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_1561465
_publ_contact_author_address
;University of South Carolina
Department of Chemistry and Biochemistry
631 Sumter St.
Columbia, SC 29208
;
_publ_contact_author_email       zurloye@mailbox.sc.edu
_publ_contact_author_fax         +1-803-777-8508
_publ_contact_author_name        'Hans-Conrad zur Loye'
_publ_contact_author_phone       +1-803-777-6916
_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 Nd8 O32)'
_chemical_formula_sum            'F Ge4 Na5 Nd4 O16'
_chemical_formula_weight         1257.27
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_Hall           'I -4'
_space_group_name_H-M_alt        'I -4'
_audit_creation_date             2015-08-11
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.0642(17)
_cell_length_b                   12.0642(17)
_cell_length_c                   5.6674(11)
_cell_measurement_reflns_used    3488
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.2996
_cell_measurement_theta_min      2.3875
_cell_volume                     824.9(2)
_computing_cell_refinement       'SAINT-Plus Version 6.45 (Bruker, 2001)'
_computing_data_collection       'SMART Version 5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT-Plus Version 6.45 (Bruker, 2001)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            5462
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.255
_diffrn_reflns_theta_min         2.387
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    19.754
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.3749
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS Version 2.05 (Bruker, 2001)'
_exptl_crystal_colour            blue-purple
_exptl_crystal_density_diffrn    5.062
_exptl_crystal_description       plate
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.934
_refine_diff_density_min         -1.203
_refine_diff_density_rms         0.299
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.07(6)
_refine_ls_extinction_coef       0.0044(3)
_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   1.105
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     70
_refine_ls_number_reflns         1005
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0212
_refine_ls_R_factor_gt           0.0209
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0110P)^2^+20.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0559
_refine_ls_wR_factor_ref         0.0561
_reflns_Friedel_coverage         0.815
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                997
_reflns_number_total             1005
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            JSSC-2016-239-200.cif
_cod_data_source_block           Na5Nd4F[GeO4]4
_cod_original_cell_volume        824.9(3)
_cod_database_code               1561465
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.93(6) 0.07(6)
;
_shelx_res_checksum              6812
_shelx_hkl_checksum              41513
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'