# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_requested_category 'FM ' _publ_contact_author_name 'Anthony F. Hill' _publ_contact_author_address ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' 61 2 6125 8577 ' _publ_contact_author_fax ' 61 2 6125 3216 ' _publ_contact_author_email a.hill@rsc.anu.edu.au _publ_section_title ; Novel Poly(methimazolyl)borate Complexes of Niobium and Tantalum ; loop_ _publ_author_name _publ_author_address M.K.Smith ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; A.F.Hill ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; #==== # 4. TEXT _publ_section_abstract #Text of the abstract ; The crystal structure of [6.5 H8 B0.5 N2 S1 Cl2 Ta0.5] is reported. ; _publ_section_comment #Text of the paper ; The crystallographic asymmetric unit consists of one molecule of [6.5 H8 B0.5 N2 S1 Cl2 Ta0.5]. Hydrogen atoms attached to C atoms were included at idealized positions and ride on the atom to which they bonded. The hydrogen atom attached to boron was located but not refined. ; _publ_section_exptl_refinement # see also _refine_ls_hydrogen for refinement keywords. ; Hydrogen atoms attached to C atoms were included at idealized positions and ride on the atom to which they bonded. The hydrogen atom attached to boron was located but not refined. ; _publ_section_exptl_prep ; The compound was prepared by MKS and recrystallized from tetrahydrofuran. The sample ID is mks39. . ; data_c:\docume~1\admini~1\desktop\newxta~1\mks30\mks30 _database_code_depnum_ccdc_archive 'CCDC 243423' _audit_creation_method SHELXL-97 #==== # 4. TEXT _publ_section_abstract #Text of the abstract ; The crystal structure of [C31 H33 B1 N6 S3 Cl2 Sn1] is reported. ; _publ_section_comment #Text of the paper ; The crystallographic asymmetric unit consists of one molecule of [C30 H31 B1 N6 S3 Sn1] and one molecule of CH2Cl2. Hydrogen atoms attached to C atoms were included at idealized positions and ride on the atom to which they bonded. The H atoms bonded to the B were located but not refined ; _publ_section_exptl_refinement # see also _refine_ls_hydrogen for refinement keywords. ; Hydrogen atoms attached to C atoms were included at idealized positions and ride on the atom to which they bonded. The H atoms bonded to the B were located but not refined ; _publ_section_exptl_prep ; The compound was prepared by MKS and recrystallized from dichloromethane. The sample ID is mks30. . ; #===== _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H33 B Cl2 N6 S3 Sn' _chemical_formula_weight 786.21 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 '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 9.1800(18) _cell_length_b 10.140(2) _cell_length_c 21.540(4) _cell_angle_alpha 96.09(3) _cell_angle_beta 98.22(3) _cell_angle_gamma 114.39(3) _cell_volume 1776.8(6) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 35015 _cell_measurement_theta_min 27.48 _cell_measurement_theta_max 2.91 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.470 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 796 _exptl_absorpt_coefficient_mu 1.076 # Absorption correction loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 0 0.250 -1 0 0 0.260 0 1 0 0.150 0 -1 0 0.160 0 0 1 0.180 0 0 -1 0.030 5 -3 -1 0.310 -1 -10 0 0.153 0 -2 3 0.162 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.634 _exptl_absorpt_correction_T_max 0.828 _exptl_absorpt_process_details ; Gaussian integration (Coppens, 1970) ; _diffrn_ambient_temperature 200(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 _diffrn_measurement_method ' \f and \w scans with CCD ' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 40860 _diffrn_reflns_av_R_equivalents 0.0680 _diffrn_reflns_av_sigmaI/netI 0.0431 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8125 _reflns_number_gt 6587 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction 'X -Seed' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed / POV-Ray' _computing_publication_material 'Microsoft Office 2000' _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^)+(0.0585P)^2^+0.6556P] 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 8125 _refine_ls_number_parameters 400 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0542 _refine_ls_R_factor_gt 0.0383 _refine_ls_wR_factor_ref 0.1067 _refine_ls_wR_factor_gt 0.0979 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.013 _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 Sn1 Sn 0.69239(2) 0.73271(2) 0.686836(9) 0.03663(8) Uani 1 1 d . . . Cl1 Cl 0.59545(16) 0.87730(14) 0.50825(7) 0.0884(3) Uani 1 1 d . . . C1 C 0.4938(6) 0.8134(5) 0.4294(2) 0.0869(14) Uani 1 1 d . . . H1A H 0.5158 0.8983 0.4072 0.104 Uiso 1 1 calc R . . H1B H 0.5374 0.7499 0.4085 0.104 Uiso 1 1 calc R . . B1 B 1.1312(4) 0.9072(3) 0.83331(15) 0.0318(6) Uani 1 1 d . . . Cl2 Cl 0.2867(2) 0.7153(2) 0.42081(9) 0.1474(8) Uani 1 1 d . . . S11 S 0.75473(8) 0.64731(8) 0.78540(3) 0.03669(16) Uani 1 1 d . . . N11 N 0.9815(3) 0.9125(2) 0.85905(10) 0.0325(5) Uani 1 1 d . . . C11 C 0.8266(3) 0.8107(3) 0.84009(13) 0.0340(6) Uani 1 1 d . . . N12 N 0.7335(3) 0.8497(3) 0.87426(12) 0.0441(6) Uani 1 1 d . . . C12 C 0.9853(4) 1.0177(3) 0.90595(14) 0.0419(7) Uani 1 1 d . . . H12 H 1.0799 1.1030 0.9280 0.050 Uiso 1 1 calc R . . C13 C 0.8330(4) 0.9795(4) 0.91527(16) 0.0495(8) Uani 1 1 d . . . H13 H 0.8002 1.0326 0.9448 0.059 Uiso 1 1 calc R . . C14 C 0.5569(4) 0.7702(4) 0.86778(19) 0.0631(10) Uani 1 1 d . . . H14A H 0.5031 0.8227 0.8455 0.095 Uiso 1 1 calc R . . H14B H 0.5306 0.7638 0.9102 0.095 Uiso 1 1 calc R . . H14C H 0.5185 0.6707 0.8432 0.095 Uiso 1 1 calc R . . S21 S 1.05919(9) 0.72406(8) 0.95858(3) 0.03883(16) Uani 1 1 d . . . N21 N 1.1375(2) 0.7591(2) 0.84058(10) 0.0299(4) Uani 1 1 d . . . C21 C 1.1046(3) 0.6797(3) 0.88835(13) 0.0308(5) Uani 1 1 d . . . N22 N 1.1150(3) 0.5522(2) 0.86894(11) 0.0364(5) Uani 1 1 d . . . C22 C 1.1645(3) 0.6773(3) 0.79169(13) 0.0335(6) Uani 1 1 d . . . H22 H 1.1882 0.7064 0.7524 0.040 Uiso 1 1 calc R . . C23 C 1.1518(3) 0.5504(3) 0.80890(14) 0.0390(6) Uani 1 1 d . . . H23 H 1.1654 0.4740 0.7846 0.047 Uiso 1 1 calc R . . C24 C 1.0883(5) 0.4348(4) 0.90627(17) 0.0543(8) Uani 1 1 d . . . H24A H 1.1441 0.4781 0.9508 0.081 Uiso 1 1 calc R . . H24B H 1.1322 0.3689 0.8889 0.081 Uiso 1 1 calc R . . H24C H 0.9709 0.3788 0.9040 0.081 Uiso 1 1 calc R . . S31 S 1.26864(10) 1.24263(9) 0.80218(4) 0.04652(19) Uani 1 1 d . . . N31 N 1.2885(3) 1.0376(2) 0.87223(11) 0.0327(5) Uani 1 1 d . . . C31 C 1.3518(3) 1.1774(3) 0.85929(14) 0.0349(6) Uani 1 1 d . . . N32 N 1.4952(3) 1.2549(3) 0.90161(12) 0.0412(6) Uani 1 1 d . . . C32 C 1.3958(3) 1.0334(3) 0.92347(14) 0.0418(7) Uani 1 1 d . . . H32 H 1.3817 0.9499 0.9426 0.050 Uiso 1 1 calc R . . C33 C 1.5221(4) 1.1663(3) 0.94131(15) 0.0459(7) Uani 1 1 d . . . H33 H 1.6136 1.1945 0.9752 0.055 Uiso 1 1 calc R . . C34 C 1.6041(5) 1.4100(3) 0.9054(2) 0.0625(10) Uani 1 1 d . . . H34A H 1.6089 1.4314 0.8622 0.094 Uiso 1 1 calc R . . H34B H 1.7138 1.4313 0.9283 0.094 Uiso 1 1 calc R . . H34C H 1.5626 1.4715 0.9282 0.094 Uiso 1 1 calc R . . C41 C 0.6602(3) 0.9249(3) 0.71327(14) 0.0392(6) Uani 1 1 d . . . C42 C 0.7917(4) 1.0615(3) 0.73952(17) 0.0507(8) Uani 1 1 d . . . H42 H 0.9003 1.0710 0.7456 0.061 Uiso 1 1 calc R . . C43 C 0.7634(5) 1.1823(4) 0.7566(2) 0.0656(10) Uani 1 1 d . . . H43 H 0.8531 1.2751 0.7742 0.079 Uiso 1 1 calc R . . C44 C 0.6070(5) 1.1699(4) 0.74832(19) 0.0646(10) Uani 1 1 d . . . H44 H 0.5891 1.2542 0.7601 0.078 Uiso 1 1 calc R . . C45 C 0.4753(4) 1.0355(4) 0.72290(18) 0.0562(9) Uani 1 1 d . . . H45 H 0.3669 1.0265 0.7177 0.067 Uiso 1 1 calc R . . C46 C 0.5027(4) 0.9154(4) 0.70538(16) 0.0469(7) Uani 1 1 d . . . H46 H 0.4121 0.8233 0.6874 0.056 Uiso 1 1 calc R . . C51 C 0.8896(3) 0.7687(3) 0.63922(13) 0.0390(6) Uani 1 1 d . . . C52 C 0.9539(4) 0.6671(4) 0.63434(15) 0.0465(7) Uani 1 1 d . . . H52 H 0.9110 0.5822 0.6532 0.056 Uiso 1 1 calc R . . C53 C 1.0806(4) 0.6878(4) 0.60210(17) 0.0564(9) Uani 1 1 d . . . H53 H 1.1236 0.6173 0.5987 0.068 Uiso 1 1 calc R . . C54 C 1.1425(4) 0.8111(5) 0.57523(18) 0.0618(10) Uani 1 1 d . . . H54 H 1.2288 0.8258 0.5531 0.074 Uiso 1 1 calc R . . C55 C 1.0815(4) 0.9130(4) 0.57994(18) 0.0598(9) Uani 1 1 d . . . H55 H 1.1255 0.9980 0.5612 0.072 Uiso 1 1 calc R . . C56 C 0.9554(4) 0.8925(4) 0.61204(16) 0.0495(7) Uani 1 1 d . . . H56 H 0.9138 0.9641 0.6154 0.059 Uiso 1 1 calc R . . C61 C 0.4654(3) 0.5510(3) 0.64026(13) 0.0372(6) Uani 1 1 d . . . C62 C 0.3676(4) 0.4573(4) 0.67483(15) 0.0525(8) Uani 1 1 d . . . H62 H 0.4037 0.4712 0.7196 0.063 Uiso 1 1 calc R . . C63 C 0.2168(4) 0.3427(4) 0.64509(17) 0.0615(10) Uani 1 1 d . . . H63 H 0.1509 0.2786 0.6695 0.074 Uiso 1 1 calc R . . C64 C 0.1637(4) 0.3227(4) 0.58055(16) 0.0530(8) Uani 1 1 d . . . H64 H 0.0598 0.2458 0.5603 0.064 Uiso 1 1 calc R . . C65 C 0.2599(4) 0.4134(4) 0.54499(15) 0.0511(8) Uani 1 1 d . . . H65 H 0.2236 0.3981 0.5001 0.061 Uiso 1 1 calc R . . C66 C 0.4107(4) 0.5278(3) 0.57475(14) 0.0459(7) Uani 1 1 d . . . H66 H 0.4768 0.5905 0.5500 0.055 Uiso 1 1 calc R . . H1 H 1.1092 0.9114 0.7845 0.050 Uiso 1 1 d 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 Sn1 0.03112(11) 0.03807(13) 0.03554(13) 0.00326(8) 0.00572(8) 0.01124(9) Cl1 0.0920(8) 0.0786(7) 0.1032(9) 0.0335(7) 0.0265(7) 0.0393(7) C1 0.081(3) 0.078(3) 0.103(4) 0.011(3) 0.040(3) 0.030(3) B1 0.0300(14) 0.0316(15) 0.0341(16) 0.0062(12) 0.0041(12) 0.0146(12) Cl2 0.0991(11) 0.1331(13) 0.1214(13) -0.0350(11) 0.0353(10) -0.0254(10) S11 0.0332(3) 0.0338(4) 0.0361(4) 0.0021(3) 0.0024(3) 0.0103(3) N11 0.0294(11) 0.0323(11) 0.0339(12) 0.0011(9) 0.0012(9) 0.0146(9) C11 0.0278(12) 0.0413(15) 0.0329(14) 0.0051(12) 0.0038(10) 0.0163(11) N12 0.0311(12) 0.0547(15) 0.0466(15) -0.0011(12) 0.0073(10) 0.0216(11) C12 0.0402(15) 0.0403(16) 0.0417(17) -0.0066(13) -0.0006(12) 0.0203(13) C13 0.0456(17) 0.0546(19) 0.0480(19) -0.0076(15) 0.0058(14) 0.0268(15) C14 0.0311(16) 0.074(2) 0.078(3) -0.004(2) 0.0135(16) 0.0203(16) S21 0.0441(4) 0.0376(4) 0.0315(4) 0.0046(3) 0.0098(3) 0.0143(3) N21 0.0267(10) 0.0298(11) 0.0326(12) 0.0055(9) 0.0059(8) 0.0119(9) C21 0.0254(12) 0.0282(13) 0.0355(14) 0.0066(11) 0.0045(10) 0.0088(10) N22 0.0410(13) 0.0282(11) 0.0402(13) 0.0088(10) 0.0098(10) 0.0143(10) C22 0.0309(13) 0.0362(14) 0.0334(14) 0.0063(11) 0.0086(11) 0.0139(11) C23 0.0422(15) 0.0360(15) 0.0412(16) 0.0053(12) 0.0133(12) 0.0182(13) C24 0.075(2) 0.0396(17) 0.056(2) 0.0184(15) 0.0220(18) 0.0273(17) S31 0.0485(4) 0.0417(4) 0.0578(5) 0.0209(4) 0.0107(4) 0.0251(3) N31 0.0274(10) 0.0302(11) 0.0386(13) 0.0090(9) 0.0039(9) 0.0110(9) C31 0.0317(13) 0.0312(14) 0.0435(16) 0.0073(12) 0.0100(11) 0.0144(11) N32 0.0355(12) 0.0304(12) 0.0475(15) 0.0079(11) 0.0050(11) 0.0055(10) C32 0.0363(14) 0.0393(16) 0.0440(17) 0.0126(13) -0.0010(12) 0.0128(12) C33 0.0358(15) 0.0419(16) 0.0472(18) 0.0106(14) -0.0022(13) 0.0075(13) C34 0.058(2) 0.0326(17) 0.077(3) 0.0123(16) 0.0081(18) 0.0016(15) C41 0.0347(14) 0.0400(15) 0.0392(16) 0.0073(12) 0.0066(12) 0.0130(12) C42 0.0370(16) 0.0439(17) 0.062(2) 0.0022(15) 0.0031(14) 0.0123(14) C43 0.057(2) 0.0428(19) 0.080(3) -0.0043(18) 0.0056(19) 0.0120(17) C44 0.074(3) 0.054(2) 0.072(3) 0.0019(19) 0.018(2) 0.035(2) C45 0.0513(19) 0.063(2) 0.062(2) 0.0123(18) 0.0148(17) 0.0308(18) C46 0.0365(15) 0.0490(18) 0.0497(18) 0.0030(14) 0.0067(13) 0.0152(14) C51 0.0301(13) 0.0449(16) 0.0329(15) -0.0001(12) 0.0045(11) 0.0099(12) C52 0.0444(17) 0.0518(18) 0.0421(17) 0.0046(14) 0.0075(13) 0.0212(15) C53 0.0482(19) 0.072(2) 0.051(2) -0.0051(17) 0.0028(15) 0.0346(18) C54 0.0410(18) 0.080(3) 0.052(2) 0.0001(19) 0.0135(15) 0.0165(18) C55 0.0489(19) 0.061(2) 0.060(2) 0.0138(18) 0.0203(16) 0.0108(17) C56 0.0418(16) 0.0491(18) 0.0514(19) 0.0078(15) 0.0120(14) 0.0133(14) C61 0.0322(13) 0.0372(15) 0.0363(15) 0.0018(12) 0.0040(11) 0.0113(12) C62 0.0421(17) 0.059(2) 0.0356(17) 0.0064(15) 0.0026(13) 0.0039(15) C63 0.0490(19) 0.059(2) 0.048(2) 0.0095(17) 0.0045(15) -0.0026(16) C64 0.0403(17) 0.0506(19) 0.0488(19) -0.0014(15) -0.0055(14) 0.0082(15) C65 0.0537(19) 0.054(2) 0.0335(16) -0.0015(14) -0.0038(14) 0.0185(16) C66 0.0468(17) 0.0489(18) 0.0347(16) 0.0065(13) 0.0085(13) 0.0141(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 Sn1 C41 2.121(3) . ? Sn1 C51 2.128(3) . ? Sn1 C61 2.140(3) . ? Sn1 S11 2.4569(10) . ? Cl1 C1 1.730(5) . ? C1 Cl2 1.713(5) . ? B1 N31 1.542(4) . ? B1 N21 1.550(4) . ? B1 N11 1.572(4) . ? S11 C11 1.740(3) . ? N11 C11 1.337(3) . ? N11 C12 1.375(4) . ? C11 N12 1.351(3) . ? N12 C13 1.370(4) . ? N12 C14 1.459(4) . ? C12 C13 1.339(4) . ? S21 C21 1.690(3) . ? N21 C21 1.364(3) . ? N21 C22 1.384(3) . ? C21 N22 1.361(3) . ? N22 C23 1.383(4) . ? N22 C24 1.464(4) . ? C22 C23 1.341(4) . ? S31 C31 1.690(3) . ? N31 C31 1.369(3) . ? N31 C32 1.387(4) . ? C31 N32 1.353(4) . ? N32 C33 1.373(4) . ? N32 C34 1.459(4) . ? C32 C33 1.335(4) . ? C41 C42 1.397(4) . ? C41 C46 1.393(4) . ? C42 C43 1.377(5) . ? C43 C44 1.372(5) . ? C44 C45 1.383(5) . ? C45 C46 1.368(5) . ? C51 C56 1.384(4) . ? C51 C52 1.385(4) . ? C52 C53 1.392(5) . ? C53 C54 1.372(5) . ? C54 C55 1.365(5) . ? C55 C56 1.386(5) . ? C61 C62 1.379(4) . ? C61 C66 1.389(4) . ? C62 C63 1.392(5) . ? C63 C64 1.370(5) . ? C64 C65 1.373(5) . ? C65 C66 1.391(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 C41 Sn1 C51 113.78(12) . . ? C41 Sn1 C61 111.29(11) . . ? C51 Sn1 C61 115.10(11) . . ? C41 Sn1 S11 107.40(8) . . ? C51 Sn1 S11 107.12(8) . . ? C61 Sn1 S11 100.95(9) . . ? Cl2 C1 Cl1 113.1(3) . . ? N31 B1 N21 110.4(2) . . ? N31 B1 N11 108.4(2) . . ? N21 B1 N11 109.5(2) . . ? C11 S11 Sn1 99.79(10) . . ? C11 N11 C12 107.7(2) . . ? C11 N11 B1 125.3(2) . . ? C12 N11 B1 127.0(2) . . ? N11 C11 N12 108.5(2) . . ? N11 C11 S11 126.9(2) . . ? N12 C11 S11 124.5(2) . . ? C11 N12 C13 108.2(2) . . ? C11 N12 C14 126.3(3) . . ? C13 N12 C14 125.5(3) . . ? C13 C12 N11 108.4(3) . . ? C12 C13 N12 107.3(3) . . ? C21 N21 C22 108.3(2) . . ? C21 N21 B1 130.0(2) . . ? C22 N21 B1 121.4(2) . . ? N22 C21 N21 106.4(2) . . ? N22 C21 S21 124.8(2) . . ? N21 C21 S21 128.83(19) . . ? C21 N22 C23 109.8(2) . . ? C21 N22 C24 124.5(2) . . ? C23 N22 C24 125.7(2) . . ? C23 C22 N21 108.8(2) . . ? C22 C23 N22 106.7(2) . . ? C31 N31 C32 107.9(2) . . ? C31 N31 B1 125.2(2) . . ? C32 N31 B1 126.8(2) . . ? N32 C31 N31 106.6(2) . . ? N32 C31 S31 126.1(2) . . ? N31 C31 S31 127.3(2) . . ? C31 N32 C33 109.8(2) . . ? C31 N32 C34 125.3(3) . . ? C33 N32 C34 124.9(3) . . ? C33 C32 N31 108.5(3) . . ? C32 C33 N32 107.3(3) . . ? C42 C41 C46 118.3(3) . . ? C42 C41 Sn1 122.4(2) . . ? C46 C41 Sn1 119.3(2) . . ? C43 C42 C41 119.9(3) . . ? C44 C43 C42 120.7(3) . . ? C43 C44 C45 120.3(3) . . ? C46 C45 C44 119.3(3) . . ? C45 C46 C41 121.5(3) . . ? C56 C51 C52 118.6(3) . . ? C56 C51 Sn1 121.1(2) . . ? C52 C51 Sn1 120.3(2) . . ? C51 C52 C53 120.9(3) . . ? C54 C53 C52 119.3(3) . . ? C55 C54 C53 120.7(3) . . ? C54 C55 C56 120.1(3) . . ? C51 C56 C55 120.5(3) . . ? C62 C61 C66 118.4(3) . . ? C62 C61 Sn1 120.8(2) . . ? C66 C61 Sn1 120.7(2) . . ? C61 C62 C63 121.0(3) . . ? C64 C63 C62 119.7(3) . . ? C63 C64 C65 120.3(3) . . ? C64 C65 C66 119.9(3) . . ? C61 C66 C65 120.6(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.617 _refine_diff_density_min -0.877 _refine_diff_density_rms 0.101 data_c:\docume~1\admini~1\desktop\newxta~1\mks40\mks40 _database_code_depnum_ccdc_archive 'CCDC 252476' _audit_creation_method SHELXL-97 #==== # 4. TEXT _publ_section_abstract #Text of the abstract ; The crystal structure of [C16 H22 B1 N4 S2 Cl4 Nb] is reported. ; _publ_section_comment #Text of the paper ; The crystallographic asymmetric unit consists of one molecule of [C16 H22 B1 N4 S2 Cl4 Nb] and half a molecule of disordered cyclohexane. Hydrogen atoms attached to C atoms were included at idealized positions and ride on the atom to which they bonded. The hydrogen atom attached to boron was located but not refined. ; _publ_section_exptl_refinement # see also _refine_ls_hydrogen for refinement keywords. ; Hydrogen atoms attached to C atoms were included at idealized positions and ride on the atom to which they bonded. The hydrogen atom attached to boron was located but not refined. ; _publ_section_exptl_prep ; The compound was prepared by MKS and recrystallized from tetrahydrofuran and cyclohexane. The sample ID is mks39. . ; #===== _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H44 B2 Cl8 N8 Nb2 S4' _chemical_formula_weight 1160.03 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.983(5) _cell_length_b 10.429(5) _cell_length_c 16.715(5) _cell_angle_alpha 90 _cell_angle_beta 109.247(5) _cell_angle_gamma 90 _cell_volume 4276(3) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 33836 _cell_measurement_theta_min 27.48 _cell_measurement_theta_max 2.91 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.802 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2336 _exptl_absorpt_coefficient_mu 1.270 # Absorption correction loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 0 0.100 -1 0 0 0.080 0 1 0 0.050 0 -1 0 0.030 0 0 1 0.080 0 0 -1 0.070 1 0 -1 0.047 -1 -1 1 0.026 -3 1 3 0.036 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.910 _exptl_absorpt_correction_T_max 0.958 _exptl_absorpt_process_details ; Gaussian integration (Coppens, 1970) ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CCD _diffrn_measurement_method ' \f and \w scans with CCD ' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 46909 _diffrn_reflns_av_R_equivalents 0.0625 _diffrn_reflns_av_sigmaI/netI 0.0267 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4905 _reflns_number_gt 4095 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction 'X -Seed' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed / POV-Ray' _computing_publication_material 'Microsoft Office 2000' _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^)+(0.0567P)^2^+7.2805P] 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 0.00094(14) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4905 _refine_ls_number_parameters 259 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0481 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.1034 _refine_ls_wR_factor_gt 0.0958 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.041 _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 Nb1 Nb 0.377563(10) 0.33375(3) 0.824661(16) 0.03187(11) Uani 1 1 d . . . Cl1 Cl 0.31917(3) 0.23503(9) 0.89971(5) 0.0439(2) Uani 1 1 d . . . C1 C 0.45747(19) 0.4698(5) 0.8853(3) 0.0693(13) Uani 1 1 d . . . H1 H 0.4661 0.5308 0.8495 0.083 Uiso 1 1 calc R . . B1 B 0.40860(15) 0.1396(3) 0.6092(2) 0.0352(7) Uani 1 1 d . . . H1B1 H 0.4418(16) 0.163(4) 0.659(2) 0.050 Uiso 1 1 d . . . Cl2 Cl 0.31851(3) 0.52268(8) 0.80155(5) 0.0453(2) Uani 1 1 d . . . C2 C 0.42480(19) 0.4914(5) 0.9347(3) 0.0733(15) Uani 1 1 d . . . H2 H 0.4073 0.5698 0.9390 0.088 Uiso 1 1 calc R . . Cl3 Cl 0.30137(3) 0.25884(7) 0.70393(4) 0.03361(17) Uani 1 1 d . . . C3 C 0.42212(16) 0.3810(6) 0.9757(3) 0.0724(15) Uani 1 1 d . . . H3 H 0.4022 0.3691 1.0137 0.087 Uiso 1 1 calc R . . Cl4 Cl 0.42831(4) 0.06185(9) 0.52281(5) 0.0500(2) Uani 1 1 d . . . C4 C 0.45320(17) 0.2875(4) 0.9532(2) 0.0621(11) Uani 1 1 d . . . H4 H 0.4583 0.2013 0.9726 0.074 Uiso 1 1 calc R . . C5 C 0.47523(14) 0.3451(5) 0.8969(3) 0.0591(11) Uani 1 1 d . . . H5 H 0.4986 0.3051 0.8710 0.071 Uiso 1 1 calc R . . C6 C 0.4488(3) -0.2361(6) 0.7611(8) 0.128(3) Uani 1 1 d U . . H6A H 0.4235 -0.1659 0.7625 0.154 Uiso 1 1 calc R . . H6B H 0.4343 -0.3187 0.7736 0.154 Uiso 1 1 calc R . . C7 C 0.4582(4) -0.2391(9) 0.6939(6) 0.135(4) Uani 1 1 d U . . H7A H 0.4336 -0.1765 0.6553 0.163 Uiso 1 1 calc R . . H7B H 0.4476 -0.3251 0.6689 0.163 Uiso 1 1 calc R . . C8 C 0.5070(5) -0.2166(19) 0.6932(9) 0.326(13) Uani 1 1 d U . . H8A H 0.5070 -0.2555 0.6392 0.391 Uiso 1 1 calc R . . H8B H 0.5068 -0.1228 0.6838 0.391 Uiso 1 1 calc R . . S11 S 0.41548(3) 0.11703(8) 0.80895(4) 0.03362(17) Uani 1 1 d . . . N11 N 0.37448(10) 0.0423(2) 0.64135(15) 0.0339(5) Uani 1 1 d . . . C11 C 0.37308(11) 0.0365(3) 0.72087(19) 0.0327(6) Uani 1 1 d . . . N12 N 0.33565(10) -0.0503(3) 0.72371(17) 0.0368(6) Uani 1 1 d . . . C12 C 0.33593(13) -0.0428(3) 0.5932(2) 0.0404(7) Uani 1 1 d . . . H12 H 0.3278 -0.0584 0.5343 0.049 Uiso 1 1 calc R . . C13 C 0.31198(13) -0.0998(3) 0.6436(2) 0.0405(7) Uani 1 1 d . . . H13 H 0.2839 -0.1625 0.6271 0.049 Uiso 1 1 calc R . . C14 C 0.32268(15) -0.0868(4) 0.7989(2) 0.0503(9) Uani 1 1 d . . . H14A H 0.3553 -0.0782 0.8490 0.075 Uiso 1 1 calc R . . H14B H 0.3101 -0.1759 0.7935 0.075 Uiso 1 1 calc R . . H14C H 0.2939 -0.0307 0.8048 0.075 Uiso 1 1 calc R . . S21 S 0.41301(3) 0.41497(8) 0.70841(5) 0.03666(18) Uani 1 1 d . . . N21 N 0.37116(10) 0.2557(3) 0.57036(15) 0.0361(6) Uani 1 1 d . . . C21 C 0.36862(13) 0.3661(3) 0.61056(19) 0.0355(6) Uani 1 1 d . . . N22 N 0.32704(11) 0.4365(3) 0.56054(17) 0.0401(6) Uani 1 1 d . . . C22 C 0.32905(14) 0.2579(4) 0.4940(2) 0.0428(7) Uani 1 1 d . . . H22 H 0.3206 0.1916 0.4527 0.051 Uiso 1 1 calc R . . C23 C 0.30211(14) 0.3683(4) 0.4877(2) 0.0454(8) Uani 1 1 d . . . H23 H 0.2714 0.3949 0.4416 0.054 Uiso 1 1 calc R . . C24 C 0.30847(16) 0.5588(4) 0.5827(2) 0.0519(9) Uani 1 1 d . . . H24A H 0.2770 0.5448 0.6016 0.078 Uiso 1 1 calc R . . H24B H 0.2979 0.6152 0.5330 0.078 Uiso 1 1 calc R . . H24C H 0.3380 0.5990 0.6284 0.078 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 Nb1 0.02623(16) 0.04090(18) 0.02760(15) -0.00509(10) 0.00768(11) 0.00140(10) Cl1 0.0381(4) 0.0612(5) 0.0363(4) 0.0057(3) 0.0176(3) 0.0060(3) C1 0.072(3) 0.070(3) 0.047(2) -0.010(2) -0.007(2) -0.036(2) B1 0.0364(17) 0.0383(18) 0.0343(17) -0.0054(14) 0.0162(14) -0.0024(14) Cl2 0.0436(4) 0.0462(5) 0.0433(4) -0.0069(3) 0.0108(3) 0.0106(3) C2 0.059(3) 0.076(3) 0.063(3) -0.039(2) -0.010(2) 0.014(2) Cl3 0.0258(3) 0.0423(4) 0.0309(3) -0.0021(3) 0.0069(3) 0.0003(3) C3 0.041(2) 0.135(5) 0.039(2) -0.034(3) 0.0088(16) -0.016(3) Cl4 0.0521(5) 0.0602(5) 0.0448(4) -0.0136(4) 0.0258(4) -0.0010(4) C4 0.057(2) 0.061(2) 0.043(2) -0.0016(18) -0.0176(18) -0.0057(19) C5 0.0248(16) 0.091(3) 0.056(2) -0.038(2) 0.0062(15) -0.0059(17) C6 0.089(5) 0.056(3) 0.246(11) 0.045(5) 0.063(7) 0.024(3) C7 0.101(6) 0.119(6) 0.131(7) 0.015(6) -0.037(5) -0.015(5) C8 0.089(7) 0.58(3) 0.300(18) 0.29(2) 0.053(9) 0.103(12) S11 0.0281(3) 0.0402(4) 0.0310(4) -0.0014(3) 0.0077(3) 0.0014(3) N11 0.0303(12) 0.0363(13) 0.0341(12) -0.0052(10) 0.0094(10) -0.0026(10) C11 0.0274(13) 0.0339(15) 0.0366(15) 0.0011(12) 0.0102(12) 0.0007(11) N12 0.0302(12) 0.0365(14) 0.0426(14) 0.0015(11) 0.0105(11) -0.0024(10) C12 0.0364(16) 0.0398(17) 0.0395(16) -0.0107(13) 0.0048(13) -0.0038(13) C13 0.0309(15) 0.0360(17) 0.0475(18) -0.0043(14) 0.0033(13) -0.0044(12) C14 0.0467(19) 0.057(2) 0.051(2) 0.0100(17) 0.0217(16) -0.0079(16) S21 0.0354(4) 0.0383(4) 0.0374(4) -0.0040(3) 0.0136(3) -0.0054(3) N21 0.0364(13) 0.0450(15) 0.0292(12) -0.0025(11) 0.0138(10) -0.0053(11) C21 0.0364(15) 0.0406(16) 0.0340(15) 0.0044(12) 0.0178(13) -0.0001(12) N22 0.0424(14) 0.0435(15) 0.0369(13) 0.0081(11) 0.0165(12) 0.0032(12) C22 0.0416(17) 0.059(2) 0.0285(15) -0.0016(14) 0.0122(13) -0.0035(15) C23 0.0407(17) 0.064(2) 0.0311(15) 0.0080(15) 0.0115(13) 0.0029(16) C24 0.060(2) 0.049(2) 0.0477(19) 0.0082(16) 0.0189(17) 0.0128(17) _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 Nb1 C5 2.427(3) . ? Nb1 C4 2.434(4) . ? Nb1 C1 2.442(4) . ? Nb1 Cl3 2.4430(8) . ? Nb1 Cl2 2.4485(11) . ? Nb1 C3 2.455(4) . ? Nb1 C2 2.470(4) . ? Nb1 Cl1 2.4881(9) . ? Nb1 S11 2.5137(13) . ? Nb1 S21 2.5537(10) . ? C1 C5 1.372(7) . ? C1 C2 1.384(7) . ? B1 N21 1.555(5) . ? B1 N11 1.555(4) . ? B1 Cl4 1.869(4) . ? C2 C3 1.353(7) . ? C3 C4 1.394(7) . ? C4 C5 1.388(6) . ? C6 C8 1.168(12) 2_656 ? C6 C7 1.227(11) . ? C7 C8 1.292(12) . ? C7 C8 1.818(14) 2_656 ? C8 C6 1.168(12) 2_656 ? C8 C7 1.818(14) 2_656 ? S11 C11 1.737(3) . ? N11 C11 1.343(4) . ? N11 C12 1.381(4) . ? C11 N12 1.341(4) . ? N12 C13 1.377(4) . ? N12 C14 1.455(4) . ? C12 C13 1.340(5) . ? S21 C21 1.738(3) . ? N21 C21 1.346(4) . ? N21 C22 1.380(4) . ? C21 N22 1.345(4) . ? N22 C23 1.373(5) . ? N22 C24 1.455(5) . ? C22 C23 1.334(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 C5 Nb1 C4 33.18(16) . . ? C5 Nb1 C1 32.73(16) . . ? C4 Nb1 C1 54.56(16) . . ? C5 Nb1 Cl3 148.90(9) . . ? C4 Nb1 Cl3 149.80(11) . . ? C1 Nb1 Cl3 151.07(11) . . ? C5 Nb1 Cl2 122.50(11) . . ? C4 Nb1 Cl2 125.46(11) . . ? C1 Nb1 Cl2 90.05(14) . . ? Cl3 Nb1 Cl2 80.32(3) . . ? C5 Nb1 C3 54.35(14) . . ? C4 Nb1 C3 33.13(16) . . ? C1 Nb1 C3 53.74(16) . . ? Cl3 Nb1 C3 153.20(11) . . ? Cl2 Nb1 C3 93.40(14) . . ? C5 Nb1 C2 54.24(14) . . ? C4 Nb1 C2 54.29(16) . . ? C1 Nb1 C2 32.72(17) . . ? Cl3 Nb1 C2 153.67(11) . . ? Cl2 Nb1 C2 73.37(11) . . ? C3 Nb1 C2 31.89(17) . . ? C5 Nb1 Cl1 118.71(12) . . ? C4 Nb1 Cl1 85.54(12) . . ? C1 Nb1 Cl1 127.42(12) . . ? Cl3 Nb1 Cl1 79.71(3) . . ? Cl2 Nb1 Cl1 87.59(4) . . ? C3 Nb1 Cl1 73.98(12) . . ? C2 Nb1 Cl1 97.82(15) . . ? C5 Nb1 S11 73.40(11) . . ? C4 Nb1 S11 71.58(11) . . ? C1 Nb1 S11 104.88(14) . . ? Cl3 Nb1 S11 82.24(3) . . ? Cl2 Nb1 S11 162.53(3) . . ? C3 Nb1 S11 102.69(15) . . ? C2 Nb1 S11 124.09(11) . . ? Cl1 Nb1 S11 90.33(4) . . ? C5 Nb1 S21 77.44(12) . . ? C4 Nb1 S21 110.39(12) . . ? C1 Nb1 S21 69.66(11) . . ? Cl3 Nb1 S21 82.81(3) . . ? Cl2 Nb1 S21 88.71(3) . . ? C3 Nb1 S21 123.34(12) . . ? C2 Nb1 S21 97.49(16) . . ? Cl1 Nb1 S21 162.50(3) . . ? S11 Nb1 S21 88.09(3) . . ? C5 C1 C2 108.3(4) . . ? C5 C1 Nb1 73.1(2) . . ? C2 C1 Nb1 74.8(3) . . ? N21 B1 N11 107.6(3) . . ? N21 B1 Cl4 108.0(2) . . ? N11 B1 Cl4 108.5(2) . . ? C3 C2 C1 107.9(4) . . ? C3 C2 Nb1 73.4(2) . . ? C1 C2 Nb1 72.5(2) . . ? C2 C3 C4 109.1(4) . . ? C2 C3 Nb1 74.7(2) . . ? C4 C3 Nb1 72.6(2) . . ? C5 C4 C3 106.6(4) . . ? C5 C4 Nb1 73.1(2) . . ? C3 C4 Nb1 74.2(2) . . ? C1 C5 C4 108.1(4) . . ? C1 C5 Nb1 74.2(2) . . ? C4 C5 Nb1 73.7(2) . . ? C8 C6 C7 98.8(9) 2_656 . ? C6 C7 C8 119.7(10) . . ? C6 C7 C8 39.4(6) . 2_656 ? C8 C7 C8 80.3(10) . 2_656 ? C6 C8 C7 135.9(12) 2_656 . ? C6 C8 C7 41.8(7) 2_656 2_656 ? C7 C8 C7 97.0(8) . 2_656 ? C11 S11 Nb1 111.24(10) . . ? C11 N11 C12 107.3(3) . . ? C11 N11 B1 125.1(2) . . ? C12 N11 B1 127.2(3) . . ? N12 C11 N11 108.8(3) . . ? N12 C11 S11 124.1(2) . . ? N11 C11 S11 126.9(2) . . ? C11 N12 C13 108.4(3) . . ? C11 N12 C14 125.8(3) . . ? C13 N12 C14 125.9(3) . . ? C13 C12 N11 108.4(3) . . ? C12 C13 N12 107.1(3) . . ? C21 S21 Nb1 108.96(10) . . ? C21 N21 C22 107.0(3) . . ? C21 N21 B1 125.8(3) . . ? C22 N21 B1 126.5(3) . . ? N21 C21 N22 108.6(3) . . ? N21 C21 S21 126.4(2) . . ? N22 C21 S21 124.9(3) . . ? C21 N22 C23 108.4(3) . . ? C21 N22 C24 125.9(3) . . ? C23 N22 C24 125.5(3) . . ? C23 C22 N21 108.8(3) . . ? C22 C23 N22 107.2(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.064 _refine_diff_density_min -0.736 _refine_diff_density_rms 0.088 #===== data_c:\docume~1\admini~1\desktop\newxta~1\mks39\mks39 _database_code_depnum_ccdc_archive 'CCDC 252477' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6.50 H8 B0.50 Cl2 N2 S Ta0.50' _chemical_formula_weight 312.99 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 11.343(5) _cell_length_b 12.087(5) _cell_length_c 13.837(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1897.1(13) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 15740 _cell_measurement_theta_min 27.48 _cell_measurement_theta_max 2.91 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.147 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.192 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1200 _exptl_absorpt_coefficient_mu 6.583 # Absorption correction loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 0 0.150 -1 0 0 0.160 0 1 0 0.080 0 -1 0 0.160 0 0 1 0.060 1 -1 0 0.087 -1 0 -16 0.102 -1 0 3 0.082 -1 1 0 0.091 3 -4 -8 0.086 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.090 _exptl_absorpt_correction_T_max 0.260 _exptl_absorpt_process_details ; Gaussian integration (Coppens, 1970) ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CCD _diffrn_measurement_method ' \f and \w scans with CCD ' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 24989 _diffrn_reflns_av_R_equivalents 0.0898 _diffrn_reflns_av_sigmaI/netI 0.0318 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 27.49 _reflns_number_total 2270 _reflns_number_gt 2055 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction 'X -Seed' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed / POV-Ray' _computing_publication_material 'Microsoft Office 2000' _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^)+(0.0523P)^2^+1.2594P] 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 0.0031(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2270 _refine_ls_number_parameters 125 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0359 _refine_ls_R_factor_gt 0.0317 _refine_ls_wR_factor_ref 0.0816 _refine_ls_wR_factor_gt 0.0783 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.098 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ta1 Ta 0.329293(16) 0.2500 0.082317(15) 0.02335(12) Uani 1 2 d S . . Cl1 Cl 0.25095(8) 0.38959(9) 0.19312(7) 0.0369(2) Uani 1 1 d . . . C1 C 0.4824(5) 0.2500 0.2040(5) 0.0385(13) Uani 1 2 d S . . H1 H 0.4590 0.2500 0.2699 0.046 Uiso 1 2 calc SR . . B1 B 0.2194(6) 0.2500 -0.2200(5) 0.0309(12) Uani 1 2 d S . . Cl2 Cl 0.12121(10) 0.2500 0.03561(9) 0.0283(3) Uani 1 2 d S . . C2 C 0.5027(3) 0.1564(4) 0.1468(3) 0.0345(9) Uani 1 1 d . . . H2 H 0.4960 0.0817 0.1674 0.041 Uiso 1 1 calc R . . Cl3 Cl 0.18652(18) 0.2500 -0.35191(13) 0.0529(4) Uani 1 2 d S . . C3 C 0.5343(3) 0.1917(3) 0.0546(3) 0.0327(8) Uani 1 1 d . . . H3 H 0.5526 0.1454 0.0012 0.039 Uiso 1 1 calc R . . S11 S 0.34569(8) 0.10319(8) -0.04911(8) 0.0289(2) Uani 1 1 d . . . N11 N 0.1630(3) 0.1450(3) -0.1762(3) 0.0307(7) Uani 1 1 d . . . C11 C 0.2104(4) 0.0833(3) -0.1055(3) 0.0290(8) Uani 1 1 d . . . N12 N 0.1370(3) -0.0006(3) -0.0852(2) 0.0312(7) Uani 1 1 d . . . C12 C 0.0542(4) 0.0989(4) -0.1985(3) 0.0360(9) Uani 1 1 d . . . H12 H 0.0000 0.1264 -0.2450 0.043 Uiso 1 1 calc R . . C13 C 0.0385(3) 0.0084(4) -0.1430(3) 0.0366(9) Uani 1 1 d . . . H13 H -0.0277 -0.0398 -0.1436 0.044 Uiso 1 1 calc R . . C14 C 0.1638(3) -0.0928(4) -0.0205(4) 0.0388(10) Uani 1 1 d . . . H14A H 0.2204 -0.1425 -0.0518 0.058 Uiso 1 1 calc R . . H14B H 0.0912 -0.1335 -0.0059 0.058 Uiso 1 1 calc R . . H14C H 0.1979 -0.0642 0.0396 0.058 Uiso 1 1 calc R . . H1B1 H 0.310(7) 0.2500 -0.226(6) 0.050 Uiso 1 2 d S . . 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 Ta1 0.01837(15) 0.02361(16) 0.02806(17) 0.000 -0.00084(7) 0.000 Cl1 0.0286(4) 0.0409(5) 0.0412(6) -0.0131(4) -0.0009(4) 0.0038(4) C1 0.028(3) 0.055(4) 0.033(3) 0.000 -0.004(2) 0.000 B1 0.033(3) 0.032(3) 0.028(3) 0.000 0.000(2) 0.000 Cl2 0.0200(5) 0.0295(6) 0.0354(7) 0.000 -0.0010(5) 0.000 C2 0.0200(16) 0.037(2) 0.047(2) 0.0084(18) -0.0054(15) 0.0032(15) Cl3 0.0719(11) 0.0573(11) 0.0296(8) 0.000 -0.0046(7) 0.000 C3 0.0170(16) 0.036(2) 0.045(2) -0.0063(19) -0.0045(16) 0.0016(15) S11 0.0238(4) 0.0253(5) 0.0377(5) -0.0037(4) -0.0031(4) 0.0014(3) N11 0.0286(16) 0.0297(17) 0.0337(19) -0.0041(15) -0.0034(12) -0.0004(12) C11 0.0280(18) 0.0270(19) 0.0320(19) -0.0045(16) 0.0005(16) 0.0011(15) N12 0.0280(16) 0.0263(17) 0.039(2) -0.0046(13) -0.0013(13) -0.0046(15) C12 0.0283(18) 0.039(2) 0.041(2) -0.0074(18) -0.0097(16) 0.0007(16) C13 0.0273(18) 0.036(2) 0.046(2) -0.0099(18) -0.0026(16) -0.0024(16) C14 0.033(2) 0.029(2) 0.055(3) 0.001(2) 0.0018(17) -0.0024(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ta1 C1 2.419(6) . ? Ta1 C2 2.438(4) 8_565 ? Ta1 C2 2.438(4) . ? Ta1 Cl1 2.4469(11) . ? Ta1 Cl1 2.4469(11) 8_565 ? Ta1 Cl2 2.4472(16) . ? Ta1 C3 2.460(4) 8_565 ? Ta1 C3 2.460(4) . ? Ta1 S11 2.5477(13) . ? Ta1 S11 2.5477(13) 8_565 ? C1 C2 1.400(6) . ? C1 C2 1.400(6) 8_565 ? B1 N11 1.545(5) 8_565 ? B1 N11 1.545(5) . ? B1 Cl3 1.862(7) . ? C2 C3 1.393(6) . ? C3 C3 1.410(8) 8_565 ? S11 C11 1.738(4) . ? N11 C11 1.342(5) . ? N11 C12 1.390(5) . ? C11 N12 1.343(5) . ? N12 C13 1.379(5) . ? N12 C14 1.461(6) . ? C12 C13 1.348(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 C1 Ta1 C2 33.50(13) . 8_565 ? C1 Ta1 C2 33.50(13) . . ? C2 Ta1 C2 55.3(2) 8_565 . ? C1 Ta1 Cl1 79.89(11) . . ? C2 Ta1 Cl1 75.14(10) 8_565 . ? C2 Ta1 Cl1 112.56(11) . . ? C1 Ta1 Cl1 79.89(11) . 8_565 ? C2 Ta1 Cl1 112.56(11) 8_565 8_565 ? C2 Ta1 Cl1 75.14(10) . 8_565 ? Cl1 Ta1 Cl1 87.19(6) . 8_565 ? C1 Ta1 Cl2 151.19(15) . . ? C2 Ta1 Cl2 151.00(10) 8_565 . ? C2 Ta1 Cl2 151.00(10) . . ? Cl1 Ta1 Cl2 79.35(4) . . ? Cl1 Ta1 Cl2 79.35(4) 8_565 . ? C1 Ta1 C3 55.26(17) . 8_565 ? C2 Ta1 C3 33.03(14) 8_565 8_565 ? C2 Ta1 C3 55.09(13) . 8_565 ? Cl1 Ta1 C3 104.09(10) . 8_565 ? Cl1 Ta1 C3 129.70(10) 8_565 8_565 ? Cl2 Ta1 C3 150.51(10) . 8_565 ? C1 Ta1 C3 55.26(17) . . ? C2 Ta1 C3 55.09(13) 8_565 . ? C2 Ta1 C3 33.03(14) . . ? Cl1 Ta1 C3 129.70(10) . . ? Cl1 Ta1 C3 104.09(10) 8_565 . ? Cl2 Ta1 C3 150.51(10) . . ? C3 Ta1 C3 33.32(19) 8_565 . ? C1 Ta1 S11 116.39(10) . . ? C2 Ta1 S11 121.71(10) 8_565 . ? C2 Ta1 S11 83.06(11) . . ? Cl1 Ta1 S11 162.57(3) . . ? Cl1 Ta1 S11 89.63(5) 8_565 . ? Cl2 Ta1 S11 83.22(3) . . ? C3 Ta1 S11 91.10(10) 8_565 . ? C3 Ta1 S11 67.66(10) . . ? C1 Ta1 S11 116.39(10) . 8_565 ? C2 Ta1 S11 83.06(11) 8_565 8_565 ? C2 Ta1 S11 121.71(10) . 8_565 ? Cl1 Ta1 S11 89.63(5) . 8_565 ? Cl1 Ta1 S11 162.57(3) 8_565 8_565 ? Cl2 Ta1 S11 83.22(3) . 8_565 ? C3 Ta1 S11 67.66(10) 8_565 8_565 ? C3 Ta1 S11 91.10(10) . 8_565 ? S11 Ta1 S11 88.29(6) . 8_565 ? C2 C1 C2 107.9(5) . 8_565 ? C2 C1 Ta1 74.0(3) . . ? C2 C1 Ta1 74.0(3) 8_565 . ? N11 B1 N11 110.4(5) 8_565 . ? N11 B1 Cl3 107.6(3) 8_565 . ? N11 B1 Cl3 107.6(3) . . ? C3 C2 C1 108.2(4) . . ? C3 C2 Ta1 74.3(2) . . ? C1 C2 Ta1 72.5(3) . . ? C2 C3 C3 107.8(3) . 8_565 ? C2 C3 Ta1 72.6(2) . . ? C3 C3 Ta1 73.34(10) 8_565 . ? C11 S11 Ta1 110.62(13) . . ? C11 N11 C12 107.2(3) . . ? C11 N11 B1 125.2(4) . . ? C12 N11 B1 127.6(4) . . ? N11 C11 N12 108.9(3) . . ? N11 C11 S11 127.2(3) . . ? N12 C11 S11 123.9(3) . . ? C11 N12 C13 108.7(4) . . ? C11 N12 C14 125.1(4) . . ? C13 N12 C14 125.8(4) . . ? C13 C12 N11 108.4(4) . . ? C12 C13 N12 106.7(4) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.862 _refine_diff_density_min -1.466 _refine_diff_density_rms 0.162