#------------------------------------------------------------------------------ #$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $ #$Revision: 176467 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/07/51/4075166.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4075166 loop_ _publ_author_name 'Anderson, Laura L.' 'Schmidt, Joseph A. R.' 'Arnold, John' 'Bergman, Robert G.' _publ_section_title ; Neutral and Cationic Alkyl Tantalum Imido Complexes: Synthesis and Migratory Insertion Reactions. ; _journal_issue 14 _journal_name_full Organometallics _journal_page_first 3394 _journal_page_last 3406 _journal_paper_doi 10.1021/om060081t _journal_volume 25 _journal_year 2006 _chemical_formula_moiety 'C25 H30 N Ta ' _chemical_formula_sum 'C25 H30 N Ta' _chemical_formula_weight 525.47 _space_group_IT_number 159 _symmetry_cell_setting trigonal _symmetry_Int_Tables_number 159 _symmetry_space_group_name_Hall 'P 3 -2c' _symmetry_space_group_name_H-M 'P 3 1 c' _atom_sites_solution_primary direct _audit_creation_date 'Sat Feb 2 17:57:44 2002' _audit_creation_method 'by teXsan' _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_formula_units_Z 2 _cell_length_a 11.1584(4) _cell_length_b 11.1584(4) _cell_length_c 10.1563(5) _cell_measurement_reflns_used 4201 _cell_measurement_temperature 133.2 _cell_measurement_theta_max 45.0 _cell_measurement_theta_min 3.0 _cell_volume 1095.14(8) _computing_cell_refinement 'Bruker SAINT v5.04' _computing_data_collection 'Bruker SMART v5.052d' _computing_data_reduction 'Bruker SAINT v5.04' _computing_publication_material teXsan _computing_structure_refinement teXsan _computing_structure_solution SIR92 _diffrn_ambient_temperature 133.2 _diffrn_measurement_device_type 'SMART CCD' _diffrn_measurement_method \w-scan _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents 0.0413 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 4878 _diffrn_reflns_theta_max 24.70 _diffrn_standards_decay_% 0.00 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 5.020 _exptl_absorpt_correction_T_max 0.58 _exptl_absorpt_correction_T_min 0.32 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'Blessing, 1995' _exptl_crystal_colour color _exptl_crystal_density_diffrn 1.593 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 520.00 _exptl_crystal_size_max 0.330 _exptl_crystal_size_mid 0.240 _exptl_crystal_size_min 0.150 _refine_diff_density_max 0.50 _refine_diff_density_min -1.48 _refine_ls_extinction_coef 0.00000 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.253 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 81 _refine_ls_number_reflns 2062 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.253 _refine_ls_R_factor_all 0.0258 _refine_ls_R_factor_gt 0.0239 _refine_ls_shift/su_max 0.0000 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme sigma _refine_ls_wR_factor_all 0.0315 _refine_ls_wR_factor_gt 0.0307 _reflns_number_gt 2062 _reflns_number_total 2340 _reflns_threshold_expression I>3.00sigma _cod_data_source_file om060081tsi20060125_023927.cif _cod_data_source_block Bn3Ta_NtBu_for_L2A_by_JS _cod_original_cell_volume 1095.14(7) _cod_original_sg_symbol_H-M 'P 3 1 c ' _cod_original_formula_sum 'C25 H30 N Ta ' _cod_database_code 4075166 loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -y, +x-y, +z' ' -x+y, -x, +z' ' +y, +x,1/2+z' ' -x, -x+y,1/2+z' ' +x-y, -y,1/2+z' loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ta(1) 0.0217(1) 0.022 0.0258(1) 0.011 0.000 0.000 N(1) 0.029(2) 0.029 0.006(3) 0.015 0.000 0.000 C(1) 0.027(2) 0.020(2) 0.037(3) 0.010(2) 0.002(2) 0.001(2) C(2) 0.016(2) 0.022(2) 0.043(3) 0.005(2) 0.011(2) 0.002(2) C(3) 0.035(2) 0.025(2) 0.036(3) 0.013(2) 0.004(2) -0.007(2) C(4) 0.043(3) 0.041(3) 0.030(3) 0.018(2) 0.007(2) 0.003(2) C(5) 0.035(2) 0.027(2) 0.041(3) 0.014(2) 0.012(2) 0.010(2) C(6) 0.022(2) 0.023(2) 0.045(3) 0.006(2) 0.007(2) -0.009(2) C(7) 0.021(2) 0.025(2) 0.038(3) 0.005(2) 0.000(2) -0.004(2) C(8) 0.037(3) 0.037 0.020(4) 0.018 0.000 0.000 C(9) 0.039(3) 0.053(3) 0.048(3) 0.019(3) 0.013(2) 0.011(3) loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type Ta(1) -0.333 0.333 0.270 0.023 Uij N(1) -0.333 0.333 0.4411(6) 0.021 Uij C(1) -0.1076(4) 0.4513(5) 0.2322(4) 0.030 Uij C(2) -0.1203(4) 0.5652(5) 0.1709(5) 0.027 Uij C(3) -0.1559(5) 0.5609(5) 0.0374(5) 0.033 Uij C(4) -0.1830(6) 0.6596(5) -0.0159(5) 0.039 Uij C(5) -0.1735(5) 0.7662(5) 0.0616(5) 0.035 Uij C(6) -0.1366(4) 0.7732(5) 0.1936(5) 0.032 Uij C(7) -0.1110(5) 0.6756(4) 0.2482(5) 0.031 Uij C(8) -0.333 0.333 0.5860(8) 0.025 Uij C(9) -0.4835(6) 0.2604(6) 0.6315(6) 0.050 Uij H(1) -0.077 0.406 0.174 0.036 Uij H(2) -0.053 0.478 0.310 0.036 Uij H(3) -0.162 0.489 -0.017 0.040 Uij H(4) -0.207 0.655 -0.106 0.047 Uij H(5) -0.193 0.833 0.025 0.042 Uij H(6) -0.128 0.847 0.247 0.039 Uij H(7) -0.087 0.682 0.339 0.037 Uij H(8) -0.530 0.167 0.600 0.060 Uij H(9) -0.528 0.307 0.598 0.060 Uij H(10) -0.487 0.260 0.725 0.060 Uij loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 50 0.003 0.002 'International Tables' H 0 60 0.000 0.000 'International Tables' N 0 2 0.006 0.003 'International Tables' Ta 0 2 -0.705 6.523 'International Tables' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag N(1) Ta(1) C(1) 100.0(1) yes N(1) Ta(1) C(1) 100.0(1) yes N(1) Ta(1) C(1) 100.0(1) yes C(1) Ta(1) C(1) 117.06(7) yes C(1) Ta(1) C(1) 117.06(7) yes C(1) Ta(1) C(1) 117.06(7) yes Ta(1) N(1) C(8) 180.0 yes Ta(1) C(1) C(2) 90.8(3) yes C(1) C(2) C(3) 121.4(4) yes C(1) C(2) C(7) 120.9(5) yes C(3) C(2) C(7) 117.4(4) yes C(2) C(3) C(4) 121.2(4) yes C(3) C(4) C(5) 120.4(5) yes C(4) C(5) C(6) 119.2(5) yes C(5) C(6) C(7) 121.2(4) yes C(2) C(7) C(6) 120.7(5) yes N(1) C(8) C(9) 107.7(4) yes N(1) C(8) C(9) 107.7(4) yes N(1) C(8) C(9) 107.7(4) yes C(9) C(8) C(9) 111.2(4) yes C(9) C(8) C(9) 111.2(4) yes C(9) C(8) C(9) 111.2(4) yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Ta(1) N(1) 1.737(6) yes Ta(1) C(1) 2.216(4) yes Ta(1) C(1) 2.216(4) yes Ta(1) C(1) 2.216(4) yes N(1) C(8) 1.47(1) yes C(1) C(2) 1.485(6) yes C(2) C(3) 1.407(7) yes C(2) C(7) 1.420(7) yes C(3) C(4) 1.389(8) yes C(4) C(5) 1.385(7) yes C(5) C(6) 1.393(7) yes C(6) C(7) 1.373(8) yes C(8) C(9) 1.524(6) yes C(8) C(9) 1.524(6) yes C(8) C(9) 1.524(6) yes