Thiophosphate Phase Diagrams Developed in Conjunction with the Synthesis of the New Compounds KLaP2S6, K2La(P2S6)1/2(PS4), K3La(PS4)2, K4La0.67(PS4)2, K9-xLa1+x/3(PS4)4 (x = 0.5), K4Eu(PS4)2, and KEuPS4
Evenson; Peter K. Dorhout; Inorganic Chemistry 40 (2001) 2884–2891; doi:10.1021/ic000596r

data_4319725
_publ_section_title
;
 Thiophosphate Phase Diagrams Developed in Conjunction with the Synthesis
 of the New Compounds KLaP2S6, K2La(P2S6)1/2(PS4), K3La(PS4)2,
 K4La0.67(PS4)2, K9-xLa1+x/3(PS4)4 (x = 0.5), K4Eu(PS4)2, and KEuPS4
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2884
_journal_page_last               2891
_journal_paper_doi               10.1021/ic000596r
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'K8.5 La1.17 P4 S16'
_chemical_formula_weight         1131.02
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           68
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2a 2ac'
_symmetry_space_group_name_H-M   'C c c a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.529(9)
_cell_length_b                   36.430(28)
_cell_length_c                   9.782(4)
_cell_measurement_temperature    167(2)
_cell_volume                     6247(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      167(2)
_diffrn_measurement_device       'Bruker CCD'
_diffrn_measurement_method       '\w 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  0.1352
_diffrn_reflns_av_sigmaI/netI    0.1030
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            19212
_diffrn_reflns_theta_max         28.39
_diffrn_reflns_theta_min         1.12
_exptl_absorpt_coefficient_mu    3.995
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            clear
_exptl_crystal_density_diffrn    2.405
_exptl_crystal_description       plate
_exptl_crystal_F_000             4351
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.21
_refine_diff_density_max         2.153
_refine_diff_density_min         -1.917
_refine_diff_density_rms         0.243
_refine_ls_extinction_coef       0.00014(2)
_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_all   1.049
_refine_ls_goodness_of_fit_obs   1.168
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         3879
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_restrained_S_obs      1.168
_refine_ls_R_factor_all          0.1705
_refine_ls_R_factor_obs          0.0676
_refine_ls_shift/esd_max         0.240
_refine_ls_shift/esd_mean        0.041
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0313P)^2^+176.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1550
_refine_ls_wR_factor_obs         0.1160
_reflns_number_observed          1815
_reflns_number_total             3880
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000596r_5.cif
_cod_data_source_block           K9-xLa1+x/3(PS4)4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0313P)^2^+176.0000P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0313P)^2^+176.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        6246.1(63)
_cod_original_sg_symbol_H-M      'C c c a'
_cod_original_formula_sum        'K8.50 La1.17 P4 S16'
_cod_database_code               4319725