#------------------------------------------------------------------------------ #$Date: 2013-08-29 18:37:19 +0300 (Thu, 29 Aug 2013) $ #$Revision: 88064 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/24/2012436.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_2012436 loop_ _publ_author_name 'Matkovi\'c-\O,N,O')mercury(II) _journal_issue 1 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first m39 _journal_page_last m40 _journal_volume 58 _journal_year 2002 _chemical_formula_iupac '[Hg Br (C7 H4 N O4) (H2 O)]' _chemical_formula_moiety 'C7 H6 Br Hg N O5' _chemical_formula_sum 'C7 H6 Br Hg N O5' _chemical_formula_weight 464.63 _chemical_name_common aquabromo(hydrogenpicolinato)mercury(II) _chemical_name_systematic ; Aquabromo(6-carboxypyridine-2-carboxylato-O,N,O')mercury(II) ; _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_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 91.05(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 6.967(3) _cell_length_b 9.068(3) _cell_length_c 16.007(5) _cell_measurement_reflns_used 56 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 19 _cell_measurement_theta_min 10 _cell_volume 1011.1(6) _computing_cell_refinement STADI4 _computing_data_collection 'STADI4 (Stoe & Cie, 1995)' _computing_data_reduction 'X-RED (Stoe & Cie, 1995)' _computing_molecular_graphics 'PLATON98 (Spek, 1990)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full .936 _diffrn_measured_fraction_theta_max .900 _diffrn_measurement_device_type 'Philips PW1100 updated by Stoe' _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 .030 _diffrn_reflns_av_sigmaI/netI .042 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 4339 _diffrn_reflns_theta_full 27.50 _diffrn_reflns_theta_max 29.99 _diffrn_reflns_theta_min 3.21 _diffrn_standards_decay_% 2.2 _diffrn_standards_interval_time 90 _diffrn_standards_number 5 _exptl_absorpt_coefficient_mu 19.174 _exptl_absorpt_correction_T_max .091 _exptl_absorpt_correction_T_min .031 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details '(X-RED; Stoe & Cie, 1995)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 3.052 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_description Parallelepiped _exptl_crystal_F_000 840 _exptl_crystal_size_max .28 _exptl_crystal_size_mid .28 _exptl_crystal_size_min .22 _refine_diff_density_max .98 _refine_diff_density_min -.97 _refine_ls_extinction_coef .00157(14) _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 .992 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 149 _refine_ls_number_reflns 2658 _refine_ls_number_restraints 3 _refine_ls_restrained_S_all .992 _refine_ls_R_factor_all .060 _refine_ls_R_factor_gt .028 _refine_ls_shift/su_max .001 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0312P)^2^+0.6877P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt .058 _refine_ls_wR_factor_ref .066 _reflns_number_gt 1907 _reflns_number_total 2658 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file jz1482.cif _[local]_cod_data_source_block I _[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 ; _cod_database_code 2012436 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -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 Hg .04957(3) .02939(2) .278042(14) .03554(9) Uani d . 1 . . Hg Br1 .19617(10) -.04826(8) .40844(4) .04991(17) Uani d . 1 . . Br N -.1059(6) .0594(5) .1578(3) .0297(9) Uani d . 1 . . N O1 -.0253(6) .2893(5) .2626(3) .0451(10) Uani d . 1 . . O O2 -.1743(6) .4440(4) .1759(3) .0486(11) Uani d . 1 . . O O3 -.1577(7) -.3122(5) .0919(3) .0517(11) Uani d D 1 . . O H31 -.134(13) -.399(4) .109(6) .10(3) Uiso d D 1 . . H O4 -.0080(6) -.2228(5) .2047(3) .0458(10) Uani d . 1 . . O O5 .3513(7) .0505(5) .1820(3) .0464(10) Uani d D 1 . . O H51 .422(10) .117(7) .204(5) .09(3) Uiso d D 1 . . H H52 .423(11) -.025(6) .188(7) .10(4) Uiso d D 1 . . H C1 -.1473(7) -.0565(5) .1067(3) .0283(11) Uani d . 1 . . C C2 -.2330(8) -.0351(7) .0290(4) .0400(13) Uani d . 1 . . C H2 -.2595 -.1146 -.0060 .048 Uiso calc R 1 . . H C3 -.2782(8) .1075(7) .0047(4) .0418(14) Uani d . 1 . . C H3 -.3345 .1242 -.0476 .050 Uiso calc R 1 . . H C4 -.2414(8) .2228(7) .0565(4) .0422(14) Uani d . 1 . . C H4 -.2740 .3184 .0406 .051 Uiso calc R 1 . . H C5 -.1534(7) .1955(6) .1340(4) .0319(11) Uani d . 1 . . C C6 -.1130(8) .3199(6) .1953(4) .0385(13) Uani d . 1 . . C C7 -.0960(8) -.2054(6) .1392(4) .0349(12) Uani d . 1 . . C 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 .04376(12) .03023(11) .03230(14) .00064(10) -.00815(8) .00045(10) Br1 .0570(4) .0622(5) .0302(3) .0011(3) -.0106(3) .0019(3) N .0314(19) .025(2) .033(3) -.0021(16) -.0015(17) .0032(18) O1 .064(3) .027(2) .043(3) .0002(19) -.010(2) -.0040(18) O2 .054(2) .025(2) .068(3) .0013(17) .008(2) .006(2) O3 .086(3) .026(2) .043(3) -.003(2) -.017(2) -.0049(19) O4 .064(3) .029(2) .043(3) .0034(19) -.020(2) .0011(18) O5 .051(2) .039(3) .049(3) .001(2) -.004(2) .001(2) C1 .032(2) .025(3) .028(3) -.0027(18) -.001(2) .0016(19) C2 .042(3) .040(3) .038(3) -.005(3) -.004(2) .002(3) C3 .044(3) .045(4) .036(3) .002(3) -.009(2) .015(3) C4 .045(3) .038(3) .043(4) .005(2) .000(3) .015(3) C5 .032(2) .028(3) .035(3) -.001(2) .002(2) .002(2) C6 .038(3) .031(3) .048(4) .003(2) .011(3) .006(3) C7 .040(3) .029(3) .036(3) -.003(2) .000(2) -.004(2) 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 N . 2.208(5) yes Hg Br1 . 2.4120(10) yes Hg O1 . 2.425(4) yes Hg O4 . 2.599(4) yes Hg O5 . 2.634(5) yes N C5 . 1.332(7) ? N C1 . 1.358(7) ? O1 C6 . 1.260(8) ? O2 C6 . 1.241(7) ? O3 C7 . 1.298(7) ? O3 H31 . .85(5) ? O4 C7 . 1.215(6) ? O5 H51 . .85(7) ? O5 H52 . .85(7) ? C1 C2 . 1.383(8) ? C1 C7 . 1.488(8) ? C2 C3 . 1.385(8) ? C2 H2 . .9300 ? C3 C4 . 1.356(9) ? C3 H3 . .9300 ? C4 C5 . 1.396(8) ? C4 H4 . .9300 ? C5 C6 . 1.518(8) ? 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' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -.2901 2.4595 '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' 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 N Hg Br1 169.57(11) yes N Hg O1 71.98(15) yes Br1 Hg O1 117.29(11) yes N Hg O4 69.22(14) yes Br1 Hg O4 101.16(9) yes O1 Hg O4 141.10(13) yes N Hg O5 82.31(16) yes Br1 Hg O5 101.33(11) yes O1 Hg O5 92.44(14) yes O4 Hg O5 85.32(15) yes C5 N C1 119.7(5) ? C5 N Hg 118.6(4) ? C1 N Hg 121.6(3) ? C6 O1 Hg 113.6(4) ? C7 O3 H31 117(7) ? C7 O4 Hg 110.3(4) ? Hg O5 H51 106(6) ? Hg O5 H52 110(6) ? H51 O5 H52 101(9) ? N C1 C2 121.1(5) ? N C1 C7 116.4(5) ? C2 C1 C7 122.6(5) ? C1 C2 C3 118.4(6) ? C1 C2 H2 120.8 ? C3 C2 H2 120.8 ? C4 C3 C2 120.6(5) ? C4 C3 H3 119.7 ? C2 C3 H3 119.7 ? C3 C4 C5 118.8(5) ? C3 C4 H4 120.6 ? C5 C4 H4 120.6 ? N C5 C4 121.4(5) ? N C5 C6 117.5(5) ? C4 C5 C6 121.1(5) ? O2 C6 O1 124.9(6) ? O2 C6 C5 116.9(6) ? O1 C6 C5 118.1(5) ? O4 C7 O3 124.2(6) ? O4 C7 C1 122.3(5) ? O3 C7 C1 113.5(5) ? 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 O3 H31 O2 1_545 .85(5) 1.81(7) 2.591(6) 153(9) yes O5 H51 O4 2_555 .85(7) 2.14(7) 2.938(7) 157(7) yes O5 H52 O1 2_545 .86(7) 1.99(7) 2.798(7) 159(8) yes _cod_database_fobs_code 2012436