#------------------------------------------------------------------------------ #$Date: 2015-01-23 14:30:19 +0200 (Fri, 23 Jan 2015) $ #$Revision: 130086 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/00/56/2005683.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2005683 loop_ _publ_author_name 'Mahoui, A.' 'Lapasset, J.' 'Moret, J.' 'Saint Gr\'egoire, P.' _publ_section_title ; Tetraethylammonium Tetramethylammonium Tetrachlorocuprate(II), [(C~2~H~5~)~4~N][(CH~3~)~4~N][CuCl~4~] ; _journal_issue 11 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 2674 _journal_page_last 2676 _journal_paper_doi 10.1107/S0108270196009031 _journal_volume 52 _journal_year 1996 _chemical_formula_iupac '(C8 H20 N) (C4 H12 N) [Cu Cl4]' _chemical_formula_moiety '(C8 H20 N) 1+, (C4 H12 N) 1+, Cl4 Cu 2-' _chemical_formula_structural '(C8 H20 N, C4 H12 N) Cu Cl4' _chemical_formula_sum 'C12 H32 Cl4 Cu N2' _chemical_formula_weight 409.74 _chemical_name_systematic ; (tetraethylammonium,tetramethylammonium)-tetrachlorocuprate ; _space_group_IT_number 113 _symmetry_cell_setting tetragonal _symmetry_space_group_name_Hall 'P -4 2ab' _symmetry_space_group_name_H-M 'P -4 21 m' _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 13.078(10) _cell_length_b 13.078(10) _cell_length_c 11.871(10) _cell_measurement_reflns_used 20 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 55 _cell_measurement_theta_min 42 _cell_volume 2030(3) _computing_cell_refinement 'Enraf-Nonius CAD3' _computing_data_collection 'Enraf-Nonius CAD3' _computing_data_reduction 'Local program' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL93 _computing_structure_refinement 'SHELXL93 (Sheldrick, 1993)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measurement_device 'Enraf-Nonius CAD3' _diffrn_measurement_method \q/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.5418 _diffrn_reflns_av_R_equivalents 0.0238 _diffrn_reflns_av_sigmaI/netI 0.0198 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 1765 _diffrn_reflns_theta_max 65.12 _diffrn_reflns_theta_min 5.03 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 40 _diffrn_standards_number 2 _exptl_absorpt_coefficient_mu 6.280 _exptl_absorpt_correction_T_max 0.4250 _exptl_absorpt_correction_T_min 0.1783 _exptl_absorpt_correction_type 'SHELX76 gaussian (Sheldrick, 1976)' _exptl_crystal_colour yellow-orange _exptl_crystal_density_diffrn 1.340 _exptl_crystal_density_meas ? _exptl_crystal_description prism _exptl_crystal_F_000 860 _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.20 _refine_diff_density_max 0.492 _refine_diff_density_min -0.484 _refine_ls_abs_structure_details 'Flack (1983)' _refine_ls_abs_structure_Flack -0.14(10) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 1.097 _refine_ls_goodness_of_fit_obs 1.123 _refine_ls_hydrogen_treatment noref _refine_ls_matrix_type full _refine_ls_number_parameters 73 _refine_ls_number_reflns 952 _refine_ls_number_restraints 4 _refine_ls_restrained_S_all 1.096 _refine_ls_restrained_S_obs 1.121 _refine_ls_R_factor_all 0.0761 _refine_ls_R_factor_obs 0.0702 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme 'calc w = 1/[\s^2^(Fo^2^)+(0.0838P)^2^+5.7928P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_wR_factor_all 0.1763 _refine_ls_wR_factor_obs 0.1716 _reflns_number_observed 866 _reflns_number_total 952 _reflns_observed_criterion >2sigma(I) _[local]_cod_data_source_file sk1018.cif _[local]_cod_data_source_block teatmacucl _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'not measured' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas ; _cod_original_cell_volume 2030.(3) _cod_database_code 2005683 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' '-y+1/2, -x+1/2, z' 'y+1/2, x+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 Cu 0.0526(7) 0.0526(7) 0.0467(9) 0.0001(10) -0.0026(7) -0.0026(7) Cl1 0.149(3) 0.054(2) 0.082(2) 0.025(2) -0.033(2) -0.009(2) Cl2 0.136(3) 0.136(3) 0.047(2) 0.041(5) -0.008(2) -0.008(2) Cl3 0.082(2) 0.082(2) 0.076(2) -0.022(2) 0.005(2) 0.0047(15) loop_ _atom_site_label _atom_site_occupancy _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_type_symbol Cu 1 0.74605(10) 0.24605(10) 0.80803(15) 0.0507(5) Uani d S Cu Cl1 1 0.7926(3) 0.0865(2) 0.7612(3) 0.0951(12) Uani d . Cl Cl2 1 0.7517(4) 0.2517(4) 0.9967(3) 0.106(2) Uani d S Cl Cl3 1 0.8503(2) 0.3503(2) 0.7081(3) 0.0801(12) Uani d S Cl N1 1 0.2897(6) 0.7897(6) 0.3923(8) 0.045(2) Uiso d S N C111 1 0.3802(8) 0.7492(9) 0.3248(9) 0.067(3) Uiso d . C H1111 1 0.3566(8) 0.7311(9) 0.2500(9) 0.101 Uiso calc R H H1112 1 0.4301(8) 0.8036(9) 0.3167(9) 0.101 Uiso calc R H C112 1 0.4323(10) 0.6571(10) 0.3765(11) 0.092(4) Uiso d . C H1121 1 0.4883(10) 0.6364(10) 0.3295(11) 0.138 Uiso calc R H H1122 1 0.3841(10) 0.6020(10) 0.3827(11) 0.138 Uiso calc R H H1123 1 0.4574(10) 0.6746(10) 0.4500(11) 0.138 Uiso calc R H C121 1 0.3227(9) 0.8227(9) 0.5087(14) 0.076(4) Uiso d S C H1211 0.50 0.3479(9) 0.7633(9) 0.5489(14) 0.114 Uiso calc PR H H1212 0.50 0.2633(9) 0.8479(9) 0.5489(14) 0.114 Uiso calc PR H C122 1 0.4039(10) 0.9039(10) 0.5107(16) 0.089(5) Uiso d S C H1221 1 0.4206(10) 0.9203(10) 0.5873(16) 0.134 Uiso calc SR H H1222 0.50 0.3792(10) 0.9641(10) 0.4732(16) 0.134 Uiso calc PR H H1223 0.50 0.4639(10) 0.8793(10) 0.4728(16) 0.134 Uiso calc PR H C131 1 0.2095(10) 0.7095(10) 0.4090(16) 0.087(5) Uiso d S C H1311 0.50 0.2387(10) 0.6541(10) 0.4528(16) 0.130 Uiso calc PR H H1312 0.50 0.1541(10) 0.7387(10) 0.4528(16) 0.130 Uiso calc PR H C132 1 0.1659(11) 0.6659(11) 0.3019(15) 0.090(5) Uiso d S C H1321 1 0.1150(11) 0.6157(11) 0.3200(15) 0.135 Uiso calc SR H H1322 0.50 0.2196(11) 0.6345(11) 0.2590(15) 0.135 Uiso calc PR H H1323 0.50 0.1354(11) 0.7198(11) 0.2585(15) 0.135 Uiso calc PR H N2 1 0.0000 0.0000 0.0000 0.064(5) Uiso d S N C2 1 0.0321(10) 0.0869(10) -0.0709(11) 0.081(3) Uiso d . C H21 1 -0.0240(10) 0.1082(10) -0.1174(11) 0.122 Uiso calc R H H22 1 0.0883(10) 0.0664(10) -0.1177(11) 0.122 Uiso calc R H H23 1 0.0529(10) 0.1427(10) -0.0237(11) 0.122 Uiso calc R H N3 1 0.0000 0.5000 0.0054(14) 0.056(5) Uiso d SD N C31 0.25 -0.023(5) 0.607(3) -0.031(5) 0.105(10) Uiso d PD C H311 0.25 -0.057(2) 0.606(3) -0.102(5) 0.157 Uiso calc PR H H312 0.25 0.040(5) 0.644(3) -0.038(5) 0.157 Uiso calc PR H H313 0.25 -0.065(5) 0.639(3) 0.025(5) 0.157 Uiso calc PR H C32 0.25 -0.100(3) 0.443(4) 0.024(4) 0.105(10) Uiso d PD C H321 0.25 -0.133(3) 0.431(4) -0.047(4) 0.157 Uiso calc PR H H322 0.25 -0.144(3) 0.483(4) 0.072(4) 0.157 Uiso calc PR H H323 0.25 -0.086(3) 0.378(4) 0.060(4) 0.157 Uiso calc PR H C33 0.25 0.051(4) 0.518(4) 0.114(3) 0.105(10) Uiso d PD C H331 0.25 0.066(4) 0.453(4) 0.149(3) 0.157 Uiso calc PR H H332 0.25 0.008(4) 0.557(4) 0.162(3) 0.157 Uiso calc PR H H333 0.25 0.114(4) 0.554(4) 0.101(3) 0.157 Uiso calc PR H C34 0.50 0.060(2) 0.441(2) -0.076(4) 0.105(10) Uiso d SPD C H341 0.25 0.020(2) 0.431(2) -0.144(4) 0.157 Uiso calc PR H H342 0.25 0.076(2) 0.375(2) -0.045(4) 0.157 Uiso calc PR H H343 0.25 0.122(2) 0.476(2) -0.094(4) 0.157 Uiso calc PR H loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 '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_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl1 Cu Cl1 8_545 116.3(2) yes Cl1 Cu Cl2 . 105.60(10) yes Cl1 Cu Cl3 . 105.50(10) yes Cl2 Cu Cl3 . 118.9(2) yes C111 N1 C111 8_455 105.3(10) yes C111 N1 C121 . 111.0(7) yes C111 N1 C131 . 111.7(7) yes C121 N1 C131 . 106.2(11) yes C112 C111 N1 . 114.4(9) yes C122 C121 N1 . 115.0(10) yes C132 C131 N1 . 115.0(10) yes C2 N2 C2 2 110.4(10) yes C2 N2 C2 4 109.0(5) yes C31 N3 C32 . 109(4) yes C31 N3 C33 . 101(3) yes C31 N3 C34 . 114(3) yes C32 N3 C33 . 110(3) yes C32 N3 C34 . 107(2) yes C33 N3 C34 . 115(3) yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Cu Cl1 2.243(3) yes Cu Cl2 2.242(5) yes Cu Cl3 2.264(5) yes N1 C111 1.520(10) yes N1 C121 1.51(2) yes N1 C131 1.50(2) yes C111 C112 1.51(2) yes C121 C122 1.50(2) yes C131 C132 1.51(3) yes N2 C2 1.480(10) yes N3 C31 1.49(4) yes N3 C32 1.52(4) yes N3 C33 1.47(3) yes N3 C34 1.47(3) yes