# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Frederic Poineau' _publ_contact_author_email FREDER29@UNLV.NEVADA.EDU _publ_section_title ; Synthesis, Structure, and First-Principles Calculations of the TcBr2(PMe3)4 and Tc2Br4(PMe3)4 Complexes ; loop_ _publ_author_name 'Frederic Poineau' 'Ken Czerwinski' 'Paul M. Forster' 'Alfred P. Sattelberger' 'Philippe Weck' # Attachment 'Tc2Br4_PMe3_4.cif' data_Tc2Br4(PMe3)4 _database_code_depnum_ccdc_archive 'CCDC 743297' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H18 Br2 P2 Tc' _chemical_formula_weight 409.96 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' P P 0.1023 0.0942 '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' Tc Tc -1.4390 0.7593 '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 18.0903(19) _cell_length_b 9.3365(10) _cell_length_c 17.232(3) _cell_angle_alpha 90.00 _cell_angle_beta 115.1040(10) _cell_angle_gamma 90.00 _cell_volume 2635.5(6) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.066 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1576 _exptl_absorpt_coefficient_mu 7.352 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6428 _exptl_absorpt_correction_T_max .7457 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18170 _diffrn_reflns_av_R_equivalents 0.0261 _diffrn_reflns_av_sigmaI/netI 0.0186 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 28.52 _reflns_number_total 3335 _reflns_number_gt 2999 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0309P)^2^+8.7069P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3335 _refine_ls_number_parameters 101 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0272 _refine_ls_R_factor_gt 0.0228 _refine_ls_wR_factor_ref 0.0638 _refine_ls_wR_factor_gt 0.0620 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.087 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tc1 Tc 0.5000 0.32584(3) 0.2500 0.01635(8) Uani 1 2 d S . . Tc2 Tc 0.5000 0.09753(3) 0.2500 0.01558(8) Uani 1 2 d S . . Br1 Br 0.38767(2) 0.43740(4) 0.12021(2) 0.02877(9) Uani 1 1 d . . . Br2 Br 0.58275(2) -0.01354(4) 0.17930(2) 0.02639(8) Uani 1 1 d . . . P1 P 0.58735(5) 0.38119(9) 0.17780(5) 0.02441(17) Uani 1 1 d . . . P2 P 0.38290(5) 0.04109(9) 0.11569(5) 0.02217(16) Uani 1 1 d . . . C1 C 0.5947(3) 0.5765(4) 0.1741(3) 0.0368(8) Uani 1 1 d . . . H1A H 0.5409 0.6171 0.1490 0.055 Uiso 1 1 calc R . . H1B H 0.6232 0.6019 0.1401 0.055 Uiso 1 1 calc R . . H1C H 0.6239 0.6129 0.2312 0.055 Uiso 1 1 calc R . . C2 C 0.6940(2) 0.3280(4) 0.2257(3) 0.0388(9) Uani 1 1 d . . . H2A H 0.7176 0.3497 0.2859 0.058 Uiso 1 1 calc R . . H2B H 0.7228 0.3792 0.1988 0.058 Uiso 1 1 calc R . . H2C H 0.6980 0.2269 0.2179 0.058 Uiso 1 1 calc R . . C3 C 0.5547(3) 0.3319(4) 0.0658(2) 0.0363(8) Uani 1 1 d . . . H3A H 0.4982 0.3562 0.0340 0.054 Uiso 1 1 calc R . . H3B H 0.5618 0.2307 0.0617 0.054 Uiso 1 1 calc R . . H3C H 0.5870 0.3829 0.0427 0.054 Uiso 1 1 calc R . . C4 C 0.2816(2) 0.0947(4) 0.1024(2) 0.0318(7) Uani 1 1 d . . . H4A H 0.2755 0.0738 0.1539 0.048 Uiso 1 1 calc R . . H4B H 0.2412 0.0429 0.0554 0.048 Uiso 1 1 calc R . . H4C H 0.2746 0.1956 0.0909 0.048 Uiso 1 1 calc R . . C5 C 0.3821(2) 0.0897(4) 0.0131(2) 0.0337(8) Uani 1 1 d . . . H5A H 0.4337 0.0654 0.0131 0.051 Uiso 1 1 calc R . . H5B H 0.3729 0.1908 0.0040 0.051 Uiso 1 1 calc R . . H5C H 0.3393 0.0384 -0.0320 0.051 Uiso 1 1 calc R . . C6 C 0.3739(2) -0.1538(4) 0.1079(2) 0.0363(8) Uani 1 1 d . . . H6A H 0.3736 -0.1917 0.1595 0.054 Uiso 1 1 calc R . . H6B H 0.4194 -0.1928 0.1000 0.054 Uiso 1 1 calc R . . H6C H 0.3240 -0.1794 0.0599 0.054 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 Tc1 0.01625(15) 0.01656(15) 0.01538(15) 0.000 0.00587(12) 0.000 Tc2 0.01601(15) 0.01658(15) 0.01400(15) 0.000 0.00621(12) 0.000 Br1 0.02608(16) 0.02854(17) 0.02428(16) 0.00624(12) 0.00352(13) 0.00477(12) Br2 0.02870(17) 0.02895(17) 0.02560(16) -0.00105(12) 0.01545(13) 0.00606(12) P1 0.0253(4) 0.0238(4) 0.0275(4) 0.0038(3) 0.0145(3) -0.0010(3) P2 0.0222(4) 0.0238(4) 0.0172(4) -0.0023(3) 0.0052(3) -0.0015(3) C1 0.044(2) 0.0263(17) 0.045(2) 0.0020(15) 0.0241(18) -0.0044(15) C2 0.0274(17) 0.042(2) 0.052(2) 0.0088(18) 0.0219(17) -0.0009(15) C3 0.051(2) 0.0364(19) 0.0295(18) 0.0060(15) 0.0251(17) 0.0021(16) C4 0.0184(15) 0.0405(19) 0.0286(17) -0.0023(14) 0.0024(13) -0.0042(13) C5 0.0362(19) 0.043(2) 0.0184(15) -0.0018(14) 0.0085(14) -0.0002(15) C6 0.043(2) 0.0240(16) 0.0347(19) -0.0087(14) 0.0101(16) -0.0072(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 Tc1 Tc2 2.1316(5) . ? Tc1 P1 2.4454(8) . ? Tc1 P1 2.4454(8) 2_655 ? Tc1 Br1 2.5218(4) 2_655 ? Tc1 Br1 2.5218(4) . ? Tc2 P2 2.4415(8) . ? Tc2 P2 2.4415(8) 2_655 ? Tc2 Br2 2.5196(4) . ? Tc2 Br2 2.5196(4) 2_655 ? P1 C2 1.816(4) . ? P1 C3 1.822(4) . ? P1 C1 1.832(4) . ? P2 C4 1.819(3) . ? P2 C5 1.819(3) . ? P2 C6 1.827(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 Tc2 Tc1 P1 102.20(2) . . ? Tc2 Tc1 P1 102.20(2) . 2_655 ? P1 Tc1 P1 155.60(4) . 2_655 ? Tc2 Tc1 Br1 114.393(11) . 2_655 ? P1 Tc1 Br1 84.98(2) . 2_655 ? P1 Tc1 Br1 85.01(2) 2_655 2_655 ? Tc2 Tc1 Br1 114.393(11) . . ? P1 Tc1 Br1 85.01(2) . . ? P1 Tc1 Br1 84.98(2) 2_655 . ? Br1 Tc1 Br1 131.21(2) 2_655 . ? Tc1 Tc2 P2 102.46(2) . . ? Tc1 Tc2 P2 102.46(2) . 2_655 ? P2 Tc2 P2 155.07(4) . 2_655 ? Tc1 Tc2 Br2 114.305(11) . . ? P2 Tc2 Br2 84.68(2) . . ? P2 Tc2 Br2 85.12(2) 2_655 . ? Tc1 Tc2 Br2 114.305(11) . 2_655 ? P2 Tc2 Br2 85.12(2) . 2_655 ? P2 Tc2 Br2 84.68(2) 2_655 2_655 ? Br2 Tc2 Br2 131.39(2) . 2_655 ? C2 P1 C3 102.5(2) . . ? C2 P1 C1 102.08(18) . . ? C3 P1 C1 102.12(18) . . ? C2 P1 Tc1 120.12(13) . . ? C3 P1 Tc1 119.79(13) . . ? C1 P1 Tc1 107.49(13) . . ? C4 P2 C5 102.54(17) . . ? C4 P2 C6 102.19(18) . . ? C5 P2 C6 102.29(18) . . ? C4 P2 Tc2 118.86(12) . . ? C5 P2 Tc2 120.88(12) . . ? C6 P2 Tc2 107.42(13) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.52 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.786 _refine_diff_density_min -0.404 _refine_diff_density_rms 0.124 # Attachment 'TcBr2_PMe3_4.cif' data_TcBr2(PME3)4 _database_code_depnum_ccdc_archive 'CCDC 743298' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H36 Br2 P4 Tc' _chemical_formula_weight 562.11 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' P P 0.1023 0.0942 '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' Tc Tc -1.4390 0.7593 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I-42m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x, y, -z' 'x, -y, -z' '-y, -x, z' 'y, x, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, x+1/2, z+1/2' _cell_length_a 9.4771(10) _cell_length_b 9.4771(10) _cell_length_c 12.123(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1088.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.715 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 562 _exptl_absorpt_coefficient_mu 4.614 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6362 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 2631 _diffrn_reflns_av_R_equivalents 0.0272 _diffrn_reflns_av_sigmaI/netI 0.0403 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 30.49 _reflns_number_total 889 _reflns_number_gt 771 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0245P)^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 0.000(15) _refine_ls_number_reflns 889 _refine_ls_number_parameters 34 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0311 _refine_ls_R_factor_gt 0.0236 _refine_ls_wR_factor_ref 0.0538 _refine_ls_wR_factor_gt 0.0516 _refine_ls_goodness_of_fit_ref 0.963 _refine_ls_restrained_S_all 0.963 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tc1 Tc 1.0000 1.0000 1.0000 0.01474(12) Uani 1 8 d S . . Br1 Br 1.0000 1.0000 0.78615(4) 0.02387(14) Uani 1 4 d S . . P1 P 0.82147(8) 0.82147(8) 0.96941(7) 0.0179(2) Uani 1 2 d S . . C1 C 0.6679(3) 0.8738(3) 0.8870(2) 0.0263(6) Uani 1 1 d . . . H1A H 0.6997 0.9224 0.8202 0.039 Uiso 1 1 calc R . . H1B H 0.6080 0.9372 0.9304 0.039 Uiso 1 1 calc R . . H1C H 0.6139 0.7896 0.8665 0.039 Uiso 1 1 calc R . . C2 C 0.7364(4) 0.7364(4) 1.0865(4) 0.0296(10) Uani 1 2 d S . . H1C2 H 0.689(4) 0.793(4) 1.127(3) 0.044 Uiso 1 1 d . . . H2C2 H 0.664(4) 0.664(4) 1.066(4) 0.044 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 Tc1 0.01447(17) 0.01447(17) 0.0153(2) 0.000 0.000 0.000 Br1 0.02769(19) 0.02769(19) 0.0162(2) 0.000 0.000 -0.0041(4) P1 0.0179(3) 0.0179(3) 0.0179(4) 0.0000(2) 0.0000(2) -0.0015(4) C1 0.0221(15) 0.0302(16) 0.0266(13) -0.0027(12) -0.0044(14) 0.0018(11) C2 0.0307(16) 0.0307(16) 0.027(3) 0.0042(13) 0.0042(13) -0.004(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tc1 P1 2.4213(11) 2_775 ? Tc1 P1 2.4213(11) 4_757 ? Tc1 P1 2.4213(11) 3_577 ? Tc1 P1 2.4213(11) . ? Tc1 Br1 2.5925(7) . ? Tc1 Br1 2.5925(7) 3_577 ? P1 C2 1.821(5) . ? P1 C1 1.833(3) 8 ? P1 C1 1.833(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 P1 Tc1 P1 91.344(6) 2_775 4_757 ? P1 Tc1 P1 91.344(6) 2_775 3_577 ? P1 Tc1 P1 162.38(4) 4_757 3_577 ? P1 Tc1 P1 162.38(4) 2_775 . ? P1 Tc1 P1 91.344(6) 4_757 . ? P1 Tc1 P1 91.344(6) 3_577 . ? P1 Tc1 Br1 81.19(2) 2_775 . ? P1 Tc1 Br1 98.81(2) 4_757 . ? P1 Tc1 Br1 98.81(2) 3_577 . ? P1 Tc1 Br1 81.19(2) . . ? P1 Tc1 Br1 98.81(2) 2_775 3_577 ? P1 Tc1 Br1 81.19(2) 4_757 3_577 ? P1 Tc1 Br1 81.19(2) 3_577 3_577 ? P1 Tc1 Br1 98.81(2) . 3_577 ? Br1 Tc1 Br1 180.0 . 3_577 ? C2 P1 C1 101.11(14) . 8 ? C2 P1 C1 101.11(14) . . ? C1 P1 C1 97.6(2) 8 . ? C2 P1 Tc1 119.98(16) . . ? C1 P1 Tc1 116.69(10) 8 . ? C1 P1 Tc1 116.69(10) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 30.49 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.773 _refine_diff_density_min -0.324 _refine_diff_density_rms 0.094