#------------------------------------------------------------------------------ #$Date: 2015-04-02 12:22:18 +0100 (Thu, 02 Apr 2015) $ #$Revision: 134621 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/84/2008421.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_2008421 loop_ _publ_author_name 'Ng, Seik Weng' _publ_section_title ; Coordination complexes of triphenyltin coumarin-3-carboxylate with O-donor ligands: (coumarin-3-carboxylato)triphenyltin--L (L = ethanol, diphenylcyclopropenone and quinoline N-oxide) and bis[(coumarin-3-carboxylato)triphenyltin]--L (L = triphenylphosphine oxide and triphenylarsine oxide) ; _journal_issue 4 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 523 _journal_page_last 531 _journal_paper_doi 10.1107/S0108270198014991 _journal_volume 55 _journal_year 1999 _chemical_formula_moiety '[Sn(C6H5)3(C10H5O4)(C2H6O)]' _chemical_formula_sum 'C30 H26 O5 Sn' _chemical_formula_weight 585.20 _chemical_name_systematic ; (Coumarin-3-carboxylato)triphenyltin^.^ethanol ; _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 93.532(9) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 9.115(2) _cell_length_b 14.226(2) _cell_length_c 20.224(4) _cell_measurement_reflns_used 25 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 10.0 _cell_measurement_theta_min 8.0 _cell_volume 2617.5(9) _computing_cell_refinement 'CELDIM in CAD-4 VAX/PC' _computing_data_collection 'CAD-4 VAX/PC (Enraf-Nonius, 1988)' _computing_data_reduction 'XCAD-4 (Harms, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1990)' _diffrn_ambient_temperature 298(2) _diffrn_measured_fraction_theta_full 0.952 _diffrn_measured_fraction_theta_max 0.952 _diffrn_measurement_device_type 'Enraf-Nonius CAD-4' _diffrn_measurement_method \w-2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.038 _diffrn_reflns_av_sigmaI/netI 0.0847 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 3651 _diffrn_reflns_theta_full 22.44 _diffrn_reflns_theta_max 22.44 _diffrn_reflns_theta_min 1.75 _diffrn_standards_decay_% 4 _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.014 _exptl_absorpt_correction_T_max 0.897 _exptl_absorpt_correction_T_min 0.852 _exptl_absorpt_correction_type '\y scan (North et al., 1968)' _exptl_crystal_colour Colorless _exptl_crystal_density_diffrn 1.485 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Plate _exptl_crystal_F_000 1184 _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.11 _refine_diff_density_max 0.395 _refine_diff_density_min -0.552 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_hydrogen_treatment 'H atoms riding; U(H) = 1.5U~eq~(C,O)' _refine_ls_matrix_type full _refine_ls_number_parameters 289 _refine_ls_number_reflns 3398 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.992 _refine_ls_R_factor_all 0.096 _refine_ls_R_factor_gt 0.052 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0500P)^2^] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.118 _reflns_number_gt 2244 _reflns_number_total 3398 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file sk1234.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P 21/c' _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' 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: '_refine_ls_weighting_scheme' value 'calc w = 1/[\s^2^(Fo^2^)+(0.0500P)^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^)+(0.0500P)^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 2617.6(8) _cod_database_code 2008421 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 0.58236(6) 0.47436(4) 0.30411(3) 0.0428(2) Uani d . 1 . . Sn O1 0.7396(6) 0.5866(4) 0.3140(3) 0.053(2) Uani d . 1 . . O O2 0.6213(7) 0.6935(4) 0.2521(3) 0.069(2) Uani d . 1 . . O O3 0.9221(6) 0.8044(4) 0.4332(3) 0.058(2) Uani d . 1 . . O O4 0.7841(7) 0.6789(5) 0.4390(3) 0.072(2) Uani d . 1 . . O O5 0.4169(6) 0.3462(4) 0.3201(3) 0.055(2) Uani d . 1 . . O C1 0.5263(6) 0.4572(4) 0.2010(2) 0.045(2) Uani d G 1 . . C C2 0.4446(7) 0.5256(4) 0.1662(3) 0.063(2) Uani d G 1 . . C C3 0.3988(7) 0.5108(5) 0.1002(3) 0.086(3) Uani d G 1 . . C C4 0.4348(8) 0.4276(6) 0.0690(2) 0.087(4) Uani d G 1 . . C C5 0.5165(8) 0.3592(4) 0.1038(3) 0.082(3) Uani d G 1 . . C C6 0.5622(6) 0.3740(4) 0.1698(3) 0.063(3) Uani d G 1 . . C C7 0.7492(5) 0.3849(4) 0.3481(3) 0.049(2) Uani d G 1 . . C C8 0.7506(6) 0.2900(4) 0.3318(3) 0.074(3) Uani d G 1 . . C C9 0.8592(8) 0.2315(3) 0.3602(4) 0.092(4) Uani d G 1 . . C C10 0.9663(6) 0.2679(5) 0.4049(3) 0.090(4) Uani d G 1 . . C C11 0.9650(6) 0.3628(6) 0.4213(3) 0.078(3) Uani d G 1 . . C C12 0.8564(7) 0.4213(4) 0.3929(3) 0.059(2) Uani d G 1 . . C C13 0.4235(5) 0.5489(4) 0.3556(3) 0.042(2) Uani d G 1 . . C C14 0.2853(7) 0.5604(5) 0.3236(2) 0.078(3) Uani d G 1 . . C C15 0.1733(5) 0.6029(5) 0.3564(4) 0.092(4) Uani d G 1 . . C C16 0.1994(7) 0.6339(5) 0.4212(4) 0.088(4) Uani d G 1 . . C C17 0.3375(8) 0.6224(5) 0.4533(3) 0.088(4) Uani d G 1 . . C C18 0.4496(6) 0.5799(4) 0.4205(3) 0.066(3) Uani d G 1 . . C C19 0.7130(9) 0.6699(6) 0.2961(4) 0.049(2) Uani d . 1 . . C C20 0.8049(9) 0.7441(6) 0.3318(4) 0.041(2) Uani d . 1 . . C C21 0.8655(9) 0.8144(6) 0.2991(4) 0.048(2) Uani d . 1 . . C C22 0.9595(8) 0.8841(6) 0.3310(4) 0.044(2) Uani d . 1 . . C C23 1.0270(10) 0.9583(6) 0.2998(5) 0.060(3) Uani d . 1 . . C C24 1.1160(10) 1.0210(7) 0.3338(6) 0.072(3) Uani d . 1 . . C C25 1.1380(10) 1.0101(7) 0.4007(6) 0.074(3) Uani d . 1 . . C C26 1.0760(10) 0.9357(7) 0.4351(5) 0.066(3) Uani d . 1 . . C C27 0.9842(9) 0.8759(6) 0.3981(5) 0.052(2) Uani d . 1 . . C C28 0.8323(9) 0.7366(6) 0.4026(5) 0.050(2) Uani d . 1 . . C C29 0.3590(10) 0.3275(8) 0.3817(6) 0.094(4) Uani d . 1 . . C C30 0.399(2) 0.2430(10) 0.4128(7) 0.133(5) Uani d . 1 . . C HO5 0.3898 0.3076 0.2843 0.082 Uiso calc R 1 . . H H2 0.4206 0.5813 0.1871 0.095 Uiso calc R 1 . . H H3 0.3442 0.5566 0.0770 0.128 Uiso calc R 1 . . H H4 0.4042 0.4177 0.0249 0.131 Uiso calc R 1 . . H H5 0.5405 0.3036 0.0829 0.122 Uiso calc R 1 . . H H6 0.6169 0.3283 0.1931 0.095 Uiso calc R 1 . . H H8 0.6789 0.2657 0.3018 0.111 Uiso calc R 1 . . H H9 0.8601 0.1680 0.3492 0.139 Uiso calc R 1 . . H H10 1.0390 0.2287 0.4239 0.136 Uiso calc R 1 . . H H11 1.0367 0.3871 0.4512 0.117 Uiso calc R 1 . . H H12 0.8555 0.4848 0.4038 0.089 Uiso calc R 1 . . H H14 0.2678 0.5396 0.2802 0.117 Uiso calc R 1 . . H H15 0.0808 0.6105 0.3350 0.138 Uiso calc R 1 . . H H16 0.1244 0.6623 0.4432 0.132 Uiso calc R 1 . . H H17 0.3550 0.6431 0.4966 0.131 Uiso calc R 1 . . H H18 0.5420 0.5722 0.4419 0.099 Uiso calc R 1 . . H H21 0.8458 0.8184 0.2536 0.071 Uiso calc R 1 . . H H23 1.0108 0.9653 0.2542 0.090 Uiso calc R 1 . . H H24 1.1596 1.0700 0.3120 0.109 Uiso calc R 1 . . H H25 1.1973 1.0535 0.4244 0.110 Uiso calc R 1 . . H H26 1.0953 0.9273 0.4804 0.099 Uiso calc R 1 . . H H29a 0.3892 0.3781 0.4117 0.141 Uiso calc R 1 . . H H29b 0.2530 0.3295 0.3758 0.141 Uiso calc R 1 . . H H30a 0.3531 0.2384 0.4543 0.200 Uiso calc R 1 . . H H30b 0.5034 0.2397 0.4206 0.200 Uiso calc R 1 . . H H30c 0.3659 0.1911 0.3849 0.200 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 0.0390(3) 0.0387(3) 0.0500(4) 0.0031(3) -0.0030(2) -0.0001(4) O1 0.042(3) 0.039(4) 0.078(4) 0.004(3) -0.007(3) 0.007(3) O2 0.082(5) 0.038(4) 0.080(5) -0.005(3) -0.034(4) 0.000(3) O3 0.058(4) 0.061(4) 0.054(4) -0.016(3) -0.005(3) -0.006(3) O4 0.084(5) 0.083(5) 0.048(4) -0.026(4) -0.004(4) 0.013(4) O5 0.054(4) 0.050(4) 0.060(4) -0.008(3) 0.005(3) -0.004(3) C1 0.043(5) 0.038(6) 0.055(5) -0.009(4) 0.002(4) -0.008(4) C2 0.078(6) 0.048(5) 0.062(6) -0.001(6) -0.008(5) 0.005(5) C3 0.095(8) 0.110(10) 0.057(7) 0.001(7) -0.013(6) 0.000(7) C4 0.101(9) 0.100(10) 0.057(7) -0.022(8) -0.006(6) -0.020(7) C5 0.104(9) 0.070(8) 0.072(8) -0.008(7) 0.013(7) -0.019(6) C6 0.074(7) 0.067(7) 0.050(6) -0.010(6) 0.012(5) -0.002(5) C7 0.039(5) 0.048(6) 0.059(6) 0.007(4) 0.006(4) 0.008(5) C8 0.051(6) 0.057(7) 0.113(9) 0.017(5) -0.008(6) 0.019(6) C9 0.063(7) 0.058(7) 0.156(12) 0.014(6) 0.009(8) 0.043(7) C10 0.054(7) 0.110(10) 0.110(10) 0.018(7) 0.012(7) 0.050(8) C11 0.050(6) 0.120(10) 0.064(7) 0.021(7) -0.017(5) 0.020(7) C12 0.055(6) 0.071(7) 0.053(6) 0.001(5) 0.004(5) 0.003(5) C13 0.045(5) 0.024(5) 0.058(6) 0.005(4) -0.001(4) -0.003(4) C14 0.057(6) 0.104(9) 0.072(7) 0.031(6) -0.005(6) -0.004(6) C15 0.061(7) 0.130(10) 0.080(8) 0.033(7) -0.010(6) -0.008(8) C16 0.072(8) 0.090(9) 0.100(10) 0.034(7) 0.018(7) -0.011(7) C17 0.084(8) 0.110(10) 0.071(8) -0.005(7) 0.027(7) -0.031(7) C18 0.066(7) 0.071(7) 0.062(7) -0.003(6) 0.004(5) -0.010(6) C19 0.044(5) 0.045(6) 0.059(6) -0.001(5) 0.003(5) -0.004(5) C20 0.043(5) 0.036(5) 0.043(6) -0.005(4) -0.007(4) 0.005(4) C21 0.047(5) 0.049(6) 0.044(5) 0.004(5) -0.013(4) -0.004(5) C22 0.032(5) 0.044(5) 0.056(6) -0.001(4) -0.001(4) -0.002(5) C23 0.057(6) 0.050(6) 0.073(7) -0.002(5) 0.002(5) 0.006(5) C24 0.051(6) 0.059(6) 0.107(9) -0.009(6) 0.006(6) -0.006(7) C25 0.063(7) 0.054(7) 0.103(9) -0.012(5) 0.008(6) -0.017(7) C26 0.071(7) 0.060(6) 0.067(7) -0.004(6) -0.005(6) -0.010(6) C27 0.041(5) 0.046(6) 0.068(7) -0.009(5) 0.006(5) -0.013(5) C28 0.042(5) 0.046(6) 0.062(7) -0.001(5) -0.005(5) -0.002(5) C29 0.109(9) 0.071(8) 0.110(10) -0.004(7) 0.042(8) 0.028(7) C30 0.150(10) 0.140(10) 0.110(10) -0.020(10) 0.020(10) 0.020(10) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 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 C1 Sn1 C13 114.1(2) yes C1 Sn1 C7 117.5(2) yes C1 Sn1 O1 107.2(2) yes C1 Sn1 O5 86.0(2) yes C7 Sn1 C13 125.7(2) yes C7 Sn1 O1 87.1(2) yes C7 Sn1 O5 85.9(2) yes C13 Sn1 O1 93.1(2) yes C13 Sn1 O5 81.9(2) yes O1 Sn1 O5 166.8(2) yes C19 O1 Sn1 123.9(5) no C28 O3 C27 122.1(7) no C29 O5 Sn1 122.3(6) no C2 C1 C6 120.0 no C2 C1 Sn1 120.3(3) no C6 C1 Sn1 119.5(3) no C1 C2 C3 120.0 no C4 C3 C2 120.0 no C3 C4 C5 120.0 no C4 C5 C6 120.0 no C5 C6 C1 120.0 no C8 C7 C12 120.0 no C8 C7 Sn1 119.7(3) no C12 C7 Sn1 120.3(3) no C9 C8 C7 120.0 no C8 C9 C10 120.0 no C11 C10 C9 120.0 no C10 C11 C12 120.0 no C11 C12 C7 120.0 no C14 C13 C18 120.0 no C14 C13 Sn1 117.2(3) no C18 C13 Sn1 122.7(3) no C15 C14 C13 120.0 no C14 C15 C16 120.0 no C15 C16 C17 120.0 no C18 C17 C16 120.0 no C17 C18 C13 120.0 no O2 C19 O1 125.1(8) no O2 C19 C20 119.4(8) no O1 C19 C20 115.5(8) no C21 C20 C28 119.7(8) no C21 C20 C19 121.5(8) no C28 C20 C19 118.8(8) no C20 C21 C22 123.2(8) no C27 C22 C23 117.6(8) no C27 C22 C21 116.3(8) no C23 C22 C21 126.0(8) no C24 C23 C22 122.2(9) no C25 C24 C23 118.0(10) no C24 C25 C26 122.0(10) no C27 C26 C25 116.5(9) no C22 C27 C26 122.9(9) no C22 C27 O3 121.7(7) no C26 C27 O3 115.4(9) no O4 C28 O3 115.4(8) no O4 C28 C20 127.6(8) no O3 C28 C20 117.0(8) no C30 C29 O5 118.0(10) no 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 C1 . 2.129(4) yes Sn1 C7 . 2.135(4) yes Sn1 C13 . 2.120(4) yes Sn1 O1 . 2.147(5) yes Sn1 O5 . 2.401(5) yes O1 C19 . 1.259(9) no O2 C19 . 1.229(9) no O3 C28 . 1.386(9) no O3 C27 . 1.380(10) no O4 C28 . 1.204(9) no O5 C29 . 1.410(10) no C1 C2 . 1.3900 no C1 C6 . 1.3900 no C2 C3 . 1.3900 no C3 C4 . 1.3900 no C4 C5 . 1.3900 no C5 C6 . 1.3900 no C7 C8 . 1.3900 no C7 C12 . 1.3900 no C8 C9 . 1.3900 no C9 C10 . 1.3900 no C10 C11 . 1.3900 no C11 C12 . 1.3900 no C13 C14 . 1.3900 no C13 C18 . 1.3900 no C14 C15 . 1.3900 no C15 C16 . 1.3900 no C16 C17 . 1.3900 no C17 C18 . 1.3900 no C19 C20 . 1.510(10) no C20 C21 . 1.340(10) no C20 C28 . 1.440(10) no C21 C22 . 1.440(10) no C22 C27 . 1.370(10) no C22 C23 . 1.390(10) no C23 C24 . 1.360(10) no C24 C25 . 1.370(10) no C25 C26 . 1.410(10) no C26 C27 . 1.380(10) no C29 C30 . 1.400(10) no O2 O5 2_655 2.629(8) no