#------------------------------------------------------------------------------ #$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2011230.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_2011230 loop_ _publ_author_name 'Zeng, Xi-Rui' 'Xiong, Ren-Geng' 'Xu, Yan' 'Liu, Yong-Jiang' 'You, Xiao-Zeng' _publ_section_title ; Tetraaquabis[2-(4-pyridyl)ethanesulfonato-N]zinc(II) ; _journal_issue 8 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 943 _journal_page_last 944 _journal_volume 56 _journal_year 2000 _chemical_formula_iupac '[Zn (C7 H8 NO3 S)2 (H2 O)4 ]' _chemical_formula_moiety 'C14 H24 N2 O10 S2 Zn' _chemical_formula_sum 'C14 H24 N2 O10 S2 Zn' _chemical_formula_weight 509.84 _chemical_name_systematic ; Bis(4-Pyridineethanesulfonato-N) Tetraaquazinc ; _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' _cell_angle_alpha 90.00 _cell_angle_beta 94.910(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 9.0967(14) _cell_length_b 8.8122(13) _cell_length_c 12.5396(14) _cell_measurement_reflns_used 45 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 11.78 _cell_measurement_theta_min 5.16 _cell_volume 1001.5(2) _computing_cell_refinement XSCANS _computing_data_collection 'XSCANS (Siemens, 1994)' _computing_data_reduction 'SHELXTL (Sheldrick, 1997)' _computing_publication_material SHELXTL _computing_structure_refinement SHELXTL _computing_structure_solution SHELXTL _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full .900 _diffrn_measured_fraction_theta_max .900 _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '2\q/\w scans' _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 .0232 _diffrn_reflns_av_sigmaI/netI .0319 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 2411 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_min 2.25 _diffrn_standards_decay_% 6.11 _diffrn_standards_interval_count 97 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.491 _exptl_absorpt_correction_T_max .800 _exptl_absorpt_correction_T_min .618 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details '(North et al., 1968)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.691 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Block _exptl_crystal_F_000 528 _exptl_crystal_size_max .60 _exptl_crystal_size_mid .40 _exptl_crystal_size_min .15 _refine_diff_density_max .757 _refine_diff_density_min -.558 _refine_ls_extinction_coef .0129(17) _refine_ls_extinction_method 'SHELXTL (Sheldrick, 1997)' _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 134 _refine_ls_number_reflns 1765 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.181 _refine_ls_R_factor_all .0370 _refine_ls_R_factor_gt .0329 _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^)+(0.0494P)^2^+1.0422P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .0915 _reflns_number_gt 1429 _reflns_number_total 1765 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file na1464.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P2(1)/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_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2011230 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 Zn1 .0000 .0000 .5000 .0225(2) Uani d S 1 Zn S1 -.75531(10) .05693(10) .90620(6) .0267(3) Uani d . 1 S N1 -.1723(3) .0233(3) .6004(2) .0230(6) Uani d . 1 N O1 -.8216(4) -.0820(3) .9369(2) .0524(8) Uani d U 1 O O2 -.6995(3) .1494(3) .99661(18) .0388(7) Uani d . 1 O O3 -.8524(3) .1444(3) .82937(17) .0340(6) Uani d . 1 O O1W -.0704(3) .2054(3) .42483(18) .0312(6) Uani d . 1 O H3 -.1028 .2746 .4644 .047 Uiso d R 1 H H4 -.0053 .2458 .3884 .047 Uiso d R 1 H O2W .1542(3) .1264(3) .60733(17) .0345(6) Uani d . 1 O H1 .1931 .2043 .5804 .052 Uiso d R 1 H H2 .1491 .1431 .6739 .052 Uiso d R 1 H C1 -.3056(4) .0726(4) .5596(3) .0270(8) Uani d . 1 C H1A -.3225 .0823 .4857 .032 Uiso calc R 1 H C2 -.4177(4) .1094(4) .6214(3) .0292(8) Uani d . 1 C H2A -.5078 .1430 .5893 .035 Uiso calc R 1 H C3 -.3963(4) .0964(4) .7318(3) .0282(8) Uani d . 1 C C4 -.2609(4) .0404(4) .7735(3) .0300(8) Uani d . 1 C H4A -.2426 .0263 .8470 .036 Uiso calc R 1 H C5 -.1534(4) .0057(4) .7065(3) .0266(8) Uani d . 1 C H5A -.0636 -.0317 .7364 .032 Uiso calc R 1 H C6 -.5137(4) .1420(4) .8033(3) .0364(9) Uani d . 1 C H6A -.5802 .2142 .7659 .044 Uiso calc R 1 H H6B -.4679 .1914 .8668 .044 Uiso calc R 1 H C7 -.6011(4) .0055(4) .8362(3) .0290(8) Uani d . 1 C H7A -.5367 -.0601 .8813 .035 Uiso calc R 1 H H7B -.6354 -.0515 .7727 .035 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 Zn1 .0216(3) .0265(3) .0207(3) .0009(2) .0092(2) .0007(2) S1 .0275(5) .0297(5) .0250(4) .0024(4) .0138(3) .0023(3) N1 .0205(15) .0282(15) .0210(13) .0000(12) .0069(11) -.0015(11) O1 .0546(12) .0493(11) .0569(11) -.0025(9) .0247(9) .0042(9) O2 .0363(15) .0558(17) .0247(11) .0112(13) .0046(10) -.0077(11) O3 .0285(15) .0479(16) .0265(11) .0077(12) .0073(10) -.0024(10) O1W .0324(14) .0287(13) .0346(12) .0028(11) .0150(10) .0046(10) O2W .0403(16) .0416(14) .0226(11) -.0130(12) .0079(10) -.0030(10) C1 .0245(19) .0338(19) .0229(15) .0009(16) .0038(14) .0003(13) C2 .0196(18) .0317(18) .0369(18) .0006(15) .0057(15) .0007(15) C3 .0284(19) .0221(16) .0368(17) -.0057(15) .0173(15) -.0035(14) C4 .034(2) .0355(18) .0218(16) -.0034(17) .0090(15) -.0030(14) C5 .0218(19) .0322(18) .0262(16) -.0014(14) .0035(14) -.0005(13) C6 .035(2) .0319(19) .046(2) -.0029(17) .0221(17) -.0083(16) C7 .030(2) .0265(17) .0334(18) .0057(15) .0161(15) .0009(14) 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' Zn Zn .2839 1.4301 '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 N1 Zn1 N1 3_556 . 180.0 N1 Zn1 O1W 3_556 . 91.68(10) N1 Zn1 O1W . . 88.32(10) N1 Zn1 O1W 3_556 3_556 88.32(10) N1 Zn1 O1W . 3_556 91.68(10) O1W Zn1 O1W . 3_556 180.0 N1 Zn1 O2W 3_556 3_556 93.10(10) N1 Zn1 O2W . 3_556 86.90(10) O1W Zn1 O2W . 3_556 90.46(9) O1W Zn1 O2W 3_556 3_556 89.54(9) N1 Zn1 O2W 3_556 . 86.90(10) N1 Zn1 O2W . . 93.10(10) O1W Zn1 O2W . . 89.54(9) O1W Zn1 O2W 3_556 . 90.46(9) O2W Zn1 O2W 3_556 . 180.0 O1 S1 O2 . . 113.39(17) O1 S1 O3 . . 112.45(18) O2 S1 O3 . . 111.58(15) O1 S1 C7 . . 106.45(17) O2 S1 C7 . . 106.94(17) O3 S1 C7 . . 105.40(15) C5 N1 C1 . . 116.7(3) C5 N1 Zn1 . . 123.1(2) C1 N1 Zn1 . . 119.8(2) N1 C1 C2 . . 123.4(3) C1 C2 C3 . . 119.8(3) C2 C3 C4 . . 116.7(3) C2 C3 C6 . . 121.8(3) C4 C3 C6 . . 121.5(3) C5 C4 C3 . . 120.2(3) N1 C5 C4 . . 123.0(3) C3 C6 C7 . . 111.4(3) C6 C7 S1 . . 112.7(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance Zn1 N1 3_556 2.102(3) Zn1 N1 . 2.102(3) Zn1 O1W . 2.114(2) Zn1 O1W 3_556 2.114(2) Zn1 O2W 3_556 2.167(2) Zn1 O2W . 2.167(2) S1 O1 . 1.432(3) S1 O2 . 1.452(3) S1 O3 . 1.469(3) S1 C7 . 1.776(4) N1 C5 . 1.336(4) N1 C1 . 1.347(4) C1 C2 . 1.372(5) C2 C3 . 1.386(5) C3 C4 . 1.387(5) C3 C6 . 1.506(5) C4 C5 . 1.377(5) C6 C7 . 1.518(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 O2W H1 O2 4_665 .85(5) 1.97(4) 2.814(4) 167(2) yes O2W H2 O3 1_655 .85(3) 1.950(10) 2.795(3) 170.0(10) yes O1W H3 O1 2_456 .85(4) 1.93(6) 2.788(4) 175.0(10) yes O1W H4 O3 4_665 .85(6) 1.89(6) 2.743(4) 170.0(10) yes C4 H4A O2 3_457 .930(10) 2.58(8) 3.379(4) 143.0(10) yes