#------------------------------------------------------------------------------ #$Date: 2008-03-02 13:24:56 +0000 (Sun, 02 Mar 2008) $ #$Revision: 199 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003215.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_2003215 _journal_name_full 'Acta Crystallographica' _journal_volume C51 _journal_page_first 220 _journal_page_last 222 _publ_section_title ; Tetraethylammonium Tetramethylammonium Tetrachlorozincate(II), [(C~2~H~5~)~4~N][(CH~3~)~4~N]ZnCl~4~ ; loop_ _publ_author_name 'Odile Ca\"etano' 'Jacques Lapasset' 'Pierre Saint Gr\'egoire' _chemical_formula_sum 'C12 H32 Cl4 N2 Zn1' _chemical_formula_structural '[N (C2 H5 )4 ] [N (C H3 )4 ] Zn Cl4' _chemical_formula_weight 411.61 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' _symmetry_space_group_name_H-M 'P -4 21 m' _cell_length_a 13.087(2) _cell_length_b 13.087(2) _cell_length_c 11.793(1) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2019.8(5) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.353 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _cell_measurement_reflns_used 23 _cell_measurement_theta_min 13.6 _cell_measurement_theta_max 23 _exptl_absorpt_coefficient_mu 1.629 _cell_measurement_temperature 298 _exptl_crystal_description square _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.10 _exptl_crystal_colour colourless _diffrn_measurement_device 'Nonius CAD4 four-circle diffractometer' _diffrn_measurement_method '\q/2\q' _exptl_absorpt_correction_type 'SHELX76 (Sheldrick, 1976) Gaussian' _exptl_absorpt_correction_T_min .69 _exptl_absorpt_correction_T_max .86 _diffrn_reflns_number 3323 _reflns_number_total 1744 _reflns_number_observed 737 _reflns_observed_criterion 'F > 4\s(F)' _diffrn_reflns_av_R_equivalents 0.0123 _diffrn_reflns_theta_max 30 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.041 _refine_ls_wR_factor_obs 0.042 _refine_ls_goodness_of_fit_obs 1.33 _refine_ls_number_reflns 737 _refine_ls_number_parameters 75 _refine_ls_hydrogen_treatment 'refU' _refine_ls_weighting_scheme 'calc w=1/[\s^2^(F)+0.001033 F^2^]' _refine_ls_shift/esd_max 0.04 _refine_diff_density_max 0.474 _refine_diff_density_min -0.390 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag C 'Cromer and Mann (1968)' 0 0 H 'Cromer and Mann (1968)' 0 0 N 'Cromer and Mann (1968)' 0 0 Cl 'Cromer and Mann (1968)' .1 .2 Zn 'IntTabIV Table 2.2B' .3 1.5 _refine_ls_abs_structure_details ? ##;ORTEPII (Johnson, 1976), adapted to the Macintosh (Andr\'e & Michalowicz, ## 1991) ##; 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 Zn 1 .7460(1) .2460(1) .8127(1) .0366(4) Cl1 1 .7841(2) .0835(2) .7612(2) .074(2) Cl2 1 .7581(4) .2581(4) 1.0039(2) .073(2) Cl3 1 .8539(4) .3539(4) .7205(3) .075(2) N1 1 .291(1) .791(1) .3937(7) .048(2) N2 1 .0000 .0000 .0000 .057(5) N3 1 .0000 .5000 .012(1) .052(4) C111 1 .3798(6) .7496(7) .3244(7) .065(2) C112 1 .4325(8) .6575(7) .3781(8) .086(3) C121 1 .328(1) .828(1) .509(1) .066(4) C122 1 .407(2) .907(2) .504(1) .103(5) C131 1 .211(2) .711(2) .415(1) .068(4) C132 1 .165(2) .665(2) .3097(12) .088(5) C2 1 .0336(8) .0884(7) -.0745(9) .076(3) C31 .25 -.021(3) .612(3) -.0246(25) .059(5) C32 .25 -.097(2) .445(2) .0296(24) .059(5) C33 .25 .051(2) .522(2) .125(2) .059(5) C34 .25 .075(2) .459(2) -.064(3) .059(5) H1111 1 .3512(6) .7272(7) .2421(7) .08(1) H1112 1 .4356(6) .8097(6) .3143(6) .08(1) H1121 1 .4944(8) .6325(7) .3241(8) .13(2) H1122 1 .3780(8) .5962(7) .3880(8) .13(2) H1123 1 .4625(8) .6787(7) .4601(8) .13(2) H1211 .5 .358(1) .763(1) .555(1) .08(1) H1212 .5 .263(1) .858(1) .555(1) .08(1) H1221 .5 .4287(16) .9287(16) .589(1) .13(2) H1222 .5 .3777(16) .973(2) .459(2) .13(2) H1223 .5 .473(2) .8777(16) .459(2) .13(2) H1311 .5 .2456(15) .650(2) .464(1) .08(1) H1312 .5 .150(2) .7456(15) .464(1) .08(1) H1321 .5 .1089(16) .6089(16) .333(1) .13(2) H1322 .5 .2248(16) .6295(16) .260(1) .13(2) H1323 .5 .1295(16) .7248(16) .260(1) .13(2) H21 1 .0576(8) .1514(7) -.0217(9) .101(12) H22 1 -.0294(8) .1123(7) -.1273(9) .101(12) H23 1 .0966(8) .0643(7) -.1273(9) .101(12) H311 .25 -.059(3) .613(2) -.106(3) .09(3) H312 .25 .0499(26) .654(2) -.0308(25) .09(3) H313 .25 -.0699(26) .6489(24) .0375(25) .09(3) H321 .25 -.132(2) .4298(21) -.052(2) .09(3) H322 .25 -.147(2) .490(2) .0811(2) .09(3) H323 .25 -.0815(2) .3729(2) .0719(24) .09(3) H331 .25 .072(2) .450(2) .165(2) .09(3) H332 .25 -.001(2) .563(2) .179(2) .09(3) H333 .25 .119(2) .567(2) .111(2) .09(3) H341 .25 .039(2) .443(2) -.145(3) .09(3) H342 .25 .106(2) .389(2) -.0296(24) .09(3) H343 .25 .136(2) .513(3) -.076(3) .09(3) loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 Zn .0374(4) -.0008(8) -.0044(4) .0374(4) -.0044(5) .0349(5) Cl1 .0986(17) .0152(11) -.0277(13) .0524(11) -.0088(11) .0718(12) Cl2 .0870(12) .008(3) -.0074(11) .0870(12) -.0074(11) .0461(12) Cl3 .0750(13) -.0155(18) .0071(11) .0750(13) .0071(11) .075(21)