data_global _audit_creation_date 12-05-02 _audit_creation_method CRYSTALS_ver_12.87 _oxford_structure_analysis_title 'K3D(SO4)2 14K' _chemical_name_systematic ? _chemical_melting_point ? #looking for refcif # Check this file using the IUCr facility at: # http://checkcif.iucr.org/ # The content below is held in the file 'script/refcif.dat'. This is a text # file which you may edit to reflect local conditions. # Items which need looking at are represented by a '?'. # Items for which there are choices are prefixed with 'choose from'. _publ_contact_letter ; Please consider this CIF submission for publication in JCP ; _publ_contact_author_name 'François Fillaux' _publ_contact_author_address ; UMR 7075, CNRS, Université Pierre et Marie Curie, Box 49, 4 place Jussieu, 75252 PARIS Cedex05, France ; _publ_contact_author_phone '+33 144273339' _publ_contact_author_email 'francois.fillaux@upmc.fr' _publ_requested_journal 'JCP' _publ_requested_coeditor_name ' ' _publ_section_title # Title of paper ; Neutron scattering studies of K3H(SO4)2 and K3D(SO4)2 : Infinite square-wells and quantum phase transition ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_contact_author_name 'François Fillaux' _publ_contact_author_address ; UMR 7075, CNRS, Université Pierre et Marie Curie, Box 49, 4 place Jussieu, 75252 PARIS Cedex05, France ; _publ_author_name 'Alain Cousson' _publ_author_address ; Laboratoire Léon Brillouin (CEA-CNRS), C.E. Saclay, 91191 Gif-sur-Yvette cedex, France ; _publ_section_abstract # Text of the abstract # (a) The Abstract must be self-contained and comprehensible # without the rest of the paper. This means no references # to atom names or to compound numbers; compounds must be # identified as the title compound, or by name or by some other # means such as derivatives of each other (e.g. "the # corresponding ketone"). # (b) The chemical formula of "the title compound" must be given. # (c) Any crystallographic molecular symmetry should be # mentioned, and also the presence of more than one molecule # in the asymmetric unit (i.e. anything other than Z'=1). ; ? ; _publ_section_related_literature # Not in version 2.3.1 ############################################################### # Essential references (e.g. to the origin of the material studied, related # structural studies, and to information supporting the reported structure) # should be cited in this section, with appropriate very brief explanatory # text, for example `The synthesis of the complex is described by Jones # (2001). The anhydrous complex has essentially the same coordination # geometry (Smith, 2003).' In addition, all references included in the # supplementary materials, but not elsewhere in the published article, # should be given here. The simple text `For related literature, see:...' # may be used, but further details should be provided in the Comment # section, which forms part of the supplementary material. ############################################################### ; ? ; _publ_section_comment # Text of the paper # Note that atoms are referenced as N2, not N(2) or N~2~ # If text containing () occur within (), the outer ones should be [] # Figures should be referenced as Fig. ; ; _publ_section_acknowledgements # Acknowledgments ; ; _publ_section_figure_captions # Captions to figures - Start each caption on a new line after a blank line _publ_section_exptl_refinement _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ; # Hand-made tables can be put in the cif. The number of columns # is set in the loop header. # The contants of each column can either be a piece of text # without any spaces (eg a number) or other text enclosed in " " # Remove the leading # in the following example #geom_extra_table_head_A #; #Table 2. #; # #loop_ #_geom_extra_tableA_col_1 #_geom_extra_tableA_col_2 #_geom_extra_tableA_col_3 #_geom_extra_tableA_col_4 # #Parameter "Observed Value" "MOGUL Value" "MOGUL e.s.d" #N5-C6-C4 129 124 "7 (\%)" #C3-O10-C2 105 109 "2 (\%)" #C6-O7 1.25 1.22 ".02 (\%A)" # data_1 _exptl_special_details ; ; _refine_special_details ; ; # End of 'script/refcif.dat' #end of refcif _cell_length_a 9.7770(10) _cell_length_b 5.6740(10) _cell_length_c 14.6670(10) _cell_angle_alpha 90 _cell_angle_beta 102.970(10) _cell_angle_gamma 90 _cell_volume 792.89(17) _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'A 1 2/a 1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' 'x,y+1/2,z+1/2' '-x,-y+1/2,-z+1/2' '-x+1/2,y,-z' 'x+1/2,-y,z' '-x+1/2,y+1/2,-z+1/2' 'x+1/2,-y+1/2,z+1/2' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source K 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 3.6700 'International Tables Vol C 4.2.6.8 and 6.1.1.4' S 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 2.8470 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 5.8030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 -3.7390 'International Tables Vol C 4.2.6.8 and 6.1.1.4' D 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 6.6710 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 8 # Given Formula = H0.12 D0.12 K0.12 O0.12 S0.12 # Dc = 0.19 Fooo = 270.00 Mu = 2.04 M = 11.27 # Found Formula = D0.25 K1.25 O4 S1 # Dc = 2.61 FOOO = 270.00 Mu = 22.57 M = 155.72 _chemical_formula_sum 'D0.25 K1.25 O4 S1' _chemical_formula_moiety 'D0.25 K1.25 O4 S1' _chemical_compound_source ? _chemical_formula_weight 155.72 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 15 _cell_measurement_theta_max 25 _cell_measurement_temperature 14 _exptl_crystal_description 'prism' _exptl_crystal_colour 'white' _exptl_crystal_size_min ? _exptl_crystal_size_mid ? _exptl_crystal_size_max ? _exptl_crystal_density_diffrn 2.609 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 270 _exptl_absorpt_coefficient_mu 2.257 # Sheldrick geometric approximatio 1.00 1.00 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 1.0000 _exptl_absorpt_correction_T_max 1.0000 _diffrn_measurement_device 'Stoe' _diffrn_measurement_device_type 'Serial' _diffrn_radiation_monochromator 'copper' _diffrn_radiation_type ' neutron ' _diffrn_radiation_wavelength 0.83080 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'STOE REVISED PROGRAM' _computing_cell_refinement 'STOE DEFINED CELL REFINEMENT' _computing_data_reduction 'COLL5 DEFINED DATA REDUCTION' _computing_structure_solution 'PREVIOUSLY X-RAY STRUCTURE SOLUTION' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_ambient_temperature 14 _diffrn_reflns_number 1822 _reflns_number_total 1253 _diffrn_reflns_av_R_equivalents 0.042 # Number of reflections without Friedels Law is 1253 # Number of reflections with Friedels Law is 0 # Theoretical number of reflections is about 1276 _diffrn_reflns_theta_min 3.332 _diffrn_reflns_theta_max 37.158 _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 33.814 _diffrn_measured_fraction_theta_full 0.985 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 2 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _reflns_limit_h_min -14 _reflns_limit_h_max 13 _reflns_limit_k_min 0 _reflns_limit_k_max 8 _reflns_limit_l_min 0 _reflns_limit_l_max 21 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.46 _refine_diff_density_max 1.13 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>3.0\s(I) _refine_ls_number_reflns 999 _refine_ls_number_restraints 0 _refine_ls_number_parameters 67 _oxford_refine_ls_R_factor_ref 0.0474 _refine_ls_wR_factor_ref 0.0333 _refine_ls_goodness_of_fit_ref 1.0907 _refine_ls_shift/su_max 0.0010080 _refine_ls_shift/su_mean 9.4039021 # The values computed from all data _oxford_reflns_number_all 1253 _refine_ls_R_factor_all 0.0726 _refine_ls_wR_factor_all 0.0359 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 1053 _refine_ls_R_factor_gt 0.0517 _refine_ls_wR_factor_gt 0.0342 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration '.' _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment none # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.905 -0.693 0.653 -0.972E-01 0.113 ; # Insert your own references if required - in alphabetical order _publ_section_references ; User-defined structure solution reference User-defined data collection reference User defined data reduction User defined cell refinement Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens K1 K 0.2500 0.7515(3) 0.0000 0.0041 1.0000 Uani S T . . . . . K2 K 0.34828(12) 0.7342(2) 0.30568(8) 0.0052 1.0000 Uani . . . . . . . S1 S 0.03850(14) 0.2703(3) -0.11645(10) 0.0026 1.0000 Uani . . . . . . . O1 O 0.09942(8) 0.47697(14) -0.15382(5) 0.0049 1.0000 Uani . . . . . . . O2 O 0.10851(8) 0.05052(14) -0.13140(5) 0.0057 1.0000 Uani . . . . . . . O3 O -0.11494(7) 0.25884(14) -0.15247(5) 0.0051 1.0000 Uani . . . . . . . O4 O 0.06276(8) 0.30903(14) -0.00885(5) 0.0055 1.0000 Uani . . . . . . . D10 D -0.0050 0.5143 0.0002 0.0366 1.0000 Uani S . . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 K1 0.0036(6) 0.0053(6) 0.0032(6) 0.0000 0.0006(4) 0.0000 K2 0.0042(4) 0.0042(5) 0.0071(4) -0.0015(4) 0.0012(3) -0.0004(4) S1 0.0022(5) 0.0028(6) 0.0025(5) 0.0007(5) -0.0003(4) -0.0003(5) O1 0.0058(3) 0.0032(3) 0.0060(3) 0.0006(2) 0.0021(2) -0.0013(2) O2 0.0062(3) 0.0040(3) 0.0070(3) 0.0002(2) 0.0019(2) 0.0016(2) O3 0.0035(3) 0.0057(3) 0.0059(3) -0.0013(2) 0.0009(2) -0.0003(2) O4 0.0075(3) 0.0055(3) 0.0037(3) -0.0013(2) 0.0015(2) 0.0018(3) D10 0.0328(8) 0.0666(14) 0.0112(5) -0.0058(7) 0.0067(5) -0.0310(10) _refine_ls_extinction_coef 5.3(4) _refine_ls_extinction_method 'Larson (1970), Equation 22' _oxford_refine_ls_scale 0.2035(8) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag S1 . O1 . 1.4752(16) yes S1 . O2 . 1.4628(17) yes S1 . O3 . 1.4758(16) yes S1 . O4 . 1.5579(16) yes O4 . D10 2_565 1.171 yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 . S1 . O2 . 112.36(10) yes O1 . S1 . O3 . 111.40(10) yes O2 . S1 . O3 . 112.39(11) yes O1 . S1 . O4 . 106.38(10) yes O2 . S1 . O4 . 107.58(10) yes O3 . S1 . O4 . 106.28(9) yes D10 2_565 O4 . S1 . 105.228 yes