A5RE4X[TO4]4 crystal growth: Fluoride flux synthesis of Na5Ln4F[GeO4]4 (Ln=Pr, Nd), the first quaternary germanate oxyfluorides
Latshaw, Allison M.; Wilkins, Branford O.; Morrison, Gregory; Smith, Mark D.; zur Loye, Hans-Conrad; Journal of Solid State Chemistry 239 (2016) 200–203; doi:10.1016/j.jssc.2016.04.038

data_1561464
_publ_section_title
;
 A5RE4X[TO4]4 crystal growth: Fluoride flux synthesis of Na5Ln4F[GeO4]4
 (Ln=Pr, Nd), the first quaternary germanate oxyfluorides
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              200
_journal_page_last               203
_journal_paper_doi               10.1016/j.jssc.2016.04.038
_journal_volume                  239
_journal_year                    2016
_chemical_formula_moiety         '0.5(F2 Ge8 Na10 O32 Pr8)'
_chemical_formula_sum            'F Ge4 Na5 O16 Pr4'
_chemical_formula_weight         1243.95
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_Hall           'I -4'
_space_group_name_H-M_alt        'I -4'
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.1173(4)
_cell_length_b                   12.1173(4)
_cell_length_c                   5.6795(2)
_cell_measurement_reflns_used    9889
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      37.83
_cell_measurement_theta_min      2.375
_cell_volume                     833.92(5)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      300(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_unetI/netI     0.0177
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            24672
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         37.828
_diffrn_reflns_theta_min         2.377
_diffrn_source                   'microfocus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    18.772
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    4.954
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   0.1688
_exptl_transmission_factor_min   0.1061
_refine_diff_density_max         0.476
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.137
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.039(12)
_refine_ls_extinction_coef       0.00202(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     70
_refine_ls_number_reflns         2244
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0128
_refine_ls_R_factor_gt           0.0116
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0072P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0209
_refine_ls_wR_factor_ref         0.0210
_reflns_Friedel_coverage         0.856
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2175
_reflns_number_total             2244
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            JSSC-2016-239-200.cif
_cod_data_source_block           Na5Pr4F[GeO4]4
_cod_original_cell_volume        833.92(6)
_cod_database_code               1561464
_shelx_estimated_absorpt_t_max   0.603
_shelx_estimated_absorpt_t_min   0.255
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.961(12) 0.039(12)
;
_shelx_res_checksum              32056
_shelx_hkl_checksum              53260
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'