Mixed-metal phosphates K~1.64~Na~0.36~TiFe(PO~4~)~3~ and K~0.97~Na~1.03~Ti~1.26~Fe~0.74~(PO~4~)~3~ with a langbeinite framework
Zatovsky, Igor V.; Strutynska, Nataliia Yu.; Ogorodnyk, Ivan V.; Baumer, Vyacheslav N.; Slobodyanik, Nickolai S.; Butenko, Denis S.; Acta Crystallographica Section E 77 (2021) 1299–1302; doi:10.1107/S2056989021011877

data_2243991
_publ_section_title
;
 Mixed-metal phosphates K~1.64~Na~0.36~TiFe(PO~4~)~3~ and
 K~0.97~Na~1.03~Ti~1.26~Fe~0.74~(PO~4~)~3~ with a langbeinite framework
;
_journal_coeditor_code           WM5625
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1299
_journal_page_last               1302
_journal_paper_doi               10.1107/S2056989021011877
_journal_volume                  77
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_iupac          'K0.97 Na1.03 Ti1.26 Fe0.74 (P O4)3'
_chemical_formula_moiety         'Fe0.74 O12 P3 Ti1.26, 0.97(K), 1.03(Na)'
_chemical_formula_sum            'Fe0.74 K0.97 Na1.03 O12 P3 Ti1.26'
_chemical_formula_weight         448.16
_chemical_name_systematic
;
Potassium sodium titanium iron tris(phosphate)
;
_space_group_IT_number           198
_space_group_name_Hall           'P 2ac 2ab 3'
_space_group_name_H-M_alt        'P 21 3'
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P 21 3'
_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                   9.79450(10)
_cell_length_b                   9.79450(10)
_cell_length_c                   9.79450(10)
_cell_measurement_reflns_used    10546
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.951
_cell_measurement_theta_min      2.941
_cell_volume                     939.608(17)
_computing_cell_refinement
;
CrysAlis CCD (Oxford Diffraction, 2006)
;
_computing_data_collection
;
CrysAlis CCD (Oxford Diffraction, 2006)
;
_computing_data_reduction
;
CrysAlis RED (Oxford Diffraction, 2006)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2006)
;
_computing_publication_material
;
WinGX (Farrugia, 2012), enCIFer (Allen <i>et al.</i>,  2004)
and publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device_type  'Oxford Diffraction 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  0.0258
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10546
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.951
_diffrn_reflns_theta_min         2.941
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.271
_exptl_absorpt_correction_T_max  0.8351
_exptl_absorpt_correction_T_min  0.6217
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(Blessing, 1995)
;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    3.168
_exptl_crystal_description       Tetrahedron
_exptl_crystal_F_000             870.9
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.285
_refine_diff_density_min         -0.274
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 349 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.02
_refine_ls_extinction_coef       0.0015(10)
_refine_ls_extinction_method
;
SHELXL-2018/3 (Sheldrick 2015)
;
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     63
_refine_ls_number_reflns         837
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0165
_refine_ls_R_factor_gt           0.0164
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
'w=1/[\s^2^(Fo^2^)+(0.0186P)^2^+1.1348P] where P=(Fo^2^+2Fc^2^)/3'
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0429
_reflns_number_gt                833
_reflns_number_total             837
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5625sup1.cif
_cod_data_source_block           II
_cod_original_cell_volume        939.61(3)
_cod_database_code               2243991
_shelx_hkl_checksum              49453
_shelx_res_checksum              59154
_cod_database_fobs_code 2243991