# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_40js _database_code_depnum_ccdc_archive 'CCDC 270734' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Hydrotris-(1-tert-butyl-imidazol-2-ylidene)boratomagnesium bromide ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H42 B Br Mg N6' _chemical_formula_weight 577.71 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' Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) 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' _cell_length_a 18.8479(19) _cell_length_b 16.3926(17) _cell_length_c 10.1499(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3136.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.224 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1216 _exptl_absorpt_coefficient_mu 1.357 _exptl_absorpt_correction_type 'multiscan (SADABS program, Sheldrick, 2000)' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 35582 _diffrn_reflns_av_R_equivalents 0.0509 _diffrn_reflns_av_sigmaI/netI 0.0678 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 28.30 _reflns_number_total 7513 _reflns_number_gt 5390 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0623P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.002(9) _refine_ls_number_reflns 7513 _refine_ls_number_parameters 348 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0807 _refine_ls_R_factor_gt 0.0507 _refine_ls_wR_factor_ref 0.1253 _refine_ls_wR_factor_gt 0.1110 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.285 _refine_ls_shift/su_mean 0.019 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 Br Br 0.91603(2) 0.87330(2) 0.46941(5) 0.06741(15) Uani 1 1 d . . . Mg Mg 0.80943(5) 0.89285(6) 0.33510(10) 0.0335(2) Uani 1 1 d . . . B B 0.67377(19) 0.9117(2) 0.1657(3) 0.0346(7) Uani 1 1 d . . . N11 N 0.73974(13) 0.90439(14) 0.0746(2) 0.0338(5) Uani 1 1 d . . . N21 N 0.84791(13) 0.89718(15) 0.0069(3) 0.0371(6) Uani 1 1 d . . . C11 C 0.80833(16) 0.89829(18) 0.1170(3) 0.0344(6) Uani 1 1 d . . . C21 C 0.73922(18) 0.9068(2) -0.0615(3) 0.0420(7) Uani 1 1 d . . . H21 H 0.6983 0.9113 -0.1156 0.050 Uiso 1 1 calc R . . C31 C 0.80602(18) 0.9016(2) -0.1037(3) 0.0444(8) Uani 1 1 d . . . H31 H 0.8216 0.9011 -0.1927 0.053 Uiso 1 1 calc R . . C41 C 0.92697(17) 0.8916(2) 0.0061(4) 0.0456(8) Uani 1 1 d . . . C51 C 0.9464(2) 0.8058(3) 0.0552(6) 0.0866(16) Uani 1 1 d . . . H51A H 0.9233 0.7648 -0.0005 0.130 Uiso 1 1 calc R . . H51B H 0.9303 0.7992 0.1464 0.130 Uiso 1 1 calc R . . H51C H 0.9980 0.7985 0.0512 0.130 Uiso 1 1 calc R . . C61 C 0.9548(2) 0.9087(5) -0.1283(5) 0.113(2) Uani 1 1 d . . . H61A H 0.9410 0.8645 -0.1881 0.169 Uiso 1 1 calc R . . H61B H 1.0067 0.9126 -0.1251 0.169 Uiso 1 1 calc R . . H61C H 0.9351 0.9604 -0.1604 0.169 Uiso 1 1 calc R . . C71 C 0.9567(2) 0.9534(3) 0.1019(5) 0.0749(13) Uani 1 1 d . . . H71A H 1.0086 0.9500 0.1021 0.112 Uiso 1 1 calc R . . H71B H 0.9387 0.9419 0.1905 0.112 Uiso 1 1 calc R . . H71C H 0.9421 1.0083 0.0751 0.112 Uiso 1 1 calc R . . N12 N 0.68259(12) 0.98705(14) 0.2563(2) 0.0343(5) Uani 1 1 d . . . N22 N 0.72340(13) 1.07050(15) 0.4016(2) 0.0356(5) Uani 1 1 d . . . C12 C 0.73656(16) 0.99823(16) 0.3429(3) 0.0339(6) Uani 1 1 d . . . C22 C 0.63692(16) 1.0525(2) 0.2604(3) 0.0411(7) Uani 1 1 d . . . H22 H 0.5953 1.0594 0.2087 0.049 Uiso 1 1 calc R . . C32 C 0.66206(18) 1.10481(19) 0.3512(3) 0.0422(8) Uani 1 1 d . . . H32 H 0.6416 1.1555 0.3760 0.051 Uiso 1 1 calc R . . C42 C 0.76932(19) 1.10714(19) 0.5052(3) 0.0430(8) Uani 1 1 d . . . C52 C 0.7773(2) 1.0450(2) 0.6163(4) 0.0626(11) Uani 1 1 d . . . H52A H 0.7302 1.0268 0.6450 0.094 Uiso 1 1 calc R . . H52B H 0.8022 1.0702 0.6906 0.094 Uiso 1 1 calc R . . H52C H 0.8045 0.9980 0.5846 0.094 Uiso 1 1 calc R . . C62 C 0.8413(2) 1.1260(3) 0.4448(5) 0.0682(12) Uani 1 1 d . . . H62A H 0.8627 1.0755 0.4116 0.102 Uiso 1 1 calc R . . H62B H 0.8723 1.1500 0.5118 0.102 Uiso 1 1 calc R . . H62C H 0.8354 1.1646 0.3719 0.102 Uiso 1 1 calc R . . C72 C 0.7355(2) 1.1847(2) 0.5574(4) 0.0608(10) Uani 1 1 d . . . H72A H 0.7347 1.2260 0.4876 0.091 Uiso 1 1 calc R . . H72B H 0.7632 1.2051 0.6323 0.091 Uiso 1 1 calc R . . H72C H 0.6869 1.1732 0.5860 0.091 Uiso 1 1 calc R . . N13 N 0.66771(13) 0.83419(15) 0.2528(2) 0.0366(6) Uani 1 1 d . . . N23 N 0.69033(15) 0.74188(16) 0.3975(3) 0.0433(6) Uani 1 1 d . . . C13 C 0.71790(16) 0.80969(17) 0.3400(3) 0.0357(6) Uani 1 1 d . . . C23 C 0.61094(18) 0.7815(2) 0.2562(3) 0.0449(8) Uani 1 1 d . . . H23 H 0.5693 0.7852 0.2036 0.054 Uiso 1 1 calc R . . C33 C 0.6246(2) 0.7240(2) 0.3465(4) 0.0526(9) Uani 1 1 d . . . H33 H 0.5948 0.6797 0.3705 0.063 Uiso 1 1 calc R . . C43 C 0.7281(2) 0.69652(19) 0.5051(3) 0.0513(9) Uani 1 1 d . . . C53 C 0.6812(3) 0.6255(3) 0.5510(5) 0.0772(14) Uani 1 1 d . . . H53A H 0.6354 0.6467 0.5810 0.116 Uiso 1 1 calc R . . H53B H 0.7047 0.5969 0.6237 0.116 Uiso 1 1 calc R . . H53C H 0.6737 0.5876 0.4776 0.116 Uiso 1 1 calc R . . C63 C 0.7974(2) 0.6645(3) 0.4506(4) 0.0692(11) Uani 1 1 d . . . H63A H 0.7877 0.6270 0.3776 0.104 Uiso 1 1 calc R . . H63B H 0.8232 0.6355 0.5202 0.104 Uiso 1 1 calc R . . H63C H 0.8262 0.7102 0.4188 0.104 Uiso 1 1 calc R . . C73 C 0.7405(2) 0.7548(2) 0.6184(4) 0.0638(11) Uani 1 1 d . . . H73A H 0.7715 0.7992 0.5894 0.096 Uiso 1 1 calc R . . H73B H 0.7629 0.7255 0.6915 0.096 Uiso 1 1 calc R . . H73C H 0.6949 0.7773 0.6476 0.096 Uiso 1 1 calc R . . C1T C 0.4437(4) 0.0230(7) 0.2059(14) 0.153(4) Uani 1 1 d . . . C2T C 0.4477(6) 0.0625(13) 0.3057(14) 0.208(10) Uani 1 1 d . . . H2T H 0.4436 0.0318 0.3848 0.250 Uiso 1 1 calc R . . C3T C 0.4557(6) 0.1323(15) 0.3205(13) 0.215(9) Uani 1 1 d . . . H3T H 0.4543 0.1550 0.4065 0.258 Uiso 1 1 calc R . . C4T C 0.4676(5) 0.1839(8) 0.209(2) 0.179(4) Uani 1 1 d . . . H4T H 0.4803 0.2397 0.2182 0.215 Uiso 1 1 calc R . . C5T C 0.4593(8) 0.1469(13) 0.0849(15) 0.235(9) Uani 1 1 d . . . H5T H 0.4628 0.1769 0.0051 0.282 Uiso 1 1 calc R . . C6T C 0.4449(5) 0.0577(10) 0.0870(9) 0.173(5) Uani 1 1 d . . . H6T H 0.4370 0.0274 0.0086 0.207 Uiso 1 1 calc R . . C7T C 0.4358(4) -0.0574(7) 0.210(2) 0.257(10) Uani 1 1 d . . . H7T1 H 0.4558 -0.0785 0.2920 0.386 Uiso 1 1 calc R . . H7T2 H 0.4606 -0.0820 0.1347 0.386 Uiso 1 1 calc R . . H7T3 H 0.3853 -0.0710 0.2052 0.386 Uiso 1 1 calc R . . H1B H 0.6259(17) 0.9185(18) 0.102(3) 0.037(8) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br 0.0571(2) 0.0729(3) 0.0722(3) 0.0049(2) -0.0322(2) 0.00315(19) Mg 0.0343(5) 0.0318(5) 0.0345(5) 0.0001(4) -0.0092(4) 0.0025(4) B 0.0336(18) 0.0372(18) 0.0330(17) -0.0049(14) -0.0070(14) 0.0002(15) N11 0.0347(14) 0.0342(12) 0.0325(13) -0.0001(10) -0.0047(10) 0.0016(10) N21 0.0333(13) 0.0406(13) 0.0374(14) 0.0036(11) 0.0010(11) 0.0032(10) C11 0.0333(16) 0.0316(15) 0.0381(16) 0.0014(13) -0.0071(14) -0.0006(12) C21 0.0406(18) 0.0518(18) 0.0335(18) 0.0022(13) -0.0073(13) 0.0015(14) C31 0.047(2) 0.0510(19) 0.0348(16) 0.0033(15) -0.0006(15) 0.0042(16) C41 0.0321(17) 0.0519(19) 0.053(2) 0.0030(15) 0.0037(14) -0.0002(13) C51 0.049(2) 0.057(3) 0.154(5) 0.006(3) -0.012(3) 0.014(2) C61 0.037(3) 0.233(8) 0.069(3) 0.019(4) 0.012(2) 0.002(3) C71 0.045(2) 0.082(3) 0.099(4) -0.012(3) -0.002(2) -0.016(2) N12 0.0313(13) 0.0359(13) 0.0357(13) 0.0003(10) -0.0040(11) 0.0041(10) N22 0.0396(14) 0.0328(13) 0.0343(13) -0.0022(11) -0.0006(11) 0.0025(11) C12 0.0331(15) 0.0301(14) 0.0386(15) 0.0000(13) -0.0033(12) 0.0014(11) C22 0.0352(17) 0.0465(19) 0.0415(18) 0.0064(14) -0.0007(14) 0.0086(14) C32 0.0438(19) 0.0350(15) 0.048(2) -0.0011(14) 0.0062(15) 0.0123(14) C42 0.0503(19) 0.0368(16) 0.0421(19) -0.0081(13) -0.0098(15) 0.0048(14) C52 0.095(3) 0.049(2) 0.0432(19) -0.0068(18) -0.017(2) 0.007(2) C62 0.050(2) 0.087(3) 0.067(3) -0.018(2) -0.007(2) -0.017(2) C72 0.073(3) 0.048(2) 0.062(2) -0.0175(18) -0.009(2) 0.0033(19) N13 0.0350(13) 0.0367(13) 0.0382(14) -0.0063(11) -0.0027(11) -0.0055(11) N23 0.0587(17) 0.0350(14) 0.0360(14) -0.0010(11) 0.0022(13) -0.0073(12) C13 0.0429(17) 0.0308(14) 0.0333(14) -0.0016(13) -0.0010(13) -0.0010(12) C23 0.0407(18) 0.0476(19) 0.0464(19) -0.0076(16) 0.0005(15) -0.0114(15) C33 0.057(2) 0.0459(19) 0.055(2) -0.0070(18) 0.0051(18) -0.0179(16) C43 0.076(2) 0.0372(17) 0.0404(18) 0.0089(14) 0.0016(17) -0.0028(16) C53 0.117(4) 0.052(2) 0.063(3) 0.014(2) 0.000(3) -0.013(2) C63 0.093(3) 0.059(2) 0.056(2) 0.006(2) -0.016(2) 0.023(2) C73 0.100(3) 0.052(2) 0.0386(19) 0.0061(17) -0.005(2) -0.004(2) C1T 0.050(4) 0.193(9) 0.217(12) -0.056(9) -0.002(5) 0.000(5) C2T 0.059(5) 0.42(3) 0.149(9) -0.167(14) -0.007(5) 0.052(9) C3T 0.069(5) 0.47(3) 0.104(7) -0.071(13) -0.008(5) 0.032(11) C4T 0.112(7) 0.212(12) 0.215(14) -0.029(11) -0.005(8) 0.039(7) C5T 0.214(14) 0.33(2) 0.157(12) 0.094(14) 0.000(10) 0.142(15) C6T 0.140(7) 0.296(16) 0.082(6) 0.004(8) -0.037(5) 0.080(10) C7T 0.075(5) 0.158(9) 0.54(3) -0.018(13) -0.002(9) -0.038(6) _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 Br Mg 2.4491(10) . ? Mg C13 2.199(3) . ? Mg C12 2.208(3) . ? Mg C11 2.216(3) . ? B N12 1.549(4) . ? B N13 1.552(4) . ? B N11 1.554(4) . ? N11 C11 1.366(4) . ? N11 C21 1.381(4) . ? N21 C11 1.344(4) . ? N21 C31 1.374(4) . ? N21 C41 1.493(4) . ? C21 C31 1.333(5) . ? C41 C61 1.489(6) . ? C41 C71 1.512(6) . ? C41 C51 1.537(5) . ? N12 C12 1.357(4) . ? N12 C22 1.376(4) . ? N22 C12 1.349(4) . ? N22 C32 1.383(4) . ? N22 C42 1.489(4) . ? C22 C32 1.346(5) . ? C42 C72 1.518(5) . ? C42 C62 1.521(5) . ? C42 C52 1.527(5) . ? N13 C13 1.356(4) . ? N13 C23 1.376(4) . ? N23 C13 1.359(4) . ? N23 C33 1.374(5) . ? N23 C43 1.501(4) . ? C23 C33 1.340(5) . ? C43 C73 1.512(5) . ? C43 C63 1.512(6) . ? C43 C53 1.534(6) . ? C1T C2T 1.205(13) . ? C1T C7T 1.327(12) . ? C1T C6T 1.335(14) . ? C2T C3T 1.16(3) . ? C3T C4T 1.43(2) . ? C4T C5T 1.406(18) . ? C5T C6T 1.49(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 C13 Mg C12 89.79(11) . . ? C13 Mg C11 92.31(12) . . ? C12 Mg C11 89.93(12) . . ? C13 Mg Br 123.35(9) . . ? C12 Mg Br 126.34(9) . . ? C11 Mg Br 124.68(9) . . ? N12 B N13 108.8(2) . . ? N12 B N11 109.2(2) . . ? N13 B N11 109.6(2) . . ? C11 N11 C21 108.9(3) . . ? C11 N11 B 125.1(3) . . ? C21 N11 B 125.9(3) . . ? C11 N21 C31 111.1(2) . . ? C11 N21 C41 124.0(3) . . ? C31 N21 C41 124.9(3) . . ? N21 C11 N11 105.3(3) . . ? N21 C11 Mg 145.6(2) . . ? N11 C11 Mg 109.1(2) . . ? C31 C21 N11 108.2(3) . . ? C21 C31 N21 106.5(3) . . ? C61 C41 N21 110.2(3) . . ? C61 C41 C71 109.4(4) . . ? N21 C41 C71 109.0(3) . . ? C61 C41 C51 112.7(4) . . ? N21 C41 C51 107.0(3) . . ? C71 C41 C51 108.4(4) . . ? C12 N12 C22 110.1(2) . . ? C12 N12 B 125.0(2) . . ? C22 N12 B 124.9(3) . . ? C12 N22 C32 110.4(3) . . ? C12 N22 C42 124.0(3) . . ? C32 N22 C42 125.6(3) . . ? N22 C12 N12 105.5(2) . . ? N22 C12 Mg 144.8(2) . . ? N12 C12 Mg 109.70(19) . . ? C32 C22 N12 107.3(3) . . ? C22 C32 N22 106.7(3) . . ? N22 C42 C72 109.9(3) . . ? N22 C42 C62 108.4(3) . . ? C72 C42 C62 110.2(3) . . ? N22 C42 C52 108.0(3) . . ? C72 C42 C52 110.1(3) . . ? C62 C42 C52 110.2(3) . . ? C13 N13 C23 109.9(3) . . ? C13 N13 B 124.3(2) . . ? C23 N13 B 125.8(3) . . ? C13 N23 C33 111.0(3) . . ? C13 N23 C43 122.4(3) . . ? C33 N23 C43 126.6(3) . . ? N13 C13 N23 104.8(3) . . ? N13 C13 Mg 110.4(2) . . ? N23 C13 Mg 144.8(2) . . ? C33 C23 N13 108.0(3) . . ? C23 C33 N23 106.3(3) . . ? N23 C43 C73 108.3(3) . . ? N23 C43 C63 108.4(3) . . ? C73 C43 C63 111.4(4) . . ? N23 C43 C53 108.9(3) . . ? C73 C43 C53 109.7(3) . . ? C63 C43 C53 110.2(3) . . ? C2T C1T C7T 121(2) . . ? C2T C1T C6T 122.0(14) . . ? C7T C1T C6T 116.9(15) . . ? C3T C2T C1T 130(2) . . ? C2T C3T C4T 120.0(16) . . ? C5T C4T C3T 115.8(15) . . ? C4T C5T C6T 115.6(12) . . ? C1T C6T C5T 115.8(11) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.579 _refine_diff_density_min -0.187 _refine_diff_density_rms 0.067 data_44js1m _database_code_depnum_ccdc_archive 'CCDC 270735' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Hydrotris-(1-tert-butylimidazol-2-ylidene)boratoiron(II) bromide ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H42 B Br Fe N6' _chemical_formula_weight 609.25 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) 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' _cell_length_a 18.9117(19) _cell_length_b 16.2675(17) _cell_length_c 10.1250(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3114.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.299 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1272 _exptl_absorpt_coefficient_mu 1.793 _exptl_absorpt_correction_type 'multiscan (SADABS program, Sheldrick, 2000)' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 35273 _diffrn_reflns_av_R_equivalents 0.0375 _diffrn_reflns_av_sigmaI/netI 0.0566 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 28.30 _reflns_number_total 7489 _reflns_number_gt 6320 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0824P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.002(10) _refine_ls_number_reflns 7489 _refine_ls_number_parameters 348 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0617 _refine_ls_R_factor_gt 0.0498 _refine_ls_wR_factor_ref 0.1331 _refine_ls_wR_factor_gt 0.1253 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.023 _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 Br Br 0.91084(2) 0.12172(3) 0.35477(5) 0.05892(14) Uani 1 1 d . . . Fe Fe 0.80444(3) 0.10283(3) 0.48822(5) 0.03963(13) Uani 1 1 d . . . B B 0.67176(19) 0.0849(2) 0.6557(3) 0.0294(6) Uani 1 1 d . . . N11 N 0.73723(13) 0.09219(15) 0.7459(3) 0.0285(5) Uani 1 1 d . . . N21 N 0.84634(14) 0.10019(16) 0.8085(3) 0.0327(5) Uani 1 1 d . . . C11 C 0.80443(16) 0.09829(18) 0.6990(3) 0.0309(6) Uani 1 1 d . . . C21 C 0.73807(18) 0.0901(2) 0.8825(3) 0.0372(7) Uani 1 1 d . . . H21 H 0.6980 0.0858 0.9388 0.045 Uiso 1 1 calc R . . C31 C 0.80579(19) 0.0953(2) 0.9208(4) 0.0418(8) Uani 1 1 d . . . H31 H 0.8226 0.0956 1.0092 0.050 Uiso 1 1 calc R . . C41 C 0.92527(18) 0.1060(2) 0.8058(4) 0.0409(8) Uani 1 1 d . . . C51 C 0.9535(2) 0.0392(3) 0.7164(5) 0.0622(11) Uani 1 1 d . . . H51A H 0.9427 -0.0147 0.7545 0.093 Uiso 1 1 calc R . . H51B H 1.0049 0.0452 0.7075 0.093 Uiso 1 1 calc R . . H51C H 0.9314 0.0438 0.6292 0.093 Uiso 1 1 calc R . . C61 C 0.9444(2) 0.1893(3) 0.7481(6) 0.0687(13) Uani 1 1 d . . . H61A H 0.9287 0.1920 0.6559 0.103 Uiso 1 1 calc R . . H61B H 0.9958 0.1970 0.7521 0.103 Uiso 1 1 calc R . . H61C H 0.9210 0.2328 0.7991 0.103 Uiso 1 1 calc R . . C71 C 0.9532(3) 0.0942(5) 0.9445(6) 0.0876(19) Uani 1 1 d . . . H71A H 0.9225 0.1229 1.0072 0.131 Uiso 1 1 calc R . . H71B H 1.0012 0.1166 0.9504 0.131 Uiso 1 1 calc R . . H71C H 0.9542 0.0354 0.9657 0.131 Uiso 1 1 calc R . . N12 N 0.68092(13) 0.00885(16) 0.5653(2) 0.0304(5) Uani 1 1 d . . . N22 N 0.72346(14) -0.07297(15) 0.4175(3) 0.0308(5) Uani 1 1 d . . . C12 C 0.73494(14) 0.00050(16) 0.4784(3) 0.0292(5) Uani 1 1 d . . . C22 C 0.63606(16) -0.05818(19) 0.5581(3) 0.0338(6) Uani 1 1 d . . . H22 H 0.5943 -0.0663 0.6086 0.041 Uiso 1 1 calc R . . C32 C 0.66233(19) -0.10949(18) 0.4669(4) 0.0382(7) Uani 1 1 d . . . H32 H 0.6430 -0.1609 0.4408 0.046 Uiso 1 1 calc R . . C42 C 0.77065(19) -0.10802(19) 0.3139(4) 0.0376(7) Uani 1 1 d . . . C52 C 0.7386(2) -0.1874(2) 0.2607(4) 0.0540(10) Uani 1 1 d . . . H52A H 0.7396 -0.2296 0.3298 0.081 Uiso 1 1 calc R . . H52B H 0.7660 -0.2063 0.1844 0.081 Uiso 1 1 calc R . . H52C H 0.6895 -0.1774 0.2339 0.081 Uiso 1 1 calc R . . C62 C 0.7761(3) -0.0459(3) 0.2021(4) 0.0566(10) Uani 1 1 d . . . H62A H 0.7286 -0.0318 0.1709 0.085 Uiso 1 1 calc R . . H62B H 0.8034 -0.0697 0.1293 0.085 Uiso 1 1 calc R . . H62C H 0.7998 0.0039 0.2341 0.085 Uiso 1 1 calc R . . C72 C 0.8423(2) -0.1244(3) 0.3758(5) 0.0588(11) Uani 1 1 d . . . H72A H 0.8616 -0.0729 0.4108 0.088 Uiso 1 1 calc R . . H72B H 0.8744 -0.1466 0.3088 0.088 Uiso 1 1 calc R . . H72C H 0.8370 -0.1642 0.4477 0.088 Uiso 1 1 calc R . . N13 N 0.66600(14) 0.16238(16) 0.5678(3) 0.0315(5) Uani 1 1 d . . . N23 N 0.69133(14) 0.25440(16) 0.4213(3) 0.0376(6) Uani 1 1 d . . . C13 C 0.71704(16) 0.18503(17) 0.4815(3) 0.0323(6) Uani 1 1 d . . . C23 C 0.6101(2) 0.2165(2) 0.5626(4) 0.0430(8) Uani 1 1 d . . . H23 H 0.5681 0.2137 0.6138 0.052 Uiso 1 1 calc R . . C33 C 0.62566(19) 0.2737(2) 0.4725(4) 0.0464(8) Uani 1 1 d . . . H33 H 0.5969 0.3191 0.4482 0.056 Uiso 1 1 calc R . . C43 C 0.7301(2) 0.2987(2) 0.3148(4) 0.0481(9) Uani 1 1 d . . . C53 C 0.7418(3) 0.2386(3) 0.2017(4) 0.0589(11) Uani 1 1 d . . . H53A H 0.7714 0.1929 0.2321 0.088 Uiso 1 1 calc R . . H53B H 0.7654 0.2669 0.1285 0.088 Uiso 1 1 calc R . . H53C H 0.6961 0.2172 0.1717 0.088 Uiso 1 1 calc R . . C63 C 0.6865(3) 0.3706(3) 0.2666(5) 0.0654(13) Uani 1 1 d . . . H63A H 0.6421 0.3504 0.2289 0.098 Uiso 1 1 calc R . . H63B H 0.7130 0.4007 0.1988 0.098 Uiso 1 1 calc R . . H63C H 0.6762 0.4074 0.3408 0.098 Uiso 1 1 calc R . . C73 C 0.8000(2) 0.3289(3) 0.3701(4) 0.0608(11) Uani 1 1 d . . . H73A H 0.7914 0.3748 0.4307 0.091 Uiso 1 1 calc R . . H73B H 0.8304 0.3474 0.2975 0.091 Uiso 1 1 calc R . . H73C H 0.8233 0.2841 0.4178 0.091 Uiso 1 1 calc R . . C1T C 0.4438(3) 0.9733(8) 0.6184(15) 0.154(4) Uani 1 1 d . . . C2T C 0.4482(4) 0.9323(10) 0.5107(9) 0.146(5) Uani 1 1 d . . . H2T H 0.4430 0.9617 0.4302 0.176 Uiso 1 1 calc R . . C3T C 0.4592(6) 0.8553(16) 0.5033(17) 0.205(10) Uani 1 1 d . . . H3T H 0.4603 0.8285 0.4199 0.246 Uiso 1 1 calc R . . C4T C 0.4690(6) 0.8127(11) 0.614(2) 0.182(6) Uani 1 1 d . . . H4T H 0.4811 0.7560 0.6114 0.219 Uiso 1 1 calc R . . C5T C 0.4607(9) 0.8543(16) 0.7389(18) 0.231(11) Uani 1 1 d . . . H5T H 0.4633 0.8248 0.8196 0.277 Uiso 1 1 calc R . . C6T C 0.4489(7) 0.9381(13) 0.7385(11) 0.184(8) Uani 1 1 d . . . H6T H 0.4446 0.9689 0.8178 0.220 Uiso 1 1 calc R . . C7T C 0.4355(5) 1.0574(7) 0.615(2) 0.233(9) Uani 1 1 d . . . H7T1 H 0.4815 1.0835 0.6005 0.350 Uiso 1 1 calc R . . H7T2 H 0.4156 1.0763 0.6990 0.350 Uiso 1 1 calc R . . H7T3 H 0.4033 1.0721 0.5428 0.350 Uiso 1 1 calc R . . H1B H 0.630(2) 0.071(2) 0.700(4) 0.039(9) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br 0.0503(2) 0.0626(2) 0.0639(3) 0.0034(2) 0.0281(2) 0.00010(17) Fe 0.0413(3) 0.0372(2) 0.0404(3) -0.0003(2) 0.0086(2) -0.00122(18) B 0.0281(16) 0.0318(16) 0.0284(16) -0.0025(13) 0.0056(13) 0.0011(13) N11 0.0291(13) 0.0294(12) 0.0271(12) 0.0023(9) 0.0028(10) -0.0006(9) N21 0.0284(13) 0.0368(13) 0.0328(14) 0.0030(10) -0.0020(10) -0.0019(10) C11 0.0315(15) 0.0298(14) 0.0315(15) -0.0003(12) 0.0052(12) -0.0007(11) C21 0.0337(16) 0.0462(17) 0.0316(17) -0.0004(13) 0.0058(12) -0.0016(13) C31 0.046(2) 0.049(2) 0.0306(17) 0.0034(15) 0.0007(14) -0.0006(15) C41 0.0250(16) 0.0482(19) 0.049(2) 0.0024(15) -0.0051(13) -0.0015(12) C51 0.040(2) 0.062(3) 0.085(3) -0.002(2) 0.000(2) 0.0124(17) C61 0.040(2) 0.061(3) 0.105(4) 0.009(2) 0.006(2) -0.0116(18) C71 0.039(2) 0.161(6) 0.063(3) 0.018(3) -0.013(2) -0.006(3) N12 0.0297(12) 0.0314(12) 0.0301(13) 0.0007(10) 0.0043(10) -0.0028(9) N22 0.0348(13) 0.0276(12) 0.0301(13) -0.0013(10) 0.0019(10) -0.0007(10) C12 0.0295(13) 0.0268(12) 0.0312(14) 0.0026(12) 0.0042(12) -0.0006(10) C22 0.0274(15) 0.0368(16) 0.0372(16) 0.0053(12) 0.0004(12) -0.0078(11) C32 0.0414(18) 0.0327(15) 0.040(2) 0.0000(13) -0.0016(14) -0.0113(12) C42 0.0411(19) 0.0351(16) 0.0366(17) -0.0066(12) 0.0050(14) -0.0014(12) C52 0.070(3) 0.0399(19) 0.053(2) -0.0161(16) 0.0115(19) -0.0034(17) C62 0.086(3) 0.050(2) 0.0342(18) -0.0069(17) 0.0129(19) -0.005(2) C72 0.053(2) 0.072(3) 0.052(3) -0.0157(19) 0.0046(19) 0.019(2) N13 0.0297(13) 0.0344(13) 0.0304(13) -0.0051(10) 0.0024(10) 0.0054(10) N23 0.0496(16) 0.0275(12) 0.0358(14) -0.0021(11) -0.0013(12) 0.0053(11) C13 0.0423(16) 0.0267(12) 0.0279(14) -0.0030(13) 0.0034(13) 0.0016(11) C23 0.0421(18) 0.0454(18) 0.0416(18) -0.0070(15) 0.0015(14) 0.0108(15) C33 0.054(2) 0.0381(16) 0.047(2) 0.0003(15) -0.0041(17) 0.0163(14) C43 0.076(3) 0.0328(17) 0.0355(18) 0.0027(13) -0.0017(17) 0.0005(16) C53 0.095(3) 0.049(2) 0.0327(18) 0.0035(16) 0.009(2) 0.002(2) C63 0.104(4) 0.040(2) 0.053(3) 0.0122(18) -0.003(2) 0.009(2) C73 0.080(3) 0.056(2) 0.047(2) 0.0055(19) 0.004(2) -0.0240(19) C1T 0.035(3) 0.216(11) 0.213(13) -0.051(11) 0.013(5) -0.005(4) C2T 0.043(3) 0.317(17) 0.079(5) -0.082(8) -0.005(3) -0.015(6) C3T 0.079(6) 0.42(3) 0.118(10) -0.092(16) 0.022(6) -0.045(11) C4T 0.098(7) 0.250(16) 0.199(14) -0.047(14) 0.028(9) -0.068(8) C5T 0.185(14) 0.36(3) 0.147(13) 0.087(17) 0.015(10) -0.144(18) C6T 0.150(10) 0.32(2) 0.078(6) 0.017(9) 0.046(6) -0.098(13) C7T 0.083(5) 0.131(8) 0.49(3) -0.002(14) -0.016(11) 0.041(6) _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 Br Fe 2.4432(6) . ? Fe C12 2.123(3) . ? Fe C13 2.127(3) . ? Fe C11 2.135(3) . ? B N11 1.543(5) . ? B N13 1.547(4) . ? B N12 1.548(4) . ? N11 C11 1.360(4) . ? N11 C21 1.384(4) . ? N21 C11 1.363(4) . ? N21 C31 1.374(5) . ? N21 C41 1.496(4) . ? C21 C31 1.341(5) . ? C41 C51 1.512(6) . ? C41 C71 1.512(7) . ? C41 C61 1.520(6) . ? N12 C12 1.355(4) . ? N12 C22 1.383(4) . ? N22 C12 1.362(4) . ? N22 C32 1.393(4) . ? N22 C42 1.490(4) . ? C22 C32 1.341(5) . ? C42 C72 1.515(6) . ? C42 C62 1.522(5) . ? C42 C52 1.526(5) . ? N13 C13 1.353(4) . ? N13 C23 1.376(4) . ? N23 C13 1.372(4) . ? N23 C33 1.382(5) . ? N23 C43 1.490(5) . ? C23 C33 1.336(5) . ? C43 C63 1.512(6) . ? C43 C73 1.517(6) . ? C43 C53 1.522(5) . ? C1T C2T 1.281(14) . ? C1T C6T 1.348(18) . ? C1T C7T 1.377(15) . ? C2T C3T 1.27(3) . ? C3T C4T 1.33(2) . ? C4T C5T 1.44(2) . ? C5T C6T 1.38(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 C12 Fe C13 90.59(11) . . ? C12 Fe C11 91.12(12) . . ? C13 Fe C11 93.07(12) . . ? C12 Fe Br 125.63(8) . . ? C13 Fe Br 122.91(9) . . ? C11 Fe Br 123.85(9) . . ? N11 B N13 109.5(3) . . ? N11 B N12 108.8(2) . . ? N13 B N12 108.6(2) . . ? C11 N11 C21 109.9(3) . . ? C11 N11 B 123.3(3) . . ? C21 N11 B 126.8(3) . . ? C11 N21 C31 110.3(3) . . ? C11 N21 C41 124.5(3) . . ? C31 N21 C41 125.2(3) . . ? N11 C11 N21 105.1(3) . . ? N11 C11 Fe 110.6(2) . . ? N21 C11 Fe 144.3(2) . . ? C31 C21 N11 107.4(3) . . ? C21 C31 N21 107.3(3) . . ? N21 C41 C51 108.6(3) . . ? N21 C41 C71 108.9(3) . . ? C51 C41 C71 109.9(4) . . ? N21 C41 C61 107.5(3) . . ? C51 C41 C61 109.1(4) . . ? C71 C41 C61 112.8(4) . . ? C12 N12 C22 110.4(2) . . ? C12 N12 B 123.2(2) . . ? C22 N12 B 126.3(3) . . ? C12 N22 C32 110.1(3) . . ? C12 N22 C42 124.0(2) . . ? C32 N22 C42 125.9(3) . . ? N12 C12 N22 105.2(2) . . ? N12 C12 Fe 110.96(19) . . ? N22 C12 Fe 143.9(2) . . ? C32 C22 N12 107.4(3) . . ? C22 C32 N22 106.8(3) . . ? N22 C42 C72 108.2(3) . . ? N22 C42 C62 108.1(3) . . ? C72 C42 C62 111.3(4) . . ? N22 C42 C52 109.5(3) . . ? C72 C42 C52 110.6(3) . . ? C62 C42 C52 109.1(3) . . ? C13 N13 C23 110.4(3) . . ? C13 N13 B 122.9(2) . . ? C23 N13 B 126.7(3) . . ? C13 N23 C33 109.8(3) . . ? C13 N23 C43 123.0(3) . . ? C33 N23 C43 127.2(3) . . ? N13 C13 N23 105.0(3) . . ? N13 C13 Fe 111.3(2) . . ? N23 C13 Fe 143.8(2) . . ? C33 C23 N13 107.7(3) . . ? C23 C33 N23 107.2(3) . . ? N23 C43 C63 109.9(3) . . ? N23 C43 C73 108.6(3) . . ? C63 C43 C73 110.1(4) . . ? N23 C43 C53 107.8(3) . . ? C63 C43 C53 109.5(3) . . ? C73 C43 C53 111.1(4) . . ? C2T C1T C6T 122.8(15) . . ? C2T C1T C7T 120.2(18) . . ? C6T C1T C7T 117.0(17) . . ? C3T C2T C1T 125.0(17) . . ? C2T C3T C4T 119.0(16) . . ? C3T C4T C5T 118.6(19) . . ? C6T C5T C4T 118.7(15) . . ? C1T C6T C5T 115.7(15) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 1.010 _refine_diff_density_min -0.485 _refine_diff_density_rms 0.095 #===END