#------------------------------------------------------------------------------ #$Date: 2013-08-29 18:37:19 +0300 (Thu, 29 Aug 2013) $ #$Revision: 88064 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/06/2010666.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_2010666 loop_ _publ_author_name 'K\"onig, Uwe-Christoph' 'Berkei, Michael' 'Neikes, Frank' 'Preut, Hans' 'Mitchell, Terence Nigel' _publ_section_title ; A 1:1 adduct between dimethyltin dibromide and N-methylpyrrolidinone (NMP) ; _journal_issue 2 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first e53 _journal_page_last e54 _journal_volume 56 _journal_year 2000 _chemical_formula_iupac '[Sn Br2 (C H3)2 (C5 H9 N O)]' _chemical_formula_sum 'C7 H15 Br2 N O Sn' _chemical_formula_weight 407.71 _chemical_name_systematic ; ? ; _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' _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 93.360(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 10.6520(10) _cell_length_b 7.0020(10) _cell_length_c 16.4270(10) _cell_measurement_reflns_used 9229 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 27.11 _cell_measurement_theta_min 2.48 _cell_volume 1223.1(2) _computing_cell_refinement 'DENZO and SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_collection 'Nonius KappaCCD software' _computing_data_reduction 'DENZO and SCALEPACK (Otwinowski & Minor, 1997)' _computing_publication_material 'SHELXL97 (Sheldrick, 1997) 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 .917 _diffrn_measured_fraction_theta_max .917 _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method ; 626 frames via \w rotation (\D\w = 1\%) at different \q values and two times 38 s per frame ; _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71069 _diffrn_reflns_av_R_equivalents .041 _diffrn_reflns_av_sigmaI/netI .0352 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 9229 _diffrn_reflns_theta_full 27.11 _diffrn_reflns_theta_max 27.11 _diffrn_reflns_theta_min 2.48 _diffrn_standards_decay_% 0 _diffrn_standards_number none _exptl_absorpt_coefficient_mu 8.585 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.214 _exptl_crystal_density_method 'not measured' _exptl_crystal_description parallelepiped _exptl_crystal_F_000 768 _exptl_crystal_size_max .2 _exptl_crystal_size_mid .2 _exptl_crystal_size_min .2 _refine_diff_density_max .884 _refine_diff_density_min -.931 _refine_ls_extinction_coef .0025(3) _refine_ls_extinction_method SHELXL97 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 113 _refine_ls_number_reflns 2682 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.049 _refine_ls_R_factor_all .029 _refine_ls_R_factor_gt .024 _refine_ls_shift/su_max .001 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme 'calc w = 1/[\s^2^(Fo^2^)+(0.0317P)^2^] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_wR_factor_ref .059 _reflns_number_gt 2379 _reflns_number_total 2682 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file qa0215.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P 21/c' _cod_database_code 2010666 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 Sn1 .811080(16) .74951(2) .185142(10) .02277(9) Uani d . 1 . . Sn Br1 .92241(3) .61543(4) .323657(17) .03551(10) Uani d . 1 . . Br Br2 .63049(3) .51577(3) .184962(15) .02864(10) Uani d . 1 . . Br C1 .7468(3) .9990(3) .24263(15) .0299(6) Uani d . 1 . . C H1A .8067 1.1000 .2375 .045 Uiso calc R 1 . . H H1B .7372 .9733 .2993 .045 Uiso calc R 1 . . H H1C .6672 1.0368 .2171 .045 Uiso calc R 1 . . H C2 .9500(3) .6407(4) .11158(17) .0353(7) Uani d . 1 . . C H2A .9222 .6532 .0552 .053 Uiso calc R 1 . . H H2B .9643 .5083 .1242 .053 Uiso calc R 1 . . H H2C 1.0267 .7109 .1218 .053 Uiso calc R 1 . . H O1 .7131(2) .8522(3) .06305(10) .0349(5) Uani d . 1 . . O C11 .7122(3) .9969(3) .01788(14) .0246(6) Uani d . 1 . . C C12 .7847(3) 1.1782(4) .03235(16) .0317(6) Uani d . 1 . . C H12A .8729 1.1600 .0228 .048 Uiso calc R 1 . . H H12B .7774 1.2239 .0876 .048 Uiso calc R 1 . . H C13 .7228(3) 1.3176(4) -.02993(16) .0322(6) Uani d . 1 . . C H13A .6603 1.3960 -.0052 .048 Uiso calc R 1 . . H H13B .7849 1.4000 -.0527 .048 Uiso calc R 1 . . H C14 .6613(3) 1.1865(4) -.09545(16) .0314(6) Uani d . 1 . . C H14A .5811 1.2374 -.1164 .047 Uiso calc R 1 . . H H14B .7154 1.1692 -.1403 .047 Uiso calc R 1 . . H N1 .6447(2) 1.0080(3) -.05207(12) .0247(5) Uani d . 1 . . N C15 .5759(3) .8472(4) -.08914(16) .0337(6) Uani d . 1 . . C H15A .6190 .8014 -.1350 .051 Uiso calc R 1 . . H H15B .4927 .8876 -.1071 .051 Uiso calc R 1 . . H H15C .5705 .7467 -.0498 .051 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 Sn1 .02696(14) .01880(12) .02245(13) .00207(6) .00053(9) .00061(6) Br1 .03496(19) .03579(17) .03442(17) -.00065(12) -.00950(13) .00971(11) Br2 .03064(18) .02591(15) .02893(16) -.00345(10) -.00191(12) .00106(10) C1 .0378(17) .0252(12) .0266(14) .0062(11) .0017(12) -.0024(10) C2 .0341(17) .0335(15) .0394(16) .0022(12) .0103(13) -.0070(12) O1 .0518(13) .0280(10) .0240(10) .0012(9) -.0051(9) .0071(7) C11 .0283(15) .0276(13) .0180(12) .0068(10) .0012(11) -.0004(10) C12 .0368(16) .0303(13) .0276(14) -.0014(12) -.0031(12) .0003(11) C13 .0438(18) .0246(13) .0286(14) .0010(12) .0065(13) .0013(11) C14 .0397(17) .0271(13) .0271(14) .0057(12) .0006(13) .0052(11) N1 .0303(13) .0241(10) .0194(10) .0030(9) -.0012(9) .0021(8) C15 .0373(17) .0337(14) .0299(14) -.0029(12) .0009(13) -.0022(11) 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 Sn1 C2 . 2.107(3) ? Sn1 C1 . 2.119(2) ? Sn1 O1 . 2.3205(17) ? Sn1 Br2 . 2.5256(4) ? Sn1 Br1 . 2.6737(4) ? C1 H1A . .9600 ? C1 H1B . .9600 ? C1 H1C . .9600 ? C2 H2A . .9600 ? C2 H2B . .9600 ? C2 H2C . .9600 ? O1 C11 . 1.256(3) ? C11 N1 . 1.321(3) ? C11 C12 . 1.498(4) ? C12 C13 . 1.535(4) ? C12 H12A . .9700 ? C12 H12B . .9700 ? C13 C14 . 1.532(4) ? C13 H13A . .9700 ? C13 H13B . .9700 ? C14 N1 . 1.454(3) ? C14 H14A . .9700 ? C14 H14B . .9700 ? N1 C15 . 1.458(3) ? C15 H15A . .9600 ? C15 H15B . .9600 ? C15 H15C . .9600 ? 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' Br Br -.2901 2.4595 '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 C2 Sn1 C1 144.11(11) C2 Sn1 O1 84.94(10) C1 Sn1 O1 89.35(9) C2 Sn1 Br2 108.98(8) C1 Sn1 Br2 105.58(8) O1 Sn1 Br2 84.02(5) C2 Sn1 Br1 94.00(8) C1 Sn1 Br1 92.82(7) O1 Sn1 Br1 177.50(5) Br2 Sn1 Br1 94.201(12) 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 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 C11 O1 Sn1 138.44(17) O1 C11 N1 123.1(2) O1 C11 C12 127.2(2) N1 C11 C12 109.7(2) C11 C12 C13 103.6(2) C11 C12 H12A 111.0 C13 C12 H12A 111.0 C11 C12 H12B 111.0 C13 C12 H12B 111.0 H12A C12 H12B 109.0 C14 C13 C12 103.7(2) C14 C13 H13A 111.0 C12 C13 H13A 111.0 C14 C13 H13B 111.0 C12 C13 H13B 111.0 H13A C13 H13B 109.0 N1 C14 C13 103.3(2) N1 C14 H14A 111.1 C13 C14 H14A 111.1 N1 C14 H14B 111.1 C13 C14 H14B 111.1 H14A C14 H14B 109.1 C11 N1 C14 113.7(2) C11 N1 C15 123.5(2) C14 N1 C15 122.1(2) N1 C15 H15A 109.5 N1 C15 H15B 109.5 H15A C15 H15B 109.5 N1 C15 H15C 109.5 H15A C15 H15C 109.5 H15B C15 H15C 109.5 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 C2 Sn1 O1 C11 -90.0(3) C1 Sn1 O1 C11 54.5(3) Br2 Sn1 O1 C11 160.3(3) Br1 Sn1 O1 C11 -155.2(10) Sn1 O1 C11 N1 178.07(18) Sn1 O1 C11 C12 -1.3(4) O1 C11 C12 C13 -166.4(3) N1 C11 C12 C13 14.1(3) C11 C12 C13 C14 -22.8(3) C12 C13 C14 N1 23.4(3) O1 C11 N1 C14 -178.1(2) C12 C11 N1 C14 1.3(3) O1 C11 N1 C15 -7.5(4) C12 C11 N1 C15 172.0(2) C13 C14 N1 C11 -16.2(3) C13 C14 N1 C15 173.0(2) _cod_database_fobs_code 2010666