#------------------------------------------------------------------------------ #$Date: 2016-02-14 14:26:36 +0000 (Sun, 14 Feb 2016) $ #$Revision: 176435 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/01/2010174.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_2010174 loop_ _publ_author_name 'Ross, Jennifer-Nicola' 'Wardell, James L.' 'Ferguson, George' 'Low, John N.' _publ_section_title ; Symmetrical tetrasubstituted tin compounds: tetrakis(2-methoxyphenyl)tin and tetrakis(2-methoxybenzyl)tin ; _journal_issue 11 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1703 _journal_page_last 1707 _journal_paper_doi 10.1107/S0108270194006815 _journal_volume 50 _journal_year 1994 _chemical_formula_moiety 'C32 H36 O4 Sn ' _chemical_formula_sum 'C32 H36 O4 Sn' _chemical_formula_weight 603.32 _chemical_name_common tetrakis(2-methoxybenzyl)tin _chemical_name_systematic ; tetrakis(2-methoxybenzyl)tin ; _space_group_IT_number 114 _symmetry_cell_setting tetragonal _symmetry_space_group_name_Hall 'P -4 2n' _symmetry_space_group_name_H-M 'P -4 21 c' _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 90.0 _cell_formula_units_Z 2 _cell_length_a 14.2266(17) _cell_length_b 14.2266(17) _cell_length_c 7.3943(7) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293 _cell_measurement_theta_max 14.75 _cell_measurement_theta_min 12.50 _cell_volume 1496.6(3) _computing_cell_refinement 'Enraf-Nonius CELDIM' _computing_data_collection 'Enraf-Nonius CAD4' _computing_data_reduction 'NRCVAX DATRD2' _computing_molecular_graphics NRCVAX _computing_publication_material 'NRCVAX TABLES (Jan. 94 Version)' _computing_structure_refinement 'NRCVAX LSTSQ' _computing_structure_solution 'Heavy-atom method and NRCVAX' _diffrn_ambient_temperature 293 _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method '\q/2\q scan b/P/b ' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'xray tube' _diffrn_radiation_type 'Molybdenum K\a' _diffrn_radiation_wavelength 0.71067 _diffrn_reflns_av_R_equivalents 0.018 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 4687 _diffrn_reflns_theta_max 29.90 _diffrn_reflns_theta_min 2.00 _diffrn_standards_decay_% 2.5 _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.84 _exptl_absorpt_correction_T_max 0.8165 _exptl_absorpt_correction_T_min 0.6540 _exptl_absorpt_correction_type empirical _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.339 _exptl_crystal_description plate _exptl_crystal_F_000 620 _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _refine_diff_density_max 0.16 _refine_diff_density_min -0.57 _refine_ls_abs_structure_Rogers 1.000 _refine_ls_goodness_of_fit_obs 1.05 _refine_ls_hydrogen_treatment 'H atoms refined as riding (C-H 0.95\%A)' _refine_ls_matrix_type full _refine_ls_number_parameters 84 _refine_ls_number_reflns 1425 _refine_ls_R_factor_all 0.049 _refine_ls_R_factor_obs 0.025 _refine_ls_shift/esd_max 0.001 _refine_ls_structure_factor_coef F _refine_ls_weighting_details 'w = 1/[\s^2^(F)+0.0008F^2^]' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.047 _refine_ls_wR_factor_obs 0.037 _reflns_number_observed 1425 _reflns_number_total 2182 _reflns_observed_criterion 'Inet > 2.5\s(Inet)' _cod_data_source_file ha1113.cif _cod_data_source_block II _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal' 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 'Tetragonal' changed to 'tetragonal' 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 The following automatic conversions were performed: '_refine_ls_weighting_scheme' value '1/[\s^2^(F)+0.0008F^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^2^(F)+0.0008F^2^]'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_cell_volume 1496.6(2) _cod_original_formula_sum 'C32 H36 O4 Sn ' _cod_database_code 2010174 loop_ _symmetry_equiv_pos_as_xyz x,y,z y,-x,-z -x,-y,z -y,x,-z 1/2-x,1/2+y,1/2-z 1/2-y,1/2-x,1/2+z 1/2+x,1/2-y,1/2-z 1/2+y,1/2+x,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 _atom_site_aniso_type_symbol Sn1 0.05471(16) 0.05471 0.0643(2) 0.0 0.0 0.0 Sn O21 0.086(2) 0.115(3) 0.096(3) -0.0328(19) -0.0192(19) 0.018(2) O C11 0.061(2) 0.083(3) 0.084(3) -0.0074(18) 0.014(2) -0.023(2) C C1 0.080(2) 0.071(2) 0.068(2) -0.0009(17) 0.0180(18) -0.0192(19) C C2 0.100(3) 0.075(2) 0.065(2) -0.027(2) 0.011(2) -0.005(2) C C3 0.138(4) 0.105(4) 0.091(4) -0.050(3) 0.013(3) -0.012(3) C C4 0.200(7) 0.074(3) 0.142(6) -0.042(4) 0.033(6) -0.017(4) C C5 0.196(6) 0.069(3) 0.135(5) 0.028(4) 0.023(5) -0.006(3) C C6 0.124(4) 0.083(3) 0.104(4) 0.029(3) 0.013(3) -0.021(3) C C21 0.090(3) 0.199(7) 0.095(5) -0.044(4) -0.021(3) 0.033(5) C loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_type_symbol Sn1 0.0 0.0 0.0 0.0579(2) Uani ? S Sn O21 -0.1009(3) -0.1251(3) -0.3107(7) 0.099(2) Uani ? . O C11 0.0703(3) -0.1021(3) -0.1697(8) 0.076(2) Uani ? . C C1 0.0247(3) -0.1956(3) -0.1666(6) 0.073(2) Uani ? . C C2 -0.0639(3) -0.2057(3) -0.2422(7) 0.080(2) Uani ? . C C3 -0.1104(4) -0.2919(4) -0.2441(9) 0.112(4) Uani ? . C C4 -0.0665(6) -0.3671(4) -0.1648(12) 0.138(6) Uani ? . C C5 0.0186(6) -0.3598(4) -0.0856(12) 0.133(5) Uani ? . C C6 0.0643(3) -0.2740(3) -0.0870(8) 0.104(3) Uani ? . C C21 -0.1945(4) -0.1274(7) -0.3859(9) 0.128(5) Uani ? . C H11A 0.134 -0.106 -0.131 0.0863 Uiso ? . H H11B 0.071 -0.079 -0.290 0.0863 Uiso ? . H H3 -0.169 -0.302 -0.302 0.1217 Uiso ? . H H4 -0.092 -0.429 -0.156 0.1484 Uiso ? . H H5 0.049 -0.409 -0.023 0.1434 Uiso ? . H H6 0.124 -0.270 -0.031 0.1136 Uiso ? . H H21A -0.214 -0.067 -0.428 0.1380 Uiso ? . H H21B -0.197 -0.175 -0.475 0.1380 Uiso ? . H H21C -0.234 -0.148 -0.290 0.1380 Uiso ? . H loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0.002 0.002 'International Tables Vol. IV Table 2.2B' H 0.000 0.000 'International Tables Vol. IV Table 2.2B' O 0.008 0.006 'International Tables Vol. IV Table 2.2B' Sn -0.873 1.424 'International Tables Vol. IV Table 2.2B' loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -6 -2 4 -6 2 4 -2 6 4 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C11 Sn1 C11 2_555 109.6(2) yes C11 Sn1 C11 3_555 109.1(2) yes C2 O21 C21 . 118.8(6) yes Sn1 C11 C1 . 113.1(3) yes C11 C1 C2 . 119.0(5) yes C11 C1 C6 . 123.7(5) yes C2 C1 C6 . 117.3(5) no O21 C2 C1 . 114.5(5) yes O21 C2 C3 . 123.7(6) yes C1 C2 C3 . 121.8(6) no C2 C3 C4 . 117.8(7) no C3 C4 C5 . 122.3(6) no C4 C5 C6 . 119.2(7) no C1 C6 C5 . 121.6(7) 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 Sn1 C11 . . 2.165(5) yes O21 C2 . . 1.360(8) yes O21 C21 . . 1.444(8) yes C11 C1 . . 1.480(7) yes C1 C2 . . 1.387(8) no C1 C6 . . 1.380(8) no C2 C3 . . 1.394(8) no C3 C4 . . 1.370(15) no C4 C5 . . 1.349(17) no C5 C6 . . 1.383(11) no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_2 _geom_contact_publ_flag O21 O21 4.573(9) 3_555 no O21 O21 5.619(9) 2_555 no 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 _geom_torsion_publ_flag C21 O21 C2 C1 -177.5(11) no C21 O21 C2 C3 1.6(7) no Sn1 C11 C1 C2 67.6(5) no Sn1 C11 C1 C6 -110.3(7) no C11 C1 C2 O21 -1.0(5) no C11 C1 C2 C3 179.8(10) no C6 C1 C2 O21 177.0(10) no C6 C1 C2 C3 -2.2(6) no C11 C1 C6 C5 179.3(11) no C2 C1 C6 C5 1.3(6) no O21 C2 C3 C4 -177.7(13) no C1 C2 C3 C4 1.4(6) no C2 C3 C4 C5 0.4(7) no C3 C4 C5 C6 -1.2(6) no C4 C5 C6 C1 0.3(7) no