#------------------------------------------------------------------------------ #$Date: 2016-03-23 00:41:36 +0200 (Wed, 23 Mar 2016) $ #$Revision: 179123 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/30/85/4308588.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_4308588 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_paper_doi 10.1021/ic048780q _journal_volume 44 _journal_year 2005 _chemical_formula_moiety 'C4 H8 O, C4 B N4, H4 N' _chemical_formula_structural 'C4 H8 O, C4 B N4, H4 N' _chemical_formula_sum 'C8 H12 B N5 O' _chemical_formula_weight 205.04 _chemical_name_systematic Ammonium-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 8.831(1) _cell_length_b 9.366(2) _cell_length_c 15.061(3) _cell_measurement_reflns_used 30 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 27 _cell_measurement_theta_min 1.75 _cell_volume 1245.7(4) _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 0.917 _diffrn_measured_fraction_theta_max 0.917 _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 0.0379 _diffrn_reflns_av_sigmaI/netI 0.0225 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 1 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 1956 _diffrn_reflns_theta_full 27.00 _diffrn_reflns_theta_max 27.00 _diffrn_reflns_theta_min 2.56 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 98 _diffrn_standards_number 2 _exptl_absorpt_coefficient_mu 0.076 _exptl_absorpt_correction_T_max 0.930 _exptl_absorpt_correction_T_min 0.738 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details 'North, Phillips & Mathews (1968)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.093 _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'irregular block' _exptl_crystal_F_000 432 _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.19 _refine_diff_density_max 0.324 _refine_diff_density_min -0.175 _refine_diff_density_rms 0.067 _refine_ls_extinction_coef 0.046(12) _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 1.079 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 88 _refine_ls_number_reflns 1448 _refine_ls_number_restraints 3 _refine_ls_restrained_S_all 1.078 _refine_ls_R_factor_all 0.0876 _refine_ls_R_factor_gt 0.0692 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1193P)^2^+0.1556P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1932 _refine_ls_wR_factor_ref 0.2179 _reflns_number_gt 1021 _reflns_number_total 1448 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic048780qsi20041119_090312_7.cif _cod_data_source_block NH4B(CN)4_THF _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_absorpt_correction_type' tag value 'psi-scans' was replaced with 'psi-scan' value. Automatic conversion script Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w=1/[\s^2^(Fo^2^)+(0.1193P)^2^+0.1556P] where P=(Fo^2^+2Fc^2^)/3' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w=1/[\s^2^(Fo^2^)+(0.1193P)^2^+0.1556P] where P=(Fo^2^+2Fc^2^)/3'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_database_code 4308588 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.6472(3) 0.2500 0.36389(19) 0.0573(7) Uani 1 d S . . N1 N 0.8127(3) 0.0140(2) 0.40766(13) 0.0878(7) Uani 1 d . . . C1 C 0.7432(2) 0.1119(2) 0.38823(12) 0.0631(6) Uani 1 d . . . N2 N 0.5826(3) 0.2500 0.18656(19) 0.0955(10) Uani 1 d S . . C2 C 0.6104(3) 0.2500 0.26065(19) 0.0698(8) Uani 1 d S . . N3 N 0.3864(3) 0.2500 0.4591(2) 0.1054(11) Uani 1 d S . . C3 C 0.4941(3) 0.2500 0.41920(19) 0.0727(8) Uani 1 d S . . N4 N 0.0599(2) 0.2500 0.51273(15) 0.0590(6) Uani 1 d SD . . H1A H -0.033(3) 0.2500 0.534(2) 0.089 Uiso 1 d SD . . H1B H 0.068(4) 0.2500 0.4540(16) 0.089 Uiso 1 d SD . . H1C H 0.109(2) 0.173(2) 0.5302(16) 0.089 Uiso 1 d D . . O1 O -0.2279(3) 0.2500 0.59567(19) 0.1035(9) Uani 1 d S . . C4 C -0.2887(4) 0.1267(3) 0.6365(2) 0.1215(11) Uani 1 d . . . H4A H -0.2119 0.0791 0.6717 0.182 Uiso 1 calc R . . H4B H -0.3251 0.0604 0.5918 0.182 Uiso 1 calc R . . C5 C -0.4119(5) 0.1731(7) 0.6922(3) 0.190(2) Uani 1 d . . . H5A H -0.5073 0.1374 0.6694 0.284 Uiso 1 calc R . . H5B H -0.3984 0.1374 0.7521 0.284 Uiso 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 B1 0.0562(14) 0.0533(14) 0.0624(14) 0.000 -0.0030(12) 0.000 N1 0.0951(14) 0.0674(11) 0.1008(14) 0.0091(9) -0.0008(10) 0.0157(11) C1 0.0645(10) 0.0565(10) 0.0682(11) 0.0001(8) -0.0001(8) -0.0007(9) N2 0.103(2) 0.113(2) 0.0707(16) 0.000 -0.0124(14) 0.000 C2 0.0723(17) 0.0689(16) 0.0682(16) 0.000 -0.0050(13) 0.000 N3 0.0670(16) 0.133(3) 0.116(2) 0.000 0.0161(16) 0.000 C3 0.0595(16) 0.0753(18) 0.0834(19) 0.000 -0.0005(14) 0.000 N4 0.0552(12) 0.0556(12) 0.0661(12) 0.000 0.0023(10) 0.000 O1 0.0929(17) 0.0796(15) 0.138(2) 0.000 0.0463(15) 0.000 C4 0.141(3) 0.101(2) 0.122(2) 0.0210(18) 0.025(2) -0.0166(19) C5 0.168(3) 0.229(6) 0.171(3) 0.053(3) 0.084(3) -0.013(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' 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 C3 B1 C2 109.8(2) . . C3 B1 C1 109.45(14) . 7_565 C2 B1 C1 109.58(14) . 7_565 C3 B1 C1 109.45(14) . . C2 B1 C1 109.58(14) . . C1 B1 C1 108.9(2) 7_565 . N1 C1 B1 178.4(2) . . N2 C2 B1 179.5(3) . . N3 C3 B1 179.4(3) . . C4 O1 C4 109.5(3) 7_565 . O1 C4 C5 107.1(3) . . C5 C5 C4 107.6(3) 7_565 . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 B1 C3 1.588(4) . B1 C2 1.589(4) . B1 C1 1.589(2) 7_565 B1 C1 1.589(2) . N1 C1 1.142(3) . N2 C2 1.142(4) . N3 C3 1.125(4) . O1 C4 1.414(3) 7_565 O1 C4 1.414(3) . O1 C5 2.296(4) . O1 C5 2.296(4) 7_565 C4 C5 1.441(5) . C5 C5 1.440(12) 7_565