#------------------------------------------------------------------------------ #$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2005066.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_2005066 loop_ _publ_author_name 'Basu Baul, T. S.' 'Tiekink, E. R. T.' _publ_section_title ; Polymeric [p-(2-Hydroxy-5-methylphenylazo)benzoato]trimethyltin ; _journal_issue 6 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1428 _journal_page_last 1430 _journal_volume 52 _journal_year 1996 _chemical_formula_iupac '[Sn (C14 H11 N2 O3) (C1 H3)3]n' _chemical_formula_moiety 'C17 H20 N2 O3 Sn' _chemical_formula_sum 'C17 H20 N2 O3 Sn' _chemical_formula_weight 419.05 _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _cell_angle_alpha 90. _cell_angle_beta 98.270(10) _cell_angle_gamma 90. _cell_formula_units_Z 8 _cell_length_a 13.165(3) _cell_length_b 9.530(5) _cell_length_c 28.924(2) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293 _cell_measurement_theta_max 23.9 _cell_measurement_theta_min 21.6 _cell_volume 3591(2) _computing_cell_refinement 'MSC/AFC Diffractometer Control Software' _computing_data_collection ; MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1988) ; _computing_data_reduction 'TEXSAN (Molecular Structure Corporation, 1992)' _computing_publication_material TEXSAN _computing_structure_refinement 'TEXSAN; all reflection data used' _diffrn_ambient_temperature 293 _diffrn_measurement_device 'Rigaku AFC6R' _diffrn_measurement_method \w/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents 0.0356 _diffrn_reflns_av_sigmaI/netI 13.9 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_number 4605 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_min 3.0 _diffrn_standards_decay_% 0.58 _diffrn_standards_interval_count 400 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.438 _exptl_absorpt_correction_T_max 0.825 _exptl_absorpt_correction_T_min 0.627 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details 'Tompa analytical' _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.550 _exptl_crystal_description block _exptl_crystal_F_000 1680.00 _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _refine_diff_density_max 0.95 _refine_diff_density_min -0.64 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 1.572 _refine_ls_goodness_of_fit_obs 1.572 _refine_ls_hydrogen_treatment noref _refine_ls_matrix_type full _refine_ls_number_parameters 208 _refine_ls_number_reflns 4160 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0639 _refine_ls_R_factor_obs 0.0639 _refine_ls_shift/esd_max 0.0007 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme sigma _refine_ls_wR_factor_all 0.0848 _refine_ls_wR_factor_obs 0.0848 _reflns_number_observed 4160 _reflns_number_total 4160 _[local]_cod_data_source_file ta1087.cif _[local]_cod_data_source_block me3snd2 _[local]_cod_cif_authors_sg_H-M 'C 2/c' _cod_original_cell_volume 3591.0(10) _cod_database_code 2005066 loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, +y,1/2-z' ' -x, -y, -z' ' +x, -y,1/2+z' 1/2+x,1/2+y,z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,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 Sn 0.0560(2) 0.0438(2) 0.0487(2) -0.0022(2) 0.02110(10) -0.00130(10) O(1) 0.070(2) 0.048(2) 0.057(2) -0.004(2) 0.0270(10) -0.0110(10) O(2) 0.085(2) 0.052(2) 0.0430(10) 0.005(2) 0.027(2) 0.0040(10) O(3) 0.108(3) 0.086(3) 0.066(2) 0.004(2) 0.045(2) 0.006(2) N(1) 0.058(2) 0.062(2) 0.043(2) 0.010(2) 0.017(2) -0.004(2) N(2) 0.053(2) 0.062(2) 0.044(2) 0.008(2) 0.012(2) -0.009(2) C(1) 0.052(2) 0.047(2) 0.042(2) 0.011(2) 0.010(2) 0.001(2) C(2) 0.049(2) 0.045(2) 0.040(2) 0.006(2) 0.013(2) 0.000(2) C(3) 0.074(3) 0.045(2) 0.047(2) 0.000(2) 0.028(2) 0.000(2) C(4) 0.070(3) 0.051(3) 0.053(2) 0.001(2) 0.024(2) -0.005(2) C(5) 0.052(2) 0.054(2) 0.042(2) 0.008(2) 0.014(2) -0.001(2) C(6) 0.064(3) 0.061(3) 0.054(2) -0.002(2) 0.028(2) 0.001(2) C(7) 0.061(3) 0.047(2) 0.057(2) 0.001(2) 0.020(2) -0.004(2) C(8) 0.049(3) 0.074(3) 0.040(2) 0.014(2) 0.008(2) -0.008(2) C(9) 0.059(3) 0.079(4) 0.051(2) 0.012(3) 0.008(2) -0.012(2) C(10) 0.070(3) 0.089(4) 0.057(3) 0.025(3) -0.003(2) -0.025(3) C(10') 0.099(5) 0.100(5) 0.096(4) 0.016(4) 0.000(3) -0.046(4) C(11) 0.078(4) 0.111(5) 0.042(2) 0.042(4) 0.002(2) -0.019(3) C(12) 0.085(4) 0.113(5) 0.041(2) 0.029(4) 0.023(2) 0.002(3) C(13) 0.070(3) 0.077(3) 0.042(2) 0.018(3) 0.014(2) 0.003(2) C(21) 0.090(4) 0.049(3) 0.065(3) -0.002(3) 0.039(3) -0.002(2) C(31) 0.059(3) 0.055(3) 0.064(3) -0.003(2) 0.013(2) -0.004(2) C(41) 0.061(3) 0.070(3) 0.059(3) 0.008(2) 0.016(2) 0.003(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_thermal_displace_type Sn 0.29093(2) 0.29113(3) 0.235520(10) 0.04819(8) Uij O(1) 0.3224(2) 0.1550(3) 0.18053(9) 0.0563(9) Uij O(2) 0.2442(2) -0.0300(3) 0.20570(9) 0.0581(9) Uij O(3) 0.4773(3) -0.2629(4) -0.05760(10) 0.0830(10) Uij N(1) 0.3901(3) -0.2640(4) 0.01680(10) 0.0530(10) Uij N(2) 0.3595(3) -0.3885(4) 0.01110(10) 0.0530(10) Uij C(1) 0.2939(3) 0.0262(4) 0.17740(10) 0.0460(10) Uij C(2) 0.3226(3) -0.0526(4) 0.13640(10) 0.0440(10) Uij C(3) 0.2904(3) -0.1907(4) 0.12820(10) 0.0540(10) Uij C(4) 0.3123(4) -0.2635(5) 0.08980(10) 0.0570(10) Uij C(5) 0.3655(3) -0.1980(5) 0.05820(10) 0.0490(10) Uij C(6) 0.3989(3) -0.0614(5) 0.06610(10) 0.0580(10) Uij C(7) 0.3771(3) 0.0111(4) 0.10500(10) 0.0540(10) Uij C(8) 0.3854(3) -0.4552(5) -0.02890(10) 0.0540(10) Uij C(9) 0.3512(3) -0.5928(5) -0.03480(10) 0.0630(10) Uij C(10) 0.3707(4) -0.6756(6) -0.0720(2) 0.073(2) Uij C(10') 0.3313(5) -0.8228(7) -0.0783(2) 0.100(2) Uij C(11) 0.4277(4) -0.6137(7) -0.1033(2) 0.078(2) Uij C(12) 0.4631(4) -0.4783(7) -0.0983(2) 0.078(2) Uij C(13) 0.4427(4) -0.3952(6) -0.06120(10) 0.0630(10) Uij C(21) 0.3601(4) 0.4560(5) 0.2023(2) 0.0650(10) Uij C(31) 0.1277(3) 0.2779(5) 0.2245(2) 0.0590(10) Uij C(41) 0.3866(3) 0.1874(5) 0.29020(10) 0.0630(10) Uij H(1) 0.4478 -0.2280 -0.0265 0.0834 Uij H(3) 0.2517 -0.2365 0.1501 0.0645 Uij H(4) 0.2904 -0.3603 0.0849 0.0678 Uij H(6) 0.4379 -0.0160 0.0443 0.0694 Uij H(7) 0.4003 0.1072 0.1101 0.0645 Uij H(9) 0.3121 -0.6326 -0.0120 0.0755 Uij H(10a) 0.2570 -0.8221 -0.0818 0.1196 Uij H(10b) 0.3533 -0.8632 -0.1061 0.1196 Uij H(10c) 0.3583 -0.8784 -0.0512 0.1196 Uij H(11) 0.4432 -0.6682 -0.1297 0.0932 Uij H(12) 0.5030 -0.4400 -0.1210 0.0942 Uij H(21a) 0.4309 0.4319 0.2002 0.0786 Uij H(21b) 0.3232 0.4701 0.1711 0.0786 Uij H(21c) 0.3581 0.5415 0.2203 0.0786 Uij H(31a) 0.1000 0.3361 0.2472 0.0708 Uij H(31b) 0.1017 0.3102 0.1932 0.0708 Uij H(31c) 0.1070 0.1812 0.2280 0.0708 Uij H(41a) 0.3638 0.0911 0.2923 0.0751 Uij H(41b) 0.4569 0.1882 0.2837 0.0751 Uij H(41c) 0.3829 0.2353 0.3195 0.0751 Uij loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0.003 0.002 'International Tables' H 0.000 0.000 'International Tables' N 0.006 0.003 'International Tables' O 0.011 0.006 'International Tables' Sn -0.654 1.425 'International Tables' loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 2 4 0 2 6 1 1 7 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 O(1) Sn O(2) 6_555 174.30(10) yes O(1) Sn C(21) ? 88.30(10) yes O(1) Sn C(31) ? 98.70(10) yes O(1) Sn C(41) ? 96.50(10) yes O(2) Sn C(21) ? 86.30(10) yes O(2) Sn C(31) ? 82.00(10) yes O(2) Sn C(41) ? 87.70(10) yes C(21) Sn C(31) ? 117.9(2) yes C(21) Sn C(41) ? 115.9(2) yes C(31) Sn C(41) ? 124.2(2) yes Sn O(1) C(1) ? 123.2(2) yes Sn O(2) C(1) ? 155.6(3) yes N(2) N(1) C(5) ? 114.8(3) yes N(1) N(2) C(8) ? 115.1(4) yes O(1) C(1) O(2) ? 122.8(4) yes O(1) C(1) C(2) ? 115.6(3) yes O(2) C(1) C(2) ? 121.6(4) yes C(1) C(2) C(3) ? 120.2(4) no C(1) C(2) C(7) ? 121.1(4) no C(3) C(2) C(7) ? 118.6(4) no C(2) C(3) C(4) ? 121.3(4) no C(3) C(4) C(5) ? 119.5(4) no N(1) C(5) C(4) ? 123.6(4) no N(1) C(5) C(6) ? 116.6(4) no C(4) C(5) C(6) ? 119.8(4) no C(5) C(6) C(7) ? 120.4(4) no C(2) C(7) C(6) ? 120.3(4) no N(2) C(8) C(9) ? 114.5(4) no N(2) C(8) C(13) ? 125.5(5) no C(9) C(8) C(13) ? 119.9(4) no C(8) C(9) C(10) ? 122.6(5) no C(9) C(10) C(10') ? 121.8(5) no C(9) C(10) C(11) ? 116.2(5) no C(10') C(10) C(11) ? 121.9(5) no C(10) C(11) C(12) ? 122.5(4) no C(11) C(12) C(13) ? 121.2(5) no O(3) C(13) C(8) ? 122.7(4) no O(3) C(13) C(12) ? 119.7(5) no C(8) C(13) C(12) ? 117.6(5) 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 Sn O(1) ? 2.139(3) yes Sn O(2) 6_555 2.497(3) yes Sn C(21) ? 2.115(4) yes Sn C(31) ? 2.131(4) yes Sn C(41) ? 2.119(4) yes O(1) C(1) ? 1.283(5) yes O(2) C(1) ? 1.241(4) yes O(3) C(13) ? 1.340(6) yes N(1) N(2) ? 1.255(5) yes N(1) C(5) ? 1.430(5) yes N(2) C(8) ? 1.405(5) yes C(1) C(2) ? 1.497(5) yes C(2) C(3) ? 1.393(5) no C(2) C(7) ? 1.378(5) no C(3) C(4) ? 1.377(5) no C(4) C(5) ? 1.378(5) no C(5) C(6) ? 1.383(6) no C(6) C(7) ? 1.384(5) no C(8) C(9) ? 1.389(6) no C(8) C(13) ? 1.404(6) no C(9) C(10) ? 1.389(6) no C(10) C(10') ? 1.498(8) no C(10) C(11) ? 1.387(7) no C(11) C(12) ? 1.372(8) no C(12) C(13) ? 1.389(6) no