#------------------------------------------------------------------------------ #$Date: 2011-09-10 06:16:28 +0300 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2102085.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_2102085 loop_ _publ_author_name 'Figgis, Brian N.' 'Sobolev, Alexandre N.' 'Simmons, Charles J.' 'Hitchman, Michael A.' 'Stratemeier, Horst' 'Riley, Mark J.' _publ_section_title ; Bonding effects and the crystal structures of (NH~4~)~2~[Cu(H~2~O)~6~](SO~4~)~2~ and its H~2~^18^O substituted form at 9.5K ; _journal_issue 3 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 438 _journal_page_last 443 _journal_volume 56 _journal_year 2000 _chemical_formula_iupac '(N H4)2[Cu(H2 ^18^O)6](S O4)2' _chemical_formula_sum 'Cu H20 N2 O14 S2' _chemical_formula_weight 411.84 _chemical_name_common 'Ammonium copper Tutton salt (18-O water)' _chemical_name_systematic ; ? ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yab' _symmetry_space_group_name_H-M 'P 1 21/a 1' _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 106.277(5) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 9.0921(6) _cell_length_b 12.2195(8) _cell_length_c 6.3442(5) _cell_measurement_reflns_used 12 _cell_measurement_temperature 9.5(2) _cell_measurement_theta_max 23.41 _cell_measurement_theta_min 20.79 _cell_volume 676.59(8) _computing_cell_refinement 'Local diffractometer control software' _computing_data_collection 'Local diffractometer control software' _computing_data_reduction 'PROFIT (Streltsov & Zavodnik, 1989)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1983)' _computing_publication_material 'SHELXTL (Sheldrick, 1983)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 9.5(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Huber 512' _diffrn_measurement_method \w/2\q _diffrn_radiation_monochromator none _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .0127 _diffrn_reflns_av_sigmaI/netI .0114 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_number 4102 _diffrn_reflns_theta_full 30.07 _diffrn_reflns_theta_max 30.07 _diffrn_reflns_theta_min 2.87 _diffrn_standards_decay_% .5 _diffrn_standards_interval_count 100 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.995 _exptl_absorpt_correction_T_max .5170 _exptl_absorpt_correction_T_min .4047 _exptl_absorpt_correction_type gaussian _exptl_crystal_colour LightBlue _exptl_crystal_density_diffrn 2.022 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 414 _exptl_crystal_size_max .70 _exptl_crystal_size_mid .53 _exptl_crystal_size_min .40 _refine_diff_density_max .490 _refine_diff_density_min -.460 _refine_ls_extinction_coef .050(2) _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.184 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 129 _refine_ls_number_reflns 1986 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.184 _refine_ls_R_factor_all .0208 _refine_ls_R_factor_gt .0199 _refine_ls_shift/su_max .000 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0285P)^2^+0.3880P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .0540 _reflns_number_gt 1949 _reflns_number_total 1986 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file ta0006.cif _[local]_cod_data_source_block so _[local]_cod_cif_authors_sg_H-M 'P 21/a' _[local]_cod_cif_authors_sg_Hall '-P 2ac' _[local]_cod_chemical_formula_sum_orig 'H20 Cu N2 O14 S2' _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. '_exptl_absorpt_correction_type' value 'Gaussian' changed to 'gaussian' 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 2102085 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' '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_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol Cu .0000 .0000 .0000 .00300(8) Uani d S 1 Cu S1 .41999(3) .13461(2) .74317(4) .00333(8) Uani d . 1 S O3 .43010(9) .22763(7) .59597(13) .00560(15) Uani d . 1 O O4 .55825(9) .06705(7) .78309(14) .00667(16) Uani d . 1 O O5 .28403(9) .06783(6) .63190(13) .00544(16) Uani d . 1 O O6 .40192(9) .17916(7) .95197(13) .00589(15) Uani d . 1 O O7 .18678(10) .11864(7) .17781(15) .00661(16) Uani d . 1 O O8 -.15725(10) .10919(7) .02927(14) .00568(16) Uani d . 1 O O9 -.00620(10) -.06428(7) .28256(14) .00572(15) Uani d . 1 O N1 .14189(12) .34172(8) .35758(17) .00676(18) Uani d . 1 N H11 .088(2) .3284(17) .221(3) .014(4) Uiso d . 1 H H12 .215(3) .2988(19) .385(3) .021(5) Uiso d . 1 H H13 .081(2) .3250(18) .443(3) .018(5) Uiso d . 1 H H14 .162(3) .414(2) .367(4) .026(5) Uiso d . 1 H H15 .219(2) .0963(18) .299(4) .019(5) Uiso d . 1 H H16 .248(2) .1212(17) .124(4) .016(5) Uiso d . 1 H H17 -.238(3) .0957(19) -.047(4) .020(5) Uiso d . 1 H H18 -.139(2) .1732(19) .005(3) .017(5) Uiso d . 1 H H19 -.087(3) -.057(2) .313(4) .029(6) Uiso d . 1 H H20 .012(3) -.1308(19) .301(4) .023(5) 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 Cu .00314(11) .00297(11) .00320(11) .00050(5) .00140(7) .00052(5) S1 .00326(12) .00311(12) .00373(13) -.00005(8) .00116(9) -.00011(8) O3 .0073(3) .0042(3) .0056(3) -.0006(3) .0024(3) .0015(3) O4 .0044(3) .0064(4) .0089(4) .0017(3) .0014(3) .0000(3) O5 .0043(3) .0054(4) .0063(4) -.0017(3) .0009(3) -.0009(3) O6 .0080(4) .0061(3) .0041(3) -.0001(3) .0026(3) -.0011(3) O7 .0061(4) .0082(4) .0057(4) -.0006(3) .0020(3) .0005(3) O8 .0043(3) .0046(4) .0081(4) .0004(3) .0017(3) .0001(3) O9 .0064(4) .0055(4) .0063(3) .0014(3) .0035(3) .0015(3) N1 .0069(4) .0060(4) .0078(4) -.0001(3) .0026(3) -.0001(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source N N .0061 .0033 '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' Cu Cu .3201 1.2651 '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 O9 Cu O9 . 3 180.00(7) yes O9 Cu O8 . . 88.74(3) yes O9 Cu O8 3 . 91.26(3) yes O9 Cu O8 . 3 91.26(3) yes O9 Cu O8 3 3 88.74(3) yes O8 Cu O8 . 3 180.00(5) yes O9 Cu O7 . 3 89.39(3) yes O9 Cu O7 3 3 90.61(3) yes O8 Cu O7 . 3 91.00(3) yes O8 Cu O7 3 3 89.00(3) yes O9 Cu O7 . . 90.61(3) yes O9 Cu O7 3 . 89.39(3) yes O8 Cu O7 . . 89.00(3) yes O8 Cu O7 3 . 91.00(3) yes O7 Cu O7 3 . 180.00(6) yes O4 S1 O6 . . 110.90(5) yes O4 S1 O5 . . 109.40(5) yes O6 S1 O5 . . 109.91(5) yes O4 S1 O3 . . 109.72(5) yes O6 S1 O3 . . 108.75(5) yes O5 S1 O3 . . 108.10(5) yes Cu O7 H15 . . 106.5(16) yes Cu O7 H16 . . 110.8(17) yes H15 O7 H16 . . 110(2) yes Cu O8 H17 . . 112.2(17) yes Cu O8 H18 . . 115.3(15) yes H17 O8 H18 . . 107(2) yes Cu O9 H19 . . 115.4(17) yes Cu O9 H20 . . 117.6(16) yes H19 O9 H20 . . 104(2) yes H11 N1 H12 . . 106.2(19) yes H11 N1 H13 . . 106.6(18) yes H12 N1 H13 . . 109(2) yes H11 N1 H14 . . 107.0(19) yes H12 N1 H14 . . 118(2) yes H13 N1 H14 . . 109(2) yes 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 Cu O9 . 1.9724(8) yes Cu O9 3 1.9724(8) yes Cu O8 . 2.0019(8) yes Cu O8 3 2.0019(8) yes Cu O7 3 2.2769(9) yes Cu O7 . 2.2769(9) yes S1 O4 . 1.4655(8) yes S1 O6 . 1.4832(8) yes S1 O5 . 1.4843(8) yes S1 O3 . 1.4902(8) yes O7 H15 . .79(2) yes O7 H16 . .73(2) yes O8 H17 . .78(2) yes O8 H18 . .82(2) yes O9 H19 . .82(3) yes O9 H20 . .83(2) yes N1 H11 . .89(2) yes N1 H12 . .82(2) yes N1 H13 . .90(2) yes N1 H14 . .90(3) yes 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 H11 O6 4_564 .89(2) 2.04(2) 2.8810(13) 158(2) yes N1 H12 O3 . .82(2) 2.22(2) 2.9792(13) 154(2) yes N1 H13 O3 4_565 .90(2) 2.00(2) 2.8890(13) 171(2) yes N1 H14 O5 2_556 .90(3) 1.94(3) 2.8402(13) 175(2) yes O7 H15 O5 . .79(2) 2.06(2) 2.8353(12) 168(2) yes O7 H16 O6 1_554 .73(2) 2.12(2) 2.8279(12) 162(2) yes O8 H17 O4 1_454 .78(2) 1.90(2) 2.6704(12) 176(2) yes O8 H18 O6 4_564 .82(2) 1.89(2) 2.7141(12) 179(2) yes O9 H19 O5 3_556 .82(3) 1.92(3) 2.7287(12) 169(2) yes O9 H20 O3 2_546 .83(2) 1.87(2) 2.6906(12) 168(2) yes