#------------------------------------------------------------------------------ #$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $ #$Revision: 176789 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/22/93/2229368.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_2229368 loop_ _publ_author_name 'Hameau, Aur\'elien' 'Guyon, Fabrice' 'Knorr, Michael' 'Colquhoun, Victoria P.' 'Strohmann, Carsten' _publ_section_title ; Two-dimensional polymeric [Hg~4~(\m~2~-I)~6~I~2~(\m~2~-C~4~S~6~)]~n~ ; _journal_coeditor_code FI2103 _journal_issue 3 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m389 _journal_paper_doi 10.1107/S1600536811006556 _journal_volume 67 _journal_year 2011 _chemical_formula_iupac '[Hg4 I8 (C4 S6)]' _chemical_formula_moiety 'C2 Hg2 I4 S3' _chemical_formula_sum 'C2 Hg2 I4 S3' _chemical_formula_weight 1028.98 _chemical_name_systematic ; Poly[(\m~2~-2H,5H-1,3-dithiolo[4,5-d][1,3]dithiole- 2,5-dithione)hexa-\m~2~-iodido-diiodidotetramercury(II)] ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL97 _cell_angle_alpha 90.00 _cell_angle_beta 91.3430(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 8.5502(6) _cell_length_b 11.2156(8) _cell_length_c 13.4634(9) _cell_measurement_reflns_used 8987 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 26 _cell_measurement_theta_min 2.36 _cell_volume 1290.73(16) _computing_cell_refinement 'SAINT-Plus (Bruker, 1999)' _computing_data_collection 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT-Plus (Bruker, 1999)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'SHELXL97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _diffrn_ambient_temperature 173(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Bruker APEX CCD' _diffrn_measurement_method \w _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 0.0861 _diffrn_reflns_av_sigmaI/netI 0.0328 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 24415 _diffrn_reflns_theta_full 26.00 _diffrn_reflns_theta_max 26.00 _diffrn_reflns_theta_min 2.36 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 50 _diffrn_standards_number 1 _exptl_absorpt_coefficient_mu 33.761 _exptl_absorpt_correction_T_max 0.1333 _exptl_absorpt_correction_T_min 0.0352 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Bruker, 1999)' _exptl_crystal_colour 'dark red' _exptl_crystal_density_diffrn 5.295 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 1728 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _refine_diff_density_max 3.557 _refine_diff_density_min -3.288 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_matrix_type full _refine_ls_number_parameters 100 _refine_ls_number_reflns 2543 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.025 _refine_ls_R_factor_all 0.0413 _refine_ls_R_factor_gt 0.0386 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0770P)^2^+7.1937P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1113 _refine_ls_wR_factor_ref 0.1136 _reflns_number_gt 2337 _reflns_number_total 2543 _reflns_threshold_expression I>2\s(I) _cod_data_source_file fi2103.cif _cod_data_source_block I _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 2229368 _cod_database_fobs_code 2229368 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_type_symbol _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 C C1 0.0263(12) 0.9542(9) 1.0288(7) 0.029(2) Uani d . 1 . . C C2 0.2439(12) 0.9942(9) 0.9076(8) 0.033(2) Uani d . 1 . . Hg Hg1 0.51629(6) 0.77041(5) 0.83365(5) 0.05585(19) Uani d . 1 . . Hg Hg2 0.22624(7) 0.46970(6) 0.97826(5) 0.0672(2) Uani d . 1 . . I I1 0.82359(9) 0.77867(6) 0.83985(5) 0.0374(2) Uani d . 1 . . I I2 0.25603(8) 0.64475(6) 0.79810(5) 0.0372(2) Uani d . 1 . . I I3 0.08558(9) 0.60123(6) 1.11662(5) 0.03616(19) Uani d . 1 . . I I4 0.45656(8) 0.32667(6) 0.92556(5) 0.03444(19) Uani d . 1 . . S S1 0.2076(3) 0.8973(2) 1.0033(2) 0.0374(6) Uani d . 1 . . S S2 0.4123(3) 0.9968(3) 0.8465(2) 0.0427(6) Uani d . 1 . . S S3 -0.0987(3) 0.9043(2) 1.1185(2) 0.0363(6) Uani d . 1 . . 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 C1 0.025(5) 0.035(5) 0.028(5) -0.001(4) 0.003(4) 0.002(4) C2 0.031(5) 0.029(5) 0.039(5) -0.002(4) 0.003(4) -0.001(4) Hg1 0.0325(3) 0.0672(4) 0.0682(4) -0.0029(2) 0.0078(2) 0.0044(3) Hg2 0.0477(4) 0.0668(4) 0.0881(5) 0.0157(3) 0.0243(3) -0.0110(3) I1 0.0303(4) 0.0452(4) 0.0369(4) -0.0012(3) 0.0048(3) -0.0032(3) I2 0.0332(4) 0.0424(4) 0.0359(4) -0.0019(3) 0.0013(3) 0.0038(3) I3 0.0351(4) 0.0365(4) 0.0369(4) -0.0014(3) 0.0029(3) -0.0047(3) I4 0.0305(4) 0.0404(4) 0.0326(4) 0.0048(3) 0.0041(3) -0.0024(3) S1 0.0310(14) 0.0406(14) 0.0410(14) 0.0074(11) 0.0101(11) 0.0073(11) S2 0.0350(15) 0.0365(13) 0.0576(17) 0.0020(11) 0.0205(13) 0.0038(12) S3 0.0339(14) 0.0372(13) 0.0383(13) 0.0051(10) 0.0128(11) 0.0067(11) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' I I -0.4742 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 C1 S1 3_577 . 117.1(11) ? C1 C1 S3 3_577 . 116.3(11) ? S1 C1 S3 . . 126.6(6) ? S2 C2 S3 . 3_577 121.0(6) ? S2 C2 S1 . . 123.4(6) ? S3 C2 S1 3_577 . 115.5(6) ? I1 Hg1 I2 . . 148.57(3) ? I1 Hg1 S2 . . 107.19(7) ? I2 Hg1 S2 . . 103.53(7) ? I4 Hg2 I3 . . 150.11(4) ? I4 Hg2 I3 . 3_567 112.31(3) ? I3 Hg2 I3 . 3_567 91.87(3) ? I4 Hg2 I2 . . 95.60(3) ? I3 Hg2 I2 . . 103.81(3) ? I3 Hg2 I2 3_567 . 85.70(3) ? Hg1 I2 Hg2 . . 105.93(3) ? Hg2 I3 Hg2 . 3_567 88.13(3) ? C1 S1 C2 . . 95.4(5) ? C2 S2 Hg1 . . 107.7(4) ? C2 S3 C1 3_577 . 95.7(5) ? 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 C1 C1 3_577 1.36(2) ? C1 S1 . 1.718(11) ? C1 S3 . 1.724(11) ? C2 S2 . 1.675(11) ? C2 S3 3_577 1.715(11) ? C2 S1 . 1.720(11) ? Hg1 I1 . 2.6285(9) ? Hg1 I2 . 2.6678(9) ? Hg1 S2 . 2.697(3) ? Hg2 I4 . 2.6496(9) ? Hg2 I3 . 2.6828(9) ? Hg2 I3 3_567 3.0353(10) ? Hg2 I2 . 3.1357(10) ? I3 Hg2 3_567 3.0353(10) ? S3 C2 3_577 1.715(11) ?