#------------------------------------------------------------------------------ #$Date: 2017-01-19 16:22:45 +0000 (Thu, 19 Jan 2017) $ #$Revision: 190732 $ #$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 ; Adding the _atom_site_type_symbol data item. Antanas Vaitkus, 2017-01-19 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_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type Sn Sn 1.00000 0.00000 1.00000 0.0286(3) Uij Cl Cl 1.22355(18) -0.01780(6) 0.81218(17) 0.0440(7) Uij N1 N 0.9368(5) 0.2903(2) 1.1277(4) 0.034(2) Uij C2 C 0.9341(7) 0.3297(2) 0.9839(5) 0.035(2) Uij N3 N 0.9294(5) 0.3055(1) 0.8145(4) 0.031(2) Uij C4 C 0.9296(5) 0.2329(2) 0.7933(5) 0.027(2) Uij C5 C 0.9344(5) 0.1873(2) 0.9390(5) 0.026(2) Uij C6 C 0.9342(5) 0.2172(2) 1.1105(5) 0.029(2) Uij N7 N 0.9378(5) 0.1184(1) 0.8742(4) 0.030(2) Uij C8 C 0.9315(6) 0.1291(2) 0.6959(5) 0.035(3) Uij N9 N 0.9261(5) 0.1970(2) 0.6380(4) 0.034(2) Uij C10 C 0.7542(7) -0.0353(2) 0.7583(6) 0.041(3) Uij N11 N 0.9320(6) 0.1797(2) 1.2576(5) 0.039(2) Uij C12 C 0.9176(8) 0.3534(2) 0.6560(6) 0.044(3) Uij H2 H 0.943(7) 0.375(3) 1.001(5) 0.045(12) Uiso H8 H 0.937(6) 0.092(2) 0.628(5) 0.032(10) Uiso H10a H 0.718(8) -0.078(3) 0.743(7) 0.069(16) Uiso H10b H 0.795(9) -0.034(4) 0.652(9) 0.090(19) Uiso H10c H 0.645(12) -0.011(3) 0.765(11) 0.076(23) Uiso HN11a H 0.915(8) 0.134(3) 1.259(7) 0.068(16) Uiso HN11b H 0.900(7) 0.201(3) 1.354(6) 0.052(13) Uiso H12a H 0.887(10) 0.403(3) 0.684(8) 0.097(20) Uiso H12b H 1.006(8) 0.347(3) 0.612(7) 0.054(14) Uiso H12c H 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