data_Li4P2S6

_publ_contact_author
;
Schmedt auf der G"unne, J"orn
Inorganic Materials Chemistry
University of Siegen
Adolf-Reichwein-Strasse 2
57068 Siegen
Germany 
;

_publ_contact_author_phone        '+49/271/7404219'
_publ_contact_author_fax          '+49/271/7402555'
_publ_contact_author_email        'gunnej@chemie.uni-siegen.de'
_publ_requested_journal
;
Dalton Transactions
Volume XXX
Year 2018
;
_publ_section_title
;
Refinement of the Crystal Structure of Li4P2S6 using NMR Crystallography
;
_publ_section_abstract
;
The structure of Li4P2S6 was solved, based on a combination of X-ray powder diffraction data, density functional theory calculations and solid state nuclear magnetic resonance (NMR). 
Two-dimensional 31P single quantum/double quantum correlation spectra yielded important constraints regarding the space group symmetry allowing the crystal structure to be solved by the Rietveld method. 
Li4P2S6 crystallizes in a trigonal space group with a = 10.51452(6) Å; c = 6.59149(8) Å. The structure contains two distinct P2S64- ions in a 2:1 ratio: in the first one the two P atoms of the 
hexahypothiophosphate unit are crystallographically distinct, whereas in the second one they are crystallographically identical.
;

loop_
_publ_author_name
_publ_author_address
'Neuberger, Sven'
;Inorganic Materials Chemistry
University of Siegen
Adolf-Reichwein-Strasse 2
57068 Siegen
Germany
;
'Culver, Sean P.'
;Institute of Physical Chemistry
Justus-Liebig-University Giessen
Heinrich-Buff-Ring 17
35392 Giessen
Germany
;
'Eckert, Hellmut'
;Institute of Physics in São Carlos 
University of São Paulo
Av. Trabalhador Sãocarlense 400, 
Sao Carlos, SP 13566-590 
Brazil
Institute of Physical Chemistry
WWU Münster
Corrensstrasse 30
48149 Münster
Germany
;
'Zeier, Wolfgang G.'
;Institute of Physical Chemistry
Justus-Liebig-University Giessen
Heinrich-Buff-Ring 17
35392 Giessen
Germany
;
'Schmedt auf der Günne, Jörn'
;Inorganic Materials Chemistry
University of Siegen
Adolf-Reichwein-Strasse 2
57068 Siegen
Germany
;

_publ_section_exptl_prep
;
A powder diffraction pattern was recorded with a Stoe Stadi P diffractometer in
Debye-Scherrer geometry using Ge(111) monochromated Cu-Kalpha1 radiation of
154.0596 pm.
;

_diffrn_measurement_device_type        'STOE STADI P'
_diffrn_source                         'sealed X-ray tube'
_diffrn_radiation_probe                x-ray
_diffrn_radiation_polarisn_ratio       1.0
_diffrn_radiation_wavelength           1.54056
_diffrn_radiation_type                 'Cu K\a~1~'
_diffrn_radiation_monochromator        'Ge-111'
_diffrn_ambient_temperature				298
_geom_special_details                  Debye-Scherrer
_diffrn_ambient_pressure	       	   1
_cell_measurement_temperature          298

_solution_special_details
; 
?
;
                                  	
_computing_molecular_graphics     	  'Diamond 4'
_computing_publication_material   	  'TOPAS ACADEMIC 4.1 + TOPAS ACADEMIC 6.1'
_audit_creation_method		      	  'TOPAS ACADEMIC 4.1 + PLATON'
_pd_calc_method                   	  'Rietveld Refinement'
_computing_structure_solution     	  'Powdercell'
_computing_structure_refinement   	  'TOPAS ACADEMIC 4.1 + TOPAS ACADEMIC 6.1'
                                  	
_refine_ls_shift/su_mean          	   1.92
_refine_ls_shift/su_max           	   ?
_refine_ls_matrix_type            	   full
_refine_ls_number_parameters      	   39
_refine_ls_number_constraints     	   2
_refine_ls_number_restraints      	   0
_refine_ls_goodness_of_fit_all    	   1.92
_refine_ls_R_factor_all				   3.22
_pd_proc_ls_prof_wR_factor        	   3.22
_pd_proc_ls_prof_R_expected       	   1.68
                                  	                         	                                 	                                	
_pd_char_colour                   	white-yellow
_pd_char_particle_morphology      	powder
_chemical_name_systematic 		  	'Tetralithium thiodiphosphate'
_chemical_name_common 			  	'Tetralithium thiodiphosphate'
_chemical_formula_structural 	  	'Li4 P2 S6'
_chemical_formula_sum 			  	'Li4 P2 S6'
_chemical_formula_weight 				282.072
_chemical_formula_moiety 				'P2 S6, 4(Li)'
_chemical_properties_physical  			'air-sensitive, moisture-sensitive, hygroscopic'
                                  	
_exptl_crystal_density_diffrn    		 2.23
_exptl_crystal_description        	 'microcrystalline'
##_exptl_crystal_density_meas     	 none
##_exptl_crystal_density_method   	 none
##_cell_special_details           	 none
_exptl_absorpt_coefficient_mu     	 17.929208(586)
_exptl_absorpt_correction_type   		 cylinder 
_exptl_absorpt_process_details    	 '(A. Cohelo, TOPAS_Academic, Version 4.1)'

_cell_measurement_theta_min	     	   10.000
_cell_measurement_theta_max	     	   90.000
_diffrn_reflns_theta_max         	   89.2
_pd_meas_number_of_points              5345
_pd_proc_number_of_points              5345
_diffrn_reflns_number				   220
_reflns_number_total                   220
_reflns_limit_h_min                    0
_reflns_limit_h_max                    8
_reflns_limit_k_min                    0
_reflns_limit_k_max                    8
_reflns_limit_l_min                    0
_reflns_limit_l_max                    6


loop_
_symmetry_equiv_pos_as_xyz
	'-x, -x+y, -z'
	'-x+y, -x, z'
	'-y, x-y, z'
	'y, x, -z'
	'x-y, -y, -z'
	'x, y, z'

_cell_length_a 10.51452(6)
_cell_length_b 10.51452(6)
_cell_length_c 6.59148(8)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_volume 631.092(10)
_cell_formula_units_Z 3
_symmetry_cell_setting 'trigonal'
_symmetry_space_group_name_H-M 'P 3 2 1'
_symmetry_space_group_name_Hall  'P 3 2"'
_symmetry_Int_Tables_number 150
_shelx_F_squared_multiplier 1

loop_
_atom_type_symbol
_atom_type_oxidation_number
Li 1
P 4
S -2

_atom_type_scat_source
;
Default data set used by TOPAS Academic 4.1 & TOPAS Academic 6
(A. Cohelo, TOPAS_Academic, Version 4.1)
(A. Cohelo, TOPAS_Academic, Version 6)
;

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_B_iso_or_equiv
_atom_site_U_iso_or_equiv
Li1 Li   3 3e 0.625 0 0 1 5 0.0633
Li2 Li   3 3f 0.631 0 0.5 1 5 0.0633
Li3 Li   3 3e 0.317 0 0 1 5 0.0633
Li4 Li   3 3f 0.329 0 0.5 1 5 0.0633
P1 P   2 2c 0 0 0.17 1 2.73(14) 0.0346
P2 P   2 2d 0.3333333 0.6666667 0.66288 1 2.73(14) 0.0346
P3 P   2 2d 0.3333333 0.6666667 0.33517 1 2.73(14) 0.0346
S1 S   6 6g 0.108(6) 0.2165(7) 0.2410(8) 1 0.73934 0.0094
S2 S   6 6g 0.1220(9) 0.561(6) 0.2500(9) 1 0.73934 0.0094
S3 S   6 6g 0.4515(7) 0.226(6) 0.2546(10) 1 0.73934 0.0094

loop_
_geom_bond_atom_site_label_1                 
_geom_bond_atom_site_label_2                 
_geom_bond_distance   
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
S1	P1	2.026(6)	.	.
S2	P3	2.01(4)		.	.	
S3	P2	2.03(4) 	.	4_556
P1	P1	2.2411(1)	.	4_555
P2	P3	2.1601(1)	.	.             

                                  
loop_
_geom_angle_atom_site_label_1                
_geom_angle_atom_site_label_2                
_geom_angle_atom_site_label_3                
_geom_angle 
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
S1	P1	P1	103.35(15)	.		.	4_555
S1	P1	S1	115(2)		.		.	2_555					
S2	P3	P2	106.3(4)	.		.	.       
S2	P3	S2	113(2)		.		.	2_565		
S3	P2	S3	113(2)		5_566	.	1_666		
S3	P2	P3	105.52(19)	4_556	.	.
