#------------------------------------------------------------------------------ #$Date: 2010-01-30 15:59:17 +0200 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/1100685.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100685 _chemical_formula_moiety 'C7 H7 N1 O7 Sn1 2(H2 O)' _chemical_formula_sum 'C7 H11 N O9 Sn' _chemical_formula_weight 371.86 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' 'N' 'N' 0.0061 0.0033 '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' _symmetry_cell_setting 'Triclinic' _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.5534(13) _cell_length_b 7.4907(15) _cell_length_c 12.030(2) _cell_angle_alpha 85.42(3) _cell_angle_beta 82.92(3) _cell_angle_gamma 74.83(3) _cell_volume 564.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 10.0 _cell_measurement_theta_max 15.0 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.186 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 364 _exptl_absorpt_coefficient_mu 2.305 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.25 _exptl_absorpt_correction_T_max 0.49 _exptl_absorpt_process_details 'North et al. (1968)' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens P3/PC' _diffrn_measurement_method '\q/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3258 _diffrn_reflns_av_R_equivalents 0.0288 _diffrn_reflns_av_sigmaI/netI 0.0337 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 29.06 _reflns_number_total 3008 _reflns_number_gt 2641 _reflns_threshold_expression 'I>2\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1161P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'difmap and geom' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3008 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0608 _refine_ls_R_factor_gt 0.0528 _refine_ls_wR_factor_ref 0.1400 _refine_ls_wR_factor_gt 0.1371 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 1.00563(4) 0.43188(4) -0.13313(2) 0.02346(14) Uani 1 1 d . . . O1 O 1.3169(6) 0.2358(6) -0.1831(3) 0.0313(8) Uani 1 1 d . . . O2 O 1.5301(6) 0.0669(7) -0.3163(4) 0.0444(11) Uani 1 1 d . . . O3 O 0.6890(6) 0.5563(6) -0.1965(3) 0.0351(9) Uani 1 1 d . . . O4 O 0.4794(6) 0.5761(7) -0.3322(4) 0.0402(10) Uani 1 1 d . . . O5 O 0.9080(7) 0.2016(6) -0.0751(4) 0.0381(9) Uani 1 1 d . . . H5 H 0.7893 0.1923 -0.0323 0.050 Uiso 1 1 d . . . O6 O 0.8198(6) 0.5851(5) -0.0029(3) 0.0312(8) Uani 1 1 d . . . H6 H 0.7020 0.6615 -0.0183 0.050 Uiso 1 1 d . . . C1 C 1.3602(8) 0.1711(7) -0.2810(4) 0.0275(9) Uani 1 1 d . . . C2 C 1.1844(7) 0.2289(7) -0.3549(4) 0.0245(9) Uani 1 1 d . . . C3 C 1.1918(9) 0.1709(8) -0.4627(5) 0.0343(11) Uani 1 1 d . . . H3A H 1.3156 0.0951 -0.4970 0.041 Uiso 1 1 calc R . . C4 C 1.0109(10) 0.2287(9) -0.5178(5) 0.0378(12) Uani 1 1 d . . . H4A H 1.0124 0.1911 -0.5898 0.045 Uiso 1 1 calc R . . C5 C 0.8278(9) 0.3420(8) -0.4665(4) 0.0303(10) Uani 1 1 d . . . H5A H 0.7051 0.3810 -0.5027 0.036 Uiso 1 1 calc R . . C6 C 0.8329(7) 0.3958(7) -0.3591(4) 0.0237(8) Uani 1 1 d . . . C7 C 0.6492(7) 0.5198(7) -0.2923(4) 0.0272(9) Uani 1 1 d . . . N1 N 1.0062(6) 0.3394(5) -0.3073(3) 0.0213(7) Uani 1 1 d . . . O1W O 1.1001(7) 0.6501(5) -0.2047(4) 0.0353(8) Uani 1 1 d . . . H1WA H 1.2276 0.6718 -0.2270 0.050 Uiso 1 1 d . . . H1WB H 1.0520 0.7746 -0.2121 0.050 Uiso 1 1 d . . . O2W O 0.4300(9) 0.8390(7) -0.0643(5) 0.0543(12) Uani 1 1 d . . . H2WB H 0.3995 0.9564 -0.0923 0.050 Uiso 1 1 d . . . H2WA H 0.5149 0.7475 -0.1074 0.050 Uiso 1 1 d . . . O3W O 0.1141(8) 0.0184(6) 0.2124(5) 0.0509(12) Uani 1 1 d . . . H3WA H 0.2351 0.0103 0.2422 0.050 Uiso 1 1 d . . . H3WB H 0.1060 -0.0621 0.1629 0.050 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.02317(19) 0.0306(2) 0.01369(19) -0.01007(12) -0.00131(11) 0.00067(12) O1 0.0271(17) 0.042(2) 0.0190(17) -0.0121(15) -0.0036(13) 0.0046(14) O2 0.031(2) 0.056(3) 0.036(2) -0.021(2) -0.0045(17) 0.0141(18) O3 0.0254(16) 0.054(2) 0.0197(17) -0.0167(16) -0.0028(13) 0.0053(15) O4 0.0256(18) 0.064(3) 0.025(2) -0.0120(18) -0.0056(14) 0.0028(17) O5 0.044(2) 0.040(2) 0.029(2) -0.0098(16) 0.0011(17) -0.0087(17) O6 0.0246(16) 0.044(2) 0.0175(17) -0.0185(15) -0.0037(13) 0.0099(14) C1 0.027(2) 0.032(2) 0.018(2) -0.0101(17) -0.0003(17) 0.0042(18) C2 0.025(2) 0.028(2) 0.016(2) -0.0088(17) -0.0003(16) 0.0018(17) C3 0.036(3) 0.043(3) 0.020(2) -0.014(2) -0.001(2) 0.000(2) C4 0.046(3) 0.053(3) 0.013(2) -0.014(2) -0.005(2) -0.006(3) C5 0.033(2) 0.043(3) 0.015(2) -0.0071(19) -0.0059(18) -0.005(2) C6 0.025(2) 0.031(2) 0.0124(19) -0.0065(16) -0.0007(16) -0.0022(17) C7 0.021(2) 0.040(3) 0.018(2) -0.0066(19) -0.0024(16) -0.0028(18) N1 0.0217(17) 0.0237(17) 0.0156(18) -0.0052(14) 0.0006(14) -0.0006(14) O1W 0.0337(19) 0.0306(18) 0.038(2) -0.0060(16) 0.0051(16) -0.0038(15) O2W 0.058(3) 0.048(3) 0.045(3) -0.005(2) 0.009(2) 0.002(2) O3W 0.052(3) 0.039(2) 0.061(3) -0.012(2) -0.021(2) 0.000(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 O1W 1.992(4) . ? Sn1 O5 2.036(4) . ? Sn1 O6 2.084(3) . ? Sn1 O6 2.086(4) 2_765 ? Sn1 O1 2.225(4) . ? Sn1 O3 2.241(4) . ? Sn1 N1 2.258(4) . ? O1 C1 1.281(6) . ? O2 C1 1.229(6) . ? O3 C7 1.277(6) . ? O4 C7 1.226(6) . ? O6 Sn1 2.086(4) 2_765 ? C1 C2 1.495(7) . ? C2 N1 1.335(6) . ? C2 C3 1.391(7) . ? C3 C4 1.382(8) . ? C4 C5 1.381(8) . ? C5 C6 1.391(6) . ? C6 N1 1.319(6) . ? C6 C7 1.501(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1W Sn1 O5 174.52(16) . . ? O1W Sn1 O6 92.57(17) . . ? O5 Sn1 O6 91.75(17) . . ? O1W Sn1 O6 92.94(18) . 2_765 ? O5 Sn1 O6 91.72(18) . 2_765 ? O6 Sn1 O6 69.56(16) . 2_765 ? O1W Sn1 O1 92.91(16) . . ? O5 Sn1 O1 85.48(17) . . ? O6 Sn1 O1 144.74(14) . . ? O6 Sn1 O1 75.39(14) 2_765 . ? O1W Sn1 O3 87.99(18) . . ? O5 Sn1 O3 89.93(18) . . ? O6 Sn1 O3 74.57(14) . . ? O6 Sn1 O3 144.13(14) 2_765 . ? O1 Sn1 O3 140.42(14) . . ? O1W Sn1 N1 87.76(16) . . ? O5 Sn1 N1 86.76(16) . . ? O6 Sn1 N1 144.39(14) . . ? O6 Sn1 N1 146.01(14) 2_765 . ? O1 Sn1 N1 70.65(14) . . ? O3 Sn1 N1 69.85(14) . . ? C1 O1 Sn1 121.2(3) . . ? C7 O3 Sn1 121.6(3) . . ? Sn1 O6 Sn1 110.44(16) . 2_765 ? O2 C1 O1 125.2(5) . . ? O2 C1 C2 119.4(5) . . ? O1 C1 C2 115.3(4) . . ? N1 C2 C3 120.1(5) . . ? N1 C2 C1 114.2(4) . . ? C3 C2 C1 125.6(4) . . ? C4 C3 C2 118.5(5) . . ? C3 C4 C5 120.4(5) . . ? C4 C5 C6 117.9(5) . . ? N1 C6 C5 121.2(5) . . ? N1 C6 C7 114.1(4) . . ? C5 C6 C7 124.7(4) . . ? O4 C7 O3 126.2(5) . . ? O4 C7 C6 119.1(5) . . ? O3 C7 C6 114.7(4) . . ? C6 N1 C2 121.9(4) . . ? C6 N1 Sn1 119.6(3) . . ? C2 N1 Sn1 118.4(3) . . ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1W Sn1 O1 C1 -83.0(4) . . . . ? O5 Sn1 O1 C1 91.8(4) . . . . ? O6 Sn1 O1 C1 178.4(4) . . . . ? O6 Sn1 O1 C1 -175.3(5) 2_765 . . . ? O3 Sn1 O1 C1 7.4(6) . . . . ? N1 Sn1 O1 C1 3.6(4) . . . . ? O1W Sn1 O3 C7 90.3(5) . . . . ? O5 Sn1 O3 C7 -84.6(5) . . . . ? O6 Sn1 O3 C7 -176.5(5) . . . . ? O6 Sn1 O3 C7 -177.5(4) 2_765 . . . ? O1 Sn1 O3 C7 -1.8(6) . . . . ? N1 Sn1 O3 C7 2.0(4) . . . . ? O1W Sn1 O6 Sn1 -92.2(2) . . . 2_765 ? O5 Sn1 O6 Sn1 91.2(2) . . . 2_765 ? O6 Sn1 O6 Sn1 0.0 2_765 . . 2_765 ? O1 Sn1 O6 Sn1 6.5(4) . . . 2_765 ? O3 Sn1 O6 Sn1 -179.4(2) . . . 2_765 ? N1 Sn1 O6 Sn1 178.07(17) . . . 2_765 ? Sn1 O1 C1 O2 177.7(5) . . . . ? Sn1 O1 C1 C2 -3.0(7) . . . . ? O2 C1 C2 N1 178.8(5) . . . . ? O1 C1 C2 N1 -0.4(7) . . . . ? O2 C1 C2 C3 1.8(9) . . . . ? O1 C1 C2 C3 -177.5(5) . . . . ? N1 C2 C3 C4 -0.7(9) . . . . ? C1 C2 C3 C4 176.2(5) . . . . ? C2 C3 C4 C5 0.3(9) . . . . ? C3 C4 C5 C6 0.4(9) . . . . ? C4 C5 C6 N1 -0.5(8) . . . . ? C4 C5 C6 C7 179.3(5) . . . . ? Sn1 O3 C7 O4 177.4(5) . . . . ? Sn1 O3 C7 C6 -2.6(7) . . . . ? N1 C6 C7 O4 -178.3(5) . . . . ? C5 C6 C7 O4 1.8(8) . . . . ? N1 C6 C7 O3 1.7(7) . . . . ? C5 C6 C7 O3 -178.2(5) . . . . ? C5 C6 N1 C2 0.1(7) . . . . ? C7 C6 N1 C2 -179.7(4) . . . . ? C5 C6 N1 Sn1 179.8(4) . . . . ? C7 C6 N1 Sn1 0.0(6) . . . . ? C3 C2 N1 C6 0.5(8) . . . . ? C1 C2 N1 C6 -176.7(4) . . . . ? C3 C2 N1 Sn1 -179.2(4) . . . . ? C1 C2 N1 Sn1 3.6(6) . . . . ? O1W Sn1 N1 C6 -89.6(4) . . . . ? O5 Sn1 N1 C6 90.2(4) . . . . ? O6 Sn1 N1 C6 1.7(5) . . . . ? O6 Sn1 N1 C6 178.5(3) 2_765 . . . ? O1 Sn1 N1 C6 176.6(4) . . . . ? O3 Sn1 N1 C6 -0.9(3) . . . . ? O1W Sn1 N1 C2 90.1(4) . . . . ? O5 Sn1 N1 C2 -90.1(4) . . . . ? O6 Sn1 N1 C2 -178.6(3) . . . . ? O6 Sn1 N1 C2 -1.8(5) 2_765 . . . ? O1 Sn1 N1 C2 -3.7(3) . . . . ? O3 Sn1 N1 C2 178.8(4) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 29.06 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 3.248 _refine_diff_density_min -2.550 _refine_diff_density_rms 0.292 _cod_database_code 1100685