Ln~3~<i>M</i>~1{-~δ}<i>TX</i>~7~ ‒ quasi-isostructural compounds: stereochemistry and silver-ion motion in the Ln~3~Ag~1{-~δ}GeS~7~ (Ln = La‒Nd, Sm, Gd‒Er and Y; δ = 0.11‒0.50) compounds
Daszkiewicz, Marek; Gulay, Lubomir D.; Lychmanyuk, Olga S.; Acta Crystallographica Section B 65 (2009) 126–133; doi:10.1107/S010876810900144X

data_2104305
_publ_section_title
;
 Ln~3~<i>M</i>~1{-~\d}<i>TX</i>~7~ -- quasi-isostructural compounds:
 stereochemistry and silver-ion motion in the Ln~3~Ag~1{-~\d}GeS~7~ (Ln
 = La--Nd, Sm, Gd--Er and Y; \d = 0.11--0.50) compounds
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              126
_journal_page_last               133
_journal_paper_doi               10.1107/S010876810900144X
_journal_volume                  65
_journal_year                    2009
_chemical_formula_moiety         'Ag0.89 Ge Pr3 S7'
_chemical_formula_sum            'Ag0.89 Ge Pr3 S7'
_chemical_formula_weight         815.74
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           173
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 6c'
_symmetry_space_group_name_H-M   'P 63'
_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                120.00
_cell_formula_units_Z            2
_cell_length_a                   10.2290(14)
_cell_length_b                   10.2290(14)
_cell_length_c                   5.7760(11)
_cell_measurement_reflns_used    585
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      3.98
_cell_volume                     523.39(14)
_computing_cell_refinement       'CrysAlis RED'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2007)'
_computing_data_reduction        'CrysAlis RED'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean '1024x1024 with blocks 2x2, 33.133pixel/mm'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'KUMA KM-4 with area CCD detector'
_diffrn_measurement_method       \w-scan
_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  0.0590
_diffrn_reflns_av_sigmaI/netI    0.0280
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            5174
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.98
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    19.504
_exptl_absorpt_correction_T_max  0.272
_exptl_absorpt_correction_T_min  0.163
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'CrysAlis (Oxford Diffraction, 2007)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    5.176
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             726
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.222
_refine_diff_density_min         -0.727
_refine_ls_abs_structure_details
'Flack H D (1983), Acta Cryst. A39, 876-881, 265 Friedel pairs'
_refine_ls_abs_structure_Flack   0.05(3)
_refine_ls_extinction_coef       0.0145(7)
_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   1.092
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     43
_refine_ls_number_reflns         602
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0246
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0287P)^2^+1.0320P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0509
_refine_ls_wR_factor_ref         0.0514
_reflns_number_gt                585
_reflns_number_total             602
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            bp5017.cif
_cod_data_source_block           pr
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Hexagonal' changed to 'hexagonal'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Hexagonal' changed to 'hexagonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2104305