#------------------------------------------------------------------------------ #$Date: 2016-02-19 22:18:51 +0000 (Fri, 19 Feb 2016) $ #$Revision: 176760 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/14/2011474.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_2011474 loop_ _publ_author_name 'K\"onig, Uwe-Christoph' 'Berkei, Michael' 'Hirsch, Claudia' 'Preut, Hans' 'Mitchell, Terence Nigel' _publ_section_title Chlorodimethyl(N-methylpyrrolidinone)tin(IV)-\m-chloro-dichlorodimethyltin(IV) _journal_issue 10 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first e450 _journal_page_last e451 _journal_paper_doi 10.1107/S0108270100011963 _journal_volume 56 _journal_year 2000 _chemical_formula_iupac '[Sn2 Cl4 (C H3)4 (C5 H9 N O)]' _chemical_formula_moiety 'C9 H21 Cl4 N O Sn2' _chemical_formula_sum 'C9 H21 Cl4 N O Sn2' _chemical_formula_weight 538.45 _chemical_name_systematic ; ? ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _audit_creation_method SHELXL-97 _cell_angle_alpha 78.45(3) _cell_angle_beta 84.36(3) _cell_angle_gamma 84.38(3) _cell_formula_units_Z 2 _cell_length_a 7.3650(15) _cell_length_b 10.311(2) _cell_length_c 12.311(3) _cell_measurement_reflns_used 5442 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 27.06 _cell_measurement_theta_min 2.38 _cell_volume 908.6(4) _computing_cell_refinement 'DENZO and SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_data_reduction 'DENZO and SCALEPACK' _computing_publication_material 'SHELXL97 and PARST95 (Nardelli, 1995)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _diffrn_ambient_temperature 173(2) _diffrn_detector_area_resol_mean '10 vertical, 18 horizontal' _diffrn_measured_fraction_theta_full .937 _diffrn_measured_fraction_theta_max .889 _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method ; 278 frames via \w-rotation (\D\w = 1\%) at different \k values and two times 25 s per frame ; _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .046 _diffrn_reflns_av_sigmaI/netI .0933 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 5442 _diffrn_reflns_theta_full 25.0 _diffrn_reflns_theta_max 27.06 _diffrn_reflns_theta_min 2.38 _diffrn_standards_decay_% 0 _exptl_absorpt_coefficient_mu 3.324 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.968 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description parallelepiped _exptl_crystal_F_000 516 _exptl_crystal_size_max .1 _exptl_crystal_size_mid .08 _exptl_crystal_size_min .08 _refine_diff_density_max .760 _refine_diff_density_min -.854 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref .804 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 159 _refine_ls_number_reflns 3557 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all .804 _refine_ls_R_factor_all .057 _refine_ls_R_factor_gt .030 _refine_ls_shift/su_max .012 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .063 _reflns_number_gt 2466 _reflns_number_total 3557 _reflns_threshold_expression I>2\s(I) _cod_data_source_file qd0036.cif _cod_data_source_block I _cod_depositor_comments ; 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 'calc w = 1/[\s^2^(Fo^2^)] where P = (Fo^2^+2Fc^2^)/3' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w = 1/[\s^2^(Fo^2^)] where P = (Fo^2^+2Fc^2^)/3'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_cell_volume 908.6(3) _cod_database_code 2011474 _cod_database_fobs_code 2011474 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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 Sn2 .15732(4) .68299(3) .01703(2) .02798(11) Uani d . 1 . . Sn Sn1 .26442(3) .58316(3) -.38866(2) .02607(11) Uani d . 1 . . Sn Cl1 .32671(13) .60116(11) -.58757(9) .0339(3) Uani d . 1 . . Cl Cl4 .18459(14) .53686(12) -.13112(9) .0383(3) Uani d . 1 . . Cl Cl2 -.01390(14) .71989(12) -.39842(10) .0407(3) Uani d . 1 . . Cl Cl3 .39646(14) .81139(12) -.07790(10) .0429(3) Uani d . 1 . . Cl O1 .1197(3) .8157(3) .1463(2) .0332(8) Uani d . 1 . . O C2 .1886(5) .3871(4) -.3464(3) .0308(11) Uani d . 1 . . C H2A .2533 .3399 -.2845 .037 Uiso calc R 1 . . H H2B .2187 .3441 -.4088 .037 Uiso calc R 1 . . H H2C .0593 .3879 -.3264 .037 Uiso calc R 1 . . H C3 .2802(5) .5299(4) .1326(3) .0345(12) Uani d . 1 . . C H3A .2443 .5445 .2066 .041 Uiso calc R 1 . . H H3B .4109 .5290 .1193 .041 Uiso calc R 1 . . H H3C .2416 .4462 .1248 .041 Uiso calc R 1 . . H C1 .4562(5) .7078(4) -.3577(3) .0337(11) Uani d . 1 . . C H1A .4364 .7194 -.2819 .040 Uiso calc R 1 . . H H1B .4415 .7926 -.4065 .040 Uiso calc R 1 . . H H1C .5778 .6682 -.3707 .040 Uiso calc R 1 . . H N1 .1412(4) .9352(3) .2788(3) .0284(9) Uani d . 1 . . N C5 .2134(6) .8677(4) .2037(4) .0285(11) Uani d . 1 . . C C6 .4188(5) .8692(4) .1933(4) .0328(11) Uani d . 1 . . C H6A .4606 .9252 .1241 .039 Uiso calc R 1 . . H H6B .4774 .7803 .1964 .039 Uiso calc R 1 . . H C7 -.0538(5) .9594(5) .3041(4) .0429(13) Uani d . 1 . . C H7A -.1187 .9163 .2593 .051 Uiso calc R 1 . . H H7B -.0873 1.0532 .2883 .051 Uiso calc R 1 . . H H7C -.0847 .9248 .3813 .051 Uiso calc R 1 . . H C4 -.0891(5) .7858(5) -.0360(4) .0474(14) Uani d . 1 . . C H4A -.1896 .7522 .0140 .057 Uiso calc R 1 . . H H4B -.1051 .7733 -.1096 .057 Uiso calc R 1 . . H H4C -.0852 .8787 -.0367 .057 Uiso calc R 1 . . H C8 .2747(5) .9906(5) .3324(4) .0442(13) Uani d . 1 . . C H8A .2534 .9683 .4127 .053 Uiso calc R 1 . . H H8B .2699 1.0865 .3094 .053 Uiso calc R 1 . . H C9 .4596(5) .9255(4) .2925(4) .0319(11) Uani d . 1 . . C H9A .5495 .9906 .2708 .038 Uiso calc R 1 . . H H9B .5056 .8555 .3507 .038 Uiso calc R 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 Sn2 .02822(18) .0325(2) .0236(2) -.00442(14) -.00504(14) -.00406(15) Sn1 .02558(18) .0271(2) .0262(2) -.00203(13) -.00240(14) -.00664(15) Cl1 .0363(6) .0395(7) .0247(7) -.0024(5) -.0034(5) -.0034(6) Cl4 .0447(7) .0481(8) .0253(7) -.0134(6) -.0025(5) -.0102(6) Cl2 .0341(6) .0407(8) .0485(8) .0096(5) -.0082(6) -.0154(6) Cl3 .0478(7) .0498(8) .0331(7) -.0207(6) .0030(6) -.0078(6) O1 .0299(16) .038(2) .035(2) -.0046(14) -.0026(14) -.0142(16) C2 .029(2) .029(3) .035(3) .000(2) -.005(2) -.007(2) C3 .035(3) .034(3) .034(3) -.003(2) -.010(2) -.002(2) C1 .040(3) .035(3) .030(3) -.007(2) -.006(2) -.012(2) N1 .0250(19) .028(2) .032(2) .0007(16) -.0018(17) -.0092(18) C5 .034(3) .020(3) .029(3) -.002(2) -.003(2) .004(2) C6 .029(2) .030(3) .039(3) .000(2) -.001(2) -.008(2) C7 .029(3) .049(3) .055(4) .001(2) -.006(2) -.020(3) C4 .046(3) .042(3) .055(4) .001(2) -.028(3) -.003(3) C8 .033(3) .055(4) .051(3) -.001(2) -.006(2) -.026(3) C9 .030(2) .031(3) .036(3) -.005(2) -.004(2) -.008(2) 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' O O .0106 .0060 '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 _geom_angle_publ_flag C3 Sn2 C4 146.29(17) y C3 Sn2 O1 89.91(14) y C4 Sn2 O1 83.59(15) y C3 Sn2 Cl3 106.58(11) y C4 Sn2 Cl3 106.37(13) y O1 Sn2 Cl3 89.24(8) y C3 Sn2 Cl4 91.98(12) y C4 Sn2 Cl4 93.81(14) y O1 Sn2 Cl4 177.35(7) y Cl3 Sn2 Cl4 92.00(5) y C2 Sn1 C1 142.33(17) y C2 Sn1 Cl2 105.64(11) y C1 Sn1 Cl2 103.99(12) y C2 Sn1 Cl1 99.50(12) y C1 Sn1 Cl1 100.18(12) y Cl2 Sn1 Cl1 95.67(5) y Sn1 Cl4 Sn2 135.56(5) y C5 O1 Sn2 140.0(3) ? Sn1 C2 H2A 109.5 ? Sn1 C2 H2B 109.5 ? H2A C2 H2B 109.5 ? Sn1 C2 H2C 109.5 ? H2A C2 H2C 109.5 ? H2B C2 H2C 109.5 ? Sn2 C3 H3A 109.5 ? Sn2 C3 H3B 109.5 ? H3A C3 H3B 109.5 ? Sn2 C3 H3C 109.5 ? H3A C3 H3C 109.5 ? H3B C3 H3C 109.5 ? Sn1 C1 H1A 109.5 ? Sn1 C1 H1B 109.5 ? H1A C1 H1B 109.5 ? Sn1 C1 H1C 109.5 ? H1A C1 H1C 109.5 ? H1B C1 H1C 109.5 ? C5 N1 C7 124.0(4) ? C5 N1 C8 114.0(3) ? C7 N1 C8 121.9(4) ? O1 C5 N1 123.2(4) ? O1 C5 C6 126.5(4) ? N1 C5 C6 110.2(4) ? C5 C6 C9 104.2(3) ? C5 C6 H6A 110.9 ? C9 C6 H6A 110.9 ? C5 C6 H6B 110.9 ? C9 C6 H6B 110.9 ? H6A C6 H6B 108.9 ? N1 C7 H7A 109.5 ? N1 C7 H7B 109.5 ? H7A C7 H7B 109.5 ? N1 C7 H7C 109.5 ? H7A C7 H7C 109.5 ? H7B C7 H7C 109.5 ? Sn2 C4 H4A 109.5 ? Sn2 C4 H4B 109.5 ? H4A C4 H4B 109.5 ? Sn2 C4 H4C 109.5 ? H4A C4 H4C 109.5 ? H4B C4 H4C 109.5 ? N1 C8 C9 103.9(3) ? N1 C8 H8A 111.0 ? C9 C8 H8A 111.0 ? N1 C8 H8B 111.0 ? C9 C8 H8B 111.0 ? H8A C8 H8B 109.0 ? C6 C9 C8 104.7(3) ? C6 C9 H9A 110.8 ? C8 C9 H9A 110.8 ? C6 C9 H9B 110.8 ? C8 C9 H9B 110.8 ? H9A C9 H9B 108.9 ? 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 Sn2 C3 . 2.100(4) y Sn2 C4 . 2.103(4) y Sn2 O1 . 2.278(3) y Sn2 Cl3 . 2.3777(13) y Sn2 Cl4 . 2.5704(13) y Sn1 C2 . 2.100(4) y Sn1 C1 . 2.109(4) y Sn1 Cl2 . 2.3702(13) ? Sn1 Cl1 . 2.4197(12) y Sn1 Cl4 . 3.1159(13) y O1 C5 . 1.259(5) ? C2 H2A . .9600 ? C2 H2B . .9600 ? C2 H2C . .9600 ? C3 H3A . .9600 ? C3 H3B . .9600 ? C3 H3C . .9600 ? C1 H1A . .9600 ? C1 H1B . .9600 ? C1 H1C . .9600 ? N1 C5 . 1.308(5) ? N1 C7 . 1.447(5) ? N1 C8 . 1.455(5) ? C5 C6 . 1.507(5) ? C6 C9 . 1.519(5) ? C6 H6A . .9700 ? C6 H6B . .9700 ? C7 H7A . .9600 ? C7 H7B . .9600 ? C7 H7C . .9600 ? C4 H4A . .9600 ? C4 H4B . .9600 ? C4 H4C . .9600 ? C8 C9 . 1.539(5) ? C8 H8A . .9700 ? C8 H8B . .9700 ? C9 H9A . .9700 ? C9 H9B . .9700 ? 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 C3 Sn2 O1 C5 61.5(4) C4 Sn2 O1 C5 -151.6(4) Cl3 Sn2 O1 C5 -45.1(4) Cl4 Sn2 O1 C5 -163.0(14) Sn2 O1 C5 N1 -175.3(3) Sn2 O1 C5 C6 8.3(7) C7 N1 C5 O1 -.7(7) C8 N1 C5 O1 -177.9(4) C7 N1 C5 C6 176.3(4) C8 N1 C5 C6 -1.0(5) O1 C5 C6 C9 -171.8(4) N1 C5 C6 C9 11.5(5) C5 N1 C8 C9 -9.8(5) C7 N1 C8 C9 172.9(4) C5 C6 C9 C8 -16.5(5) N1 C8 C9 C6 16.0(5)