#------------------------------------------------------------------------------ #$Date: 2016-02-14 14:26:36 +0000 (Sun, 14 Feb 2016) $ #$Revision: 176435 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/61/2006144.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_2006144 loop_ _publ_author_name 'Ferguson, George' 'Spalding, Trevor R.' 'Herlihy, Emmet A.' _publ_section_title ; Dipotassium Hexaaquairon(II) Bis(sulfate)--Dipotassium Hexaaquanickel(II) Bis(sulfate) (0.07/0.93) ; _journal_issue 5 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first IUC9700002 _journal_paper_doi 10.1107/S010827019709954X _journal_volume 53 _journal_year 1997 _chemical_formula_iupac 'K2 [Ni0.93 Fe0.07 (H2 O)6] (S O4)2' _chemical_formula_moiety '2K, [Ni0.93 Fe0.07 (H2 O)6], 2(S O4) ' _chemical_formula_sum 'Fe0.07 H12 K2 Ni0.93 O14 S2' _chemical_formula_weight 436.92 _chemical_name_systematic ; Potassium Hexaaquanickel(II)/Hexaaquairon(II)(0.93/0.07) Sulfate ; _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 105.070(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 6.1276(7) _cell_length_b 12.1791(12) _cell_length_c 8.9973(12) _cell_measurement_reflns_used 25 _cell_measurement_temperature 294.0(10) _cell_measurement_theta_max 29.52 _cell_measurement_theta_min 20.02 _cell_volume 648.36(13) _computing_cell_refinement 'SET4 & CELDIM (Enraf-Nonius, 1992)' _computing_data_collection 'CAD4 (Enraf-Nonius, 1992)' _computing_data_reduction 'DATRD2 in NRCVAX96 (Gabe, Le Page, Charland, Lee & White, 1989)' _computing_molecular_graphics 'NRCVAX96, ORTEP (Johnson, 1976), PLATON (Spek, 1996a), PLUTON (Spek 1996b)' _computing_publication_material 'NRCVAX96, SHELXL93 and WordPerfect macro PRPCIF97 (Ferguson, 1997)' _computing_structure_refinement 'NRCVAX96 and SHELXL93 (Sheldrick, 1993)' _computing_structure_solution 'NRCVAX96 via Patterson heavy-atom method' _diffrn_ambient_temperature 294.0(10) _diffrn_measured_fraction_theta_full 1.0 _diffrn_measured_fraction_theta_max 1.0 _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method \q/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_type 'Molybdenum K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents 0.009 _diffrn_reflns_av_sigmaI/netI 0.0083 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 2157 _diffrn_reflns_theta_full 29.91 _diffrn_reflns_theta_max 29.91 _diffrn_reflns_theta_min 2.87 _diffrn_standards_decay_% 2.0 _diffrn_standards_interval_time 120 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 2.504 _exptl_absorpt_correction_T_max 0.4884 _exptl_absorpt_correction_T_min 0.3356 _exptl_absorpt_correction_type 'psi-scans at 4\% steps (North, Phillips & Mathews, 1968)' _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_crystal_colour pale_blue _exptl_crystal_density_diffrn 2.238 _exptl_crystal_density_meas ? _exptl_crystal_description 'block cut from a larger piece' _exptl_crystal_F_000 444 _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.25 _refine_diff_density_max 0.444 _refine_diff_density_min -0.415 _refine_ls_extinction_coef 0.0324(16) _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_all 1.176 _refine_ls_goodness_of_fit_ref 1.197 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 110 _refine_ls_number_reflns 1893 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.174 _refine_ls_restrained_S_obs 1.195 _refine_ls_R_factor_all 0.0220 _refine_ls_R_factor_gt 0.0204 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0255P)^2^+0.4210P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.0572 _refine_ls_wR_factor_ref 0.0567 _reflns_number_gt 1797 _reflns_number_total 1893 _reflns_threshold_expression >2\s(I) _cod_data_source_file qa0002.cif _cod_data_source_block 97-01 _cod_depositor_comments ; 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 The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w=1/[\s^2^(Fo^2^)+(0.0255P)^2^+0.4210P] where P=(Fo^2^+2Fc^2^)/3' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w=1/[\s^2^(Fo^2^)+(0.0255P)^2^+0.4210P] where P=(Fo^2^+2Fc^2^)/3'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_sg_symbol_H-M 'P 21/c' _cod_original_formula_sum 'H12 Fe0.07 K2 Ni0.93 O14 S2' _cod_database_code 2006144 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_disorder_group _atom_site_type_symbol Ni1 .0000 .0000 .0000 .01556(9) Uani d SP .93(2) . Ni Fe1 .0000 .0000 .0000 .01556(9) Uani d SP .07(2) . Fe K10 .34273(7) .34578(3) .13408(5) .03086(11) Uani d . 1 . K S2 .72635(6) .13518(3) .41174(4) .01848(10) Uani d . 1 . S O3 .5750(2) .22979(10) .4094(2) .0340(3) Uani d . 1 . O O4 .7556(3) .07508(13) .55642(15) .0400(3) Uani d . 1 . O O5 .6187(2) .06153(10) .28373(13) .0251(2) Uani d . 1 . O O6 .9472(2) .17388(10) .39375(15) .0281(3) Uani d . 1 . O O7 .1629(2) .11108(10) .16724(13) .0235(2) Uani d D 1 . O O8 .0356(2) .11242(9) -.16628(13) .0225(2) Uani d D 1 . O O9 .3014(2) -.06656(9) .00025(14) .0229(2) Uani d D 1 . O H15 .2887 .0904 .2085 .040(3) Uiso d D 1 . H H16 .1006 .1229 .2340 .040(3) Uiso d D 1 . H H17 -.0489 .1005 -.2493 .040(3) Uiso d D 1 . H H18 .0109 .1746 -.1455 .040(3) Uiso d D 1 . H H19 .3403 -.0637 -.0784 .040(3) Uiso d D 1 . H H20 .3294 -.1299 .0224 .040(3) Uiso d 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 Ni1 .01607(13) .01619(14) .01425(13) .00002(8) .00366(9) -.00086(8) Fe1 .01607(13) .01619(14) .01425(13) .00002(8) .00366(9) -.00086(8) K10 .0304(2) .0316(2) .0326(2) -.00018(14) .01185(14) -.00217(14) S2 .0191(2) .0196(2) .0164(2) -.00188(12) .00422(12) -.00223(11) O3 .0255(6) .0260(6) .0503(8) .0020(5) .0097(5) -.0114(5) O4 .0448(8) .0519(8) .0198(6) -.0098(7) .0022(5) .0087(6) O5 .0275(6) .0268(5) .0214(5) -.0053(4) .0068(4) -.0077(4) O6 .0212(5) .0264(6) .0380(7) -.0047(4) .0102(5) -.0038(5) O7 .0214(5) .0262(5) .0216(5) -.0005(4) .0033(4) -.0060(4) O8 .0276(5) .0219(5) .0185(5) .0003(4) .0066(4) .0015(4) O9 .0217(5) .0224(5) .0266(5) .0030(4) .0096(4) .0015(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ni Ni 0.3393 1.1124 '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' K K 0.2009 0.2494 '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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 4 3 0 4 -3 -2 5 0 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 O9 Ni1 O9 3 . 180.0 no O9 Ni1 O7 3 . 90.38(5) no O9 Ni1 O7 . . 89.62(5) no O9 Ni1 O7 3 3 89.62(5) no O9 Ni1 O7 . 3 90.38(5) no O7 Ni1 O7 . 3 180.0 no O9 Ni1 O8 3 . 90.10(5) no O9 Ni1 O8 . . 89.90(5) no O7 Ni1 O8 . . 88.38(5) no O7 Ni1 O8 3 . 91.62(5) no O9 Ni1 O8 3 3 89.90(5) no O9 Ni1 O8 . 3 90.10(5) no O7 Ni1 O8 . 3 91.62(5) no O7 Ni1 O8 3 3 88.38(5) no O8 Ni1 O8 . 3 180.0 no O9 Fe1 O9 3 . 180.0 no O9 Fe1 O7 3 . 90.38(5) no O9 Fe1 O7 . . 89.62(5) no O9 Fe1 O7 3 3 89.62(5) no O9 Fe1 O7 . 3 90.38(5) no O7 Fe1 O7 . 3 180.0 no O9 Fe1 O8 3 . 90.10(5) no O9 Fe1 O8 . . 89.90(5) no O7 Fe1 O8 . . 88.38(5) no O7 Fe1 O8 3 . 91.62(5) no O9 Fe1 O8 3 3 89.90(5) no O9 Fe1 O8 . 3 90.10(5) no O7 Fe1 O8 . 3 91.62(5) no O7 Fe1 O8 3 3 88.38(5) no O8 Fe1 O8 . 3 180.0 no O5 K10 O6 2_655 4_465 106.74(4) no O5 K10 O3 2_655 . 104.52(4) no O6 K10 O3 4_465 . 138.93(4) no O5 K10 O3 2_655 4_565 118.08(4) no O6 K10 O3 4_465 4_565 85.31(4) no O3 K10 O3 . 4_565 102.74(3) no O5 K10 O4 2_655 4_565 74.36(4) no O6 K10 O4 4_465 4_565 117.80(4) no O3 K10 O4 . 4_565 95.80(4) no O3 K10 O4 4_565 4_565 48.33(4) no O5 K10 O8 2_655 4_566 72.16(3) no O6 K10 O8 4_465 4_566 85.66(4) no O3 K10 O8 . 4_566 79.22(4) no O3 K10 O8 4_565 4_566 168.05(4) no O4 K10 O8 4_565 4_566 143.57(4) no O5 K10 O7 2_655 . 150.45(3) no O6 K10 O7 4_465 . 74.85(3) no O3 K10 O7 . . 64.85(3) no O3 K10 O7 4_565 . 91.46(3) no O4 K10 O7 4_565 . 132.04(4) no O8 K10 O7 4_566 . 78.63(3) no O5 K10 O4 2_655 2_655 45.99(3) no O6 K10 O4 4_465 2_655 70.28(4) no O3 K10 O4 . 2_655 148.87(4) no O3 K10 O4 4_565 2_655 87.85(4) no O4 K10 O4 4_565 2_655 69.39(5) no O8 K10 O4 4_566 2_655 96.44(4) no O7 K10 O4 . 2_655 145.06(4) no O3 S2 O4 . . 109.54(9) no O3 S2 O5 . . 108.19(7) no O3 S2 O6 . . 109.79(7) no O4 S2 O5 . . 108.50(8) no O4 S2 O6 . . 110.62(8) no O5 S2 O6 . . 110.14(7) no S2 O3 K10 . . 124.22(8) no S2 O3 K10 . 4_566 99.34(7) no K10 O3 K10 . 4_566 122.04(5) no S2 O4 K10 . 4_566 97.62(8) no S2 O4 K10 . 2_645 89.86(7) no K10 O4 K10 4_566 2_645 110.61(5) no S2 O5 K10 . 2_645 112.68(6) no S2 O6 K10 . 4_666 121.27(7) no Fe1 O7 K10 . . 130.24(5) no Ni1 O7 K10 . . 130.24(5) no Fe1 O8 K10 . 4_565 138.63(5) no Ni1 O8 K10 . 4_565 138.63(5) no H15 O7 H16 . . 107 ? H17 O8 H18 . . 106 ? H19 O9 H20 . . 100 ? 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 Ni1 O7 . 2.0761(11) yes Ni1 O7 3 2.0761(11) no Ni1 O8 . 2.0809(11) yes Ni1 O8 3 2.0809(11) no Ni1 O9 . 2.0162(11) yes Ni1 O9 3 2.0162(11) no Fe1 O7 . 2.0761(11) no Fe1 O7 3 2.0761(11) no Fe1 O8 . 2.0809(11) no Fe1 O8 3 2.0809(11) no Fe1 O9 3 2.0162(11) no Fe1 O9 . 2.0162(11) no K10 O3 . 2.885(2) yes K10 O3 4_565 2.908(2) yes K10 O4 4_565 2.956(2) yes K10 O4 2_655 3.250(2) yes K10 O5 2_655 2.7233(13) yes K10 O6 4_465 2.8075(14) yes K10 O7 . 3.1055(13) yes K10 O8 4_566 2.9641(12) yes S2 O3 . 1.4759(13) no S2 O4 . 1.4632(13) no S2 O5 . 1.4734(11) no S2 O6 . 1.4809(12) no O3 K10 4_566 2.908(2) no O4 K10 4_566 2.956(2) no O4 K10 2_645 3.250(2) no O5 K10 2_645 2.7233(13) no O6 K10 4_666 2.8076(14) no O8 K10 4_565 2.9641(12) 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 O7 H15 O5 . 0.80 1.99 2.7823(18) 168 yes O7 H16 O6 1_455 0.80 2.01 2.8082(18) 172 yes O8 H17 O4 1_454 0.80 1.87 2.6738(19) 179 yes O8 H18 O6 4_465 0.80 1.94 2.7407(17) 178 yes O9 H19 O5 3_655 0.80 1.93 2.7244(17) 171 yes O9 H20 O3 2_645 0.80 1.86 2.6582(17) 173 yes