#------------------------------------------------------------------------------ #$Date: 2015-01-07 16:25:02 +0000 (Wed, 07 Jan 2015) $ #$Revision: 129439 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/50/2205002.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_2205002 loop_ _publ_author_name 'Zhu, Zhi-Biao' 'Shan Gao' 'Huo, Li-Hua' 'Ng, Seik Weng' _publ_section_title ; Poly[bis[aquamercury(I)]-di-\m-aqua-\m-1,5-naphthalenedisulfonato] ; _journal_issue 2 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m288 _journal_page_last m289 _journal_volume 61 _journal_year 2005 _chemical_formula_iupac '[Hg2 (C10 H6 O6 S2) (H2 O)4]' _chemical_formula_moiety 'C10 H6 O6 S2 , 4H2 O , 2Hg' _chemical_formula_sum 'C10 H14 Hg2 O10 S2' _chemical_formula_weight 759.51 _chemical_name_systematic ; Poly[bis[aquamercury(I)]-di-\m-aqua-\m-1,5-naphthalenedisulfonato] ; _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_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL97 _cell_angle_alpha 90 _cell_angle_beta 112.79(3) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 13.199(3) _cell_length_b 5.6990(10) _cell_length_c 11.039(2) _cell_measurement_reflns_used 3608 _cell_measurement_temperature 295(2) _cell_measurement_theta_max 26.2 _cell_measurement_theta_min 3.8 _cell_volume 765.5(3) _computing_cell_refinement RAPID-AUTO _computing_data_collection 'RAPID-AUTO (Rigaku, 1998)' _computing_data_reduction 'CrystalStructure (Rigaku/MSC, 2002)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 295(2) _diffrn_measured_fraction_theta_full 0.99 _diffrn_measured_fraction_theta_max 0.99 _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _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 0.090 _diffrn_reflns_av_sigmaI/netI 0.065 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 4829 _diffrn_reflns_theta_full 27.5 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_min 3.4 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 20.356 _exptl_absorpt_correction_T_max 0.177 _exptl_absorpt_correction_T_min 0.002 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details '(NUMABS in ABSCORR; Higashi, 1995)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 3.295 _exptl_crystal_density_meas ? _exptl_crystal_density_method . _exptl_crystal_description block _exptl_crystal_F_000 692 _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.13 _refine_diff_density_max 1.62 _refine_diff_density_min -1.72 _refine_ls_extinction_coef 0.0069(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL97 (Sheldrick, 1997)' _refine_ls_goodness_of_fit_ref 1.11 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 111 _refine_ls_number_reflns 1759 _refine_ls_number_restraints 36 _refine_ls_restrained_S_all 1.10 _refine_ls_R_factor_all 0.054 _refine_ls_R_factor_gt 0.046 _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^)+(0.0734P)^2^+3.8951P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.117 _refine_ls_wR_factor_ref 0.136 _reflns_number_gt 1526 _reflns_number_total 1759 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file bt6580.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P 21/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 2205002 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_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_type_symbol Hg1 0.57380(3) 0.64585(7) 0.53826(4) 0.0428(2) Uani d . 1 Hg S1 0.7463(2) 0.2789(4) 0.4123(2) 0.0290(5) Uani d . 1 S O1W 0.7157(7) 0.8490(10) 0.6432(7) 0.037(2) Uani d . 1 O O2W 0.5116(5) 0.9750(10) 0.3585(6) 0.040(2) Uani d . 1 O O1 0.6908(6) 0.4980(10) 0.3591(7) 0.039(2) Uani d . 1 O O2 0.7536(5) 0.2420(10) 0.5446(6) 0.036(2) Uani d . 1 O O3 0.7000(6) 0.0820(10) 0.3276(7) 0.041(2) Uani d . 1 O C1 0.8786(6) 0.3170(10) 0.4216(7) 0.024(2) Uani d DU 1 C C2 0.9133(7) 0.1530(10) 0.3534(8) 0.030(2) Uani d DU 1 C C3 1.0206(7) 0.168(2) 0.3621(8) 0.033(2) Uani d DU 1 C C4 1.0895(7) 0.3420(10) 0.4349(8) 0.032(2) Uani d DU 1 C C5 1.0532(4) 0.5070(10) 0.5021(7) 0.028(2) Uani d DU 1 C H1W1 0.7210 0.8685 0.7218 0.045 Uiso calc R 1 H H1W2 0.7105 0.9820 0.6063 0.045 Uiso calc R 1 H H2W1 0.4624 0.9224 0.2881 0.048 Uiso calc R 1 H H2W2 0.5659 1.0210 0.3414 0.048 Uiso calc R 1 H H2 0.8660 0.0373 0.3033 0.036 Uiso calc R 1 H H3 1.0463 0.0586 0.3182 0.040 Uiso calc R 1 H H4 1.1612 0.3493 0.4393 0.038 Uiso calc R 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 Hg1 0.0447(3) 0.0464(3) 0.0445(3) -0.0159(2) 0.0252(2) -0.0088(2) S1 0.0230(10) 0.0430(10) 0.0240(10) -0.0060(10) 0.0130(10) 0.0000(10) O1W 0.051(4) 0.034(4) 0.039(4) -0.008(3) 0.030(3) -0.005(3) O2W 0.025(3) 0.055(4) 0.038(3) -0.009(3) 0.013(3) -0.004(3) O1 0.031(3) 0.052(4) 0.037(3) 0.004(3) 0.014(3) 0.009(3) O2 0.029(3) 0.055(4) 0.030(3) -0.012(3) 0.016(3) 0.000(3) O3 0.024(3) 0.062(4) 0.045(4) -0.010(3) 0.022(3) -0.011(3) C1 0.016(3) 0.035(4) 0.028(3) 0.008(3) 0.016(3) 0.008(3) C2 0.032(4) 0.037(4) 0.029(4) -0.001(3) 0.019(3) -0.001(3) C3 0.038(5) 0.039(4) 0.029(4) 0.000(3) 0.020(4) -0.003(3) C4 0.028(4) 0.042(5) 0.034(4) 0.004(3) 0.021(4) 0.003(3) C5 0.028(4) 0.040(4) 0.016(3) -0.008(3) 0.009(3) 0.000(3) 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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' 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 Hg1 Hg1 O1W 3_666 . 166.9(2) no Hg1 Hg1 O2W 3_666 . 104.5(2) no Hg1 Hg1 O2W 3_666 3_676 105.40(10) no O1 Hg1 O1W . . 86.8(2) yes O1 Hg1 O2W . . 78.2(2) yes O1 Hg1 O2W . 3_676 146.9(2) yes O1W Hg1 O2W . . 88.5(2) yes O1W Hg1 O2W . 3_676 76.8(2) yes O2W Hg1 O2W . 3_676 72.9(2) yes Hg1 O2W Hg1 . 3_676 107.1(2) yes O1 S1 O3 . . 112.8(5) no O1 S1 O2 . . 111.3(4) no O2 S1 O3 . . 112.9(4) no O1 S1 C1 . . 104.9(4) no O2 S1 C1 . . 106.8(4) no O3 S1 C1 . . 107.6(4) no S1 O1 Hg1 . . 106.1(3) no C2 C1 C5 . 3_766 122.8(7) no C2 C1 S1 . . 115.2(6) no C5 C1 S1 3_766 . 122.0(5) no C1 C2 C3 . . 117.9(8) no C4 C3 C2 . . 120.7(8) no C3 C4 C5 . . 120.9(7) no C1 C5 C5 3_766 3_766 118.1(8) no C1 C5 C4 3_766 . 122.3(5) no C5 C5 C4 3_766 . 119.5(8) no Hg1 O1W H1W1 . . 109.5 no Hg1 O1W H1W2 . . 109.5 no H1W1 O1W H1W2 . . 109.5 no Hg1 O2W H2W1 . . 110.3 no Hg1 O2W H2W1 3_676 . 110.3 no Hg1 O2W H2W2 . . 110.3 no Hg1 O2W H2W2 3_676 . 110.3 no H2W1 O2W H2W2 . . 108.6 no C1 C2 H2 . . 121.0 no C3 C2 H2 . . 121.0 no C4 C3 H3 . . 119.7 no C2 C3 H3 . . 119.7 no C3 C4 H4 . . 119.6 no C5 C4 H4 . . 119.6 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 Hg1 Hg1 3_666 2.4488(9) yes Hg1 O1 . 3.062(7) yes Hg1 O1W . 2.124(7) yes Hg1 O2W . 2.619(7) yes Hg1 O2W 3_676 2.872(7) yes S1 O1 . 1.450(8) no S1 O2 . 1.441(6) no S1 O3 . 1.438(8) no S1 C1 . 1.723(7) no C1 C2 . 1.383(8) no C1 C5 3_766 1.392(8) no C2 C3 . 1.384(8) no C3 C4 . 1.375(8) no C4 C5 . 1.394(8) no C5 C1 3_766 1.392(8) no C5 C5 3_766 1.390(9) no O1W H1W1 . 0.85 no O1W H1W2 . 0.85 no O2W H2W1 . 0.85 no O2W H2W2 . 0.85 no C2 H2 . 0.93 no C3 H3 . 0.93 no C4 H4 . 0.93 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 _geom_hbond_publ_flag O1W H1W1 O1 4_576 0.85 1.87 2.680(10) 157 yes O1W H1W2 O2 1_565 0.85 1.81 2.620(10) 158 yes O2W H2W1 O1 2_655 0.85 2.09 2.820(10) 144 yes O2W H2W2 O3 1_565 0.85 1.87 2.710(10) 169 yes 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 _geom_torsion_publ_flag O1W Hg1 O2W Hg1 . 3_676 -76.6(3) no Hg1 Hg1 O2W Hg1 3_666 3_676 102.0(2) no O2W Hg1 O2W Hg1 3_676 3_676 0.0 no O1 Hg1 O2W Hg1 . 3_676 -163.6(2) no O3 S1 O1 Hg1 . . 112.2(4) no O2 S1 O1 Hg1 . . -15.8(5) no C1 S1 O1 Hg1 . . -131.0(3) no O1W Hg1 O1 S1 . . 93.8(4) no Hg1 Hg1 O1 S1 3_666 . -73.6(4) no O2W Hg1 O1 S1 . . -177.0(4) no O2W Hg1 O1 S1 3_676 . 153.4(3) no O3 S1 C1 C2 . . -2.3(8) no O2 S1 C1 C2 . . 119.2(7) no O1 S1 C1 C2 . . -122.6(7) no O3 S1 C1 C5 . 3_766 -179.2(7) no O2 S1 C1 C5 . 3_766 -57.7(8) no O1 S1 C1 C5 . 3_766 60.5(8) no C5 C1 C2 C3 3_766 . .0(10) no S1 C1 C2 C3 . . -177.0(7) no C1 C2 C3 C4 . . -1.0(10) no C2 C3 C4 C5 . . .0(10) no C3 C4 C5 C1 . 3_766 178.9(8) no C3 C4 C5 C5 . 3_766 2(2) no _cod_database_fobs_code 2205002 _journal_paper_doi 10.1107/S160053680500053X