#------------------------------------------------------------------------------ #$Date: 2016-02-14 14:26:36 +0000 (Sun, 14 Feb 2016) $ #$Revision: 176435 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/14/2011452.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_2011452 loop_ _publ_author_name 'Willett, Roger D.' 'Haddad, Salim F.' _publ_section_title ; Bis[4-(dimethylamino)pyridinium] hexachlorostannate(IV) ; _journal_issue 10 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first e438 _journal_page_last e438 _journal_paper_doi 10.1107/S0108270100012129 _journal_volume 56 _journal_year 2000 _chemical_formula_iupac '(C7 H11 N2)2 [Sn1 Cl6]' _chemical_formula_moiety '2C7 H11 N2 1+, Sn1 Cl6 2-' _chemical_formula_sum 'C14 H22 Cl6 N4 Sn' _chemical_formula_weight 577.74 _chemical_name_common (4-DMAP)2[SnCl6] _chemical_name_systematic ; 4-Dimethylaminopyridinium hexachlorostanate ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _cell_angle_alpha 90.00 _cell_angle_beta 106.92(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 8.3328(17) _cell_length_b 11.680(2) _cell_length_c 11.724(2) _cell_measurement_reflns_used 4787 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 28.19 _cell_measurement_theta_min 1.98 _cell_volume 1091.7(4) _computing_cell_refinement 'SAINT (Bruker, 1996)' _computing_data_collection 'SMART (Bruker, 1996)' _computing_data_reduction SAINT _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full .995 _diffrn_measured_fraction_theta_max .995 _diffrn_measurement_device_type 'Siemens SMART 1000' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .035 _diffrn_reflns_av_sigmaI/netI .0281 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 5296 _diffrn_reflns_theta_full 24.71 _diffrn_reflns_theta_max 24.71 _diffrn_reflns_theta_min 2.52 _diffrn_standards_decay_% 2.4 _diffrn_standards_interval_time 'beginning and end' _diffrn_standards_number '50 frames' _exptl_absorpt_coefficient_mu 1.911 _exptl_absorpt_correction_T_max .751 _exptl_absorpt_correction_T_min .528 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Bruker, 1996)' _exptl_crystal_colour Colourless _exptl_crystal_density_diffrn 1.758 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Parallelepiped _exptl_crystal_F_000 572 _exptl_crystal_size_max .4 _exptl_crystal_size_mid .2 _exptl_crystal_size_min .15 _refine_diff_density_max .317 _refine_diff_density_min -.341 _refine_ls_extinction_coef .0036(6) _refine_ls_extinction_method SHELXL97 _refine_ls_goodness_of_fit_ref 1.186 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 162 _refine_ls_number_reflns 1854 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.186 _refine_ls_R_factor_all .032 _refine_ls_R_factor_gt .025 _refine_ls_shift/su_max .001 _refine_ls_shift/su_mean <0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0309P)^2^+0.2141P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .065 _reflns_number_gt 1629 _reflns_number_total 1854 _reflns_threshold_expression I>2\s(I) _cod_data_source_file qa0379.cif _cod_data_source_block I _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' 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 'Monoclinic' changed to 'monoclinic' 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 ; _cod_original_sg_symbol_H-M 'P 21/c' _cod_original_formula_sum 'C14 H22 Cl6 N4 Sn1' _cod_database_code 2011452 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y+1/2, z+1/2' loop_ _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_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Sn .5000 .5000 .0000 .03134(14) Uani d SP .989(2) . . Sn Cl1 .50471(12) .63254(7) .16141(7) .0573(3) Uani d . 1 . . Cl Cl2 .58090(12) .34573(7) .14365(7) .0564(3) Uani d . 1 . . Cl Cl3 .79094(11) .54174(10) .02168(9) .0663(3) Uani d . 1 . . Cl N1 .9065(3) .3422(2) .5524(2) .0489(7) Uani d . 1 . . N C1 .8195(4) .4351(3) .5633(2) .0391(7) Uani d . 1 . . C N2 .6484(4) .6321(3) .5846(4) .0643(9) Uani d . 1 . . N C2 .8081(5) .4737(3) .6747(3) .0528(9) Uani d . 1 . . C C4 .6528(5) .5979(3) .4765(4) .0578(9) Uani d . 1 . . C C5 .7331(4) .5015(3) .4624(3) .0461(8) Uani d . 1 . . C C3 .7220(5) .5714(4) .6811(4) .0623(11) Uani d . 1 . . C C6 .9064(6) .2969(4) .4362(4) .0626(11) Uani d . 1 . . C C7 1.0031(7) .2747(5) .6545(5) .0742(13) Uani d . 1 . . C H6A .945(7) .351(5) .397(5) .13(2) Uiso d . 1 . . H H4 .593(4) .645(3) .417(3) .056(10) Uiso d . 1 . . H H2 .870(5) .432(3) .737(3) .066(12) Uiso d . 1 . . H H7B 1.045(6) .331(5) .712(4) .11(2) Uiso d . 1 . . H H7A .924(6) .244(4) .686(4) .094(16) Uiso d . 1 . . H H5 .731(4) .483(3) .388(4) .050(10) Uiso d . 1 . . H H6C .803(6) .272(4) .387(4) .081(13) Uiso d . 1 . . H H3 .709(5) .590(4) .756(4) .088(13) Uiso d . 1 . . H H2' .594(5) .691(3) .589(3) .068(12) Uiso d . 1 . . H H6B .974(7) .242(5) .453(5) .12(2) Uiso d . 1 . . H H7C 1.098(7) .249(5) .634(5) .13(2) Uiso d . 1 . . H 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 Sn .0338(2) .03110(19) .02929(18) -.00423(11) .00937(12) .00026(10) Cl1 .0886(7) .0444(5) .0451(5) -.0089(4) .0290(4) -.0106(4) Cl2 .0752(6) .0434(5) .0438(5) -.0007(4) .0063(4) .0124(4) Cl3 .0401(5) .0851(7) .0745(6) -.0151(5) .0178(4) .0008(5) N1 .0483(16) .0497(17) .0455(15) .0081(13) .0084(12) .0054(12) C1 .0375(16) .0409(18) .0381(16) -.0046(13) .0098(13) .0011(13) N2 .055(2) .0481(19) .094(3) -.0010(15) .0294(18) -.0173(19) C2 .054(2) .061(2) .045(2) -.0087(18) .0160(17) -.0010(17) C4 .051(2) .050(2) .067(2) .0057(17) .0093(18) .0063(19) C5 .048(2) .049(2) .0391(18) .0004(15) .0090(14) .0025(15) C3 .061(2) .074(3) .059(2) -.021(2) .028(2) -.025(2) C6 .063(3) .060(3) .062(2) .007(2) .013(2) -.013(2) C7 .072(3) .074(3) .071(3) .018(2) .013(3) .027(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl .1484 .1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -.6537 1.4246 '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 Cl3 Sn Cl3 3_665 . 180.00(5) Cl3 Sn Cl2 3_665 . 89.47(4) Cl3 Sn Cl2 . . 90.53(4) Cl3 Sn Cl2 3_665 3_665 90.53(4) Cl3 Sn Cl2 . 3_665 89.47(4) Cl2 Sn Cl2 . 3_665 180.00(3) Cl3 Sn Cl1 3_665 3_665 90.07(4) Cl3 Sn Cl1 . 3_665 89.93(4) Cl2 Sn Cl1 . 3_665 90.33(3) Cl2 Sn Cl1 3_665 3_665 89.67(3) Cl3 Sn Cl1 3_665 . 89.93(4) Cl3 Sn Cl1 . . 90.07(4) Cl2 Sn Cl1 . . 89.67(3) Cl2 Sn Cl1 3_665 . 90.33(3) Cl1 Sn Cl1 3_665 . 180.00(2) C1 N1 C6 . . 122.2(3) C1 N1 C7 . . 123.1(3) C6 N1 C7 . . 114.7(4) N1 C1 C2 . . 122.3(3) N1 C1 C5 . . 121.5(3) C2 C1 C5 . . 116.2(3) C3 N2 C4 . . 121.0(4) C3 C2 C1 . . 119.8(4) N2 C4 C5 . . 121.2(4) C4 C5 C1 . . 120.3(3) N2 C3 C2 . . 121.4(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Sn Cl3 3_665 2.4127(10) ? Sn Cl3 . 2.4127(10) ? Sn Cl2 . 2.4242(9) ? Sn Cl2 3_665 2.4242(9) ? Sn Cl1 3_665 2.4364(8) ? Sn Cl1 . 2.4364(8) ? N1 C1 . 1.331(4) ? N1 C6 . 1.461(5) ? N1 C7 . 1.464(5) ? C1 C2 . 1.411(4) ? C1 C5 . 1.423(4) ? N2 C3 . 1.325(5) ? N2 C4 . 1.340(5) ? C2 C3 . 1.362(6) ? C4 C5 . 1.344(5) ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion C6 N1 C1 C2 174.7(4) C7 N1 C1 C2 -2.5(5) C6 N1 C1 C5 -5.6(5) C7 N1 C1 C5 177.2(4) N1 C1 C2 C3 177.9(3) C5 C1 C2 C3 -1.8(5) C3 N2 C4 C5 -.6(6) N2 C4 C5 C1 -1.8(5) N1 C1 C5 C4 -176.8(3) C2 C1 C5 C4 2.9(5) C4 N2 C3 C2 1.6(6) C1 C2 C3 N2 -.3(6)