Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _audit_creation_date 99-05-07 _audit_creation_method CRYSTALS _journal_coden_Cambridge 0222 loop_ _publ_author_name 'Michel Etienne' 'Marcus L. Cole' 'Joelle Jaffart' 'Feliu Maseras' 'John McGrady' 'Meike Reinhold' _publ_contact_author_name 'Dr Michel Etienne' _publ_contact_author_address ; Laboratoire de Chimie de Coordination CNRS, UPR8241 205 Route de Narbonne Toulouse Cedex 4 31077 FRANCE ; _publ_contact_author_phone ' +33 (0)5 61 33 31 76' _publ_contact_author_fax ' +33 (0)5 61 55 30 03' _publ_contact_author_email etienne@lcc-toulouse.fr _publ_section_title ; C-H and C-C Agostic Interactions in Cycloalkyl Tris(pyrazolyl)boratoniobium Complexes ; _publ_requested_coeditor_name ' ?' _publ_contact_letter ; Please consider this CIF submission for publication as Supplementary material to a 'J. Chem. Soc., Dalton Trans.' paper ; data_compound1 _database_code_CSD 210405 #================================================================= # 4. TEXT _publ_section_exptl_refinement ; #LIST 12 FULL NB(1, X'S, U'S) UNTIL C(513), C(1000, X'S, U[ISO]) UNTIL H(11) END #USE LAST In the asymmetric unit, half a molecule of toluene is disordered around the inversion center. The corresponding carbon atoms C(1000) to C(5000) were refined isotropically with half occupancy for C(2000), C(3000) and C(4000). ; _publ_section_references # Add your own references - in alphabetic order ; Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435 Carruthers, J.R. and Watkin, D.J. (1979), (Chebychev Weighting) Acta Cryst, A35, 698-699 Watkin, D.J., Prout, C.K. Carruthers, R.J. & Betteridge, P. (1996) CRYSTALS Issue 10. Chemical Crystallography Laboratory, OXFORD, UK. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; #========================================================================== # Now, all the strucure specific goodies #========================================================================== _computing_data_collection ' STOE IPDS ' _computing_cell_refinement ' STOE IPDS ' _computing_data_reduction ; STOE XRED ; _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_publication_material ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_molecular_graphics ; CAMERON (Watkin, Prout & Pearce, 1996) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' #========================================================================== # NOW THE GOODIES TO BE ENTERED BY HAND #========================================================================== _chemical_melting_point ? _diffrn_radiation_monochromator graphite _diffrn_measurement_device ' STOE IPDS ' _refine_ls_matrix_type full _refine_ls_weighting_scheme ; w = w'[1-(?F/6?(F))2]2. w' = 1/?(r=1,3)ArTr(x) where Ar are the coefficients for the Chebyshev polynomial Tr(x) with x = Fc/Fc(max) (Carruthers & Watkin, 1979) coef 1.76, -2.34, 1.57, -0.939, 0.220 ; _atom_sites_solution_primary 'Direct_Methods SIR92' _atom_sites_solution_hydrogens 'Geometric or located (Fourier difference)' _refine_ls_hydrogen_treatment ; H atoms placed geometrically after each cycle, except H1 and H11 located and refined isotropically ; #**************************************************************************** _chemical_name_systematic ; # IUPAC name, in full ? ; _cell_length_a 39.571(5) _cell_angle_alpha 90 _cell_length_b 13.711(1) _cell_angle_beta 96.52(2) _cell_length_c 10.669(1) _cell_angle_gamma 90 _cell_volume 5751(1) _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'C 2/c ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x+1/2,y+1/2,z -x+1/2,-y+1/2,-z -x,y,-z+1/2 x,-y,z+1/2 -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'B ' 0.0000 0.0010 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 International_Tables_Vol_IV_Table_2.2B 'Cl ' 0.1320 0.1590 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 International_Tables_Vol_IV_Table_2.2B 'Nb ' -2.1970 0.6210 17.6142 1.1887 12.0144 11.7660 4.0418 0.2048 3.5335 69.7957 3.7559 International_Tables_Vol_IV_Table_2.2B _chemical_formula_sum ' C24 H37 Nb1 Cl1 N6 B1, 0.5 C7 H8' _chemical_formula_moiety ' C24 H37 Nb1 Cl1 N6 B1, 0.5 C7 H8' _chemical_compound_source ; ? ; _chemical_formula_weight 594.84 _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 1.6 _cell_measurement_theta_max 27.6 _cell_measurement_temperature 160 _cell_formula_units_Z 8 _exptl_crystal_description ' box ' _exptl_crystal_colour ' orange ' _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_max 0.40 _exptl_crystal_density_diffrn 1.37 _exptl_crystal_density_meas ? _exptl_crystal_F_000 2354 _exptl_absorpt_coefficient_mu 0.54 _exptl_absorpt_correction_type none _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 160 _diffrn_reflns_number 3734 _reflns_number_total 16617 _diffrn_reflns_av_R_equivalents 0.00 _reflns_number_observed 2705 _diffrn_reflns_theta_min 1.6 _diffrn_reflns_theta_max 27.6 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 11 _reflns_limit_h_min -42 _reflns_limit_h_max 41 _reflns_limit_k_min 0 _reflns_limit_k_max 14 _reflns_limit_l_min 0 _reflns_limit_l_max 11 _reflns_observed_criterion >2.00\s(I) _refine_diff_density_min -0.37 _refine_diff_density_max 0.71 _refine_ls_number_reflns 2705 _refine_ls_number_parameters 351 _refine_ls_R_factor_obs 0.0340 _refine_ls_wR_factor_obs 0.0349 _refine_ls_goodness_of_fit_obs 1.1384 _refine_ls_shift/esd_max 0.001378 _refine_ls_structure_factor_coef F _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f rotation' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_calc_flag NB1 0.100714(9) 0.25982(2) 0.09981(3) 0.0253 1.0000 Uani d CL1 0.11744(3) 0.28119(8) -0.11067(9) 0.0412 1.0000 Uani d N1 0.10271(8) 0.2518(2) 0.3156(3) 0.0297 1.0000 Uani d N2 0.13384(8) 0.2399(2) 0.3869(3) 0.0265 1.0000 Uani d N3 0.15100(8) 0.1660(2) 0.1320(3) 0.0257 1.0000 Uani d N4 0.17409(8) 0.1847(2) 0.2363(3) 0.0247 1.0000 Uani d N5 0.13863(8) 0.3788(2) 0.1673(3) 0.0301 1.0000 Uani d N6 0.16326(8) 0.3637(2) 0.2667(3) 0.0266 1.0000 Uani d B1 0.1669(1) 0.2635(3) 0.3312(4) 0.0256 1.0000 Uani d C1 0.0772(1) 0.1173(3) 0.1112(4) 0.0316 1.0000 Uani d C2 0.0930(1) 0.0375(3) 0.2017(4) 0.0363 1.0000 Uani d C3 0.0635(1) -0.0212(3) 0.2425(4) 0.0431 1.0000 Uani d C4 0.0363(1) -0.0126(4) 0.1312(4) 0.0452 1.0000 Uani d C5 0.0390(1) 0.0928(3) 0.0922(4) 0.0431 1.0000 Uani d C6 0.0286(1) 0.3071(4) -0.0966(5) 0.0568 1.0000 Uani d C7 0.0546(1) 0.3112(3) 0.0161(4) 0.0380 1.0000 Uani d C8 0.0640(1) 0.3650(3) 0.1145(4) 0.0357 1.0000 Uani d C9 0.0531(1) 0.4514(4) 0.1823(5) 0.0568 1.0000 Uani d C101 0.0793(1) 0.2394(3) 0.3960(4) 0.0335 1.0000 Uani d C102 0.0953(1) 0.2195(3) 0.5156(4) 0.0348 1.0000 Uani d C103 0.1294(1) 0.2202(3) 0.5080(4) 0.0284 1.0000 Uani d C111 0.0421(1) 0.2486(4) 0.3595(4) 0.0483 1.0000 Uani d C113 0.1582(1) 0.2026(3) 0.6079(4) 0.0388 1.0000 Uani d C301 0.1642(1) 0.0927(3) 0.0710(4) 0.0271 1.0000 Uani d C302 0.1952(1) 0.0649(3) 0.1337(4) 0.0295 1.0000 Uani d C303 0.2009(1) 0.1242(3) 0.2369(4) 0.0287 1.0000 Uani d C311 0.1473(1) 0.0483(3) -0.0480(4) 0.0352 1.0000 Uani d C313 0.2306(1) 0.1275(3) 0.3361(4) 0.0417 1.0000 Uani d C501 0.1424(1) 0.4710(3) 0.1296(4) 0.0344 1.0000 Uani d C502 0.1690(1) 0.5149(3) 0.2053(4) 0.0371 1.0000 Uani d C503 0.1818(1) 0.4457(3) 0.2909(4) 0.0328 1.0000 Uani d C511 0.1209(1) 0.5145(3) 0.0192(5) 0.0497 1.0000 Uani d C513 0.2101(1) 0.4526(3) 0.3936(4) 0.0447 1.0000 Uani d C1000 0.2692(2) 0.3414(5) 0.1537(7) 0.088(2) 1.0000 Uiso d C2000 0.2907(3) 0.2615(7) 0.0874(9) 0.051(2) 0.5000 Uiso d C3000 0.2448(3) 0.2098(7) -0.0621(9) 0.048(2) 0.5000 Uiso d C4000 0.2643(3) 0.1654(8) -0.089(1) 0.056(3) 0.5000 Uiso d C5000 0.2776(1) 0.2130(4) -0.0009(5) 0.055(1) 1.0000 Uiso d H1 0.1881(9) 0.264(3) 0.404(3) 0.03(1) 1.0000 Uiso d H11 0.086(1) 0.111(3) 0.033(4) 0.03(1) 1.0000 Uiso d H21 0.1058 0.0667 0.2738 0.0430 1.0000 Uiso calc H22 0.1076 -0.0039 0.1591 0.0430 1.0000 Uiso calc H31 0.0699 -0.0881 0.2576 0.0517 1.0000 Uiso calc H32 0.0558 0.0060 0.3172 0.0517 1.0000 Uiso calc H41 0.0408 -0.0558 0.0643 0.0542 1.0000 Uiso calc H42 0.0142 -0.0265 0.1557 0.0542 1.0000 Uiso calc H51 0.0267 0.1340 0.1441 0.0497 1.0000 Uiso calc H52 0.0301 0.1010 0.0053 0.0497 1.0000 Uiso calc H61 0.0322 0.2497 -0.1450 0.0651 1.0000 Uiso calc H62 0.0306 0.3640 -0.1478 0.0651 1.0000 Uiso calc H63 0.0063 0.3050 -0.0696 0.0651 1.0000 Uiso calc H91 0.0694 0.4644 0.2543 0.0694 1.0000 Uiso calc H92 0.0517 0.5068 0.1269 0.0694 1.0000 Uiso calc H93 0.0312 0.4392 0.2097 0.0694 1.0000 Uiso calc H1021 0.0843 0.2075 0.5899 0.0417 1.0000 Uiso calc H1111 0.0379 0.2626 0.2709 0.0562 1.0000 Uiso calc H1112 0.0333 0.3006 0.4066 0.0562 1.0000 Uiso calc H1113 0.0311 0.1886 0.3772 0.0562 1.0000 Uiso calc H1131 0.1494 0.1900 0.6867 0.0441 1.0000 Uiso calc H1132 0.1726 0.2590 0.6163 0.0441 1.0000 Uiso calc H1133 0.1710 0.1472 0.5853 0.0441 1.0000 Uiso calc H3021 0.2098 0.0140 0.1096 0.0351 1.0000 Uiso calc H3111 0.1614 -0.0029 -0.0749 0.0421 1.0000 Uiso calc H3112 0.1441 0.0974 -0.1124 0.0421 1.0000 Uiso calc H3113 0.1257 0.0221 -0.0330 0.0421 1.0000 Uiso calc H3131 0.2468 0.0785 0.3189 0.0484 1.0000 Uiso calc H3132 0.2411 0.1906 0.3361 0.0484 1.0000 Uiso calc H3133 0.2231 0.1154 0.4170 0.0484 1.0000 Uiso calc H5021 0.1769 0.5808 0.1990 0.0436 1.0000 Uiso calc H5111 0.1045 0.4674 -0.0152 0.0582 1.0000 Uiso calc H5112 0.1351 0.5329 -0.0441 0.0582 1.0000 Uiso calc H5113 0.1094 0.5711 0.0461 0.0582 1.0000 Uiso calc H5131 0.2198 0.5168 0.3944 0.0539 1.0000 Uiso calc H5132 0.2272 0.4053 0.3800 0.0539 1.0000 Uiso calc H5133 0.2017 0.4401 0.4730 0.0539 1.0000 Uiso calc 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 NB1 0.0242(2) 0.0283(2) 0.0229(2) 0.0026(2) 0.0013(1) 0.0031(2) CL1 0.0501(7) 0.0482(7) 0.0266(5) 0.0066(5) 0.0105(5) 0.0127(5) N1 0.026(2) 0.031(2) 0.033(2) 0.002(2) 0.004(1) -0.002(2) N2 0.028(2) 0.026(2) 0.025(2) -0.001(1) 0.003(1) -0.001(1) N3 0.027(2) 0.026(2) 0.024(2) -0.000(1) 0.001(2) -0.000(1) N4 0.025(2) 0.028(2) 0.020(2) 0.000(1) -0.002(1) -0.000(1) N5 0.030(2) 0.030(2) 0.031(2) 0.005(2) 0.005(2) 0.004(1) N6 0.031(2) 0.024(2) 0.026(2) -0.001(1) 0.006(2) -0.001(1) B1 0.028(2) 0.024(2) 0.023(2) 0.001(2) -0.001(2) 0.001(2) C1 0.029(2) 0.038(2) 0.027(2) -0.003(2) 0.002(2) 0.002(2) C2 0.038(3) 0.032(2) 0.038(3) 0.007(2) -0.001(2) -0.004(2) C3 0.049(3) 0.043(3) 0.038(3) -0.005(2) 0.008(2) -0.009(2) C4 0.040(3) 0.054(3) 0.043(3) -0.010(2) 0.010(2) -0.018(2) C5 0.030(2) 0.051(3) 0.047(3) -0.007(2) -0.002(2) -0.004(2) C6 0.043(3) 0.074(4) 0.050(3) 0.010(3) -0.008(2) 0.015(3) C7 0.036(3) 0.043(3) 0.035(3) 0.009(2) 0.008(2) 0.007(2) C8 0.033(2) 0.035(2) 0.041(3) 0.007(2) 0.009(2) 0.005(2) C9 0.052(3) 0.061(3) 0.061(3) -0.001(3) 0.022(3) 0.020(3) C101 0.038(2) 0.030(2) 0.034(2) -0.004(2) 0.012(2) -0.006(2) C102 0.047(3) 0.032(2) 0.028(2) 0.001(2) 0.016(2) -0.007(2) C103 0.040(3) 0.022(2) 0.024(2) -0.002(2) 0.006(2) -0.004(2) C111 0.034(2) 0.069(3) 0.044(3) -0.001(3) 0.013(2) -0.005(2) C113 0.055(3) 0.037(2) 0.024(2) 0.004(2) 0.005(2) -0.001(2) C301 0.030(2) 0.026(2) 0.025(2) 0.002(2) 0.004(2) 0.001(2) C302 0.030(2) 0.025(2) 0.034(2) 0.000(2) 0.003(2) 0.007(2) C303 0.026(2) 0.027(2) 0.033(2) 0.007(2) 0.006(2) 0.006(2) C311 0.039(3) 0.033(2) 0.033(2) -0.005(2) 0.005(2) 0.003(2) C313 0.032(3) 0.050(3) 0.041(3) 0.001(2) -0.005(2) 0.012(2) C501 0.042(3) 0.023(2) 0.040(3) 0.010(2) 0.017(2) 0.005(2) C502 0.042(3) 0.023(2) 0.049(3) -0.001(2) 0.019(2) -0.007(2) C503 0.036(2) 0.033(2) 0.033(2) -0.010(2) 0.016(2) -0.008(2) C511 0.059(3) 0.033(3) 0.058(3) 0.020(2) 0.011(3) 0.004(2) C513 0.050(3) 0.043(3) 0.042(3) -0.011(2) 0.009(2) -0.020(2) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag NB1 . CL1 . 2.430(1) yes NB1 . N1 . 2.297(3) yes NB1 . N3 . 2.361(3) yes NB1 . N5 . 2.277(3) yes NB1 . C1 . 2.174(4) yes NB1 . C7 . 2.061(4) yes NB1 . C8 . 2.065(4) yes N1 . N2 . 1.382(4) yes N1 . C101 . 1.344(5) yes N2 . B1 . 1.531(5) yes N2 . C103 . 1.351(5) yes N3 . N4 . 1.381(4) yes N3 . C301 . 1.337(5) yes N4 . B1 . 1.529(5) yes N4 . C303 . 1.346(5) yes N5 . N6 . 1.372(4) yes N5 . C501 . 1.341(5) yes N6 . B1 . 1.536(5) yes N6 . C503 . 1.351(5) yes B1 . H1 . 1.08(4) no C1 . C2 . 1.544(6) yes C1 . C5 . 1.540(6) yes C1 . H11 . 0.94(4) no C2 . C3 . 1.523(6) yes C2 . H21 . 0.960(4) no C2 . H22 . 0.960(4) no C3 . C4 . 1.513(7) yes C3 . H31 . 0.960(5) no C3 . H32 . 0.960(5) no C4 . C5 . 1.511(7) yes C4 . H41 . 0.960(5) no C4 . H42 . 0.960(4) no C5 . H51 . 0.960(5) no C5 . H52 . 0.960(5) no C6 . C7 . 1.494(6) yes C6 . H61 . 0.960(6) no C6 . H62 . 0.960(5) no C6 . H63 . 0.960(5) no C7 . C8 . 1.303(6) yes C8 . C9 . 1.478(6) yes C9 . H91 . 0.960(6) no C9 . H92 . 0.960(5) no C9 . H93 . 0.960(5) no C101 . C102 . 1.385(6) yes C101 . C111 . 1.483(6) yes C102 . C103 . 1.362(6) yes C102 . H1021 . 0.960(4) no C103 . C113 . 1.488(6) yes C111 . H1111 . 0.960(5) no C111 . H1112 . 0.960(5) no C111 . H1113 . 0.960(5) no C113 . H1131 . 0.960(4) no C113 . H1132 . 0.960(4) no C113 . H1133 . 0.960(4) no C301 . C302 . 1.380(5) yes C301 . C311 . 1.495(6) yes C302 . C303 . 1.366(6) yes C302 . H3021 . 0.960(4) no C303 . C313 . 1.490(6) yes C311 . H3111 . 0.960(4) no C311 . H3112 . 0.960(4) no C311 . H3113 . 0.960(4) no C313 . H3131 . 0.960(4) no C313 . H3132 . 0.960(5) no C313 . H3133 . 0.960(5) no C501 . C502 . 1.389(6) yes C501 . C511 . 1.496(6) yes C502 . C503 . 1.373(6) yes C502 . H5021 . 0.960(4) no C503 . C513 . 1.478(6) yes C511 . H5111 . 0.960(5) no C511 . H5112 . 0.960(5) no C511 . H5113 . 0.960(5) no C513 . H5131 . 0.960(4) no C513 . H5132 . 0.960(5) no C513 . H5133 . 0.960(4) no C1000 . C2000 . 1.60(1) yes C1000 . C3000 4_555 1.28(1) yes C1000 . C4000 4_555 1.43(1) yes C2000 . C3000 4_555 1.46(1) yes C2000 . C5000 . 1.22(1) yes C3000 . C3000 4_555 1.74(2) yes C3000 . C4000 . 1.05(1) yes C3000 . C5000 . 1.38(1) yes C3000 . C5000 4_555 1.58(1) yes C4000 . C5000 . 1.21(1) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag CL1 . NB1 . N1 . 161.81(8) yes CL1 . NB1 . N3 . 83.50(8) yes N1 . NB1 . N3 . 84.0(1) yes CL1 . NB1 . N5 . 88.10(9) yes N1 . NB1 . N5 . 76.8(1) yes N3 . NB1 . N5 . 80.2(1) yes CL1 . NB1 . C1 . 108.9(1) yes N1 . NB1 . C1 . 82.4(1) yes N3 . NB1 . C1 . 82.0(1) yes N5 . NB1 . C1 . 153.8(1) yes CL1 . NB1 . C7 . 83.0(1) yes N1 . NB1 . C7 . 112.2(1) yes N3 . NB1 . C7 . 159.8(1) yes N5 . NB1 . C7 . 114.3(2) yes C1 . NB1 . C7 . 88.2(2) yes CL1 . NB1 . C8 . 104.7(1) yes N1 . NB1 . C8 . 84.4(1) yes N3 . NB1 . C8 . 163.2(1) yes N5 . NB1 . C8 . 85.4(1) yes C1 . NB1 . C8 . 108.4(2) yes C7 . NB1 . C8 . 36.8(2) yes NB1 . N1 . N2 . 119.0(2) yes NB1 . N1 . C101 . 134.3(3) yes N2 . N1 . C101 . 105.6(3) yes N1 . N2 . B1 . 120.5(3) yes N1 . N2 . C103 . 110.2(3) yes B1 . N2 . C103 . 128.6(3) yes NB1 . N3 . N4 . 119.0(2) yes NB1 . N3 . C301 . 135.2(3) yes N4 . N3 . C301 . 105.8(3) yes N3 . N4 . B1 . 120.5(3) yes N3 . N4 . C303 . 109.8(3) yes B1 . N4 . C303 . 129.7(3) yes NB1 . N5 . N6 . 121.4(2) yes NB1 . N5 . C501 . 132.3(3) yes N6 . N5 . C501 . 106.3(3) yes N5 . N6 . B1 . 120.2(3) yes N5 . N6 . C503 . 110.2(3) yes B1 . N6 . C503 . 129.6(3) yes N2 . B1 . N4 . 109.9(3) yes N2 . B1 . N6 . 108.9(3) yes N4 . B1 . N6 . 110.5(3) yes N2 . B1 . H1 . 110.3(19) no N4 . B1 . H1 . 106.9(19) no N6 . B1 . H1 . 110.3(20) no NB1 . C1 . C2 . 121.8(3) yes NB1 . C1 . C5 . 127.5(3) yes C2 . C1 . C5 . 104.4(4) yes NB1 . C1 . H11 . 79.9(24) no C2 . C1 . H11 . 109.3(25) no C5 . C1 . H11 . 108.6(25) no C1 . C2 . C3 . 106.5(3) yes C1 . C2 . H21 . 110.2(4) no C3 . C2 . H21 . 110.2(4) no C1 . C2 . H22 . 110.2(4) no C3 . C2 . H22 . 110.2(4) no H21 . C2 . H22 . 109.5(4) no C2 . C3 . C4 . 103.6(4) yes C2 . C3 . H31 . 110.9(4) no C4 . C3 . H31 . 110.9(4) no C2 . C3 . H32 . 110.9(4) no C4 . C3 . H32 . 110.9(4) no H31 . C3 . H32 . 109.5(4) no C3 . C4 . C5 . 103.0(4) yes C3 . C4 . H41 . 111.1(4) no C5 . C4 . H41 . 111.1(4) no C3 . C4 . H42 . 111.1(4) no C5 . C4 . H42 . 111.1(5) no H41 . C4 . H42 . 109.5(4) no C1 . C5 . C4 . 105.7(4) yes C1 . C5 . H51 . 110.4(4) no C4 . C5 . H51 . 110.4(4) no C1 . C5 . H52 . 110.4(4) no C4 . C5 . H52 . 110.4(4) no H51 . C5 . H52 . 109.5(4) no C7 . C6 . H61 . 109.5(4) no C7 . C6 . H62 . 109.5(5) no H61 . C6 . H62 . 109.5(5) no C7 . C6 . H63 . 109.5(4) no H61 . C6 . H63 . 109.5(5) no H62 . C6 . H63 . 109.5(5) no NB1 . C7 . C6 . 146.3(3) yes NB1 . C7 . C8 . 71.8(3) yes C6 . C7 . C8 . 141.1(4) yes NB1 . C8 . C7 . 71.4(3) yes NB1 . C8 . C9 . 147.6(4) yes C7 . C8 . C9 . 140.9(4) yes C8 . C9 . H91 . 109.5(4) no C8 . C9 . H92 . 109.5(4) no H91 . C9 . H92 . 109.5(6) no C8 . C9 . H93 . 109.5(5) no H91 . C9 . H93 . 109.5(5) no H92 . C9 . H93 . 109.5(5) no N1 . C101 . C102 . 109.7(4) yes N1 . C101 . C111 . 123.8(4) yes C102 . C101 . C111 . 126.5(4) yes C101 . C102 . C103 . 107.3(3) yes C101 . C102 . H1021 . 126.4(4) no C103 . C102 . H1021 . 126.4(4) no N2 . C103 . C102 . 107.2(3) yes N2 . C103 . C113 . 123.1(4) yes C102 . C103 . C113 . 129.7(4) yes C101 . C111 . H1111 . 109.5(4) no C101 . C111 . H1112 . 109.5(4) no H1111 . C111 . H1112 . 109.5(5) no C101 . C111 . H1113 . 109.5(4) no H1111 . C111 . H1113 . 109.5(5) no H1112 . C111 . H1113 . 109.5(4) no C103 . C113 . H1131 . 109.5(4) no C103 . C113 . H1132 . 109.5(4) no H1131 . C113 . H1132 . 109.5(4) no C103 . C113 . H1133 . 109.5(4) no H1131 . C113 . H1133 . 109.5(4) no H1132 . C113 . H1133 . 109.5(5) no N3 . C301 . C302 . 110.2(3) yes N3 . C301 . C311 . 123.9(3) yes C302 . C301 . C311 . 125.9(4) yes C301 . C302 . C303 . 106.5(3) yes C301 . C302 . H3021 . 126.7(4) no C303 . C302 . H3021 . 126.7(4) no N4 . C303 . C302 . 107.7(3) yes N4 . C303 . C313 . 122.8(4) yes C302 . C303 . C313 . 129.5(4) yes C301 . C311 . H3111 . 109.5(4) no C301 . C311 . H3112 . 109.5(4) no H3111 . C311 . H3112 . 109.5(4) no C301 . C311 . H3113 . 109.5(4) no H3111 . C311 . H3113 . 109.5(4) no H3112 . C311 . H3113 . 109.5(4) no C303 . C313 . H3131 . 109.5(4) no C303 . C313 . H3132 . 109.5(4) no H3131 . C313 . H3132 . 109.5(4) no C303 . C313 . H3133 . 109.5(4) no H3131 . C313 . H3133 . 109.5(4) no H3132 . C313 . H3133 . 109.5(4) no N5 . C501 . C502 . 109.7(4) yes N5 . C501 . C511 . 122.6(4) yes C502 . C501 . C511 . 127.6(4) yes C501 . C502 . C503 . 106.6(3) yes C501 . C502 . H5021 . 126.7(4) no C503 . C502 . H5021 . 126.7(5) no N6 . C503 . C502 . 107.3(4) yes N6 . C503 . C513 . 122.9(4) yes C502 . C503 . C513 . 129.8(4) yes C501 . C511 . H5111 . 109.5(4) no C501 . C511 . H5112 . 109.5(4) no H5111 . C511 . H5112 . 109.5(5) no C501 . C511 . H5113 . 109.5(5) no H5111 . C511 . H5113 . 109.5(5) no H5112 . C511 . H5113 . 109.5(4) no C503 . C513 . H5131 . 109.5(4) no C503 . C513 . H5132 . 109.5(4) no H5131 . C513 . H5132 . 109.5(4) no C503 . C513 . H5133 . 109.5(4) no H5131 . C513 . H5133 . 109.5(4) no H5132 . C513 . H5133 . 109.5(5) no C2000 . C1000 . C3000 4_555 59.6(7) yes C2000 . C1000 . C4000 4_555 104.6(7) yes C3000 4_555 C1000 . C4000 4_555 45.1(6) yes C1000 . C2000 . C3000 4_555 49.2(5) yes C1000 . C2000 . C5000 . 120.9(8) yes C3000 4_555 C2000 . C5000 . 71.7(7) yes C1000 4_555 C3000 . C2000 4_555 71.2(7) yes C1000 4_555 C3000 . C3000 4_555 167.5(12) yes C2000 4_555 C3000 . C3000 4_555 96.2(9) yes C1000 4_555 C3000 . C4000 . 75.0(9) yes C2000 4_555 C3000 . C4000 . 146.3(12) yes C3000 4_555 C3000 . C4000 . 117.5(12) yes C1000 4_555 C3000 . C5000 . 133.0(9) yes C2000 4_555 C3000 . C5000 . 155.8(9) yes C3000 4_555 C3000 . C5000 . 59.5(6) yes C4000 . C3000 . C5000 . 58.0(8) yes C1000 4_555 C3000 . C5000 4_555 118.4(8) yes C2000 4_555 C3000 . C5000 4_555 47.2(5) yes C3000 4_555 C3000 . C5000 4_555 49.1(5) yes C4000 . C3000 . C5000 4_555 166.5(11) yes C5000 . C3000 . C5000 4_555 108.6(7) yes C1000 4_555 C4000 . C3000 . 59.9(8) yes C1000 4_555 C4000 . C5000 . 135.0(10) yes C3000 . C4000 . C5000 . 75.1(9) yes C2000 . C5000 . C3000 . 132.5(8) yes C2000 . C5000 . C3000 4_555 61.2(6) yes C3000 . C5000 . C3000 4_555 71.4(7) yes C2000 . C5000 . C4000 . 179.4(9) yes C3000 . C5000 . C4000 . 46.9(6) yes C3000 4_555 C5000 . C4000 . 118.3(7) yes