#------------------------------------------------------------------------------ #$Date: 2012-02-03 17:16:24 +0000 (Fri, 03 Feb 2012) $ #$Revision: 32112 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/12/2011212.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_2011212 loop_ _publ_author_name 'Casas, Jos\'e S.' 'Garc\'ia-Mart\'inez, Emilia' 'Garc\'ia-Tasende, Soledad' 'S\'anchez, Agust\'in' 'Sordo, Jos\'e' 'V\'azquez-L\'opez, Ezequiel M.' 'Vidarte, Mar\'ia Jos\'e' _publ_section_title ; Dichlorobis(3,5-dimethylpyrazole-N^2^)methylphenyltin(IV) ; _journal_issue 8 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 932 _journal_page_last 933 _journal_volume 56 _journal_year 2000 _chemical_formula_iupac '[SnCl2 (CH3 )(C6 H5 )(C5 H8 N2 )2 ]' _chemical_formula_moiety 'C17 H24 Cl2 N4 Sn' _chemical_formula_sum 'C17 H24 Cl2 N4 Sn' _chemical_formula_weight 473.99 _chemical_melting_point 457 _chemical_name_systematic ; ? ; _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 _cell_angle_beta 95.982(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 15.590(2) _cell_length_b 10.889(2) _cell_length_c 11.8700(10) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 36.40 _cell_measurement_theta_min 17.62 _cell_volume 2004.1(5) _computing_cell_refinement 'CAD4-Express Software' _computing_data_collection 'CAD4-Express Software (Nonius, 1994)' _computing_data_reduction 'HELENA (Spek, 1993)' _computing_molecular_graphics 'ZORTEP (Zolsnai & Huttner, 1997)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full .473 _diffrn_measured_fraction_theta_max .473 _diffrn_measurement_device_type 'Enraf Nonius MACH3' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .0164 _diffrn_reflns_av_sigmaI/netI .0436 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 2131 _diffrn_reflns_theta_full 26.28 _diffrn_reflns_theta_max 26.28 _diffrn_reflns_theta_min 2.63 _diffrn_standards_decay_% <1 _diffrn_standards_interval_time 120 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.548 _exptl_absorpt_correction_T_max .8010 _exptl_absorpt_correction_T_min .6983 _exptl_absorpt_correction_type '\y-scan (North et al., 1968)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.571 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Prism _exptl_crystal_F_000 952 _exptl_crystal_size_max .25 _exptl_crystal_size_mid .25 _exptl_crystal_size_min .15 _refine_diff_density_max .38 _refine_diff_density_min -.27 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 114 _refine_ls_number_reflns 2028 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.020 _refine_ls_R_factor_all .0516 _refine_ls_R_factor_gt .0273 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme 'calc w = 1/[\s^2^(Fo^2^)+(0.0211P)^2^+1.9268P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_wR_factor_ref .0626 _reflns_number_gt 1617 _reflns_number_total 2028 _reflns_threshold_expression >2\s(I) _[local]_cod_data_source_file gg1001.cif _[local]_cod_data_source_block I _[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 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_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2011212 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 .0000 .16014(3) .2500 .03192(10) Uani d S 1 . . Sn Cl1 -.05689(5) .15652(9) .03840(6) .0462(2) Uani d . 1 . . Cl C1 .0000 -.0352(4) .2500 .0511(13) Uani d S 1 . . C H1A -.0409 -.0646 .2988 .077 Uiso calc PR .50 . . H H1B .0565 -.0646 .2768 .077 Uiso calc PR .50 . . H H1C -.0156 -.0646 .1744 .077 Uiso calc PR .50 . . H N1 .13773(16) .1588(3) .1848(2) .0404(6) Uani d . 1 . . N N2 .15010(17) .0881(3) .0931(2) .0409(7) Uani d . 1 . . N H2 .1100 .0457 .0560 .049 Uiso calc R 1 . . H C3 .2313(2) .0920(3) .0675(3) .0440(8) Uani d . 1 . . C C4 .2740(2) .1671(4) .1463(3) .0547(9) Uani d . 1 . . C H4 .3322 .1875 .1512 .066 Uiso calc R 1 . . H C5 .2152(2) .2074(3) .2178(3) .0415(8) Uani d . 1 . . C C6 .2280(3) .2935(4) .3163(3) .0609(11) Uani d . 1 . . C H6A .2038 .3721 .2946 .091 Uiso calc R 1 . . H H6B .2885 .3024 .3394 .091 Uiso calc R 1 . . H H6C .1998 .2612 .3780 .091 Uiso calc R 1 . . H C7 .2610(3) .0230(4) -.0297(4) .0665(12) Uani d . 1 . . C H7A .2567 -.0636 -.0161 .100 Uiso calc R 1 . . H H7B .3199 .0439 -.0376 .100 Uiso calc R 1 . . H H7C .2255 .0441 -.0979 .100 Uiso calc R 1 . . H C11 .0000 .3563(4) .2500 .0329(10) Uani d S 1 . . C C12 .0270(2) .4211(3) .1598(3) .0436(8) Uani d . 1 . . C H12 .0451 .3788 .0984 .052 Uiso calc R 1 . . H C13 .0275(2) .5477(3) .1598(4) .0540(10) Uani d . 1 . . C H13 .0463 .5904 .0991 .065 Uiso calc R 1 . . H C14 .0000 .6109(5) .2500 .0584(16) Uani d S 1 . . C H14 .0000 .6963 .2500 .070 Uiso calc SR 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 .04015(18) .02860(16) .02741(16) .000 .00539(12) .000 Cl1 .0573(5) .0467(5) .0332(4) -.0007(4) -.0014(4) -.0070(4) C1 .078(4) .028(3) .050(3) .000 .023(3) .000 N1 .0421(14) .0448(15) .0351(14) -.0031(14) .0077(11) -.0057(14) N2 .0414(16) .0420(16) .0404(16) -.0029(13) .0088(13) -.0089(13) C3 .047(2) .0356(19) .052(2) .0027(16) .0167(17) .0049(17) C4 .0350(17) .059(2) .071(3) -.0023(19) .0077(17) .012(2) C5 .0442(19) .0370(17) .0421(19) -.0055(15) -.0017(15) .0064(15) C6 .067(3) .062(2) .052(2) -.021(2) -.002(2) -.005(2) C7 .077(3) .057(3) .073(3) .010(2) .044(2) .002(2) C11 .036(2) .030(2) .032(2) .000 -.0009(18) .000 C12 .050(2) .0407(19) .040(2) -.0004(16) .0052(16) .0037(16) C13 .054(2) .042(2) .065(3) -.0053(17) .005(2) .0161(19) C14 .051(3) .028(2) .093(5) .000 -.008(3) .000 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) y Sn1 C11 . 2.135(4) y Sn1 N1 2 2.357(3) ? Sn1 N1 . 2.357(3) y Sn1 Cl1 . 2.5753(8) y Sn1 Cl1 2 2.5753(8) ? C1 H1A . .9600 ? C1 H1B . .9600 ? C1 H1C . .9600 ? N1 C5 . 1.339(4) ? N1 N2 . 1.363(4) ? N2 C3 . 1.334(4) ? N2 H2 . .8600 ? C3 C4 . 1.363(5) ? C3 C7 . 1.490(5) ? C4 C5 . 1.384(5) ? C4 H4 . .9300 ? C5 C6 . 1.495(5) ? C6 H6A . .9600 ? C6 H6B . .9600 ? C6 H6C . .9600 ? C7 H7A . .9600 ? C7 H7B . .9600 ? C7 H7C . .9600 ? C11 C12 2 1.385(4) ? C11 C12 . 1.385(4) ? C12 C13 . 1.378(5) ? C12 H12 . .9300 ? C13 C14 . 1.378(5) ? C13 H13 . .9300 ? C14 C13 2 1.378(5) ? C14 H14 . .9300 ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl .1484 .1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -.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 C11 . . 180.0 y C1 Sn1 N1 . 2 89.64(7) ? C11 Sn1 N1 . 2 90.36(7) ? C1 Sn1 N1 . . 89.64(7) y C11 Sn1 N1 . . 90.36(7) y N1 Sn1 N1 2 . 179.28(14) y C1 Sn1 Cl1 . . 89.12(2) y C11 Sn1 Cl1 . . 90.88(2) y N1 Sn1 Cl1 2 . 95.00(7) ? N1 Sn1 Cl1 . . 84.99(7) y C1 Sn1 Cl1 . 2 89.12(2) ? C11 Sn1 Cl1 . 2 90.88(2) ? N1 Sn1 Cl1 2 2 84.99(7) ? N1 Sn1 Cl1 . 2 95.00(7) ? Cl1 Sn1 Cl1 . 2 178.24(4) y Sn1 C1 H1A . . 109.5 ? Sn1 C1 H1B . . 109.5 ? H1A C1 H1B . . 109.5 ? Sn1 C1 H1C . . 109.5 ? H1A C1 H1C . . 109.5 ? H1B C1 H1C . . 109.5 ? C5 N1 N2 . . 105.0(3) ? C5 N1 Sn1 . . 136.6(2) ? N2 N1 Sn1 . . 118.37(19) ? C3 N2 N1 . . 112.4(3) ? C3 N2 H2 . . 123.8 ? N1 N2 H2 . . 123.8 ? N2 C3 C4 . . 105.6(3) ? N2 C3 C7 . . 122.7(3) ? C4 C3 C7 . . 131.7(3) ? C3 C4 C5 . . 107.7(3) ? C3 C4 H4 . . 126.2 ? C5 C4 H4 . . 126.2 ? N1 C5 C4 . . 109.3(3) ? N1 C5 C6 . . 121.3(3) ? C4 C5 C6 . . 129.4(3) ? C5 C6 H6A . . 109.5 ? C5 C6 H6B . . 109.5 ? H6A C6 H6B . . 109.5 ? C5 C6 H6C . . 109.5 ? H6A C6 H6C . . 109.5 ? H6B C6 H6C . . 109.5 ? C3 C7 H7A . . 109.5 ? C3 C7 H7B . . 109.5 ? H7A C7 H7B . . 109.5 ? C3 C7 H7C . . 109.5 ? H7A C7 H7C . . 109.5 ? H7B C7 H7C . . 109.5 ? C12 C11 C12 2 . 118.7(4) ? C12 C11 Sn1 2 . 120.7(2) ? C12 C11 Sn1 . . 120.7(2) ? C13 C12 C11 . . 120.8(4) ? C13 C12 H12 . . 119.6 ? C11 C12 H12 . . 119.6 ? C14 C13 C12 . . 119.8(4) ? C14 C13 H13 . . 120.1 ? C12 C13 H13 . . 120.1 ? C13 C14 C13 . 2 120.1(5) ? C13 C14 H14 . . 119.9 ? C13 C14 H14 2 . 119.9 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag C12 H12 N1 . .93 2.93 3.335(4) 108 y C12 H12 Cl1 . .93 2.94 3.420(4) 113 y N2 H2 Cl1 . .86 2.86 3.310(3) 115 y C6 H6C Cl1 2 .96 2.78 3.643(4) 151 y N2 H2 Cl1 5 .86 2.57 3.342(3) 150 y C7 H7A Cl1 5 .96 3.26 3.726(4) 112 y 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_site_symmetry_1 _geom_torsion_site_symmetry_4 _geom_torsion C1 Sn1 N1 C5 . . -125.5(3) C11 Sn1 N1 C5 . . 54.5(3) N1 Sn1 N1 C5 2 . -125.5(3) Cl1 Sn1 N1 C5 . . 145.3(3) Cl1 Sn1 N1 C5 2 . -36.5(3) C1 Sn1 N1 N2 . . 50.3(2) C11 Sn1 N1 N2 . . -129.7(2) N1 Sn1 N1 N2 2 . 50.3(2) Cl1 Sn1 N1 N2 . . -38.8(2) Cl1 Sn1 N1 N2 2 . 139.4(2) C5 N1 N2 C3 . . -.7(4) Sn1 N1 N2 C3 . . -177.8(2) N1 N2 C3 C4 . . .8(4) N1 N2 C3 C7 . . -179.7(3) N2 C3 C4 C5 . . -.5(4) C7 C3 C4 C5 . . 180.0(4) N2 N1 C5 C4 . . .3(4) Sn1 N1 C5 C4 . . 176.6(3) N2 N1 C5 C6 . . 178.9(3) Sn1 N1 C5 C6 . . -4.8(5) C3 C4 C5 N1 . . .1(4) C3 C4 C5 C6 . . -178.3(4) C1 Sn1 C11 C12 . 2 6E1(10) N1 Sn1 C11 C12 2 2 44.36(18) N1 Sn1 C11 C12 . 2 -135.64(18) Cl1 Sn1 C11 C12 . 2 139.36(17) Cl1 Sn1 C11 C12 2 2 -40.64(17) C1 Sn1 C11 C12 . . -12E1(10) N1 Sn1 C11 C12 2 . -135.64(18) N1 Sn1 C11 C12 . . 44.36(18) Cl1 Sn1 C11 C12 . . -40.64(17) Cl1 Sn1 C11 C12 2 . 139.36(17) C12 C11 C12 C13 2 . .3(3) Sn1 C11 C12 C13 . . -179.7(3) C11 C12 C13 C14 . . -.6(5) C12 C13 C14 C13 . 2 .3(3)