#------------------------------------------------------------------------------ #$Date: 2018-05-24 04:53:41 +0100 (Thu, 24 May 2018) $ #$Revision: 207948 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/72/2007249.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_2007249 loop_ _publ_author_name 'Davidovi\'c, Naka' 'Matkovi\'c-\S)chloromercury(II)] ; _journal_issue 5 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 574 _journal_page_last 576 _journal_paper_doi 10.1107/S0108270197016788 _journal_volume 54 _journal_year 1998 _chemical_formula_iupac '[Hg2 Cl4 (C6 H7 NS)2]' _chemical_formula_moiety 'C12 H14 N2 S2 Hg2 Cl4' _chemical_formula_structural '(C6 H7 N S Hg Cl2)2' _chemical_formula_sum 'C12 H14 Cl4 Hg2 N2 S2' _chemical_formula_weight 793.36 _chemical_name_systematic ; bis{\m-chloro-[chloro-2-ammoniobenzenethiolato]mercury(II)} ; _space_group_IT_number 61 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_space_group_name_H-M 'P b c a' _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 17.786(2) _cell_length_b 14.5040(10) _cell_length_c 7.437(3) _cell_measurement_reflns_used 39 _cell_measurement_temperature 295.00(10) _cell_measurement_theta_max 18.7 _cell_measurement_theta_min 11.1 _cell_volume 1918.5(8) _computing_cell_refinement STADI4 _computing_data_collection 'STADI4 (Stoe, 1995a)' _computing_data_reduction 'X-RED (Stoe, 1995b)' _computing_molecular_graphics 'PLATON97 (Spek, 1997), PLUTON96 (Spek, 1996)' _computing_publication_material PLATON97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _diffrn_measured_fraction_theta_full 0.880 _diffrn_measured_fraction_theta_max 0.880 _diffrn_measurement_device_type 'Philips PW1100 diffractometer updated by Stoe' _diffrn_measurement_method \w-2\q _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 0.0254 _diffrn_reflns_av_sigmaI/netI 0.0428 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -3 _diffrn_reflns_number 5516 _diffrn_reflns_theta_full 30.01 _diffrn_reflns_theta_max 30.01 _diffrn_reflns_theta_min 2.69 _diffrn_standards_decay_% 4.6 _diffrn_standards_interval_time 90 _diffrn_standards_number 4 _exptl_absorpt_coefficient_mu 16.755 _exptl_absorpt_correction_T_max 0.2644 _exptl_absorpt_correction_T_min 0.0154 _exptl_absorpt_correction_type integration _exptl_crystal_colour transparent _exptl_crystal_density_diffrn 2.747 _exptl_crystal_density_meas ? _exptl_crystal_description Prism _exptl_crystal_F_000 1440 _exptl_crystal_size_max 0.283 _exptl_crystal_size_mid 0.276 _exptl_crystal_size_min 0.043 _refine_diff_density_max 1.56_(0.86\%A_from_Hg) _refine_diff_density_min -0.84 _refine_ls_extinction_coef 0.00278(13) _refine_ls_extinction_method SHELXL97_(Sheldrick,_1997) _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_hydrogen_treatment H_atoms:_see_below _refine_ls_matrix_type full _refine_ls_number_parameters 127 _refine_ls_number_reflns 2791 _refine_ls_number_restraints 15 _refine_ls_restrained_S_all 1.036 _refine_ls_R_factor_all 0.0778 _refine_ls_R_factor_gt 0.0368 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0356P)^2^+1.4042P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.0772 _reflns_number_gt 1857 _reflns_number_total 2791 _reflns_threshold_expression I>2\s(I) _cod_data_source_file mu1360.cif _cod_data_source_block mu1360 _cod_depositor_comments ; Removing duplicate lines from the aniso value loop. Antanas Vaitkus, 2018-05-24 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 'calc w = 1/[\s^2^(Fo^2^)+(0.0356P)^2^+1.4042P] where P=(Fo^2^+2Fc^2^)/3' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w = 1/[\s^2^(Fo^2^)+(0.0356P)^2^+1.4042P] where P=(Fo^2^+2Fc^2^)/3'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_formula_sum 'C12 H14 N2 S2 Hg2 Cl4' _cod_database_code 2007249 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' 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 Hg .084125(14) .100320(13) .07617(3) .04134(10) Uani d . 1 . . Hg Cl1 .04713(9) .22324(8) -.1172(2) .0411(3) Uani d . 1 . . Cl Cl2 .06727(8) -.03139(8) -.1810(2) .0378(3) Uani d . 1 . . Cl S .14397(10) .05345(9) .3411(2) .0442(4) Uani d . 1 . . S N .0448(3) -.1114(3) .4194(6) .0350(10) Uani d D 1 . . N C1 .1681(3) -.0644(4) .3007(8) .0350(12) Uani d . 1 . . C C2 .1186(3) -.1353(3) .3478(8) .0332(11) Uani d D 1 . . C C3 .1378(4) -.2270(4) .3327(9) .0402(14) Uani d D 1 . . C C4 .2089(5) -.2491(5) .2669(10) .0547(18) Uani d D 1 . . C C5 .2578(4) -.1812(6) .2187(11) .066(2) Uani d D 1 . . C C6 .2381(4) -.0888(5) .2352(10) .0550(17) Uani d D 1 . . C H6 .274(3) -.044(4) .192(8) .050(18) Uiso d D 1 . . H H3 .104(3) -.277(4) .359(10) .06(2) Uiso d D 1 . . H H4 .222(4) -.313(3) .258(10) .08(2) Uiso d D 1 . . H H5 .305(3) -.190(4) .163(10) .07(2) Uiso d D 1 . . H H11 .016(3) -.070(4) .345(7) .100(18) Uiso d D 1 . . H H12 .051(3) -.089(4) .541(4) .100(18) Uiso d D 1 . . H H13 .016(3) -.168(3) .422(8) .100(18) Uiso d D 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 Hg .05226(15) .03830(12) .03344(14) .00320(9) -.00442(12) .00617(8) Cl1 .0594(9) .0299(5) .0339(8) .0053(6) -.0002(7) .0025(5) Cl2 .0432(7) .0348(6) .0353(8) -.0012(5) .0022(6) -.0063(5) S .0646(10) .0325(6) .0354(9) -.0115(6) -.0160(8) .0035(6) N .039(2) .0289(18) .037(3) -.0030(17) .004(2) -.0026(18) C1 .036(3) .040(2) .029(3) -.002(2) -.005(3) .004(2) C2 .038(3) .035(2) .027(3) .005(2) -.006(3) -.001(2) C3 .048(3) .034(2) .039(4) .008(2) -.003(3) .003(2) C4 .066(5) .056(3) .042(4) .029(3) -.004(4) -.004(3) C5 .042(4) .101(6) .055(5) .025(4) .000(4) .006(4) C6 .043(3) .069(4) .053(5) -.007(3) .003(4) .019(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Hg Hg -2.3894 9.2266 '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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' H H 0.0000 0.0000 '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_3 _geom_angle _geom_angle_publ_flag S Hg Cl1 . 148.31(5) yes S Hg Cl2 . 115.99(5) yes Cl1 Hg Cl2 . 94.05(5) yes S Hg Cl2 5 95.36(5) yes Cl1 Hg Cl2 5 99.19(5) yes Cl2 Hg Cl2 5 81.29(5) yes Hg Cl2 Hg 5 98.71(5) no C1 S Hg . 104.22(19) yes C2 N H11 . 115(3) no C2 N H12 . 109(4) no H11 N H12 . 113(4) no C2 N H13 . 107(3) no H11 N H13 . 104(4) no H12 N H13 . 109(4) no C6 C1 C2 . 117.8(5) no C6 C1 S . 121.4(4) no C2 C1 S . 120.7(4) no C3 C2 C1 . 122.3(6) no C3 C2 N . 118.8(5) no C1 C2 N . 118.9(4) no C2 C3 C4 . 118.4(6) no C2 C3 H3 . 124(4) no C4 C3 H3 . 118(4) no C5 C4 C3 . 120.4(6) no C5 C4 H4 . 122(5) no C3 C4 H4 . 118(5) no C4 C5 C6 . 120.7(7) no C4 C5 H5 . 126(4) no C6 C5 H5 . 113(4) no C1 C6 C5 . 120.4(6) no C1 C6 H6 . 123(4) no C5 C6 H6 . 117(4) no 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 Hg S . 2.3404(17) yes Hg Cl1 . 2.3834(14) yes Hg Cl2 . 2.7199(14) yes Hg Cl2 5 2.9762(14) yes Cl2 Hg 5 2.9762(14) no S C1 . 1.788(5) yes N C2 . 1.459(7) yes N H11 . .96(2) no N H12 . .96(2) no N H13 . .97(2) no C1 C6 . 1.382(9) no C1 C2 . 1.399(8) no C2 C3 . 1.377(7) no C3 C4 . 1.393(10) no C3 H3 . .96(4) no C4 C5 . 1.362(11) no C4 H4 . .95(4) no C5 C6 . 1.391(10) no C5 H5 . .94(4) no C6 H6 . .96(4) no 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 N H11 Cl2 5_555 0.96(6) 2.42(5) 3.377(5) 174(4) N H12 Cl2 1_556 0.97(3) 2.25(4) 3.215(5) 178(5) N H13 Cl1 3_545 0.97(5) 2.42(5) 3.254(5) 144(5) N H13 Cl1 5_555 0.97(5) 2.65(6) 3.218(5) 118(4)