# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1628 #============================================================================== data_global #============================================================================== _audit_creation_date 28-07-99 _audit_creation_method from_SDP_and_SHELX97 _audit_update_record ; ? ; # 1. SUBMISSION DETAILS _publ_contact_author ; Ulli Englert Institut fuer Anorganische Chemie RWTH Aachen Prof.-Pirlet-Str.1 52074 Aachen Germany ; _publ_contact_author_email 'ullrich.englert@ac.rwth-aachen.de' _publ_contact_author_fax '(0241) 8888288' _publ_contact_author_phone '(0241) 804666' _publ_requested_journal 'Chemical Communications' _publ_requested_coeditor_name ? _publ_contact_letter ; ? ; # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? # 3. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis and structure of the first boron bridged constrained geometry complexes. ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Braunschweig, Holger' #<--'Last name, first name' ; Institut fuer Anorganische Chemie RWTH Aachen Prof.-Pirlet-Str.1 52074 Aachen Germany ; 'von Koblinski, Carsten' #<--'Last name, first name' ; Institut fuer Anorganische Chemie RWTH Aachen Prof.-Pirlet-Str.1 52074 Aachen Germany ; 'Englert, Ulli' #<--'Last name, first name' ; Institut fuer Anorganische Chemie RWTH Aachen Prof.-Pirlet-Str.1 52074 Aachen Germany ; # 4. TEXT _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_experimental ; Backgrounds were obtained from analysis of the scan profile (Blessing, Coppens _& Becker, 1974) ; _publ_section_references ; Blessing, R.H., Coppens, P. & Becker, P. (1974). J. Appl. Cryst., 7, 488-492. Enraf-Nonius, CAD4 Operations Manual, Delft, 1977. Fair, C.K. (1990). MolEN, An Interactive Intelligent System for Crystal Structure Analysis, User Manual, Enraf - Nonius, Delft, The Netherlands. International Tables for X-Ray Crystallography, T. Hahn E Vol. A, D. Reidel Publ. Comp., Dordrecht, (1983) Johnson, C.K. (1976). ORTEP. Report ORNL-5138. Oak Ridge National Laboratory, Tennessee, USA. ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ? ; data_KV6170799 # 5. CRYSTAL DATA _chemical_compound_source 'see paper' _exptl_crystal_description 'platelet' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.15 _chemical_name_systematic ; ? ; _chemical_name_common ; Complex 1 ; _chemical_formula_sum 'C21 H35 B1 N4 Ti1' _chemical_formula_weight 402.25 _symmetry_cell_setting triclinic _symmetry_space_group_name_h-m 'P-1' _cell_length_a 9.464(6) _cell_length_b 9.754(4) _cell_length_c 13.596(4) _cell_angle_alpha 101.94(2) _cell_angle_beta 102.32(4) _cell_angle_gamma 103.37(4) _cell_volume 1149(1) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 11 _cell_measurement_theta_max 13 _cell_formula_units_z 2.00 _exptl_crystal_density_diffrn 1.17 _exptl_crystal_density_meas none _diffrn_radiation_type Mo-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 0.380 _cell_measurement_temperature 213 _exptl_crystal_F_000 432 # 6. DATA COLLECTION _diffrn_ambient_temperature 213 _diffrn_measurement_device Enraf_Nonius_CAD4 _diffrn_measurement_method \q/2\q _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.000 _exptl_absorpt_correction_T_max 0.000 _diffrn_reflns_number 4351 _reflns_number_total 4351 _diffrn_reflns_av_R_equivalents 0.021 _diffrn_reflns_theta_min 3.1 _diffrn_reflns_theta_max 26.0 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_max 16 _diffrn_standards_number 3 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0.00 # 8. COMPUTING DATA _computing_data_collection CAD4_(Enraf-Nonius,_1977) _computing_cell_refinement CAD4_(Enraf-Nonius,_1977) _computing_data_reduction PROCESS_MolEN_(Fair,_1990) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _reflns_number_gt 3347 _reflns_threshold_expression >2sigma(I) _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 w=1/[\s^2^(Fo^2^)+(0.0697P)^2^+0.1442P] 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 4068 _refine_ls_number_parameters 252 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0578 _refine_ls_R_factor_gt 0.0444 _refine_ls_wR_factor_ref 0.1162 _refine_ls_wR_factor_gt 0.1106 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti Ti 0.48966(4) 0.31917(4) 0.20166(3) 0.02737(13) Uani 1 d . . . N1 N 0.71708(19) 0.3937(2) 0.23969(14) 0.0309(4) Uani 1 d . . . N2 N 0.88284(19) 0.6513(2) 0.35117(14) 0.0313(4) Uani 1 d . . . N3 N 0.4063(2) 0.2896(2) 0.05588(14) 0.0329(4) Uani 1 d . . . N4 N 0.4428(2) 0.1254(2) 0.21870(15) 0.0370(5) Uani 1 d . . . C1 C 0.5839(2) 0.5460(2) 0.31686(16) 0.0325(5) Uani 1 d . . . C2 C 0.4691(2) 0.5603(3) 0.23669(18) 0.0351(5) Uani 1 d . . . H2 H 0.4853 0.6213 0.1889 0.046 Uiso 1 calc R . . C3 C 0.3283(3) 0.4728(3) 0.23680(19) 0.0410(6) Uani 1 d . . . H3 H 0.2306 0.4610 0.1885 0.053 Uiso 1 calc R . . C4 C 0.3520(3) 0.4058(3) 0.31772(19) 0.0432(6) Uani 1 d . . . H4 H 0.2740 0.3389 0.3362 0.056 Uiso 1 calc R . . C5 C 0.5068(3) 0.4510(3) 0.36781(17) 0.0386(5) Uani 1 d . . . H5 H 0.5548 0.4220 0.4283 0.050 Uiso 1 calc R . . C10 C 0.8086(2) 0.3252(2) 0.18935(16) 0.0308(5) Uani 1 d . . . C11 C 0.8499(3) 0.3647(3) 0.10486(18) 0.0405(6) Uani 1 d . . . H11 H 0.8167 0.4429 0.0806 0.053 Uiso 1 calc R . . C12 C 0.9370(3) 0.2958(3) 0.0544(2) 0.0505(7) Uani 1 d . . . H12 H 0.9642 0.3253 -0.0053 0.066 Uiso 1 calc R . . C13 C 0.9855(3) 0.1867(3) 0.0869(2) 0.0542(7) Uani 1 d . . . H13 H 1.0484 0.1390 0.0516 0.070 Uiso 1 calc R . . C14 C 0.9446(3) 0.1451(3) 0.1698(3) 0.0576(8) Uani 1 d . . . H14 H 0.9782 0.0666 0.1933 0.075 Uiso 1 calc R . . C15 C 0.8567(3) 0.2127(3) 0.2207(2) 0.0459(6) Uani 1 d . . . H15 H 0.8281 0.1810 0.2793 0.060 Uiso 1 calc R . . C20 C 1.0306(2) 0.6365(3) 0.33997(18) 0.0360(5) Uani 1 d . . . H20 H 1.0132 0.5357 0.2994 0.047 Uiso 1 calc R . . C21 C 1.1437(3) 0.6589(3) 0.4442(2) 0.0536(7) Uani 1 d . . . H21A H 1.1695 0.7607 0.4855 0.070 Uiso 1 calc R . . H21B H 1.2352 0.6367 0.4318 0.070 Uiso 1 calc R . . H21C H 1.0991 0.5936 0.4825 0.070 Uiso 1 calc R . . C22 C 1.0962(3) 0.7364(3) 0.2781(2) 0.0535(7) Uani 1 d . . . H22A H 1.0249 0.7145 0.2091 0.070 Uiso 1 calc R . . H22B H 1.1918 0.7203 0.2696 0.070 Uiso 1 calc R . . H22C H 1.1141 0.8387 0.3157 0.070 Uiso 1 calc R . . C23 C 0.8872(2) 0.7966(2) 0.41377(17) 0.0359(5) Uani 1 d . . . H23 H 0.9930 0.8559 0.4364 0.047 Uiso 1 calc R . . C24 C 0.7995(3) 0.8764(3) 0.3509(2) 0.0530(7) Uani 1 d . . . H24A H 0.8311 0.8776 0.2869 0.069 Uiso 1 calc R . . H24B H 0.8193 0.9770 0.3926 0.069 Uiso 1 calc R . . H24C H 0.6913 0.8261 0.3325 0.069 Uiso 1 calc R . . C25 C 0.8391(3) 0.7879(3) 0.5129(2) 0.0509(7) Uani 1 d . . . H25A H 0.7314 0.7355 0.4942 0.066 Uiso 1 calc R . . H25B H 0.8573 0.8870 0.5567 0.066 Uiso 1 calc R . . H25C H 0.8977 0.7356 0.5515 0.066 Uiso 1 calc R . . C31 C 0.4657(3) 0.1883(3) -0.00672(19) 0.0447(6) Uani 1 d . . . H31A H 0.3818 0.1080 -0.0558 0.058 Uiso 1 calc R . . H31B H 0.5303 0.1488 0.0394 0.058 Uiso 1 calc R . . H31C H 0.5250 0.2402 -0.0458 0.058 Uiso 1 calc R . . C32 C 0.3123(3) 0.3511(3) -0.01093(19) 0.0488(7) Uani 1 d . . . H32A H 0.3734 0.4072 -0.0470 0.063 Uiso 1 calc R . . H32B H 0.2699 0.4158 0.0317 0.063 Uiso 1 calc R . . H32C H 0.2301 0.2720 -0.0626 0.063 Uiso 1 calc R . . C41 C 0.3135(3) 0.0046(3) 0.1528(2) 0.0483(6) Uani 1 d . . . H41A H 0.3433 -0.0858 0.1410 0.063 Uiso 1 calc R . . H41B H 0.2777 0.0248 0.0856 0.063 Uiso 1 calc R . . H41C H 0.2324 -0.0063 0.1875 0.063 Uiso 1 calc R . . C42 C 0.5020(4) 0.0944(4) 0.3171(2) 0.0634(8) Uani 1 d . . . H42A H 0.4240 0.0827 0.3544 0.082 Uiso 1 calc R . . H42B H 0.5901 0.1756 0.3602 0.082 Uiso 1 calc R . . H42C H 0.5317 0.0041 0.3030 0.082 Uiso 1 calc R . . B B 0.7468(3) 0.5380(3) 0.30476(19) 0.0303(5) Uani 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti 0.02190(19) 0.0302(2) 0.0278(2) 0.00611(15) 0.00532(14) 0.00622(15) N1 0.0229(8) 0.0307(9) 0.0358(9) 0.0036(8) 0.0075(7) 0.0067(7) N2 0.0254(8) 0.0318(10) 0.0332(9) 0.0045(8) 0.0068(7) 0.0063(8) N3 0.0288(9) 0.0387(11) 0.0312(9) 0.0077(8) 0.0060(7) 0.0132(8) N4 0.0303(9) 0.0352(11) 0.0440(11) 0.0147(9) 0.0046(8) 0.0083(8) C1 0.0298(11) 0.0308(11) 0.0317(11) -0.0021(9) 0.0090(9) 0.0079(9) C2 0.0312(11) 0.0350(12) 0.0416(12) 0.0077(10) 0.0126(9) 0.0143(10) C3 0.0267(11) 0.0468(14) 0.0463(13) 0.0011(11) 0.0116(10) 0.0133(10) C4 0.0347(12) 0.0498(15) 0.0422(13) 0.0028(11) 0.0209(10) 0.0057(11) C5 0.0371(12) 0.0470(14) 0.0306(11) 0.0052(10) 0.0150(9) 0.0091(11) C10 0.0193(9) 0.0321(11) 0.0337(11) 0.0016(9) 0.0016(8) 0.0052(9) C11 0.0330(12) 0.0523(15) 0.0388(12) 0.0134(11) 0.0083(10) 0.0182(11) C12 0.0344(12) 0.072(2) 0.0393(13) 0.0048(13) 0.0111(10) 0.0120(13) C13 0.0319(12) 0.0504(17) 0.0674(18) -0.0110(14) 0.0148(12) 0.0104(12) C14 0.0434(15) 0.0418(15) 0.093(2) 0.0162(15) 0.0211(15) 0.0232(13) C15 0.0380(13) 0.0447(15) 0.0607(16) 0.0193(13) 0.0154(11) 0.0163(11) C20 0.0256(10) 0.0362(12) 0.0412(12) 0.0040(10) 0.0071(9) 0.0066(9) C21 0.0350(13) 0.0598(18) 0.0572(16) 0.0084(14) -0.0005(12) 0.0158(12) C22 0.0450(14) 0.0549(17) 0.0628(17) 0.0149(14) 0.0273(13) 0.0081(13) C23 0.0312(11) 0.0314(12) 0.0380(12) 0.0013(10) 0.0074(9) 0.0049(9) C24 0.0557(16) 0.0321(13) 0.0630(17) 0.0064(12) 0.0053(13) 0.0127(12) C25 0.0523(15) 0.0469(16) 0.0417(14) -0.0043(12) 0.0159(12) 0.0035(12) C31 0.0423(13) 0.0523(15) 0.0365(12) 0.0028(11) 0.0091(10) 0.0179(12) C32 0.0450(14) 0.076(2) 0.0373(13) 0.0240(13) 0.0126(11) 0.0311(14) C41 0.0376(13) 0.0364(13) 0.0634(16) 0.0105(12) 0.0109(12) 0.0020(11) C42 0.0610(18) 0.0628(19) 0.0696(19) 0.0373(16) 0.0052(15) 0.0181(15) B 0.0286(11) 0.0349(13) 0.0291(11) 0.0104(10) 0.0079(9) 0.0111(10) _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 Ti N3 1.9045(19) . ? Ti N4 1.913(2) . ? Ti N1 2.020(2) . ? Ti C1 2.282(2) . ? Ti C5 2.309(2) . ? Ti C2 2.364(3) . ? Ti C4 2.396(2) . ? Ti C3 2.426(3) . ? Ti B 2.712(3) . ? N1 C10 1.414(3) . ? N1 B 1.428(3) . ? N2 B 1.409(3) . ? N2 C20 1.476(3) . ? N2 C23 1.481(3) . ? N3 C32 1.451(3) . ? N3 C31 1.460(3) . ? N4 C41 1.456(3) . ? N4 C42 1.457(3) . ? C1 C2 1.420(3) . ? C1 C5 1.429(3) . ? C1 B 1.604(3) . ? C2 C3 1.408(3) . ? C3 C4 1.396(4) . ? C4 C5 1.399(3) . ? C10 C11 1.388(3) . ? C10 C15 1.391(3) . ? C11 C12 1.382(4) . ? C12 C13 1.369(4) . ? C13 C14 1.374(4) . ? C14 C15 1.385(4) . ? C20 C21 1.523(3) . ? C20 C22 1.525(3) . ? C23 C24 1.516(4) . ? C23 C25 1.524(3) . ? 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 N3 Ti N4 103.44(9) . . ? N3 Ti N1 110.25(9) . . ? N4 Ti N1 106.33(9) . . ? N3 Ti C1 122.66(9) . . ? N4 Ti C1 133.22(9) . . ? N1 Ti C1 67.01(9) . . ? N3 Ti C5 145.47(9) . . ? N4 Ti C5 99.77(9) . . ? N1 Ti C5 86.89(9) . . ? C1 Ti C5 36.26(8) . . ? N3 Ti C2 90.82(9) . . ? N4 Ti C2 151.26(9) . . ? N1 Ti C2 91.44(9) . . ? C1 Ti C2 35.54(8) . . ? C5 Ti C2 57.99(9) . . ? N3 Ti C4 117.72(9) . . ? N4 Ti C4 94.33(9) . . ? N1 Ti C4 120.91(9) . . ? C1 Ti C4 59.04(9) . . ? C5 Ti C4 34.53(9) . . ? C2 Ti C4 56.95(9) . . ? N3 Ti C3 89.09(9) . . ? N4 Ti C3 120.02(9) . . ? N1 Ti C3 123.80(9) . . ? C1 Ti C3 58.52(9) . . ? C5 Ti C3 56.99(9) . . ? C2 Ti C3 34.16(8) . . ? C4 Ti C3 33.64(9) . . ? N3 Ti B 119.47(8) . . ? N4 Ti B 126.01(8) . . ? N1 Ti B 30.94(8) . . ? C1 Ti B 36.18(8) . . ? C5 Ti B 62.28(8) . . ? C2 Ti B 63.03(9) . . ? C4 Ti B 93.18(9) . . ? C3 Ti B 93.29(9) . . ? C10 N1 B 131.67(18) . . ? C10 N1 Ti 124.23(14) . . ? B N1 Ti 102.40(14) . . ? B N2 C20 123.20(19) . . ? B N2 C23 121.99(19) . . ? C20 N2 C23 114.80(17) . . ? C32 N3 C31 110.28(19) . . ? C32 N3 Ti 137.65(17) . . ? C31 N3 Ti 111.64(15) . . ? C41 N4 C42 110.3(2) . . ? C41 N4 Ti 124.81(17) . . ? C42 N4 Ti 122.15(18) . . ? C2 C1 C5 105.4(2) . . ? C2 C1 B 123.89(19) . . ? C5 C1 B 119.4(2) . . ? C2 C1 Ti 75.37(14) . . ? C5 C1 Ti 72.91(13) . . ? B C1 Ti 86.69(14) . . ? C3 C2 C1 109.2(2) . . ? C3 C2 Ti 75.35(15) . . ? C1 C2 Ti 69.09(13) . . ? C4 C3 C2 108.1(2) . . ? C4 C3 Ti 72.01(14) . . ? C2 C3 Ti 70.49(14) . . ? C3 C4 C5 108.0(2) . . ? C3 C4 Ti 74.35(14) . . ? C5 C4 Ti 69.33(13) . . ? C4 C5 C1 109.3(2) . . ? C4 C5 Ti 76.13(14) . . ? C1 C5 Ti 70.83(12) . . ? C11 C10 C15 117.6(2) . . ? C11 C10 N1 121.2(2) . . ? C15 C10 N1 121.2(2) . . ? C12 C11 C10 121.2(3) . . ? C13 C12 C11 120.7(3) . . ? C12 C13 C14 119.0(2) . . ? C13 C14 C15 120.9(3) . . ? C14 C15 C10 120.6(3) . . ? N2 C20 C21 112.9(2) . . ? N2 C20 C22 111.9(2) . . ? C21 C20 C22 111.0(2) . . ? N2 C23 C24 113.00(19) . . ? N2 C23 C25 112.1(2) . . ? C24 C23 C25 111.6(2) . . ? N2 B N1 131.0(2) . . ? N2 B C1 125.4(2) . . ? N1 B C1 103.57(18) . . ? N2 B Ti 175.77(16) . . ? N1 B Ti 46.66(10) . . ? C1 B Ti 57.13(11) . . ? _diffrn_measured_fraction_theta_max 0.903 _diffrn_reflns_theta_full 25.96 _diffrn_measured_fraction_theta_full 0.903 _refine_diff_density_max 0.437 _refine_diff_density_min -0.200 _refine_diff_density_rms 0.069