#------------------------------------------------------------------------------ #$Date: 2016-02-19 14:29:56 +0000 (Fri, 19 Feb 2016) $ #$Revision: 176759 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/60/2006025.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_2006025 loop_ _publ_author_name 'Hazell, A.' 'Ouyang, J.' 'Khoo, L. E.' _publ_contact_author ; Alan Hazell Department of Chemistry Aarhus University Langelandsgade 140 DK-8000 \%Arhus C Denmark ; _publ_section_title ; Dichlorodimethylbis(3-methyladenine-N^7^)tin(IV) ; _journal_issue 4 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 406 _journal_page_last 408 _journal_paper_doi 10.1107/S0108270196015132 _journal_volume 53 _journal_year 1997 _chemical_formula_moiety '[Sn Cl2 (C H3)2 (C6 H7 N5)2]' _chemical_formula_sum 'C14 H20 Cl2 N10 Sn' _chemical_formula_weight 518.0 _chemical_melting_point 297.0(10) _chemical_name_systematic ; bis(3-methyladenine)dichlorodimethyltin(IV) ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yab' _symmetry_space_group_name_H-M 'P 1 21/a 1' _atom_type_scat_source IntTabIV _cell_angle_alpha 90.0 _cell_angle_beta 113.078(14) _cell_angle_gamma 90.0 _cell_formula_units_Z 2 _cell_length_a 7.435(2) _cell_length_b 18.709(3) _cell_length_c 7.5618(13) _cell_measurement_reflns_used 60 _cell_measurement_temperature 294 _cell_measurement_theta_max 15.95 _cell_measurement_theta_min 12.00 _cell_volume 967.7(4) _computing_cell_refinement MAD _computing_data_collection 'MAD (Allibon, 1995)' _computing_data_reduction 'KRYSTAL (Hazell, 1995)' _computing_molecular_graphics 'ORTEPIII (Burnett & Johnson, 1996), KRYSTAL' _computing_publication_material KRYSTAL _computing_structure_refinement 'Modified ORFLS (1962), KRYSTAL' _computing_structure_solution 'SIR92 (Altomare et al., 1994), KRYSTAL' _diffrn_ambient_temperature 294 _diffrn_measurement_device 'Huber four-circle diffractometer' _diffrn_measurement_method \q/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'x-ray tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.079 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 1978 _diffrn_reflns_reduction_process 1899 _diffrn_reflns_theta_max 25.0 _diffrn_reflns_theta_min 2.0 _diffrn_standards_decay_% 3 _diffrn_standards_interval_count 50 _diffrn_standards_number 2 _exptl_absorpt_coefficient_mu 1.619 _exptl_absorpt_correction_T_max 0.766 _exptl_absorpt_correction_T_min 0.347 _exptl_absorpt_correction_type integration _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.778 _exptl_crystal_density_meas ? _exptl_crystal_description tabular _exptl_crystal_F_000 516 _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.70 _exptl_crystal_size_min 0.18 _refine_diff_density_max 1.2(2) _refine_diff_density_min -1.5(2) _refine_ls_extinction_coef 1.0(3)\\times10^3^ _refine_ls_extinction_method 'B -- C type 1 Lorentzian isotropic (Becker & Coppens, 1974)' _refine_ls_goodness_of_fit_obs 1.81 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 165 _refine_ls_number_reflns 1658 _refine_ls_R_factor_obs 0.043 _refine_ls_shift/esd_max 0.028 _refine_ls_shift/esd_mean 0.002 _refine_ls_structure_factor_coef F _refine_ls_weighting_details 'w = 1/{[\s~cs~(F^2^)+1.03F^2^]^1/2^-|F|}^2^' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_obs 0.054 _reflns_number_observed 1658 _reflns_number_total 1761 _reflns_observed_criterion I>0 _cod_data_source_file ab1424.cif _cod_data_source_block h43 _cod_depositor_comments ; The following automatic conversions were performed: '_chemical_melting_point' value '296-298' was changed to '297.0(10)' - the average value was taken and precision was estimated. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'not measured' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas The following automatic conversions were performed: '_refine_ls_weighting_scheme' value ' 1/{[\s~cs~(F^2^)+1.03F^2^]^1/2^-|F|}^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~cs~(F^2^)+1.03F^2^]^1/2^-|F|}^2^'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_sg_symbol_H-M 'P 21/a' _cod_database_code 2006025 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,-z -x,-y,-z 1/2+x,1/2-y,z loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 Sn 0.0286(3) -0.0018(1) 0.0196(2) 0.0160(3) -0.0016(1) 0.0324(3) Cl 0.0440(7) -0.0014(5) 0.0396(6) 0.0272(5) -0.0016(5) 0.0604(7) N1 0.034(2) 0.000(1) 0.021(2) 0.020(1) -0.003(1) 0.041(2) C2 0.035(2) 0.001(2) 0.019(2) 0.016(2) -0.003(1) 0.045(2) N3 0.031(2) 0.001(1) 0.021(1) 0.015(1) 0.004(1) 0.042(2) C4 0.027(2) 0.003(1) 0.018(2) 0.016(2) 0.001(1) 0.035(2) C5 0.026(2) 0.000(1) 0.014(1) 0.018(2) 0.001(1) 0.032(2) C6 0.029(2) 0.002(1) 0.018(2) 0.022(2) -0.001(1) 0.034(2) N7 0.030(2) 0.002(1) 0.022(1) 0.017(1) 0.000(1) 0.031(1) C8 0.035(3) 0.000(2) 0.025(2) 0.021(2) -0.002(1) 0.033(2) N9 0.034(2) 0.003(1) 0.024(1) 0.023(2) 0.001(1) 0.034(2) C10 0.041(3) -0.011(2) 0.018(2) 0.025(2) -0.005(2) 0.043(2) N11 0.039(2) 0.002(2) 0.031(2) 0.027(2) -0.001(1) 0.034(2) C12 0.044(3) 0.004(2) 0.030(2) 0.026(2) 0.014(2) 0.049(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 1.00000 0.00000 1.00000 0.0286(3) Uij Cl 1.22355(18) -0.01780(6) 0.81218(17) 0.0440(7) Uij N1 0.9368(5) 0.2903(2) 1.1277(4) 0.034(2) Uij C2 0.9341(7) 0.3297(2) 0.9839(5) 0.035(2) Uij N3 0.9294(5) 0.3055(1) 0.8145(4) 0.031(2) Uij C4 0.9296(5) 0.2329(2) 0.7933(5) 0.027(2) Uij C5 0.9344(5) 0.1873(2) 0.9390(5) 0.026(2) Uij C6 0.9342(5) 0.2172(2) 1.1105(5) 0.029(2) Uij N7 0.9378(5) 0.1184(1) 0.8742(4) 0.030(2) Uij C8 0.9315(6) 0.1291(2) 0.6959(5) 0.035(3) Uij N9 0.9261(5) 0.1970(2) 0.6380(4) 0.034(2) Uij C10 0.7542(7) -0.0353(2) 0.7583(6) 0.041(3) Uij N11 0.9320(6) 0.1797(2) 1.2576(5) 0.039(2) Uij C12 0.9176(8) 0.3534(2) 0.6560(6) 0.044(3) Uij H2 0.943(7) 0.375(3) 1.001(5) 0.045(12) Uiso H8 0.937(6) 0.092(2) 0.628(5) 0.032(10) Uiso H10a 0.718(8) -0.078(3) 0.743(7) 0.069(16) Uiso H10b 0.795(9) -0.034(4) 0.652(9) 0.090(19) Uiso H10c 0.645(12) -0.011(3) 0.765(11) 0.076(23) Uiso HN11a 0.915(8) 0.134(3) 1.259(7) 0.068(16) Uiso HN11b 0.900(7) 0.201(3) 1.354(6) 0.052(13) Uiso H12a 0.887(10) 0.403(3) 0.684(8) 0.097(20) Uiso H12b 1.006(8) 0.347(3) 0.612(7) 0.054(14) Uiso H12c 0.798(13) 0.337(4) 0.546(11) 0.138(29) Uiso loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 4 0 0 0 0 3 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 C10 Sn C10 . 3_757 180.0 no N7 Sn C10 . . 88.80(10) no N7 Sn C10 3_757 . 91.20(10) no Cl Sn C10 . . 90.50(10) no Cl Sn C10 3_757 . 89.50(10) no N7 Sn C10 . 3_757 91.20(10) no N7 Sn C10 3_757 3_757 88.80(10) no Cl Sn C10 . 3_757 89.50(10) no Cl Sn C10 3_757 3_757 90.50(10) no N7 Sn N7 . 3_757 180.0 no Cl Sn N7 . . 88.07(7) no Cl Sn N7 3_757 . 91.93(7) no Cl Sn N7 . 3_757 91.93(7) no Cl Sn N7 3_757 3_757 88.07(7) no Cl Sn Cl . 3_757 180.00 no Sn N7 C8 . . 117.6(2) yes Sn N7 C5 . . 138.8(2) yes C2 N1 C6 . . 119.2(3) no N1 C2 H2 . . 117(3) no N3 C2 H2 . . 117(3) no N1 C2 N3 . . 126.0(3) no C2 N3 C4 . . 116.4(3) no C2 N3 C12 . . 122.7(3) no C4 N3 C12 . . 120.8(3) no N3 C4 N9 . . 126.8(3) no C5 C4 N9 . . 111.9(3) yes N3 C4 C5 . . 121.3(3) no C4 C5 N7 . . 106.9(3) yes C6 C5 N7 . . 134.6(3) no C4 C5 C6 . . 118.5(3) no N1 C6 N11 . . 117.0(3) no C5 C6 N11 . . 124.5(3) no N1 C6 C5 . . 118.5(3) no C5 N7 C8 . . 102.6(3) yes N9 C8 H8 . . 124(3) no N7 C8 H8 . . 119(3) no N7 C8 N9 . . 117.0(3) yes C4 N9 C8 . . 101.6(3) yes H10a C10 H10c . . 103(5) no H10a C10 H10b . . 95(5) no H10b C10 H10c . . 126(6) no HN11a N11 HN11b . . 109(4) no C6 N11 HN11a . . 126(3) no C6 N11 HN11b . . 121(3) no H12b C12 H12c . . 101(6) no H12a C12 H12b . . 120(5) no N3 C12 H12b . . 115(3) no H12a C12 H12c . . 105(5) no N3 C12 H12c . . 104(4) no N3 C12 H12a . . 110(3) no loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Sn . Cl . 2.596(1) yes Sn . Cl 3_757 2.596(1) no Sn . N7 . 2.384(3) yes Sn . N7 3_757 2.384(3) no Sn . C10 . 2.121(4) yes Sn . C10 3_757 2.121(4) no N1 . C2 . 1.308(5) yes N1 . C6 . 1.372(4) yes C2 . H2 . 0.86(5) no C2 . N3 . 1.346(5) yes N3 . C4 . 1.367(4) yes N3 . C12 . 1.472(5) yes C4 . N9 . 1.344(4) yes C4 . C5 . 1.383(5) yes C5 . N7 . 1.383(4) yes C5 . C6 . 1.413(5) yes C6 . N11 . 1.321(5) yes N7 . C8 . 1.345(4) yes C8 . H8 . 0.87(4) no C8 . N9 . 1.338(5) yes C10 . H10a . 0.84(6) no C10 . H10c . 0.95(8) no C10 . H10b . 0.97(6) no N11 . HN11a . 0.87(6) no N11 . HN11b . 0.94(5) no C12 . H12b . 0.85(5) no C12 . H12c . 1.00(8) no C12 . H12a . 1.00(7) no