#------------------------------------------------------------------------------ #$Date: 2015-01-23 12:30:19 +0000 (Fri, 23 Jan 2015) $ #$Revision: 130086 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/65/2006592.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_2006592 loop_ _publ_author_name 'Spengler, Roland' 'Zouari, Fatma' 'Ben Salah, Abdelhamid' 'Burzlaff, Hans' _publ_section_title ; Bis(piperidinium) Tetrachloromercurate ; _journal_issue 10 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1407 _journal_page_last 1409 _journal_paper_doi 10.1107/S0108270197008512 _journal_volume 53 _journal_year 1997 _chemical_formula_iupac '(C5 N H12)2 [Hg Cl4]' _chemical_formula_structural '(C5 N H12)2 HgCl4' _chemical_formula_sum 'C10 H24 Cl4 Hg N2' _chemical_formula_weight 514.72 _chemical_name_systematic ; Bis(piperidinium) Tetrachloromercurate ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_type_scat_source International_Tables_Vol_IV_Table_2.2B _cell_angle_alpha 90 _cell_angle_beta 100.760(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 14.954(2) _cell_length_b 12.1570(10) _cell_length_c 9.7010(10) _cell_measurement_reflns_used 30 _cell_measurement_temperature 293 _cell_measurement_theta_max 10.9 _cell_measurement_theta_min 8.5 _cell_volume 1732.6(3) _computing_cell_refinement 'local software' _computing_data_collection 'local software (Gomm, 1993)' _computing_data_reduction 'local software' _computing_molecular_graphics 'CRYSTAN (Burzlaff & Rothammel, 1988)' _computing_publication_material CRYSTAN _computing_structure_refinement 'CRYSTAN (Spengler & Zimmermann, 1996)' _computing_structure_solution 'CRYSTAN (Burzlaff & Rothammel, 1988)' _diffrn_ambient_temperature 293 _diffrn_measurement_device_type 'Rebuilt Philips PW1100 diffractometer (Gomm, 1993)' _diffrn_measurement_method \q/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'X-Ray Tube' _diffrn_radiation_type 'Mo K\a~1~' _diffrn_radiation_wavelength .70926 _diffrn_reflns_av_R_equivalents .0613 _diffrn_reflns_av_sigmaI/netI .0149 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 5978 _diffrn_reflns_theta_max 24.0 _diffrn_reflns_theta_min .0 _diffrn_standards_decay_% 1.0 _diffrn_standards_interval_count 100 _diffrn_standards_number 4 _exptl_absorpt_coefficient_mu 9.491 _exptl_absorpt_correction_T_max .418 _exptl_absorpt_correction_T_min .357 _exptl_absorpt_correction_type 'Gaussian integration (Busing & Levy, 1957)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.973 _exptl_crystal_density_meas ? _exptl_crystal_description prismatic _exptl_crystal_F_000 984 _exptl_crystal_size_max .200(10) _exptl_crystal_size_mid .150(10) _exptl_crystal_size_min .100(10) _refine_diff_density_max 1.59 _refine_diff_density_min -1.42 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 1.31 _refine_ls_goodness_of_fit_ref 1.38 _refine_ls_hydrogen_treatment noref _refine_ls_number_parameters 155 _refine_ls_number_reflns 2311 _refine_ls_R_factor_all .048 _refine_ls_R_factor_gt .039 _refine_ls_shift/su_max .00 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme ' w = 1/[\s^2^(F~obs~) + 0.015F~obs~]' _refine_ls_wR_factor_all .042 _refine_ls_wR_factor_ref .040 _reflns_number_gt 2311 _reflns_number_total 2726 _reflns_threshold_expression F>2\s(F) _[local]_cod_data_source_file jz1222.cif _[local]_cod_data_source_block hgpip1 _[local]_cod_cif_authors_sg_H-M 'P 21/n' _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 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 ; _cod_database_code 2006592 _cod_database_fobs_code 2006592 loop_ _symmetry_equiv_pos_as_xyz ' X , Y , Z ' ' 1/2-X , 1/2+Y , 1/2-Z ' ' -X , -Y , -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_occupancy Hg .08686(2) .31059(3) .19809(4) .04820(10) Uani 1.00000 Cl1 .1095(2) .2468(2) -.0396(2) .0554(9) Uani 1.00000 Cl2 -.0738(2) .2574(2) .1958(3) .0630(10) Uani 1.00000 Cl3 .1885(2) .2316(2) .3985(3) .0700(10) Uani 1.00000 Cl4 .1034(2) .5112(2) .1679(2) .0610(10) Uani 1.00000 N1 .1305(4) .4868(6) -.1756(7) .047(3) Uani 1.00000 N2 .3854(5) .2912(6) .3248(8) .053(3) Uani 1.00000 C1 .1029(6) .4434(9) -.3217(9) .060(4) Uani 1.00000 C2 .1450(8) .5083(9) -.4210(10) .075(5) Uani 1.00000 C3 .2456(9) .5090(10) -.3800(10) .086(6) Uani 1.00000 C4 .2740(6) .5540(10) -.2310(10) .085(5) Uani 1.00000 C5 .2304(6) .4885(9) -.1300(10) .068(4) Uani 1.00000 C6 .3746(8) .2776(8) .1710(10) .066(4) Uani 1.00000 C7 .4453(7) .3433(9) .1160(10) .066(4) Uani 1.00000 C8 .4420(7) .4627(9) .1540(10) .064(4) Uani 1.00000 C9 .4505(7) .4780(8) .3130(10) .061(4) Uani 1.00000 C10 .3797(7) .4090(8) .3660(10) .061(4) Uani 1.00000 H1 .10533 .44104 -.11191 .050(6) Uovl 1.00000 H2 .10832 .56057 -.17137 .050(6) Uovl 1.00000 H3 .33820 .25137 .35798 .050(6) Uovl 1.00000 H4 .44367 .26327 .36930 .050(6) Uovl 1.00000 H5 .03786 .44741 -.34817 .050(6) Uovl 1.00000 H6 .12200 .36816 -.32348 .050(6) Uovl 1.00000 H7 .12239 .58223 -.42247 .050(6) Uovl 1.00000 H8 .12797 .47640 -.51270 .050(6) Uovl 1.00000 H9 .27044 .55515 -.44383 .050(6) Uovl 1.00000 H10 .26803 .43561 -.38419 .050(6) Uovl 1.00000 H11 .25555 .62912 -.22950 .050(6) Uovl 1.00000 H12 .33897 .54879 -.20436 .050(6) Uovl 1.00000 H13 .24565 .52145 -.03913 .050(6) Uovl 1.00000 H14 .25333 .41461 -.12655 .050(6) Uovl 1.00000 H15 .38110 .20121 .14969 .050(6) Uovl 1.00000 H16 .31509 .30243 .12719 .050(6) Uovl 1.00000 H17 .50411 .31385 .15570 .050(6) Uovl 1.00000 H18 .43483 .33594 .01609 .050(6) Uovl 1.00000 H19 .49117 .50000 .12330 .050(6) Uovl 1.00000 H20 .38510 .49272 .10720 .050(6) Uovl 1.00000 H21 .51021 .45560 .35895 .050(6) Uovl 1.00000 H22 .44154 .55410 .33266 .050(6) Uovl 1.00000 H23 .38973 .41447 .46646 .050(6) Uovl 1.00000 H24 .32045 .43730 .32708 .050(6) Uovl 1.00000 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 .0504(2) .0471(2) .0471(2) -.0009(2) -.00830(10) -.0001(2) Cl1 .0650(10) .052(2) .0490(10) -.0030(10) .0000(10) -.0064(9) Cl2 .0480(10) .057(2) .083(2) -.0020(10) .0070(10) -.0030(10) Cl3 .060(2) .073(2) .0760(10) -.0060(10) -.0240(10) .0270(10) Cl4 .086(2) .045(2) .0520(10) -.0050(10) .0000(10) -.0022(9) N1 .042(4) .064(5) .037(3) -.001(4) .003(3) .008(3) N2 .060(5) .051(5) .049(4) -.007(4) -.007(3) .010(3) C1 .057(6) .073(8) .049(5) -.007(5) -.013(4) .004(4) C2 .112(9) .073(8) .039(4) .005(8) -.009(5) -.001(4) C3 .110(10) .077(8) .071(7) -.018(8) .047(7) -.001(6) C4 .040(6) .100(10) .116(9) -.012(6) .020(6) -.017(7) C5 .045(5) .089(8) .069(5) -.004(6) -.024(4) -.016(5) C6 .091(8) .044(6) .063(5) .003(6) -.029(5) -.002(4) C7 .084(8) .079(8) .035(4) .005(6) .002(4) -.005(4) C8 .068(6) .066(7) .059(5) -.002(6) -.002(4) .014(5) C9 .067(6) .053(7) .063(5) -.015(5) -.012(4) .008(4) C10 .073(6) .056(7) .054(5) .010(5) .004(4) -.004(4) loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag HG -2.389 9.227 CL 0.148 0.159 N 0.006 0.003 C 0.003 0.002 H 0.000 0.000 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 3 0 1 4 0 0 0 4 0 3 -2 0 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag Cl4 Hg Cl3 114.98(8) yes Cl2 Hg Cl3 111.34(9) yes Cl2 Hg Cl4 111.93(8) yes Cl1 Hg Cl3 116.14(9) yes Cl1 Hg Cl4 99.32(8) yes Cl1 Hg Cl2 101.94(8) yes H1 N1 H2 109.4 no C5 N1 H2 108.3 no C5 N1 H1 108.3 no C1 N1 H2 109.5 no C1 N1 H1 109.5 no C1 N1 C5 111.8(7) no H4 N2 H3 109.5 no C6 N2 H3 109.5 no C6 N2 H4 109.5 no C10 N2 H3 108.1 no C10 N2 H4 108.1 no C10 N2 C6 112.1(7) no H5 C1 H6 109 no C2 C1 H6 109.5 no C2 C1 H5 109.5 no N1 C1 H6 108.8 no N1 C1 H5 108.8 no N1 C1 C2 110.8(8) no H7 C2 H8 109 no C1 C2 H8 109 no C1 C2 H7 109 no C3 C2 H8 109 no C3 C2 H7 109 no C3 C2 C1 111.3(9) no H9 C3 H10 109 no C2 C3 H10 109 no C2 C3 H9 109 no C4 C3 H10 110 no C4 C3 H9 109 no C4 C3 C2 110.0(10) no H12 C4 H11 109 no C5 C4 H11 109 no C5 C4 H12 109 no C3 C4 H11 109 no C3 C4 H12 109 no C3 C4 C5 110.6(9) no H13 C5 H14 109.4 no N1 C5 H14 109.5 no N1 C5 H13 109.5 no C4 C5 H14 108.9 no C4 C5 H13 108.9 no C4 C5 N1 110.6(7) no H16 C6 H15 109 no N2 C6 H15 109.1 no N2 C6 H16 109 no C7 C6 H15 109 no C7 C6 H16 109.5 no C7 C6 N2 110.2(8) no H18 C7 H17 109 no C6 C7 H17 108.3 no C6 C7 H18 108.3 no C8 C7 H17 109.5 no C8 C7 H18 109 no C8 C7 C6 111.7(9) no H20 C8 H19 109 no C7 C8 H19 108 no C7 C8 H20 108.5 no C9 C8 H19 109.5 no C9 C8 H20 109 no C9 C8 C7 111.4(8) no H22 C9 H21 109.5 no C10 C9 H21 109.5 no C10 C9 H22 109 no C8 C9 H21 109.2 no C8 C9 H22 109.2 no C8 C9 C10 110.0(8) no H23 C10 H24 109 no N2 C10 H24 109.5 no N2 C10 H23 109.5 no C9 C10 H24 108.7 no C9 C10 H23 108.6 no C9 C10 N2 111.2(8) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Hg Cl1 . . 2.515(2) yes Hg Cl2 . . 2.485(2) yes Hg Cl3 . . 2.431(3) yes Hg Cl4 . . 2.475(3) yes N1 H1 . . .96 no N1 H2 . . .96 no N1 C1 . . 1.500(10) no N2 H3 . . .96 no N2 H4 . . .96 no N2 C6 . . 1.480(10) no C1 H5 . . .96 no C1 H6 . . .96 no C1 C2 . . 1.47(2) no C2 H7 . . .96 no C2 H8 . . .96 no C2 C3 . . 1.48(2) no C3 H9 . . .96 no C3 H10 . . .96 no C3 C4 . . 1.52(2) no C4 H11 . . .96 no C4 H12 . . .96 no C4 C5 . . 1.50(2) no C5 H13 . . .96 no C5 H14 . . .96 no C5 N1 . . 1.480(10) no C6 H15 . . .96 no C6 H16 . . .96 no C6 C7 . . 1.50(2) no C7 H17 . . .96 no C7 H18 . . .96 no C7 C8 . . 1.50(2) no C8 H19 . . .96 no C8 H20 . . .96 no C8 C9 . . 1.530(10) no C9 H21 . . .96 no C9 H22 . . .96 no C9 C10 . . 1.510(10) no C10 H23 . . .96 no C10 H24 . . .96 no C10 N2 . . 1.490(10) 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 N1 H1 Cl1 . .96 2.46 3.242(4) 138 yes N1 H2 Cl2 3_565 .96 2.27 3.219(4) 168 yes N2 H3 Cl3 . .96 2.36 3.239(5) 153 yes N2 H4 Cl1 4_555 .96 2.47 3.395(4) 161 yes