#------------------------------------------------------------------------------ #$Date: 2014-07-12 04:47:43 +0300 (Sat, 12 Jul 2014) $ #$Revision: 120105 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/32/27/4322700.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4322700 loop_ _publ_author_name 'Charles G. Young' 'Simon Thomas' 'Robert W. Gable' _publ_section_title ; Halocarbonyltungsten(II) Complexes Containing Tripodal Tris(pyrazolyl)borate Ligands ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 1299 _journal_page_last 1306 _journal_volume 37 _journal_year 1998 _chemical_formula_sum 'C22 H32 B I N6 O4 W' _chemical_formula_weight 766.10 _chemical_name_systematic ; ? ; _space_group_IT_number 61 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_space_group_name_H-M 'P b c a' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 11.779(2) _cell_length_b 15.975(4) _cell_length_c 29.476(3) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(1) _cell_measurement_theta_max 14.3 _cell_measurement_theta_min 10.4 _cell_volume 5546.5(18) _computing_cell_refinement 'CAD-4 Software' _computing_data_collection 'CAD-4 Software (Enraf-Nonius, 1989)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL-93 _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(1) _diffrn_measurement_device 'Enraf-Nonius CAD-4MachS diffractometer' _diffrn_measurement_method \w:2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0412 _diffrn_reflns_av_sigmaI/netI 0.0666 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_number 7944 _diffrn_reflns_theta_max 27.47 _diffrn_reflns_theta_min 2.21 _diffrn_standards_decay_% 6 _diffrn_standards_interval_time 160 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 5.316 _exptl_absorpt_correction_T_max 0.7058 _exptl_absorpt_correction_T_min 0.5703 _exptl_absorpt_correction_type 'Gaussian integration (Sheldrick, 1976)' _exptl_crystal_colour brown _exptl_crystal_density_diffrn 1.835 _exptl_crystal_density_meas 'Not measured' _exptl_crystal_density_method none _exptl_crystal_description needle _exptl_crystal_F_000 2960 _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _refine_diff_density_max 1.602 _refine_diff_density_min -1.241 _refine_diff_density_rms 0.140 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 1.031 _refine_ls_goodness_of_fit_obs 1.100 _refine_ls_hydrogen_treatment 'geom, except methanol H-atoms not included' _refine_ls_matrix_type full _refine_ls_number_parameters 354 _refine_ls_number_reflns 6341 _refine_ls_number_restraints 8 _refine_ls_restrained_S_all 1.034 _refine_ls_restrained_S_obs 1.100 _refine_ls_R_factor_all 0.0962 _refine_ls_R_factor_obs 0.0379 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0433P)^2^+7.3180P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_wR_factor_all 0.0948 _refine_ls_wR_factor_obs 0.0797 _reflns_number_observed 4083 _reflns_number_total 6346 _reflns_observed_criterion >2sigma(I) _[local]_cod_data_source_file ic970838w_1.cif _[local]_cod_data_source_block '[L^Pr^WI(CO)~3~.CH~3~OH]' _cod_database_code 4322700 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' 'x-1/2, y, -z-1/2' 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 W 0.02865(12) 0.03340(13) 0.03092(12) 0.00227(11) -0.00124(12) -0.00024(12) I 0.0545(4) 0.0550(4) 0.0584(3) -0.0129(2) -0.0098(3) -0.0105(3) C1 0.029(3) 0.037(3) 0.052(4) 0.008(3) -0.005(3) -0.002(3) O1 0.049(3) 0.076(4) 0.039(3) -0.001(2) 0.013(2) 0.001(3) C2 0.037(4) 0.048(4) 0.043(4) 0.004(3) -0.001(3) 0.004(3) O2 0.065(4) 0.050(3) 0.075(4) 0.010(3) -0.004(3) 0.004(3) C3 0.036(4) 0.044(4) 0.050(5) -0.002(3) -0.007(4) 0.003(4) O3 0.032(4) 0.094(8) 0.080(6) -0.016(5) 0.000(5) 0.013(5) N11 0.029(3) 0.036(3) 0.039(3) 0.003(2) -0.003(2) 0.003(2) N12 0.033(3) 0.035(3) 0.048(3) 0.005(2) -0.005(2) -0.002(2) C11 0.046(4) 0.040(4) 0.059(4) 0.003(3) 0.010(4) -0.010(3) C12 0.047(4) 0.044(4) 0.058(4) -0.003(3) 0.000(4) -0.012(4) C13 0.031(4) 0.044(4) 0.046(4) -0.003(3) -0.001(3) 0.003(3) C14 0.045(4) 0.043(4) 0.059(4) 0.003(3) -0.016(4) -0.007(4) C15 0.050(5) 0.086(7) 0.098(8) -0.001(6) -0.031(5) -0.001(5) C16 0.098(9) 0.082(7) 0.048(5) -0.007(5) -0.002(5) -0.012(6) N21 0.039(3) 0.055(3) 0.034(3) 0.003(2) -0.003(3) 0.004(3) N22 0.045(4) 0.051(3) 0.035(3) 0.014(2) 0.000(2) 0.000(3) C21 0.075(6) 0.072(5) 0.037(4) 0.015(4) 0.006(4) 0.001(5) C22 0.079(6) 0.086(6) 0.039(4) 0.008(4) 0.023(4) 0.004(6) C23 0.048(4) 0.071(5) 0.033(3) 0.002(3) 0.005(3) 0.005(4) C24 0.076(6) 0.071(6) 0.044(4) -0.002(4) 0.009(4) 0.017(5) C25 0.116(11) 0.089(8) 0.065(6) -0.017(5) 0.021(6) 0.016(7) C26 0.077(7) 0.127(10) 0.070(6) 0.020(7) 0.028(6) 0.047(7) N31 0.030(3) 0.034(3) 0.046(3) 0.008(2) -0.003(2) 0.003(2) N32 0.038(3) 0.042(3) 0.048(3) 0.009(3) -0.008(3) 0.001(3) C31 0.044(4) 0.054(4) 0.061(4) 0.013(4) -0.011(4) 0.013(4) C32 0.031(4) 0.057(4) 0.066(5) 0.005(4) -0.003(4) 0.010(4) C33 0.034(4) 0.044(4) 0.042(4) -0.005(3) -0.003(3) -0.004(3) C34 0.033(4) 0.060(5) 0.056(4) 0.014(4) 0.000(3) -0.002(4) C35 0.061(6) 0.088(7) 0.073(6) 0.006(5) 0.023(5) 0.013(6) C36 0.045(5) 0.082(6) 0.093(7) -0.004(5) -0.010(5) -0.028(5) B 0.043(5) 0.041(4) 0.053(5) 0.014(4) -0.006(4) -0.002(4) 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group W W 0.02796(2) 0.298993(15) 0.393073(8) 0.03099(8) Uani 1 d D . I I -0.08907(8) 0.17825(5) 0.33945(2) 0.0560(2) Uani 0.920(2) d PD 1 IA I 0.2640(6) 0.2661(16) 0.4066(9) 0.070(4) Uiso 0.080(2) d PD 2 C1 C -0.0331(6) 0.3040(4) 0.4558(2) 0.0393(14) Uani 1 d . . O1 O -0.0691(4) 0.3086(3) 0.4907(2) 0.0548(13) Uani 1 d . . C2 C 0.0397(6) 0.1870(4) 0.4203(2) 0.043(2) Uani 1 d . . O2 O 0.0535(5) 0.1229(3) 0.4384(2) 0.0632(15) Uani 1 d . . C3 C 0.1902(4) 0.2714(5) 0.4034(3) 0.043(2) Uani 0.920(2) d PD 1 O3 O 0.2832(5) 0.2575(12) 0.4076(6) 0.068(3) Uani 0.920(2) d PD 1 C3A C -0.0576(59) 0.2082(28) 0.3618(6) 0.043 Uiso 0.080(2) d PD 2 O3A O -0.1058(98) 0.1640(62) 0.3394(5) 0.067 Uiso 0.080(2) d PD 2 N11 N 0.0928(4) 0.4253(3) 0.4113(2) 0.0345(11) Uani 1 d . . N12 N 0.0711(5) 0.4896(3) 0.3815(2) 0.0385(12) Uani 1 d . . C11 C 0.1194(6) 0.5592(4) 0.3967(2) 0.048(2) Uani 1 d . . H11 H 0.1166(6) 0.6111(4) 0.3825(2) 0.028(16) Uiso 1 calc R . C12 C 0.1742(6) 0.5425(4) 0.4370(3) 0.050(2) Uani 1 d . . H12 H 0.2148(6) 0.5800(4) 0.4549(3) 0.092(30) Uiso 1 calc R . C13 C 0.1564(6) 0.4582(4) 0.4453(2) 0.040(2) Uani 1 d . . C14 C 0.1979(6) 0.4102(4) 0.4856(2) 0.049(2) Uani 1 d . . H14 H 0.1742(6) 0.3517(4) 0.4823(2) 0.035(17) Uiso 1 calc R . C15 C 0.3287(7) 0.4131(7) 0.4881(4) 0.078(3) Uani 1 d . . H15A H 0.3539(8) 0.3835(32) 0.5146(12) 0.205(67) Uiso 1 calc R . H15B H 0.3534(7) 0.4703(7) 0.4898(20) 0.074(27) Uiso 1 calc R . H15C H 0.3601(7) 0.3873(33) 0.4615(10) 0.101(38) Uiso 1 calc R . C16 C 0.1464(10) 0.4450(6) 0.5292(3) 0.076(3) Uani 1 d . . H16A H 0.1699(39) 0.5021(13) 0.5332(10) 0.097(34) Uiso 1 calc R . H16B H 0.1719(38) 0.4123(23) 0.5546(3) 0.132(43) Uiso 1 calc R . H16C H 0.0651(10) 0.4425(31) 0.5274(8) 0.066(29) Uiso 1 calc R . N21 N 0.0895(5) 0.3344(4) 0.3234(2) 0.0424(13) Uani 1 d . . N22 N 0.0602(5) 0.4132(4) 0.3078(2) 0.0436(14) Uani 1 d . . C21 C 0.1015(7) 0.4223(5) 0.2657(2) 0.061(2) Uani 1 d . . H21 H 0.0936(7) 0.4697(5) 0.2477(2) 0.051(20) Uiso 1 calc R . C22 C 0.1569(8) 0.3511(6) 0.2537(3) 0.068(2) Uani 1 d . . H22 H 0.1934(8) 0.3407(6) 0.2262(3) 0.046(19) Uiso 1 calc R . C23 C 0.1483(6) 0.2963(5) 0.2907(2) 0.051(2) Uani 1 d . . C24 C 0.2011(8) 0.2122(5) 0.2945(3) 0.064(2) Uani 1 d . . H24 H 0.1765(8) 0.1873(5) 0.3232(3) 0.053(21) Uiso 1 calc R . C25 C 0.1606(11) 0.1549(7) 0.2558(3) 0.090(3) Uani 1 d . . H25A H 0.0795(12) 0.1497(26) 0.2570(11) 0.128(49) Uiso 1 calc R . H25B H 0.1947(35) 0.1007(11) 0.2590(10) 0.068(27) Uiso 1 calc R . H25C H 0.1823(39) 0.1787(17) 0.2272(3) 0.056(23) Uiso 1 calc R . C26 C 0.3293(8) 0.2185(7) 0.2953(4) 0.091(3) Uani 1 d . . H26A H 0.3616(8) 0.1634(7) 0.2952(19) 0.101(36) Uiso 1 calc R . H26B H 0.3528(9) 0.2478(32) 0.3221(10) 0.173(60) Uiso 1 calc R . H26C H 0.3549(9) 0.2485(31) 0.2690(11) 0.057(22) Uiso 1 calc R . N31 N -0.1296(4) 0.3717(3) 0.3759(2) 0.0367(12) Uani 1 d . . N32 N -0.1167(5) 0.4443(3) 0.3517(2) 0.0428(14) Uani 1 d . . C31 C -0.2173(6) 0.4809(5) 0.3462(3) 0.053(2) Uani 1 d . . H31 H -0.2303(6) 0.5309(5) 0.3308(3) 0.054(21) Uiso 1 calc R . C32 C -0.2981(6) 0.4334(5) 0.3667(3) 0.051(2) Uani 1 d . . H32 H -0.3754(6) 0.4447(5) 0.3683(3) 0.071(25) Uiso 1 calc R . C33 C -0.2420(6) 0.3641(4) 0.3849(2) 0.040(2) Uani 1 d . . C34 C -0.2955(6) 0.2939(5) 0.4108(2) 0.050(2) Uani 1 d . . H34 H -0.2368(6) 0.2521(5) 0.4173(2) 0.046(19) Uiso 1 calc R . C35 C -0.3432(9) 0.3262(7) 0.4565(3) 0.074(3) Uani 1 d . . H35A H -0.2842(17) 0.3544(38) 0.4729(11) 0.213(76) Uiso 1 calc R . H35B H -0.3706(53) 0.2798(7) 0.4740(10) 0.158(54) Uiso 1 calc R . H35C H -0.4045(38) 0.3645(32) 0.4508(3) 0.069(25) Uiso 1 calc R . C36 C -0.3880(7) 0.2521(6) 0.3829(3) 0.073(3) Uani 1 d . . H36A H -0.4181(30) 0.2053(20) 0.3994(8) 0.082(29) Uiso 1 calc R . H36B H -0.3567(12) 0.2330(28) 0.3547(8) 0.060(25) Uiso 1 calc R . H36C H -0.4476(21) 0.2916(11) 0.3770(15) 0.077(29) Uiso 1 calc R . B B 0.0001(7) 0.4767(5) 0.3382(3) 0.046(2) Uani 1 d . . H(B) H -0.0133(58) 0.5323(44) 0.3195(23) 0.058(21) Uiso 1 d . . O4 O -0.1246(14) 0.4631(10) 0.1689(6) 0.249(7) Uiso 1 d . . C4 C -0.0968(18) 0.4503(12) 0.1284(7) 0.194(8) Uiso 1 d . . 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C2 W C3 70.6(3) . . ? C2 W C1 71.5(3) . . ? C3 W C1 102.4(3) . . ? C2 W C3A 64.0(14) . . ? C1 W C3A 106.1(12) . . ? C2 W N11 134.7(2) . . ? C3 W N11 80.4(3) . . ? C1 W N11 82.1(2) . . ? C3A W N11 161.1(16) . . ? C2 W N31 128.3(2) . . ? C3 W N31 160.8(3) . . ? C1 W N31 83.7(2) . . ? C3A W N31 81.6(23) . . ? N11 W N31 82.5(2) . . ? C2 W N21 125.3(2) . . ? C3 W N21 83.4(3) . . ? C1 W N21 163.0(2) . . ? C3A W N21 85.6(8) . . ? N11 W N21 83.2(2) . . ? N31 W N21 86.0(2) . . ? C2 W I 69.1(2) . . ? C3 W I 113.6(2) . . ? C1 W I 111.6(2) . . ? N11 W I 156.14(13) . . ? N31 W I 79.94(14) . . ? N21 W I 79.61(14) . . ? C2 W IA 73.0(5) . . ? C1 W IA 103.3(6) . . ? C3A W IA 115.0(24) . . ? N11 W IA 78.4(6) . . ? N31 W IA 158.5(5) . . ? N21 W IA 82.0(5) . . ? O1 C1 W 178.1(6) . . ? O2 C2 W 174.7(6) . . ? O3 C3 W 177.2(10) . . ? O3A C3A W 170.9(44) . . ? C13 N11 N12 106.6(5) . . ? C13 N11 W 136.0(4) . . ? N12 N11 W 117.3(4) . . ? C11 N12 N11 109.2(5) . . ? C11 N12 B 128.7(6) . . ? N11 N12 B 122.1(5) . . ? N12 C11 C12 109.3(6) . . ? N12 C11 H11 125.4(4) . . ? C12 C11 H11 125.4(4) . . ? C11 C12 C13 105.7(7) . . ? C11 C12 H12 127.2(4) . . ? C13 C12 H12 127.2(4) . . ? N11 C13 C12 109.3(6) . . ? N11 C13 C14 124.6(6) . . ? C12 C13 C14 126.1(7) . . ? C13 C14 C16 110.6(7) . . ? C13 C14 C15 110.4(7) . . ? C16 C14 C15 110.2(7) . . ? C13 C14 H14 108.5(4) . . ? C16 C14 H14 108.5(5) . . ? C15 C14 H14 108.5(5) . . ? C14 C15 H15A 109.5(5) . . ? C14 C15 H15B 109.5(5) . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5(5) . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5(5) . . ? C14 C16 H16B 109.5(5) . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5(5) . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C23 N21 N22 107.6(5) . . ? C23 N21 W 135.4(5) . . ? N22 N21 W 116.9(4) . . ? C21 N22 N21 108.5(6) . . ? C21 N22 B 129.7(6) . . ? N21 N22 B 121.6(5) . . ? N22 C21 C22 109.0(7) . . ? N22 C21 H21 125.5(5) . . ? C22 C21 H21 125.5(4) . . ? C21 C22 C23 106.5(7) . . ? C21 C22 H22 126.7(4) . . ? C23 C22 H22 126.7(5) . . ? N21 C23 C22 108.4(7) . . ? N21 C23 C24 125.2(6) . . ? C22 C23 C24 126.3(7) . . ? C23 C24 C26 111.0(8) . . ? C23 C24 C25 110.7(8) . . ? C26 C24 C25 111.2(8) . . ? C23 C24 H24 107.9(4) . . ? C26 C24 H24 107.9(5) . . ? C25 C24 H24 107.9(5) . . ? C24 C25 H25A 109.5(6) . . ? C24 C25 H25B 109.5(5) . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5(5) . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5(6) . . ? C24 C26 H26B 109.5(5) . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5(5) . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C33 N31 N32 106.6(5) . . ? C33 N31 W 135.8(4) . . ? N32 N31 W 117.6(4) . . ? C31 N32 N31 109.6(6) . . ? C31 N32 B 128.6(6) . . ? N31 N32 B 121.7(5) . . ? N32 C31 C32 108.9(7) . . ? N32 C31 H31 125.6(4) . . ? C32 C31 H31 125.6(4) . . ? C31 C32 C33 106.4(7) . . ? C31 C32 H32 126.8(4) . . ? C33 C32 H32 126.8(4) . . ? N31 C33 C32 108.4(6) . . ? N31 C33 C34 125.3(6) . . ? C32 C33 C34 126.2(7) . . ? C33 C34 C36 110.8(6) . . ? C33 C34 C35 110.3(7) . . ? C36 C34 C35 110.9(7) . . ? C33 C34 H34 108.2(4) . . ? C36 C34 H34 108.2(5) . . ? C35 C34 H34 108.2(5) . . ? C34 C35 H35A 109.5(5) . . ? C34 C35 H35B 109.5(5) . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5(5) . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5(5) . . ? C34 C36 H36B 109.5(5) . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5(5) . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N32 B N22 110.3(6) . . ? N32 B N12 108.6(6) . . ? N22 B N12 108.9(6) . . ? N32 B H(B) 106.7(38) . . ? N22 B H(B) 108.7(38) . . ? N12 B H(B) 113.6(38) . . ? 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 W C2 1.965(7) . ? W C3 1.985(4) . ? W C1 1.985(7) . ? W C3A 1.993(5) . ? W N11 2.224(5) . ? W N31 2.248(5) . ? W N21 2.250(5) . ? W I 2.8494(7) . ? W IA 2.857(5) . ? C1 O1 1.116(8) . ? C2 O2 1.167(8) . ? C3 O3 1.124(4) . ? C3A O3A 1.120(5) . ? N11 C13 1.357(8) . ? N11 N12 1.375(7) . ? N12 C11 1.328(8) . ? N12 B 1.540(10) . ? C11 C12 1.377(10) . ? C11 H11 0.93 . ? C12 C13 1.384(9) . ? C12 H12 0.93 . ? C13 C14 1.496(9) . ? C14 C16 1.527(10) . ? C14 C15 1.543(10) . ? C14 H14 0.98 . ? C15 H15A 0.96 . ? C15 H15B 0.96 . ? C15 H15C 0.96 . ? C16 H16A 0.96 . ? C16 H16B 0.96 . ? C16 H16C 0.96 . ? N21 C23 1.335(9) . ? N21 N22 1.384(7) . ? N22 C21 1.340(8) . ? N22 B 1.529(10) . ? C21 C22 1.359(11) . ? C21 H21 0.93 . ? C22 C23 1.403(10) . ? C22 H22 0.93 . ? C23 C24 1.484(10) . ? C24 C26 1.514(13) . ? C24 C25 1.538(12) . ? C24 H24 0.98 . ? C25 H25A 0.96 . ? C25 H25B 0.96 . ? C25 H25C 0.96 . ? C26 H26A 0.96 . ? C26 H26B 0.96 . ? C26 H26C 0.96 . ? N31 C33 1.355(8) . ? N31 N32 1.370(7) . ? N32 C31 1.332(9) . ? N32 B 1.522(10) . ? C31 C32 1.359(10) . ? C31 H31 0.93 . ? C32 C33 1.395(9) . ? C32 H32 0.93 . ? C33 C34 1.497(9) . ? C34 C36 1.519(10) . ? C34 C35 1.547(11) . ? C34 H34 0.98 . ? C35 H35A 0.96 . ? C35 H35B 0.96 . ? C35 H35C 0.96 . ? C36 H36A 0.96 . ? C36 H36B 0.96 . ? C36 H36C 0.96 . ? B H(B) 1.06(7) . ? O4 C4 1.25(2) . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 W C1 O1 -155.1(183) . . . . ? C3 W C1 O1 140.5(182) . . . . ? C3A W C1 O1 -100.4(184) . . . . ? N11 W C1 O1 62.2(183) . . . . ? N31 W C1 O1 -21.1(183) . . . . ? N21 W C1 O1 31.9(187) . . . . ? I W C1 O1 -97.6(183) . . . . ? IA W C1 O1 138.2(182) . . . . ? C3 W C2 O2 37.5(69) . . . . ? C1 W C2 O2 -73.6(69) . . . . ? C3A W C2 O2 167.1(74) . . . . ? N11 W C2 O2 -15.9(71) . . . . ? N31 W C2 O2 -139.2(69) . . . . ? N21 W C2 O2 103.9(69) . . . . ? I W C2 O2 163.5(70) . . . . ? IA W C2 O2 37.3(69) . . . . ? C2 W C3 O3 146.5(216) . . . . ? C1 W C3 O3 -148.5(216) . . . . ? C3A W C3 O3 97.6(216) . . . . ? N11 W C3 O3 -68.9(216) . . . . ? N31 W C3 O3 -41.6(218) . . . . ? N21 W C3 O3 15.3(216) . . . . ? I W C3 O3 90.9(216) . . . . ? IA W C3 O3 -37.4(326) . . . . ? C2 W C3A O3A -161.3(642) . . . . ? C3 W C3A O3A -109.1(635) . . . . ? C1 W C3A O3A 139.3(631) . . . . ? N11 W C3A O3A 25.4(674) . . . . ? N31 W C3A O3A 58.4(635) . . . . ? N21 W C3A O3A -28.2(634) . . . . ? I W C3A O3A -15.2(502) . . . . ? IA W C3A O3A -107.2(635) . . . . ? C2 W N11 C13 0.0(8) . . . . ? C3 W N11 C13 -50.2(6) . . . . ? C1 W N11 C13 53.9(6) . . . . ? C3A W N11 C13 171.4(56) . . . . ? N31 W N11 C13 138.6(6) . . . . ? N21 W N11 C13 -134.6(6) . . . . ? I W N11 C13 -178.7(4) . . . . ? IA W N11 C13 -51.4(8) . . . . ? C2 W N11 N12 176.5(4) . . . . ? C3 W N11 N12 126.3(5) . . . . ? C1 W N11 N12 -129.5(5) . . . . ? C3A W N11 N12 -12.0(57) . . . . ? N31 W N11 N12 -44.9(4) . . . . ? N21 W N11 N12 41.9(4) . . . . ? I W N11 N12 -2.2(7) . . . . ? IA W N11 N12 125.1(7) . . . . ? C13 N11 N12 C11 -0.1(7) . . . . ? W N11 N12 C11 -177.6(4) . . . . ? C13 N11 N12 B -179.7(6) . . . . ? W N11 N12 B 2.8(8) . . . . ? N11 N12 C11 C12 0.1(8) . . . . ? B N12 C11 C12 179.6(7) . . . . ? N12 C11 C12 C13 0.0(8) . . . . ? N12 N11 C13 C12 0.1(7) . . . . ? W N11 C13 C12 176.9(5) . . . . ? N12 N11 C13 C14 179.0(6) . . . . ? W N11 C13 C14 -4.2(10) . . . . ? C11 C12 C13 N11 -0.1(8) . . . . ? C11 C12 C13 C14 -179.0(7) . . . . ? N11 C13 C14 C16 -116.5(8) . . . . ? C12 C13 C14 C16 62.2(10) . . . . ? N11 C13 C14 C15 121.2(8) . . . . ? C12 C13 C14 C15 -60.1(10) . . . . ? C2 W N21 C23 -6.5(8) . . . . ? C3 W N21 C23 54.1(7) . . . . ? C1 W N21 C23 165.4(8) . . . . ? C3A W N21 C23 -60.1(24) . . . . ? N11 W N21 C23 135.2(7) . . . . ? N31 W N21 C23 -141.9(7) . . . . ? I W N21 C23 -61.5(7) . . . . ? IA W N21 C23 56.0(9) . . . . ? C2 W N21 N22 171.5(4) . . . . ? C3 W N21 N22 -128.0(5) . . . . ? C1 W N21 N22 -16.6(11) . . . . ? C3A W N21 N22 117.9(23) . . . . ? N11 W N21 N22 -46.9(4) . . . . ? N31 W N21 N22 36.0(4) . . . . ? I W N21 N22 116.5(4) . . . . ? IA W N21 N22 -126.0(7) . . . . ? C23 N21 N22 C21 -0.1(8) . . . . ? W N21 N22 C21 -178.6(5) . . . . ? C23 N21 N22 B -175.0(6) . . . . ? W N21 N22 B 6.5(8) . . . . ? N21 N22 C21 C22 0.1(9) . . . . ? B N22 C21 C22 174.5(7) . . . . ? N22 C21 C22 C23 -0.1(10) . . . . ? N22 N21 C23 C22 0.0(9) . . . . ? W N21 C23 C22 178.1(6) . . . . ? N22 N21 C23 C24 176.6(7) . . . . ? W N21 C23 C24 -5.3(12) . . . . ? C21 C22 C23 N21 0.1(10) . . . . ? C21 C22 C23 C24 -176.5(8) . . . . ? N21 C23 C24 C26 -110.7(9) . . . . ? C22 C23 C24 C26 65.3(11) . . . . ? N21 C23 C24 C25 125.4(9) . . . . ? C22 C23 C24 C25 -58.6(12) . . . . ? C2 W N31 C33 11.2(7) . . . . ? C3 W N31 C33 -159.1(8) . . . . ? C1 W N31 C33 -49.2(6) . . . . ? C3A W N31 C33 58.2(11) . . . . ? N11 W N31 C33 -132.0(6) . . . . ? N21 W N31 C33 144.3(6) . . . . ? I W N31 C33 64.2(6) . . . . ? IA W N31 C33 -159.6(16) . . . . ? C2 W N31 N32 -171.8(4) . . . . ? C3 W N31 N32 17.9(10) . . . . ? C1 W N31 N32 127.9(5) . . . . ? C3A W N31 N32 -124.7(10) . . . . ? N11 W N31 N32 45.0(4) . . . . ? N21 W N31 N32 -38.6(4) . . . . ? I W N31 N32 -118.7(4) . . . . ? IA W N31 N32 17.5(17) . . . . ? C33 N31 N32 C31 0.4(7) . . . . ? W N31 N32 C31 -177.4(5) . . . . ? C33 N31 N32 B 175.9(6) . . . . ? W N31 N32 B -2.0(8) . . . . ? N31 N32 C31 C32 0.2(8) . . . . ? B N32 C31 C32 -174.8(7) . . . . ? N32 C31 C32 C33 -0.8(8) . . . . ? N32 N31 C33 C32 -0.9(7) . . . . ? W N31 C33 C32 176.4(5) . . . . ? N32 N31 C33 C34 -179.8(6) . . . . ? W N31 C33 C34 -2.6(10) . . . . ? C31 C32 C33 N31 1.1(8) . . . . ? C31 C32 C33 C34 180.0(7) . . . . ? N31 C33 C34 C36 -124.1(8) . . . . ? C32 C33 C34 C36 57.1(10) . . . . ? N31 C33 C34 C35 112.7(8) . . . . ? C32 C33 C34 C35 -66.1(9) . . . . ? C31 N32 B N22 -124.6(7) . . . . ? N31 N32 B N22 61.0(8) . . . . ? C31 N32 B N12 116.2(8) . . . . ? N31 N32 B N12 -58.3(8) . . . . ? C21 N22 B N32 122.4(8) . . . . ? N21 N22 B N32 -63.8(8) . . . . ? C21 N22 B N12 -118.6(8) . . . . ? N21 N22 B N12 55.2(8) . . . . ? C11 N12 B N32 -121.2(7) . . . . ? N11 N12 B N32 58.3(8) . . . . ? C11 N12 B N22 118.7(7) . . . . ? N11 N12 B N22 -61.8(8) . . . . ? _journal_paper_doi 10.1021/ic970838w