Equilibrium langbeinite-related phosphates Cs~1+<i>x~</i>Ln~<i>x~</i>Zr~2{-~<i>x</i>}(PO~4~)~3~ (Ln = Sm‒Lu) in the melted systems Cs~2~O‒P~2~O~5~‒LnF~3~‒ZrF~4~
Ogorodnyk, Ivan V.; Baumer, Vyacheslav N.; Zatovsky, Igor V.; Slobodyanik, Nikolay S.; Shishkin, Oleg V.; Domasevitch, Konstantin V.; Acta Crystallographica Section B 63 (2007) 819–827; doi:10.1107/S0108768107049385

data_2103042
_publ_section_title
;
 Equilibrium langbeinite-related phosphates
 Cs~1+<i>x~</i>Ln~<i>x~</i>Zr~2{-~<i>x</i>}(PO~4~)~3~ (Ln = Sm--Lu) in
 the melted systems Cs~2~O--P~2~O~5~--LnF~3~--ZrF~4~
;
_journal_coeditor_code           SX5073
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              819
_journal_page_last               827
_journal_paper_doi               10.1107/S0108768107049385
_journal_volume                  63
_journal_year                    2007
_chemical_formula_moiety         'O12 P3 Tm0.70 Zr1.3, 1(Cs), 0.70(Cs)'
_chemical_formula_sum            'Cs1.7 O12 P3 Tm0.7 Zr1.3'
_chemical_formula_weight         748.46
_space_group_IT_number           198
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P 21 3'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.39820(10)
_cell_length_b                   10.39820(10)
_cell_length_c                   10.39820(10)
_cell_measurement_reflns_used    4789
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3.39
_cell_volume                     1124.280(19)
_computing_cell_refinement
'CrysAlis CCD (Oxford Diffraction Ltd., 2005)'
_computing_data_collection
'CrysAlis CCD (Oxford Diffraction Ltd., 2005)'
_computing_data_reduction
'CrysAlis RED (Oxford Diffraction Ltd., 2005)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  XCalibur-3
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4789
_diffrn_reflns_theta_full        30
_diffrn_reflns_theta_max         30
_diffrn_reflns_theta_min         3.39
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.638
_exptl_absorpt_correction_T_max  0.6221
_exptl_absorpt_correction_T_min  0.5602
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            grey
_exptl_crystal_density_diffrn    4.422
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tetrahedron
_exptl_crystal_F_000             1340.4
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.737
_refine_diff_density_min         -0.809
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.197
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     64
_refine_ls_number_reflns         1093
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.196
_refine_ls_R_factor_all          0.0282
_refine_ls_R_factor_gt           0.025
_refine_ls_shift/su_max          0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0060P)^2^+4.3663P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0384
_refine_ls_wR_factor_ref         0.0396
_reflns_number_gt                1048
_reflns_number_total             1093
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            sx5073.cif
_cod_data_source_block           CsTmZrP
_cod_original_formula_sum        'Cs1.70 O12 P3 Tm0.70 Zr1.30'
_cod_database_code               2103042
_cod_database_fobs_code          2103042