#------------------------------------------------------------------------------ #$Date: 2013-12-28 13:58:47 +0000 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/89/2008955.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_2008955 loop_ _publ_author_name 'Ng, Seik Weng' _publ_section_title ; 2,2'-Iminodipyridinium(1+) dichlorotriphenylstannate and 2,2'-iminodipyridinium(1+) tricyclohexylbis(trifluoroacetato)stannate ; _journal_issue 9 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first IUC9900098 _journal_volume 55 _journal_year 1999 _chemical_formula_iupac '(C10 H10 N3) [Sn Cl2 (C6 H5)3]' _chemical_formula_moiety '(C10 H10 N3) +, [(C6 H5)3 Cl2 Sn] -' _chemical_formula_sum 'C28 H25 Cl2 N3 Sn' _chemical_formula_weight 593.10 _chemical_name_systematic ; 2,2'-Iminodipyridinium(1+) dichlorotriphenylstannate ; _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' _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 91.443(9) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 16.2830(10) _cell_length_b 10.6940(10) _cell_length_c 15.038(2) _cell_measurement_reflns_used 25 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 13.0 _cell_measurement_theta_min 12.0 _cell_volume 2617.7(5) _computing_cell_refinement 'CELDIM (Enraf-Nonius, 1988)' _computing_data_collection 'CAD-4/PC (Kretschmar, 1994)' _computing_data_reduction 'XCAD4 (Harms, 1997)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997b)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997a)' _diffrn_ambient_temperature 298(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Enraf-Nonius CAD-4' _diffrn_measurement_method \w _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 0.0241 _diffrn_reflns_av_sigmaI/netI 0.0264 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 4787 _diffrn_reflns_theta_full 24.97 _diffrn_reflns_theta_max 24.97 _diffrn_reflns_theta_min 2.28 _diffrn_standards_decay_% 2 _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.201 _exptl_absorpt_correction_T_max 0.597 _exptl_absorpt_correction_T_min 0.500 _exptl_absorpt_correction_type '\y scan' _exptl_absorpt_process_details '(North et al., 1968) in WinGX (Farrugia, 1998)' _exptl_crystal_colour Colourless _exptl_crystal_density_diffrn 1.505 _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'Triangular block' _exptl_crystal_F_000 1192 _exptl_crystal_size_max 0.57 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.43 _refine_diff_density_max 2.116 _refine_diff_density_min -0.758 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.141 _refine_ls_hydrogen_treatment 'constr, U(H) = 1.5U~eq~(C,N)' _refine_ls_matrix_type full _refine_ls_number_parameters 130 _refine_ls_number_reflns 2302 _refine_ls_number_restraints 11 _refine_ls_restrained_S_all 1.141 _refine_ls_R_factor_all 0.0513 _refine_ls_R_factor_gt 0.0484 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0738P)^2^+17.8556P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.1449 _reflns_number_gt 2150 _reflns_number_total 2302 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file qa0153.cif _[local]_cod_data_source_block ipt170 _[local]_cod_cif_authors_sg_H-M 'C 2/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 ; _cod_database_code 2008955 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -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 0.5000 0.15646(5) 0.2500 0.0348(2) Uani d S 1 . . Sn Cl1 0.49080(10) 0.1728(2) 0.42350(10) 0.0537(4) Uani d . 1 . . Cl N1 0.3146(7) 0.2314(9) 0.4920(5) 0.053(3) Uani d PD 0.50 A -1 N N2 0.1941(9) 0.1390(10) 0.5342(7) 0.072(5) Uani d PGD 0.50 A -1 N N2' 0.2116(8) 0.3780(10) 0.4897(7) 0.056(3) Uani d PGD 0.50 A -1 C C1 0.6139(3) 0.2530(5) 0.2618(4) 0.0380(10) Uani d . 1 . . C C2 0.6238(5) 0.3622(6) 0.3126(5) 0.056(2) Uani d . 1 . . C C3 0.7001(5) 0.4168(8) 0.3228(5) 0.069(2) Uani d . 1 . . C C4 0.7667(5) 0.3675(8) 0.2823(6) 0.071(2) Uani d . 1 . . C C5 0.7596(4) 0.2599(7) 0.2354(5) 0.061(2) Uani d . 1 . . C C6 0.6829(4) 0.2037(7) 0.2242(4) 0.0490(10) Uani d . 1 . . C C7 0.5000 -0.0459(8) 0.2500 0.041(2) Uani d S 1 . . C C8 0.4962(4) -0.1108(7) 0.1714(4) 0.0490(10) Uani d . 1 . . C C9 0.4968(5) -0.2412(7) 0.1715(5) 0.063(2) Uani d . 1 . . C C10 0.5000 -0.3070(10) 0.2500 0.066(3) Uani d S 1 . . C C11 0.2776(9) 0.1300(10) 0.5179(6) 0.072(5) Uani d PGD 0.50 A -1 C C12 0.3182(6) 0.017(2) 0.5294(7) 0.072(5) Uani d PGD 0.50 A -1 C C13 0.2753(9) -0.0880(10) 0.5573(7) 0.072(5) Uani d PGD 0.50 A -1 C C14 0.1918(9) -0.0790(10) 0.5736(8) 0.072(5) Uani d PGD 0.50 A -1 C C15 0.1513(6) 0.034(2) 0.5621(8) 0.072(5) Uani d PGD 0.50 A -1 C C11' 0.2935(8) 0.3472(7) 0.4776(7) 0.056(3) Uani d PGD 0.50 A -1 N C12' 0.3481(6) 0.4370(10) 0.4483(7) 0.056(3) Uani d PGD 0.50 A -1 C C13' 0.3208(7) 0.5580(10) 0.4312(6) 0.056(3) Uani d PGD 0.50 A -1 C C14' 0.2389(8) 0.5891(8) 0.4433(7) 0.056(3) Uani d PGD 0.50 A -1 C C15' 0.1843(6) 0.4990(10) 0.4725(7) 0.056(3) Uani d PGD 0.50 A -1 C H2 0.5787 0.3980 0.3395 0.083 Uiso calc R 1 . . H H3 0.7062 0.4880 0.3578 0.104 Uiso calc R 1 . . H H4 0.8172 0.4080 0.2869 0.107 Uiso calc R 1 . . H H5 0.8057 0.2236 0.2108 0.091 Uiso calc R 1 . . H H6 0.6782 0.1310 0.1904 0.073 Uiso calc R 1 . . H H8 0.4932 -0.0676 0.1177 0.074 Uiso calc R 1 . . H H9 0.4949 -0.2843 0.1178 0.094 Uiso calc R 1 . . H H10 0.5000 -0.3937 0.2500 0.100 Uiso calc SR 1 . . H H1 0.3657 0.2185 0.4819 0.080 Uiso calc PR 0.50 A -1 H H12 0.3740 0.0108 0.5185 0.107 Uiso calc PR 0.50 A -1 H H13 0.3024 -0.1640 0.5650 0.107 Uiso calc PR 0.50 A -1 H H14 0.1631 -0.1494 0.5923 0.107 Uiso calc PR 0.50 A -1 H H15 0.0954 0.0399 0.5731 0.107 Uiso calc PR 0.50 A -1 H H2a 0.1690 0.2089 0.5271 0.107 Uiso calc PR 0.50 A -1 H H12' 0.4029 0.4167 0.4402 0.084 Uiso calc PR 0.50 A -1 H H13' 0.3573 0.6187 0.4117 0.084 Uiso calc PR 0.50 A -1 H H14' 0.2206 0.6701 0.4319 0.084 Uiso calc PR 0.50 A -1 H H15' 0.1295 0.5196 0.4806 0.084 Uiso calc PR 0.50 A -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 0.0253(3) 0.0365(3) 0.0427(3) 0.000 0.0017(2) 0.000 Cl1 0.0573(9) 0.0680(10) 0.0362(8) 0.0090(7) 0.0081(6) 0.0010(6) N1 0.044(6) 0.066(7) 0.051(6) 0.008(5) 0.010(5) 0.004(5) N2 0.076(7) 0.070(7) 0.069(7) 0.006(4) -0.004(4) 0.014(4) N2' 0.072(6) 0.044(5) 0.051(5) 0.002(3) 0.000(3) 0.006(3) C1 0.033(3) 0.036(3) 0.043(3) -0.002(2) 0.000(2) 0.004(2) C2 0.057(4) 0.052(4) 0.057(4) -0.003(3) 0.006(3) -0.005(3) C3 0.078(5) 0.058(4) 0.071(5) -0.021(4) -0.004(4) -0.009(4) C4 0.049(4) 0.078(5) 0.086(5) -0.024(4) -0.009(4) 0.016(4) C5 0.033(3) 0.070(5) 0.079(5) -0.002(3) 0.005(3) 0.010(4) C6 0.038(3) 0.055(4) 0.053(3) 0.000(3) 0.005(3) 0.001(3) C7 0.032(4) 0.040(4) 0.050(5) 0.000 0.002(3) 0.000 C8 0.047(3) 0.049(3) 0.051(4) 0.004(3) 0.002(3) -0.003(3) C9 0.067(5) 0.052(4) 0.070(5) 0.001(3) -0.005(4) -0.013(3) C10 0.074(7) 0.038(5) 0.087(8) 0.000 -0.009(6) 0.000 C11 0.076(7) 0.070(7) 0.069(7) 0.006(4) -0.004(4) 0.014(4) C12 0.076(7) 0.070(7) 0.069(7) 0.006(4) -0.004(4) 0.014(4) C13 0.076(7) 0.070(7) 0.069(7) 0.006(4) -0.004(4) 0.014(4) C14 0.076(7) 0.070(7) 0.069(7) 0.006(4) -0.004(4) 0.014(4) C15 0.076(7) 0.070(7) 0.069(7) 0.006(4) -0.004(4) 0.014(4) C11' 0.072(6) 0.044(5) 0.051(5) 0.002(3) 0.000(3) 0.006(3) C12' 0.072(6) 0.044(5) 0.051(5) 0.002(3) 0.000(3) 0.006(3) C13' 0.072(6) 0.044(5) 0.051(5) 0.002(3) 0.000(3) 0.006(3) C14' 0.072(6) 0.044(5) 0.051(5) 0.002(3) 0.000(3) 0.006(3) C15' 0.072(6) 0.044(5) 0.051(5) 0.002(3) 0.000(3) 0.006(3) 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 . 2.127(5) yes Sn1 C1 2_655 2.127(5) yes Sn1 C7 . 2.164(8) yes Sn1 Cl1 . 2.622(2) yes Sn1 Cl1 2_655 2.622(2) yes C1 C6 . 1.375(8) no C1 C2 . 1.403(9) no C2 C3 . 1.380(10) no C3 C4 . 1.360(10) no C4 C5 . 1.350(10) no C5 C6 . 1.392(9) no C7 C8 . 1.371(8) no C7 C8 2_655 1.371(8) no C8 C9 . 1.400(10) no C9 C10 . 1.373(9) no C10 C9 2_655 1.373(9) no N1 C11' . 1.300(10) no N1 C11 . 1.310(10) no C11 C12 . 1.3900 no C11 N2 . 1.3900 no C12 C13 . 1.3900 no C13 C14 . 1.3900 no C14 C15 . 1.3900 no C15 N2 . 1.3900 no C11' C12' . 1.3900 no C11' N2' . 1.3900 no C12' C13' . 1.3900 no C13' C14' . 1.3900 no C14' C15' . 1.3900 no C15' N2' . 1.3900 no 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' Cl Cl 0.1484 0.1585 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C1 Sn1 C1 . 2_655 121.9(3) yes C1 Sn1 C7 . . 119.0(2) yes C1 Sn1 Cl1 . . 87.5(2) yes C1 Sn1 Cl1 . 2_655 88.8(2) yes C1 Sn1 C7 2_655 . 119.0(2) yes C1 Sn1 Cl1 2_655 . 88.8(2) yes C1 Sn1 Cl1 2_655 2_655 87.5(2) yes C7 Sn1 Cl1 . . 93.80(10) yes C7 Sn1 Cl1 . 2_655 93.80(10) yes Cl1 Sn1 Cl1 . 2_655 172.30(10) yes C6 C1 C2 . . 117.4(6) no C6 C1 Sn1 . . 119.9(4) no C2 C1 Sn1 . . 122.5(4) no C3 C2 C1 . . 120.3(7) no C4 C3 C2 . . 120.8(7) no C5 C4 C3 . . 120.2(7) no C4 C5 C6 . . 119.7(7) no C5 C6 C1 . . 121.6(7) no C8 C7 C8 . 2_655 119.2(8) no C8 C7 Sn1 . . 120.4(4) no C8 C7 Sn1 2_655 . 120.4(4) no C7 C8 C9 . . 120.3(7) no C10 C9 C8 . . 120.8(7) no C9 C10 C9 2_655 . 119.0(10) no C11' N1 C11 . . 136.0(10) no N1 C11 C12 . . 123.0(10) no N1 C11 N2 . . 117.0(10) no C12 C11 N2 . . 120.0 no C11 C12 C13 . . 120.0 no C12 C13 C14 . . 120.0 no C15 C14 C13 . . 120.0 no C14 C15 N2 . . 120.0 no C15 N2 C11 . . 120.0 no N1 C11' C12' . . 123.0(10) no N1 C11' N2' . . 117.0(10) no C12' C11' N2' . . 120.0 no C11' C12' C13' . . 120.0 no C12' C13' C14' . . 120.0 no C15' C14' C13' . . 120.0 no C14' C15' N2' . . 120.0 no C15' N2' C11' . . 120.0 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag N1 H1 Cl1 0.86 2.29 3.320(10) 167 no _journal_paper_doi 10.1107/S0108270199098923