#------------------------------------------------------------------------------ #$Date: 2010-09-26 13:00:33 +0200 (Sun, 26 Sep 2010) $ #$Revision: 1526 $ #$URL: svn://www.crystallography.net/cod/cif/4/4308586.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_4308586 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 'C8 H8 B N4 Na O' _chemical_formula_structural 'Na B (CN)4 C4H4O' _chemical_formula_sum 'C8 H8 B N4 Na O' _chemical_formula_weight 209.98 _chemical_name_systematic Sodium-tetracyanoborate _space_group_IT_number 62 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2n' _symmetry_space_group_name_H-M 'P n m a' _atom_sites_solution_hydrogens geom _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 13.908(3) _cell_length_b 9.2880(10) _cell_length_c 8.7380(10) _cell_measurement_reflns_used 41 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 27 _cell_measurement_theta_min 1.5 _cell_volume 1128.8(3) _computing_cell_refinement 'Siemens XSCANS' _computing_data_collection 'Siemens XSCANS' _computing_data_reduction 'Siemens XSCANS' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_structure_solution 'Siemens SHELXTL' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Siemens P4' _diffrn_measurement_method '\w 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 0.0363 _diffrn_reflns_av_sigmaI/netI 0.0246 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_number 1780 _diffrn_reflns_theta_full 27.00 _diffrn_reflns_theta_max 27.00 _diffrn_reflns_theta_min 2.75 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 98 _diffrn_standards_number 2 _exptl_absorpt_coefficient_mu 0.117 _exptl_absorpt_correction_T_max 0.887 _exptl_absorpt_correction_T_min 0.852 _exptl_absorpt_correction_type psi-scans _exptl_absorpt_process_details 'North, Phillips & Mathews (1968)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.236 _exptl_crystal_density_method 'not measured' _exptl_crystal_description irregular _exptl_crystal_F_000 432 _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.29 _refine_diff_density_max 0.198 _refine_diff_density_min -0.188 _refine_diff_density_rms 0.046 _refine_ls_extinction_coef 0.038(7) _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 1.047 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 80 _refine_ls_number_reflns 1307 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.047 _refine_ls_R_factor_all 0.0700 _refine_ls_R_factor_gt 0.0496 _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^)+(0.0912P)^2^+0.1161P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1424 _refine_ls_wR_factor_ref 0.1584 _reflns_number_gt 917 _reflns_number_total 1307 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file ic048780qsi20041119_090312_5.cif _[local]_cod_data_source_block NaB(CN)4_THF _cod_database_code 4308586 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, 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 Na1 Na 0.07258(7) 0.2500 0.58285(11) 0.0470(4) Uani 1 2 d S . . B1 B 0.2734(2) 0.2500 0.0852(3) 0.0427(6) Uani 1 2 d S . . N1 N 0.1503(2) 0.2500 0.3277(3) 0.0666(7) Uani 1 2 d S . . C1 C 0.2020(2) 0.2500 0.2273(3) 0.0497(6) Uani 1 2 d S . . N2 N 0.38559(15) 0.0099(2) 0.0908(2) 0.0669(6) Uani 1 1 d . . . C2 C 0.33942(14) 0.11035(19) 0.08991(19) 0.0476(5) Uani 1 1 d . . . N3 N 0.16669(19) 0.2500 -0.1768(3) 0.0674(7) Uani 1 2 d S . . C3 C 0.2119(2) 0.2500 -0.0679(3) 0.0484(6) Uani 1 2 d S . . O1 O -0.06833(13) 0.2500 0.7293(2) 0.0536(5) Uani 1 2 d S . . C4 C -0.08816(18) 0.1248(2) 0.8197(3) 0.0729(7) Uani 1 1 d . . . H4A H -0.0342 0.0588 0.8160 0.109 Uiso 1 1 calc R . . H4B H -0.1446 0.0756 0.7810 0.109 Uiso 1 1 calc R . . C5 C -0.1045(3) 0.1727(3) 0.9759(3) 0.1337(16) Uani 1 1 d . . . H5A H -0.1657 0.1368 1.0128 0.201 Uiso 1 1 calc R . . H5B H -0.0540 0.1368 1.0424 0.201 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 Na1 0.0545(6) 0.0467(6) 0.0397(6) 0.000 0.0053(4) 0.000 B1 0.0541(15) 0.0378(13) 0.0363(13) 0.000 -0.0012(12) 0.000 N1 0.0875(17) 0.0596(15) 0.0527(14) 0.000 0.0198(14) 0.000 C1 0.0670(16) 0.0394(12) 0.0427(14) 0.000 0.0044(13) 0.000 N2 0.0858(13) 0.0543(11) 0.0605(11) 0.0044(9) 0.0011(9) 0.0193(10) C2 0.0630(10) 0.0416(9) 0.0381(9) 0.0000(8) 0.0002(8) 0.0024(8) N3 0.0731(16) 0.0775(17) 0.0517(14) 0.000 -0.0140(13) 0.000 C3 0.0572(15) 0.0447(13) 0.0432(14) 0.000 -0.0001(12) 0.000 O1 0.0667(12) 0.0448(10) 0.0493(11) 0.000 0.0128(9) 0.000 C4 0.0931(16) 0.0534(12) 0.0723(15) 0.0121(11) 0.0170(12) -0.0029(12) C5 0.227(4) 0.111(3) 0.0630(17) 0.0272(18) 0.041(2) 0.023(3) 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 '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 O1 Na1 N3 88.79(9) . 1_556 O1 Na1 N1 149.00(10) . . N3 Na1 N1 122.21(11) 1_556 . O1 Na1 N2 100.42(5) . 2 N3 Na1 N2 81.52(5) 1_556 2 N1 Na1 N2 85.58(5) . 2 O1 Na1 N2 100.42(5) . 8_666 N3 Na1 N2 81.52(5) 1_556 8_666 N1 Na1 N2 85.58(5) . 8_666 N2 Na1 N2 152.72(11) 2 8_666 C3 B1 C1 108.8(2) . . C3 B1 C2 109.44(14) . . C1 B1 C2 109.90(14) . . C3 B1 C2 109.44(14) . 7_565 C1 B1 C2 109.90(14) . 7_565 C2 B1 C2 109.4(2) . 7_565 C1 N1 Na1 166.5(3) . . N1 C1 B1 179.3(3) . . C2 N2 Na1 158.92(18) . 2_554 N2 C2 B1 178.7(2) . . C3 N3 Na1 178.4(2) . 1_554 N3 C3 B1 179.1(3) . . C4 O1 C4 108.5(2) . 7_565 C4 O1 Na1 117.56(12) . . C4 O1 Na1 117.56(12) 7_565 . O1 C4 C5 107.4(2) . . C5 C5 C4 107.83(15) 7_565 . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Na1 O1 2.341(2) . Na1 N3 2.475(3) 1_556 Na1 N1 2.477(3) . Na1 N2 2.4840(18) 2 Na1 N2 2.4840(18) 8_666 B1 C3 1.588(4) . B1 C1 1.590(4) . B1 C2 1.590(3) . B1 C2 1.590(3) 7_565 N1 C1 1.135(4) . N2 C2 1.133(2) . N2 Na1 2.4840(18) 2_554 N3 C3 1.141(3) . N3 Na1 2.475(3) 1_554 O1 C4 1.433(2) . O1 C4 1.433(2) 7_565 C4 C5 1.453(4) . C5 C5 1.436(6) 7_565