#------------------------------------------------------------------------------ #$Date: 2017-01-19 16:22:45 +0000 (Thu, 19 Jan 2017) $ #$Revision: 190732 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/73/2007316.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_2007316 loop_ _publ_author_name 'Hazell, Alan' 'Khoo, Lian Ee' 'Ouyang, Jiexiang' 'Rausch, Bernhard J.' 'Tavares, Zara Miravent' _publ_section_title ; 8-Methylaminoquinolinium Salts of Tetrachlorodimethylstannate(IV) and Tetrachlorodiphenylstannate(IV) ; _journal_issue 6 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 728 _journal_page_last 732 _journal_paper_doi 10.1107/S0108270198000626 _journal_volume 54 _journal_year 1998 _chemical_formula_iupac '(C10 H11 N2)2 [Sn Cl4 (C H3)2]' _chemical_formula_moiety '(C10 H11 N2)2 [Sn Cl4 (C H3)2]' _chemical_formula_sum 'C22 H28 Cl4 N4 Sn' _chemical_formula_weight 608.992 _chemical_melting_point 425(2) _chemical_name_systematic ; bis(8-methylaminoquinolinium) dimethyltetrachlorostannate(IV) ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_type_scat_source IntTabIV _cell_angle_alpha 90 _cell_angle_beta 92.0760(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.1020(4) _cell_length_b 12.7094(6) _cell_length_c 28.213(2) _cell_measurement_reflns_used 6627 _cell_measurement_temperature 296 _cell_measurement_theta_max 29.4 _cell_measurement_theta_min 1.4 _cell_volume 2544.9(3) _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_collection 'SMART (Siemens, 1995)' _computing_data_reduction 'SAINT and XPREP (Siemens, 1995)' _computing_molecular_graphics 'ORTEPIII (Burnett & Johnson, 1996) in KRYSTAL' _computing_publication_material KRYSTAL _computing_structure_refinement 'modified ORFLS (Busing et al., 1962) in KRYSTAL' _computing_structure_solution 'SIR92 (Altomare et al., 1994) in KRYSTAL (Hazell, 1995)' _diffrn_ambient_temperature 296 _diffrn_measurement_device 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames ' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'x-ray tube' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.038 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 12315 _diffrn_reflns_reduction_process 12315 _diffrn_reflns_theta_max 29.4 _diffrn_reflns_theta_min 1.4 _exptl_absorpt_coefficient_mu 1.441 _exptl_absorpt_correction_T_max 0.779 _exptl_absorpt_correction_T_min 0.501 _exptl_absorpt_correction_type 'numerical (XPREP; Siemens, 1995)' _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.589 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 1224 _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.16 _refine_diff_density_max 0.45 _refine_diff_density_min -0.58 _refine_ls_extinction_coef 63(12) _refine_ls_extinction_method 'B-C type 1, Lorentzian isotropic (Becker & Coppens, 1974)' _refine_ls_goodness_of_fit_obs 1.324 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_constraints 0 _refine_ls_number_parameters 393 _refine_ls_number_reflns 4583 _refine_ls_number_restraints 0 _refine_ls_R_factor_obs .034 _refine_ls_shift/esd_max 0.005 _refine_ls_shift/esd_mean 0.0006 _refine_ls_structure_factor_coef F _refine_ls_weighting_details 'w = 1/{[\s~cs~(F^2^)+1.03F^2^]^1/2^-|F|}^2^' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_obs .048 _reflns_number_observed 4583 _reflns_number_total 6333 _reflns_observed_criterion I>3\s(I) _cod_data_source_file cf1224.cif _cod_data_source_block ear1 _cod_depositor_comments ; Adding the _atom_site_type_symbol data item. Antanas Vaitkus, 2017-01-19 The following automatic conversions were performed: '_chemical_melting_point' value '423-427 K' was changed to '425(2)' - the average value was taken and precision was estimated. '_atom_site_thermal_displace_type' tag value 'Uij' was replaced with 'Uani' value 31 time. Automatic conversion script Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana The following automatic conversions were performed: '_chemical_melting_point' value '423-427 K' was changed to '425(2)' - the average value was taken and precision was estimated. 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 The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'w = 1/{[\s~cs~(F^2^)+1.03F^2^]^1/2^-|F|}^2^' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w = 1/{[\s~cs~(F^2^)+1.03F^2^]^1/2^-|F|}^2^'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_cell_volume 2544.9(2) _cod_original_sg_symbol_H-M 'P 21/n' _cod_original_formula_sum 'C22 H28 N4 Cl4 Sn' _cod_database_code 2007316 _cod_database_fobs_code 2007316 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2+x,1/2-y,1/2+z -x,-y,-z 1/2-x,1/2+y,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 Sn .0539(2) .0354(2) .03960(10) -.00330(10) -.00350(10) .00050(10) Cl1 .0987(8) .0449(6) .0601(6) .0028(5) .0291(6) -.0039(4) Cl2 .0916(8) .0433(5) .0454(5) -.0033(5) -.0033(5) .0097(4) Cl3 .0855(7) .0360(5) .0484(5) .0038(5) .0068(4) .0005(4) Cl4 .0794(7) .0484(6) .0513(5) .0008(5) -.0005(5) .0021(4) N1 .043(2) .032(2) .045(2) -.0010(10) .0030(10) -.0010(10) N2 .065(2) .050(2) .046(2) .012(2) -.0060(10) -.0070(10) C1 .043(2) .047(2) .048(2) .000(2) .0010(10) .003(2) C2 .049(2) .054(2) .046(2) -.004(2) .005(2) -.003(2) C3 .047(2) .048(2) .057(2) -.007(2) .012(2) -.014(2) C4 .037(2) .033(2) .057(2) -.0030(10) .0090(10) -.0020(10) C5 .055(2) .037(2) .074(3) .000(2) .013(2) -.002(2) C6 .060(2) .041(2) .073(3) .007(2) .007(2) .017(2) C7 .045(2) .058(3) .053(2) .006(2) .002(2) .015(2) C8 .037(2) .043(2) .048(2) .0000(10) .0030(10) .002(2) C9 .033(2) .035(2) .045(2) .0020(10) .0060(10) .0040(10) C10 .084(3) .075(4) .052(2) .013(3) -.009(2) -.010(2) N3 .043(2) .045(2) .0380(10) .0060(10) .0010(10) .0030(10) N4 .073(2) .072(3) .044(2) .020(2) -.008(2) -.009(2) C11 .048(2) .058(2) .039(2) .003(2) .0000(10) .002(2) C12 .052(2) .063(3) .051(2) -.001(2) .004(2) -.008(2) C13 .046(2) .049(2) .075(3) -.001(2) .012(2) -.006(2) C14 .036(2) .047(2) .062(2) .0020(10) .012(2) .009(2) C15 .048(2) .052(3) .084(3) .006(2) .010(2) .020(2) C16 .043(2) .082(4) .082(3) .013(2) .009(2) .040(3) C17 .041(2) .097(4) .046(2) .009(2) .002(2) .019(2) C18 .036(2) .070(3) .042(2) .008(2) .0040(10) .008(2) C19 .032(2) .051(2) .041(2) .0020(10) .0050(10) .0070(10) C20 .102(5) .125(6) .055(3) .031(4) -.021(3) -.029(3) C21 .056(2) .048(3) .065(3) -.002(2) -.011(2) .002(2) C22 .060(3) .069(3) .061(3) -.013(2) -.006(2) -.008(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_thermal_displace_type Sn Sn .11200(4) .23333(2) .352460(10) .0431(2) Uani Cl1 Cl .27758(18) .10995(8) .30231(4) .0673(7) Uani Cl2 Cl .12579(17) .37799(8) .29468(3) .0602(6) Uani Cl3 Cl .09557(16) .06545(8) .42151(3) .0565(6) Uani Cl4 Cl -.10353(16) .38357(8) .41784(3) .0598(6) Uani N1 N .1929(4) -.1469(2) .37220(10) .040(2) Uani N2 N .3245(5) -.1357(3) .46780(10) .054(2) Uani C1 C .1333(5) -.1471(3) .32720(10) .046(2) Uani C2 C .1238(6) -.2404(3) .30210(10) .049(2) Uani C3 C .1771(5) -.3313(3) .32390(10) .050(2) Uani C4 C .2414(5) -.3327(3) .37160(10) .042(2) Uani C5 C .2974(6) -.4250(3) .3955(2) .055(2) Uani C6 C .3574(6) -.4200(3) .4415(2) .058(2) Uani C7 C .3664(5) -.3250(3) .46630(10) .052(2) Uani C8 C .3130(5) -.2302(3) .44480(10) .042(2) Uani C9 C .2503(4) -.2356(3) .39630(10) .038(2) Uani C10 C .3742(9) -.1280(5) .5178(2) .070(3) Uani N3 N -.1705(4) .6214(3) .42220(10) .042(2) Uani N4 N -.2837(6) .5481(3) .33120(10) .063(2) Uani C11 C -.1170(5) .6516(3) .46540(10) .048(2) Uani C12 C -.1256(6) .7551(3) .4784(2) .055(2) Uani C13 C -.1915(5) .8276(4) .4462(2) .056(2) Uani C14 C -.2518(5) .7975(3) .40020(10) .048(2) Uani C15 C -.3215(6) .8703(4) .3658(2) .061(3) Uani C16 C -.3779(6) .8340(4) .3225(2) .069(3) Uani C17 C -.3657(6) .7272(4) .31000(10) .061(3) Uani C18 C -.2957(5) .6509(3) .34190(10) .049(2) Uani C19 C -.2391(4) .6894(3) .38800(10) .041(2) Uani C20 C -.3385(11) .5055(7) .2850(2) .095(5) Uani C21 C .3425(7) .2827(4) .3958(2) .057(3) Uani C22 C -.1679(7) .1867(5) .3375(2) .063(3) Uani HN1 H .184(5) -.088(3) .3850(10) .051(11) Uiso HN2 H .262(6) -.089(4) .4580(10) .057(13) Uiso HN3 H -.166(5) .544(3) .4160(10) .049(10) Uiso HN4 H -.233(7) .505(4) .348(2) .082(17) Uiso H1 H .086(5) -.084(3) .3120(10) .051(11) Uiso H2 H .081(7) -.239(3) .271(2) .060(13) Uiso H3 H .170(5) -.395(3) .3070(10) .036(9) Uiso H5 H .297(6) -.482(4) .3790(10) .067(14) Uiso H6 H .407(7) -.477(4) .456(2) .088(17) Uiso H7 H .395(5) -.328(3) .4970(10) .046(10) Uiso H11 H -.066(4) .594(3) .4870(10) .033(8) Uiso H12 H -.084(8) .774(4) .507(2) .082(16) Uiso H13 H -.191(7) .904(5) .453(2) .097(17) Uiso H15 H -.322(7) .945(4) .372(2) .084(16) Uiso H16 H -.422(6) .889(4) .298(2) .075(14) Uiso H17 H -.417(6) .696(4) .279(2) .068(12) Uiso H10a H .390(7) -.051(4) .527(2) .089(16) Uiso H10b H .514(11) -.152(6) .525(2) .14(3) Uiso H10c H .294(8) -.169(5) .536(2) .11(2) Uiso H20a H -.333(11) .428(6) .289(2) .14(3) Uiso H20b H -.244(7) .536(4) .263(2) .080(16) Uiso H20c H -.467(9) .525(5) .275(2) .102(19) Uiso H21a H .419(8) .224(4) .399(2) .083(17) Uiso H21b H .288(8) .308(5) .420(2) .091(18) Uiso H21c H .423(8) .321(4) .377(2) .091(17) Uiso H22a H -.247(12) .197(6) .363(3) .16(3) Uiso H22b H -.182(10) .123(6) .335(2) .13(3) Uiso H22c H -.209(8) .216(4) .308(2) .087(17) Uiso loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag C21 Sn C22 155.7(2) yes Cl1 Sn C22 100.0(2) yes Cl2 Sn C22 97.9(2) yes Cl3 Sn C22 82.3(2) yes Cl4 Sn C22 79.0(2) yes Cl1 Sn C21 98.5(2) yes Cl2 Sn C21 96.50(10) yes Cl3 Sn C21 83.00(10) yes Cl4 Sn C21 82.0(2) yes Cl1 Sn Cl2 93.70(4) yes Cl1 Sn Cl3 87.05(3) yes Cl1 Sn Cl4 178.10(5) yes Cl2 Sn Cl3 179.16(9) yes Cl2 Sn Cl4 88.07(3) yes Cl3 Sn Cl4 91.19(3) yes C1 N1 C9 123.6(3) no C8 N2 C10 122.0(4) no N1 C1 C2 120.1(4) no C1 C2 C3 119.3(4) no C2 C3 C4 121.4(4) no C3 C4 C5 123.2(4) no C5 C4 C9 119.0(4) no C3 C4 C9 117.9(3) no C4 C5 C6 119.7(4) no C5 C6 C7 121.9(4) no C6 C7 C8 121.5(4) no N2 C8 C7 122.9(4) no N2 C8 C9 120.6(3) no C7 C8 C9 116.4(3) no N1 C9 C4 117.6(3) no N1 C9 C8 120.9(3) no C4 C9 C8 121.4(3) no C11 N3 C19 123.3(3) no C18 N4 C20 123.2(5) no N3 C11 C12 120.8(4) no C11 C12 C13 119.3(4) no C12 C13 C14 121.1(4) no C13 C14 C15 122.8(4) no C13 C14 C19 117.9(3) no C15 C14 C19 119.3(4) no C14 C15 C16 118.7(5) no C15 C16 C17 122.4(4) no C16 C17 C18 122.1(4) no N4 C18 C17 123.5(4) no N4 C18 C19 121.1(3) no C17 C18 C19 115.3(4) no N3 C19 C14 117.5(3) no N3 C19 C18 120.3(3) no C14 C19 C18 122.1(3) no Sn C21 H21a 105(3) no Sn C21 H21b 102(4) no Sn C21 H21c 107(3) no Sn C22 H22a 113(5) no Sn C22 H22b 114(5) no Sn C22 H22c 109(4) no C1 N1 HN1 113(3) no C9 N1 HN1 123(3) no C8 N2 HN2 119(3) no C10 N2 HN2 113(3) no N1 C1 H1 122(2) no C2 C1 H1 118(2) no C3 C2 H2 122(3) no C1 C2 H2 119(3) no C2 C3 H3 120(2) no C4 C3 H3 119(2) no C6 C5 H5 124(3) no C4 C5 H5 116(3) no C5 C6 H6 121(3) no C7 C6 H6 117(3) no C8 C7 H7 121(3) no C6 C7 H7 118(3) no H10a C10 H10c 118(5) no H10b C10 H10c 110(5) no N2 C10 H10c 111(4) no H10a C10 H10b 97(5) no N2 C10 H10a 110(3) no N2 C10 H10b 111(4) no C11 N3 HN3 116(2) no C19 N3 HN3 121(2) no C18 N4 HN4 125(4) no C20 N4 HN4 112(4) no N3 C11 H11 115(2) no C12 C11 H11 124(2) no C13 C12 H12 121(3) no C11 C12 H12 119(3) no C12 C13 H13 122(3) no C14 C13 H13 117(3) no C16 C15 H15 119(3) no C14 C15 H15 122(3) no C15 C16 H16 117(3) no C17 C16 H16 121(3) no C18 C17 H17 113(3) no C16 C17 H17 125(3) no H20a C20 H20c 108(5) no H20b C20 H20c 110(4) no N4 C20 H20c 113(3) no H20a C20 H20b 115(5) no N4 C20 H20a 105(4) no N4 C20 H20b 105(3) no H21a C21 H21b 121(5) no H21b C21 H21c 124(5) no H21a C21 H21c 95(5) no H22b C22 H22c 106(5) no H22a C22 H22b 98(6) no H22a C22 H22c 116(6) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Sn C21 . . 2.103(4) yes Sn C22 . . 2.102(5) yes Sn Cl1 . . 2.4420(10) yes Sn Cl2 . . 2.4610(10) yes Sn Cl3 . . 2.8940(10) yes Sn Cl4 . . 3.0980(10) yes N1 C1 . . 1.322(5) no N1 C9 . . 1.372(4) no N2 C8 . . 1.366(5) no N2 C10 . . 1.446(5) no C1 C2 . . 1.382(6) no C2 C3 . . 1.356(6) no C3 C4 . . 1.406(5) no C4 C5 . . 1.405(5) no C4 C9 . . 1.417(5) no C5 C6 . . 1.351(6) no C6 C7 . . 1.396(6) no C7 C8 . . 1.395(5) no C8 C9 . . 1.425(5) no N3 C11 . . 1.322(4) no N3 C19 . . 1.372(4) no N4 C18 . . 1.344(6) no N4 C20 . . 1.452(6) no C11 C12 . . 1.367(6) no C12 C13 . . 1.365(6) no C13 C14 . . 1.405(6) no C14 C15 . . 1.416(6) no C14 C19 . . 1.421(6) no C15 C16 . . 1.355(7) no C16 C17 . . 1.406(7) no C17 C18 . . 1.401(6) no C18 C19 . . 1.433(5) no N1 HN1 . . .83(4) no N2 HN2 . . .78(4) no C1 H1 . . .96(4) no C2 H2 . . .90(5) no C3 H3 . . .95(4) no C5 H5 . . .86(4) no C6 H6 . . .90(5) no C7 H7 . . .88(4) no C10 H10c . . .93(6) no C10 H10a . . 1.01(5) no C10 H10b . . 1.05(8) no N3 HN3 . . 1.00(4) no N4 HN4 . . .79(5) no C11 H11 . . 1.01(3) no C12 H12 . . .88(5) no C13 H13 . . .99(6) no C15 H15 . . .96(5) no C16 H16 . . 1.03(5) no C17 H17 . . 1.01(4) no C20 H20c . . .98(6) no C20 H20a . . .99(7) no C20 H20b . . 1.02(5) no C21 H21b . . .86(5) no C21 H21a . . .92(5) no C21 H21c . . .93(6) no C22 H22b . . .82(7) no C22 H22c . . .93(6) no C22 H22a . . .94(9) no