#------------------------------------------------------------------------------ #$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $ #$Revision: 176760 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/05/2010587.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_2010587 loop_ _publ_author_name 'Clark, Alex M.' 'Oliver, Allen G.' 'Rickard, Clifton E. F.' 'Wright, L. James' 'Roper, Warren R.' _publ_section_title ; Bis(N,N'-dimethylimidazol-2-ylidene)mercury chlorotriiodomercury dimethyl sulfoxide solvate ; _journal_issue 1 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 26 _journal_page_last 27 _journal_paper_doi 10.1107/S0108270199012640 _journal_volume 56 _journal_year 2000 _chemical_formula_iupac '[Hg (C5 H8 N2)2][Hg Cl I3] . C2 H6 O S' _chemical_formula_moiety 'C10 H16 Hg N4 2+ , Hg Cl I3 2- , C2 H6 O S' _chemical_formula_sum 'C12 H22 Cl Hg2 I3 N4 O S' _chemical_formula_weight 1087.73 _chemical_name_systematic ; Bis(N,N'-dimethylimidazol-2-ylidene)mercury(II) Chlorotriiodomercurate(II) Dimethylsulphoxide solvate. ; _space_group_IT_number 62 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2n' _symmetry_space_group_name_H-M 'P n m a' _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 9.61190(10) _cell_length_b 13.49540(10) _cell_length_c 18.514(3) _cell_measurement_reflns_used 7498 _cell_measurement_temperature 203(2) _cell_measurement_theta_max 28.31 _cell_measurement_theta_min 1.87 _cell_volume 2401.6(4) _computing_cell_refinement 'SAINT (Siemens, 1994a)' _computing_data_collection 'SMART (Siemens, 1994a)' _computing_data_reduction SAINT _computing_molecular_graphics 'SHELXTL (Siemens, 1994b)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997b)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997a)' _diffrn_ambient_temperature 203(2) _diffrn_measured_fraction_theta_full .872 _diffrn_measured_fraction_theta_max .872 _diffrn_measurement_device_type 'Siemens SMART CCD area-detector' _diffrn_measurement_method \w _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 .0513 _diffrn_reflns_av_sigmaI/netI .0374 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 14997 _diffrn_reflns_theta_full 28.31 _diffrn_reflns_theta_max 28.31 _diffrn_reflns_theta_min 1.87 _diffrn_standards_decay_% 0 _exptl_absorpt_coefficient_mu 16.833 _exptl_absorpt_correction_T_max .4866 _exptl_absorpt_correction_T_min .0604 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Blessing, 1995)' _exptl_crystal_colour Colourless _exptl_crystal_density_diffrn 3.008 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Needle _exptl_crystal_F_000 1928 _exptl_crystal_size_max .38 _exptl_crystal_size_mid .18 _exptl_crystal_size_min .05 _refine_diff_density_max 1.328 _refine_diff_density_min -2.282 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 128 _refine_ls_number_reflns 2937 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.050 _refine_ls_R_factor_all .0537 _refine_ls_R_factor_gt .0383 _refine_ls_shift/su_max .018 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0576P)^2^+11.9641P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .1099 _reflns_number_gt 2317 _reflns_number_total 2937 _reflns_threshold_expression I>2\s(I) _cod_data_source_file ta1265.cif _cod_data_source_block I _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. '_geom_bond_publ_flag' value 'Y' changed to 'y' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (11 times). 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 'Orthorhombic' changed to 'orthorhombic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. '_geom_bond_publ_flag' value 'Y' changed to 'y' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (11 times). '_geom_angle_publ_flag' value 'Y' changed to 'y' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (6 times). Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w = 1/[\s^2^(Fo^2^)+(0.0576P)^2^+11.9641P] 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^)+(0.0576P)^2^+11.9641P] where P=(Fo^2^+2Fc^2^)/3'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_cell_volume 2401.57(5) _cod_database_code 2010587 _cod_database_fobs_code 2010587 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -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 Hg1 .5000 .0000 .5000 .03826(15) Uani d S 1 . . Hg N1 .3081(7) -.0459(5) .6294(4) .0362(15) Uani d . 1 . . N N2 .4717(7) .0541(5) .6607(3) .0332(15) Uani d . 1 . . N C1 .4214(8) .0030(6) .6044(4) .0322(17) Uani d . 1 . . C C2 .2884(11) -.0244(7) .7009(5) .048(2) Uani d . 1 . . C H2A .2172 -.0487 .7308 .058 Uiso calc R 1 . . H C3 .3919(11) .0390(7) .7203(5) .048(2) Uani d . 1 . . C H3A .4056 .0671 .7662 .057 Uiso calc R 1 . . H C4 .2185(10) -.1117(8) .5866(6) .053(2) Uani d . 1 . . C H4A .2752 -.1500 .5534 .079 Uiso calc R 1 . . H H4B .1522 -.0724 .5594 .079 Uiso calc R 1 . . H H4C .1688 -.1563 .6186 .079 Uiso calc R 1 . . H C5 .5940(10) .1170(7) .6592(5) .046(2) Uani d . 1 . . C H5A .5841 .1660 .6212 .069 Uiso calc R 1 . . H H5B .6758 .0768 .6500 .069 Uiso calc R 1 . . H H5C .6039 .1502 .7054 .069 Uiso calc R 1 . . H Hg2 .32417(5) .2500 .38947(2) .03989(15) Uani d S 1 . . Hg I1 .17973(6) .08099(5) .42725(4) .05136(19) Uani d . 1 . . I I2 .47837(9) .2500 .26846(4) .0458(2) Uani d S 1 . . I Cl1 .5064(3) .2500 .49906(14) .0359(6) Uani d S 1 . . Cl S1 .5307(6) .2056(3) .8693(3) .0471(11) Uani d P .50 . . S O1 .4624(12) .2500 .8022(5) .068(3) Uani d S 1 . . O C6 .6926(17) .2500 .8765(11) .087(6) Uani d S 1 . . C H6A .7463 .2304 .8345 .130 Uiso calc PR .50 . . H H6B .7358 .2236 .9198 .130 Uiso calc PR .50 . . H H6C .6895 .3217 .8795 .130 Uiso calc PR .50 . . H C7 .437(2) .2500 .9406(8) .077(5) Uani d S 1 . . C H7A .3432 .2243 .9384 .116 Uiso calc PR .50 . . H H7B .4349 .3218 .9386 .116 Uiso calc PR .50 . . H H7C .4807 .2292 .9854 .116 Uiso calc PR .50 . . 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 Hg1 .0309(2) .0678(3) .0161(2) -.0077(2) .00256(16) -.00307(19) N1 .040(4) .044(4) .025(3) .003(3) .011(3) -.002(3) N2 .041(4) .041(4) .017(3) .003(3) .000(3) .000(3) C1 .033(4) .041(4) .023(4) .001(3) .010(3) .003(3) C2 .059(6) .057(6) .030(5) .004(5) .021(4) -.003(4) C3 .066(6) .055(5) .023(4) .004(5) .009(4) -.002(4) C4 .041(5) .065(6) .052(6) -.014(5) .015(5) -.011(5) C5 .050(5) .055(5) .033(5) -.006(4) -.008(4) -.002(4) Hg2 .0362(3) .0552(3) .0282(3) .000 -.00212(19) .000 I1 .0395(3) .0598(4) .0548(4) -.0027(3) -.0027(3) .0009(3) I2 .0429(5) .0682(6) .0262(4) .000 .0004(3) .000 Cl1 .0319(13) .0536(17) .0222(14) .000 -.0046(10) .000 S1 .066(3) .041(2) .035(2) -.002(2) .001(2) -.0045(19) O1 .070(7) .110(9) .025(5) .000 -.009(5) .000 C6 .049(10) .15(2) .065(12) .000 .009(8) .000 C7 .077(12) .124(16) .031(8) .000 -.004(8) .000 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' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S .1246 .1234 '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' I I -.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 '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 Hg1 C1 . 5_656 180.0 ? C1 N1 C2 . . 109.7(8) ? C1 N1 C4 . . 125.6(7) ? C2 N1 C4 . . 124.7(8) ? C1 N2 C3 . . 110.5(7) ? C1 N2 C5 . . 125.4(7) ? C3 N2 C5 . . 124.1(7) ? N2 C1 N1 . . 106.0(7) ? N2 C1 Hg1 . . 127.1(6) ? N1 C1 Hg1 . . 126.9(6) ? C3 C2 N1 . . 106.8(8) ? N2 C3 C2 . . 107.0(8) ? Cl1 Hg2 I2 . . 105.72(6) y Cl1 Hg2 I1 . 7_565 97.87(4) y I2 Hg2 I1 . 7_565 119.262(18) y Cl1 Hg2 I1 . . 97.87(4) y I2 Hg2 I1 . . 119.263(19) y I1 Hg2 I1 7_565 . 111.44(3) y O1 S1 C6 . . 108.9(8) ? O1 S1 C7 . . 105.4(7) ? C6 S1 C7 . . 107.6(9) ? 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 Hg1 C1 . 2.076(7) y Hg1 C1 5_656 2.076(7) ? N1 C1 . 1.355(10) y N1 C2 . 1.367(11) y N1 C4 . 1.470(12) y N2 C1 . 1.340(10) y N2 C3 . 1.359(11) y N2 C5 . 1.449(11) y C2 C3 . 1.360(15) y Hg2 Cl1 . 2.680(3) y Hg2 I2 . 2.6863(9) y Hg2 I1 7_565 2.7602(7) ? Hg2 I1 . 2.7602(7) y S1 O1 . 1.528(11) ? S1 C6 . 1.672(16) ? S1 C7 . 1.705(16) ?