#------------------------------------------------------------------------------ #$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2200739.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_2200739 loop_ _publ_author_name 'Batsanov, Andrei S.' 'Howard, Judith A. K.' 'Moore, Nichola S.' 'Kilner, Melvyn' _publ_section_title ; Hexaaquanickel(II) bis(p-tolylsulfonate) ; _journal_issue 10 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m485 _journal_page_last m487 _journal_volume 57 _journal_year 2001 _chemical_formula_iupac '[Ni (H2 O1)6] (C7 H7 O3 S)2' _chemical_formula_moiety 'Ni O6 H12 2+,2(C7 H7 O3 S 1-)' _chemical_formula_sum 'C14 H26 Ni O12 S2' _chemical_formula_weight 509.18 _chemical_name_systematic ; Hexaaquanickel(II) bis(p-tolylsulfonate) ; _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' _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.719(15) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 6.9140(10) _cell_length_b 6.2990(10) _cell_length_c 24.933(4) _cell_measurement_reflns_used 448 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 20 _cell_measurement_theta_min 10 _cell_volume 1085.8(3) _computing_cell_refinement SMART _computing_data_collection 'SMART (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_molecular_graphics 'SHELXTL (Bruker, 1997)' _computing_publication_material SHELXTL _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 150(2) _diffrn_detector_area_resol_mean 8 _diffrn_measured_fraction_theta_full .989 _diffrn_measured_fraction_theta_max .989 _diffrn_measurement_device_type 'SMART 1K CCD area-detector' _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 .055 _diffrn_reflns_av_sigmaI/netI .051 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_number 8262 _diffrn_reflns_theta_full 28.99 _diffrn_reflns_theta_max 29.0 _diffrn_reflns_theta_min 1.63 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.142 _exptl_absorpt_correction_T_max .9451 _exptl_absorpt_correction_T_min .7633 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details '(XPREP SHELXTL; Bruker, 1997)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.557 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 532 _exptl_crystal_size_max .25 _exptl_crystal_size_mid .10 _exptl_crystal_size_min .05 _refine_diff_density_max .547 _refine_diff_density_min -.481 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.191 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 185 _refine_ls_number_reflns 2864 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.191 _refine_ls_R_factor_all .0761 _refine_ls_R_factor_gt .0501 _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^)+(0.0083P)^2^+2.4432P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .1005 _reflns_number_gt 2253 _reflns_number_total 2864 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file om6052.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_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2200739 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_type_symbol Ni .5000 .5000 .0000 .01655(14) Uani d S 1 Ni S -.01007(11) .10018(12) .09502(3) .01774(17) Uani d . 1 S O1 .2584(4) .5957(5) .04068(13) .0389(7) Uani d . 1 O H011 .233(7) .715(8) .0493(19) .054(15) Uiso d . 1 H H012 .187(6) .519(7) .0570(16) .035(11) Uiso d . 1 H O2 .6817(4) .5971(4) .06173(11) .0314(6) Uani d . 1 O H021 .790(8) .518(9) .064(2) .074(17) Uiso d . 1 H H022 .728(6) .723(8) .0622(18) .051(14) Uiso d . 1 H O3 .4859(4) .2076(4) .03275(10) .0258(5) Uani d . 1 O H031 .589(7) .158(8) .0472(18) .058(15) Uiso d . 1 H H032 .386(7) .150(7) .0455(18) .053(14) Uiso d . 1 H O4 -.1902(3) .0109(4) .07327(9) .0250(5) Uani d . 1 O O5 .1605(3) .0066(4) .07035(8) .0240(5) Uani d . 1 O O6 -.0082(3) .3329(3) .09292(9) .0234(5) Uani d . 1 O C1 -.0003(4) .0274(5) .16377(12) .0194(6) Uani d . 1 C C2 -.0562(5) .1690(6) .20302(14) .0259(7) Uani d . 1 C H2 -.090(6) .312(7) .1936(15) .038(11) Uiso d . 1 H C3 -.0495(5) .1079(7) .25688(14) .0304(8) Uani d . 1 C H3 -.077(6) .211(7) .2840(17) .052(13) Uiso d . 1 H C4 .0131(5) -.0932(6) .27168(13) .0274(7) Uani d . 1 C C5 .0660(5) -.2344(6) .23150(14) .0291(8) Uani d . 1 C H5 .116(5) -.373(6) .2418(13) .021(9) Uiso d . 1 H C6 .0603(5) -.1769(6) .17783(14) .0257(7) Uani d . 1 C H6 .101(6) -.271(7) .1525(16) .045(12) Uiso d . 1 H C7 .0302(7) -.1585(9) .32990(16) .0406(10) Uani d . 1 C H71 -.015(8) -.304(10) .335(2) .082(19) Uiso d . 1 H H72 .159(8) -.145(8) .3437(19) .065(15) Uiso d . 1 H H73 -.043(7) -.067(8) .3499(18) .054(14) Uiso d . 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 Ni .0162(2) .0104(2) .0231(3) -.0002(2) .00174(19) -.0008(2) S .0188(3) .0122(3) .0222(4) -.0008(3) .0002(3) .0001(3) O1 .0370(15) .0158(13) .065(2) .0014(12) .0306(14) .0010(14) O2 .0340(14) .0158(12) .0441(15) -.0008(11) -.0138(12) -.0027(12) O3 .0214(12) .0161(11) .0398(14) -.0007(10) -.0001(11) .0071(11) O4 .0249(11) .0176(11) .0322(12) -.0035(10) -.0082(9) .0037(11) O5 .0259(11) .0189(11) .0273(11) .0012(10) .0072(9) .0000(11) O6 .0258(11) .0123(10) .0320(12) -.0007(9) -.0007(9) .0022(10) C1 .0158(13) .0182(16) .0244(15) -.0001(12) .0012(11) .0007(13) C2 .0249(16) .0234(17) .0292(17) .0038(14) -.0009(13) -.0032(15) C3 .0273(18) .038(2) .0255(18) .0070(16) -.0013(14) -.0064(17) C4 .0196(15) .041(2) .0218(16) -.0020(15) -.0009(12) .0005(16) C5 .0300(18) .0269(19) .0303(18) .0006(15) -.0002(14) .0059(16) C6 .0303(17) .0224(17) .0244(16) .0026(14) .0029(13) .0016(15) C7 .038(2) .057(3) .0263(19) .001(2) -.0036(17) .006(2) 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' 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' Ni Ni .3393 1.1124 '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 O3 Ni O3 3_665 . 180.00(13) ? O3 Ni O1 3_665 . 88.61(11) ? O3 Ni O1 . . 91.39(11) yes O3 Ni O1 3_665 3_665 91.39(11) ? O3 Ni O1 . 3_665 88.61(11) ? O1 Ni O1 . 3_665 180.00(15) ? O3 Ni O2 3_665 3_665 90.04(11) ? O3 Ni O2 . 3_665 89.96(11) ? O1 Ni O2 . 3_665 87.94(12) ? O1 Ni O2 3_665 3_665 92.06(12) ? O3 Ni O2 3_665 . 89.96(11) ? O3 Ni O2 . . 90.04(11) yes O1 Ni O2 . . 92.06(12) yes O1 Ni O2 3_665 . 87.94(12) ? O2 Ni O2 3_665 . 180.00(10) ? O5 S O4 . . 112.11(14) yes O5 S O6 . . 112.38(14) yes O4 S O6 . . 112.23(14) yes O5 S C1 . . 106.33(14) yes O4 S C1 . . 106.27(14) yes O6 S C1 . . 107.01(14) yes Ni O1 H011 . . 126(3) ? Ni O1 H012 . . 125(3) ? H011 O1 H012 . . 107(4) ? Ni O2 H021 . . 112(3) ? Ni O2 H022 . . 121(3) ? H021 O2 H022 . . 101(4) ? Ni O3 H031 . . 117(3) ? Ni O3 H032 . . 126(3) ? H031 O3 H032 . . 112(4) ? C2 C1 C6 . . 120.2(3) ? C2 C1 S . . 120.6(3) ? C6 C1 S . . 119.2(2) ? C1 C2 C3 . . 119.7(3) ? C1 C2 H2 . . 120(2) ? C3 C2 H2 . . 120(2) ? C4 C3 C2 . . 120.9(3) ? C4 C3 H3 . . 120(3) ? C2 C3 H3 . . 119(3) ? C3 C4 C5 . . 118.4(3) ? C3 C4 C7 . . 121.6(4) ? C5 C4 C7 . . 119.9(4) ? C6 C5 C4 . . 121.5(3) ? C6 C5 H5 . . 120(2) ? C4 C5 H5 . . 119(2) ? C5 C6 C1 . . 119.2(3) ? C5 C6 H6 . . 119(3) ? C1 C6 H6 . . 121(3) ? C4 C7 H71 . . 111(3) ? C4 C7 H72 . . 113(3) ? H71 C7 H72 . . 110(4) ? C4 C7 H73 . . 108(3) ? H71 C7 H73 . . 110(4) ? H72 C7 H73 . . 105(4) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Ni O3 2.018(2) yes Ni O1 2.056(3) yes Ni O2 2.067(3) yes S O5 1.461(2) yes S O4 1.465(2) yes S O6 1.467(2) yes S C1 1.775(3) yes O1 H011 .80(5) ? O1 H012 .80(4) ? O2 H021 .90(6) ? O2 H022 .85(5) ? O3 H031 .86(5) ? O3 H032 .85(5) ? C1 C2 1.383(4) ? C1 C6 1.396(4) ? C2 C3 1.397(5) ? C2 H2 .96(4) ? C3 C4 1.387(5) ? C3 H3 .96(4) ? C4 C5 1.392(5) ? C4 C7 1.512(5) ? C5 C6 1.386(5) ? C5 H5 .97(4) ? C6 H6 .91(4) ? C7 H71 .98(6) ? C7 H72 .96(5) ? C7 H73 .92(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 O1 H011 O5 1_565 .80(5) 1.98(5) 2.778(4) 178(5) O1 H012 O6 . .80(4) 2.01(4) 2.810(4) 175(4) O2 H021 O6 1_655 .90(6) 1.95(6) 2.816(3) 161(5) O2 H022 O4 1_665 .85(5) 1.92(5) 2.767(4) 171(4) O3 H031 O4 1_655 .86(5) 1.89(5) 2.741(3) 171(5) O3 H032 O5 . .85(5) 1.91(5) 2.756(3) 176(5)