data_CRYSTALS_cif _audit_creation_date 09-06-04 _audit_creation_method CRYSTALS_ver_12.84 _oxford_structure_analysis_title 'K3D(SO4)2 RT (deutéré)' _chemical_name_systematic ? _chemical_melting_point ? _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 ; _cell_length_a 9.7776(10) _cell_length_b 5.6810(10) _cell_length_c 14.7008(10) _cell_angle_alpha 90 _cell_angle_beta 103.051(10) _cell_angle_gamma 90 _cell_volume 795.49(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 O1 S0.25 # Dc = 0.49 Fooo = 270.00 Mu = 2.99 M = 29.28 # Found Formula = D0.25 K1.25 O4 S1 # Dc = 2.60 FOOO = 270.00 Mu = 22.50 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 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_temperature 293 _exptl_crystal_description 'prism' _exptl_crystal_colour 'white' _exptl_crystal_size_min ? _exptl_crystal_size_mid ? _exptl_crystal_size_max ? _exptl_crystal_density_diffrn 2.600 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 270 _exptl_absorpt_coefficient_mu 2.250 # 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_type 'STOE' _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_% ? _diffrn_ambient_temperature 293 _diffrn_reflns_number 794 _reflns_number_total 432 _diffrn_reflns_av_R_equivalents 0.057 # Number of reflections with Friedels Law is 432 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 439 _diffrn_reflns_theta_min 3.326 _diffrn_reflns_theta_max 25.010 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.010 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 2 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _reflns_limit_h_min -9 _reflns_limit_h_max 9 _reflns_limit_k_min 0 _reflns_limit_k_max 5 _reflns_limit_l_min 0 _reflns_limit_l_max 14 _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 -0.17 _refine_diff_density_max 0.14 _refine_ls_number_reflns 404 _refine_ls_number_restraints 0 _refine_ls_number_parameters 67 #_refine_ls_R_factor_ref 0.0176 _refine_ls_wR_factor_ref 0.0200 _refine_ls_goodness_of_fit_ref 1.0636 #_reflns_number_all 432 _refine_ls_R_factor_all 0.0192 _refine_ls_wR_factor_all 0.0206 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.0\s(I) _reflns_number_gt 404 _refine_ls_R_factor_gt 0.0176 _refine_ls_wR_factor_gt 0.0200 _refine_ls_shift/su_max 0.000114 # 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: 0.287 0.126 0.173 ; _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_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 Fih. ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures - Start each caption on a new line after a blank line ; Fig. 1. The title compound with displacement ellipsoids drawn at the 50% probability level. H atoms are shown as spheres of arbitary radius. ; _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; In the absence of significant anomalous scattering, Friedel pairs were merged. The absolute configuration was arbitrarily assigned. The relatively large ratio of minimum to maximum corrections applied in the multiscan process (1:nnn) reflect changes in the illuminated volume of the crystal. Changes in illuminated volume were kept to a minimum, and were taken into account (G\"orbitz, 1999) by the multi-scan inter-frame scaling (DENZO/SCALEPACK, Otwinowski & Minor, 1997). G\"orbitz, C. H. (1999). Acta Cryst. B55, 1090-1098. The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # PROCESSING SUMMARY (IUCr Office Use Only): _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ? _journal_techeditor_code ? _journal_techeditor_notes ? _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? # End of 'script/refcif.dat' # 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 _atom_site_attached_hydrogens K1 K 0.2500 0.7559(2) 0.0000 0.0217 1.0000 Uani S T . . . . K2 K 0.34804(11) 0.73270(17) 0.30574(8) 0.0242 1.0000 Uani . . . . . . S1 S 0.03823(13) 0.2727(2) -0.11604(8) 0.0142 1.0000 Uani . . . . . . O1 O 0.09827(6) 0.47659(11) -0.15307(4) 0.0219 1.0000 Uani . . . . . . O2 O 0.10803(6) 0.05459(12) -0.13039(5) 0.0238 1.0000 Uani . . . . . . O3 O -0.11348(7) 0.26004(11) -0.15222(4) 0.0221 1.0000 Uani . . . . . . O4 O 0.06161(7) 0.31036(16) -0.01022(4) 0.0261 1.0000 Uani . . . . . . D1 D 0.0000 0.5000 0.0000 0.0533 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 0.0170(9) 0.0279(10) 0.0196(8) 0.0000 0.0030(7) 0.0000 K2 0.0174(7) 0.0240(7) 0.0301(7) -0.0057(5) 0.0033(5) -0.0006(4) S1 0.0109(7) 0.0155(7) 0.0161(7) 0.0019(5) 0.0026(5) 0.0004(4) O1 0.0227(4) 0.0200(5) 0.0243(5) 0.0010(3) 0.0079(3) -0.0051(3) O2 0.0216(4) 0.0205(5) 0.0293(4) 0.0011(3) 0.0059(3) 0.0072(3) O3 0.0115(4) 0.0298(5) 0.0243(5) -0.0028(3) 0.0029(3) -0.0009(2) O4 0.0280(5) 0.0335(5) 0.0158(5) 0.0003(3) 0.0028(3) 0.0003(4) D1 0.0464(7) 0.0907(11) 0.0222(6) -0.0052(6) 0.0066(5) -0.0370(8) _refine_ls_extinction_coef 39.8(11) _refine_ls_extinction_method 'Larson (1970), Equation 22' _oxford_refine_ls_scale 0.3224(13) 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 . 1.4585(14) yes S1 . O2 . 1.4527(13) yes S1 . O3 . 1.4602(15) yes S1 . O4 . 1.5354(14) yes O4 . D1 . 1.2598(10) 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 . 112.42(9) yes O1 . S1 . O3 . 111.38(8) yes O2 . S1 . O3 . 112.15(9) yes O1 . S1 . O4 . 106.68(8) yes O2 . S1 . O4 . 107.38(8) yes O3 . S1 . O4 . 106.41(8) yes S1 . O4 . D1 . 105.92(6) yes O4 . D1 . O4 2_565 179.991 yes