#------------------------------------------------------------------------------ #$Date: 2014-07-12 01:16:09 +0300 (Sat, 12 Jul 2014) $ #$Revision: 120081 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/30/77/4307745.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_4307745 loop_ _publ_author_name 'Johannes Etzkorn' 'Martin Ade' 'Harald Hillebrecht' _publ_contact_author_address ; Albert-Ludwigs-Universit\"at Freiburg Institut f\"ur Anorganische und Analytische Chemie Albertstr. 21 D-79104 Freiburg Germany ; _publ_contact_author_email harald.hillebrecht@ac.uni-freiburg.de _publ_contact_author_fax +49-(0)761-203-6012 _publ_contact_author_name 'Prof. Dr. Harald Hillebrecht' _publ_contact_author_phone +49-(0)761-203-6131 _publ_section_title ; Ta3AlC2 and Ta4AlC3- Single-Crystal Investigations of Two New Ternary Carbides of Tantalum Synthesized by the Molten Metal Technique ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 1410 _journal_page_last 1418 _journal_volume 46 _journal_year 2007 _chemical_formula_sum 'C2 A3 Al T' _chemical_formula_weight 593.83 _chemical_name_systematic ; ? ; _space_group_IT_number 194 _symmetry_cell_setting hexagonal _symmetry_space_group_name_Hall '-P 6c 2c' _symmetry_space_group_name_H-M 'P 63/m m c' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_formula_units_Z 2 _cell_length_a 3.1004(4) _cell_length_b 3.1004(4) _cell_length_c 19.200(4) _cell_measurement_temperature 293(2) _cell_volume 159.83(4) _computing_cell_refinement 'Software for IPDS-II, Fa. Stoe' _computing_data_collection 'Software for IPDS-II, Fa. Stoe' _computing_data_reduction 'Software for IPDS-II, Fa. Stoe' _computing_molecular_graphics 'Diamond (Crystal impact, 2000)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_area_resol_mean - _diffrn_detector_type STOE _diffrn_measured_fraction_theta_full 0.877 _diffrn_measured_fraction_theta_max 0.877 _diffrn_measurement_details ; 100 frames, detector distance = 40 mm 10 min/frame Comleteness 98.8% ; _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_measurement_method 'rotation method' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1010 _diffrn_reflns_av_sigmaI/netI 0.0560 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 1486 _diffrn_reflns_theta_full 32.75 _diffrn_reflns_theta_max 32.75 _diffrn_reflns_theta_min 4.25 _diffrn_source_current 40 _diffrn_source_power 2.00 _diffrn_source_voltage 50 _exptl_absorpt_coefficient_mu 102.421 _exptl_absorpt_correction_T_max 0.0187 _exptl_absorpt_correction_T_min 0.0020 _exptl_absorpt_correction_type 'numerical, equivalent method (XSHAPE, Fa. Stoe)' _exptl_absorpt_process_details 'program XSHAPE' _exptl_crystal_colour 'metallic lustrous' _exptl_crystal_density_diffrn 12.339 _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'hexagonal platelet' _exptl_crystal_F_000 488 _exptl_crystal_size_max 0.02 _exptl_crystal_size_min 0.005 _refine_diff_density_max 2.952 _refine_diff_density_min -3.023 _refine_diff_density_rms 0.689 _refine_ls_extinction_coef 0.0008(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 12 _refine_ls_number_reflns 146 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.025 _refine_ls_R_factor_all 0.0603 _refine_ls_R_factor_gt 0.0338 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0140P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0383 _refine_ls_wR_factor_ref 0.0407 _reflns_number_gt 111 _reflns_number_total 146 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file ic062231yrom20061123_104704.cif _[local]_cod_data_source_block ta3alc2 _[local]_cod_chemical_formula_sum_orig 'C2 Al TA3' _cod_database_code 4307745 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' 'y, x, -z' 'x-y, -y, -z' '-x, -x+y, -z' '-y, -x, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z-1/2' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' '-y, -x, z' '-x+y, y, z' 'x, x-y, z' 'y, x, z-1/2' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' 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 0.6667 0.3333 0.63423(6) 0.0095(3) Uani 1 6 d S . . Ta2 Ta 0.0000 1.0000 0.5000 0.0088(3) Uani 1 12 d S . . Al Al 0.0000 1.0000 0.7500 0.014(2) Uani 1 12 d S . . C C 0.3333 0.6667 0.5675(11) 0.008(3) Uani 1 6 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 0.0080(3) 0.0080(3) 0.0124(4) 0.000 0.000 0.00400(15) Ta2 0.0075(3) 0.0075(3) 0.0113(7) 0.000 0.000 0.00377(17) Al 0.011(3) 0.011(3) 0.022(6) 0.000 0.000 0.0053(13) C 0.010(5) 0.010(5) 0.005(9) 0.000 0.000 0.005(2) 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' Al Al 0.0645 0.0514 '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' 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 C Ta1 C 89.5(6) 1_545 1_655 ? C Ta1 C 89.5(6) 1_545 . ? C Ta1 C 89.5(6) 1_655 . ? C Ta1 Al 164.4(5) 1_545 1_655 ? C Ta1 Al 101.4(4) 1_655 1_655 ? C Ta1 Al 101.4(4) . 1_655 ? C Ta1 Al 101.4(4) 1_545 1_645 ? C Ta1 Al 101.4(4) 1_655 1_645 ? C Ta1 Al 164.4(5) . 1_645 ? Al Ta1 Al 65.80(3) 1_655 1_645 ? C Ta1 Al 101.4(4) 1_545 1_545 ? C Ta1 Al 164.4(5) 1_655 1_545 ? C Ta1 Al 101.4(4) . 1_545 ? Al Ta1 Al 65.80(3) 1_655 1_545 ? Al Ta1 Al 65.80(3) 1_645 1_545 ? C Ta1 Ta1 45.2(3) 1_545 1_445 ? C Ta1 Ta1 134.8(3) 1_655 1_445 ? C Ta1 Ta1 90.000(3) . 1_445 ? Al Ta1 Ta1 122.900(13) 1_655 1_445 ? Al Ta1 Ta1 90.0 1_645 1_445 ? Al Ta1 Ta1 57.100(13) 1_545 1_445 ? C Ta1 Ta1 134.8(3) 1_545 1_665 ? C Ta1 Ta1 45.2(3) 1_655 1_665 ? C Ta1 Ta1 90.000(3) . 1_665 ? Al Ta1 Ta1 57.100(13) 1_655 1_665 ? Al Ta1 Ta1 90.0 1_645 1_665 ? Al Ta1 Ta1 122.899(13) 1_545 1_665 ? Ta1 Ta1 Ta1 180.0 1_445 1_665 ? C Ta1 Ta1 45.2(3) 1_545 1_545 ? C Ta1 Ta1 90.000(1) 1_655 1_545 ? C Ta1 Ta1 134.8(3) . 1_545 ? Al Ta1 Ta1 122.900(13) 1_655 1_545 ? Al Ta1 Ta1 57.100(13) 1_645 1_545 ? Al Ta1 Ta1 90.0 1_545 1_545 ? Ta1 Ta1 Ta1 60.0 1_445 1_545 ? Ta1 Ta1 Ta1 120.0 1_665 1_545 ? C Ta1 Ta1 90.000(1) 1_545 1_455 ? C Ta1 Ta1 134.8(3) 1_655 1_455 ? C Ta1 Ta1 45.2(3) . 1_455 ? Al Ta1 Ta1 90.0 1_655 1_455 ? Al Ta1 Ta1 122.900(13) 1_645 1_455 ? Al Ta1 Ta1 57.100(13) 1_545 1_455 ? Ta1 Ta1 Ta1 60.0 1_445 1_455 ? Ta1 Ta1 Ta1 120.0 1_665 1_455 ? Ta1 Ta1 Ta1 120.0 1_545 1_455 ? C Ta1 Ta1 90.000(1) 1_545 1_655 ? C Ta1 Ta1 45.2(3) 1_655 1_655 ? C Ta1 Ta1 134.8(3) . 1_655 ? Al Ta1 Ta1 90.0 1_655 1_655 ? Al Ta1 Ta1 57.100(13) 1_645 1_655 ? Al Ta1 Ta1 122.900(13) 1_545 1_655 ? Ta1 Ta1 Ta1 120.0 1_445 1_655 ? Ta1 Ta1 Ta1 60.0 1_665 1_655 ? Ta1 Ta1 Ta1 60.0 1_545 1_655 ? Ta1 Ta1 Ta1 180.0 1_455 1_655 ? C Ta1 Ta1 134.8(3) 1_545 1_565 ? C Ta1 Ta1 90.000(1) 1_655 1_565 ? C Ta1 Ta1 45.2(3) . 1_565 ? Al Ta1 Ta1 57.100(13) 1_655 1_565 ? Al Ta1 Ta1 122.899(13) 1_645 1_565 ? Al Ta1 Ta1 90.0 1_545 1_565 ? Ta1 Ta1 Ta1 120.0 1_445 1_565 ? Ta1 Ta1 Ta1 60.0 1_665 1_565 ? Ta1 Ta1 Ta1 180.0 1_545 1_565 ? Ta1 Ta1 Ta1 60.0 1_455 1_565 ? Ta1 Ta1 Ta1 120.0 1_655 1_565 ? C Ta2 C 180.000(2) 13_566 1_565 ? C Ta2 C 89.1(6) 13_566 13_576 ? C Ta2 C 90.9(6) 1_565 13_576 ? C Ta2 C 90.9(6) 13_566 . ? C Ta2 C 89.1(6) 1_565 . ? C Ta2 C 180.0(9) 13_576 . ? C Ta2 C 89.1(6) 13_566 13_676 ? C Ta2 C 90.9(6) 1_565 13_676 ? C Ta2 C 89.1(6) 13_576 13_676 ? C Ta2 C 90.9(6) . 13_676 ? C Ta2 C 90.9(6) 13_566 1_455 ? C Ta2 C 89.1(6) 1_565 1_455 ? C Ta2 C 90.9(6) 13_576 1_455 ? C Ta2 C 89.1(6) . 1_455 ? C Ta2 C 180.0 13_676 1_455 ? C Ta2 Ta2 134.5(3) 13_566 1_665 ? C Ta2 Ta2 45.5(3) 1_565 1_665 ? C Ta2 Ta2 90.000(2) 13_576 1_665 ? C Ta2 Ta2 90.000(2) . 1_665 ? C Ta2 Ta2 45.5(3) 13_676 1_665 ? C Ta2 Ta2 134.5(3) 1_455 1_665 ? C Ta2 Ta2 45.5(3) 13_566 1_445 ? C Ta2 Ta2 134.5(3) 1_565 1_445 ? C Ta2 Ta2 90.000(2) 13_576 1_445 ? C Ta2 Ta2 90.000(2) . 1_445 ? C Ta2 Ta2 134.5(3) 13_676 1_445 ? C Ta2 Ta2 45.5(3) 1_455 1_445 ? Ta2 Ta2 Ta2 180.0 1_665 1_445 ? C Ta2 Ta2 134.5(3) 13_566 1_565 ? C Ta2 Ta2 45.5(3) 1_565 1_565 ? C Ta2 Ta2 45.5(3) 13_576 1_565 ? C Ta2 Ta2 134.5(3) . 1_565 ? C Ta2 Ta2 90.000(1) 13_676 1_565 ? C Ta2 Ta2 90.000(1) 1_455 1_565 ? Ta2 Ta2 Ta2 60.0 1_665 1_565 ? Ta2 Ta2 Ta2 120.0 1_445 1_565 ? C Ta2 Ta2 45.5(3) 13_566 1_545 ? C Ta2 Ta2 134.5(3) 1_565 1_545 ? C Ta2 Ta2 134.5(3) 13_576 1_545 ? C Ta2 Ta2 45.5(3) . 1_545 ? C Ta2 Ta2 90.000(1) 13_676 1_545 ? C Ta2 Ta2 90.000(1) 1_455 1_545 ? Ta2 Ta2 Ta2 120.0 1_665 1_545 ? Ta2 Ta2 Ta2 60.0 1_445 1_545 ? Ta2 Ta2 Ta2 180.0 1_565 1_545 ? C Ta2 Ta2 90.000(1) 13_566 1_455 ? C Ta2 Ta2 90.000(1) 1_565 1_455 ? C Ta2 Ta2 45.5(3) 13_576 1_455 ? C Ta2 Ta2 134.5(3) . 1_455 ? C Ta2 Ta2 134.5(3) 13_676 1_455 ? C Ta2 Ta2 45.5(3) 1_455 1_455 ? Ta2 Ta2 Ta2 120.0 1_665 1_455 ? Ta2 Ta2 Ta2 60.0 1_445 1_455 ? Ta2 Ta2 Ta2 60.0 1_565 1_455 ? Ta2 Ta2 Ta2 120.0 1_545 1_455 ? C Ta2 Ta2 90.000(1) 13_566 1_655 ? C Ta2 Ta2 90.000(1) 1_565 1_655 ? C Ta2 Ta2 134.5(3) 13_576 1_655 ? C Ta2 Ta2 45.5(3) . 1_655 ? C Ta2 Ta2 45.5(3) 13_676 1_655 ? C Ta2 Ta2 134.5(3) 1_455 1_655 ? Ta2 Ta2 Ta2 60.0 1_665 1_655 ? Ta2 Ta2 Ta2 120.0 1_445 1_655 ? Ta2 Ta2 Ta2 120.0 1_565 1_655 ? Ta2 Ta2 Ta2 60.0 1_545 1_655 ? Ta2 Ta2 Ta2 180.0 1_455 1_655 ? Ta1 Al Ta1 143.448(14) 16_567 1_455 ? Ta1 Al Ta1 143.448(14) 16_567 1_465 ? Ta1 Al Ta1 65.80(3) 1_455 1_465 ? Ta1 Al Ta1 65.80(3) 16_567 16_467 ? Ta1 Al Ta1 143.448(14) 1_455 16_467 ? Ta1 Al Ta1 102.31(3) 1_465 16_467 ? Ta1 Al Ta1 102.31(3) 16_567 1_565 ? Ta1 Al Ta1 65.80(3) 1_455 1_565 ? Ta1 Al Ta1 65.80(3) 1_465 1_565 ? Ta1 Al Ta1 143.448(14) 16_467 1_565 ? Ta1 Al Ta1 65.80(3) 16_567 16_457 ? Ta1 Al Ta1 102.31(3) 1_455 16_457 ? Ta1 Al Ta1 143.448(14) 1_465 16_457 ? Ta1 Al Ta1 65.80(3) 16_467 16_457 ? Ta1 Al Ta1 143.448(14) 1_565 16_457 ? Ta1 C Ta1 89.5(6) 1_565 1_455 ? Ta1 C Ta1 89.5(6) 1_565 . ? Ta1 C Ta1 89.5(6) 1_455 . ? Ta1 C Ta2 179.7(9) 1_565 1_545 ? Ta1 C Ta2 90.69(2) 1_455 1_545 ? Ta1 C Ta2 90.69(2) . 1_545 ? Ta1 C Ta2 90.69(2) 1_565 . ? Ta1 C Ta2 90.69(2) 1_455 . ? Ta1 C Ta2 179.7(9) . . ? Ta2 C Ta2 89.1(6) 1_545 . ? Ta1 C Ta2 90.69(2) 1_565 1_655 ? Ta1 C Ta2 179.7(9) 1_455 1_655 ? Ta1 C Ta2 90.69(2) . 1_655 ? Ta2 C Ta2 89.1(6) 1_545 1_655 ? Ta2 C Ta2 89.1(6) . 1_655 ? 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 C 2.201(13) 1_545 ? Ta1 C 2.201(13) 1_655 ? Ta1 C 2.201(13) . ? Ta1 Al 2.8540(10) 1_655 ? Ta1 Al 2.8540(10) 1_645 ? Ta1 Al 2.8540(10) 1_545 ? Ta1 Ta1 3.1004(4) 1_445 ? Ta1 Ta1 3.1004(4) 1_665 ? Ta1 Ta1 3.1004(4) 1_545 ? Ta1 Ta1 3.1004(4) 1_455 ? Ta1 Ta1 3.1004(4) 1_655 ? Ta1 Ta1 3.1004(4) 1_565 ? Ta2 C 2.210(13) 13_566 ? Ta2 C 2.210(13) 1_565 ? Ta2 C 2.210(12) 13_576 ? Ta2 C 2.210(12) . ? Ta2 C 2.210(13) 13_676 ? Ta2 C 2.210(13) 1_455 ? Ta2 Ta2 3.1004(4) 1_665 ? Ta2 Ta2 3.1004(4) 1_445 ? Ta2 Ta2 3.1004(4) 1_565 ? Ta2 Ta2 3.1004(4) 1_545 ? Ta2 Ta2 3.1004(4) 1_455 ? Ta2 Ta2 3.1004(4) 1_655 ? Al Ta1 2.8540(10) 16_567 ? Al Ta1 2.8540(10) 1_455 ? Al Ta1 2.8540(10) 1_465 ? Al Ta1 2.8540(10) 16_467 ? Al Ta1 2.8540(10) 1_565 ? Al Ta1 2.8540(10) 16_457 ? C Ta1 2.201(13) 1_565 ? C Ta1 2.201(13) 1_455 ? C Ta2 2.210(12) 1_545 ? C Ta2 2.210(12) 1_655 ? _journal_paper_doi 10.1021/ic062231y