#------------------------------------------------------------------------------ #$Date: 2010-09-26 13:00:33 +0200 (Sun, 26 Sep 2010) $ #$Revision: 1526 $ #$URL: svn://www.crystallography.net/cod/cif/4/4308590.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_4308590 loop_ _publ_author_name 'Torsten K\"uppers' 'Eduard Bernhardt' 'Helge Willner' 'Henning W. Rohm' 'Martin K\"ockerling' _publ_contact_author ; Martin K\"ockerling Universit\"at Rostock Fachbereich Chemie Anorganische Chemie/Festk\"orperchemie Albert-Einstein-Str. 3a D-18057 Rostock Germany ; _publ_contact_author_email martin.koeckerling@chemie.uni-rostock.de _publ_contact_author_fax intl-code-(0)381-498-6382 _publ_contact_author_phone intl-code-(0)381-498-6390 _publ_section_title ; Tetracyanoborate Salts M[B(CN)4] with M = Singly Charged Cations: Properties and Structures ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 1015 _journal_page_last 1022 _journal_volume 44 _journal_year 2005 _chemical_formula_moiety 'C4 B N4 Tl' _chemical_formula_structural 'Tl B (CN)4' _chemical_formula_sum 'C4 B N4 Tl' _chemical_formula_weight 319.26 _chemical_name_systematic Thallium-tetracyanoborate _space_group_IT_number 88 _symmetry_cell_setting tetragonal _symmetry_space_group_name_Hall '-I 4ad' _symmetry_space_group_name_H-M 'I 41/a :2' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_date august-2-2004 _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 7.0644(4) _cell_length_b 7.0644(4) _cell_length_c 14.6791(12) _cell_measurement_reflns_used 2574 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 37.55 _cell_measurement_theta_min 1.5 _cell_volume 732.57(8) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'Bruker SHELXTL' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.465 _diffrn_measured_fraction_theta_max 0.465 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _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 0.0491 _diffrn_reflns_av_sigmaI/netI 0.0566 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 3195 _diffrn_reflns_theta_full 39.72 _diffrn_reflns_theta_max 39.72 _diffrn_reflns_theta_min 3.20 _diffrn_standards_decay_% 0 _exptl_absorpt_coefficient_mu 21.967 _exptl_absorpt_correction_T_max 0.972 _exptl_absorpt_correction_T_min 0.875 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, Bruker, 2000)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.895 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_description irregular _exptl_crystal_F_000 552 _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.20 _refine_diff_density_max 4.429 _refine_diff_density_min -2.295 _refine_diff_density_rms 0.414 _refine_ls_extinction_coef 0.026(2) _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 1.053 _refine_ls_matrix_type full _refine_ls_number_parameters 24 _refine_ls_number_reflns 1069 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.053 _refine_ls_R_factor_all 0.0691 _refine_ls_R_factor_gt 0.0520 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0847P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_wR_factor_gt 0.1326 _refine_ls_wR_factor_ref 0.1403 _reflns_number_gt 800 _reflns_number_total 1069 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file ic048780qsi20041119_090312_9.cif _[local]_cod_data_source_block TlB(CN)4 _[local]_cod_cif_authors_sg_H-M 'I 41/a' _cod_database_code 4308590 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' 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 B1 B 0.0000 0.2500 0.1250 0.0176(17) Uani 1 d S . . C1 C 0.1507(7) 0.1445(7) 0.0636(4) 0.0204(8) Uani 1 d . . . N1 N 0.2597(8) 0.5652(8) -0.0210(5) 0.0346(12) Uani 1 d . . . Tl1 Tl 0.5000 0.7500 0.1250 0.0263(2) Uani 1 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 B1 0.015(2) 0.015(2) 0.022(5) 0.000 0.000 0.000 C1 0.018(2) 0.020(2) 0.024(2) -0.0012(17) 0.0035(16) 0.0016(14) N1 0.031(3) 0.035(3) 0.038(3) 0.007(2) -0.012(2) 0.005(2) Tl1 0.0262(2) 0.0262(2) 0.0264(3) 0.000 0.000 0.000 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' 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' Tl Tl -2.8358 9.6688 '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 C1 B1 C1 110.5(4) 12_666 15 C1 B1 C1 108.97(19) 12_666 . C1 B1 C1 108.97(19) 15 . C1 B1 C1 108.97(19) 12_666 6_454 C1 B1 C1 108.97(19) 15 6_454 C1 B1 C1 110.5(4) . 6_454 N1 C1 B1 178.3(6) 14_545 . N1 Tl1 N1 120.02(16) . 15_565 N1 Tl1 N1 120.02(16) . 12_766 N1 Tl1 N1 90.0(3) 15_565 12_766 N1 Tl1 N1 90.0(3) . 6_564 N1 Tl1 N1 120.02(16) 15_565 6_564 N1 Tl1 N1 120.02(16) 12_766 6_564 N1 Tl1 N1 163.6(2) . 8_454 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 B1 C1 1.581(5) 12_666 B1 C1 1.581(5) 15 B1 C1 1.581(5) . B1 C1 1.581(5) 6_454 C1 N1 1.139(7) 14_545 N1 C1 1.139(7) 14