Trends in rare earth thiophosphate syntheses: Rb3Ln(PS4)2 (Ln = La, Ce, Pr), Rb3−xNaxLn(PS4)2 (Ln = Ce, Pr; x = 0.50, 0.55), and RbEuPS4 obtained by molten flux crystal growth
Breton, Logan S.; Smith, Mark D.; zur Loye, Hans-Conrad; CrystEngComm 23 (2021) 5241–5248; doi:10.1039/D1CE00703C

data_7243186
_publ_section_title
;
 Trends in rare earth thiophosphate syntheses: Rb3Ln(PS4)2 (Ln = La, Ce,
 Pr), Rb3&#x2212;xNaxLn(PS4)2 (Ln = Ce, Pr; x = 0.50, 0.55), and RbEuPS4
 obtained by molten flux crystal growth
;
_journal_issue                   30
_journal_name_full               CrystEngComm
_journal_page_first              5241
_journal_page_last               5248
_journal_paper_doi               10.1039/D1CE00703C
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'La P2 Rb3 S8'
_chemical_formula_sum            'La P2 Rb3 S8'
_chemical_formula_weight         713.74
_chemical_name_systematic        'Rubidium Lanthanum Thiophosphate'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_primary     dual-space
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-05-19 deposited with the CCDC.	2021-07-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.005(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.9053(9)
_cell_length_b                   6.7376(6)
_cell_length_c                   11.4553(10)
_cell_measurement_reflns_used    9846
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      29.985
_cell_measurement_theta_min      2.718
_cell_volume                     764.50(12)
_computing_cell_refinement       'SAINT+ Ver. 8.40A (Bruker, 2019)'
_computing_data_collection       'Bruker APEX3 v2019.1-0 (Bruker, 2019)'
_computing_data_reduction        'SAINT+ Ver. 8.40A (Bruker, 2019)'
_computing_molecular_graphics    'OLEX2 (Dolomanov et al., 2009)'
_computing_publication_material  'OLEX2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      291(2)
_diffrn_detector_area_resol_mean 7.39
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0387
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            35700
_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         30.028
_diffrn_reflns_theta_min         2.718
_diffrn_source                   'microfocus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    13.545
_exptl_absorpt_correction_T_max  0.2650
_exptl_absorpt_correction_T_min  0.2051
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., 
 J. Appl. Cryst. 48 (2015) 3-10. 
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.101
_exptl_crystal_description       shard
_exptl_crystal_F_000             652
_exptl_crystal_size_max          0.040
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.990
_refine_diff_density_min         -1.683
_refine_diff_density_rms         0.239
_refine_ls_abs_structure_details
; 
 Twinning involves inversion, so Flack parameter cannot be determined 
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     132
_refine_ls_number_reflns         4460
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0493
_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^)+12.0178P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0951
_refine_ls_wR_factor_ref         0.0983
_reflns_Friedel_coverage         0.855
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                4156
_reflns_number_total             4460
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00703c2.cif
_cod_data_source_block           lb118a_la1
_cod_depositor_comments
'Adding full bibliography for 7243182--7243187.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7243186
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.613
_shelx_estimated_absorpt_t_max   0.773
_shelx_res_checksum              96
_shelx_hkl_checksum              14804