data_bns _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H18 B N S' _chemical_formula_sum 'C10 H18 B N S' _chemical_formula_weight 195.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 26.1590(18) _cell_length_b 8.5982(2) _cell_length_c 20.5101(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4613.1(3) _cell_formula_units_Z 16 _cell_measurement_temperature 85(2) _cell_measurement_reflns_used 23413 _cell_measurement_theta_min 2.7 _cell_measurement_theta_max 68.3 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.124 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1696 _exptl_absorpt_coefficient_mu 2.114 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.7021 _exptl_absorpt_correction_T_max 0.9017 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 85(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'micro-focus rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'AFC10: Kappa 3 circle, Saturn 744+ CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 55448 _diffrn_reflns_av_R_equivalents 0.0896 _diffrn_reflns_av_sigmaI/netI 0.0596 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.38 _diffrn_reflns_theta_max 68.21 _reflns_number_total 8412 _reflns_number_gt 7168 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The aromatic six-member ring is disordered by a 180 degree rotation about the B-N bond. This results in a superposition of sulphur and carbon at sites bonded to the boron. For each of the 4 independent molecules in the asymmetric unit, a free variable was assigned to refine the relative sulphur/carbon ratio for a given site. Relative occupancies: S1/C1 0.804(4)/0.196(4) S2/C11 0.927(4)/0.072(4) S3/C21 0.953(4)/0.047(4) S4/C31 0.806(4)/0.194(4) 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^)+(0.0540P)^2^+2.0904P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.093(17) _refine_ls_number_reflns 8412 _refine_ls_number_parameters 489 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0608 _refine_ls_R_factor_gt 0.0502 _refine_ls_wR_factor_ref 0.1278 _refine_ls_wR_factor_gt 0.1194 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _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 S1 S 0.73364(3) -0.05557(11) 0.44049(5) 0.0319(3) Uani 0.804(4) 1 d P A 1 S1A S 0.75882(10) 0.1497(3) 0.55145(13) 0.0478(9) Uani 0.196(4) 1 d P A 2 S2 S 0.76902(3) 0.34864(9) 0.23403(5) 0.0333(3) Uani 0.928(4) 1 d P B 1 S2A S 0.77148(11) 0.6291(3) 0.31267(15) 0.0379(10) Uani 0.072(4) 1 d P B 2 S3 S 0.52412(3) -0.11109(9) 0.56289(4) 0.0343(3) Uani 0.953(4) 1 d P C 1 S3A S 0.51974(11) 0.1681(4) 0.48427(17) 0.0379(11) Uani 0.047(4) 1 d P C 2 S4 S 1.01733(4) 0.52780(11) 0.85331(5) 0.0366(3) Uani 0.806(4) 1 d P D 1 S4A S 0.99814(11) 0.3070(3) 0.74765(13) 0.0538(10) Uani 0.194(4) 1 d P D 2 C1 C 0.75882(10) 0.1497(3) 0.55145(13) 0.0478(9) Uani 0.804(4) 1 d P A 1 H1A H 0.7814 0.2055 0.5793 0.057 Uiso 0.804(4) 1 calc PR A 1 C1A C 0.73364(3) -0.05557(11) 0.44049(5) 0.0319(3) Uani 0.196(4) 1 d P A 2 H1B H 0.7397 -0.1217 0.4042 0.038 Uiso 0.196(4) 1 calc PR A 2 C2 C 0.70759(15) 0.1587(4) 0.56021(19) 0.0417(8) Uani 1 1 d . . . H2 H 0.6966 0.2204 0.5960 0.050 Uiso 1 1 calc R A 1 C3 C 0.66878(14) 0.0896(4) 0.5238(2) 0.0455(9) Uani 1 1 d . A . H3A H 0.6345 0.1083 0.5369 0.055 Uiso 1 1 calc R . . C4 C 0.67635(16) -0.0012(4) 0.4717(2) 0.0485(11) Uani 1 1 d . . . H4 H 0.6467 -0.0389 0.4501 0.058 Uiso 1 1 calc R A 1 C5 C 0.85069(13) -0.0888(4) 0.42575(17) 0.0347(8) Uani 1 1 d . . . H5A H 0.8192 -0.1297 0.4042 0.042 Uiso 1 1 calc R . . C6 C 0.88094(14) -0.0036(5) 0.37359(19) 0.0420(9) Uani 1 1 d . . . H6A H 0.8610 0.0849 0.3575 0.063 Uiso 1 1 calc R . . H6B H 0.8882 -0.0747 0.3374 0.063 Uiso 1 1 calc R . . H6C H 0.9132 0.0340 0.3922 0.063 Uiso 1 1 calc R . . C7 C 0.87936(13) -0.2285(4) 0.4523(2) 0.0427(9) Uani 1 1 d . . . H7A H 0.9114 -0.1939 0.4723 0.064 Uiso 1 1 calc R . . H7B H 0.8869 -0.3008 0.4166 0.064 Uiso 1 1 calc R . . H7C H 0.8583 -0.2810 0.4851 0.064 Uiso 1 1 calc R . . C8 C 0.87591(12) 0.0887(4) 0.51541(17) 0.0356(8) Uani 1 1 d . . . H8A H 0.9079 0.0500 0.4943 0.043 Uiso 1 1 calc R . . C9 C 0.87709(14) 0.2654(4) 0.5085(2) 0.0447(9) Uani 1 1 d . . . H9A H 0.8771 0.2932 0.4622 0.067 Uiso 1 1 calc R . . H9B H 0.9080 0.3062 0.5293 0.067 Uiso 1 1 calc R . . H9C H 0.8469 0.3101 0.5297 0.067 Uiso 1 1 calc R . . C10 C 0.87852(15) 0.0355(5) 0.58619(18) 0.0453(9) Uani 1 1 d . . . H10A H 0.8486 0.0744 0.6098 0.068 Uiso 1 1 calc R . . H10B H 0.9097 0.0763 0.6064 0.068 Uiso 1 1 calc R . . H10C H 0.8790 -0.0784 0.5878 0.068 Uiso 1 1 calc R . . C11 C 0.77148(11) 0.6291(3) 0.31267(15) 0.0379(10) Uani 0.928(4) 1 d P B 1 H11A H 0.7728 0.7386 0.3186 0.046 Uiso 0.928(4) 1 calc PR B 1 C11A C 0.76902(3) 0.34864(9) 0.23403(5) 0.0333(3) Uani 0.072(4) 1 d P B 2 H11B H 0.7690 0.2887 0.1951 0.040 Uiso 0.072(4) 1 calc PR B 2 C12 C 0.77301(13) 0.5350(4) 0.36594(19) 0.0350(8) Uani 1 1 d . . . H12 H 0.7752 0.5853 0.4071 0.042 Uiso 1 1 calc R B 1 C13 C 0.77174(13) 0.3690(4) 0.36691(19) 0.0378(8) Uani 1 1 d . B . H13A H 0.7719 0.3177 0.4079 0.045 Uiso 1 1 calc R . . C14 C 0.77038(13) 0.2825(4) 0.31263(19) 0.0384(9) Uani 1 1 d . . . H14 H 0.7701 0.1728 0.3184 0.046 Uiso 1 1 calc R B 1 C15 C 0.76327(11) 0.8231(3) 0.18235(18) 0.0298(7) Uani 1 1 d . . . H15A H 0.7599 0.8523 0.1354 0.036 Uiso 1 1 calc R . . C16 C 0.71807(13) 0.8952(4) 0.21648(18) 0.0382(8) Uani 1 1 d . . . H16A H 0.6864 0.8487 0.1999 0.057 Uiso 1 1 calc R . . H16B H 0.7177 1.0075 0.2082 0.057 Uiso 1 1 calc R . . H16C H 0.7207 0.8765 0.2635 0.057 Uiso 1 1 calc R . . C17 C 0.81397(14) 0.8917(4) 0.2050(2) 0.0430(9) Uani 1 1 d . . . H17A H 0.8199 0.8636 0.2507 0.065 Uiso 1 1 calc R . . H17B H 0.8128 1.0052 0.2009 0.065 Uiso 1 1 calc R . . H17C H 0.8418 0.8505 0.1781 0.065 Uiso 1 1 calc R . . C18 C 0.75814(15) 0.5777(4) 0.11920(17) 0.0394(9) Uani 1 1 d . . . H18A H 0.7569 0.4628 0.1267 0.047 Uiso 1 1 calc R . . C19 C 0.70891(15) 0.6204(4) 0.08457(17) 0.0423(9) Uani 1 1 d . . . H19A H 0.6799 0.6012 0.1136 0.063 Uiso 1 1 calc R . . H19B H 0.7053 0.5569 0.0452 0.063 Uiso 1 1 calc R . . H19C H 0.7098 0.7307 0.0725 0.063 Uiso 1 1 calc R . . C20 C 0.80426(17) 0.6080(6) 0.0766(2) 0.0645(13) Uani 1 1 d . . . H20A H 0.8070 0.7197 0.0677 0.097 Uiso 1 1 calc R . . H20B H 0.8005 0.5515 0.0354 0.097 Uiso 1 1 calc R . . H20C H 0.8352 0.5725 0.0990 0.097 Uiso 1 1 calc R . . C21 C 0.51974(11) 0.1681(4) 0.48427(17) 0.0379(11) Uani 0.953(4) 1 d P C 1 H21A H 0.5187 0.2777 0.4786 0.046 Uiso 0.953(4) 1 calc PR C 1 C21A C 0.52412(3) -0.11109(9) 0.56289(4) 0.0343(3) Uani 0.047(4) 1 d P C 2 H21B H 0.5259 -0.1713 0.6017 0.041 Uiso 0.047(4) 1 calc PR C 2 C22 C 0.52157(12) 0.0773(4) 0.43049(19) 0.0351(8) Uani 1 1 d . . . H22 H 0.5216 0.1281 0.3894 0.042 Uiso 1 1 calc R C 1 C23 C 0.52349(13) -0.0875(4) 0.43045(19) 0.0379(8) Uani 1 1 d . C . H23A H 0.5239 -0.1388 0.3894 0.045 Uiso 1 1 calc R . . C24 C 0.52475(13) -0.1756(4) 0.48378(18) 0.0374(8) Uani 1 1 d . . . H24 H 0.5261 -0.2849 0.4774 0.045 Uiso 1 1 calc R C 1 C25 C 0.51413(16) 0.1143(4) 0.67817(18) 0.0443(10) Uani 1 1 d . . . H25A H 0.5110 -0.0001 0.6704 0.053 Uiso 1 1 calc R . . C26 C 0.46793(17) 0.1616(4) 0.71805(19) 0.0522(11) Uani 1 1 d . . . H26A H 0.4702 0.2725 0.7287 0.078 Uiso 1 1 calc R . . H26B H 0.4670 0.1007 0.7584 0.078 Uiso 1 1 calc R . . H26C H 0.4367 0.1422 0.6928 0.078 Uiso 1 1 calc R . . C27 C 0.56391(18) 0.1388(5) 0.7148(2) 0.0643(13) Uani 1 1 d . . . H27A H 0.5926 0.1047 0.6875 0.097 Uiso 1 1 calc R . . H27B H 0.5634 0.0780 0.7552 0.097 Uiso 1 1 calc R . . H27C H 0.5679 0.2493 0.7252 0.097 Uiso 1 1 calc R . . C28 C 0.51639(12) 0.3610(3) 0.61586(18) 0.0299(7) Uani 1 1 d . . . H28A H 0.5148 0.3887 0.6632 0.036 Uiso 1 1 calc R . . C29 C 0.47001(13) 0.4350(4) 0.58488(19) 0.0395(8) Uani 1 1 d . . . H29A H 0.4711 0.4187 0.5376 0.059 Uiso 1 1 calc R . . H29B H 0.4699 0.5468 0.5942 0.059 Uiso 1 1 calc R . . H29C H 0.4389 0.3876 0.6027 0.059 Uiso 1 1 calc R . . C30 C 0.56595(13) 0.4288(4) 0.5906(2) 0.0428(9) Uani 1 1 d . . . H30A H 0.5948 0.3799 0.6132 0.064 Uiso 1 1 calc R . . H30B H 0.5664 0.5411 0.5987 0.064 Uiso 1 1 calc R . . H30C H 0.5687 0.4091 0.5437 0.064 Uiso 1 1 calc R . . C31 C 0.99814(11) 0.3070(3) 0.74765(13) 0.0538(10) Uani 0.806(4) 1 d P D 1 H31A H 0.9773 0.2385 0.7229 0.065 Uiso 0.806(4) 1 calc PR D 1 C31A C 1.01733(4) 0.52780(11) 0.85331(5) 0.0366(3) Uani 0.194(4) 1 d P D 2 H31B H 1.0098 0.5902 0.8903 0.044 Uiso 0.194(4) 1 calc PR D 2 C32 C 1.04822(14) 0.3126(4) 0.7357(2) 0.0438(9) Uani 1 1 d . . . H32 H 1.0605 0.2482 0.7015 0.053 Uiso 1 1 calc R D 1 C33 C 1.08476(14) 0.4033(4) 0.76836(19) 0.0412(9) Uani 1 1 d . D . H33A H 1.1190 0.3976 0.7531 0.049 Uiso 1 1 calc R . . C34 C 1.07567(15) 0.4966(4) 0.8187(2) 0.0430(10) Uani 1 1 d . . . H34 H 1.1040 0.5503 0.8369 0.052 Uiso 1 1 calc R D 1 C35 C 0.90077(16) 0.5323(6) 0.8688(2) 0.0685(15) Uani 1 1 d . . . H35A H 0.9318 0.5751 0.8910 0.082 Uiso 1 1 calc R . . C36 C 0.87121(17) 0.4443(7) 0.9196(2) 0.0750(16) Uani 1 1 d . . . H36A H 0.8404 0.3996 0.8998 0.112 Uiso 1 1 calc R . . H36B H 0.8613 0.5153 0.9548 0.112 Uiso 1 1 calc R . . H36C H 0.8925 0.3607 0.9373 0.112 Uiso 1 1 calc R . . C37 C 0.87213(16) 0.6696(5) 0.8412(3) 0.0726(16) Uani 1 1 d . . . H37A H 0.8940 0.7247 0.8100 0.109 Uiso 1 1 calc R . . H37B H 0.8626 0.7402 0.8767 0.109 Uiso 1 1 calc R . . H37C H 0.8412 0.6331 0.8191 0.109 Uiso 1 1 calc R . . C38 C 0.87882(15) 0.3475(4) 0.78063(19) 0.0429(9) Uani 1 1 d . . . H38A H 0.8462 0.3854 0.8004 0.051 Uiso 1 1 calc R . . C39 C 0.87902(15) 0.1723(4) 0.7910(2) 0.0516(10) Uani 1 1 d . . . H39A H 0.9102 0.1280 0.7722 0.077 Uiso 1 1 calc R . . H39B H 0.8491 0.1265 0.7696 0.077 Uiso 1 1 calc R . . H39C H 0.8779 0.1497 0.8378 0.077 Uiso 1 1 calc R . . C40 C 0.87604(15) 0.3923(5) 0.70916(18) 0.0517(10) Uani 1 1 d . . . H40A H 0.8742 0.5058 0.7053 0.078 Uiso 1 1 calc R . . H40B H 0.8455 0.3457 0.6895 0.078 Uiso 1 1 calc R . . H40C H 0.9066 0.3544 0.6866 0.078 Uiso 1 1 calc R . . N1 N 0.83334(10) 0.0171(3) 0.47919(14) 0.0290(6) Uani 1 1 d . A . N2 N 0.76283(10) 0.6507(3) 0.18414(14) 0.0283(6) Uani 1 1 d . B . N3 N 0.51554(10) 0.1892(3) 0.61314(14) 0.0286(6) Uani 1 1 d . C . N4 N 0.91958(10) 0.4266(3) 0.81616(14) 0.0350(7) Uani 1 1 d . D . B1 B 0.78158(13) 0.0413(4) 0.49218(18) 0.0262(7) Uani 1 1 d . . . B2 B 0.76755(12) 0.5621(4) 0.2416(2) 0.0267(8) Uani 1 1 d . . . B3 B 0.51921(12) 0.1023(4) 0.5553(2) 0.0271(8) Uani 1 1 d . . . B4 B 0.97187(14) 0.4146(4) 0.80355(19) 0.0295(8) 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 S1 0.0301(5) 0.0315(5) 0.0342(6) -0.0051(4) -0.0021(4) -0.0018(4) S1A 0.0565(17) 0.0402(14) 0.0466(16) 0.0087(11) 0.0154(12) 0.0091(10) S2 0.0458(5) 0.0205(4) 0.0336(5) 0.0008(4) -0.0028(4) 0.0023(3) S2A 0.0396(17) 0.0392(17) 0.0349(19) 0.0017(13) -0.0039(13) 0.0056(12) S3 0.0501(6) 0.0212(4) 0.0317(5) -0.0018(3) -0.0009(4) 0.0027(3) S3A 0.0331(18) 0.0378(18) 0.043(2) -0.0036(14) 0.0020(13) 0.0017(12) S4 0.0362(6) 0.0344(5) 0.0393(7) -0.0054(4) -0.0062(4) 0.0020(4) S4A 0.073(2) 0.0412(14) 0.0467(17) 0.0092(11) 0.0192(13) 0.0204(12) C1 0.0565(17) 0.0402(14) 0.0466(16) 0.0087(11) 0.0154(12) 0.0091(10) C1A 0.0301(5) 0.0315(5) 0.0342(6) -0.0051(4) -0.0021(4) -0.0018(4) C2 0.060(2) 0.0260(16) 0.039(2) -0.0040(16) 0.0013(19) 0.0002(15) C3 0.035(2) 0.043(2) 0.059(3) -0.0052(19) 0.0025(18) 0.0012(16) C4 0.042(2) 0.042(2) 0.061(3) -0.0028(19) -0.015(2) -0.0061(16) C5 0.0316(17) 0.0386(18) 0.034(2) -0.0129(15) 0.0019(15) 0.0019(14) C6 0.035(2) 0.057(2) 0.033(2) 0.0006(17) 0.0015(17) 0.0000(16) C7 0.039(2) 0.0400(19) 0.049(2) -0.0035(17) 0.0044(17) 0.0018(15) C8 0.0283(17) 0.046(2) 0.033(2) -0.0049(16) -0.0065(14) -0.0057(15) C9 0.042(2) 0.039(2) 0.053(2) -0.0069(18) -0.0077(18) -0.0023(16) C10 0.041(2) 0.061(2) 0.033(2) -0.0028(18) -0.0063(16) 0.0032(18) C11 0.0396(17) 0.0392(17) 0.0349(19) 0.0017(13) -0.0039(13) 0.0056(12) C11A 0.0458(5) 0.0205(4) 0.0336(5) 0.0008(4) -0.0028(4) 0.0023(3) C12 0.039(2) 0.0330(18) 0.033(2) 0.0018(15) -0.0060(16) -0.0013(14) C13 0.042(2) 0.0334(18) 0.038(2) 0.0131(16) -0.0072(16) -0.0009(14) C14 0.044(2) 0.0239(16) 0.048(2) 0.0069(15) -0.0059(17) 0.0027(14) C15 0.0326(18) 0.0179(14) 0.039(2) 0.0041(14) -0.0051(14) 0.0003(12) C16 0.0429(19) 0.0233(15) 0.049(2) 0.0001(15) -0.0041(17) 0.0073(14) C17 0.044(2) 0.0259(16) 0.060(3) 0.0112(16) -0.0131(18) -0.0052(15) C18 0.068(3) 0.0254(16) 0.0250(18) 0.0005(14) 0.0046(17) 0.0108(16) C19 0.061(2) 0.0356(18) 0.0297(19) -0.0012(15) -0.0060(17) -0.0081(17) C20 0.069(3) 0.078(3) 0.046(3) 0.009(2) 0.018(2) 0.037(2) C21 0.0331(18) 0.0378(18) 0.043(2) -0.0036(14) 0.0020(13) 0.0017(12) C21A 0.0501(6) 0.0212(4) 0.0317(5) -0.0018(3) -0.0009(4) 0.0027(3) C22 0.0349(19) 0.0356(18) 0.035(2) 0.0029(15) 0.0036(16) 0.0031(14) C23 0.046(2) 0.0323(18) 0.036(2) -0.0053(16) 0.0062(17) 0.0020(15) C24 0.047(2) 0.0249(16) 0.040(2) -0.0045(15) 0.0046(16) 0.0065(14) C25 0.083(3) 0.0193(15) 0.031(2) -0.0016(14) -0.0075(19) 0.0033(17) C26 0.085(3) 0.038(2) 0.034(2) -0.0041(16) 0.009(2) -0.023(2) C27 0.091(3) 0.053(3) 0.049(3) -0.011(2) -0.030(2) 0.032(2) C28 0.0345(18) 0.0181(14) 0.0372(19) -0.0049(13) 0.0018(14) -0.0010(12) C29 0.0422(19) 0.0261(16) 0.050(2) -0.0016(15) -0.0006(17) 0.0085(14) C30 0.042(2) 0.0281(16) 0.059(3) -0.0101(17) 0.0085(18) -0.0081(14) C31 0.073(2) 0.0412(14) 0.0467(17) 0.0092(11) 0.0192(13) 0.0204(12) C31A 0.0362(6) 0.0344(5) 0.0393(7) -0.0054(4) -0.0062(4) 0.0020(4) C32 0.058(2) 0.0336(17) 0.040(2) -0.0025(17) -0.0072(19) 0.0032(16) C33 0.037(2) 0.0377(18) 0.049(2) 0.0073(17) -0.0037(17) 0.0030(16) C34 0.046(2) 0.0341(18) 0.049(3) 0.0034(17) -0.0159(19) -0.0047(15) C35 0.039(2) 0.098(4) 0.068(3) -0.051(3) 0.000(2) 0.011(2) C36 0.048(3) 0.148(5) 0.028(3) -0.015(3) -0.001(2) 0.018(3) C37 0.041(2) 0.056(3) 0.121(5) -0.031(3) 0.005(3) 0.008(2) C38 0.039(2) 0.050(2) 0.039(2) 0.0023(17) -0.0067(16) -0.0075(16) C39 0.046(2) 0.043(2) 0.065(3) -0.006(2) -0.008(2) -0.0022(17) C40 0.044(2) 0.079(3) 0.032(2) 0.000(2) -0.0042(17) 0.011(2) N1 0.0305(14) 0.0327(14) 0.0238(14) -0.0008(11) 0.0016(12) 0.0003(11) N2 0.0355(15) 0.0212(12) 0.0281(15) 0.0013(11) -0.0005(12) 0.0044(10) N3 0.0381(15) 0.0184(12) 0.0295(15) 0.0001(11) -0.0009(12) -0.0011(10) N4 0.0289(15) 0.0436(16) 0.0324(17) -0.0034(13) -0.0031(13) 0.0027(12) B1 0.0283(17) 0.0216(16) 0.0287(19) 0.0075(14) -0.0024(15) 0.0007(13) B2 0.0183(16) 0.0263(17) 0.036(2) 0.0030(16) -0.0052(15) 0.0027(12) B3 0.0204(17) 0.0291(18) 0.032(2) -0.0008(16) -0.0008(15) -0.0003(13) B4 0.036(2) 0.0233(17) 0.0295(19) -0.0008(15) -0.0007(16) 0.0040(14) _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 S1 C4 1.696(4) . ? S1 B1 1.841(4) . ? S1A C2 1.354(5) . ? S1A B1 1.644(4) . ? S2 C14 1.710(4) . ? S2 B2 1.842(3) . ? S2A C12 1.360(5) . ? S2A B2 1.571(5) . ? S3 C24 1.715(4) . ? S3 B3 1.846(4) . ? S3A C22 1.353(5) . ? S3A B3 1.563(5) . ? S4 C34 1.705(4) . ? S4 B4 1.845(4) . ? S4A C32 1.333(5) . ? S4A B4 1.625(4) . ? C2 C3 1.393(5) . ? C3 C4 1.338(6) . ? C5 N1 1.495(4) . ? C5 C7 1.517(5) . ? C5 C6 1.519(5) . ? C8 N1 1.474(4) . ? C8 C10 1.524(5) . ? C8 C9 1.525(5) . ? C12 C13 1.427(5) . ? C13 C14 1.340(5) . ? C15 N2 1.482(4) . ? C15 C16 1.508(4) . ? C15 C17 1.524(4) . ? C18 N2 1.478(4) . ? C18 C20 1.512(6) . ? C18 C19 1.516(5) . ? C22 C23 1.418(5) . ? C23 C24 1.331(5) . ? C25 N3 1.482(4) . ? C25 C26 1.515(6) . ? C25 C27 1.518(5) . ? C28 N3 1.478(4) . ? C28 C29 1.511(5) . ? C28 C30 1.513(4) . ? C32 C33 1.404(5) . ? C33 C34 1.329(6) . ? C35 N4 1.495(5) . ? C35 C36 1.502(7) . ? C35 C37 1.508(7) . ? C38 N4 1.460(4) . ? C38 C40 1.517(5) . ? C38 C39 1.521(5) . ? N1 B1 1.395(4) . ? N2 B2 1.408(5) . ? N3 B3 1.405(5) . ? N4 B4 1.396(5) . ? 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 C4 S1 B1 105.06(19) . . ? C2 S1A B1 119.3(3) . . ? C14 S2 B2 104.65(18) . . ? C12 S2A B2 122.0(3) . . ? C24 S3 B3 104.04(18) . . ? C22 S3A B3 123.5(3) . . ? C34 S4 B4 105.28(18) . . ? C32 S4A B4 121.6(3) . . ? S1A C2 C3 128.7(3) . . ? C4 C3 C2 124.7(4) . . ? C3 C4 S1 126.4(3) . . ? N1 C5 C7 111.7(3) . . ? N1 C5 C6 112.4(3) . . ? C7 C5 C6 112.1(3) . . ? N1 C8 C10 112.9(3) . . ? N1 C8 C9 112.6(3) . . ? C10 C8 C9 112.7(3) . . ? S2A C12 C13 127.2(3) . . ? C14 C13 C12 123.0(3) . . ? C13 C14 S2 126.8(3) . . ? N2 C15 C16 113.2(3) . . ? N2 C15 C17 112.7(3) . . ? C16 C15 C17 112.4(3) . . ? N2 C18 C20 112.4(3) . . ? N2 C18 C19 113.0(3) . . ? C20 C18 C19 111.4(3) . . ? S3A C22 C23 125.4(3) . . ? C24 C23 C22 124.7(3) . . ? C23 C24 S3 126.4(3) . . ? N3 C25 C26 112.9(3) . . ? N3 C25 C27 111.3(3) . . ? C26 C25 C27 112.3(3) . . ? N3 C28 C29 113.2(3) . . ? N3 C28 C30 112.6(3) . . ? C29 C28 C30 112.5(3) . . ? S4A C32 C33 127.0(4) . . ? C34 C33 C32 125.7(4) . . ? C33 C34 S4 125.4(3) . . ? N4 C35 C36 111.3(4) . . ? N4 C35 C37 111.7(4) . . ? C36 C35 C37 113.5(4) . . ? N4 C38 C40 113.5(3) . . ? N4 C38 C39 112.9(3) . . ? C40 C38 C39 112.7(4) . . ? B1 N1 C8 125.1(3) . . ? B1 N1 C5 121.7(3) . . ? C8 N1 C5 113.2(3) . . ? B2 N2 C18 122.1(3) . . ? B2 N2 C15 124.1(3) . . ? C18 N2 C15 113.8(3) . . ? B3 N3 C28 124.2(3) . . ? B3 N3 C25 122.0(2) . . ? C28 N3 C25 113.6(3) . . ? B4 N4 C38 126.1(3) . . ? B4 N4 C35 120.1(3) . . ? C38 N4 C35 113.8(3) . . ? N1 B1 S1A 125.3(3) . . ? N1 B1 S1 118.9(3) . . ? S1A B1 S1 115.8(2) . . ? N2 B2 S2A 125.7(3) . . ? N2 B2 S2 118.1(3) . . ? S2A B2 S2 116.2(2) . . ? N3 B3 S3A 126.5(3) . . ? N3 B3 S3 117.5(3) . . ? S3A B3 S3 115.9(3) . . ? N4 B4 S4A 125.9(3) . . ? N4 B4 S4 119.4(3) . . ? S4A B4 S4 114.7(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 68.21 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.417 _refine_diff_density_min -0.286 _refine_diff_density_rms 0.050