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_4319721
_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            'K La P2 S6'
_chemical_formula_weight         432.31
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 109.88(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.963(12)
_cell_length_b                   7.525(10)
_cell_length_c                   11.389(14)
_cell_measurement_temperature    169(2)
_cell_volume                     964(2)
_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      169(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  0.0929
_diffrn_reflns_av_sigmaI/netI    0.1257
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6077
_diffrn_reflns_theta_max         28.44
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    6.415
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            'clear, color'
_exptl_crystal_density_diffrn    2.978
_exptl_crystal_description       plate
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.563
_refine_diff_density_min         -1.677
_refine_diff_density_rms         0.430
_refine_ls_extinction_coef       0.0100(9)
_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   1.071
_refine_ls_goodness_of_fit_obs   0.957
_refine_ls_matrix_type           full
_refine_ls_number_parameters     92
_refine_ls_number_reflns         2307
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_restrained_S_obs      0.957
_refine_ls_R_factor_all          0.1140
_refine_ls_R_factor_obs          0.0583
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0652P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1564
_refine_ls_wR_factor_obs         0.1120
_reflns_number_observed          1503
_reflns_number_total             2307
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000596r_1.cif
_cod_data_source_block           KLaP2S6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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^)+(0.0652P)^2^+0.0000P] 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^)+(0.0652P)^2^+0.0000P] 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        964.1(20)
_cod_database_code               4319721