Synthesis, Crystal Structure, and Vibrational and Optical Spectroscopy of the First Quaternary Alkaline-Earth Rare Earth Thiophosphates Ba3Ln2[P4S16] (Ln = Gd-Er)
Yvonne Klawitter; Wolfgang Bensch; Claudia Wickleder; Chem. Mater. 18 (2006) 187–197; doi:10.1021/cm051860n

data_4000673
_publ_section_title
;
 Synthesis, Crystal Structure, and Vibrational and Optical Spectroscopy
 of the First Quaternary Alkaline-Earth Rare Earth Thiophosphates
 Ba3Ln2[P4S16] (Ln = Gd-Er)
;
_journal_name_full               'Chem. Mater.'
_journal_page_first              187
_journal_page_last               197
_journal_paper_doi               10.1021/cm051860n
_journal_volume                  18
_journal_year                    2006
_chemical_formula_sum            'Ba3 Ho2 P4 S16'
_chemical_formula_weight         1378.72
_chemical_name_systematic        '  ?'
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.088(3)
_cell_length_b                   10.2481(13)
_cell_length_c                   12.565(2)
_cell_measurement_reflns_used    122
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      37
_cell_measurement_theta_min      22
_cell_volume                     2457.9(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Philips PW 1100'
_diffrn_measurement_method       'omega theta scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_av_sigmaI/netI    0.0516
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       1
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7992
_diffrn_reflns_theta_full        30.07
_diffrn_reflns_theta_max         30.07
_diffrn_reflns_theta_min         2.13
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  'every 120 minutes'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    12.710
_exptl_absorpt_correction_T_max  0.3695
_exptl_absorpt_correction_T_min  0.2631
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.726
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cuboid
_exptl_crystal_F_000             2472
_exptl_crystal_size_max          0.133
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.673
_refine_diff_density_min         -1.753
_refine_diff_density_rms         0.278
_refine_ls_extinction_coef       0.00061(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         3591
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0294
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0333P)^2^+5.5169P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0684
_refine_ls_wR_factor_ref         0.0729
_reflns_number_gt                2815
_reflns_number_total             3591
_reflns_threshold_expression     >2sigma(I)
_cod_database_code               4000673