Preparation and Characterization of a New 3-Dimensional Zirconium Hydrogen Phosphate, τ-Zr(HPO~4~)~2~. Determination of the Complete Crystal Structure Combining Synchrotron X-ray Single-Crystal Diffraction and Neutron Powder Diffraction
Anne Marie Krogh Andersen; Poul Norby; Jonathan C. Hanson; Tom Vogt; Inorganic Chemistry 37 (1998) 876–881; doi:10.1021/ic971060h

data_4322672
_publ_contact_author
;Anne Marie Krogh Andersen
Department of Chemistry
University of Odense
Campusvej 55
DK-5230 Odense M
Denmark
;
_publ_contact_author_email       amka@dou.dk
_publ_contact_author_fax         '+45 66158780'
_publ_contact_author_phone       '+45 65573532'
_publ_section_title
;
 Preparation and Characterization of a New 3-Dimensional Zirconium
 Hydrogen Phosphate, \t-Zr(HPO~4~)~2~. Determination of the Complete
 Crystal Structure Combining Synchrotron X-ray Single-Crystal Diffraction
 and Neutron Powder Diffraction
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              876
_journal_page_last               881
_journal_paper_doi               10.1021/ic971060h
_journal_volume                  37
_journal_year                    1998
_chemical_formula_structural     Zr(HPO~4~)~2~
_chemical_formula_sum            'H2 O8 P2 Zr'
_chemical_formula_weight         283.18
_chemical_name_common            'Zirconium Hydrogen Phosphate'
_chemical_name_systematic        'Zirconium Bis(hydrogenorthophosphate)'
_space_group_IT_number           110
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I 4bw -2c'
_symmetry_space_group_name_H-M   'I 41 c d'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.255(2)
_cell_length_b                   11.255(2)
_cell_length_c                   10.750(2)
_cell_measurement_reflns_used    513
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      80
_cell_measurement_theta_min      9
_cell_volume                     1361.8(4)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'imaging plate'
_diffrn_measurement_method       'imaging plate'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'synchrotron X-ray'
_diffrn_radiation_wavelength     0.95400
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0363
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       1
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            379
_diffrn_reflns_theta_max         39.95
_diffrn_reflns_theta_min         4.86
_exptl_absorpt_coefficient_mu    2.086
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            transparent
_exptl_crystal_density_diffrn    2.762
_exptl_crystal_density_meas      2.78
_exptl_crystal_density_method    pycnometrically
_exptl_crystal_description       prism
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          50
_exptl_crystal_size_mid          25
_exptl_crystal_size_min          25
_refine_diff_density_max         2.260
_refine_diff_density_min         -0.971
_refine_diff_density_rms         0.191
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(29)
_refine_ls_extinction_coef       0.0003(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.796
_refine_ls_goodness_of_fit_obs   0.818
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     52
_refine_ls_number_reflns         379
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.796
_refine_ls_restrained_S_obs      0.818
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_obs          0.0354
_refine_ls_shift/esd_max         -2.185
_refine_ls_shift/esd_mean        0.042
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0925
_refine_ls_wR_factor_obs         0.0907
_reflns_number_observed          349
_reflns_number_total             379
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic971060h.cif
_cod_data_source_block           z4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] 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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4322672