#------------------------------------------------------------------------------ #$Date: 2023-03-28 14:50:48 +0100 (Tue, 28 Mar 2023) $ #$Revision: 282086 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/01/2010164.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_2010164 loop_ _publ_author_name 'Marsh, R.E.' _publ_section_title ; n-Butyltris(2-pyrimidinethiolato-N,S)tin(IV): change in space group ; _journal_issue 11 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1713 _journal_page_last 1715 _journal_paper_doi 10.1107/S0108270194005767 _journal_volume 50 _journal_year 1994 _chemical_formula_sum 'C16 H18 N6 S3 Sn' _chemical_formula_weight 509.23 _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 IntTabC _cell_angle_alpha 90. _cell_angle_beta 92.67(3) _cell_angle_gamma 90. _cell_formula_units_Z 4 _cell_length_a 9.523(2) _cell_length_b 12.849(3) _cell_length_c 17.079(3) _cell_measurement_reflns_used 50 _cell_measurement_temperature 291.0(10) _cell_measurement_theta_max 15.1 _cell_measurement_theta_min 7.8 _cell_volume 2087.5(8) _diffrn_measurement_device 'Nicolet R3m/V' _diffrn_measurement_method \w/2\q _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.018 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 6035 _diffrn_reflns_theta_max 25 _diffrn_standards_decay_% none _diffrn_standards_interval_time 150 _diffrn_standards_number 6 _exptl_absorpt_coefficient_mu 1.528 _exptl_absorpt_correction_T_max 0.961 _exptl_absorpt_correction_T_min 0.925 _exptl_absorpt_correction_type empirical _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.620 _exptl_crystal_description block _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.20 _refine_ls_hydrogen_treatment refU _refine_ls_number_parameters 259 _refine_ls_number_reflns 2664 _refine_ls_R_factor_obs 0.0311 _refine_ls_structure_factor_coef Fsqd _reflns_number_observed 2664 _reflns_number_total 3889 _reflns_observed_criterion F>1.5\s(F) _cod_data_source_file cr1153.cif _cod_data_source_block cr1153_structure_1_of_1 _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 2010164 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_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv Sn .45783(3) .25783(2) .21856(2) .05120(10) S(1) .25755(13) .38698(10) .19764(8) .0661(3) S(2) .58685(15) .35922(10) .11700(9) .0768(4) S(3) .56789(14) .34273(9) .33364(8) .0643(3) C(11) .1678(5) .3214(3) .2694(3) .0558(11) N(11) .2419(4) .2432(3) .3044(2) .0612(9) C(13) .1812(6) .1923(4) .3614(3) .0816(16) C(14) .0483(7) .2175(5) .3833(3) .0886(17) C(15) -.0183(6) .2973(5) .3440(4) .0819(16) N(12) .0383(4) .3506(3) .2861(3) .0704(11) C(21) .7257(5) .2726(3) .1343(3) .0663(13) N(21) .7031(4) .2001(3) .1895(2) .0626(10) C(23) .8057(5) .1315(4) .2049(3) .0720(14) C(24) .9295(6) .1345(4) .1673(4) .0842(17) C(25) .9423(6) .2111(4) .1119(4) .0901(18) N(22) .8428(5) .2808(3) .0940(3) .0806(12) C(31) .5941(4) .2210(3) .3785(3) .0517(10) N(31) .5449(4) .1405(3) .3359(2) .0531(9) C(33) .5679(5) .0457(3) .3673(3) .0620(13) C(34) .6342(6) .0332(4) .4379(3) .0699(14) C(35) .6793(6) .1212(5) .4763(3) .0855(18) N(32) .6615(5) .2168(3) .4474(2) .0761(12) C(1) .3853(6) .1169(4) .1650(3) .0773(15) C(2a) .322(4) .113(3) .097(2) 8.2(8) C(2b) .3777(16) .1205(8) .0747(8) .075(3) C(3a) .283(3) -.006(2) .068(2) .128(10) C(3b) .3303(17) .0263(11) .0327(9) .104(4) C(4a) .255(4) -.0108(18) -.0152(19) .129(10) C(4b) .1986(18) -.0105(12) .0462(12) .130(6) H(13) .2307 .1373 .3876 8.2 H(14) .0047 .1810 .4240 8.9 H(15) -.1099 .3160 .3586 8.2 H(23) .7925 .0790 .2431 7.2 H(24) 1.0029 .0861 .1790 8.4 H(25) 1.0271 .2144 .0848 9.0 H(33) .5364 -.0141 .3389 6.2 H(34) .6492 -.0339 .4602 7.0 H(35) .7259 .1138 .5264 8.6 H(1a) .3223 .0869 .2001 7.7 H(1b) .4658 .0737 .1618 7.7 H(1c) .2940 .1024 .1823 7.7 H(1d) .4476 .0624 .1812 7.7 H(2a) .3812 .1442 .0601 10.1 H(2b) .2373 .1522 .0987 10.1 H(2c) .4690 .1368 .0582 8.0 H(2d) .3146 .1752 .0593 8.0 H(3a) .2025 -.0294 .0935 12.6 H(3b) .3603 -.0507 .0813 12.6 H(3c) .3956 -.0274 .0462 10.3 H(3d) .3329 .0406 -.0219 10.3 H(4a) .2327 -.0804 -.0300 13.5 H(4b) .1772 .0331 .0291 13.5 H(4c) .3350 .0117 -.0413 13.5 H(4d) .1809 -.0715 .0159 12.8 H(4e) .1934 -.0269 .1004 12.8 H(4f) .1307 .0410 .0323 12.8 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 S(1) Sn S(2) 87.29(4) yes S(1) Sn S(3) 96.47(4) yes S(2) Sn S(3) 96.76(4) yes S(1) Sn C(1) 105.60(10) yes S(2) Sn C(1) 107.50(10) yes S(3) Sn C(1) 147.60(10) yes N(11) C(11) S(1) 114.0(3) yes N(12) C(11) S(1) 120.2(3) yes N(12) C(11) N(11) 125.8(4) yes C(13) N(11) C(11) 117.0(4) yes C(14) C(13) N(11) 121.4(5) yes C(15) C(14) C(13) 117.0(5) yes N(12) C(15) C(14) 123.7(5) yes C(15) N(12) C(11) 115.0(4) yes N(21) C(21) S(2) 114.5(3) yes N(22) C(21) S(2) 120.3(4) yes N(22) C(21) N(21) 125.2(4) yes C(23) N(21) C(21) 117.1(4) yes C(24) C(23) N(21) 121.9(5) yes C(25) C(24) C(23) 116.7(5) yes N(22) C(25) C(24) 123.8(5) yes C(25) N(22) C(21) 115.4(4) yes N(31) C(31) S(3) 114.4(3) yes N(32) C(31) S(3) 118.7(3) yes N(32) C(31) N(31) 126.8(4) yes C(33) N(31) C(31) 115.9(4) yes C(34) C(33) N(31) 121.8(4) yes C(35) C(34) C(33) 117.1(5) yes N(32) C(35) C(34) 123.7(5) yes C(35) N(32) C(31) 114.6(4) yes C(3a) C(2a) C(1) 113.(3) yes C(3b) C(2b) C(1) 117.6(11) yes C(4a) C(3a) C(2a) 111.(3) yes C(4b) C(3b) C(2b) 117.8(14) yes 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 S(1) . . 2.5410(10) yes Sn S(2) . . 2.5330(10) yes Sn S(3) . . 2.4410(10) yes Sn N(11) . . 2.588(4) yes Sn N(21) . . 2.522(4) yes Sn N(31) . . 2.612(4) yes Sn C(1) . . 2.130(5) yes S(1) C(11) . . 1.744(5) yes S(2) C(21) . . 1.743(5) yes S(3) C(31) . . 1.754(4) yes C(11) N(11) . . 1.351(6) yes C(11) N(12) . . 1.332(6) yes N(11) C(13) . . 1.326(7) yes C(13) C(14) . . 1.375(8) yes C(14) C(15) . . 1.366(8) yes C(15) N(12) . . 1.336(7) yes C(21) N(21) . . 1.350(6) yes C(21) N(22) . . 1.342(6) yes N(21) C(23) . . 1.333(6) yes C(23) C(24) . . 1.369(8) yes C(24) C(25) . . 1.376(8) yes C(25) N(22) . . 1.328(7) yes C(31) N(31) . . 1.337(5) yes C(31) N(32) . . 1.316(6) yes N(31) C(33) . . 1.345(6) yes C(33) C(34) . . 1.345(7) yes C(34) C(35) . . 1.366(8) yes C(35) N(32) . . 1.332(7) yes C(1) C(2a) . . 1.29(4) yes C(1) C(2b) . . 1.540(14) yes C(2a) C(3a) . . 1.65(5) yes C(2b) C(3b) . . 1.47(2) yes C(3a) C(4a) . . 1.43(5) yes C(3b) C(4b) . . 1.37(2) yes loop_ _cod_changelog_entry_id _cod_changelog_entry_author _cod_changelog_entry_date _cod_changelog_entry_text 1 'Vaitkus, Antanas' 2023-03-28T16:50:00+03:00 ; Changed the '_refine_ls_structure_factor_coef' data item value from 'F2' to 'Fsqd' after consulting the original publication. ;