) 0.0284(6) -0.0102(5) -0.0015(4) 0.0007(5) O10 0.0166(5) 0.0327(7) 0.0250(6) -0.0110(5) 0.0020(4) -0.0029(5) C1 0.018(2) 0.0249(10) 0.0243(17) 0.0046(11) 0.0117(11) 0.0067(14) C2 0.0331(12) 0.041(3) 0.0257(18) 0.0000(16) -0.0038(11) 0.0014(16) C3 0.0643(18) 0.044(2) 0.031(2) -0.0017(17) 0.0072(16) 0.0025(14) C4 0.0621(18) 0.0471(17) 0.0307(13) 0.0004(11) 0.0138(12) 0.0201(14) C5 0.0346(13) 0.029(2) 0.037(2) 0.0046(13) 0.0186(11) 0.0115(14) N1 0.019(2) 0.0277(9) 0.0242(18) -0.002(2) -0.0007(14) 0.0027(15) C21 0.018(2) 0.0249(10) 0.0243(17) 0.0046(11) 0.0117(11) 0.0067(14) C22 0.0331(12) 0.041(3) 0.0257(18) 0.0000(16) -0.0038(11) 0.0014(16) C23 0.0643(18) 0.044(2) 0.031(2) -0.0017(17) 0.0072(16) 0.0025(14) C24 0.0621(18) 0.0471(17) 0.0307(13) 0.0004(11) 0.0138(12) 0.0201(14) C25 0.0346(13) 0.029(2) 0.037(2) 0.0046(13) 0.0186(11) 0.0115(14) N21 0.019(2) 0.0277(9) 0.0242(18) -0.002(2) -0.0007(14) 0.0027(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 O1 1.455(2) . ? B1 O6 1.4701(19) . ? B1 O4 1.4715(19) . ? B1 O3 1.4763(19) . ? B2 O7 1.349(2) . ? B2 O1 1.3639(19) . ? B2 O2 1.384(2) . ? B3 O3 1.354(2) . ? B3 O8 1.358(2) . ? B3 O2 1.385(2) . ? B4 O9 1.355(2) . ? B4 O4 1.3581(19) . ? B4 O5 1.374(2) . ? B5 O6 1.354(2) . ? B5 O10 1.359(2) . ? B5 O5 1.383(2) . ? O7 H7 0.8400 . ? O8 H8 0.8400 . ? O9 H9 0.8400 . ? O10 H10 0.8400 . ? C1 N1 1.504(5) . ? C1 C5 1.533(4) . ? C1 C2 1.551(5) . ? C1 H1 1.0000 . ? C2 C3 1.539(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.492(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.529(6) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? N1 H1A 0.9100 . ? N1 H1B 0.9100 . ? N1 H1C 0.9100 . ? C21 C25 1.472(13) . ? C21 N21 1.486(14) . ? C21 C22 1.543(14) . ? C21 H21 1.0000 . ? C22 C23 1.520(15) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.441(13) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.517(15) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? N21 H21A 0.9100 . ? N21 H21B 0.9100 . ? N21 H21C 0.9100 . ? 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 O6 109.93(11) . . ? O1 B1 O4 108.62(13) . . ? O6 B1 O4 110.58(11) . . ? O1 B1 O3 110.76(11) . . ? O6 B1 O3 110.05(13) . . ? O4 B1 O3 106.84(11) . . ? O7 B2 O1 118.37(14) . . ? O7 B2 O2 120.87(13) . . ? O1 B2 O2 120.72(14) . . ? O3 B3 O8 123.23(14) . . ? O3 B3 O2 120.95(14) . . ? O8 B3 O2 115.81(13) . . ? O9 B4 O4 121.41(14) . . ? O9 B4 O5 117.94(13) . . ? O4 B4 O5 120.65(14) . . ? O6 B5 O10 123.59(14) . . ? O6 B5 O5 121.22(14) . . ? O10 B5 O5 115.18(13) . . ? B2 O1 B1 121.53(13) . . ? B2 O2 B3 118.32(12) . . ? B3 O3 B1 121.70(12) . . ? B4 O4 B1 121.79(12) . . ? B4 O5 B5 119.47(12) . . ? B5 O6 B1 122.06(12) . . ? B2 O7 H7 109.5 . . ? B3 O8 H8 109.5 . . ? B4 O9 H9 109.5 . . ? B5 O10 H10 109.5 . . ? N1 C1 C5 110.2(5) . . ? N1 C1 C2 110.2(5) . . ? C5 C1 C2 105.5(3) . . ? N1 C1 H1 110.3 . . ? C5 C1 H1 110.3 . . ? C2 C1 H1 110.3 . . ? C3 C2 C1 105.8(3) . . ? C3 C2 H2A 110.6 . . ? C1 C2 H2A 110.6 . . ? C3 C2 H2B 110.6 . . ? C1 C2 H2B 110.6 . . ? H2A C2 H2B 108.7 . . ? C4 C3 C2 105.2(3) . . ? C4 C3 H3A 110.7 . . ? C2 C3 H3A 110.7 . . ? C4 C3 H3B 110.7 . . ? C2 C3 H3B 110.7 . . ? H3A C3 H3B 108.8 . . ? C3 C4 C5 104.5(3) . . ? C3 C4 H4A 110.8 . . ? C5 C4 H4A 110.8 . . ? C3 C4 H4B 110.8 . . ? C5 C4 H4B 110.8 . . ? H4A C4 H4B 108.9 . . ? C4 C5 C1 102.9(4) . . ? C4 C5 H5A 111.2 . . ? C1 C5 H5A 111.2 . . ? C4 C5 H5B 111.2 . . ? C1 C5 H5B 111.2 . . ? H5A C5 H5B 109.1 . . ? C25 C21 N21 114.2(16) . . ? C25 C21 C22 109.5(12) . . ? N21 C21 C22 108.5(15) . . ? C25 C21 H21 108.2 . . ? N21 C21 H21 108.2 . . ? C22 C21 H21 108.2 . . ? C23 C22 C21 101.7(11) . . ? C23 C22 H22A 111.4 . . ? C21 C22 H22A 111.4 . . ? C23 C22 H22B 111.4 . . ? C21 C22 H22B 111.4 . . ? H22A C22 H22B 109.3 . . ? C24 C23 C22 110.5(11) . . ? C24 C23 H23A 109.6 . . ? C22 C23 H23A 109.6 . . ? C24 C23 H23B 109.6 . . ? C22 C23 H23B 109.6 . . ? H23A C23 H23B 108.1 . . ? C23 C24 C25 108.8(10) . . ? C23 C24 H24A 109.9 . . ? C25 C24 H24A 109.9 . . ? C23 C24 H24B 109.9 . . ? C25 C24 H24B 109.9 . . ? H24A C24 H24B 108.3 . . ? C21 C25 C24 104.7(11) . . ? C21 C25 H25A 110.8 . . ? C24 C25 H25A 110.8 . . ? C21 C25 H25B 110.8 . . ? C24 C25 H25B 110.8 . . ? H25A C25 H25B 108.9 . . ? C21 N21 H21A 109.5 . . ? C21 N21 H21B 109.5 . . ? H21A N21 H21B 109.5 . . ? C21 N21 H21C 109.5 . . ? H21A N21 H21C 109.5 . . ? H21B N21 H21C 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 1.89 2.7241(15) 169.2 1_455 O8 H8 O6 0.84 1.98 2.8194(15) 178.2 4_565 O9 H9 O4 0.84 1.82 2.6603(15) 174.1 3_755 O10 H10 O3 0.84 1.90 2.7311(14) 171.0 4_566 N1 H1A O1 0.91 2.00 2.902(12) 168.9 3_656 N1 H1B O10 0.91 2.22 3.103(8) 162.0 4_466 N1 H1C O8 0.91 2.23 3.108(10) 161.7 1_556 N1 H1C O2 0.91 2.39 3.056(8) 129.8 1_556 N21 H21A O1 0.91 2.00 2.89(4) 166.8 3_656 N21 H21B O10 0.91 2.40 3.29(2) 166.0 4_466 N21 H21C O8 0.91 2.14 3.03(3) 165.5 1_556 N21 H21C O2 0.91 2.43 3.12(2) 132.2 1_556 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.264 _refine_diff_density_min -0.270 _refine_diff_density_rms 0.057 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 846312' #TrackingRef 'web_deposit_cif_file_0_PeterNHorton_1317124519.borates1.cif' #Dr. M. A. Beckett / James Timmis _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H24 B5 N O10' _chemical_formula_weight 360.34 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 9.8889(4) _cell_length_b 11.4371(4) _cell_length_c 15.8055(5) _cell_angle_alpha 90.00 _cell_angle_beta 106.958(2) _cell_angle_gamma 90.00 _cell_volume 1709.88(11) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 4049 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description 'Cut Block' _exptl_crystal_colour 'Light Yellow' _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.400 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 0.116 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9561 _exptl_absorpt_correction_T_max 0.9873 _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: 0.6526 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 graphite _diffrn_measurement_device_type 'Bruker-Nonius Roper 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 21302 _diffrn_reflns_av_R_equivalents 0.0647 _diffrn_reflns_av_sigmaI/netI 0.0533 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.23 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3914 _reflns_number_gt 2778 _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, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0648P)^2^+0.4117P] 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 3914 _refine_ls_number_parameters 233 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0761 _refine_ls_R_factor_gt 0.0494 _refine_ls_wR_factor_ref 0.1308 _refine_ls_wR_factor_gt 0.1158 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 0.9249(2) 0.51669(17) 0.18233(12) 0.0161(4) Uani 1 1 d . . . B2 B 1.1155(2) 0.62131(17) 0.29461(12) 0.0166(4) Uani 1 1 d . . . B3 B 1.1111(2) 0.41317(17) 0.29957(12) 0.0181(4) Uani 1 1 d . . . B4 B 0.8118(2) 0.48352(17) 0.02136(12) 0.0169(4) Uani 1 1 d . . . B5 B 0.6652(2) 0.51161(17) 0.11716(12) 0.0179(4) Uani 1 1 d . . . O1 O 1.00200(12) 0.62238(10) 0.22159(7) 0.0176(3) Uani 1 1 d . . . O2 O 1.17789(12) 0.51749(10) 0.33175(8) 0.0214(3) Uani 1 1 d . . . O3 O 0.99136(12) 0.41158(10) 0.23083(7) 0.0185(3) Uani 1 1 d . . . O4 O 0.92825(12) 0.50682(10) 0.08965(7) 0.0172(3) Uani 1 1 d . . . O5 O 0.67739(12) 0.48635(11) 0.03340(7) 0.0200(3) Uani 1 1 d . . . O6 O 0.78028(12) 0.52458(10) 0.18697(7) 0.0185(3) Uani 1 1 d . . . O7 O 1.17459(12) 0.72180(10) 0.33509(7) 0.0204(3) Uani 1 1 d . . . H7 H 1.1236 0.7789 0.3123 0.031 Uiso 1 1 calc R . . O8 O 1.17120(14) 0.31394(11) 0.34115(8) 0.0266(3) Uani 1 1 d . . . H8 H 1.1234 0.2558 0.3171 0.040 Uiso 1 1 calc R . . O9 O 0.81493(12) 0.45637(11) -0.06157(7) 0.0218(3) Uani 1 1 d . . . H9 H 0.8972 0.4658 -0.0653 0.033 Uiso 1 1 calc R . . O10 O 0.53480(13) 0.52196(12) 0.12933(8) 0.0250(3) Uani 1 1 d . . . H10 H 0.4725 0.5172 0.0803 0.038 Uiso 1 1 calc R . . C1 C 0.6649(2) 0.49963(15) 0.37063(12) 0.0234(4) Uani 1 1 d . . . H1 H 0.6361 0.5184 0.3060 0.028 Uiso 1 1 calc R . . C2 C 0.8189(2) 0.53725(19) 0.40821(14) 0.0347(5) Uani 1 1 d . . . H2A H 0.8501 0.5249 0.4730 0.042 Uiso 1 1 calc R . . H2B H 0.8794 0.4893 0.3818 0.042 Uiso 1 1 calc R . . C3 C 0.8339(3) 0.6657(2) 0.38776(15) 0.0453(6) Uani 1 1 d . . . H3A H 0.8097 0.6763 0.3229 0.054 Uiso 1 1 calc R . . H3B H 0.9335 0.6900 0.4139 0.054 Uiso 1 1 calc R . . C4 C 0.7386(3) 0.7431(2) 0.42403(15) 0.0469(6) Uani 1 1 d . . . H4A H 0.7715 0.7416 0.4895 0.056 Uiso 1 1 calc R . . H4B H 0.7443 0.8247 0.4045 0.056 Uiso 1 1 calc R . . C5 C 0.5866(3) 0.70163(18) 0.39232(15) 0.0393(5) Uani 1 1 d . . . H5A H 0.5493 0.7150 0.3278 0.047 Uiso 1 1 calc R . . H5B H 0.5289 0.7483 0.4217 0.047 Uiso 1 1 calc R . . C6 C 0.5724(2) 0.57248(17) 0.41176(13) 0.0302(5) Uani 1 1 d . . . H6A H 0.6010 0.5597 0.4765 0.036 Uiso 1 1 calc R . . H6B H 0.4725 0.5480 0.3874 0.036 Uiso 1 1 calc R . . C7 C 0.7158(2) 0.30148(18) 0.32243(13) 0.0327(5) Uani 1 1 d . . . H7A H 0.6956 0.2178 0.3244 0.049 Uiso 1 1 calc R . . H7B H 0.8181 0.3143 0.3447 0.049 Uiso 1 1 calc R . . H7C H 0.6812 0.3294 0.2613 0.049 Uiso 1 1 calc R . . C8 C 0.6968(2) 0.32473(18) 0.47211(12) 0.0329(5) Uani 1 1 d . . . H8A H 0.8003 0.3299 0.4920 0.049 Uiso 1 1 calc R . . H8B H 0.6679 0.2433 0.4752 0.049 Uiso 1 1 calc R . . H8C H 0.6575 0.3732 0.5103 0.049 Uiso 1 1 calc R . . C9 C 0.4882(2) 0.33757(19) 0.34491(13) 0.0334(5) Uani 1 1 d . . . H9A H 0.4390 0.3679 0.3859 0.050 Uiso 1 1 calc R . . H9B H 0.4767 0.2525 0.3402 0.050 Uiso 1 1 calc R . . H9C H 0.4480 0.3730 0.2865 0.050 Uiso 1 1 calc R . . N1 N 0.64323(16) 0.36724(13) 0.37889(9) 0.0236(4) 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 0.0141(9) 0.0189(10) 0.0139(8) -0.0008(7) 0.0018(7) -0.0015(7) B2 0.0143(10) 0.0197(10) 0.0156(8) 0.0019(7) 0.0040(7) -0.0001(8) B3 0.0167(10) 0.0210(10) 0.0157(9) -0.0006(8) 0.0031(8) -0.0006(8) B4 0.0152(10) 0.0172(10) 0.0179(9) 0.0010(7) 0.0040(8) -0.0003(7) B5 0.0171(10) 0.0211(10) 0.0149(9) 0.0009(7) 0.0038(7) -0.0012(8) O1 0.0159(6) 0.0181(6) 0.0162(6) -0.0004(5) 0.0008(5) -0.0005(5) O2 0.0179(7) 0.0200(7) 0.0208(6) 0.0008(5) -0.0030(5) -0.0010(5) O3 0.0177(6) 0.0172(6) 0.0170(6) 0.0000(5) -0.0006(5) -0.0013(5) O4 0.0128(6) 0.0229(7) 0.0147(6) -0.0020(4) 0.0022(5) -0.0010(5) O5 0.0139(6) 0.0301(7) 0.0148(6) -0.0019(5) 0.0027(5) -0.0003(5) O6 0.0149(6) 0.0252(7) 0.0143(5) -0.0012(5) 0.0024(5) -0.0012(5) O7 0.0191(7) 0.0180(7) 0.0195(6) 0.0012(5) -0.0014(5) -0.0011(5) O8 0.0261(8) 0.0186(7) 0.0263(6) 0.0020(5) -0.0063(5) -0.0013(5) O9 0.0157(6) 0.0324(7) 0.0170(6) -0.0048(5) 0.0045(5) -0.0033(5) O10 0.0149(6) 0.0423(8) 0.0169(6) -0.0038(6) 0.0030(5) -0.0003(6) C1 0.0270(10) 0.0241(10) 0.0206(9) 0.0016(7) 0.0091(8) -0.0024(7) C2 0.0259(11) 0.0464(13) 0.0327(11) -0.0095(9) 0.0102(9) -0.0049(9) C3 0.0517(15) 0.0474(14) 0.0438(13) -0.0132(11) 0.0249(11) -0.0244(12) C4 0.0780(19) 0.0327(12) 0.0380(12) -0.0096(9) 0.0294(12) -0.0174(12) C5 0.0580(15) 0.0257(11) 0.0393(11) 0.0027(9) 0.0225(11) 0.0061(10) C6 0.0329(12) 0.0262(11) 0.0356(11) 0.0020(8) 0.0165(9) 0.0025(8) C7 0.0416(13) 0.0334(11) 0.0287(10) -0.0053(9) 0.0190(9) 0.0021(9) C8 0.0447(13) 0.0327(12) 0.0222(9) 0.0060(8) 0.0110(9) 0.0094(9) C9 0.0300(12) 0.0357(12) 0.0339(10) -0.0058(9) 0.0085(9) -0.0088(9) N1 0.0297(9) 0.0243(9) 0.0193(7) 0.0008(6) 0.0108(7) 0.0017(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 O6 1.456(2) . ? B1 O1 1.467(2) . ? B1 O3 1.473(2) . ? B1 O4 1.479(2) . ? B2 O1 1.355(2) . ? B2 O7 1.362(2) . ? B2 O2 1.387(2) . ? B3 O3 1.354(2) . ? B3 O8 1.358(2) . ? B3 O2 1.386(2) . ? B4 O4 1.355(2) . ? B4 O9 1.356(2) . ? B4 O5 1.397(2) . ? B5 O6 1.342(2) . ? B5 O10 1.364(2) . ? B5 O5 1.394(2) . ? O7 H7 0.8400 . ? O8 H8 0.8400 . ? O9 H9 0.8400 . ? O10 H10 0.8400 . ? C1 C6 1.517(3) . ? C1 C2 1.526(3) . ? C1 N1 1.540(2) . ? C1 H1 1.0000 . ? C2 C3 1.521(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.522(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.515(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.523(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 N1 1.500(2) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 N1 1.494(2) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 N1 1.508(3) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 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 O6 B1 O1 108.94(13) . . ? O6 B1 O3 108.66(13) . . ? O1 B1 O3 110.76(13) . . ? O6 B1 O4 111.13(13) . . ? O1 B1 O4 108.83(13) . . ? O3 B1 O4 108.52(13) . . ? O1 B2 O7 121.87(15) . . ? O1 B2 O2 121.60(15) . . ? O7 B2 O2 116.53(15) . . ? O3 B3 O8 122.27(16) . . ? O3 B3 O2 121.17(16) . . ? O8 B3 O2 116.56(15) . . ? O4 B4 O9 124.17(15) . . ? O4 B4 O5 120.53(15) . . ? O9 B4 O5 115.30(15) . . ? O6 B5 O10 118.96(15) . . ? O6 B5 O5 121.09(16) . . ? O10 B5 O5 119.94(16) . . ? B2 O1 B1 123.51(13) . . ? B3 O2 B2 118.42(14) . . ? B3 O3 B1 124.02(14) . . ? B4 O4 B1 123.00(13) . . ? B5 O5 B4 118.89(14) . . ? B5 O6 B1 124.14(13) . . ? B2 O7 H7 109.5 . . ? B3 O8 H8 109.5 . . ? B4 O9 H9 109.5 . . ? B5 O10 H10 109.5 . . ? C6 C1 C2 109.64(16) . . ? C6 C1 N1 112.81(14) . . ? C2 C1 N1 113.07(16) . . ? C6 C1 H1 107.0 . . ? C2 C1 H1 107.0 . . ? N1 C1 H1 107.0 . . ? C3 C2 C1 109.75(18) . . ? C3 C2 H2A 109.7 . . ? C1 C2 H2A 109.7 . . ? C3 C2 H2B 109.7 . . ? C1 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? C2 C3 C4 111.83(17) . . ? C2 C3 H3A 109.3 . . ? C4 C3 H3A 109.3 . . ? C2 C3 H3B 109.3 . . ? C4 C3 H3B 109.3 . . ? H3A C3 H3B 107.9 . . ? C5 C4 C3 110.94(18) . . ? C5 C4 H4A 109.5 . . ? C3 C4 H4A 109.5 . . ? C5 C4 H4B 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 108.0 . . ? C4 C5 C6 112.16(19) . . ? C4 C5 H5A 109.2 . . ? C6 C5 H5A 109.2 . . ? C4 C5 H5B 109.2 . . ? C6 C5 H5B 109.2 . . ? H5A C5 H5B 107.9 . . ? C1 C6 C5 110.11(15) . . ? C1 C6 H6A 109.6 . . ? C5 C6 H6A 109.6 . . ? C1 C6 H6B 109.6 . . ? C5 C6 H6B 109.6 . . ? H6A C6 H6B 108.2 . . ? N1 C7 H7A 109.5 . . ? N1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 H9A 109.5 . . ? N1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 N1 C7 109.25(15) . . ? C8 N1 C9 108.03(14) . . ? C7 N1 C9 106.76(15) . . ? C8 N1 C1 112.67(14) . . ? C7 N1 C1 109.87(13) . . ? C9 N1 C1 110.07(15) . . ? 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 2.7372(16) 175.8 2_755 O8 H8 O1 0.84 1.95 2.7796(17) 169.9 2_745 O9 H9 O4 0.84 1.90 2.7353(16) 172.3 3_765 O10 H10 O5 0.84 1.97 2.8069(17) 177.1 3_665 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.290 _refine_diff_density_min -0.329 _refine_diff_density_rms 0.059 #===END data_6 _database_code_depnum_ccdc_archive 'CCDC 846313' #TrackingRef 'web_deposit_cif_file_0_PeterNHorton_1317124519.borates1.cif' #Dr. M. Beckett/ James Timmis #One of the cyclohexylammonium cations was disordered over 2 sites. #The lower occupancy site atoms were left isotropic and mild thermal #(SIMU) and geometrical (SAME) restraints were used. There was also #disorder of one of the three solvent water molecules. It was not #possible to accurately locate the hydrogen atoms of the lower #partial occupancy water molecules. #There are a series of close contacts between disordered atoms which #can be safely ignored based on the overall atom occupancies. #A large crystal was used as attempts to cut to obtain a smaller #fragment resulted in severe straining and lose of suitable diffraction #pattern. _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H44 B8 N2 O20' _chemical_formula_weight 622.97 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 11.5041(2) _cell_length_b 11.8807(2) _cell_length_c 12.6861(2) _cell_angle_alpha 69.2430(10) _cell_angle_beta 81.7040(10) _cell_angle_gamma 63.1050(10) _cell_volume 1445.71(4) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 6559 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.82 _exptl_crystal_size_mid 0.73 _exptl_crystal_size_min 0.54 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.431 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 660 _exptl_absorpt_coefficient_mu 0.126 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9040 _exptl_absorpt_correction_T_max 0.9353 _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: 0.6957 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 graphite _diffrn_measurement_device_type 'Bruker-Nonius Roper 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 32692 _diffrn_reflns_av_R_equivalents 0.0278 _diffrn_reflns_av_sigmaI/netI 0.0219 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6619 _reflns_number_gt 5977 _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, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0370P)^2^+0.6091P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0302(18) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6619 _refine_ls_number_parameters 447 _refine_ls_number_restraints 185 _refine_ls_R_factor_all 0.0388 _refine_ls_R_factor_gt 0.0338 _refine_ls_wR_factor_ref 0.0850 _refine_ls_wR_factor_gt 0.0820 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.025 _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 0.86619(11) 0.83415(11) 0.33417(9) 0.0107(2) Uani 1 1 d . . . B2 B 0.93119(11) 0.89536(11) 0.13498(10) 0.0119(2) Uani 1 1 d . . . B3 B 0.93243(11) 1.01957(11) 0.25455(9) 0.0112(2) Uani 1 1 d . . . B4 B 1.06806(11) 0.81388(12) 0.39810(10) 0.0136(2) Uani 1 1 d . . . B5 B 0.77124(11) 1.23908(12) 0.26866(10) 0.0134(2) Uani 1 1 d . . . B6 B 0.74134(11) 1.04881(12) 0.39596(10) 0.0120(2) Uani 1 1 d . . . B7 B 0.65738(11) 0.87972(12) 0.43158(9) 0.0122(2) Uani 1 1 d . . . O1 O 0.82561(7) 0.98009(7) 0.31222(6) 0.00996(15) Uani 1 1 d . . . O2 O 0.88951(7) 0.81599(7) 0.22268(6) 0.01264(16) Uani 1 1 d . . . O3 O 0.95281(7) 0.99537(7) 0.14456(6) 0.01244(15) Uani 1 1 d . . . O4 O 0.98637(7) 0.75634(7) 0.40333(6) 0.01365(16) Uani 1 1 d . . . O5 O 1.04991(7) 0.93658(7) 0.32494(6) 0.01348(16) Uani 1 1 d . . . O6 O 0.89093(7) 1.15994(7) 0.23632(6) 0.01262(16) Uani 1 1 d . . . O7 O 0.69007(7) 1.19068(7) 0.33669(6) 0.01433(16) Uani 1 1 d . . . O8 O 0.63937(7) 1.00254(8) 0.42918(6) 0.01385(16) Uani 1 1 d . . . O9 O 0.76467(7) 0.79662(7) 0.39002(6) 0.01234(15) Uani 1 1 d . . . O10 O 0.95127(8) 0.86789(8) 0.03535(6) 0.01528(16) Uani 1 1 d . . . H10 H 0.9779 0.9201 -0.0133 0.023 Uiso 1 1 calc R . . O11 O 1.17557(8) 0.74557(9) 0.47003(7) 0.02119(18) Uani 1 1 d . . . H11 H 1.1841 0.6675 0.5049 0.032 Uiso 1 1 calc R . . O12 O 0.72985(8) 1.37505(8) 0.23369(7) 0.02053(18) Uani 1 1 d . . . H12 H 0.7889 1.3943 0.1968 0.031 Uiso 1 1 calc R . . O13 O 0.81743(8) 1.01045(8) 0.49587(6) 0.01697(17) Uani 1 1 d . . . H13 H 0.8342 1.0734 0.4929 0.025 Uiso 1 1 calc R . . O14 O 0.56414(7) 0.83497(8) 0.47882(7) 0.01620(17) Uani 1 1 d . . . H14 H 0.5059 0.8901 0.5070 0.024 Uiso 1 1 calc R . . B21 B 0.90225(13) 0.57941(13) 0.12212(11) 0.0180(2) Uani 1 1 d . . . O21 O 0.84146(11) 0.62542(10) 0.20802(8) 0.0341(2) Uani 1 1 d . . . H21 H 0.8518 0.6928 0.2027 0.051 Uiso 1 1 calc R . . O22 O 0.96184(8) 0.64001(8) 0.03590(6) 0.01696(17) Uani 1 1 d . . . H22 H 0.9534 0.7106 0.0438 0.025 Uiso 1 1 calc R . . O23 O 0.90438(10) 0.46243(9) 0.12402(8) 0.0276(2) Uani 1 1 d . . . H23 H 0.9440 0.4425 0.0675 0.041 Uiso 1 1 calc R . . C1 C 0.22151(11) 0.17712(11) 0.21749(9) 0.0173(2) Uani 1 1 d D . . H1 H 0.1887 0.2568 0.1478 0.021 Uiso 1 1 calc R . . C2 C 0.26861(12) 0.05214(13) 0.18528(10) 0.0230(3) Uani 1 1 d D . . H2A H 0.1966 0.0554 0.1482 0.028 Uiso 1 1 calc R . . H2B H 0.2963 -0.0276 0.2539 0.028 Uiso 1 1 calc R . . C3 C 0.38320(13) 0.04179(14) 0.10508(10) 0.0259(3) Uani 1 1 d D . . H3A H 0.4163 -0.0424 0.0879 0.031 Uiso 1 1 calc R . . H3B H 0.3529 0.1170 0.0335 0.031 Uiso 1 1 calc R . . C4 C 0.49356(12) 0.04477(14) 0.15676(11) 0.0261(3) Uani 1 1 d D . . H4A H 0.5296 -0.0351 0.2245 0.031 Uiso 1 1 calc R . . H4B H 0.5644 0.0422 0.1018 0.031 Uiso 1 1 calc R . . C5 C 0.44447(12) 0.17025(13) 0.18914(10) 0.0233(3) Uani 1 1 d D . . H5A H 0.4157 0.2499 0.1205 0.028 Uiso 1 1 calc R . . H5B H 0.5162 0.1683 0.2256 0.028 Uiso 1 1 calc R . . C6 C 0.33072(11) 0.17975(12) 0.27008(10) 0.0192(2) Uani 1 1 d D . . H6A H 0.3613 0.1040 0.3413 0.023 Uiso 1 1 calc R . . H6B H 0.2975 0.2636 0.2879 0.023 Uiso 1 1 calc R . . N1 N 0.11194(9) 0.18617(10) 0.29902(8) 0.0188(2) Uani 1 1 d D . . H1A H 0.0471 0.1826 0.2688 0.028 Uiso 1 1 calc R . . H1B H 0.0805 0.2646 0.3132 0.028 Uiso 1 1 calc R . . H1C H 0.1417 0.1168 0.3645 0.028 Uiso 1 1 calc R . . C11 C 0.6033(2) 0.4218(2) 0.7352(2) 0.0178(4) Uani 0.869(4) 1 d PDU A 1 H11A H 0.6803 0.3690 0.6971 0.021 Uiso 0.869(4) 1 calc PR A 1 C12 C 0.5774(3) 0.3264(3) 0.8409(2) 0.0339(6) Uani 0.869(4) 1 d PDU A 1 H12A H 0.5637 0.2598 0.8211 0.041 Uiso 0.869(4) 1 calc PR A 1 H12B H 0.4969 0.3765 0.8761 0.041 Uiso 0.869(4) 1 calc PR A 1 C13 C 0.6919(2) 0.2544(3) 0.92510(19) 0.0382(6) Uani 0.869(4) 1 d PDU A 1 H13A H 0.6709 0.1963 0.9952 0.046 Uiso 0.869(4) 1 calc PR A 1 H13B H 0.7702 0.1971 0.8928 0.046 Uiso 0.869(4) 1 calc PR A 1 C14 C 0.72049(16) 0.3537(2) 0.95243(15) 0.0327(5) Uani 0.869(4) 1 d PDU A 1 H14A H 0.7973 0.3052 1.0040 0.039 Uiso 0.869(4) 1 calc PR A 1 H14B H 0.6452 0.4055 0.9912 0.039 Uiso 0.869(4) 1 calc PR A 1 C15 C 0.74699(17) 0.44874(16) 0.84519(16) 0.0315(5) Uani 0.869(4) 1 d PDU A 1 H15A H 0.8269 0.3977 0.8101 0.038 Uiso 0.869(4) 1 calc PR A 1 H15B H 0.7619 0.5151 0.8644 0.038 Uiso 0.869(4) 1 calc PR A 1 C16 C 0.63220(17) 0.52160(15) 0.76084(16) 0.0274(4) Uani 0.869(4) 1 d PDU A 1 H16A H 0.5541 0.5798 0.7928 0.033 Uiso 0.869(4) 1 calc PR A 1 H16B H 0.6537 0.5787 0.6903 0.033 Uiso 0.869(4) 1 calc PR A 1 N11 N 0.4867(3) 0.4932(3) 0.6572(3) 0.0176(5) Uani 0.869(4) 1 d PDU A 1 H11B H 0.4136 0.5301 0.6949 0.026 Uiso 0.869(4) 1 calc PR A 1 H11C H 0.4792 0.4341 0.6318 0.026 Uiso 0.869(4) 1 calc PR A 1 H11D H 0.4967 0.5587 0.5977 0.026 Uiso 0.869(4) 1 calc PR A 1 C21 C 0.6016(18) 0.4105(15) 0.7626(12) 0.018(4) Uiso 0.131(4) 1 d PDU A 2 H21A H 0.6901 0.3757 0.7297 0.021 Uiso 0.131(4) 1 calc PR A 2 C22 C 0.5832(14) 0.2956(13) 0.8422(11) 0.011(3) Uiso 0.131(4) 1 d PDU A 2 H22A H 0.5846 0.2373 0.8019 0.013 Uiso 0.131(4) 1 calc PR A 2 H22B H 0.4981 0.3264 0.8794 0.013 Uiso 0.131(4) 1 calc PR A 2 C23 C 0.6953(15) 0.2174(13) 0.9312(12) 0.022(3) Uiso 0.131(4) 1 d PDU A 2 H23A H 0.6836 0.1407 0.9875 0.026 Uiso 0.131(4) 1 calc PR A 2 H23B H 0.7798 0.1823 0.8942 0.026 Uiso 0.131(4) 1 calc PR A 2 C24 C 0.6957(14) 0.3078(14) 0.9890(12) 0.042(3) Uiso 0.131(4) 1 d PDU A 2 H24A H 0.7700 0.2578 1.0434 0.050 Uiso 0.131(4) 1 calc PR A 2 H24B H 0.6144 0.3354 1.0318 0.050 Uiso 0.131(4) 1 calc PR A 2 C25 C 0.7063(12) 0.4309(12) 0.9068(12) 0.034(3) Uiso 0.131(4) 1 d PDU A 2 H25A H 0.7914 0.4043 0.8691 0.041 Uiso 0.131(4) 1 calc PR A 2 H25B H 0.7020 0.4893 0.9483 0.041 Uiso 0.131(4) 1 calc PR A 2 C26 C 0.5949(11) 0.5091(10) 0.8171(10) 0.027(3) Uiso 0.131(4) 1 d PDU A 2 H26A H 0.5094 0.5440 0.8528 0.033 Uiso 0.131(4) 1 calc PR A 2 H26B H 0.6066 0.5852 0.7598 0.033 Uiso 0.131(4) 1 calc PR A 2 N21 N 0.506(2) 0.482(2) 0.6698(18) 0.019(5) Uiso 0.131(4) 1 d PDU A 2 H21B H 0.4982 0.4225 0.6452 0.028 Uiso 0.131(4) 1 calc PR A 2 H21C H 0.5320 0.5371 0.6122 0.028 Uiso 0.131(4) 1 calc PR A 2 H21D H 0.4270 0.5317 0.6944 0.028 Uiso 0.131(4) 1 calc PR A 2 O31 O 0.44197(8) 0.70180(8) 0.44171(8) 0.02183(18) Uani 1 1 d D . . H31A H 0.4751(12) 0.7513(12) 0.4452(14) 0.033 Uiso 1 1 d D . . H31B H 0.3595(5) 0.7426(13) 0.4455(14) 0.033 Uiso 1 1 d D . . O32 O 0.06276(10) 0.39842(10) 0.38305(8) 0.0316(2) Uani 1 1 d D . . H32A H 0.0455(16) 0.3627(15) 0.4511(6) 0.047 Uiso 1 1 d D . . H32B H 0.0011(12) 0.4763(8) 0.3595(13) 0.047 Uiso 1 1 d D . . O41 O 0.25718(10) 0.46884(11) 0.58075(9) 0.0269(3) Uani 0.877(2) 1 d PD B 1 H41A H 0.2312(19) 0.446(2) 0.6452(9) 0.040 Uiso 0.877(2) 1 d PD B 1 H41B H 0.236(2) 0.449(2) 0.5323(15) 0.040 Uiso 0.877(2) 1 d PD B 1 O42 O 0.2745(10) 0.4220(11) 0.4173(9) 0.0269(3) Uani 0.084(2) 1 d P C 2 O43 O 0.229(3) 0.482(3) 0.510(2) 0.0269(3) Uani 0.039(3) 1 d P D 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 0.0118(5) 0.0118(5) 0.0106(5) -0.0048(4) 0.0023(4) -0.0066(4) B2 0.0117(5) 0.0116(5) 0.0129(5) -0.0050(4) 0.0017(4) -0.0052(4) B3 0.0115(5) 0.0137(5) 0.0123(5) -0.0063(4) 0.0040(4) -0.0083(4) B4 0.0109(5) 0.0179(6) 0.0139(5) -0.0077(4) 0.0032(4) -0.0069(5) B5 0.0142(5) 0.0145(5) 0.0143(5) -0.0069(4) 0.0016(4) -0.0073(5) B6 0.0124(5) 0.0149(5) 0.0123(5) -0.0073(4) 0.0045(4) -0.0078(4) B7 0.0125(5) 0.0168(5) 0.0107(5) -0.0058(4) 0.0014(4) -0.0084(4) O1 0.0097(3) 0.0119(3) 0.0107(3) -0.0055(3) 0.0033(3) -0.0062(3) O2 0.0174(4) 0.0137(3) 0.0111(3) -0.0065(3) 0.0043(3) -0.0097(3) O3 0.0159(4) 0.0140(3) 0.0112(3) -0.0065(3) 0.0049(3) -0.0094(3) O4 0.0118(3) 0.0141(4) 0.0153(4) -0.0039(3) -0.0003(3) -0.0064(3) O5 0.0114(3) 0.0161(4) 0.0156(4) -0.0059(3) 0.0017(3) -0.0081(3) O6 0.0133(4) 0.0134(4) 0.0152(4) -0.0074(3) 0.0042(3) -0.0082(3) O7 0.0125(4) 0.0136(4) 0.0186(4) -0.0079(3) 0.0050(3) -0.0064(3) O8 0.0127(4) 0.0173(4) 0.0171(4) -0.0101(3) 0.0069(3) -0.0097(3) O9 0.0126(4) 0.0141(3) 0.0130(3) -0.0055(3) 0.0039(3) -0.0082(3) O10 0.0253(4) 0.0157(4) 0.0111(3) -0.0056(3) 0.0056(3) -0.0147(3) O11 0.0169(4) 0.0226(4) 0.0228(4) -0.0008(3) -0.0054(3) -0.0108(3) O12 0.0195(4) 0.0138(4) 0.0283(4) -0.0084(3) 0.0093(3) -0.0085(3) O13 0.0244(4) 0.0213(4) 0.0138(4) -0.0078(3) 0.0014(3) -0.0159(3) O14 0.0149(4) 0.0202(4) 0.0215(4) -0.0134(3) 0.0088(3) -0.0118(3) B21 0.0241(6) 0.0162(6) 0.0182(6) -0.0076(5) 0.0049(5) -0.0122(5) O21 0.0612(7) 0.0295(5) 0.0324(5) -0.0227(4) 0.0292(5) -0.0357(5) O22 0.0259(4) 0.0149(4) 0.0168(4) -0.0083(3) 0.0053(3) -0.0134(3) O23 0.0456(6) 0.0249(5) 0.0275(5) -0.0181(4) 0.0218(4) -0.0268(4) C1 0.0193(5) 0.0217(5) 0.0131(5) -0.0023(4) -0.0006(4) -0.0130(5) C2 0.0301(6) 0.0305(6) 0.0192(6) -0.0107(5) 0.0030(5) -0.0208(5) C3 0.0337(7) 0.0333(7) 0.0195(6) -0.0132(5) 0.0057(5) -0.0199(6) C4 0.0244(6) 0.0335(7) 0.0223(6) -0.0117(5) 0.0046(5) -0.0133(5) C5 0.0220(6) 0.0328(7) 0.0224(6) -0.0099(5) 0.0021(4) -0.0178(5) C6 0.0203(6) 0.0251(6) 0.0190(5) -0.0095(5) 0.0011(4) -0.0140(5) N1 0.0188(5) 0.0231(5) 0.0172(5) -0.0045(4) -0.0007(4) -0.0127(4) C11 0.0147(8) 0.0174(9) 0.0209(11) -0.0093(8) 0.0001(8) -0.0043(6) C12 0.0306(11) 0.0269(13) 0.0406(12) 0.0018(10) -0.0073(7) -0.0168(10) C13 0.0329(10) 0.0295(12) 0.0384(11) 0.0088(10) -0.0099(7) -0.0138(10) C14 0.0248(8) 0.0401(11) 0.0237(9) -0.0105(8) -0.0061(6) -0.0042(8) C15 0.0334(9) 0.0264(8) 0.0371(11) -0.0067(7) -0.0155(7) -0.0130(7) C16 0.0326(8) 0.0209(7) 0.0311(10) -0.0036(6) -0.0125(7) -0.0136(6) N11 0.0152(11) 0.0181(9) 0.0216(10) -0.0111(7) -0.0011(7) -0.0051(8) O31 0.0160(4) 0.0242(4) 0.0350(5) -0.0196(4) 0.0058(3) -0.0108(3) O32 0.0328(5) 0.0277(5) 0.0217(5) -0.0034(4) 0.0050(4) -0.0074(4) O41 0.0233(5) 0.0288(6) 0.0239(6) -0.0039(4) 0.0046(4) -0.0123(4) O42 0.0233(5) 0.0288(6) 0.0239(6) -0.0039(4) 0.0046(4) -0.0123(4) O43 0.0233(5) 0.0288(6) 0.0239(6) -0.0039(4) 0.0046(4) -0.0123(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 O9 1.4399(13) . ? B1 O4 1.4679(13) . ? B1 O2 1.4742(13) . ? B1 O1 1.5049(13) . ? B2 O3 1.3663(14) . ? B2 O2 1.3669(13) . ? B2 O10 1.3774(13) . ? B3 O6 1.4494(13) . ? B3 O5 1.4542(13) . ? B3 O3 1.4878(13) . ? B3 O1 1.5113(12) . ? B4 O5 1.3608(14) . ? B4 O4 1.3733(14) . ? B4 O11 1.3833(14) . ? B5 O7 1.3598(13) . ? B5 O6 1.3738(14) . ? B5 O12 1.3749(14) . ? B6 O7 1.4437(14) . ? B6 O13 1.4595(13) . ? B6 O8 1.4603(13) . ? B6 O1 1.5286(13) . ? B7 O9 1.3619(14) . ? B7 O8 1.3675(14) . ? B7 O14 1.3773(13) . ? O10 H10 0.8400 . ? O11 H11 0.8400 . ? O12 H12 0.8400 . ? O13 H13 0.8400 . ? O14 H14 0.8400 . ? B21 O21 1.3535(15) . ? B21 O22 1.3626(14) . ? B21 O23 1.3706(15) . ? O21 H21 0.8400 . ? O22 H22 0.8400 . ? O23 H23 0.8400 . ? C1 N1 1.5001(14) . ? C1 C2 1.5178(17) . ? C1 C6 1.5220(15) . ? C1 H1 1.0000 . ? C2 C3 1.5307(17) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.5298(18) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.5216(18) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.5298(16) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? N1 H1A 0.9100 . ? N1 H1B 0.9100 . ? N1 H1C 0.9100 . ? C11 N11 1.502(3) . ? C11 C16 1.511(2) . ? C11 C12 1.512(3) . ? C11 H11A 1.0000 . ? C12 C13 1.532(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.515(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.523(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.5347(19) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? N11 H11B 0.9100 . ? N11 H11C 0.9100 . ? N11 H11D 0.9100 . ? C21 N21 1.464(15) . ? C21 C22 1.466(14) . ? C21 C26 1.528(14) . ? C21 H21A 1.0000 . ? C22 C23 1.547(14) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.501(14) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.512(14) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.548(12) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? N21 H21B 0.9100 . ? N21 H21C 0.9100 . ? N21 H21D 0.9100 . ? O31 H31A 0.848(5) . ? O31 H31B 0.851(5) . ? O32 H32A 0.855(5) . ? O32 H32B 0.849(5) . ? O41 H41A 0.822(9) . ? O41 H41B 0.834(9) . ? O43 H41B 0.37(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O9 B1 O4 110.74(8) . . ? O9 B1 O2 109.95(8) . . ? O4 B1 O2 110.84(8) . . ? O9 B1 O1 110.77(8) . . ? O4 B1 O1 108.40(8) . . ? O2 B1 O1 106.04(8) . . ? O3 B2 O2 122.70(9) . . ? O3 B2 O10 121.52(9) . . ? O2 B2 O10 115.78(9) . . ? O6 B3 O5 111.18(8) . . ? O6 B3 O3 110.14(8) . . ? O5 B3 O3 110.88(8) . . ? O6 B3 O1 109.44(8) . . ? O5 B3 O1 108.66(8) . . ? O3 B3 O1 106.39(8) . . ? O5 B4 O4 123.59(10) . . ? O5 B4 O11 116.87(10) . . ? O4 B4 O11 119.54(10) . . ? O7 B5 O6 123.74(10) . . ? O7 B5 O12 116.72(10) . . ? O6 B5 O12 119.52(9) . . ? O7 B6 O13 111.52(9) . . ? O7 B6 O8 112.58(9) . . ? O13 B6 O8 109.00(8) . . ? O7 B6 O1 106.43(8) . . ? O13 B6 O1 111.04(8) . . ? O8 B6 O1 106.13(8) . . ? O9 B7 O8 123.39(9) . . ? O9 B7 O14 117.11(9) . . ? O8 B7 O14 119.51(9) . . ? B1 O1 B3 110.92(7) . . ? B1 O1 B6 120.84(7) . . ? B3 O1 B6 117.92(7) . . ? B2 O2 B1 121.00(8) . . ? B2 O3 B3 119.64(8) . . ? B4 O4 B1 119.21(8) . . ? B4 O5 B3 119.89(8) . . ? B5 O6 B3 122.56(8) . . ? B5 O7 B6 118.25(8) . . ? B7 O8 B6 122.68(8) . . ? B7 O9 B1 122.44(8) . . ? B2 O10 H10 109.5 . . ? B4 O11 H11 109.5 . . ? B5 O12 H12 109.5 . . ? B6 O13 H13 109.5 . . ? B7 O14 H14 109.5 . . ? O21 B21 O22 124.77(10) . . ? O21 B21 O23 116.77(10) . . ? O22 B21 O23 118.45(10) . . ? B21 O21 H21 109.5 . . ? B21 O22 H22 109.5 . . ? B21 O23 H23 109.5 . . ? N1 C1 C2 110.49(9) . . ? N1 C1 C6 109.02(9) . . ? C2 C1 C6 111.64(10) . . ? N1 C1 H1 108.5 . . ? C2 C1 H1 108.5 . . ? C6 C1 H1 108.5 . . ? C1 C2 C3 109.96(10) . . ? C1 C2 H2A 109.7 . . ? C3 C2 H2A 109.7 . . ? C1 C2 H2B 109.7 . . ? C3 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? C4 C3 C2 111.27(10) . . ? C4 C3 H3A 109.4 . . ? C2 C3 H3A 109.4 . . ? C4 C3 H3B 109.4 . . ? C2 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? C5 C4 C3 110.78(11) . . ? C5 C4 H4A 109.5 . . ? C3 C4 H4A 109.5 . . ? C5 C4 H4B 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? C4 C5 C6 110.51(10) . . ? C4 C5 H5A 109.5 . . ? C6 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? C6 C5 H5B 109.5 . . ? H5A C5 H5B 108.1 . . ? C1 C6 C5 110.40(9) . . ? C1 C6 H6A 109.6 . . ? C5 C6 H6A 109.6 . . ? C1 C6 H6B 109.6 . . ? C5 C6 H6B 109.6 . . ? H6A C6 H6B 108.1 . . ? C1 N1 H1A 109.5 . . ? C1 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? C1 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? N11 C11 C16 110.13(18) . . ? N11 C11 C12 108.8(2) . . ? C16 C11 C12 112.0(2) . . ? N11 C11 H11A 108.6 . . ? C16 C11 H11A 108.6 . . ? C12 C11 H11A 108.6 . . ? C11 C12 C13 110.75(19) . . ? C11 C12 H12A 109.5 . . ? C13 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? C13 C12 H12B 109.5 . . ? H12A C12 H12B 108.1 . . ? C14 C13 C12 110.9(2) . . ? C14 C13 H13A 109.5 . . ? C12 C13 H13A 109.5 . . ? C14 C13 H13B 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 108.0 . . ? C13 C14 C15 110.59(14) . . ? C13 C14 H14A 109.5 . . ? C15 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? C15 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? C14 C15 C16 111.11(14) . . ? C14 C15 H15A 109.4 . . ? C16 C15 H15A 109.4 . . ? C14 C15 H15B 109.4 . . ? C16 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? C11 C16 C15 110.22(14) . . ? C11 C16 H16A 109.6 . . ? C15 C16 H16A 109.6 . . ? C11 C16 H16B 109.6 . . ? C15 C16 H16B 109.6 . . ? H16A C16 H16B 108.1 . . ? N21 C21 C22 111.0(14) . . ? N21 C21 C26 108.8(14) . . ? C22 C21 C26 113.6(11) . . ? N21 C21 H21A 107.7 . . ? C22 C21 H21A 107.7 . . ? C26 C21 H21A 107.7 . . ? C21 C22 C23 108.1(11) . . ? C21 C22 H22A 110.1 . . ? C23 C22 H22A 110.1 . . ? C21 C22 H22B 110.1 . . ? C23 C22 H22B 110.1 . . ? H22A C22 H22B 108.4 . . ? C24 C23 C22 109.8(11) . . ? C24 C23 H23A 109.7 . . ? C22 C23 H23A 109.7 . . ? C24 C23 H23B 109.7 . . ? C22 C23 H23B 109.7 . . ? H23A C23 H23B 108.2 . . ? C23 C24 C25 112.4(11) . . ? C23 C24 H24A 109.1 . . ? C25 C24 H24A 109.1 . . ? C23 C24 H24B 109.1 . . ? C25 C24 H24B 109.1 . . ? H24A C24 H24B 107.8 . . ? C24 C25 C26 110.8(10) . . ? C24 C25 H25A 109.5 . . ? C26 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? C26 C25 H25B 109.5 . . ? H25A C25 H25B 108.1 . . ? C21 C26 C25 106.5(9) . . ? C21 C26 H26A 110.4 . . ? C25 C26 H26A 110.4 . . ? C21 C26 H26B 110.4 . . ? C25 C26 H26B 110.4 . . ? H26A C26 H26B 108.6 . . ? C21 N21 H21B 109.5 . . ? C21 N21 H21C 109.5 . . ? H21B N21 H21C 109.5 . . ? C21 N21 H21D 109.5 . . ? H21B N21 H21D 109.5 . . ? H21C N21 H21D 109.5 . . ? H31A O31 H31B 108.5(10) . . ? H32A O32 H32B 106.7(11) . . ? H41A O41 H41B 117.7(18) . . ? 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 O10 H10 O3 0.84 1.89 2.7080(10) 164.2 2_775 O11 H11 O43 0.84 2.00 2.77(3) 151.5 1_655 O11 H11 O41 0.84 2.01 2.8246(14) 164.0 1_655 O12 H12 O23 0.84 1.83 2.6646(11) 169.9 1_565 O13 H13 O11 0.84 2.31 3.1155(11) 160.3 2_776 O14 H14 O8 0.84 1.87 2.7000(11) 170.6 2_676 O21 H21 O2 0.84 1.81 2.6318(11) 167.2 . O22 H22 O10 0.84 1.82 2.6522(11) 169.0 . O23 H23 O22 0.84 1.84 2.6684(11) 167.0 2_765 N1 H1A O6 0.91 2.05 2.9445(12) 167.6 1_445 N1 H1B O32 0.91 2.00 2.8734(15) 160.1 . N1 H1C O13 0.91 1.83 2.7335(12) 172.7 2_666 N11 H11B O12 0.91 1.85 2.754(3) 172.2 2_676 N11 H11C O31 0.91 1.95 2.768(3) 148.9 2_666 N11 H11D O31 0.91 2.05 2.886(3) 151.9 . N21 H21B O31 0.91 1.97 2.81(3) 152.7 2_666 N21 H21C O31 0.91 2.32 3.04(2) 135.7 . N21 H21D O12 0.91 1.94 2.84(3) 172.4 2_676 O31 H31A O14 0.848(5) 1.889(6) 2.7259(11) 169.0(15) . O31 H31B O11 0.851(5) 2.080(7) 2.8574(11) 151.6(13) 1_455 O32 H32A O4 0.855(5) 1.992(6) 2.8303(12) 166.4(17) 2_666 O32 H32B O21 0.849(5) 2.422(11) 3.1401(15) 142.8(16) 1_455 O41 H41A O21 0.822(9) 1.991(10) 2.8049(13) 170.3(19) 2_666 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.646 _refine_diff_density_min -0.238 _refine_diff_density_rms 0.043 #===END data_7 _database_code_depnum_ccdc_archive 'CCDC 846314' #TrackingRef 'web_deposit_cif_file_0_PeterNHorton_1317124519.borates1.cif' #Dr. M. Beckett/ James Timmis #The cycloheptylammonium cations are disordered over 2 and 4 sites #respectively. Due to their partial occupancies, the atoms were left #isotropic and mild thermal (SIMU) and geometrical (SAME) restraints #were used on these cations. There was also disorder of one of the #two solvent water molecules. It was not possible to accurately locate #the hydrogen atoms of the water molecules. #There are a series of close contacts between disordered atoms which #can be safely ignored based on the overall atom occupancies. #A large crystal was used as attempts to cut to obtain a smaller #fragment resulted in severe straining and lose of suitable diffraction #pattern. _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H47 B9 N2 O22' _chemical_formula_weight 692.83 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 13.0200(3) _cell_length_b 13.5845(4) _cell_length_c 18.4005(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.5130(10) _cell_angle_gamma 90.00 _cell_volume 3253.36(14) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 7597 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description Slab _exptl_crystal_colour Colourless _exptl_crystal_size_max 1.10 _exptl_crystal_size_mid 0.80 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.414 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1464 _exptl_absorpt_coefficient_mu 0.123 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8762 _exptl_absorpt_correction_T_max 0.9639 _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: 0.6804 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 graphite _diffrn_measurement_device_type 'Bruker-Nonius Roper 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 36724 _diffrn_reflns_av_R_equivalents 0.0369 _diffrn_reflns_av_sigmaI/netI 0.0314 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7438 _reflns_number_gt 6135 _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, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.1037P)^2^+5.0530P] 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 7438 _refine_ls_number_parameters 509 _refine_ls_number_restraints 423 _refine_ls_R_factor_all 0.0801 _refine_ls_R_factor_gt 0.0672 _refine_ls_wR_factor_ref 0.1956 _refine_ls_wR_factor_gt 0.1849 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.108 _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 0.5129(2) 0.78652(18) 0.21523(14) 0.0143(5) Uani 1 1 d . . . B2 B 0.4302(2) 0.72252(18) 0.09402(14) 0.0135(5) Uani 1 1 d . . . B3 B 0.4216(2) 0.90232(19) 0.11888(15) 0.0158(5) Uani 1 1 d . . . B4 B 0.5630(2) 0.62994(19) 0.16331(14) 0.0151(5) Uani 1 1 d . . . B5 B 0.5394(2) 0.96701(19) 0.21362(15) 0.0170(5) Uani 1 1 d . . . B6 B 0.4452(2) 0.8439(2) -0.00476(15) 0.0179(5) Uani 1 1 d . . . B7 B 0.2694(2) 0.7966(2) 0.13596(15) 0.0168(5) Uani 1 1 d . . . O1 O 0.47535(12) 0.80710(11) 0.13701(8) 0.0128(3) Uani 1 1 d . . . O2 O 0.58654(13) 0.70645(12) 0.20922(9) 0.0166(4) Uani 1 1 d . . . O3 O 0.48591(13) 0.63334(12) 0.11172(9) 0.0152(3) Uani 1 1 d . . . O4 O 0.56214(14) 0.87613(12) 0.24147(9) 0.0188(4) Uani 1 1 d . . . O5 O 0.46740(14) 0.98208(12) 0.15956(10) 0.0192(4) Uani 1 1 d . . . O6 O 0.43957(13) 0.74686(12) 0.01711(9) 0.0167(4) Uani 1 1 d . . . O7 O 0.43143(14) 0.92017(12) 0.04161(9) 0.0197(4) Uani 1 1 d . . . O8 O 0.32010(13) 0.71404(11) 0.11328(9) 0.0148(3) Uani 1 1 d . . . O9 O 0.31244(13) 0.88834(12) 0.13828(9) 0.0171(4) Uani 1 1 d . . . O10 O 0.42879(14) 0.76006(12) 0.26161(9) 0.0182(4) Uani 1 1 d . . . H10 H 0.4245 0.6985 0.2642 0.027 Uiso 1 1 calc R . . O11 O 0.62051(14) 0.54499(13) 0.16721(10) 0.0218(4) Uani 1 1 d . . . H11 H 0.6595 0.5469 0.2043 0.033 Uiso 1 1 calc R . . O12 O 0.59107(14) 1.04894(12) 0.23858(10) 0.0202(4) Uani 1 1 d . . . H12 H 0.6336 1.0325 0.2715 0.030 Uiso 1 1 calc R . . O13 O 0.46702(16) 0.85687(14) -0.07687(10) 0.0266(4) Uani 1 1 d . . . H13 H 0.4743 0.9172 -0.0854 0.040 Uiso 1 1 calc R . . O14 O 0.16896(15) 0.78787(15) 0.15691(12) 0.0288(4) Uani 1 1 d . . . H14 H 0.1492 0.8417 0.1741 0.043 Uiso 1 1 calc R . . B21 B 0.1539(2) 0.5315(2) 0.18426(16) 0.0213(6) Uani 1 1 d . . . O21 O 0.25005(14) 0.53368(13) 0.15615(10) 0.0221(4) Uani 1 1 d . . . H21 H 0.2596 0.5883 0.1360 0.033 Uiso 1 1 calc R . . O22 O 0.08889(15) 0.60977(15) 0.17818(14) 0.0341(5) Uani 1 1 d . . . H22 H 0.1230 0.6622 0.1793 0.051 Uiso 1 1 calc R . . O23 O 0.12197(16) 0.44837(14) 0.21931(12) 0.0302(5) Uani 1 1 d . . . H23 H 0.1683 0.4054 0.2181 0.045 Uiso 1 1 calc R . . B31 B 0.1355(2) 0.0297(2) 0.23242(16) 0.0218(6) Uani 1 1 d . . . O31 O 0.23713(14) 0.03077(14) 0.21726(11) 0.0251(4) Uani 1 1 d . . . H31 H 0.2517 -0.0198 0.1933 0.038 Uiso 1 1 calc R . . O32 O 0.09463(16) 0.11356(15) 0.26060(13) 0.0321(5) Uani 1 1 d . . . H32 H 0.1330 0.1615 0.2516 0.048 Uiso 1 1 calc R . . O33 O 0.07568(15) -0.05198(15) 0.22133(12) 0.0299(5) Uani 1 1 d . . . H33 H 0.0147 -0.0390 0.2318 0.045 Uiso 1 1 calc R . . O41 O 0.22224(16) 0.26886(19) 0.22736(12) 0.0386(5) Uani 1 1 d . . . C1 C 0.7383(6) 0.3458(6) 0.1109(5) 0.023(3) Uiso 0.607(9) 1 d PDU A 1 H1 H 0.7672 0.3731 0.1576 0.027 Uiso 0.607(9) 1 calc PR A 1 C2 C 0.7730(5) 0.2372(4) 0.1042(4) 0.0239(18) Uiso 0.607(9) 1 d PDU A 1 H2A H 0.7781 0.2193 0.0523 0.029 Uiso 0.607(9) 1 calc PR A 1 H2B H 0.7217 0.1934 0.1263 0.029 Uiso 0.607(9) 1 calc PR A 1 C3 C 0.8798(4) 0.2235(4) 0.1437(3) 0.0277(12) Uiso 0.607(9) 1 d PDU A 1 H3A H 0.8731 0.2439 0.1950 0.033 Uiso 0.607(9) 1 calc PR A 1 H3B H 0.8966 0.1524 0.1438 0.033 Uiso 0.607(9) 1 calc PR A 1 C4 C 0.9679(6) 0.2779(6) 0.1131(5) 0.057(2) Uiso 0.607(9) 1 d PDU A 1 H4A H 1.0203 0.2823 0.1530 0.069 Uiso 0.607(9) 1 calc PR A 1 H4B H 0.9970 0.2337 0.0761 0.069 Uiso 0.607(9) 1 calc PR A 1 C5 C 0.9641(5) 0.3737(5) 0.0804(4) 0.0485(17) Uiso 0.607(9) 1 d PDU A 1 H5A H 1.0318 0.3865 0.0591 0.058 Uiso 0.607(9) 1 calc PR A 1 H5B H 0.9553 0.4224 0.1198 0.058 Uiso 0.607(9) 1 calc PR A 1 C6 C 0.8831(5) 0.3937(5) 0.0227(3) 0.0459(17) Uiso 0.607(9) 1 d PDU A 1 H6A H 0.8817 0.3373 -0.0114 0.055 Uiso 0.607(9) 1 calc PR A 1 H6B H 0.9044 0.4524 -0.0050 0.055 Uiso 0.607(9) 1 calc PR A 1 C7 C 0.7744(6) 0.4108(6) 0.0479(4) 0.027(2) Uiso 0.607(9) 1 d PDU A 1 H7A H 0.7266 0.4007 0.0058 0.033 Uiso 0.607(9) 1 calc PR A 1 H7B H 0.7684 0.4805 0.0629 0.033 Uiso 0.607(9) 1 calc PR A 1 N1 N 0.6224(5) 0.3514(5) 0.1125(4) 0.014(2) Uiso 0.607(9) 1 d PDU A 1 H1A H 0.5949 0.3222 0.0719 0.022 Uiso 0.607(9) 1 calc PR A 1 H1B H 0.6026 0.4156 0.1137 0.022 Uiso 0.607(9) 1 calc PR A 1 H1C H 0.6000 0.3198 0.1527 0.022 Uiso 0.607(9) 1 calc PR A 1 C61 C 0.7458(9) 0.3444(9) 0.1162(8) 0.021(4) Uiso 0.393(9) 1 d PDU A 2 H61 H 0.7705 0.3738 0.1633 0.025 Uiso 0.393(9) 1 calc PR A 2 C62 C 0.7758(8) 0.2386(7) 0.1187(7) 0.029(3) Uiso 0.393(9) 1 d PDU A 2 H62A H 0.7445 0.2106 0.1626 0.035 Uiso 0.393(9) 1 calc PR A 2 H62B H 0.7409 0.2068 0.0764 0.035 Uiso 0.393(9) 1 calc PR A 2 C63 C 0.8824(10) 0.2045(12) 0.1193(11) 0.088(5) Uiso 0.393(9) 1 d PDU A 2 H63A H 0.9007 0.1932 0.1712 0.106 Uiso 0.393(9) 1 calc PR A 2 H63B H 0.8796 0.1385 0.0965 0.106 Uiso 0.393(9) 1 calc PR A 2 C64 C 0.9694(8) 0.2501(8) 0.0902(7) 0.047(2) Uiso 0.393(9) 1 d PDU A 2 H64A H 1.0056 0.1996 0.0618 0.056 Uiso 0.393(9) 1 calc PR A 2 H64B H 1.0157 0.2680 0.1317 0.056 Uiso 0.393(9) 1 calc PR A 2 C65 C 0.9586(12) 0.3386(10) 0.0435(9) 0.091(4) Uiso 0.393(9) 1 d PDU A 2 H65A H 0.9308 0.3143 -0.0038 0.109 Uiso 0.393(9) 1 calc PR A 2 H65B H 1.0297 0.3606 0.0345 0.109 Uiso 0.393(9) 1 calc PR A 2 C66 C 0.8987(6) 0.4320(6) 0.0590(5) 0.038(2) Uiso 0.393(9) 1 d PDU A 2 H66A H 0.9191 0.4577 0.1076 0.045 Uiso 0.393(9) 1 calc PR A 2 H66B H 0.9145 0.4829 0.0224 0.045 Uiso 0.393(9) 1 calc PR A 2 C67 C 0.7860(9) 0.4103(10) 0.0564(8) 0.038(4) Uiso 0.393(9) 1 d PDU A 2 H67A H 0.7688 0.3792 0.0090 0.046 Uiso 0.393(9) 1 calc PR A 2 H67B H 0.7486 0.4737 0.0580 0.046 Uiso 0.393(9) 1 calc PR A 2 N61 N 0.6345(8) 0.3515(9) 0.1153(7) 0.020(4) Uiso 0.393(9) 1 d PDU A 2 H61A H 0.6089 0.3326 0.0709 0.030 Uiso 0.393(9) 1 calc PR A 2 H61B H 0.6157 0.4149 0.1240 0.030 Uiso 0.393(9) 1 calc PR A 2 H61C H 0.6090 0.3116 0.1502 0.030 Uiso 0.393(9) 1 calc PR A 2 C11 C 0.3039(5) 0.2419(5) 0.0269(3) 0.0121(12) Uiso 0.354(3) 1 d PDU B 1 H11D H 0.3524 0.2374 -0.0142 0.014 Uiso 0.354(3) 1 calc PR B 1 C12 C 0.2591(10) 0.1417(8) 0.0429(6) 0.030(3) Uiso 0.354(3) 1 d PDU B 1 H12A H 0.1892 0.1504 0.0619 0.036 Uiso 0.354(3) 1 calc PR B 1 H12B H 0.3018 0.1097 0.0815 0.036 Uiso 0.354(3) 1 calc PR B 1 C13 C 0.2528(7) 0.0723(7) -0.0248(5) 0.0362(19) Uiso 0.354(3) 1 d PDU B 1 H13A H 0.3226 0.0466 -0.0333 0.043 Uiso 0.354(3) 1 calc PR B 1 H13B H 0.2089 0.0154 -0.0127 0.043 Uiso 0.354(3) 1 calc PR B 1 C14 C 0.2125(10) 0.1156(7) -0.0939(5) 0.042(2) Uiso 0.354(3) 1 d PDU B 1 H14A H 0.2495 0.0878 -0.1355 0.050 Uiso 0.354(3) 1 calc PR B 1 H14B H 0.1385 0.1003 -0.1005 0.050 Uiso 0.354(3) 1 calc PR B 1 C15 C 0.2271(8) 0.2189(7) -0.0907(6) 0.043(2) Uiso 0.354(3) 1 d PDU B 1 H15A H 0.2450 0.2360 -0.1411 0.051 Uiso 0.354(3) 1 calc PR B 1 H15B H 0.2920 0.2258 -0.0618 0.051 Uiso 0.354(3) 1 calc PR B 1 C16 C 0.1670(7) 0.3030(7) -0.0678(4) 0.0291(18) Uiso 0.354(3) 1 d PDU B 1 H16A H 0.0929 0.2874 -0.0658 0.035 Uiso 0.354(3) 1 calc PR B 1 H16B H 0.1773 0.3611 -0.0992 0.035 Uiso 0.354(3) 1 calc PR B 1 C17 C 0.2160(6) 0.3168(6) 0.0082(4) 0.0230(15) Uiso 0.354(3) 1 d PDU B 1 H17A H 0.1619 0.3103 0.0447 0.028 Uiso 0.354(3) 1 calc PR B 1 H17B H 0.2441 0.3844 0.0120 0.028 Uiso 0.354(3) 1 calc PR B 1 N11 N 0.3580(4) 0.2817(4) 0.0933(3) 0.0121(11) Uiso 0.354(3) 1 d PDU B 1 H11A H 0.3152 0.2791 0.1316 0.018 Uiso 0.354(3) 1 calc PR B 1 H11B H 0.3766 0.3453 0.0853 0.018 Uiso 0.354(3) 1 calc PR B 1 H11C H 0.4150 0.2450 0.1034 0.018 Uiso 0.354(3) 1 calc PR B 1 C21 C 0.2687(17) 0.123(2) 0.0484(11) 0.016(5) Uiso 0.118(4) 1 d PDU C 2 H21D H 0.2808 0.0511 0.0541 0.019 Uiso 0.118(4) 1 calc PR C 2 C22 C 0.1550(16) 0.134(2) 0.0577(15) 0.046(6) Uiso 0.118(4) 1 d PDU C 2 H22A H 0.1319 0.1946 0.0328 0.055 Uiso 0.118(4) 1 calc PR C 2 H22B H 0.1422 0.1419 0.1102 0.055 Uiso 0.118(4) 1 calc PR C 2 C23 C 0.089(2) 0.049(2) 0.0293(15) 0.060(7) Uiso 0.118(4) 1 d PDU C 2 H23A H 0.1095 -0.0105 0.0575 0.072 Uiso 0.118(4) 1 calc PR C 2 H23B H 0.0172 0.0637 0.0414 0.072 Uiso 0.118(4) 1 calc PR C 2 C24 C 0.090(3) 0.022(3) -0.0482(15) 0.071(7) Uiso 0.118(4) 1 d PDU C 2 H24A H 0.0758 -0.0496 -0.0515 0.085 Uiso 0.118(4) 1 calc PR C 2 H24B H 0.0307 0.0557 -0.0724 0.085 Uiso 0.118(4) 1 calc PR C 2 C25 C 0.180(2) 0.042(2) -0.0914(17) 0.062(6) Uiso 0.118(4) 1 d PDU C 2 H25A H 0.2306 -0.0096 -0.0771 0.074 Uiso 0.118(4) 1 calc PR C 2 H25B H 0.1587 0.0267 -0.1422 0.074 Uiso 0.118(4) 1 calc PR C 2 C26 C 0.240(2) 0.1327(19) -0.0956(12) 0.033(6) Uiso 0.118(4) 1 d PDU C 2 H26A H 0.1923 0.1895 -0.1003 0.039 Uiso 0.118(4) 1 calc PR C 2 H26B H 0.2827 0.1309 -0.1391 0.039 Uiso 0.118(4) 1 calc PR C 2 C27 C 0.3083(18) 0.145(2) -0.0275(11) 0.041(5) Uiso 0.118(4) 1 d PDU C 2 H27A H 0.3326 0.2142 -0.0272 0.049 Uiso 0.118(4) 1 calc PR C 2 H27B H 0.3695 0.1032 -0.0341 0.049 Uiso 0.118(4) 1 calc PR C 2 N21 N 0.334(3) 0.167(4) 0.1068(17) 0.039(13) Uiso 0.118(4) 1 d PDU C 2 H21A H 0.3136 0.2298 0.1153 0.058 Uiso 0.118(4) 1 calc PR C 2 H21B H 0.4008 0.1671 0.0930 0.058 Uiso 0.118(4) 1 calc PR C 2 H21C H 0.3285 0.1307 0.1481 0.058 Uiso 0.118(4) 1 calc PR C 2 C31 C 0.2862(18) 0.1888(16) 0.0202(12) 0.059(5) Uiso 0.172(7) 1 d PDU D 3 H31D H 0.3460 0.1941 -0.0125 0.071 Uiso 0.172(7) 1 calc PR D 3 C32 C 0.252(2) 0.0856(15) 0.0148(14) 0.061(5) Uiso 0.172(7) 1 d PDU D 3 H32A H 0.2133 0.0766 0.0601 0.074 Uiso 0.172(7) 1 calc PR D 3 H32B H 0.3163 0.0482 0.0227 0.074 Uiso 0.172(7) 1 calc PR D 3 C33 C 0.193(2) 0.0229(14) -0.0382(13) 0.050(5) Uiso 0.172(7) 1 d PDU D 3 H33A H 0.1577 -0.0283 -0.0101 0.060 Uiso 0.172(7) 1 calc PR D 3 H33B H 0.2442 -0.0114 -0.0682 0.060 Uiso 0.172(7) 1 calc PR D 3 C34 C 0.1157(15) 0.0679(12) -0.0890(10) 0.031(4) Uiso 0.172(7) 1 d PDU D 3 H34A H 0.1239 0.0382 -0.1376 0.037 Uiso 0.172(7) 1 calc PR D 3 H34B H 0.0465 0.0496 -0.0724 0.037 Uiso 0.172(7) 1 calc PR D 3 C35 C 0.1192(14) 0.1745(12) -0.0969(10) 0.019(4) Uiso 0.172(7) 1 d PDU D 3 H35A H 0.1507 0.1782 -0.1452 0.023 Uiso 0.172(7) 1 calc PR D 3 H35B H 0.0454 0.1869 -0.1073 0.023 Uiso 0.172(7) 1 calc PR D 3 C36 C 0.148(3) 0.2691(15) -0.0701(15) 0.076(7) Uiso 0.172(7) 1 d PDU D 3 H36A H 0.0836 0.3064 -0.0618 0.091 Uiso 0.172(7) 1 calc PR D 3 H36B H 0.1842 0.3037 -0.1090 0.091 Uiso 0.172(7) 1 calc PR D 3 C37 C 0.214(2) 0.2756(17) -0.0012(13) 0.066(6) Uiso 0.172(7) 1 d PDU D 3 H37A H 0.1673 0.2864 0.0398 0.079 Uiso 0.172(7) 1 calc PR D 3 H37B H 0.2569 0.3353 -0.0049 0.079 Uiso 0.172(7) 1 calc PR D 3 N31 N 0.328(2) 0.211(2) 0.0949(13) 0.084(9) Uiso 0.172(7) 1 d PDU D 3 H31A H 0.3882 0.1782 0.1026 0.126 Uiso 0.172(7) 1 calc PR D 3 H31B H 0.2820 0.1918 0.1284 0.126 Uiso 0.172(7) 1 calc PR D 3 H31C H 0.3393 0.2770 0.0992 0.126 Uiso 0.172(7) 1 calc PR D 3 C41 C 0.2890(7) 0.1400(7) 0.0322(5) 0.020(2) Uiso 0.357(7) 1 d PDU E 4 H41 H 0.3468 0.1047 0.0086 0.024 Uiso 0.357(7) 1 calc PR E 4 C42 C 0.2022(7) 0.0706(6) 0.0385(5) 0.033(2) Uiso 0.357(7) 1 d PDU E 4 H42A H 0.1446 0.1063 0.0607 0.040 Uiso 0.357(7) 1 calc PR E 4 H42B H 0.2236 0.0178 0.0728 0.040 Uiso 0.357(7) 1 calc PR E 4 C43 C 0.1627(13) 0.0234(10) -0.0295(7) 0.066(4) Uiso 0.357(7) 1 d PDU E 4 H43A H 0.1210 -0.0347 -0.0166 0.079 Uiso 0.357(7) 1 calc PR E 4 H43B H 0.2217 -0.0003 -0.0575 0.079 Uiso 0.357(7) 1 calc PR E 4 C44 C 0.0987(14) 0.0903(11) -0.0768(10) 0.088(5) Uiso 0.357(7) 1 d PDU E 4 H44A H 0.0969 0.0601 -0.1258 0.106 Uiso 0.357(7) 1 calc PR E 4 H44B H 0.0279 0.0861 -0.0587 0.106 Uiso 0.357(7) 1 calc PR E 4 C45 C 0.1194(6) 0.1950(6) -0.0877(4) 0.0132(18) Uiso 0.357(7) 1 d PDU E 4 H45A H 0.0969 0.2056 -0.1389 0.016 Uiso 0.357(7) 1 calc PR E 4 H45B H 0.0661 0.2272 -0.0585 0.016 Uiso 0.357(7) 1 calc PR E 4 C46 C 0.2053(15) 0.2611(14) -0.0794(10) 0.096(5) Uiso 0.357(7) 1 d PDU E 4 H46A H 0.1799 0.3297 -0.0777 0.116 Uiso 0.357(7) 1 calc PR E 4 H46B H 0.2497 0.2548 -0.1220 0.116 Uiso 0.357(7) 1 calc PR E 4 C47 C 0.2686(7) 0.2393(7) -0.0103(5) 0.034(2) Uiso 0.357(7) 1 d PDU E 4 H47A H 0.2405 0.2844 0.0265 0.041 Uiso 0.357(7) 1 calc PR E 4 H47B H 0.3380 0.2648 -0.0205 0.041 Uiso 0.357(7) 1 calc PR E 4 N41 N 0.3267(9) 0.1760(11) 0.1059(5) 0.022(3) Uiso 0.357(7) 1 d PDU E 4 H41A H 0.2730 0.1797 0.1363 0.032 Uiso 0.357(7) 1 calc PR E 4 H41B H 0.3555 0.2367 0.1012 0.032 Uiso 0.357(7) 1 calc PR E 4 H41C H 0.3745 0.1334 0.1244 0.032 Uiso 0.357(7) 1 calc PR E 4 O51 O 0.4508(4) 0.4572(3) 0.0326(3) 0.0379(13) Uani 0.504(5) 1 d P F 5 O52 O 0.3960(4) 0.3768(4) 0.1137(2) 0.0302(11) Uani 0.439(4) 1 d P G 6 O53 O 0.300(3) 0.381(3) 0.0674(18) 0.0302(11) Uani 0.056(5) 1 d P H 7 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 0.0178(12) 0.0102(11) 0.0149(12) 0.0004(9) -0.0021(9) 0.0002(9) B2 0.0152(12) 0.0105(11) 0.0147(12) 0.0001(9) -0.0014(9) -0.0017(9) B3 0.0166(12) 0.0107(11) 0.0198(12) 0.0021(9) -0.0028(10) -0.0008(9) B4 0.0154(12) 0.0118(11) 0.0180(12) 0.0005(9) 0.0015(10) 0.0001(9) B5 0.0190(13) 0.0119(12) 0.0200(13) -0.0009(9) -0.0012(10) 0.0007(10) B6 0.0201(13) 0.0161(12) 0.0173(12) 0.0043(10) -0.0028(10) -0.0042(10) B7 0.0174(12) 0.0143(12) 0.0185(12) 0.0012(9) -0.0019(10) 0.0010(10) O1 0.0154(8) 0.0088(7) 0.0142(7) 0.0014(6) -0.0015(6) -0.0010(6) O2 0.0185(8) 0.0120(8) 0.0190(8) 0.0001(6) -0.0038(6) 0.0009(6) O3 0.0186(8) 0.0108(7) 0.0163(8) 0.0000(6) -0.0014(6) 0.0001(6) O4 0.0234(9) 0.0112(8) 0.0215(8) -0.0012(6) -0.0074(7) -0.0012(6) O5 0.0233(9) 0.0092(8) 0.0246(9) 0.0005(6) -0.0068(7) -0.0010(6) O6 0.0215(9) 0.0141(8) 0.0144(8) 0.0022(6) -0.0002(6) -0.0033(6) O7 0.0263(9) 0.0132(8) 0.0196(8) 0.0057(6) -0.0016(7) -0.0019(7) O8 0.0151(8) 0.0113(7) 0.0180(8) 0.0002(6) 0.0008(6) -0.0016(6) O9 0.0160(8) 0.0117(8) 0.0235(9) -0.0001(6) -0.0019(7) 0.0015(6) O10 0.0267(9) 0.0114(8) 0.0167(8) -0.0003(6) 0.0045(7) -0.0002(7) O11 0.0235(9) 0.0149(8) 0.0267(9) -0.0037(7) -0.0067(7) 0.0051(7) O12 0.0234(9) 0.0119(8) 0.0249(9) -0.0012(7) -0.0074(7) -0.0012(7) O13 0.0391(11) 0.0226(9) 0.0179(9) 0.0066(7) -0.0007(8) -0.0094(8) O14 0.0186(9) 0.0251(10) 0.0431(12) 0.0034(9) 0.0072(8) 0.0013(7) B21 0.0196(13) 0.0177(13) 0.0263(14) 0.0011(11) -0.0011(11) -0.0027(10) O21 0.0199(9) 0.0195(9) 0.0268(9) 0.0061(7) 0.0007(7) -0.0002(7) O22 0.0209(10) 0.0189(10) 0.0627(15) 0.0044(9) 0.0049(9) -0.0014(8) O23 0.0273(10) 0.0215(10) 0.0421(12) 0.0086(9) 0.0054(9) -0.0014(8) B31 0.0186(13) 0.0202(14) 0.0266(14) -0.0035(11) -0.0017(11) 0.0027(10) O31 0.0179(9) 0.0204(9) 0.0370(11) -0.0125(8) -0.0011(8) 0.0012(7) O32 0.0267(10) 0.0202(10) 0.0496(13) -0.0070(9) 0.0074(9) 0.0054(8) O33 0.0211(9) 0.0263(10) 0.0425(12) -0.0088(9) 0.0046(9) -0.0035(8) O41 0.0257(11) 0.0524(14) 0.0371(12) -0.0108(10) -0.0075(9) 0.0077(10) O51 0.040(3) 0.029(2) 0.044(3) -0.0132(19) -0.005(2) 0.0053(18) O52 0.042(3) 0.032(2) 0.017(2) -0.0036(17) -0.0025(19) 0.002(2) O53 0.042(3) 0.032(2) 0.017(2) -0.0036(17) -0.0025(19) 0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 O10 1.451(3) . ? B1 O4 1.452(3) . ? B1 O2 1.456(3) . ? B1 O1 1.533(3) . ? B2 O3 1.445(3) . ? B2 O6 1.462(3) . ? B2 O8 1.490(3) . ? B2 O1 1.506(3) . ? B3 O5 1.438(3) . ? B3 O7 1.451(3) . ? B3 O9 1.487(3) . ? B3 O1 1.504(3) . ? B4 O3 1.364(3) . ? B4 O2 1.369(3) . ? B4 O11 1.376(3) . ? B5 O5 1.364(3) . ? B5 O4 1.366(3) . ? B5 O12 1.373(3) . ? B6 O7 1.357(3) . ? B6 O13 1.376(3) . ? B6 O6 1.381(3) . ? B7 O9 1.367(3) . ? B7 O8 1.372(3) . ? B7 O14 1.378(3) . ? O10 H10 0.8400 . ? O11 H11 0.8400 . ? O12 H12 0.8400 . ? O13 H13 0.8400 . ? O14 H14 0.8400 . ? B21 O22 1.362(4) . ? B21 O21 1.368(3) . ? B21 O23 1.371(3) . ? O21 H21 0.8400 . ? O22 H22 0.8400 . ? O23 H23 0.8400 . ? B31 O31 1.360(3) . ? B31 O32 1.365(3) . ? B31 O33 1.368(4) . ? O31 H31 0.8400 . ? O32 H32 0.8400 . ? O33 H33 0.8400 . ? C1 N1 1.512(8) . ? C1 C7 1.541(8) . ? C1 C2 1.549(8) . ? C1 H1 1.0000 . ? C2 C3 1.564(7) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.489(8) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.434(9) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.500(8) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.519(8) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? N1 H1A 0.9100 . ? N1 H1B 0.9100 . ? N1 H1C 0.9100 . ? C61 N61 1.452(12) . ? C61 C62 1.489(11) . ? C61 C67 1.523(12) . ? C61 H61 1.0000 . ? C62 C63 1.464(13) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.409(13) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C65 1.483(13) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 C66 1.520(13) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 C67 1.496(12) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? N61 H61A 0.9100 . ? N61 H61B 0.9100 . ? N61 H61C 0.9100 . ? C11 N11 1.494(7) . ? C11 C12 1.513(11) . ? C11 C17 1.562(9) . ? C11 H11D 1.0000 . ? C12 C13 1.563(11) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.484(11) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.417(12) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.453(11) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.532(9) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? N11 H11A 0.9100 . ? N11 H11B 0.9100 . ? N11 H11C 0.9100 . ? C21 N21 1.477(16) . ? C21 C22 1.501(17) . ? C21 C27 1.531(16) . ? C21 H21D 1.0000 . ? C22 C23 1.520(17) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.474(17) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.464(17) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.460(17) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.528(16) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? N21 H21A 0.9100 . ? N21 H21B 0.9100 . ? N21 H21C 0.9100 . ? C31 C32 1.475(16) . ? C31 N31 1.496(16) . ? C31 C37 1.554(16) . ? C31 H31D 1.0000 . ? C32 C33 1.489(15) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.490(15) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.457(15) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.422(16) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.517(16) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? N31 H31A 0.9100 . ? N31 H31B 0.9100 . ? N31 H31C 0.9100 . ? C41 C42 1.479(11) . ? C41 N41 1.511(9) . ? C41 C47 1.578(10) . ? C41 H41 1.0000 . ? C42 C43 1.486(12) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.496(14) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.463(13) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.439(14) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.525(14) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? N41 H41A 0.9100 . ? N41 H41B 0.9100 . ? N41 H41C 0.9100 . ? 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 O10 B1 O4 110.21(19) . . ? O10 B1 O2 111.60(19) . . ? O4 B1 O2 111.4(2) . . ? O10 B1 O1 111.73(19) . . ? O4 B1 O1 106.63(18) . . ? O2 B1 O1 105.02(18) . . ? O3 B2 O6 110.71(19) . . ? O3 B2 O8 111.22(18) . . ? O6 B2 O8 110.69(18) . . ? O3 B2 O1 109.55(18) . . ? O6 B2 O1 107.14(18) . . ? O8 B2 O1 107.38(18) . . ? O5 B3 O7 109.76(19) . . ? O5 B3 O9 110.9(2) . . ? O7 B3 O9 111.48(19) . . ? O5 B3 O1 110.40(19) . . ? O7 B3 O1 107.97(19) . . ? O9 B3 O1 106.21(18) . . ? O3 B4 O2 123.5(2) . . ? O3 B4 O11 117.0(2) . . ? O2 B4 O11 119.5(2) . . ? O5 B5 O4 123.2(2) . . ? O5 B5 O12 116.3(2) . . ? O4 B5 O12 120.5(2) . . ? O7 B6 O13 122.9(2) . . ? O7 B6 O6 122.5(2) . . ? O13 B6 O6 114.7(2) . . ? O9 B7 O8 123.7(2) . . ? O9 B7 O14 117.5(2) . . ? O8 B7 O14 118.8(2) . . ? B3 O1 B2 111.52(17) . . ? B3 O1 B1 119.99(17) . . ? B2 O1 B1 117.67(17) . . ? B4 O2 B1 118.49(19) . . ? B4 O3 B2 122.76(18) . . ? B5 O4 B1 122.92(19) . . ? B5 O5 B3 122.29(19) . . ? B6 O6 B2 120.30(19) . . ? B6 O7 B3 120.32(19) . . ? B7 O8 B2 118.87(18) . . ? B7 O9 B3 120.20(19) . . ? B1 O10 H10 109.5 . . ? B4 O11 H11 109.5 . . ? B5 O12 H12 109.5 . . ? B6 O13 H13 109.5 . . ? B7 O14 H14 109.5 . . ? O22 B21 O21 121.7(2) . . ? O22 B21 O23 119.1(2) . . ? O21 B21 O23 119.2(2) . . ? B21 O21 H21 109.5 . . ? B21 O22 H22 109.5 . . ? B21 O23 H23 109.5 . . ? O31 B31 O32 117.4(2) . . ? O31 B31 O33 122.1(2) . . ? O32 B31 O33 120.5(2) . . ? B31 O31 H31 109.5 . . ? B31 O32 H32 109.5 . . ? B31 O33 H33 109.5 . . ? N1 C1 C7 108.0(6) . . ? N1 C1 C2 110.1(6) . . ? C7 C1 C2 113.0(7) . . ? N1 C1 H1 108.5 . . ? C7 C1 H1 108.5 . . ? C2 C1 H1 108.5 . . ? C1 C2 C3 109.5(5) . . ? C1 C2 H2A 109.8 . . ? C3 C2 H2A 109.8 . . ? C1 C2 H2B 109.8 . . ? C3 C2 H2B 109.8 . . ? H2A C2 H2B 108.2 . . ? C4 C3 C2 116.7(5) . . ? C4 C3 H3A 108.1 . . ? C2 C3 H3A 108.1 . . ? C4 C3 H3B 108.1 . . ? C2 C3 H3B 108.1 . . ? H3A C3 H3B 107.3 . . ? C5 C4 C3 126.2(6) . . ? C5 C4 H4A 105.8 . . ? C3 C4 H4A 105.8 . . ? C5 C4 H4B 105.8 . . ? C3 C4 H4B 105.8 . . ? H4A C4 H4B 106.2 . . ? C4 C5 C6 118.5(6) . . ? C4 C5 H5A 107.7 . . ? C6 C5 H5A 107.7 . . ? C4 C5 H5B 107.7 . . ? C6 C5 H5B 107.7 . . ? H5A C5 H5B 107.1 . . ? C5 C6 C7 117.1(6) . . ? C5 C6 H6A 108.0 . . ? C7 C6 H6A 108.0 . . ? C5 C6 H6B 108.0 . . ? C7 C6 H6B 108.0 . . ? H6A C6 H6B 107.3 . . ? C6 C7 C1 116.5(6) . . ? C6 C7 H7A 108.2 . . ? C1 C7 H7A 108.2 . . ? C6 C7 H7B 108.2 . . ? C1 C7 H7B 108.2 . . ? H7A C7 H7B 107.3 . . ? N61 C61 C62 109.0(9) . . ? N61 C61 C67 108.3(10) . . ? C62 C61 C67 119.6(11) . . ? N61 C61 H61 106.4 . . ? C62 C61 H61 106.4 . . ? C67 C61 H61 106.4 . . ? C63 C62 C61 123.6(10) . . ? C63 C62 H62A 106.4 . . ? C61 C62 H62A 106.4 . . ? C63 C62 H62B 106.4 . . ? C61 C62 H62B 106.4 . . ? H62A C62 H62B 106.5 . . ? C64 C63 C62 129.0(12) . . ? C64 C63 H63A 105.0 . . ? C62 C63 H63A 105.0 . . ? C64 C63 H63B 105.0 . . ? C62 C63 H63B 105.0 . . ? H63A C63 H63B 105.9 . . ? C63 C64 C65 120.8(11) . . ? C63 C64 H64A 107.1 . . ? C65 C64 H64A 107.1 . . ? C63 C64 H64B 107.1 . . ? C65 C64 H64B 107.1 . . ? H64A C64 H64B 106.8 . . ? C64 C65 C66 127.5(12) . . ? C64 C65 H65A 105.4 . . ? C66 C65 H65A 105.4 . . ? C64 C65 H65B 105.4 . . ? C66 C65 H65B 105.4 . . ? H65A C65 H65B 106.0 . . ? C67 C66 C65 109.7(10) . . ? C67 C66 H66A 109.7 . . ? C65 C66 H66A 109.7 . . ? C67 C66 H66B 109.7 . . ? C65 C66 H66B 109.7 . . ? H66A C66 H66B 108.2 . . ? C66 C67 C61 116.7(10) . . ? C66 C67 H67A 108.1 . . ? C61 C67 H67A 108.1 . . ? C66 C67 H67B 108.1 . . ? C61 C67 H67B 108.1 . . ? H67A C67 H67B 107.3 . . ? C61 N61 H61A 109.5 . . ? C61 N61 H61B 109.5 . . ? H61A N61 H61B 109.5 . . ? C61 N61 H61C 109.5 . . ? H61A N61 H61C 109.5 . . ? H61B N61 H61C 109.5 . . ? N11 C11 C12 110.0(6) . . ? N11 C11 C17 105.7(5) . . ? C12 C11 C17 110.2(7) . . ? N11 C11 H11D 110.3 . . ? C12 C11 H11D 110.3 . . ? C17 C11 H11D 110.3 . . ? C11 C12 C13 113.6(8) . . ? C11 C12 H12A 108.9 . . ? C13 C12 H12A 108.9 . . ? C11 C12 H12B 108.9 . . ? C13 C12 H12B 108.9 . . ? H12A C12 H12B 107.7 . . ? C14 C13 C12 117.0(8) . . ? C14 C13 H13A 108.0 . . ? C12 C13 H13A 108.0 . . ? C14 C13 H13B 108.0 . . ? C12 C13 H13B 108.0 . . ? H13A C13 H13B 107.3 . . ? C15 C14 C13 108.2(9) . . ? C15 C14 H14A 110.1 . . ? C13 C14 H14A 110.1 . . ? C15 C14 H14B 110.1 . . ? C13 C14 H14B 110.1 . . ? H14A C14 H14B 108.4 . . ? C14 C15 C16 135.9(10) . . ? C14 C15 H15A 103.2 . . ? C16 C15 H15A 103.2 . . ? C14 C15 H15B 103.2 . . ? C16 C15 H15B 103.2 . . ? H15A C15 H15B 105.2 . . ? C15 C16 C17 98.4(7) . . ? C15 C16 H16A 112.1 . . ? C17 C16 H16A 112.1 . . ? C15 C16 H16B 112.1 . . ? C17 C16 H16B 112.1 . . ? H16A C16 H16B 109.7 . . ? C16 C17 C11 114.0(6) . . ? C16 C17 H17A 108.8 . . ? C11 C17 H17A 108.8 . . ? C16 C17 H17B 108.8 . . ? C11 C17 H17B 108.8 . . ? H17A C17 H17B 107.7 . . ? N21 C21 C22 116(2) . . ? N21 C21 C27 112.7(19) . . ? C22 C21 C27 116.3(17) . . ? N21 C21 H21D 103.3 . . ? C22 C21 H21D 103.3 . . ? C27 C21 H21D 103.3 . . ? C21 C22 C23 116.1(19) . . ? C21 C22 H22A 108.3 . . ? C23 C22 H22A 108.3 . . ? C21 C22 H22B 108.3 . . ? C23 C22 H22B 108.3 . . ? H22A C22 H22B 107.4 . . ? C24 C23 C22 120(2) . . ? C24 C23 H23A 107.3 . . ? C22 C23 H23A 107.3 . . ? C24 C23 H23B 107.3 . . ? C22 C23 H23B 107.3 . . ? H23A C23 H23B 106.9 . . ? C25 C24 C23 120(2) . . ? C25 C24 H24A 107.3 . . ? C23 C24 H24A 107.3 . . ? C25 C24 H24B 107.3 . . ? C23 C24 H24B 107.3 . . ? H24A C24 H24B 106.9 . . ? C26 C25 C24 128(2) . . ? C26 C25 H25A 105.2 . . ? C24 C25 H25A 105.2 . . ? C26 C25 H25B 105.2 . . ? C24 C25 H25B 105.2 . . ? H25A C25 H25B 105.9 . . ? C25 C26 C27 110.5(18) . . ? C25 C26 H26A 109.6 . . ? C27 C26 H26A 109.6 . . ? C25 C26 H26B 109.6 . . ? C27 C26 H26B 109.6 . . ? H26A C26 H26B 108.1 . . ? C26 C27 C21 121.5(16) . . ? C26 C27 H27A 106.9 . . ? C21 C27 H27A 106.9 . . ? C26 C27 H27B 106.9 . . ? C21 C27 H27B 106.9 . . ? H27A C27 H27B 106.7 . . ? C21 N21 H21A 109.5 . . ? C21 N21 H21B 109.5 . . ? H21A N21 H21B 109.5 . . ? C21 N21 H21C 109.5 . . ? H21A N21 H21C 109.5 . . ? H21B N21 H21C 109.5 . . ? C32 C31 N31 111.0(18) . . ? C32 C31 C37 121.5(17) . . ? N31 C31 C37 106.4(17) . . ? C32 C31 H31D 105.6 . . ? N31 C31 H31D 105.6 . . ? C37 C31 H31D 105.6 . . ? C31 C32 C33 137.5(19) . . ? C31 C32 H32A 102.7 . . ? C33 C32 H32A 102.7 . . ? C31 C32 H32B 102.7 . . ? C33 C32 H32B 102.7 . . ? H32A C32 H32B 105.0 . . ? C32 C33 C34 120.2(15) . . ? C32 C33 H33A 107.3 . . ? C34 C33 H33A 107.3 . . ? C32 C33 H33B 107.3 . . ? C34 C33 H33B 107.3 . . ? H33A C33 H33B 106.9 . . ? C35 C34 C33 116.6(14) . . ? C35 C34 H34A 108.2 . . ? C33 C34 H34A 108.2 . . ? C35 C34 H34B 108.2 . . ? C33 C34 H34B 108.2 . . ? H34A C34 H34B 107.3 . . ? C36 C35 C34 150.9(16) . . ? C36 C35 H35A 98.9 . . ? C34 C35 H35A 98.9 . . ? C36 C35 H35B 98.9 . . ? C34 C35 H35B 98.9 . . ? H35A C35 H35B 103.9 . . ? C35 C36 C37 118.6(17) . . ? C35 C36 H36A 107.7 . . ? C37 C36 H36A 107.7 . . ? C35 C36 H36B 107.7 . . ? C37 C36 H36B 107.7 . . ? H36A C36 H36B 107.1 . . ? C36 C37 C31 119.7(17) . . ? C36 C37 H37A 107.4 . . ? C31 C37 H37A 107.4 . . ? C36 C37 H37B 107.4 . . ? C31 C37 H37B 107.4 . . ? H37A C37 H37B 106.9 . . ? C42 C41 N41 111.5(8) . . ? C42 C41 C47 117.7(7) . . ? N41 C41 C47 102.4(8) . . ? C42 C41 H41 108.3 . . ? N41 C41 H41 108.3 . . ? C47 C41 H41 108.3 . . ? C41 C42 C43 117.2(9) . . ? C41 C42 H42A 108.0 . . ? C43 C42 H42A 108.0 . . ? C41 C42 H42B 108.0 . . ? C43 C42 H42B 108.0 . . ? H42A C42 H42B 107.2 . . ? C42 C43 C44 113.8(11) . . ? C42 C43 H43A 108.8 . . ? C44 C43 H43A 108.8 . . ? C42 C43 H43B 108.8 . . ? C44 C43 H43B 108.8 . . ? H43A C43 H43B 107.7 . . ? C45 C44 C43 124.7(12) . . ? C45 C44 H44A 106.2 . . ? C43 C44 H44A 106.2 . . ? C45 C44 H44B 106.2 . . ? C43 C44 H44B 106.2 . . ? H44A C44 H44B 106.4 . . ? C46 C45 C44 137.4(11) . . ? C46 C45 H45A 102.8 . . ? C44 C45 H45A 102.8 . . ? C46 C45 H45B 102.8 . . ? C44 C45 H45B 102.8 . . ? H45A C45 H45B 105.0 . . ? C45 C46 C47 111.7(10) . . ? C45 C46 H46A 109.3 . . ? C47 C46 H46A 109.3 . . ? C45 C46 H46B 109.3 . . ? C47 C46 H46B 109.3 . . ? H46A C46 H46B 107.9 . . ? C46 C47 C41 131.2(9) . . ? C46 C47 H47A 104.5 . . ? C41 C47 H47A 104.5 . . ? C46 C47 H47B 104.5 . . ? C41 C47 H47B 104.5 . . ? H47A C47 H47B 105.6 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.867 _refine_diff_density_min -0.649 _refine_diff_density_rms 0.082 #===END