Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_coden_Cambridge 222 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name G.Parkin 'Jonathan G. Melnick' _publ_contact_author_name 'Prof G Parkin ' _publ_contact_author_address ; Department of Chemistry Columbia University Havemeyer Hall MC3115, 3000 Broadway New York NY 10027 UNITED STATES OF AMERICA ; _publ_contact_author_email PARKIN@COLUMBIA.EDU _publ_section_title ; Methyl and Arylchalcogenolate Complexes of Cadmium in a Sulfur Rich Coordination Environment: Syntheses and Structural Characterization of the Tris(2-mercapto-1-t-butylimidazolyl)hydroborato Cadmium Complexes [TmBut]CdMe, and [TmBut]CdAr (E = O, S, Se, Te) and Analysis of the Bonding in Chalcogenolate Compounds ; # Attachment 'CDIS10.CIF' data_cdis10 _database_code_depnum_ccdc_archive 'CCDC 609897' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H34 B Cd I N6 S3' _chemical_formula_weight 716.83 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.7361(6) _cell_length_b 16.8058(9) _cell_length_c 16.2519(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.2860(10) _cell_angle_gamma 90.00 _cell_volume 2932.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 243(2) _cell_measurement_reflns_used 5097 _cell_measurement_theta_min 2.265 _cell_measurement_theta_max 27.815 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.624 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1424 _exptl_absorpt_coefficient_mu 2.032 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.4299 _exptl_absorpt_correction_T_max 0.5809 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 243(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19600 _diffrn_reflns_av_R_equivalents 0.0202 _diffrn_reflns_av_sigmaI/netI 0.0220 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 28.31 _reflns_number_total 6673 _reflns_number_gt 5377 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0316P)^2^+1.0453P] 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 0.00182(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6673 _refine_ls_number_parameters 303 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0385 _refine_ls_R_factor_gt 0.0270 _refine_ls_wR_factor_ref 0.0670 _refine_ls_wR_factor_gt 0.0635 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.032 _refine_ls_shift/su_mean 0.003 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 Cd Cd 0.366405(16) -0.430317(10) 0.256369(12) 0.03972(7) Uani 1 1 d . . . I I 0.556905(19) -0.325108(12) 0.268991(19) 0.07847(10) Uani 1 1 d . . . S1 S 0.25279(6) -0.46569(4) 0.38862(4) 0.04055(15) Uani 1 1 d . . . S2 S 0.18007(6) -0.41081(3) 0.15992(4) 0.03952(15) Uani 1 1 d . . . S3 S 0.44690(6) -0.56665(4) 0.21275(4) 0.03887(14) Uani 1 1 d . . . B B 0.1323(3) -0.59840(16) 0.24517(18) 0.0353(6) Uani 1 1 d . . . H1 H 0.063(2) -0.6459(13) 0.2395(13) 0.027(6) Uiso 1 1 d . . . N11 N 0.06641(17) -0.53104(11) 0.29383(12) 0.0347(4) Uani 1 1 d . . . N12 N 0.00504(18) -0.42684(11) 0.36480(12) 0.0353(4) Uani 1 1 d . . . N21 N 0.16443(18) -0.57429(11) 0.15502(12) 0.0355(4) Uani 1 1 d . . . N22 N 0.21852(18) -0.52107(11) 0.03688(12) 0.0369(4) Uani 1 1 d . . . N31 N 0.24698(18) -0.63400(11) 0.29150(12) 0.0356(4) Uani 1 1 d . . . N32 N 0.42575(19) -0.66056(11) 0.35133(13) 0.0395(5) Uani 1 1 d . . . C11 C 0.1047(2) -0.47415(13) 0.34708(14) 0.0345(5) Uani 1 1 d . . . C12 C -0.0592(2) -0.51915(15) 0.27898(16) 0.0416(6) Uani 1 1 d . . . H12A H -0.1096 -0.5506 0.2444 0.050 Uiso 1 1 calc R . . C13 C -0.0973(2) -0.45587(16) 0.32156(17) 0.0444(6) Uani 1 1 d . . . H13A H -0.1784 -0.4348 0.3222 0.053 Uiso 1 1 calc R . . C14 C 0.0028(2) -0.35376(15) 0.41852(17) 0.0430(6) Uani 1 1 d . . . C15 C -0.1289(3) -0.32037(17) 0.4191(2) 0.0577(8) Uani 1 1 d . . . H15A H -0.1849 -0.3591 0.4433 0.087 Uiso 1 1 calc R . . H15B H -0.1553 -0.3090 0.3632 0.087 Uiso 1 1 calc R . . H15C H -0.1306 -0.2718 0.4513 0.087 Uiso 1 1 calc R . . C16 C 0.0391(3) -0.3768(2) 0.50626(18) 0.0583(8) Uani 1 1 d . . . H16A H -0.0182 -0.4168 0.5265 0.087 Uiso 1 1 calc R . . H16B H 0.0354 -0.3301 0.5413 0.087 Uiso 1 1 calc R . . H16C H 0.1231 -0.3980 0.5067 0.087 Uiso 1 1 calc R . . C17 C 0.0904(3) -0.29194(17) 0.3816(2) 0.0650(9) Uani 1 1 d . . . H17A H 0.0639 -0.2796 0.3259 0.097 Uiso 1 1 calc R . . H17B H 0.1745 -0.3130 0.3807 0.097 Uiso 1 1 calc R . . H17C H 0.0885 -0.2439 0.4147 0.097 Uiso 1 1 calc R . . C21 C 0.1880(2) -0.50476(13) 0.11647(15) 0.0342(5) Uani 1 1 d . . . C22 C 0.1795(2) -0.63511(14) 0.09811(16) 0.0417(6) Uani 1 1 d . . . H22A H 0.1682 -0.6897 0.1084 0.050 Uiso 1 1 calc R . . C23 C 0.2127(2) -0.60314(15) 0.02653(16) 0.0429(6) Uani 1 1 d . . . H23A H 0.2292 -0.6311 -0.0223 0.052 Uiso 1 1 calc R . . C24 C 0.2500(2) -0.46337(16) -0.03055(15) 0.0416(6) Uani 1 1 d . . . C25 C 0.1358(3) -0.41112(19) -0.04743(19) 0.0566(7) Uani 1 1 d . . . H25A H 0.0661 -0.4444 -0.0638 0.085 Uiso 1 1 calc R . . H25B H 0.1544 -0.3738 -0.0912 0.085 Uiso 1 1 calc R . . H25C H 0.1144 -0.3820 0.0021 0.085 Uiso 1 1 calc R . . C26 C 0.2823(3) -0.50989(19) -0.10812(17) 0.0564(7) Uani 1 1 d . . . H26A H 0.2118 -0.5426 -0.1243 0.085 Uiso 1 1 calc R . . H26B H 0.3538 -0.5437 -0.0973 0.085 Uiso 1 1 calc R . . H26C H 0.3018 -0.4730 -0.1521 0.085 Uiso 1 1 calc R . . C27 C 0.3634(3) -0.41353(19) -0.0053(2) 0.0581(8) Uani 1 1 d . . . H27A H 0.4338 -0.4484 0.0048 0.087 Uiso 1 1 calc R . . H27B H 0.3445 -0.3841 0.0445 0.087 Uiso 1 1 calc R . . H27C H 0.3836 -0.3766 -0.0490 0.087 Uiso 1 1 calc R . . C31 C 0.3711(2) -0.62079(13) 0.28745(15) 0.0338(5) Uani 1 1 d . . . C32 C 0.2247(3) -0.68484(15) 0.35625(17) 0.0458(6) Uani 1 1 d . . . H32A H 0.1466 -0.7049 0.3718 0.055 Uiso 1 1 calc R . . C33 C 0.3332(3) -0.70070(16) 0.39316(18) 0.0494(7) Uani 1 1 d . . . H33A H 0.3446 -0.7334 0.4395 0.059 Uiso 1 1 calc R . . C34 C 0.5611(3) -0.65897(17) 0.37669(18) 0.0505(7) Uani 1 1 d . . . C35 C 0.5759(3) -0.7070(2) 0.4561(2) 0.0797(11) Uani 1 1 d . . . H35A H 0.5304 -0.6812 0.5000 0.120 Uiso 1 1 calc R . . H35B H 0.6634 -0.7102 0.4709 0.120 Uiso 1 1 calc R . . H35C H 0.5432 -0.7603 0.4478 0.120 Uiso 1 1 calc R . . C36 C 0.5991(3) -0.57291(19) 0.3943(2) 0.0684(9) Uani 1 1 d . . . H36A H 0.5504 -0.5525 0.4398 0.103 Uiso 1 1 calc R . . H36B H 0.5839 -0.5406 0.3458 0.103 Uiso 1 1 calc R . . H36C H 0.6869 -0.5710 0.4085 0.103 Uiso 1 1 calc R . . C37 C 0.6395(3) -0.6966(2) 0.3091(2) 0.0789(11) Uani 1 1 d . . . H37A H 0.6144 -0.7515 0.3014 0.118 Uiso 1 1 calc R . . H37B H 0.7267 -0.6945 0.3246 0.118 Uiso 1 1 calc R . . H37C H 0.6271 -0.6675 0.2581 0.118 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 Cd 0.03496(10) 0.03773(10) 0.04645(12) -0.00218(8) -0.00161(8) -0.00523(7) I 0.04130(12) 0.04370(11) 0.1503(3) -0.00303(12) -0.00940(13) -0.00988(8) S1 0.0299(3) 0.0536(4) 0.0381(3) -0.0055(3) -0.0059(3) -0.0009(3) S2 0.0467(4) 0.0309(3) 0.0409(4) -0.0021(2) -0.0056(3) 0.0027(2) S3 0.0364(3) 0.0401(3) 0.0402(3) 0.0029(3) 0.0049(3) 0.0006(2) B 0.0330(14) 0.0333(12) 0.0397(16) 0.0007(11) -0.0022(11) -0.0037(11) N11 0.0292(10) 0.0401(10) 0.0348(11) 0.0014(8) -0.0031(8) -0.0024(8) N12 0.0298(10) 0.0390(10) 0.0371(11) 0.0016(9) -0.0013(8) -0.0001(8) N21 0.0375(11) 0.0328(9) 0.0360(11) -0.0037(8) -0.0081(8) 0.0007(8) N22 0.0359(11) 0.0391(10) 0.0355(11) -0.0019(8) -0.0050(9) 0.0022(8) N31 0.0360(11) 0.0340(10) 0.0368(11) 0.0048(8) 0.0007(9) 0.0001(8) N32 0.0380(11) 0.0374(10) 0.0430(12) 0.0056(9) -0.0025(9) 0.0058(8) C11 0.0318(12) 0.0382(12) 0.0333(13) 0.0049(10) -0.0014(10) -0.0030(9) C12 0.0284(12) 0.0503(14) 0.0460(15) -0.0022(12) -0.0076(11) -0.0041(10) C13 0.0292(12) 0.0521(14) 0.0518(16) -0.0022(12) -0.0050(11) 0.0007(11) C14 0.0410(14) 0.0402(13) 0.0477(16) -0.0051(11) 0.0005(12) 0.0022(11) C15 0.0506(17) 0.0542(16) 0.068(2) -0.0091(14) 0.0035(15) 0.0119(13) C16 0.0611(19) 0.0699(19) 0.0439(17) -0.0136(14) -0.0020(14) 0.0083(15) C17 0.060(2) 0.0424(15) 0.092(3) 0.0004(15) 0.0079(17) -0.0083(14) C21 0.0314(12) 0.0329(11) 0.0382(13) -0.0019(10) -0.0070(10) 0.0012(9) C22 0.0441(14) 0.0341(12) 0.0467(16) -0.0084(11) -0.0065(12) 0.0023(10) C23 0.0445(14) 0.0441(13) 0.0401(15) -0.0127(11) -0.0037(11) 0.0046(11) C24 0.0359(13) 0.0526(14) 0.0362(14) 0.0040(11) -0.0031(11) 0.0014(11) C25 0.0544(18) 0.0696(18) 0.0458(17) 0.0141(14) -0.0083(13) 0.0136(14) C26 0.0522(17) 0.075(2) 0.0425(16) -0.0021(14) 0.0026(13) -0.0031(15) C27 0.0449(16) 0.0658(18) 0.064(2) 0.0044(15) 0.0004(14) -0.0092(14) C31 0.0380(13) 0.0296(10) 0.0336(12) -0.0013(9) -0.0004(10) 0.0029(9) C32 0.0448(15) 0.0425(13) 0.0502(16) 0.0130(12) 0.0051(12) -0.0014(11) C33 0.0522(16) 0.0452(14) 0.0507(16) 0.0184(12) 0.0023(13) 0.0059(12) C34 0.0398(15) 0.0554(16) 0.0563(18) 0.0075(13) -0.0106(13) 0.0090(12) C35 0.064(2) 0.090(2) 0.085(3) 0.035(2) -0.0275(19) 0.0077(19) C36 0.062(2) 0.067(2) 0.077(2) 0.0030(17) -0.0279(17) -0.0058(16) C37 0.0528(19) 0.094(3) 0.090(3) -0.009(2) -0.0025(18) 0.0346(19) _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 Cd S1 2.5470(7) . ? Cd S3 2.5506(6) . ? Cd S2 2.5564(7) . ? Cd I 2.7105(3) . ? S1 C11 1.730(2) . ? S2 C21 1.732(2) . ? S3 C31 1.725(2) . ? B N11 1.553(3) . ? B N21 1.560(3) . ? B N31 1.559(3) . ? N11 C11 1.352(3) . ? N11 C12 1.383(3) . ? N12 C11 1.365(3) . ? N12 C13 1.389(3) . ? N12 C14 1.507(3) . ? N21 C21 1.350(3) . ? N21 C22 1.388(3) . ? N22 C21 1.364(3) . ? N22 C23 1.391(3) . ? N22 C24 1.503(3) . ? N31 C31 1.353(3) . ? N31 C32 1.377(3) . ? N32 C31 1.365(3) . ? N32 C33 1.383(3) . ? N32 C34 1.509(3) . ? C12 C13 1.334(4) . ? C14 C15 1.522(4) . ? C14 C16 1.526(4) . ? C14 C17 1.526(4) . ? C22 C23 1.332(4) . ? C24 C26 1.525(4) . ? C24 C27 1.532(4) . ? C24 C25 1.532(4) . ? C32 C33 1.334(4) . ? C34 C37 1.524(4) . ? C34 C36 1.529(4) . ? C34 C35 1.530(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 S1 Cd S3 100.91(2) . . ? S1 Cd S2 99.83(2) . . ? S3 Cd S2 102.12(2) . . ? S1 Cd I 116.920(17) . . ? S3 Cd I 110.513(16) . . ? S2 Cd I 123.409(16) . . ? C11 S1 Cd 97.63(8) . . ? C21 S2 Cd 95.34(8) . . ? C31 S3 Cd 96.69(8) . . ? N11 B N21 113.09(19) . . ? N11 B N31 113.2(2) . . ? N21 B N31 112.0(2) . . ? C11 N11 C12 107.6(2) . . ? C11 N11 B 134.7(2) . . ? C12 N11 B 117.54(19) . . ? C11 N12 C13 107.9(2) . . ? C11 N12 C14 127.7(2) . . ? C13 N12 C14 124.4(2) . . ? C21 N21 C22 107.8(2) . . ? C21 N21 B 134.7(2) . . ? C22 N21 B 117.5(2) . . ? C21 N22 C23 107.6(2) . . ? C21 N22 C24 128.2(2) . . ? C23 N22 C24 124.2(2) . . ? C31 N31 C32 108.3(2) . . ? C31 N31 B 133.6(2) . . ? C32 N31 B 117.9(2) . . ? C31 N32 C33 107.8(2) . . ? C31 N32 C34 127.5(2) . . ? C33 N32 C34 124.6(2) . . ? N11 C11 N12 108.1(2) . . ? N11 C11 S1 125.73(18) . . ? N12 C11 S1 126.14(18) . . ? C13 C12 N11 109.0(2) . . ? C12 C13 N12 107.4(2) . . ? N12 C14 C15 108.8(2) . . ? N12 C14 C16 109.3(2) . . ? C15 C14 C16 108.7(2) . . ? N12 C14 C17 108.4(2) . . ? C15 C14 C17 109.0(2) . . ? C16 C14 C17 112.7(2) . . ? N21 C21 N22 108.21(19) . . ? N21 C21 S2 126.16(18) . . ? N22 C21 S2 125.63(18) . . ? C23 C22 N21 108.5(2) . . ? C22 C23 N22 107.9(2) . . ? N22 C24 C26 109.0(2) . . ? N22 C24 C27 109.8(2) . . ? C26 C24 C27 108.6(2) . . ? N22 C24 C25 108.5(2) . . ? C26 C24 C25 109.3(2) . . ? C27 C24 C25 111.7(2) . . ? N31 C31 N32 107.6(2) . . ? N31 C31 S3 126.11(18) . . ? N32 C31 S3 126.24(18) . . ? C33 C32 N31 108.3(2) . . ? C32 C33 N32 108.0(2) . . ? N32 C34 C37 109.3(2) . . ? N32 C34 C36 108.9(2) . . ? C37 C34 C36 112.3(3) . . ? N32 C34 C35 108.5(2) . . ? C37 C34 C35 109.5(3) . . ? C36 C34 C35 108.4(3) . . ? _diffrn_measured_fraction_theta_max 0.915 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.915 _refine_diff_density_max 1.165 _refine_diff_density_min -1.299 _refine_diff_density_rms 0.060 # Attachment 'CDOPHS10.CIF' data_cdophs10 _database_code_depnum_ccdc_archive 'CCDC 609898' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H55 B Cd N6 O S3' _chemical_formula_weight 927.35 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' Cd Cd -0.8075 1.2024 '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' S S 0.1246 0.1234 '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 22.379(3) _cell_length_b 10.8272(13) _cell_length_c 21.656(3) _cell_angle_alpha 90.00 _cell_angle_beta 118.560(3) _cell_angle_gamma 90.00 _cell_volume 4608.8(10) _cell_formula_units_Z 4 _cell_measurement_temperature 243(2) _cell_measurement_reflns_used 1242 _cell_measurement_theta_min 2.612 _cell_measurement_theta_max 17.900 _exptl_crystal_description PLATE _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.336 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1928 _exptl_absorpt_coefficient_mu 0.651 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.7809 _exptl_absorpt_correction_T_max 0.8809 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 243(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12510 _diffrn_reflns_av_R_equivalents 0.1125 _diffrn_reflns_av_sigmaI/netI 0.1887 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 23.26 _reflns_number_total 5652 _reflns_number_gt 2642 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0133P)^2^+0.0000P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5652 _refine_ls_number_parameters 515 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1597 _refine_ls_R_factor_gt 0.0588 _refine_ls_wR_factor_ref 0.0961 _refine_ls_wR_factor_gt 0.0804 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.004 _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 Cd Cd 0.18429(4) 0.08522(7) 0.91011(3) 0.0390(2) Uani 1 1 d . . . O O 0.1870(3) 0.1524(5) 0.8201(3) 0.0411(19) Uani 1 1 d . . . S1 S 0.09875(12) 0.1679(2) 0.94615(11) 0.0422(8) Uani 1 1 d . . . S2 S 0.29700(12) 0.1258(2) 1.01981(12) 0.0447(8) Uani 1 1 d . . . S3 S 0.16659(13) -0.1453(2) 0.91544(12) 0.0425(8) Uani 1 1 d . . . B B 0.2023(7) -0.0382(12) 1.0803(6) 0.039(4) Uani 1 1 d . . . H1 H 0.205(3) -0.072(6) 1.124(3) 0.007(18) Uiso 1 1 d . . . N11 N 0.1933(4) 0.1066(8) 1.0823(4) 0.039(2) Uani 1 1 d . . . N12 N 0.1752(4) 0.3101(8) 1.0634(4) 0.041(2) Uani 1 1 d . . . N21 N 0.2676(4) -0.0725(9) 1.0791(4) 0.036(2) Uani 1 1 d . . . N22 N 0.3571(4) -0.1041(9) 1.0648(4) 0.036(2) Uani 1 1 d . . . N31 N 0.1352(4) -0.0976(7) 1.0213(3) 0.040(2) Uani 1 1 d . . . N32 N 0.0485(4) -0.1612(6) 0.9244(4) 0.035(2) Uani 1 1 d . . . C11 C 0.1585(5) 0.1974(10) 1.0345(4) 0.031(3) Uani 1 1 d . . . C12 C 0.2327(5) 0.1703(11) 1.1453(4) 0.048(3) Uani 1 1 d . . . H12A H 0.2623 0.1333 1.1886 0.057 Uiso 1 1 calc R . . C13 C 0.2219(5) 0.2902(10) 1.1346(5) 0.048(3) Uani 1 1 d . . . H13A H 0.2420 0.3521 1.1690 0.058 Uiso 1 1 calc R . . C14 C 0.1518(5) 0.4347(10) 1.0304(5) 0.045(3) Uani 1 1 d . . . C15 C 0.1672(5) 0.4444(9) 0.9689(4) 0.064(3) Uani 1 1 d . . . H15A H 0.1424 0.3808 0.9346 0.097 Uiso 1 1 calc R . . H15B H 0.2156 0.4336 0.9861 0.097 Uiso 1 1 calc R . . H15C H 0.1533 0.5250 0.9471 0.097 Uiso 1 1 calc R . . C16 C 0.1919(5) 0.5329(8) 1.0853(4) 0.068(4) Uani 1 1 d . . . H16A H 0.1816 0.5270 1.1240 0.103 Uiso 1 1 calc R . . H16B H 0.1793 0.6142 1.0641 0.103 Uiso 1 1 calc R . . H16C H 0.2402 0.5200 1.1028 0.103 Uiso 1 1 calc R . . C17 C 0.0775(5) 0.4494(8) 1.0090(4) 0.056(3) Uani 1 1 d . . . H17A H 0.0712 0.4429 1.0502 0.084 Uiso 1 1 calc R . . H17B H 0.0516 0.3851 0.9757 0.084 Uiso 1 1 calc R . . H17C H 0.0619 0.5296 0.9872 0.084 Uiso 1 1 calc R . . C21 C 0.3069(6) -0.0235(9) 1.0552(4) 0.035(3) Uani 1 1 d . . . C22 C 0.2932(6) -0.1890(10) 1.1064(5) 0.048(3) Uani 1 1 d . . . H22A H 0.2757 -0.2446 1.1270 0.057 Uiso 1 1 calc R . . C23 C 0.3475(6) -0.2060(10) 1.0974(5) 0.049(3) Uani 1 1 d . . . H23A H 0.3751 -0.2769 1.1112 0.059 Uiso 1 1 calc R . . C24 C 0.4095(5) -0.0865(11) 1.0407(5) 0.048(3) Uani 1 1 d . . . C25 C 0.4537(5) 0.0249(9) 1.0744(5) 0.075(4) Uani 1 1 d . . . H25A H 0.4257 0.0987 1.0608 0.112 Uiso 1 1 calc R . . H25B H 0.4878 0.0315 1.0590 0.112 Uiso 1 1 calc R . . H25C H 0.4760 0.0160 1.1251 0.112 Uiso 1 1 calc R . . C26 C 0.4555(5) -0.2029(9) 1.0632(5) 0.077(4) Uani 1 1 d . . . H26A H 0.4795 -0.2085 1.1141 0.116 Uiso 1 1 calc R . . H26B H 0.4881 -0.1970 1.0458 0.116 Uiso 1 1 calc R . . H26C H 0.4275 -0.2759 1.0438 0.116 Uiso 1 1 calc R . . C27 C 0.3742(4) -0.0780(10) 0.9607(4) 0.070(3) Uani 1 1 d . . . H27A H 0.3453 -0.0054 0.9456 0.106 Uiso 1 1 calc R . . H27B H 0.3466 -0.1512 0.9407 0.106 Uiso 1 1 calc R . . H27C H 0.4080 -0.0721 0.9450 0.106 Uiso 1 1 calc R . . C31 C 0.1152(5) -0.1355(7) 0.9551(5) 0.026(3) Uani 1 1 d . . . C32 C 0.0810(5) -0.1081(9) 1.0336(5) 0.049(3) Uani 1 1 d . . . H32A H 0.0809 -0.0907 1.0761 0.059 Uiso 1 1 calc R . . C33 C 0.0275(5) -0.1482(8) 0.9736(5) 0.039(3) Uani 1 1 d . . . H33A H -0.0165 -0.1643 0.9669 0.047 Uiso 1 1 calc R . . C34 C 0.0005(5) -0.1960(10) 0.8477(4) 0.042(3) Uani 1 1 d . . . C35 C 0.0234(4) -0.3198(8) 0.8292(4) 0.057(3) Uani 1 1 d . . . H35A H 0.0685 -0.3099 0.8338 0.086 Uiso 1 1 calc R . . H35B H -0.0084 -0.3427 0.7812 0.086 Uiso 1 1 calc R . . H35C H 0.0245 -0.3839 0.8610 0.086 Uiso 1 1 calc R . . C36 C -0.0703(5) -0.2128(8) 0.8395(4) 0.058(3) Uani 1 1 d . . . H36A H -0.0855 -0.1358 0.8503 0.087 Uiso 1 1 calc R . . H36B H -0.0693 -0.2766 0.8715 0.087 Uiso 1 1 calc R . . H36C H -0.1015 -0.2369 0.7915 0.087 Uiso 1 1 calc R . . C37 C 0.0000(4) -0.0888(9) 0.8016(4) 0.058(3) Uani 1 1 d . . . H37A H -0.0152 -0.0144 0.8148 0.087 Uiso 1 1 calc R . . H37B H -0.0307 -0.1078 0.7527 0.087 Uiso 1 1 calc R . . H37C H 0.0455 -0.0762 0.8081 0.087 Uiso 1 1 calc R . . C41 C 0.2398(6) 0.1252(10) 0.8122(4) 0.037(3) Uani 1 1 d . . . C42 C 0.2955(6) 0.2086(11) 0.8354(5) 0.040(3) Uani 1 1 d . . . C43 C 0.3526(6) 0.1811(13) 0.8280(5) 0.063(4) Uani 1 1 d . . . H43A H 0.3883 0.2386 0.8432 0.076 Uiso 1 1 calc R . . C44 C 0.3577(6) 0.0701(14) 0.7983(5) 0.067(4) Uani 1 1 d . . . H44A H 0.3964 0.0526 0.7934 0.080 Uiso 1 1 calc R . . C45 C 0.3053(6) -0.0132(11) 0.7764(5) 0.060(4) Uani 1 1 d . . . H45A H 0.3088 -0.0885 0.7568 0.072 Uiso 1 1 calc R . . C46 C 0.2473(6) 0.0101(11) 0.7823(5) 0.043(3) Uani 1 1 d . . . C51 C 0.2970(6) 0.3273(12) 0.8703(5) 0.053(3) Uani 1 1 d . . . C52 C 0.3533(6) 0.3658(12) 0.9312(6) 0.082(4) Uani 1 1 d . . . H52A H 0.3918 0.3144 0.9511 0.098 Uiso 1 1 calc R . . C53 C 0.3557(7) 0.4779(14) 0.9647(6) 0.084(5) Uani 1 1 d . . . H53A H 0.3952 0.4994 1.0063 0.100 Uiso 1 1 calc R . . C54 C 0.3006(7) 0.5572(12) 0.9371(7) 0.091(5) Uani 1 1 d . . . H54A H 0.3013 0.6332 0.9584 0.109 Uiso 1 1 calc R . . C55 C 0.2445(6) 0.5180(11) 0.8765(6) 0.058(3) Uani 1 1 d . . . H55A H 0.2060 0.5693 0.8566 0.070 Uiso 1 1 calc R . . C56 C 0.2420(6) 0.4055(13) 0.8431(5) 0.058(3) Uani 1 1 d . . . H56A H 0.2024 0.3836 0.8018 0.070 Uiso 1 1 calc R . . C61 C 0.1912(5) -0.0819(12) 0.7546(4) 0.038(3) Uani 1 1 d . . . C62 C 0.2041(6) -0.2086(13) 0.7605(5) 0.053(3) Uani 1 1 d . . . H62A H 0.2490 -0.2367 0.7873 0.064 Uiso 1 1 calc R . . C63 C 0.1529(8) -0.2927(12) 0.7282(6) 0.076(4) Uani 1 1 d . . . H63A H 0.1634 -0.3772 0.7308 0.091 Uiso 1 1 calc R . . C64 C 0.0864(7) -0.2551(12) 0.6920(5) 0.066(4) Uani 1 1 d . . . H64A H 0.0513 -0.3139 0.6716 0.079 Uiso 1 1 calc R . . C65 C 0.0712(6) -0.1322(12) 0.6856(5) 0.056(4) Uani 1 1 d . . . H65A H 0.0258 -0.1059 0.6596 0.067 Uiso 1 1 calc R . . C66 C 0.1228(5) -0.0461(10) 0.7175(4) 0.046(3) Uani 1 1 d . . . H66A H 0.1117 0.0382 0.7141 0.056 Uiso 1 1 calc R . . C101 C 0.4025(14) 0.640(2) 0.8323(16) 0.45(3) Uani 1 1 d . . . H10A H 0.3629 0.5878 0.8073 0.676 Uiso 1 1 calc R . . H10B H 0.3925 0.7226 0.8125 0.676 Uiso 1 1 calc R . . H10C H 0.4142 0.6438 0.8816 0.676 Uiso 1 1 calc R . . C102 C 0.4542(10) 0.5940(14) 0.8264(9) 0.235(18) Uani 1 1 d G . . C103 C 0.4268(5) 0.4908(18) 0.7840(8) 0.178(11) Uani 1 1 d G . . H10D H 0.3812 0.4687 0.7685 0.213 Uiso 1 1 calc R . . C104 C 0.4669(11) 0.4202(10) 0.7644(6) 0.30(2) Uani 1 1 d G . . H10E H 0.4484 0.3503 0.7357 0.363 Uiso 1 1 calc R . . C105 C 0.5343(10) 0.4528(15) 0.7872(10) 0.237(16) Uani 1 1 d G . . H10F H 0.5614 0.4051 0.7740 0.285 Uiso 1 1 calc R . . C106 C 0.5616(5) 0.556(2) 0.8297(8) 0.253(16) Uani 1 1 d G . . H10G H 0.6072 0.5782 0.8452 0.303 Uiso 1 1 calc R . . C107 C 0.5216(11) 0.6267(11) 0.8493(6) 0.173(11) Uani 1 1 d G . . H10H H 0.5401 0.6965 0.8780 0.208 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 Cd 0.0383(5) 0.0441(5) 0.0366(3) 0.0042(4) 0.0195(3) 0.0023(5) O 0.036(5) 0.052(5) 0.043(4) 0.005(3) 0.026(4) 0.010(4) S1 0.0336(17) 0.057(2) 0.0333(13) -0.0046(13) 0.0136(13) 0.0045(14) S2 0.0362(18) 0.044(2) 0.0490(15) 0.0111(13) 0.0162(13) -0.0024(14) S3 0.045(2) 0.036(2) 0.0556(15) -0.0045(14) 0.0320(15) -0.0022(14) B 0.056(11) 0.030(11) 0.031(7) 0.006(6) 0.022(7) -0.004(7) N11 0.036(5) 0.049(8) 0.036(4) 0.003(5) 0.021(4) -0.009(5) N12 0.051(6) 0.030(7) 0.035(5) -0.007(5) 0.015(5) -0.002(5) N21 0.029(6) 0.039(8) 0.049(5) 0.002(5) 0.024(5) -0.005(5) N22 0.021(5) 0.042(7) 0.036(4) -0.004(5) 0.005(4) -0.002(5) N31 0.041(6) 0.043(6) 0.038(5) 0.004(5) 0.020(4) -0.006(5) N32 0.027(6) 0.043(6) 0.044(5) -0.013(4) 0.025(5) -0.010(4) C11 0.042(7) 0.026(8) 0.037(6) -0.003(5) 0.028(6) -0.004(6) C12 0.041(7) 0.060(9) 0.028(6) -0.007(6) 0.006(5) 0.000(7) C13 0.043(8) 0.052(9) 0.039(6) -0.015(6) 0.012(6) -0.012(7) C14 0.046(8) 0.040(10) 0.050(6) 0.002(6) 0.022(6) 0.007(7) C15 0.083(9) 0.048(9) 0.074(7) 0.010(6) 0.047(7) 0.016(7) C16 0.077(9) 0.046(9) 0.061(7) -0.011(6) 0.016(6) -0.023(7) C17 0.058(8) 0.046(9) 0.063(6) 0.002(5) 0.028(6) 0.019(6) C21 0.029(7) 0.044(9) 0.029(5) -0.001(5) 0.011(5) -0.009(7) C22 0.027(7) 0.032(9) 0.067(7) 0.010(6) 0.009(6) 0.008(6) C23 0.058(9) 0.029(9) 0.050(6) 0.021(6) 0.016(7) 0.007(7) C24 0.045(8) 0.036(9) 0.072(7) -0.001(7) 0.035(6) 0.011(7) C25 0.049(9) 0.076(11) 0.106(9) -0.018(8) 0.043(7) -0.023(7) C26 0.065(10) 0.080(11) 0.083(8) -0.003(7) 0.032(7) 0.027(8) C27 0.064(8) 0.103(10) 0.058(6) 0.003(7) 0.040(6) 0.009(8) C31 0.033(7) 0.020(7) 0.040(6) 0.007(4) 0.028(6) 0.002(5) C32 0.046(7) 0.067(9) 0.048(6) -0.009(6) 0.034(6) -0.011(7) C33 0.023(7) 0.049(8) 0.053(6) -0.008(5) 0.024(6) -0.002(5) C34 0.026(7) 0.060(10) 0.034(6) -0.005(6) 0.008(5) -0.011(6) C35 0.054(8) 0.043(8) 0.061(7) -0.017(6) 0.016(6) 0.001(6) C36 0.054(9) 0.071(9) 0.044(6) -0.015(6) 0.018(6) -0.021(7) C37 0.044(7) 0.080(9) 0.049(6) 0.000(7) 0.020(5) -0.001(7) C41 0.038(8) 0.039(10) 0.033(6) 0.012(5) 0.016(6) -0.002(7) C42 0.044(9) 0.047(10) 0.036(6) 0.016(6) 0.025(6) 0.007(7) C43 0.027(8) 0.100(14) 0.053(7) 0.014(7) 0.012(6) 0.009(8) C44 0.039(9) 0.098(14) 0.067(8) 0.024(8) 0.028(7) 0.012(9) C45 0.039(8) 0.087(12) 0.054(7) 0.014(7) 0.022(7) 0.025(8) C46 0.041(9) 0.041(10) 0.045(6) 0.018(6) 0.018(6) 0.022(7) C51 0.047(9) 0.052(10) 0.050(7) 0.020(7) 0.015(7) 0.001(8) C52 0.063(10) 0.064(11) 0.070(8) 0.014(7) -0.007(7) 0.002(8) C53 0.083(12) 0.081(13) 0.062(8) 0.000(8) 0.015(8) -0.023(10) C54 0.081(11) 0.050(12) 0.120(11) 0.000(9) 0.031(9) -0.027(9) C55 0.054(9) 0.064(11) 0.069(8) 0.030(7) 0.039(7) 0.002(7) C56 0.075(10) 0.057(10) 0.044(6) 0.006(7) 0.029(6) -0.010(9) C61 0.047(8) 0.034(9) 0.031(5) 0.000(6) 0.017(5) 0.015(8) C62 0.060(10) 0.059(11) 0.035(6) 0.002(6) 0.019(6) 0.017(8) C63 0.115(14) 0.055(12) 0.059(8) -0.006(7) 0.043(9) 0.023(10) C64 0.088(12) 0.051(11) 0.063(8) -0.006(7) 0.039(8) 0.001(9) C65 0.054(9) 0.063(11) 0.053(7) -0.001(7) 0.028(6) 0.008(8) C66 0.043(8) 0.039(9) 0.048(6) 0.004(6) 0.015(6) -0.003(7) C101 0.55(5) 0.42(4) 0.67(6) 0.37(4) 0.52(5) 0.39(4) C102 0.16(3) 0.17(3) 0.39(4) 0.21(3) 0.14(3) 0.04(2) C103 0.19(2) 0.10(2) 0.154(18) 0.041(14) 0.010(14) -0.033(16) C104 0.67(6) 0.16(3) 0.20(2) 0.09(2) 0.30(3) 0.11(4) C105 0.31(3) 0.25(4) 0.31(3) 0.21(3) 0.27(3) 0.17(2) C106 0.51(4) 0.10(3) 0.126(18) 0.052(15) 0.13(2) 0.05(3) C107 0.34(3) 0.083(17) 0.117(13) -0.006(11) 0.124(19) -0.02(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 Cd O 2.109(6) . ? Cd S3 2.538(3) . ? Cd S2 2.544(2) . ? Cd S1 2.550(3) . ? O C41 1.305(10) . ? S1 C11 1.762(9) . ? S2 C21 1.758(10) . ? S3 C31 1.737(9) . ? B N21 1.519(13) . ? B N31 1.571(12) . ? B N11 1.585(13) . ? N11 C11 1.368(10) . ? N11 C12 1.403(10) . ? N12 C11 1.341(10) . ? N12 C13 1.406(10) . ? N12 C14 1.500(11) . ? N21 C21 1.325(10) . ? N21 C22 1.395(11) . ? N22 C21 1.358(11) . ? N22 C23 1.382(11) . ? N22 C24 1.507(11) . ? N31 C31 1.346(9) . ? N31 C32 1.366(9) . ? N32 C31 1.341(9) . ? N32 C33 1.360(9) . ? N32 C34 1.533(10) . ? C12 C13 1.321(11) . ? C14 C17 1.505(11) . ? C14 C16 1.527(11) . ? C14 C15 1.530(11) . ? C22 C23 1.330(11) . ? C24 C27 1.523(10) . ? C24 C25 1.508(12) . ? C24 C26 1.550(12) . ? C32 C33 1.351(10) . ? C34 C37 1.527(11) . ? C34 C36 1.519(11) . ? C34 C35 1.555(11) . ? C41 C42 1.421(12) . ? C41 C46 1.451(12) . ? C42 C43 1.396(13) . ? C42 C51 1.482(13) . ? C43 C44 1.393(13) . ? C44 C45 1.373(13) . ? C45 C46 1.387(12) . ? C46 C61 1.485(13) . ? C51 C52 1.383(13) . ? C51 C56 1.373(13) . ? C52 C53 1.402(13) . ? C53 C54 1.383(14) . ? C54 C55 1.379(12) . ? C55 C56 1.404(13) . ? C61 C62 1.395(13) . ? C61 C66 1.402(11) . ? C62 C63 1.365(13) . ? C63 C64 1.371(13) . ? C64 C65 1.365(12) . ? C65 C66 1.383(11) . ? C101 C102 1.320(19) . ? C102 C103 1.3900 . ? C102 C107 1.3900 . ? C103 C104 1.3900 . ? C104 C105 1.3900 . ? C105 C106 1.3900 . ? C106 C107 1.3900 . ? 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 O Cd S3 117.07(17) . . ? O Cd S2 110.49(17) . . ? S3 Cd S2 103.54(8) . . ? O Cd S1 121.31(18) . . ? S3 Cd S1 100.07(8) . . ? S2 Cd S1 101.99(8) . . ? C41 O Cd 118.1(5) . . ? C11 S1 Cd 96.0(3) . . ? C21 S2 Cd 96.3(3) . . ? C31 S3 Cd 96.7(3) . . ? N21 B N31 116.1(9) . . ? N21 B N11 112.3(9) . . ? N31 B N11 110.0(9) . . ? C11 N11 C12 104.4(9) . . ? C11 N11 B 136.4(8) . . ? C12 N11 B 118.9(8) . . ? C11 N12 C13 105.5(8) . . ? C11 N12 C14 129.8(8) . . ? C13 N12 C14 124.6(8) . . ? C21 N21 C22 108.2(9) . . ? C21 N21 B 137.0(10) . . ? C22 N21 B 114.7(10) . . ? C21 N22 C23 105.7(9) . . ? C21 N22 C24 126.2(10) . . ? C23 N22 C24 128.0(11) . . ? C31 N31 C32 108.0(8) . . ? C31 N31 B 133.8(9) . . ? C32 N31 B 117.9(8) . . ? C31 N32 C33 108.1(7) . . ? C31 N32 C34 128.6(8) . . ? C33 N32 C34 123.3(8) . . ? N12 C11 N11 111.7(8) . . ? N12 C11 S1 124.7(8) . . ? N11 C11 S1 123.6(8) . . ? C13 C12 N11 109.6(9) . . ? C12 C13 N12 108.7(8) . . ? C17 C14 N12 109.0(8) . . ? C17 C14 C16 108.5(8) . . ? N12 C14 C16 108.3(7) . . ? C17 C14 C15 113.5(7) . . ? N12 C14 C15 107.7(8) . . ? C16 C14 C15 109.7(9) . . ? N21 C21 N22 109.8(9) . . ? N21 C21 S2 124.7(10) . . ? N22 C21 S2 125.4(10) . . ? C23 C22 N21 106.4(10) . . ? C22 C23 N22 109.9(11) . . ? N22 C24 C27 109.5(8) . . ? N22 C24 C25 111.8(8) . . ? C27 C24 C25 111.5(9) . . ? N22 C24 C26 107.3(9) . . ? C27 C24 C26 108.2(8) . . ? C25 C24 C26 108.4(8) . . ? N31 C31 N32 108.4(8) . . ? N31 C31 S3 125.7(8) . . ? N32 C31 S3 125.9(7) . . ? C33 C32 N31 107.4(8) . . ? C32 C33 N32 108.0(9) . . ? C37 C34 C36 109.5(8) . . ? C37 C34 C35 112.8(8) . . ? C36 C34 C35 108.7(8) . . ? C37 C34 N32 107.7(8) . . ? C36 C34 N32 107.9(7) . . ? C35 C34 N32 110.2(8) . . ? O C41 C42 120.4(11) . . ? O C41 C46 123.8(10) . . ? C42 C41 C46 115.8(11) . . ? C43 C42 C41 121.3(12) . . ? C43 C42 C51 116.4(12) . . ? C41 C42 C51 122.3(11) . . ? C44 C43 C42 121.3(13) . . ? C43 C44 C45 118.7(13) . . ? C44 C45 C46 122.1(13) . . ? C45 C46 C41 120.7(12) . . ? C45 C46 C61 119.2(11) . . ? C41 C46 C61 120.1(11) . . ? C52 C51 C56 116.4(12) . . ? C52 C51 C42 122.4(12) . . ? C56 C51 C42 121.2(11) . . ? C51 C52 C53 123.1(12) . . ? C52 C53 C54 120.5(12) . . ? C55 C54 C53 116.0(14) . . ? C54 C55 C56 123.5(12) . . ? C55 C56 C51 120.4(11) . . ? C62 C61 C66 116.4(11) . . ? C62 C61 C46 121.7(11) . . ? C66 C61 C46 121.8(11) . . ? C61 C62 C63 121.6(12) . . ? C62 C63 C64 120.7(13) . . ? C65 C64 C63 119.8(13) . . ? C66 C65 C64 119.9(11) . . ? C65 C66 C61 121.5(11) . . ? C101 C102 C103 104(2) . . ? C101 C102 C107 136(2) . . ? C103 C102 C107 120.0 . . ? C102 C103 C104 120.0 . . ? C105 C104 C103 120.0 . . ? C104 C105 C106 120.0 . . ? C107 C106 C105 120.0 . . ? C106 C107 C102 120.0 . . ? _diffrn_measured_fraction_theta_max 0.856 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.856 _refine_diff_density_max 0.731 _refine_diff_density_min -0.489 _refine_diff_density_rms 0.092 # Attachment 'CDSES10.CIF' data_cdses10 _database_code_depnum_ccdc_archive 'CCDC 609899' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H39 B Cd N6 S3 Se' _chemical_formula_weight 745.99 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 '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 10.4001(6) _cell_length_b 32.699(2) _cell_length_c 10.6389(7) _cell_angle_alpha 90.00 _cell_angle_beta 113.7170(10) _cell_angle_gamma 90.00 _cell_volume 3312.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 243(2) _cell_measurement_reflns_used 4984 _cell_measurement_theta_min 2.473 _cell_measurement_theta_max 26.442 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.496 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1512 _exptl_absorpt_coefficient_mu 1.974 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.5889 _exptl_absorpt_correction_T_max 0.8271 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 243(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23017 _diffrn_reflns_av_R_equivalents 0.0548 _diffrn_reflns_av_sigmaI/netI 0.0847 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -43 _diffrn_reflns_limit_k_max 42 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 28.29 _reflns_number_total 7646 _reflns_number_gt 4284 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0203P)^2^+0.0000P] 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 0.00009(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7646 _refine_ls_number_parameters 357 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1029 _refine_ls_R_factor_gt 0.0419 _refine_ls_wR_factor_ref 0.0712 _refine_ls_wR_factor_gt 0.0620 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.043 _refine_ls_shift/su_mean 0.004 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 Cd Cd 0.63867(3) 0.373685(8) 0.91979(3) 0.04096(10) Uani 1 1 d . . . Se Se 0.48709(4) 0.349479(14) 1.04442(4) 0.05756(14) Uani 1 1 d . . . S1 S 0.53547(9) 0.41023(3) 0.68582(10) 0.0459(3) Uani 1 1 d . . . S2 S 0.80694(9) 0.32632(3) 0.86815(10) 0.0410(2) Uani 1 1 d . . . S3 S 0.81123(9) 0.42719(3) 1.07319(10) 0.0447(3) Uani 1 1 d . . . B B 0.8946(5) 0.42241(14) 0.7895(5) 0.0453(12) Uani 1 1 d . . . H1 H 0.967(3) 0.4396(8) 0.743(3) 0.032(8) Uiso 1 1 d . . . N11 N 0.7803(3) 0.45484(9) 0.7785(3) 0.0465(8) Uani 1 1 d . . . N12 N 0.5952(3) 0.49114(9) 0.7591(3) 0.0479(8) Uani 1 1 d . . . N21 N 0.8326(3) 0.38499(9) 0.6935(3) 0.0429(8) Uani 1 1 d . . . N22 N 0.7304(3) 0.32879(9) 0.5875(3) 0.0426(8) Uani 1 1 d . . . N31 N 0.9824(3) 0.40980(9) 0.9406(3) 0.0426(8) Uani 1 1 d . . . N32 N 1.0709(3) 0.39027(9) 1.1564(3) 0.0424(8) Uani 1 1 d . . . C11 C 0.6391(4) 0.45304(11) 0.7422(3) 0.0406(9) Uani 1 1 d . . . C12 C 0.8223(4) 0.49447(12) 0.8185(4) 0.0580(12) Uani 1 1 d . . . H12A H 0.9150 0.5042 0.8499 0.070 Uiso 1 1 calc R . . C13 C 0.7105(5) 0.51668(12) 0.8055(4) 0.0571(12) Uani 1 1 d . . . H13A H 0.7101 0.5447 0.8245 0.069 Uiso 1 1 calc R . . C14 C 0.4459(4) 0.50460(12) 0.7272(4) 0.0519(11) Uani 1 1 d . . . C15 C 0.3849(5) 0.47940(13) 0.8121(4) 0.0774(14) Uani 1 1 d . . . H15A H 0.4396 0.4843 0.9091 0.116 Uiso 1 1 calc R . . H15B H 0.3884 0.4506 0.7923 0.116 Uiso 1 1 calc R . . H15C H 0.2882 0.4875 0.7886 0.116 Uiso 1 1 calc R . . C16 C 0.4481(5) 0.54979(12) 0.7654(4) 0.0739(14) Uani 1 1 d . . . H16A H 0.4895 0.5657 0.7143 0.111 Uiso 1 1 calc R . . H16B H 0.5033 0.5532 0.8630 0.111 Uiso 1 1 calc R . . H16C H 0.3529 0.5591 0.7430 0.111 Uiso 1 1 calc R . . C17 C 0.3577(4) 0.49946(12) 0.5739(4) 0.0598(11) Uani 1 1 d . . . H17A H 0.3971 0.5160 0.5224 0.090 Uiso 1 1 calc R . . H17B H 0.2621 0.5082 0.5529 0.090 Uiso 1 1 calc R . . H17C H 0.3579 0.4709 0.5488 0.090 Uiso 1 1 calc R . . C21 C 0.7882(3) 0.34732(11) 0.7128(4) 0.0391(9) Uani 1 1 d . . . C22 C 0.8006(4) 0.38904(13) 0.5562(4) 0.0552(11) Uani 1 1 d . . . H22A H 0.8206 0.4121 0.5146 0.066 Uiso 1 1 calc R . . C23 C 0.7370(4) 0.35547(14) 0.4906(4) 0.0574(11) Uani 1 1 d . . . H23A H 0.7029 0.3508 0.3955 0.069 Uiso 1 1 calc R . . C24 C 0.6585(4) 0.28765(12) 0.5541(4) 0.0490(10) Uani 1 1 d . . . C25 C 0.7643(4) 0.25414(12) 0.6258(4) 0.0663(13) Uani 1 1 d . . . H25A H 0.8428 0.2559 0.5988 0.100 Uiso 1 1 calc R . . H25B H 0.7195 0.2276 0.5998 0.100 Uiso 1 1 calc R . . H25C H 0.7979 0.2575 0.7244 0.100 Uiso 1 1 calc R . . C26 C 0.5355(4) 0.28715(13) 0.5985(4) 0.0633(12) Uani 1 1 d . . . H26A H 0.4715 0.3093 0.5537 0.095 Uiso 1 1 calc R . . H26B H 0.5708 0.2905 0.6973 0.095 Uiso 1 1 calc R . . H26C H 0.4862 0.2613 0.5727 0.095 Uiso 1 1 calc R . . C27 C 0.6006(5) 0.28084(14) 0.3995(4) 0.0856(15) Uani 1 1 d . . . H27A H 0.5352 0.3026 0.3532 0.128 Uiso 1 1 calc R . . H27B H 0.5524 0.2547 0.3773 0.128 Uiso 1 1 calc R . . H27C H 0.6772 0.2809 0.3696 0.128 Uiso 1 1 calc R . . C31 C 0.9585(3) 0.40826(10) 1.0558(4) 0.0377(9) Uani 1 1 d . . . C32 C 1.1137(4) 0.39199(12) 0.9705(5) 0.0508(11) Uani 1 1 d . . . H32A H 1.1572 0.3888 0.9089 0.061 Uiso 1 1 calc R . . C33 C 1.1660(4) 0.38037(11) 1.1005(5) 0.0504(11) Uani 1 1 d . . . H33A H 1.2533 0.3675 1.1471 0.061 Uiso 1 1 calc R . . C34 C 1.0874(4) 0.37938(13) 1.2997(4) 0.0582(12) Uani 1 1 d . . . C35 C 1.2343(4) 0.36055(14) 1.3756(4) 0.0868(16) Uani 1 1 d . . . H35A H 1.2402 0.3350 1.3317 0.130 Uiso 1 1 calc R . . H35B H 1.2501 0.3554 1.4705 0.130 Uiso 1 1 calc R . . H35C H 1.3049 0.3794 1.3725 0.130 Uiso 1 1 calc R . . C36 C 1.0773(4) 0.41771(14) 1.3770(4) 0.0742(14) Uani 1 1 d . . . H36A H 1.0815 0.4101 1.4667 0.111 Uiso 1 1 calc R . . H36B H 0.9892 0.4316 1.3256 0.111 Uiso 1 1 calc R . . H36C H 1.1549 0.4359 1.3880 0.111 Uiso 1 1 calc R . . C37 C 0.9773(4) 0.34750(13) 1.2897(4) 0.0690(13) Uani 1 1 d . . . H37A H 0.9904 0.3235 1.2426 0.103 Uiso 1 1 calc R . . H37B H 0.8844 0.3587 1.2389 0.103 Uiso 1 1 calc R . . H37C H 0.9870 0.3400 1.3813 0.103 Uiso 1 1 calc R . . C41 C 0.3456(3) 0.31788(12) 0.9077(4) 0.0462(10) Uani 1 1 d . . . C42 C 0.3251(4) 0.31734(15) 0.7734(5) 0.0764(15) Uani 1 1 d . . . H42A H 0.3793 0.3348 0.7440 0.092 Uiso 1 1 calc R . . C43 C 0.2269(5) 0.29188(18) 0.6774(5) 0.104(2) Uani 1 1 d . . . H43A H 0.2183 0.2915 0.5860 0.125 Uiso 1 1 calc R . . C44 C 0.1446(5) 0.26784(18) 0.7162(6) 0.0975(18) Uani 1 1 d . . . H44A H 0.0785 0.2504 0.6522 0.117 Uiso 1 1 calc R . . C45 C 0.1573(5) 0.26884(15) 0.8477(6) 0.0833(16) Uani 1 1 d . . . H45A H 0.0965 0.2531 0.8740 0.100 Uiso 1 1 calc R . . C46 C 0.2589(4) 0.29278(13) 0.9436(5) 0.0630(12) Uani 1 1 d . . . H46A H 0.2695 0.2920 1.0355 0.076 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 Cd 0.04062(14) 0.03901(18) 0.04496(18) 0.00152(15) 0.01897(13) -0.00018(14) Se 0.0605(3) 0.0653(3) 0.0583(3) -0.0050(2) 0.0357(2) -0.0096(2) S1 0.0510(5) 0.0343(6) 0.0435(6) -0.0004(5) 0.0098(5) -0.0024(5) S2 0.0502(5) 0.0344(6) 0.0410(6) 0.0022(5) 0.0210(5) 0.0028(5) S3 0.0406(5) 0.0453(7) 0.0458(6) -0.0084(5) 0.0150(5) 0.0046(5) B 0.055(3) 0.039(3) 0.046(3) -0.003(2) 0.024(2) -0.007(2) N11 0.057(2) 0.030(2) 0.043(2) 0.0012(15) 0.0110(16) -0.0090(17) N12 0.066(2) 0.033(2) 0.037(2) -0.0003(15) 0.0124(17) 0.0021(18) N21 0.0571(18) 0.033(2) 0.041(2) -0.0015(15) 0.0232(17) -0.0021(15) N22 0.0526(18) 0.039(2) 0.041(2) -0.0061(17) 0.0235(17) -0.0043(16) N31 0.0377(16) 0.039(2) 0.051(2) -0.0064(16) 0.0168(16) -0.0030(15) N32 0.0335(15) 0.040(2) 0.048(2) -0.0020(16) 0.0102(16) -0.0020(14) C11 0.058(2) 0.031(2) 0.027(2) 0.0038(17) 0.0103(18) 0.002(2) C12 0.067(3) 0.034(3) 0.060(3) 0.000(2) 0.012(2) -0.015(2) C13 0.080(3) 0.023(2) 0.057(3) -0.004(2) 0.015(2) -0.008(2) C14 0.074(3) 0.042(3) 0.040(3) 0.002(2) 0.022(2) 0.010(2) C15 0.109(4) 0.070(4) 0.070(3) 0.008(3) 0.053(3) 0.018(3) C16 0.106(3) 0.046(3) 0.067(3) 0.001(2) 0.032(3) 0.023(3) C17 0.065(2) 0.058(3) 0.049(3) 0.006(2) 0.015(2) 0.018(2) C21 0.042(2) 0.037(2) 0.045(3) -0.002(2) 0.0251(19) 0.0017(19) C22 0.076(3) 0.049(3) 0.048(3) 0.006(2) 0.034(2) -0.008(2) C23 0.077(3) 0.057(3) 0.043(3) -0.001(2) 0.029(2) -0.002(3) C24 0.053(2) 0.043(3) 0.048(3) -0.012(2) 0.017(2) -0.005(2) C25 0.067(3) 0.042(3) 0.090(4) -0.014(2) 0.031(3) 0.002(2) C26 0.048(2) 0.063(3) 0.069(3) 0.001(2) 0.014(2) 0.000(2) C27 0.114(4) 0.072(4) 0.062(3) -0.027(3) 0.027(3) -0.025(3) C31 0.0365(19) 0.032(2) 0.040(2) -0.0071(19) 0.0116(19) -0.0059(17) C32 0.041(2) 0.048(3) 0.066(3) -0.010(2) 0.023(2) 0.000(2) C33 0.0320(19) 0.045(3) 0.069(3) -0.004(2) 0.015(2) 0.0023(18) C34 0.049(2) 0.063(3) 0.050(3) 0.007(2) 0.007(2) -0.003(2) C35 0.052(3) 0.112(5) 0.069(3) 0.016(3) -0.004(2) 0.014(3) C36 0.080(3) 0.087(4) 0.043(3) -0.008(3) 0.011(2) -0.012(3) C37 0.058(3) 0.066(3) 0.070(3) 0.014(3) 0.013(2) -0.007(2) C41 0.036(2) 0.051(3) 0.056(3) 0.003(2) 0.023(2) 0.0040(19) C42 0.055(3) 0.102(4) 0.068(4) 0.006(3) 0.020(3) -0.026(3) C43 0.082(3) 0.156(6) 0.069(4) -0.003(4) 0.025(3) -0.053(4) C44 0.063(3) 0.131(5) 0.095(5) -0.009(4) 0.028(3) -0.034(3) C45 0.061(3) 0.085(4) 0.113(5) 0.000(4) 0.045(3) -0.022(3) C46 0.062(3) 0.061(3) 0.076(3) 0.001(3) 0.039(3) 0.004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd S2 2.5568(9) . ? Cd Se 2.5595(5) . ? Cd S3 2.5669(10) . ? Cd S1 2.5743(10) . ? Se C41 1.904(4) . ? S1 C11 1.721(4) . ? S2 C21 1.726(4) . ? S3 C31 1.730(3) . ? B N31 1.552(5) . ? B N11 1.562(5) . ? B N21 1.558(5) . ? N11 C11 1.362(4) . ? N11 C12 1.379(4) . ? N12 C11 1.363(4) . ? N12 C13 1.379(4) . ? N12 C14 1.516(4) . ? N21 C21 1.360(4) . ? N21 C22 1.367(4) . ? N22 C21 1.365(4) . ? N22 C23 1.373(5) . ? N22 C24 1.510(4) . ? N31 C31 1.346(4) . ? N31 C32 1.399(4) . ? N32 C31 1.360(4) . ? N32 C33 1.382(4) . ? N32 C34 1.507(5) . ? C12 C13 1.331(5) . ? C14 C17 1.525(5) . ? C14 C15 1.536(5) . ? C14 C16 1.530(5) . ? C22 C23 1.326(5) . ? C24 C25 1.522(5) . ? C24 C27 1.523(5) . ? C24 C26 1.532(5) . ? C32 C33 1.322(5) . ? C34 C37 1.520(5) . ? C34 C36 1.526(6) . ? C34 C35 1.540(5) . ? C41 C42 1.357(5) . ? C41 C46 1.382(5) . ? C42 C43 1.393(6) . ? C43 C44 1.344(6) . ? C44 C45 1.352(6) . ? C45 C46 1.380(6) . ? 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 S2 Cd Se 122.78(3) . . ? S2 Cd S3 100.69(3) . . ? Se Cd S3 107.47(3) . . ? S2 Cd S1 97.39(3) . . ? Se Cd S1 122.71(3) . . ? S3 Cd S1 102.20(3) . . ? C41 Se Cd 102.68(12) . . ? C11 S1 Cd 94.68(12) . . ? C21 S2 Cd 98.10(12) . . ? C31 S3 Cd 96.37(12) . . ? N31 B N11 111.8(3) . . ? N31 B N21 112.7(3) . . ? N11 B N21 112.5(3) . . ? C11 N11 C12 107.4(3) . . ? C11 N11 B 133.9(3) . . ? C12 N11 B 118.5(3) . . ? C11 N12 C13 108.2(3) . . ? C11 N12 C14 127.1(3) . . ? C13 N12 C14 124.7(3) . . ? C21 N21 C22 107.3(3) . . ? C21 N21 B 133.5(3) . . ? C22 N21 B 118.9(3) . . ? C21 N22 C23 108.4(3) . . ? C21 N22 C24 127.4(3) . . ? C23 N22 C24 124.0(3) . . ? C31 N31 C32 107.4(3) . . ? C31 N31 B 134.9(3) . . ? C32 N31 B 117.4(3) . . ? C31 N32 C33 107.5(3) . . ? C31 N32 C34 127.6(3) . . ? C33 N32 C34 124.8(3) . . ? N11 C11 N12 107.6(3) . . ? N11 C11 S1 125.9(3) . . ? N12 C11 S1 126.4(3) . . ? C13 C12 N11 109.0(4) . . ? C12 C13 N12 107.7(3) . . ? C17 C14 N12 109.2(3) . . ? C17 C14 C15 110.9(4) . . ? N12 C14 C15 109.9(3) . . ? C17 C14 C16 109.2(3) . . ? N12 C14 C16 108.4(3) . . ? C15 C14 C16 109.1(3) . . ? N21 C21 N22 107.3(3) . . ? N21 C21 S2 126.2(3) . . ? N22 C21 S2 126.5(3) . . ? C23 C22 N21 109.7(4) . . ? C22 C23 N22 107.2(4) . . ? C25 C24 N22 109.5(3) . . ? C25 C24 C27 109.1(3) . . ? N22 C24 C27 109.1(3) . . ? C25 C24 C26 111.3(3) . . ? N22 C24 C26 109.4(3) . . ? C27 C24 C26 108.3(3) . . ? N31 C31 N32 108.5(3) . . ? N31 C31 S3 125.4(3) . . ? N32 C31 S3 126.0(3) . . ? C33 C32 N31 108.1(4) . . ? C32 C33 N32 108.6(3) . . ? N32 C34 C37 108.4(3) . . ? N32 C34 C36 110.3(3) . . ? C37 C34 C36 112.8(4) . . ? N32 C34 C35 108.1(3) . . ? C37 C34 C35 108.8(3) . . ? C36 C34 C35 108.3(3) . . ? C42 C41 C46 116.1(4) . . ? C42 C41 Se 123.9(3) . . ? C46 C41 Se 120.0(3) . . ? C41 C42 C43 122.5(4) . . ? C44 C43 C42 119.6(5) . . ? C43 C44 C45 119.7(5) . . ? C44 C45 C46 120.4(5) . . ? C45 C46 C41 121.6(4) . . ? _diffrn_measured_fraction_theta_max 0.929 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.929 _refine_diff_density_max 0.400 _refine_diff_density_min -0.459 _refine_diff_density_rms 0.079 # Attachment 'CDTES10.CIF' data_cdtes10 _database_code_depnum_ccdc_archive 'CCDC 609900' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H39 B Cd N6 S3 Te' _chemical_formula_weight 794.63 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 '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 10.6859(6) _cell_length_b 32.5774(17) _cell_length_c 10.8236(5) _cell_angle_alpha 90.00 _cell_angle_beta 115.5480(10) _cell_angle_gamma 90.00 _cell_volume 3399.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 243(2) _cell_measurement_reflns_used 5517 _cell_measurement_theta_min 2.498 _cell_measurement_theta_max 25.008 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.553 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1584 _exptl_absorpt_coefficient_mu 1.694 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.7281 _exptl_absorpt_correction_T_max 0.8489 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 243(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23627 _diffrn_reflns_av_R_equivalents 0.0507 _diffrn_reflns_av_sigmaI/netI 0.0762 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -40 _diffrn_reflns_limit_k_max 43 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 28.29 _reflns_number_total 7931 _reflns_number_gt 4522 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0450P)^2^+0.0000P] 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 0.00010(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7931 _refine_ls_number_parameters 357 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1030 _refine_ls_R_factor_gt 0.0459 _refine_ls_wR_factor_ref 0.1101 _refine_ls_wR_factor_gt 0.0940 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.019 _refine_ls_shift/su_mean 0.003 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 Cd Cd 0.12995(4) 0.126036(11) 0.41201(4) 0.04237(12) Uani 1 1 d . . . Te Te -0.03217(4) 0.148870(13) 0.53559(4) 0.05965(15) Uani 1 1 d . . . S1 S 0.30007(14) 0.07214(4) 0.56838(13) 0.0479(3) Uani 1 1 d . . . S2 S 0.29677(14) 0.17385(4) 0.36989(12) 0.0415(3) Uani 1 1 d . . . S3 S 0.03250(15) 0.08957(4) 0.17837(12) 0.0470(3) Uani 1 1 d . . . B B 0.3857(7) 0.0776(2) 0.2967(6) 0.0492(16) Uani 1 1 d . . . H1 H 0.459(4) 0.0612(12) 0.261(4) 0.027(11) Uiso 1 1 d . . . N11 N 0.4716(4) 0.09021(12) 0.4469(4) 0.0435(10) Uani 1 1 d . . . N12 N 0.5560(4) 0.10864(13) 0.6633(4) 0.0467(11) Uani 1 1 d . . . N21 N 0.3266(5) 0.11543(12) 0.2002(4) 0.0448(11) Uani 1 1 d . . . N22 N 0.2246(4) 0.17170(13) 0.0924(4) 0.0444(10) Uani 1 1 d . . . N31 N 0.2742(5) 0.04500(12) 0.2791(4) 0.0472(11) Uani 1 1 d . . . N32 N 0.0918(5) 0.00871(13) 0.2538(4) 0.0494(11) Uani 1 1 d . . . C11 C 0.4467(5) 0.09125(15) 0.5598(5) 0.0426(12) Uani 1 1 d . . . C12 C 0.5996(6) 0.10757(18) 0.4839(6) 0.0576(15) Uani 1 1 d . . . H12A H 0.6438 0.1108 0.4260 0.069 Uiso 1 1 calc R . . C13 C 0.6516(6) 0.11920(17) 0.6149(6) 0.0553(15) Uani 1 1 d . . . H13A H 0.7374 0.1322 0.6648 0.066 Uiso 1 1 calc R . . C14 C 0.5727(6) 0.11857(19) 0.8054(5) 0.0617(16) Uani 1 1 d . . . C15 C 0.7166(7) 0.1370(2) 0.8860(6) 0.091(2) Uani 1 1 d . . . H15A H 0.7866 0.1165 0.8977 0.136 Uiso 1 1 calc R . . H15B H 0.7260 0.1459 0.9751 0.136 Uiso 1 1 calc R . . H15C H 0.7286 0.1603 0.8365 0.136 Uiso 1 1 calc R . . C16 C 0.5627(7) 0.0788(2) 0.8777(5) 0.081(2) Uani 1 1 d . . . H16A H 0.4718 0.0666 0.8277 0.121 Uiso 1 1 calc R . . H16B H 0.5766 0.0851 0.9703 0.121 Uiso 1 1 calc R . . H16C H 0.6335 0.0596 0.8806 0.121 Uiso 1 1 calc R . . C17 C 0.4615(7) 0.14891(19) 0.7943(6) 0.0741(19) Uani 1 1 d . . . H17A H 0.3711 0.1363 0.7466 0.111 Uiso 1 1 calc R . . H17B H 0.4673 0.1729 0.7439 0.111 Uiso 1 1 calc R . . H17C H 0.4748 0.1571 0.8853 0.111 Uiso 1 1 calc R . . C21 C 0.2819(5) 0.15268(15) 0.2165(5) 0.0403(12) Uani 1 1 d . . . C22 C 0.2971(6) 0.11168(18) 0.0643(5) 0.0570(15) Uani 1 1 d . . . H22A H 0.3176 0.0886 0.0243 0.068 Uiso 1 1 calc R . . C23 C 0.2361(6) 0.14501(18) -0.0013(5) 0.0582(16) Uani 1 1 d . . . H23A H 0.2056 0.1499 -0.0954 0.070 Uiso 1 1 calc R . . C24 C 0.1528(6) 0.21331(16) 0.0561(5) 0.0514(14) Uani 1 1 d . . . C25 C 0.0285(6) 0.21274(19) 0.0912(6) 0.0668(17) Uani 1 1 d . . . H25A H -0.0337 0.1906 0.0418 0.100 Uiso 1 1 calc R . . H25B H -0.0204 0.2387 0.0652 0.100 Uiso 1 1 calc R . . H25C H 0.0608 0.2085 0.1889 0.100 Uiso 1 1 calc R . . C26 C 0.1001(8) 0.2201(2) -0.0959(6) 0.089(2) Uani 1 1 d . . . H26A H 0.1775 0.2198 -0.1202 0.134 Uiso 1 1 calc R . . H26B H 0.0533 0.2464 -0.1204 0.134 Uiso 1 1 calc R . . H26C H 0.0355 0.1984 -0.1449 0.134 Uiso 1 1 calc R . . C27 C 0.2539(6) 0.24690(18) 0.1326(6) 0.0683(17) Uani 1 1 d . . . H27A H 0.3317 0.2463 0.1088 0.102 Uiso 1 1 calc R . . H27B H 0.2872 0.2426 0.2303 0.102 Uiso 1 1 calc R . . H27C H 0.2079 0.2733 0.1077 0.102 Uiso 1 1 calc R . . C31 C 0.1359(6) 0.04657(15) 0.2400(5) 0.0448(13) Uani 1 1 d . . . C32 C 0.3151(7) 0.00563(18) 0.3194(5) 0.0633(16) Uani 1 1 d . . . H32A H 0.4066 -0.0041 0.3527 0.076 Uiso 1 1 calc R . . C33 C 0.2067(7) -0.01646(18) 0.3043(6) 0.0649(17) Uani 1 1 d . . . H33A H 0.2074 -0.0446 0.3244 0.078 Uiso 1 1 calc R . . C34 C -0.0534(7) -0.00444(16) 0.2218(5) 0.0569(16) Uani 1 1 d . . . C35 C -0.1112(8) 0.0207(2) 0.3066(7) 0.087(2) Uani 1 1 d . . . H35A H -0.0547 0.0158 0.4033 0.131 Uiso 1 1 calc R . . H35B H -0.2060 0.0123 0.2828 0.131 Uiso 1 1 calc R . . H35C H -0.1092 0.0496 0.2869 0.131 Uiso 1 1 calc R . . C36 C -0.0530(8) -0.04935(18) 0.2596(6) 0.088(2) Uani 1 1 d . . . H36A H 0.0007 -0.0527 0.3576 0.132 Uiso 1 1 calc R . . H36B H -0.0119 -0.0657 0.2117 0.132 Uiso 1 1 calc R . . H36C H -0.1475 -0.0584 0.2337 0.132 Uiso 1 1 calc R . . C37 C -0.1443(6) 0.00028(18) 0.0691(5) 0.0633(16) Uani 1 1 d . . . H37A H -0.1068 -0.0162 0.0183 0.095 Uiso 1 1 calc R . . H37B H -0.1464 0.0289 0.0434 0.095 Uiso 1 1 calc R . . H37C H -0.2377 -0.0088 0.0482 0.095 Uiso 1 1 calc R . . C41 C -0.1796(6) 0.18489(17) 0.3821(6) 0.0558(15) Uani 1 1 d . . . C42 C -0.1875(7) 0.1890(2) 0.2555(6) 0.079(2) Uani 1 1 d . . . H42A H -0.1258 0.1738 0.2325 0.095 Uiso 1 1 calc R . . C43 C -0.2827(8) 0.2145(3) 0.1569(7) 0.104(3) Uani 1 1 d . . . H43A H -0.2850 0.2160 0.0692 0.125 Uiso 1 1 calc R . . C44 C -0.3706(8) 0.2370(3) 0.1859(7) 0.098(3) Uani 1 1 d . . . H44A H -0.4325 0.2552 0.1208 0.117 Uiso 1 1 calc R . . C45 C -0.3690(7) 0.2330(2) 0.3141(7) 0.090(2) Uani 1 1 d . . . H45A H -0.4326 0.2479 0.3352 0.108 Uiso 1 1 calc R . . C46 C -0.2748(7) 0.2074(2) 0.4107(7) 0.0737(19) Uani 1 1 d . . . H46A H -0.2748 0.2050 0.4973 0.088 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 Cd 0.0421(2) 0.0430(2) 0.0446(2) -0.00097(18) 0.02104(18) 0.00106(18) Te 0.0583(3) 0.0731(3) 0.0587(2) 0.0021(2) 0.0356(2) 0.0059(2) S1 0.0478(8) 0.0494(9) 0.0461(7) 0.0085(6) 0.0200(7) -0.0028(7) S2 0.0494(8) 0.0386(8) 0.0394(7) -0.0022(6) 0.0219(6) -0.0029(6) S3 0.0551(9) 0.0360(8) 0.0423(7) 0.0014(6) 0.0138(7) 0.0019(6) B 0.059(4) 0.047(4) 0.045(3) -0.002(3) 0.025(3) 0.014(3) N11 0.035(3) 0.045(3) 0.052(3) 0.005(2) 0.020(2) 0.009(2) N12 0.034(3) 0.050(3) 0.050(3) 0.004(2) 0.012(2) 0.003(2) N21 0.059(3) 0.036(3) 0.048(2) 0.0016(19) 0.031(2) 0.005(2) N22 0.055(3) 0.045(3) 0.035(2) 0.0071(19) 0.022(2) 0.000(2) N31 0.058(3) 0.030(3) 0.047(2) 0.0003(19) 0.016(2) 0.010(2) N32 0.073(3) 0.030(3) 0.036(2) 0.0008(19) 0.015(2) -0.004(2) C11 0.039(3) 0.035(3) 0.048(3) 0.010(2) 0.014(3) 0.008(2) C12 0.049(4) 0.057(4) 0.067(4) 0.018(3) 0.026(3) 0.014(3) C13 0.039(3) 0.059(4) 0.062(4) 0.005(3) 0.015(3) 0.003(3) C14 0.047(4) 0.080(5) 0.049(3) -0.004(3) 0.012(3) 0.008(3) C15 0.059(5) 0.121(6) 0.068(4) -0.023(4) 0.004(4) -0.007(4) C16 0.091(5) 0.094(6) 0.041(3) 0.013(3) 0.014(3) 0.015(4) C17 0.072(5) 0.082(5) 0.058(4) -0.012(3) 0.019(3) 0.010(4) C21 0.046(3) 0.037(3) 0.042(3) -0.001(2) 0.022(2) -0.005(2) C22 0.080(4) 0.055(4) 0.049(3) -0.007(3) 0.040(3) -0.003(3) C23 0.087(5) 0.057(4) 0.040(3) 0.002(3) 0.036(3) 0.002(3) C24 0.062(4) 0.044(3) 0.051(3) 0.013(3) 0.027(3) 0.005(3) C25 0.053(4) 0.064(4) 0.073(4) 0.009(3) 0.017(3) 0.005(3) C26 0.124(7) 0.084(5) 0.057(4) 0.029(4) 0.036(4) 0.027(4) C27 0.073(4) 0.049(4) 0.084(4) 0.010(3) 0.035(4) -0.006(3) C31 0.068(4) 0.030(3) 0.032(3) -0.003(2) 0.018(3) -0.003(3) C32 0.079(5) 0.044(4) 0.052(3) 0.006(3) 0.015(3) 0.012(3) C33 0.096(5) 0.035(3) 0.052(3) 0.002(3) 0.021(4) 0.003(4) C34 0.088(5) 0.041(3) 0.040(3) -0.004(2) 0.027(3) -0.020(3) C35 0.119(6) 0.087(5) 0.083(5) -0.016(4) 0.069(5) -0.026(5) C36 0.142(7) 0.047(4) 0.076(4) 0.003(3) 0.048(5) -0.032(4) C37 0.070(4) 0.062(4) 0.052(3) -0.007(3) 0.021(3) -0.022(3) C41 0.053(4) 0.057(4) 0.063(4) -0.011(3) 0.030(3) -0.005(3) C42 0.065(5) 0.113(6) 0.059(4) 0.014(4) 0.026(4) 0.025(4) C43 0.086(6) 0.170(9) 0.067(5) 0.019(5) 0.043(4) 0.041(6) C44 0.084(6) 0.132(7) 0.079(5) 0.029(5) 0.037(5) 0.037(5) C45 0.074(5) 0.107(6) 0.092(5) 0.004(5) 0.038(5) 0.033(4) C46 0.077(5) 0.082(5) 0.075(4) -0.003(4) 0.045(4) 0.011(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 Cd S2 2.5520(13) . ? Cd S1 2.5687(14) . ? Cd S3 2.5727(13) . ? Cd Te 2.7097(5) . ? Te C41 2.088(6) . ? S1 C11 1.725(5) . ? S2 C21 1.740(5) . ? S3 C31 1.730(5) . ? B H1 1.14(4) . ? B N11 1.540(7) . ? B N31 1.545(8) . ? B N21 1.562(7) . ? N11 C11 1.358(6) . ? N11 C12 1.371(7) . ? N12 C11 1.346(6) . ? N12 C13 1.378(6) . ? N12 C14 1.505(6) . ? N21 C21 1.343(6) . ? N21 C22 1.370(6) . ? N22 C21 1.362(6) . ? N22 C23 1.381(6) . ? N22 C24 1.524(6) . ? N31 C31 1.351(7) . ? N31 C32 1.364(6) . ? N32 C31 1.352(6) . ? N32 C33 1.379(7) . ? N32 C34 1.499(7) . ? C12 C13 1.336(7) . ? C14 C17 1.510(8) . ? C14 C15 1.526(8) . ? C14 C16 1.542(8) . ? C22 C23 1.307(7) . ? C24 C26 1.508(7) . ? C24 C27 1.509(8) . ? C24 C25 1.532(8) . ? C32 C33 1.313(8) . ? C34 C37 1.521(7) . ? C34 C36 1.519(7) . ? C34 C35 1.542(8) . ? C41 C42 1.342(7) . ? C41 C46 1.393(8) . ? C42 C43 1.390(9) . ? C43 C44 1.330(9) . ? C44 C45 1.387(9) . ? C45 C46 1.377(9) . ? 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 S2 Cd S1 100.63(4) . . ? S2 Cd S3 97.12(4) . . ? S1 Cd S3 101.74(4) . . ? S2 Cd Te 124.42(3) . . ? S1 Cd Te 106.49(3) . . ? S3 Cd Te 122.55(4) . . ? C41 Te Cd 100.67(15) . . ? C11 S1 Cd 96.83(16) . . ? C21 S2 Cd 98.34(16) . . ? C31 S3 Cd 94.28(16) . . ? H1 B N11 107.2(19) . . ? H1 B N31 104(2) . . ? N11 B N31 113.0(4) . . ? H1 B N21 106.5(19) . . ? N11 B N21 112.3(5) . . ? N31 B N21 113.1(5) . . ? C11 N11 C12 106.6(4) . . ? C11 N11 B 134.3(5) . . ? C12 N11 B 118.9(5) . . ? C11 N12 C13 108.0(4) . . ? C11 N12 C14 128.3(4) . . ? C13 N12 C14 123.6(5) . . ? C21 N21 C22 107.0(4) . . ? C21 N21 B 133.6(4) . . ? C22 N21 B 119.1(4) . . ? C21 N22 C23 107.1(4) . . ? C21 N22 C24 128.4(4) . . ? C23 N22 C24 124.4(4) . . ? C31 N31 C32 107.0(5) . . ? C31 N31 B 133.9(4) . . ? C32 N31 B 118.9(5) . . ? C31 N32 C33 107.0(5) . . ? C31 N32 C34 127.7(5) . . ? C33 N32 C34 125.3(5) . . ? N12 C11 N11 108.8(4) . . ? N12 C11 S1 126.1(4) . . ? N11 C11 S1 125.0(4) . . ? C13 C12 N11 109.5(5) . . ? C12 C13 N12 107.1(5) . . ? N12 C14 C17 108.5(4) . . ? N12 C14 C15 108.4(5) . . ? C17 C14 C15 110.6(5) . . ? N12 C14 C16 109.5(5) . . ? C17 C14 C16 111.5(5) . . ? C15 C14 C16 108.3(5) . . ? N21 C21 N22 108.4(4) . . ? N21 C21 S2 126.3(4) . . ? N22 C21 S2 125.3(4) . . ? C23 C22 N21 109.8(5) . . ? C22 C23 N22 107.8(4) . . ? C26 C24 C27 109.6(5) . . ? C26 C24 N22 108.7(4) . . ? C27 C24 N22 110.0(5) . . ? C26 C24 C25 108.5(5) . . ? C27 C24 C25 111.4(5) . . ? N22 C24 C25 108.6(4) . . ? N32 C31 N31 108.5(5) . . ? N32 C31 S3 125.9(5) . . ? N31 C31 S3 125.6(4) . . ? C33 C32 N31 109.4(6) . . ? C32 C33 N32 108.1(5) . . ? N32 C34 C37 109.5(4) . . ? N32 C34 C36 109.3(5) . . ? C37 C34 C36 108.4(5) . . ? N32 C34 C35 110.6(4) . . ? C37 C34 C35 111.1(5) . . ? C36 C34 C35 107.8(5) . . ? C42 C41 C46 116.4(6) . . ? C42 C41 Te 124.1(5) . . ? C46 C41 Te 119.4(4) . . ? C41 C42 C43 123.1(6) . . ? C44 C43 C42 120.4(7) . . ? C43 C44 C45 118.7(7) . . ? C46 C45 C44 120.4(7) . . ? C45 C46 C41 121.0(6) . . ? _diffrn_measured_fraction_theta_max 0.939 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.939 _refine_diff_density_max 0.938 _refine_diff_density_min -1.076 _refine_diff_density_rms 0.094 # Attachment 'SANDS10.CIF' data_sands10 _database_code_depnum_ccdc_archive 'CCDC 609901' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H68 B2 Cd N12 S6' _chemical_formula_weight 1067.46 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I4(1)/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 19.7140(8) _cell_length_b 19.7140(8) _cell_length_c 30.1310(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11710.2(9) _cell_formula_units_Z 8 _cell_measurement_temperature 243(2) _cell_measurement_reflns_used 5103 _cell_measurement_theta_min 2.274 _cell_measurement_theta_max 26.483 _exptl_crystal_description COLORLESS _exptl_crystal_colour BLOCK _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.211 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4464 _exptl_absorpt_coefficient_mu 0.625 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.7882 _exptl_absorpt_correction_T_max 0.8347 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 243(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40055 _diffrn_reflns_av_R_equivalents 0.0488 _diffrn_reflns_av_sigmaI/netI 0.0460 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 1.23 _diffrn_reflns_theta_max 28.25 _reflns_number_total 6946 _reflns_number_gt 4703 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1367P)^2^+2.4785P] 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 0.00018(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6946 _refine_ls_number_parameters 290 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0887 _refine_ls_R_factor_gt 0.0566 _refine_ls_wR_factor_ref 0.2122 _refine_ls_wR_factor_gt 0.1937 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.039 _refine_ls_shift/su_mean 0.003 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 Cd Cd 0.0000 0.7500 0.091682(15) 0.03474(18) Uani 1 2 d S . . S1 S -0.08579(6) 0.69795(6) 0.03770(4) 0.0436(3) Uani 1 1 d . . . S2 S 0.04844(5) 0.64878(6) 0.13484(4) 0.0378(3) Uani 1 1 d . . . S3 S -0.23224(7) 0.54454(6) 0.18090(4) 0.0487(3) Uani 1 1 d . . . B B -0.1177(2) 0.6575(2) 0.14003(17) 0.0325(10) Uani 1 1 d . . . H1 H -0.0839(18) 0.6984(18) 0.1436(12) 0.016(9) Uiso 1 1 d . . . N11 N -0.17482(17) 0.67576(18) 0.10649(12) 0.0360(8) Uani 1 1 d . . . N12 N -0.22421(19) 0.71653(19) 0.04634(13) 0.0431(9) Uani 1 1 d . . . N21 N -0.07844(17) 0.59405(17) 0.12254(11) 0.0319(7) Uani 1 1 d . . . N22 N 0.00304(18) 0.53221(18) 0.09356(12) 0.0364(8) Uani 1 1 d . . . N31 N -0.14499(17) 0.65116(16) 0.18776(11) 0.0330(7) Uani 1 1 d . . . N32 N -0.19583(19) 0.62663(19) 0.25128(13) 0.0415(9) Uani 1 1 d . . . C11 C -0.1628(2) 0.6972(2) 0.06435(14) 0.0373(9) Uani 1 1 d . . . C12 C -0.2426(2) 0.6842(3) 0.11543(17) 0.0471(12) Uani 1 1 d . . . H12A H -0.2641 0.6746 0.1425 0.057 Uiso 1 1 calc R . . C13 C -0.2725(2) 0.7084(3) 0.07908(18) 0.0533(13) Uani 1 1 d . . . H13A H -0.3189 0.7184 0.0762 0.064 Uiso 1 1 calc R . . C14 C -0.2369(3) 0.7453(3) 0.00130(17) 0.0529(13) Uani 1 1 d . . . C15 C -0.2013(3) 0.8137(3) -0.0023(2) 0.0648(16) Uani 1 1 d . . . H15A H -0.1527 0.8073 0.0006 0.097 Uiso 1 1 calc R . . H15B H -0.2173 0.8434 0.0212 0.097 Uiso 1 1 calc R . . H15C H -0.2112 0.8340 -0.0309 0.097 Uiso 1 1 calc R . . C16 C -0.3148(3) 0.7550(3) -0.0036(2) 0.0759(19) Uani 1 1 d . . . H16A H -0.3377 0.7129 0.0037 0.114 Uiso 1 1 calc R . . H16B H -0.3254 0.7675 -0.0340 0.114 Uiso 1 1 calc R . . H16C H -0.3300 0.7906 0.0163 0.114 Uiso 1 1 calc R . . C17 C -0.2126(3) 0.6969(3) -0.03437(19) 0.0674(16) Uani 1 1 d . . . H17A H -0.1640 0.6903 -0.0315 0.101 Uiso 1 1 calc R . . H17B H -0.2226 0.7157 -0.0634 0.101 Uiso 1 1 calc R . . H17C H -0.2355 0.6537 -0.0311 0.101 Uiso 1 1 calc R . . C21 C -0.0106(2) 0.5897(2) 0.11631(13) 0.0319(9) Uani 1 1 d . . . C22 C -0.1076(2) 0.5382(2) 0.10240(16) 0.0410(10) Uani 1 1 d . . . H22A H -0.1543 0.5286 0.1012 0.049 Uiso 1 1 calc R . . C23 C -0.0586(2) 0.5001(2) 0.08490(16) 0.0456(11) Uani 1 1 d . . . H23A H -0.0645 0.4591 0.0695 0.055 Uiso 1 1 calc R . . C24 C 0.0715(2) 0.5060(3) 0.07823(17) 0.0469(11) Uani 1 1 d . . . C25 C 0.1046(3) 0.5586(3) 0.0484(2) 0.0661(16) Uani 1 1 d . . . H25A H 0.1110 0.6004 0.0649 0.099 Uiso 1 1 calc R . . H25B H 0.0757 0.5671 0.0230 0.099 Uiso 1 1 calc R . . H25C H 0.1482 0.5418 0.0383 0.099 Uiso 1 1 calc R . . C26 C 0.0617(3) 0.4416(3) 0.0517(2) 0.0716(17) Uani 1 1 d . . . H26A H 0.0344 0.4513 0.0257 0.107 Uiso 1 1 calc R . . H26B H 0.0388 0.4081 0.0699 0.107 Uiso 1 1 calc R . . H26C H 0.1055 0.4241 0.0426 0.107 Uiso 1 1 calc R . . C27 C 0.1142(3) 0.4907(3) 0.11862(19) 0.0605(15) Uani 1 1 d . . . H27A H 0.1208 0.5320 0.1356 0.091 Uiso 1 1 calc R . . H27B H 0.1579 0.4731 0.1093 0.091 Uiso 1 1 calc R . . H27C H 0.0913 0.4573 0.1369 0.091 Uiso 1 1 calc R . . C31 C -0.1906(2) 0.6075(2) 0.20714(14) 0.0347(9) Uani 1 1 d . . . C32 C -0.1232(2) 0.6974(2) 0.21935(15) 0.0414(10) Uani 1 1 d . . . H32A H -0.0921 0.7328 0.2147 0.050 Uiso 1 1 calc R . . C33 C -0.1546(3) 0.6827(3) 0.25781(17) 0.0509(12) Uani 1 1 d . . . H33A H -0.1494 0.7065 0.2846 0.061 Uiso 1 1 calc R . . C34 C -0.2440(3) 0.5987(3) 0.28472(16) 0.0493(12) Uani 1 1 d . . . C35 C -0.2330(4) 0.6348(4) 0.3292(2) 0.083(2) Uani 1 1 d . . . H35A H -0.2413 0.6830 0.3256 0.124 Uiso 1 1 calc R . . H35B H -0.1867 0.6278 0.3390 0.124 Uiso 1 1 calc R . . H35C H -0.2641 0.6166 0.3511 0.124 Uiso 1 1 calc R . . C36 C -0.3160(3) 0.6117(3) 0.2690(2) 0.0665(16) Uani 1 1 d . . . H36A H -0.3229 0.6601 0.2652 0.100 Uiso 1 1 calc R . . H36B H -0.3478 0.5946 0.2909 0.100 Uiso 1 1 calc R . . H36C H -0.3234 0.5888 0.2409 0.100 Uiso 1 1 calc R . . C37 C -0.2309(3) 0.5234(3) 0.2914(2) 0.0611(14) Uani 1 1 d . . . H37A H -0.2366 0.4999 0.2633 0.092 Uiso 1 1 calc R . . H37B H -0.2629 0.5055 0.3129 0.092 Uiso 1 1 calc R . . H37C H -0.1851 0.5168 0.3021 0.092 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 Cd 0.0366(3) 0.0323(3) 0.0352(3) 0.000 0.000 -0.00336(17) S1 0.0437(6) 0.0556(7) 0.0315(6) -0.0017(5) -0.0040(5) -0.0058(5) S2 0.0320(5) 0.0363(6) 0.0450(6) 0.0029(5) -0.0075(4) -0.0032(4) S3 0.0530(7) 0.0424(6) 0.0508(7) -0.0057(5) 0.0043(6) -0.0164(5) B 0.033(2) 0.030(2) 0.034(2) 0.0039(19) 0.0000(19) 0.0000(18) N11 0.0339(18) 0.0382(19) 0.0360(19) 0.0039(15) -0.0039(15) 0.0014(14) N12 0.041(2) 0.040(2) 0.048(2) 0.0074(17) -0.0134(18) -0.0014(15) N21 0.0303(17) 0.0319(17) 0.0336(18) -0.0006(14) -0.0030(14) -0.0022(13) N22 0.0381(19) 0.0357(19) 0.0354(19) -0.0037(15) 0.0001(15) 0.0008(15) N31 0.0332(18) 0.0307(17) 0.0350(19) -0.0016(14) 0.0003(14) -0.0012(13) N32 0.044(2) 0.043(2) 0.038(2) -0.0022(16) 0.0078(16) -0.0064(16) C11 0.039(2) 0.035(2) 0.038(2) -0.0024(18) -0.0101(18) -0.0023(17) C12 0.034(2) 0.051(3) 0.056(3) 0.010(2) 0.002(2) 0.008(2) C13 0.035(2) 0.058(3) 0.066(3) 0.013(3) -0.006(2) 0.006(2) C14 0.062(3) 0.047(3) 0.049(3) 0.006(2) -0.027(2) -0.007(2) C15 0.079(4) 0.049(3) 0.066(4) 0.015(3) -0.027(3) -0.015(3) C16 0.072(4) 0.070(4) 0.086(5) 0.021(3) -0.049(4) -0.005(3) C17 0.086(4) 0.065(4) 0.051(3) -0.002(3) -0.031(3) -0.007(3) C21 0.034(2) 0.030(2) 0.031(2) 0.0020(16) -0.0029(16) 0.0004(15) C22 0.034(2) 0.040(2) 0.050(3) -0.005(2) -0.0073(19) -0.0037(18) C23 0.047(3) 0.039(2) 0.050(3) -0.012(2) -0.003(2) -0.004(2) C24 0.045(3) 0.048(3) 0.048(3) -0.006(2) 0.007(2) 0.007(2) C25 0.066(4) 0.074(4) 0.058(3) 0.006(3) 0.027(3) 0.005(3) C26 0.067(4) 0.065(4) 0.082(4) -0.027(3) 0.016(3) 0.012(3) C27 0.045(3) 0.071(4) 0.065(4) 0.005(3) 0.002(2) 0.021(3) C31 0.035(2) 0.030(2) 0.040(2) 0.0009(17) 0.0021(17) -0.0016(16) C32 0.043(2) 0.036(2) 0.045(3) -0.0079(19) 0.001(2) -0.0080(18) C33 0.057(3) 0.055(3) 0.041(3) -0.014(2) 0.002(2) -0.012(2) C34 0.054(3) 0.051(3) 0.043(3) 0.003(2) 0.013(2) -0.006(2) C35 0.104(5) 0.096(5) 0.048(3) -0.007(3) 0.027(3) -0.032(4) C36 0.052(3) 0.066(4) 0.081(4) 0.010(3) 0.020(3) 0.010(3) C37 0.062(3) 0.060(3) 0.062(4) 0.016(3) 0.012(3) 0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd S1 2.5610(12) . ? Cd S1 2.5610(12) 6_464 ? Cd S2 2.5662(11) 6_464 ? Cd S2 2.5662(11) . ? S1 C11 1.717(5) . ? S2 C21 1.738(4) . ? S3 C31 1.686(4) . ? B N31 1.541(6) . ? B N11 1.555(6) . ? B N21 1.563(6) . ? N11 C11 1.359(6) . ? N11 C12 1.373(6) . ? N12 C13 1.380(6) . ? N12 C11 1.381(5) . ? N12 C14 1.492(6) . ? N21 C21 1.353(5) . ? N21 C22 1.383(5) . ? N22 C21 1.352(5) . ? N22 C23 1.395(6) . ? N22 C24 1.518(6) . ? N31 C31 1.374(5) . ? N31 C32 1.386(5) . ? N32 C33 1.387(6) . ? N32 C31 1.386(6) . ? N32 C34 1.489(6) . ? C12 C13 1.332(7) . ? C14 C17 1.516(8) . ? C14 C15 1.524(7) . ? C14 C16 1.554(8) . ? C22 C23 1.332(6) . ? C24 C27 1.510(7) . ? C24 C26 1.512(7) . ? C24 C25 1.518(7) . ? C32 C33 1.345(7) . ? C34 C37 1.520(7) . ? C34 C36 1.519(7) . ? C34 C35 1.532(8) . ? 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 S1 Cd S1 101.15(6) . 6_464 ? S1 Cd S2 112.81(4) . 6_464 ? S1 Cd S2 104.84(4) 6_464 6_464 ? S1 Cd S2 104.84(4) . . ? S1 Cd S2 112.81(4) 6_464 . ? S2 Cd S2 119.10(6) 6_464 . ? C11 S1 Cd 106.86(14) . . ? C21 S2 Cd 96.24(14) . . ? N31 B N11 111.9(3) . . ? N31 B N21 115.0(3) . . ? N11 B N21 108.9(4) . . ? C11 N11 C12 108.4(4) . . ? C11 N11 B 123.5(4) . . ? C12 N11 B 127.2(4) . . ? C13 N12 C11 107.0(4) . . ? C13 N12 C14 125.3(4) . . ? C11 N12 C14 127.6(4) . . ? C21 N21 C22 107.5(3) . . ? C21 N21 B 125.9(3) . . ? C22 N21 B 125.4(3) . . ? C21 N22 C23 107.5(4) . . ? C21 N22 C24 128.1(4) . . ? C23 N22 C24 124.4(4) . . ? C31 N31 C32 108.8(3) . . ? C31 N31 B 132.5(3) . . ? C32 N31 B 118.6(3) . . ? C33 N32 C31 108.0(4) . . ? C33 N32 C34 124.9(4) . . ? C31 N32 C34 126.6(4) . . ? N11 C11 N12 107.4(4) . . ? N11 C11 S1 126.4(3) . . ? N12 C11 S1 126.1(3) . . ? C13 C12 N11 108.2(4) . . ? C12 C13 N12 108.9(4) . . ? N12 C14 C17 110.6(4) . . ? N12 C14 C15 108.8(4) . . ? C17 C14 C15 111.2(5) . . ? N12 C14 C16 107.4(5) . . ? C17 C14 C16 108.8(4) . . ? C15 C14 C16 109.9(5) . . ? N22 C21 N21 108.6(3) . . ? N22 C21 S2 126.2(3) . . ? N21 C21 S2 125.1(3) . . ? C23 C22 N21 108.7(4) . . ? C22 C23 N22 107.6(4) . . ? C27 C24 C26 109.2(5) . . ? C27 C24 N22 108.6(4) . . ? C26 C24 N22 109.4(4) . . ? C27 C24 C25 112.0(5) . . ? C26 C24 C25 108.4(5) . . ? N22 C24 C25 109.3(4) . . ? N31 C31 N32 106.7(3) . . ? N31 C31 S3 125.5(3) . . ? N32 C31 S3 127.8(3) . . ? C33 C32 N31 107.9(4) . . ? C32 C33 N32 108.6(4) . . ? N32 C34 C37 110.0(4) . . ? N32 C34 C36 108.8(4) . . ? C37 C34 C36 111.3(5) . . ? N32 C34 C35 109.3(4) . . ? C37 C34 C35 108.4(5) . . ? C36 C34 C35 109.0(5) . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 28.25 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 2.534 _refine_diff_density_min -0.330 _refine_diff_density_rms 0.151 # Attachment 'TMMES10.CIF' data_tmmes10 _database_code_depnum_ccdc_archive 'CCDC 609902' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H42 B Cd N6 O0.50 S3' _chemical_formula_weight 642.03 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 '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 10.8046(7) _cell_length_b 12.3830(8) _cell_length_c 14.3266(9) _cell_angle_alpha 89.9760(10) _cell_angle_beta 69.6970(10) _cell_angle_gamma 64.5050(10) _cell_volume 1597.35(18) _cell_formula_units_Z 2 _cell_measurement_temperature 243(2) _cell_measurement_reflns_used 5089 _cell_measurement_theta_min 2.575 _cell_measurement_theta_max 27.686 _exptl_crystal_description COLORLESS _exptl_crystal_colour BLOCK _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.335 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 666 _exptl_absorpt_coefficient_mu 0.904 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.7138 _exptl_absorpt_correction_T_max 0.7732 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 243(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10843 _diffrn_reflns_av_R_equivalents 0.0170 _diffrn_reflns_av_sigmaI/netI 0.0304 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 28.12 _reflns_number_total 6931 _reflns_number_gt 5352 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0462P)^2^+0.0000P] 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 0.0014(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6931 _refine_ls_number_parameters 360 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0470 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0839 _refine_ls_wR_factor_gt 0.0785 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 4.034 _refine_ls_shift/su_mean 0.083 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 Cd Cd 0.90200(2) 0.793143(17) 0.215516(14) 0.05417(9) Uani 1 1 d . . . C1 C 0.7402(5) 0.8904(5) 0.1519(3) 0.0971(16) Uani 1 1 d . . . H1A H 0.683(5) 0.970(4) 0.184(3) 0.110(14) Uiso 1 1 d . . . H1B H 0.785(5) 0.888(4) 0.084(4) 0.132(16) Uiso 1 1 d . . . H1C H 0.684(5) 0.844(4) 0.165(3) 0.120(19) Uiso 1 1 d . . . S1 S 1.12268(9) 0.57878(6) 0.12056(5) 0.05972(19) Uani 1 1 d . . . S2 S 0.82387(7) 0.73328(6) 0.39418(5) 0.04808(15) Uani 1 1 d . . . S3 S 1.06969(8) 0.88058(6) 0.24300(5) 0.05363(17) Uani 1 1 d . . . B B 1.2037(3) 0.6088(3) 0.3292(2) 0.0503(7) Uani 1 1 d . . . H1 H 1.283(3) 0.556(2) 0.3597(17) 0.045(6) Uiso 1 1 d . . . N11 N 1.1512(2) 0.51941(18) 0.29927(15) 0.0493(5) Uani 1 1 d . . . N12 N 1.0528(3) 0.42453(19) 0.24310(16) 0.0585(6) Uani 1 1 d . . . N21 N 1.0748(2) 0.71513(18) 0.41638(14) 0.0442(4) Uani 1 1 d . . . N22 N 0.8689(2) 0.86492(18) 0.52355(14) 0.0440(4) Uani 1 1 d . . . N31 N 1.2842(2) 0.65392(19) 0.23819(16) 0.0550(5) Uani 1 1 d . . . N32 N 1.3549(3) 0.7338(2) 0.10537(18) 0.0654(6) Uani 1 1 d . . . C11 C 1.1079(3) 0.5067(2) 0.22377(18) 0.0519(6) Uani 1 1 d . . . C12 C 1.1236(3) 0.4442(2) 0.3662(2) 0.0576(7) Uani 1 1 d . . . H12A H 1.1435 0.4356 0.4254 0.069 Uiso 1 1 calc R . . C13 C 1.0642(4) 0.3862(3) 0.3329(2) 0.0641(8) Uani 1 1 d . . . H13A H 1.0351 0.3295 0.3641 0.077 Uiso 1 1 calc R . . C14 C 0.9814(4) 0.3861(3) 0.1850(2) 0.0745(9) Uani 1 1 d . . . C15 C 0.9383(5) 0.2918(4) 0.2356(3) 0.1092(15) Uani 1 1 d . . . H15A H 0.8687 0.3274 0.3048 0.164 Uiso 1 1 calc R . . H15B H 1.0265 0.2221 0.2351 0.164 Uiso 1 1 calc R . . H15C H 0.8924 0.2662 0.1988 0.164 Uiso 1 1 calc R . . C16 C 1.0905(5) 0.3284(3) 0.0768(3) 0.0999(13) Uani 1 1 d . . . H16A H 1.1776 0.2580 0.0770 0.150 Uiso 1 1 calc R . . H16B H 1.1197 0.3869 0.0440 0.150 Uiso 1 1 calc R . . H16C H 1.0437 0.3033 0.0404 0.150 Uiso 1 1 calc R . . C17 C 0.8419(4) 0.4969(3) 0.1883(3) 0.0902(11) Uani 1 1 d . . . H17A H 0.7741 0.5314 0.2580 0.135 Uiso 1 1 calc R . . H17B H 0.7941 0.4726 0.1523 0.135 Uiso 1 1 calc R . . H17C H 0.8689 0.5570 0.1565 0.135 Uiso 1 1 calc R . . C21 C 0.9249(3) 0.7725(2) 0.44530(17) 0.0415(5) Uani 1 1 d . . . C22 C 1.1102(3) 0.7731(2) 0.47794(19) 0.0506(6) Uani 1 1 d . . . H22A H 1.2066 0.7512 0.4747 0.061 Uiso 1 1 calc R . . C23 C 0.9863(3) 0.8649(2) 0.54262(19) 0.0504(6) Uani 1 1 d . . . H23A H 0.9797 0.9194 0.5919 0.060 Uiso 1 1 calc R . . C24 C 0.7085(3) 0.9570(2) 0.5788(2) 0.0551(6) Uani 1 1 d . . . C25 C 0.6175(3) 0.8907(3) 0.6262(2) 0.0668(8) Uani 1 1 d . . . H25A H 0.6228 0.8380 0.5733 0.100 Uiso 1 1 calc R . . H25B H 0.5149 0.9497 0.6635 0.100 Uiso 1 1 calc R . . H25C H 0.6571 0.8424 0.6718 0.100 Uiso 1 1 calc R . . C26 C 0.6980(4) 1.0403(3) 0.6631(3) 0.0799(9) Uani 1 1 d . . . H26A H 0.7560 1.0826 0.6339 0.120 Uiso 1 1 calc R . . H26B H 0.7364 0.9921 0.7092 0.120 Uiso 1 1 calc R . . H26C H 0.5951 1.0992 0.6997 0.120 Uiso 1 1 calc R . . C27 C 0.6557(4) 1.0329(3) 0.5035(3) 0.0720(8) Uani 1 1 d . . . H27A H 0.7172 1.0727 0.4756 0.108 Uiso 1 1 calc R . . H27B H 0.5531 1.0938 0.5378 0.108 Uiso 1 1 calc R . . H27C H 0.6633 0.9805 0.4494 0.108 Uiso 1 1 calc R . . C31 C 1.2395(3) 0.7526(2) 0.19350(19) 0.0530(6) Uani 1 1 d . . . C32 C 1.4296(3) 0.5744(3) 0.1773(2) 0.0760(9) Uani 1 1 d . . . H32A H 1.4884 0.4992 0.1908 0.091 Uiso 1 1 calc R . . C33 C 1.4720(4) 0.6220(3) 0.0967(3) 0.0884(11) Uani 1 1 d . . . H33A H 1.5654 0.5861 0.0430 0.106 Uiso 1 1 calc R . . C34 C 1.3550(4) 0.8130(3) 0.0247(2) 0.0741(9) Uani 1 1 d . . . C35 C 1.2349(5) 0.8250(4) -0.0127(3) 0.0902(11) Uani 1 1 d . . . H35A H 1.2548 0.7451 -0.0404 0.135 Uiso 1 1 calc R . . H35B H 1.2343 0.8751 -0.0648 0.135 Uiso 1 1 calc R . . H35C H 1.1390 0.8626 0.0431 0.135 Uiso 1 1 calc R . . C36 C 1.3319(4) 0.9357(3) 0.0683(2) 0.0824(10) Uani 1 1 d . . . H36A H 1.4115 0.9236 0.0905 0.124 Uiso 1 1 calc R . . H36B H 1.2374 0.9750 0.1254 0.124 Uiso 1 1 calc R . . H36C H 1.3321 0.9865 0.0168 0.124 Uiso 1 1 calc R . . C37 C 1.5069(5) 0.7515(4) -0.0637(3) 0.1168(16) Uani 1 1 d . . . H37A H 1.5838 0.7446 -0.0404 0.175 Uiso 1 1 calc R . . H37B H 1.5067 0.7999 -0.1169 0.175 Uiso 1 1 calc R . . H37C H 1.5260 0.6711 -0.0896 0.175 Uiso 1 1 calc R . . O O 0.5772(7) 0.4191(5) 0.4170(5) 0.1067(17) Uani 0.50 1 d PD A -1 C101 C 0.6323(13) 0.2408(11) 0.3160(8) 0.153(5) Uani 0.50 1 d PD A -1 H10A H 0.6037 0.1764 0.3163 0.229 Uiso 0.50 1 calc PR A -1 H10B H 0.7357 0.2060 0.3078 0.229 Uiso 0.50 1 calc PR A -1 H10C H 0.6194 0.2830 0.2604 0.229 Uiso 0.50 1 calc PR A -1 C102 C 0.5370(10) 0.3286(7) 0.4139(8) 0.097(3) Uani 0.50 1 d PD A -1 H10D H 0.4328 0.3645 0.4217 0.116 Uiso 0.50 1 calc PR A -1 H10E H 0.5468 0.2851 0.4701 0.116 Uiso 0.50 1 calc PR A -1 C103 C 0.494(7) 0.504(5) 0.507(4) 0.118(5) Uani 0.50 1 d PD A -1 H10F H 0.5112 0.4649 0.5634 0.141 Uiso 0.50 1 calc PR A -1 H10G H 0.3875 0.5376 0.5200 0.141 Uiso 0.50 1 calc PR A -1 C104 C 0.5377(13) 0.6063(9) 0.4974(9) 0.132(4) Uani 0.50 1 d PD A -1 H10H H 0.4816 0.6642 0.5604 0.198 Uiso 0.50 1 calc PR A -1 H10I H 0.5165 0.6471 0.4429 0.198 Uiso 0.50 1 calc PR A -1 H10J H 0.6430 0.5728 0.4831 0.198 Uiso 0.50 1 calc PR A -1 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 Cd 0.05581(14) 0.05584(13) 0.04710(13) 0.01083(9) -0.02494(10) -0.01835(10) C1 0.081(3) 0.098(3) 0.056(2) -0.001(2) -0.032(2) 0.012(3) S1 0.0716(5) 0.0530(4) 0.0365(3) 0.0082(3) -0.0181(3) -0.0151(3) S2 0.0487(4) 0.0616(4) 0.0407(3) 0.0056(3) -0.0198(3) -0.0291(3) S3 0.0507(4) 0.0480(3) 0.0546(4) 0.0094(3) -0.0176(3) -0.0182(3) B 0.0480(17) 0.0530(16) 0.0460(16) 0.0136(13) -0.0189(14) -0.0191(14) N11 0.0561(13) 0.0475(11) 0.0398(11) 0.0104(9) -0.0207(10) -0.0181(10) N12 0.0767(16) 0.0500(12) 0.0498(13) 0.0070(10) -0.0309(12) -0.0247(12) N21 0.0428(11) 0.0528(11) 0.0425(11) 0.0126(9) -0.0204(9) -0.0234(9) N22 0.0469(11) 0.0502(11) 0.0403(11) 0.0078(9) -0.0175(9) -0.0262(10) N31 0.0423(12) 0.0563(12) 0.0522(13) 0.0136(10) -0.0115(10) -0.0155(10) N32 0.0521(14) 0.0629(14) 0.0568(14) 0.0157(11) -0.0037(11) -0.0186(12) C11 0.0582(16) 0.0433(13) 0.0408(13) 0.0037(10) -0.0164(12) -0.0137(12) C12 0.0758(19) 0.0523(15) 0.0482(15) 0.0168(12) -0.0297(14) -0.0277(14) C13 0.091(2) 0.0552(15) 0.0542(16) 0.0211(13) -0.0341(16) -0.0361(16) C14 0.108(3) 0.0631(18) 0.067(2) 0.0078(15) -0.0494(19) -0.0392(18) C15 0.177(4) 0.102(3) 0.115(3) 0.031(2) -0.092(3) -0.093(3) C16 0.140(4) 0.079(2) 0.077(2) -0.0116(19) -0.054(2) -0.036(2) C17 0.096(3) 0.095(3) 0.096(3) 0.017(2) -0.055(2) -0.045(2) C21 0.0460(13) 0.0479(13) 0.0364(12) 0.0130(10) -0.0180(10) -0.0247(11) C22 0.0504(15) 0.0615(15) 0.0550(15) 0.0184(13) -0.0282(13) -0.0324(13) C23 0.0613(17) 0.0579(15) 0.0522(15) 0.0152(12) -0.0308(13) -0.0377(14) C24 0.0481(15) 0.0560(15) 0.0546(16) -0.0008(12) -0.0163(12) -0.0209(12) C25 0.0540(17) 0.083(2) 0.0519(16) -0.0039(14) -0.0040(13) -0.0340(16) C26 0.067(2) 0.079(2) 0.077(2) -0.0186(17) -0.0185(17) -0.0269(17) C27 0.0637(19) 0.0573(16) 0.092(2) 0.0112(16) -0.0370(17) -0.0196(14) C31 0.0503(15) 0.0551(14) 0.0454(14) 0.0093(11) -0.0127(12) -0.0216(12) C32 0.0465(17) 0.0728(19) 0.075(2) 0.0215(16) -0.0077(15) -0.0104(15) C33 0.0560(19) 0.081(2) 0.078(2) 0.0205(18) 0.0035(17) -0.0105(17) C34 0.080(2) 0.078(2) 0.0519(17) 0.0209(15) -0.0124(16) -0.0354(17) C35 0.124(3) 0.106(3) 0.0574(19) 0.0272(19) -0.038(2) -0.065(3) C36 0.105(3) 0.088(2) 0.065(2) 0.0318(18) -0.0281(19) -0.057(2) C37 0.104(3) 0.118(3) 0.071(2) 0.028(2) 0.014(2) -0.039(3) O 0.098(4) 0.110(4) 0.125(5) 0.021(4) -0.037(4) -0.062(4) C101 0.196(12) 0.193(11) 0.120(8) 0.019(8) -0.030(8) -0.157(11) C102 0.093(6) 0.083(5) 0.148(8) 0.050(6) -0.062(6) -0.057(5) C103 0.13(2) 0.111(12) 0.116(12) 0.025(8) -0.057(10) -0.050(14) C104 0.147(10) 0.097(7) 0.158(10) 0.018(7) -0.060(9) -0.060(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 Cd C1 2.152(4) . ? Cd S3 2.6066(7) . ? Cd S2 2.6175(6) . ? Cd S1 2.6240(7) . ? S1 C11 1.722(2) . ? S2 C21 1.724(2) . ? S3 C31 1.725(3) . ? B N31 1.549(3) . ? B N21 1.564(4) . ? B N11 1.563(4) . ? N11 C11 1.352(3) . ? N11 C12 1.384(3) . ? N12 C11 1.369(3) . ? N12 C13 1.398(3) . ? N12 C14 1.509(4) . ? N21 C21 1.358(3) . ? N21 C22 1.382(3) . ? N22 C21 1.367(3) . ? N22 C23 1.387(3) . ? N22 C24 1.510(3) . ? N31 C31 1.357(3) . ? N31 C32 1.385(3) . ? N32 C31 1.364(3) . ? N32 C33 1.385(4) . ? N32 C34 1.515(3) . ? C12 C13 1.328(4) . ? C14 C16 1.520(5) . ? C14 C15 1.529(5) . ? C14 C17 1.525(5) . ? C22 C23 1.331(4) . ? C24 C25 1.527(4) . ? C24 C26 1.530(4) . ? C24 C27 1.528(4) . ? C32 C33 1.325(4) . ? C34 C35 1.521(5) . ? C34 C36 1.525(5) . ? C34 C37 1.536(5) . ? O C102 1.372(9) . ? O C103 1.40(2) . ? C101 C102 1.498(12) . ? C103 C104 1.52(2) . ? 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 C1 Cd S3 121.25(19) . . ? C1 Cd S2 121.17(15) . . ? S3 Cd S2 96.74(2) . . ? C1 Cd S1 119.96(13) . . ? S3 Cd S1 94.85(2) . . ? S2 Cd S1 96.77(2) . . ? C11 S1 Cd 96.86(8) . . ? C21 S2 Cd 100.52(8) . . ? C31 S3 Cd 99.63(10) . . ? N31 B N21 112.8(2) . . ? N31 B N11 113.7(2) . . ? N21 B N11 111.6(2) . . ? C11 N11 C12 108.2(2) . . ? C11 N11 B 133.3(2) . . ? C12 N11 B 118.0(2) . . ? C11 N12 C13 107.6(2) . . ? C11 N12 C14 128.0(2) . . ? C13 N12 C14 124.2(2) . . ? C21 N21 C22 107.6(2) . . ? C21 N21 B 133.5(2) . . ? C22 N21 B 118.8(2) . . ? C21 N22 C23 108.5(2) . . ? C21 N22 C24 127.3(2) . . ? C23 N22 C24 124.2(2) . . ? C31 N31 C32 107.8(2) . . ? C31 N31 B 134.1(2) . . ? C32 N31 B 117.5(2) . . ? C31 N32 C33 107.9(2) . . ? C31 N32 C34 127.5(2) . . ? C33 N32 C34 124.4(2) . . ? N11 C11 N12 107.7(2) . . ? N11 C11 S1 126.2(2) . . ? N12 C11 S1 126.1(2) . . ? C13 C12 N11 108.7(2) . . ? C12 C13 N12 107.8(2) . . ? N12 C14 C16 110.2(3) . . ? N12 C14 C15 108.6(2) . . ? C16 C14 C15 108.5(3) . . ? N12 C14 C17 108.9(3) . . ? C16 C14 C17 111.2(3) . . ? C15 C14 C17 109.3(3) . . ? N21 C21 N22 107.5(2) . . ? N21 C21 S2 126.09(18) . . ? N22 C21 S2 126.44(18) . . ? C23 C22 N21 109.3(2) . . ? C22 C23 N22 107.1(2) . . ? N22 C24 C25 109.2(2) . . ? N22 C24 C26 108.8(2) . . ? C25 C24 C26 108.8(2) . . ? N22 C24 C27 108.1(2) . . ? C25 C24 C27 112.8(2) . . ? C26 C24 C27 109.0(2) . . ? N31 C31 N32 107.6(2) . . ? N31 C31 S3 125.60(19) . . ? N32 C31 S3 126.74(19) . . ? C33 C32 N31 108.5(3) . . ? C32 C33 N32 108.2(3) . . ? N32 C34 C35 108.6(3) . . ? N32 C34 C36 109.3(3) . . ? C35 C34 C36 112.4(3) . . ? N32 C34 C37 108.9(3) . . ? C35 C34 C37 109.2(3) . . ? C36 C34 C37 108.4(3) . . ? C102 O C103 114.3(14) . . ? O C102 C101 111.0(7) . . ? O C103 C104 109.5(19) . . ? _diffrn_measured_fraction_theta_max 0.887 _diffrn_reflns_theta_full 28.12 _diffrn_measured_fraction_theta_full 0.887 _refine_diff_density_max 0.646 _refine_diff_density_min -0.421 _refine_diff_density_rms 0.049 # Attachment 'TMSPHS10.CIF' data_tmsphs10 _database_code_depnum_ccdc_archive 'CCDC 609903' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H39 B Cd N6 S4' _chemical_formula_weight 699.09 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 '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 10.2408(7) _cell_length_b 32.833(2) _cell_length_c 10.4732(7) _cell_angle_alpha 90.00 _cell_angle_beta 112.1490(10) _cell_angle_gamma 90.00 _cell_volume 3261.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 243(2) _cell_measurement_reflns_used 4842 _cell_measurement_theta_min 2.644 _cell_measurement_theta_max 25.220 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.424 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1440 _exptl_absorpt_coefficient_mu 0.953 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.7018 _exptl_absorpt_correction_T_max 0.7018 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 243(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22238 _diffrn_reflns_av_R_equivalents 0.0289 _diffrn_reflns_av_sigmaI/netI 0.0324 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 41 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 28.31 _reflns_number_total 7468 _reflns_number_gt 5777 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0416P)^2^+0.0000P] 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 0.00034(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7468 _refine_ls_number_parameters 357 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0467 _refine_ls_R_factor_gt 0.0312 _refine_ls_wR_factor_ref 0.0766 _refine_ls_wR_factor_gt 0.0721 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.023 _refine_ls_shift/su_mean 0.002 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 Cd Cd 0.144828(16) 0.126673(5) -0.075233(17) 0.04032(7) Uani 1 1 d . . . S1 S 0.03747(6) 0.089906(18) -0.30942(6) 0.04541(15) Uani 1 1 d . . . S2 S 0.31463(6) 0.172946(17) -0.13414(6) 0.04066(14) Uani 1 1 d . . . S3 S 0.31751(6) 0.073676(19) 0.07719(6) 0.04438(15) Uani 1 1 d . . . S4 S -0.00018(8) 0.15190(2) 0.04921(7) 0.05885(18) Uani 1 1 d . . . B B 0.3968(3) 0.07662(9) -0.2156(3) 0.0457(6) Uani 1 1 d . . . H1 H 0.471(2) 0.0612(7) -0.261(2) 0.048(6) Uiso 1 1 d . . . N11 N 0.2817(2) 0.04487(6) -0.22210(19) 0.0448(5) Uani 1 1 d . . . N12 N 0.0937(2) 0.00908(6) -0.23888(19) 0.0456(5) Uani 1 1 d . . . N21 N 0.3357(2) 0.11382(6) -0.31169(19) 0.0432(5) Uani 1 1 d . . . N22 N 0.2340(2) 0.16981(6) -0.41672(19) 0.0440(5) Uani 1 1 d . . . N31 N 0.48869(18) 0.08946(6) -0.0658(2) 0.0408(4) Uani 1 1 d . . . N32 N 0.57914(18) 0.10953(6) 0.1502(2) 0.0423(4) Uani 1 1 d . . . C11 C 0.1403(2) 0.04687(7) -0.2555(2) 0.0411(5) Uani 1 1 d . . . C12 C 0.3227(3) 0.00503(7) -0.1832(3) 0.0557(7) Uani 1 1 d . . . H12A H 0.4153 -0.0050 -0.1546 0.067 Uiso 1 1 calc R . . C13 C 0.2099(3) -0.01663(8) -0.1930(3) 0.0564(7) Uani 1 1 d . . . H13A H 0.2089 -0.0445 -0.1724 0.068 Uiso 1 1 calc R . . C14 C -0.0568(3) -0.00425(7) -0.2706(2) 0.0497(6) Uani 1 1 d . . . C15 C -0.1209(4) 0.02066(10) -0.1838(3) 0.0721(8) Uani 1 1 d . . . H15A H -0.1211 0.0493 -0.2064 0.108 Uiso 1 1 calc R . . H15B H -0.0651 0.0166 -0.0867 0.108 Uiso 1 1 calc R . . H15C H -0.2169 0.0117 -0.2039 0.108 Uiso 1 1 calc R . . C16 C -0.0565(3) -0.04938(8) -0.2340(3) 0.0667(8) Uani 1 1 d . . . H16A H -0.0148 -0.0652 -0.2872 0.100 Uiso 1 1 calc R . . H16B H -0.1526 -0.0584 -0.2552 0.100 Uiso 1 1 calc R . . H16C H -0.0020 -0.0531 -0.1364 0.100 Uiso 1 1 calc R . . C17 C -0.1415(3) 0.00097(9) -0.4238(2) 0.0599(7) Uani 1 1 d . . . H17A H -0.0978 -0.0145 -0.4758 0.090 Uiso 1 1 calc R . . H17B H -0.1440 0.0296 -0.4480 0.090 Uiso 1 1 calc R . . H17C H -0.2369 -0.0088 -0.4455 0.090 Uiso 1 1 calc R . . C21 C 0.2933(2) 0.15153(7) -0.2920(2) 0.0388(5) Uani 1 1 d . . . C22 C 0.3024(3) 0.10912(9) -0.4509(3) 0.0554(6) Uani 1 1 d . . . H22A H 0.3213 0.0859 -0.4933 0.067 Uiso 1 1 calc R . . C23 C 0.2392(3) 0.14261(9) -0.5159(3) 0.0550(7) Uani 1 1 d . . . H23A H 0.2044 0.1471 -0.6116 0.066 Uiso 1 1 calc R . . C24 C 0.1614(3) 0.21100(8) -0.4492(3) 0.0503(6) Uani 1 1 d . . . C25 C 0.1004(4) 0.21712(11) -0.6049(3) 0.0828(10) Uani 1 1 d . . . H25A H 0.1762 0.2174 -0.6390 0.124 Uiso 1 1 calc R . . H25B H 0.0501 0.2428 -0.6266 0.124 Uiso 1 1 calc R . . H25C H 0.0359 0.1950 -0.6481 0.124 Uiso 1 1 calc R . . C26 C 0.2672(3) 0.24452(8) -0.3821(4) 0.0702(8) Uani 1 1 d . . . H26A H 0.3425 0.2436 -0.4168 0.105 Uiso 1 1 calc R . . H26B H 0.3061 0.2406 -0.2830 0.105 Uiso 1 1 calc R . . H26C H 0.2204 0.2708 -0.4036 0.105 Uiso 1 1 calc R . . C27 C 0.0398(3) 0.21085(9) -0.3990(3) 0.0653(8) Uani 1 1 d . . . H27A H 0.0764 0.2070 -0.2999 0.098 Uiso 1 1 calc R . . H27B H -0.0245 0.1889 -0.4434 0.098 Uiso 1 1 calc R . . H27C H -0.0099 0.2366 -0.4219 0.098 Uiso 1 1 calc R . . C31 C 0.4644(2) 0.09165(6) 0.0519(2) 0.0380(5) Uani 1 1 d . . . C32 C 0.6193(2) 0.10618(8) -0.0419(3) 0.0494(6) Uani 1 1 d . . . H32A H 0.6619 0.1085 -0.1069 0.059 Uiso 1 1 calc R . . C33 C 0.6747(2) 0.11844(8) 0.0884(3) 0.0514(6) Uani 1 1 d . . . H33A H 0.7631 0.1310 0.1314 0.062 Uiso 1 1 calc R . . C34 C 0.5970(3) 0.12196(8) 0.2938(3) 0.0542(7) Uani 1 1 d . . . C35 C 0.7435(3) 0.14087(11) 0.3639(4) 0.0855(11) Uani 1 1 d . . . H35A H 0.7511 0.1649 0.3131 0.128 Uiso 1 1 calc R . . H35B H 0.8148 0.1212 0.3653 0.128 Uiso 1 1 calc R . . H35C H 0.7575 0.1485 0.4576 0.128 Uiso 1 1 calc R . . C36 C 0.4861(3) 0.15440(9) 0.2834(3) 0.0682(8) Uani 1 1 d . . . H36A H 0.4985 0.1775 0.2313 0.102 Uiso 1 1 calc R . . H36B H 0.4969 0.1632 0.3752 0.102 Uiso 1 1 calc R . . H36C H 0.3927 0.1430 0.2371 0.102 Uiso 1 1 calc R . . C37 C 0.5860(3) 0.08501(10) 0.3767(3) 0.0718(9) Uani 1 1 d . . . H37A H 0.4942 0.0725 0.3323 0.108 Uiso 1 1 calc R . . H37B H 0.5979 0.0935 0.4691 0.108 Uiso 1 1 calc R . . H37C H 0.6590 0.0656 0.3813 0.108 Uiso 1 1 calc R . . C41 C -0.1362(2) 0.18034(8) -0.0734(3) 0.0513(6) Uani 1 1 d . . . C42 C -0.1687(3) 0.17829(11) -0.2122(3) 0.0814(10) Uani 1 1 d . . . H42A H -0.1197 0.1599 -0.2467 0.098 Uiso 1 1 calc R . . C43 C -0.2728(4) 0.20292(16) -0.3036(4) 0.1247(18) Uani 1 1 d . . . H43A H -0.2906 0.2016 -0.3983 0.150 Uiso 1 1 calc R . . C44 C -0.3485(4) 0.22869(15) -0.2579(5) 0.1158(16) Uani 1 1 d . . . H44A H -0.4170 0.2457 -0.3198 0.139 Uiso 1 1 calc R . . C45 C -0.3246(4) 0.22961(11) -0.1234(5) 0.0904(11) Uani 1 1 d . . . H45A H -0.3814 0.2460 -0.0919 0.109 Uiso 1 1 calc R . . C46 C -0.2176(3) 0.20682(8) -0.0298(4) 0.0639(8) Uani 1 1 d . . . H46A H -0.1994 0.2092 0.0648 0.077 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 Cd 0.03949(10) 0.04035(11) 0.04270(11) -0.00130(7) 0.01730(7) -0.00007(7) S1 0.0485(3) 0.0357(3) 0.0435(3) 0.0003(2) 0.0076(3) 0.0026(2) S2 0.0493(3) 0.0358(3) 0.0389(3) -0.0019(2) 0.0190(3) -0.0040(2) S3 0.0385(3) 0.0483(4) 0.0451(3) 0.0093(3) 0.0144(2) -0.0050(2) S4 0.0616(4) 0.0696(5) 0.0563(4) 0.0023(3) 0.0346(3) 0.0094(3) B 0.0503(15) 0.0408(15) 0.0479(16) 0.0018(12) 0.0206(13) 0.0077(12) N11 0.0541(12) 0.0310(10) 0.0438(11) -0.0006(8) 0.0123(9) 0.0056(8) N12 0.0608(12) 0.0326(11) 0.0381(11) -0.0020(8) 0.0126(9) -0.0038(9) N21 0.0533(11) 0.0421(11) 0.0386(11) 0.0000(8) 0.0224(9) 0.0024(9) N22 0.0527(11) 0.0434(11) 0.0390(11) 0.0055(9) 0.0208(9) 0.0018(9) N31 0.0379(10) 0.0387(11) 0.0460(12) 0.0051(8) 0.0158(8) 0.0012(8) N32 0.0364(10) 0.0390(11) 0.0468(12) 0.0036(9) 0.0103(8) 0.0006(8) C11 0.0521(13) 0.0339(12) 0.0317(12) -0.0032(9) 0.0095(10) 0.0003(10) C12 0.0661(16) 0.0337(13) 0.0558(16) -0.0011(11) 0.0100(13) 0.0089(12) C13 0.0738(18) 0.0322(13) 0.0542(16) 0.0042(11) 0.0139(14) 0.0021(12) C14 0.0664(16) 0.0442(14) 0.0400(14) -0.0028(11) 0.0219(12) -0.0112(12) C15 0.098(2) 0.068(2) 0.0649(19) -0.0083(15) 0.0471(18) -0.0109(17) C16 0.094(2) 0.0490(17) 0.0608(18) -0.0003(13) 0.0328(16) -0.0191(15) C17 0.0635(16) 0.0636(18) 0.0449(15) -0.0050(12) 0.0119(13) -0.0174(13) C21 0.0408(12) 0.0386(13) 0.0400(13) 0.0025(10) 0.0186(10) -0.0014(9) C22 0.0767(17) 0.0512(16) 0.0469(15) -0.0062(12) 0.0331(13) 0.0032(14) C23 0.0721(18) 0.0612(17) 0.0374(14) 0.0041(12) 0.0271(13) 0.0073(14) C24 0.0539(14) 0.0444(14) 0.0486(15) 0.0096(11) 0.0148(12) 0.0063(11) C25 0.106(3) 0.074(2) 0.060(2) 0.0265(16) 0.0226(18) 0.0214(19) C26 0.0759(19) 0.0460(17) 0.085(2) 0.0139(15) 0.0261(17) -0.0064(14) C27 0.0477(15) 0.072(2) 0.0684(19) -0.0011(15) 0.0126(13) 0.0113(13) C31 0.0349(11) 0.0306(11) 0.0445(13) 0.0071(9) 0.0104(10) 0.0003(8) C32 0.0405(12) 0.0497(15) 0.0617(17) 0.0109(13) 0.0236(12) 0.0028(11) C33 0.0349(12) 0.0473(15) 0.0696(19) 0.0085(12) 0.0169(12) -0.0018(10) C34 0.0421(13) 0.0628(17) 0.0464(15) -0.0057(12) 0.0038(11) 0.0021(11) C35 0.0537(17) 0.107(3) 0.074(2) -0.0242(19) -0.0018(15) -0.0104(17) C36 0.0607(17) 0.0638(19) 0.0695(19) -0.0156(15) 0.0125(14) 0.0056(14) C37 0.0764(19) 0.087(2) 0.0429(16) 0.0121(15) 0.0118(14) 0.0133(17) C41 0.0408(13) 0.0504(15) 0.0702(19) -0.0033(13) 0.0296(12) -0.0101(11) C42 0.0611(18) 0.115(3) 0.065(2) -0.0078(19) 0.0195(15) 0.0306(18) C43 0.088(3) 0.194(5) 0.077(3) -0.001(3) 0.015(2) 0.066(3) C44 0.074(2) 0.151(4) 0.112(4) 0.010(3) 0.023(2) 0.052(3) C45 0.068(2) 0.080(3) 0.136(4) 0.000(2) 0.053(2) 0.0171(18) C46 0.0665(17) 0.0522(17) 0.089(2) -0.0049(15) 0.0475(16) -0.0007(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 Cd S4 2.4595(7) . ? Cd S2 2.5537(6) . ? Cd S3 2.5641(6) . ? Cd S1 2.5784(6) . ? S1 C11 1.725(2) . ? S2 C21 1.733(2) . ? S3 C31 1.726(2) . ? S4 C41 1.764(3) . ? B N31 1.553(3) . ? B N21 1.556(3) . ? B N11 1.555(4) . ? N11 C11 1.358(3) . ? N11 C12 1.387(3) . ? N12 C11 1.363(3) . ? N12 C13 1.389(3) . ? N12 C14 1.514(3) . ? N21 C21 1.354(3) . ? N21 C22 1.375(3) . ? N22 C21 1.355(3) . ? N22 C23 1.386(3) . ? N22 C24 1.519(3) . ? N31 C31 1.349(3) . ? N31 C32 1.379(3) . ? N32 C31 1.368(3) . ? N32 C33 1.393(3) . ? N32 C34 1.502(3) . ? C12 C13 1.327(4) . ? C14 C17 1.520(3) . ? C14 C16 1.530(3) . ? C14 C15 1.541(4) . ? C22 C23 1.326(4) . ? C24 C26 1.518(4) . ? C24 C25 1.523(4) . ? C24 C27 1.523(4) . ? C32 C33 1.327(4) . ? C34 C37 1.520(4) . ? C34 C36 1.531(4) . ? C34 C35 1.531(4) . ? C41 C42 1.365(4) . ? C41 C46 1.395(4) . ? C42 C43 1.392(5) . ? C43 C44 1.351(5) . ? C44 C45 1.335(5) . ? C45 C46 1.383(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 S4 Cd S2 122.00(2) . . ? S4 Cd S3 108.12(2) . . ? S2 Cd S3 100.458(19) . . ? S4 Cd S1 122.39(2) . . ? S2 Cd S1 97.68(2) . . ? S3 Cd S1 102.78(2) . . ? C11 S1 Cd 94.78(7) . . ? C21 S2 Cd 97.86(7) . . ? C31 S3 Cd 96.24(7) . . ? C41 S4 Cd 105.14(9) . . ? N31 B N21 112.5(2) . . ? N31 B N11 112.7(2) . . ? N21 B N11 112.6(2) . . ? C11 N11 C12 107.2(2) . . ? C11 N11 B 134.11(19) . . ? C12 N11 B 118.6(2) . . ? C11 N12 C13 107.6(2) . . ? C11 N12 C14 127.7(2) . . ? C13 N12 C14 124.7(2) . . ? C21 N21 C22 107.4(2) . . ? C21 N21 B 133.9(2) . . ? C22 N21 B 118.4(2) . . ? C21 N22 C23 107.9(2) . . ? C21 N22 C24 127.85(19) . . ? C23 N22 C24 124.1(2) . . ? C31 N31 C32 108.3(2) . . ? C31 N31 B 133.45(19) . . ? C32 N31 B 117.9(2) . . ? C31 N32 C33 107.2(2) . . ? C31 N32 C34 128.0(2) . . ? C33 N32 C34 124.5(2) . . ? N11 C11 N12 108.29(19) . . ? N11 C11 S1 125.74(17) . . ? N12 C11 S1 125.97(18) . . ? C13 C12 N11 108.9(2) . . ? C12 C13 N12 107.9(2) . . ? N12 C14 C17 109.1(2) . . ? N12 C14 C16 108.6(2) . . ? C17 C14 C16 108.7(2) . . ? N12 C14 C15 110.0(2) . . ? C17 C14 C15 111.3(2) . . ? C16 C14 C15 109.1(2) . . ? N21 C21 N22 108.12(19) . . ? N21 C21 S2 125.76(17) . . ? N22 C21 S2 126.11(17) . . ? C23 C22 N21 109.2(2) . . ? C22 C23 N22 107.4(2) . . ? N22 C24 C26 109.8(2) . . ? N22 C24 C25 109.0(2) . . ? C26 C24 C25 109.5(2) . . ? N22 C24 C27 108.4(2) . . ? C26 C24 C27 112.1(2) . . ? C25 C24 C27 108.1(2) . . ? N31 C31 N32 107.94(19) . . ? N31 C31 S3 126.42(17) . . ? N32 C31 S3 125.61(18) . . ? C33 C32 N31 108.5(2) . . ? C32 C33 N32 108.1(2) . . ? N32 C34 C37 110.3(2) . . ? N32 C34 C36 108.1(2) . . ? C37 C34 C36 112.6(3) . . ? N32 C34 C35 108.5(2) . . ? C37 C34 C35 108.7(2) . . ? C36 C34 C35 108.6(2) . . ? C42 C41 C46 116.3(3) . . ? C42 C41 S4 123.9(2) . . ? C46 C41 S4 119.8(2) . . ? C41 C42 C43 121.3(3) . . ? C44 C43 C42 120.9(4) . . ? C45 C44 C43 119.1(4) . . ? C44 C45 C46 121.1(4) . . ? C45 C46 C41 121.1(3) . . ? _diffrn_measured_fraction_theta_max 0.922 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.922 _refine_diff_density_max 0.317 _refine_diff_density_min -0.351 _refine_diff_density_rms 0.053 # Attachment 'TOLCDS10.CIF' data_tolcds10 _database_code_depnum_ccdc_archive 'CCDC 609904' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H50 B Cd N6 S4' _chemical_formula_weight 830.28 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.0659(9) _cell_length_b 10.9688(6) _cell_length_c 25.4342(16) _cell_angle_alpha 90.00 _cell_angle_beta 104.6080(10) _cell_angle_gamma 90.00 _cell_volume 4067.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 243(2) _cell_measurement_reflns_used 4220 _cell_measurement_theta_min 2.544 _cell_measurement_theta_max 27.098 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.356 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1724 _exptl_absorpt_coefficient_mu 0.776 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.7466 _exptl_absorpt_correction_T_max 0.7466 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 243(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27846 _diffrn_reflns_av_R_equivalents 0.0829 _diffrn_reflns_av_sigmaI/netI 0.1333 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 28.28 _reflns_number_total 9449 _reflns_number_gt 4851 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0070P)^2^+0.0000P] 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 0.00002(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9449 _refine_ls_number_parameters 447 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1312 _refine_ls_R_factor_gt 0.0480 _refine_ls_wR_factor_ref 0.0631 _refine_ls_wR_factor_gt 0.0538 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.005 _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 Cd Cd -0.036854(19) 0.88091(2) -0.846882(12) 0.03502(9) Uani 1 1 d . . . S1 S -0.07148(7) 0.69987(8) -0.79119(4) 0.0390(3) Uani 1 1 d . . . S2 S -0.20203(7) 0.95646(8) -0.88264(4) 0.0339(3) Uani 1 1 d . . . S3 S -0.00995(7) 0.75891(7) -0.92747(4) 0.0350(3) Uani 1 1 d . . . S4 S 0.06181(7) 1.05849(8) -0.81404(5) 0.0523(3) Uani 1 1 d . . . B B -0.2212(3) 0.6510(3) -0.91769(19) 0.0321(11) Uani 1 1 d . . . H1 H -0.2796(16) 0.5919(19) -0.9411(9) 0.009(7) Uiso 1 1 d . . . N11 N -0.2426(2) 0.6767(2) -0.86185(12) 0.0288(7) Uani 1 1 d . . . N12 N -0.2478(2) 0.7116(2) -0.77734(12) 0.0313(8) Uani 1 1 d . . . N21 N -0.22833(18) 0.7661(2) -0.95478(11) 0.0287(7) Uani 1 1 d . . . N22 N -0.22248(19) 0.9440(2) -0.99334(12) 0.0301(8) Uani 1 1 d . . . N31 N -0.1295(2) 0.5817(2) -0.91100(11) 0.0301(8) Uani 1 1 d . . . N32 N 0.0116(2) 0.5147(2) -0.90006(11) 0.0306(8) Uani 1 1 d . . . C11 C -0.1896(3) 0.6977(3) -0.81109(15) 0.0302(9) Uani 1 1 d . . . C12 C -0.3330(3) 0.6787(3) -0.85976(16) 0.0369(10) Uani 1 1 d . . . H12A H -0.3838 0.6664 -0.8894 0.044 Uiso 1 1 calc R . . C13 C -0.3367(3) 0.7009(3) -0.80907(16) 0.0390(10) Uani 1 1 d . . . H13A H -0.3904 0.7080 -0.7969 0.047 Uiso 1 1 calc R . . C14 C -0.2225(3) 0.7401(3) -0.71791(15) 0.0400(10) Uani 1 1 d . . . C15 C -0.3102(3) 0.7339(4) -0.69730(16) 0.0641(13) Uani 1 1 d . . . H15A H -0.2953 0.7524 -0.6588 0.096 Uiso 1 1 calc R . . H15B H -0.3362 0.6526 -0.7033 0.096 Uiso 1 1 calc R . . H15C H -0.3545 0.7927 -0.7169 0.096 Uiso 1 1 calc R . . C16 C -0.1554(3) 0.6447(3) -0.68654(14) 0.0517(11) Uani 1 1 d . . . H16A H -0.0969 0.6529 -0.6956 0.078 Uiso 1 1 calc R . . H16B H -0.1799 0.5638 -0.6963 0.078 Uiso 1 1 calc R . . H16C H -0.1469 0.6572 -0.6478 0.078 Uiso 1 1 calc R . . C17 C -0.1832(3) 0.8688(3) -0.70960(15) 0.0680(14) Uani 1 1 d . . . H17A H -0.1242 0.8706 -0.7184 0.102 Uiso 1 1 calc R . . H17B H -0.1755 0.8928 -0.6720 0.102 Uiso 1 1 calc R . . H17C H -0.2248 0.9249 -0.7331 0.102 Uiso 1 1 calc R . . C21 C -0.2169(2) 0.8873(3) -0.94476(13) 0.0281(8) Uani 1 1 d . . . C22 C -0.2409(2) 0.7487(3) -1.00992(15) 0.0361(10) Uani 1 1 d . . . H22A H -0.2510 0.6731 -1.0278 0.043 Uiso 1 1 calc R . . C23 C -0.2365(2) 0.8554(3) -1.03364(15) 0.0370(10) Uani 1 1 d . . . H23A H -0.2419 0.8687 -1.0708 0.044 Uiso 1 1 calc R . . C24 C -0.2064(3) 1.0784(3) -1.00270(15) 0.0383(10) Uani 1 1 d . . . C25 C -0.2188(3) 1.0997(3) -1.06374(15) 0.0604(13) Uani 1 1 d . . . H25A H -0.1716 1.0560 -1.0758 0.091 Uiso 1 1 calc R . . H25B H -0.2141 1.1862 -1.0705 0.091 Uiso 1 1 calc R . . H25C H -0.2787 1.0704 -1.0835 0.091 Uiso 1 1 calc R . . C26 C -0.2762(3) 1.1552(3) -0.98353(15) 0.0514(12) Uani 1 1 d . . . H26A H -0.2664 1.1464 -0.9445 0.077 Uiso 1 1 calc R . . H26B H -0.3376 1.1282 -1.0016 0.077 Uiso 1 1 calc R . . H26C H -0.2690 1.2402 -0.9923 0.077 Uiso 1 1 calc R . . C27 C -0.1070(2) 1.1101(3) -0.97208(15) 0.0524(11) Uani 1 1 d . . . H27A H -0.0649 1.0570 -0.9844 0.079 Uiso 1 1 calc R . . H27B H -0.0995 1.0990 -0.9334 0.079 Uiso 1 1 calc R . . H27C H -0.0942 1.1943 -0.9793 0.079 Uiso 1 1 calc R . . C31 C -0.0437(2) 0.6165(3) -0.91193(13) 0.0288(9) Uani 1 1 d . . . C32 C -0.1281(3) 0.4596(3) -0.89861(15) 0.0410(11) Uani 1 1 d . . . H32A H -0.1787 0.4129 -0.8953 0.049 Uiso 1 1 calc R . . C33 C -0.0424(3) 0.4185(3) -0.89206(14) 0.0368(10) Uani 1 1 d . . . H33A H -0.0225 0.3380 -0.8835 0.044 Uiso 1 1 calc R . . C34 C 0.1126(3) 0.5070(3) -0.89585(15) 0.0323(10) Uani 1 1 d . . . C35 C 0.1452(2) 0.3763(3) -0.87966(14) 0.0484(11) Uani 1 1 d . . . H35A H 0.1328 0.3562 -0.8451 0.073 Uiso 1 1 calc R . . H35B H 0.2106 0.3704 -0.8765 0.073 Uiso 1 1 calc R . . H35C H 0.1128 0.3199 -0.9072 0.073 Uiso 1 1 calc R . . C36 C 0.1633(2) 0.5931(3) -0.85056(14) 0.0477(11) Uani 1 1 d . . . H36A H 0.1506 0.5695 -0.8164 0.072 Uiso 1 1 calc R . . H36B H 0.1425 0.6761 -0.8594 0.072 Uiso 1 1 calc R . . H36C H 0.2288 0.5883 -0.8473 0.072 Uiso 1 1 calc R . . C37 C 0.1312(2) 0.5375(3) -0.95073(14) 0.0427(11) Uani 1 1 d . . . H37A H 0.1002 0.4788 -0.9777 0.064 Uiso 1 1 calc R . . H37B H 0.1966 0.5346 -0.9476 0.064 Uiso 1 1 calc R . . H37C H 0.1084 0.6187 -0.9618 0.064 Uiso 1 1 calc R . . C41 C 0.1765(3) 1.0066(3) -0.80235(14) 0.0345(10) Uani 1 1 d . . . C42 C 0.2052(3) 0.8889(3) -0.78590(14) 0.0417(10) Uani 1 1 d . . . H42A H 0.1617 0.8320 -0.7805 0.050 Uiso 1 1 calc R . . C43 C 0.2953(3) 0.8532(3) -0.77728(14) 0.0421(11) Uani 1 1 d . . . H43A H 0.3119 0.7729 -0.7661 0.051 Uiso 1 1 calc R . . C44 C 0.3624(3) 0.9339(3) -0.78477(15) 0.0404(10) Uani 1 1 d . . . C45 C 0.3342(3) 1.0506(3) -0.80096(14) 0.0404(10) Uani 1 1 d . . . H45A H 0.3778 1.1075 -0.8062 0.049 Uiso 1 1 calc R . . C46 C 0.2437(3) 1.0867(3) -0.80977(14) 0.0378(10) Uani 1 1 d . . . H46A H 0.2273 1.1671 -0.8210 0.045 Uiso 1 1 calc R . . C47 C 0.4615(3) 0.8956(3) -0.77490(17) 0.0669(13) Uani 1 1 d . . . H47A H 0.4982 0.9649 -0.7802 0.100 Uiso 1 1 calc R . . H47B H 0.4667 0.8313 -0.8002 0.100 Uiso 1 1 calc R . . H47C H 0.4833 0.8658 -0.7380 0.100 Uiso 1 1 calc R . . C101 C 0.0865(3) 1.1311(5) -0.6083(4) 0.100(2) Uani 1 1 d . . . H10A H 0.0984 1.2153 -0.6070 0.120 Uiso 1 1 calc R . . C102 C 0.0757(4) 1.0730(9) -0.5632(3) 0.098(2) Uani 1 1 d . . . H10B H 0.0793 1.1167 -0.5310 0.118 Uiso 1 1 calc R . . C103 C 0.0596(4) 0.9512(8) -0.5651(3) 0.110(2) Uani 1 1 d . . . H10C H 0.0518 0.9100 -0.5342 0.131 Uiso 1 1 calc R . . C104 C 0.0549(4) 0.8899(6) -0.6115(4) 0.121(3) Uani 1 1 d . . . H10D H 0.0436 0.8055 -0.6130 0.146 Uiso 1 1 calc R . . C105 C 0.0662(4) 0.9485(8) -0.6557(3) 0.101(2) Uani 1 1 d . . . H10E H 0.0641 0.9040 -0.6876 0.122 Uiso 1 1 calc R . . C106 C 0.0804(4) 1.0688(8) -0.6552(3) 0.099(2) Uani 1 1 d . . . H10F H 0.0859 1.1095 -0.6867 0.119 Uiso 1 1 calc R . . C201 C 0.0132(4) 0.5575(5) -0.5447(2) 0.0775(16) Uani 1 1 d . . . H20A H 0.0226 0.5977 -0.5755 0.093 Uiso 1 1 calc R . . C202 C 0.0485(3) 0.6064(4) -0.4941(3) 0.0749(16) Uani 1 1 d . . . H20B H 0.0818 0.6798 -0.4905 0.090 Uiso 1 1 calc R . . C203 C 0.0357(3) 0.5493(5) -0.4491(2) 0.0746(15) Uani 1 1 d . . . H20D H 0.0599 0.5824 -0.4143 0.090 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 Cd 0.03200(18) 0.03523(14) 0.03738(18) -0.00128(16) 0.00790(13) -0.00082(16) S1 0.0293(7) 0.0503(6) 0.0364(7) 0.0102(5) 0.0063(5) 0.0007(5) S2 0.0357(7) 0.0382(5) 0.0274(6) -0.0058(5) 0.0073(5) 0.0056(5) S3 0.0397(7) 0.0272(5) 0.0437(7) 0.0058(5) 0.0209(5) 0.0020(5) S4 0.0387(7) 0.0370(5) 0.0761(9) -0.0125(6) 0.0051(6) 0.0008(5) B 0.031(3) 0.031(2) 0.036(3) 0.002(2) 0.011(2) -0.002(2) N11 0.024(2) 0.0321(16) 0.032(2) 0.0036(15) 0.0084(16) 0.0024(15) N12 0.031(2) 0.0361(17) 0.027(2) 0.0055(15) 0.0080(17) 0.0054(16) N21 0.033(2) 0.0292(16) 0.026(2) -0.0018(15) 0.0095(15) 0.0023(14) N22 0.038(2) 0.0254(16) 0.029(2) 0.0036(15) 0.0115(16) 0.0024(14) N31 0.034(2) 0.0208(16) 0.038(2) 0.0042(13) 0.0147(16) 0.0024(14) N32 0.036(2) 0.0257(16) 0.029(2) 0.0023(14) 0.0062(16) 0.0019(16) C11 0.032(3) 0.032(2) 0.026(3) 0.0053(18) 0.005(2) 0.0023(19) C12 0.028(3) 0.042(2) 0.040(3) 0.006(2) 0.007(2) 0.005(2) C13 0.031(3) 0.049(2) 0.039(3) 0.005(2) 0.011(2) 0.009(2) C14 0.048(3) 0.046(2) 0.028(3) -0.001(2) 0.013(2) 0.008(2) C15 0.068(4) 0.089(3) 0.041(3) 0.006(2) 0.025(3) 0.028(3) C16 0.053(3) 0.062(3) 0.039(3) 0.011(2) 0.010(2) 0.009(2) C17 0.102(4) 0.045(2) 0.050(3) -0.007(2) 0.005(3) 0.001(3) C21 0.021(2) 0.0332(19) 0.030(2) 0.000(2) 0.0064(17) 0.0090(19) C22 0.045(3) 0.033(2) 0.031(3) -0.006(2) 0.010(2) 0.0015(19) C23 0.050(3) 0.037(2) 0.024(2) -0.0036(19) 0.010(2) 0.004(2) C24 0.050(3) 0.030(2) 0.035(3) 0.0023(18) 0.011(2) 0.000(2) C25 0.094(4) 0.043(2) 0.043(3) 0.008(2) 0.014(3) -0.016(2) C26 0.066(3) 0.030(2) 0.059(3) 0.010(2) 0.016(2) 0.011(2) C27 0.050(3) 0.053(2) 0.053(3) 0.006(2) 0.011(2) -0.004(2) C31 0.039(3) 0.0256(18) 0.024(2) 0.0014(18) 0.0131(18) 0.010(2) C32 0.051(3) 0.026(2) 0.047(3) 0.0060(19) 0.016(2) -0.005(2) C33 0.046(3) 0.0207(19) 0.047(3) 0.0079(17) 0.018(2) 0.0033(19) C34 0.036(3) 0.031(2) 0.031(3) 0.0006(18) 0.011(2) 0.0122(19) C35 0.051(3) 0.038(2) 0.058(3) 0.011(2) 0.017(2) 0.023(2) C36 0.048(3) 0.048(2) 0.044(3) -0.005(2) 0.006(2) 0.011(2) C37 0.044(3) 0.043(2) 0.046(3) 0.003(2) 0.020(2) 0.013(2) C41 0.037(3) 0.034(2) 0.029(3) -0.0088(18) 0.002(2) -0.007(2) C42 0.047(3) 0.029(2) 0.049(3) -0.003(2) 0.012(2) -0.006(2) C43 0.052(3) 0.027(2) 0.046(3) 0.0036(18) 0.009(2) 0.004(2) C44 0.041(3) 0.041(2) 0.035(3) -0.012(2) 0.001(2) 0.001(2) C45 0.044(3) 0.036(2) 0.042(3) -0.003(2) 0.012(2) -0.009(2) C46 0.046(3) 0.028(2) 0.036(3) -0.0007(17) 0.004(2) 0.001(2) C47 0.041(3) 0.057(3) 0.097(4) -0.007(3) 0.006(3) 0.007(2) C101 0.053(4) 0.073(4) 0.161(8) -0.008(6) 0.002(5) -0.013(3) C102 0.065(4) 0.142(7) 0.076(5) -0.016(5) -0.002(4) 0.011(4) C103 0.089(5) 0.123(6) 0.101(7) 0.058(5) -0.005(5) 0.002(5) C104 0.123(6) 0.071(4) 0.141(7) 0.023(6) -0.022(6) -0.011(4) C105 0.086(5) 0.126(6) 0.076(5) -0.009(5) -0.009(4) 0.026(5) C106 0.058(4) 0.119(6) 0.121(7) 0.047(5) 0.023(4) -0.001(4) C201 0.055(4) 0.085(4) 0.089(5) 0.038(3) 0.012(3) 0.001(3) C202 0.045(3) 0.057(3) 0.112(5) 0.008(4) 0.001(3) -0.011(3) C203 0.053(4) 0.079(4) 0.080(5) -0.001(3) -0.006(3) 0.000(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd S4 2.4648(10) . ? Cd S2 2.5622(10) . ? Cd S3 2.5643(10) . ? Cd S1 2.5680(10) . ? S1 C11 1.724(4) . ? S2 C21 1.716(3) . ? S3 C31 1.720(3) . ? S4 C41 1.772(4) . ? B N31 1.549(5) . ? B N11 1.559(5) . ? B N21 1.564(4) . ? N11 C11 1.355(4) . ? N11 C12 1.376(4) . ? N12 C11 1.381(4) . ? N12 C13 1.384(4) . ? N12 C14 1.496(4) . ? N21 C21 1.356(4) . ? N21 C22 1.380(4) . ? N22 C21 1.367(4) . ? N22 C23 1.389(4) . ? N22 C24 1.522(4) . ? N31 C31 1.353(4) . ? N31 C32 1.375(4) . ? N32 C33 1.378(4) . ? N32 C31 1.380(4) . ? N32 C34 1.501(4) . ? C12 C13 1.327(4) . ? C14 C17 1.525(4) . ? C14 C16 1.532(4) . ? C14 C15 1.542(5) . ? C22 C23 1.327(4) . ? C24 C26 1.520(4) . ? C24 C25 1.534(4) . ? C24 C27 1.543(4) . ? C32 C33 1.337(4) . ? C34 C37 1.528(4) . ? C34 C36 1.536(4) . ? C34 C35 1.537(4) . ? C41 C46 1.389(4) . ? C41 C42 1.392(4) . ? C42 C43 1.376(4) . ? C43 C44 1.393(5) . ? C44 C45 1.379(4) . ? C44 C47 1.510(5) . ? C45 C46 1.382(4) . ? C101 C106 1.358(7) . ? C101 C102 1.358(7) . ? C102 C103 1.356(7) . ? C103 C104 1.344(7) . ? C104 C105 1.343(7) . ? C105 C106 1.336(7) . ? C201 C203 1.372(5) 3_564 ? C201 C202 1.372(6) . ? C202 C203 1.361(6) . ? C203 C201 1.372(5) 3_564 ? 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 S4 Cd S2 108.27(3) . . ? S4 Cd S3 118.68(3) . . ? S2 Cd S3 102.72(3) . . ? S4 Cd S1 127.83(4) . . ? S2 Cd S1 97.56(3) . . ? S3 Cd S1 97.61(3) . . ? C11 S1 Cd 100.78(12) . . ? C21 S2 Cd 94.22(11) . . ? C31 S3 Cd 100.07(11) . . ? C41 S4 Cd 106.39(11) . . ? N31 B N11 111.9(3) . . ? N31 B N21 112.7(3) . . ? N11 B N21 113.9(3) . . ? C11 N11 C12 108.1(3) . . ? C11 N11 B 133.7(3) . . ? C12 N11 B 118.1(3) . . ? C11 N12 C13 107.5(3) . . ? C11 N12 C14 127.7(3) . . ? C13 N12 C14 124.7(3) . . ? C21 N21 C22 107.8(3) . . ? C21 N21 B 133.8(3) . . ? C22 N21 B 118.2(3) . . ? C21 N22 C23 108.1(3) . . ? C21 N22 C24 127.3(3) . . ? C23 N22 C24 124.2(3) . . ? C31 N31 C32 108.6(3) . . ? C31 N31 B 133.6(3) . . ? C32 N31 B 117.7(3) . . ? C33 N32 C31 107.8(3) . . ? C33 N32 C34 124.9(3) . . ? C31 N32 C34 127.3(3) . . ? N11 C11 N12 107.3(3) . . ? N11 C11 S1 126.7(3) . . ? N12 C11 S1 125.9(3) . . ? C13 C12 N11 109.0(3) . . ? C12 C13 N12 108.0(4) . . ? N12 C14 C17 109.0(3) . . ? N12 C14 C16 110.5(3) . . ? C17 C14 C16 112.2(3) . . ? N12 C14 C15 108.2(3) . . ? C17 C14 C15 109.3(3) . . ? C16 C14 C15 107.6(3) . . ? N21 C21 N22 107.5(3) . . ? N21 C21 S2 126.0(3) . . ? N22 C21 S2 126.5(3) . . ? C23 C22 N21 109.3(3) . . ? C22 C23 N22 107.3(3) . . ? C26 C24 N22 109.7(3) . . ? C26 C24 C25 108.8(3) . . ? N22 C24 C25 108.8(3) . . ? C26 C24 C27 112.0(3) . . ? N22 C24 C27 108.1(3) . . ? C25 C24 C27 109.4(3) . . ? N31 C31 N32 107.1(3) . . ? N31 C31 S3 126.8(3) . . ? N32 C31 S3 126.0(3) . . ? C33 C32 N31 108.4(3) . . ? C32 C33 N32 108.1(3) . . ? N32 C34 C37 109.8(3) . . ? N32 C34 C36 108.8(3) . . ? C37 C34 C36 112.3(3) . . ? N32 C34 C35 108.7(3) . . ? C37 C34 C35 109.2(3) . . ? C36 C34 C35 107.9(3) . . ? C46 C41 C42 116.5(3) . . ? C46 C41 S4 119.1(3) . . ? C42 C41 S4 124.3(3) . . ? C43 C42 C41 122.0(4) . . ? C42 C43 C44 121.2(3) . . ? C45 C44 C43 116.8(4) . . ? C45 C44 C47 121.8(4) . . ? C43 C44 C47 121.4(3) . . ? C44 C45 C46 122.1(4) . . ? C45 C46 C41 121.3(3) . . ? C106 C101 C102 120.6(7) . . ? C103 C102 C101 119.4(7) . . ? C104 C103 C102 119.6(7) . . ? C105 C104 C103 120.4(7) . . ? C106 C105 C104 121.2(7) . . ? C105 C106 C101 118.7(7) . . ? C203 C201 C202 120.8(5) 3_564 . ? C203 C202 C201 120.3(5) . . ? C202 C203 C201 118.8(5) . 3_564 ? _diffrn_measured_fraction_theta_max 0.937 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.937 _refine_diff_density_max 0.415 _refine_diff_density_min -0.395 _refine_diff_density_rms 0.088