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_4319724
_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            'K4 La0.67 P2 S8'
_chemical_formula_weight         567.89
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           72
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-I 2 2c'
_symmetry_space_group_name_H-M   'I b a m'
_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            4
_cell_length_a                   18.2020(15)
_cell_length_b                   8.7596(7)
_cell_length_c                   9.7699(8)
_cell_measurement_temperature    170(2)
_cell_volume                     1557.7(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      170(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  0.0737
_diffrn_reflns_av_sigmaI/netI    0.0595
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4880
_diffrn_reflns_theta_max         28.46
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    4.171
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            'clear, colo'
_exptl_crystal_density_diffrn    2.421
_exptl_crystal_description       polyhedral
_exptl_crystal_F_000             1089
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.154
_refine_diff_density_min         -1.064
_refine_diff_density_rms         0.192
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.055
_refine_ls_goodness_of_fit_obs   1.109
_refine_ls_matrix_type           full
_refine_ls_number_parameters     42
_refine_ls_number_reflns         1031
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_restrained_S_obs      1.109
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_obs          0.0469
_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^)+(0.0491P)^2^+9.7500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1115
_refine_ls_wR_factor_obs         0.1043
_reflns_number_observed          823
_reflns_number_total             1031
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000596r_4.cif
_cod_data_source_block           K4La0.67P2S8
_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^)+(0.0491P)^2^+9.7500P] 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^)+(0.0491P)^2^+9.7500P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4319724