#------------------------------------------------------------------------------ #$Date: 2016-02-14 04:40:26 +0000 (Sun, 14 Feb 2016) $ #$Revision: 176432 $ #$URL: svn://www.crystallography.net/cod/cif/2/23/90/2239081.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_2239081 loop_ _publ_author_name 'Ouasri, Ali' 'Rhandour, Ali' 'Saadi, Mohamed' 'El Ammari, Lahcen' _publ_section_title ; Butane-1,4-diammonium hexafluorosilicate ; _journal_coeditor_code IM2447 _journal_issue 2 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first o174 _journal_paper_doi 10.1107/S1600536814001068 _journal_volume 70 _journal_year 2014 _chemical_formula_iupac 'C4 H14 N2 2+, Si F6 2-' _chemical_formula_moiety 'C4 H14 N2 2+, F6 Si 2-' _chemical_formula_sum 'C4 H14 F6 N2 Si' _chemical_formula_weight 232.26 _chemical_name_systematic ; Butane-1,4-diammonium hexafluorosilicate ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 87.020(10) _cell_angle_beta 82.150(10) _cell_angle_gamma 61.870(10) _cell_formula_units_Z 1 _cell_length_a 5.7960(10) _cell_length_b 5.8890(10) _cell_length_c 7.774(2) _cell_measurement_reflns_used 1285 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 29.56 _cell_measurement_theta_min 3.92 _cell_volume 231.79(8) _computing_cell_refinement 'SAINT (Bruker, 2009)' _computing_data_collection 'APEX2 (Bruker, 2009)' _computing_data_reduction 'SAINT (Bruker, 2009)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 2012)' _computing_publication_material 'PLATON (Spek, 2009) and publCIF (Westrip, 2010)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measurement_device_type 'Bruker X8 APEX' _diffrn_measurement_method '\f and \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 0.0247 _diffrn_reflns_av_sigmaI/netI 0.0308 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 5351 _diffrn_reflns_theta_full 29.56 _diffrn_reflns_theta_max 29.56 _diffrn_reflns_theta_min 3.92 _exptl_absorpt_coefficient_mu 0.308 _exptl_absorpt_correction_T_max 0.6398 _exptl_absorpt_correction_T_min 0.5121 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Bruker, 2009)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.664 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 120 _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.27 _refine_diff_density_max 0.735 _refine_diff_density_min -0.326 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 61 _refine_ls_number_reflns 1285 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.052 _refine_ls_R_factor_all 0.0558 _refine_ls_R_factor_gt 0.0383 _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^)+(0.0549P)^2^+0.1270P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1051 _refine_ls_wR_factor_ref 0.1077 _reflns_number_gt 1185 _reflns_number_total 1285 _reflns_threshold_expression I>2sigma(I) _iucr_refine_instructions_details ; TITL EL13_D207_DRX14_C4SI in P-1 CELL 0.71073 5.796 5.889 7.774 87.02 82.15 61.87 ZERR 1.00 0.001 0.001 0.002 0.01 0.01 0.01 LATT 1 SFAC C H SI N F UNIT 4 14 1 2 6 MERG 2 SHEL 60 0.72 OMIT 1 0 0 OMIT 0 -1 1 FMAP 2 PLAN 10 BOND BOND $H HTAB 2.6 HTAB N1 F2 HTAB N1 F3 HTAB N1 F3_$1 HTAB N1 F1_$2 eqiv $1 -x, 1-y, -z eqiv $2 x-1, y, z ACTA L.S. 10 WGHT 0.0549 0.1270 FVAR 0.73703 C1 1 -0.162884 0.274411 0.365020 11.00000 0.03036 0.04700 = 0.02659 0.00220 -0.00290 -0.00689 AFIX 23 H1A 2 0.013833 0.240682 0.380120 11.00000 -1.20000 H1B 2 -0.173905 0.116040 0.387644 11.00000 -1.20000 AFIX 0 C2 1 -0.359265 0.478262 0.495337 11.00000 0.03679 0.06492 = 0.02777 -0.01085 0.00141 -0.02333 AFIX 23 H2A 2 -0.357296 0.639581 0.466270 11.00000 -1.20000 H2B 2 -0.302437 0.429690 0.609382 11.00000 -1.20000 AFIX 0 N1 4 -0.208608 0.350827 0.182673 11.00000 0.02623 0.02873 = 0.02359 -0.00316 0.00072 -0.01171 AFIX 33 H1NA 2 -0.089145 0.225160 0.110970 11.00000 -1.50000 H1NB 2 -0.194622 0.493906 0.160297 11.00000 -1.50000 H1NC 2 -0.369456 0.379205 0.167487 11.00000 -1.50000 AFIX 0 MOLE 1 SI1 3 0.500000 0.000000 0.000000 10.50000 0.01926 0.02029 = 0.03118 -0.00429 0.00039 -0.00873 F1 5 0.358130 0.269119 0.125418 11.00000 0.03175 0.03095 = 0.04871 -0.01821 0.00610 -0.01346 F2 5 0.323433 -0.120561 0.122590 11.00000 0.04123 0.03862 = 0.05045 -0.00371 0.01216 -0.02511 F3 5 0.252567 0.142398 -0.124587 11.00000 0.04053 0.03498 = 0.05928 0.00335 -0.02449 -0.01433 HKLF 4 REM EL13_D207_DRX14_C4SI in P-1 REM R1 = 0.0383 for 1185 Fo > 4sig(Fo) and 0.0558 for all 1285 data REM 61 parameters refined using 0 restraints END WGHT 0.0549 0.1270 REM Highest difference peak 0.735, deepest hole -0.326, 1-sigma level 0.062 Q1 1 -0.4325 0.3578 0.4834 11.00000 0.05 0.73 Q2 1 -0.1806 0.4128 0.3617 11.00000 0.05 0.41 Q3 1 0.3745 0.1013 -0.1809 11.00000 0.05 0.39 Q4 1 0.4210 0.1671 0.1845 11.00000 0.05 0.30 Q5 1 0.2310 -0.0267 0.0624 11.00000 0.05 0.24 Q6 1 0.3531 -0.0866 0.1927 11.00000 0.05 0.24 Q7 1 0.2292 0.0533 -0.0801 11.00000 0.05 0.23 Q8 1 0.2130 0.2440 -0.0882 11.00000 0.05 0.21 Q9 1 0.3020 0.2639 0.0852 11.00000 0.05 0.21 Q10 1 0.4173 -0.2010 0.0823 11.00000 0.05 0.20 ; _cod_data_source_file im2447sup1.cf _cod_data_source_block I _cod_original_sg_symbol_Hall '-p 1' _cod_original_sg_symbol_H-M 'p -1' _cod_database_code 2239081 _cod_database_fobs_code 2239081 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_symmetry_multiplicity C C1 -0.1629(3) 0.2744(4) 0.3650(2) 0.0394(4) Uani d . 1 1 H H1A 0.0138 0.2407 0.3801 0.047 Uiso calc R 1 1 H H1B -0.1739 0.1160 0.3876 0.047 Uiso calc R 1 1 C C2 -0.3593(4) 0.4783(4) 0.4953(2) 0.0435(4) Uani d . 1 1 H H2A -0.3573 0.6396 0.4663 0.052 Uiso calc R 1 1 H H2B -0.3024 0.4297 0.6094 0.052 Uiso calc R 1 1 N N1 -0.2086(2) 0.3508(2) 0.18267(15) 0.0269(3) Uani d . 1 1 H H1NA -0.0891 0.2252 0.1110 0.040 Uiso calc R 1 1 H H1NB -0.1946 0.4939 0.1603 0.040 Uiso calc R 1 1 H H1NC -0.3695 0.3792 0.1675 0.040 Uiso calc R 1 1 Si Si1 0.5000 0.0000 0.0000 0.02400(16) Uani d S 1 2 F F1 0.35813(19) 0.26912(18) 0.12542(14) 0.0381(3) Uani d . 1 1 F F2 0.3234(2) -0.1206(2) 0.12259(14) 0.0426(3) Uani d . 1 1 F F3 0.2526(2) 0.1424(2) -0.12459(15) 0.0445(3) Uani d . 1 1 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 C1 0.0304(7) 0.0470(9) 0.0266(7) -0.0069(7) -0.0029(5) 0.0022(6) C2 0.0368(9) 0.0649(12) 0.0278(7) -0.0233(8) 0.0014(6) -0.0109(7) N1 0.0262(6) 0.0287(6) 0.0236(5) -0.0117(5) 0.0007(4) -0.0032(4) Si1 0.0193(3) 0.0203(3) 0.0312(3) -0.00873(19) 0.00039(18) -0.00429(18) F1 0.0318(5) 0.0310(5) 0.0487(6) -0.0135(4) 0.0061(4) -0.0182(4) F2 0.0412(6) 0.0386(5) 0.0505(6) -0.0251(5) 0.0122(4) -0.0037(4) F3 0.0405(6) 0.0350(5) 0.0593(7) -0.0143(4) -0.0245(5) 0.0034(5) 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' Si Si 0.0817 0.0704 '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' F F 0.0171 0.0103 '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_1 _geom_angle_site_symmetry_3 _geom_angle N1 C1 C2 . . 112.70(13) N1 C1 H1A . . 109.1 C2 C1 H1A . . 109.1 N1 C1 H1B . . 109.1 C2 C1 H1B . . 109.1 H1A C1 H1B . . 107.8 C1 C2 C2 . 2_466 114.65(19) C1 C2 H2A . . 108.6 C2 C2 H2A 2_466 . 108.6 C1 C2 H2B . . 108.6 C2 C2 H2B 2_466 . 108.6 H2A C2 H2B . . 107.6 C1 N1 H1NA . . 109.5 C1 N1 H1NB . . 109.5 H1NA N1 H1NB . . 109.5 C1 N1 H1NC . . 109.5 H1NA N1 H1NC . . 109.5 H1NB N1 H1NC . . 109.5 F2 Si1 F2 2_655 . 180.0 F2 Si1 F1 2_655 . 89.09(5) F2 Si1 F1 . . 90.91(5) F2 Si1 F1 2_655 2_655 90.91(5) F2 Si1 F1 . 2_655 89.09(5) F1 Si1 F1 . 2_655 180.0 F2 Si1 F3 2_655 . 91.03(6) F2 Si1 F3 . . 88.98(6) F1 Si1 F3 . . 89.04(6) F1 Si1 F3 2_655 . 90.96(6) F2 Si1 F3 2_655 2_655 88.97(6) F2 Si1 F3 . 2_655 91.02(6) F1 Si1 F3 . 2_655 90.96(6) F1 Si1 F3 2_655 2_655 89.04(6) F3 Si1 F3 . 2_655 180.0 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance C1 N1 . 1.4853(19) C1 C2 . 1.512(2) C1 H1A . 0.9700 C1 H1B . 0.9700 C2 C2 2_466 1.519(4) C2 H2A . 0.9700 C2 H2B . 0.9700 N1 H1NA . 0.8900 N1 H1NB . 0.8900 N1 H1NC . 0.8900 Si1 F2 2_655 1.6757(10) Si1 F2 . 1.6757(10) Si1 F1 . 1.6886(9) Si1 F1 2_655 1.6886(9) Si1 F3 . 1.6908(10) Si1 F3 2_655 1.6908(10) loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA N1 H1NA F2 . 0.89 2.31 3.017(2) 136.7 N1 H1NA F3 . 0.89 2.39 3.134(2) 141.5 N1 H1NB F3 2_565 0.89 2.02 2.890(2) 167.0 N1 H1NC F1 1_455 0.89 2.04 2.864(2) 154.1