# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Ag3LiIr2O6
_database_code_depnum_ccdc_archive 'CCDC 1912803'
loop_
_audit_author_name
_audit_author_address
'Sebastian Bette'
;Max Planck Institute for Solid State Research
Germany
;
_audit_update_record             
;
2019-04-29 deposited with the CCDC.	2019-05-27 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_POWD002_Ag3LiIr2O6          
;
PROBLEM: _refine_ls_goodness_of_fit_all is missing (this is chi, i.e.
RESPONSE: We did not report any GOF, as its definition is not suitable for up-to-date detectors. Modern point sensitive Mythen detectors (the devices we used) provide large global and local count rates, smooth intensity distribution with little statistical fluctuations and a high dynamic range; therefor weak reflections can be accurately measure in proximity of strong peaks. In addition these devices are almost noise free. Accordingly the powder pattern is treated by the software like if the scan time was far too long, although the applied scan time was moderate (see Table S1 in the supporting information). This leads to an artificial high GOF value, even for good fits. Hence we reported Rwp-, are R-F^2^- and R-p-values as well as a figure (Table S1) showing the fit of the whole powder pattern as the quality of the refinement might be better judged be these criteria. This problem is well known to powder diffractionists using a synchrotron beam line source and a 2D image plate detector or an array of Mythen detectors. 
;
# Added during the CSD deposition process: Monday 29 April 2019 10:27 AM
# end Validation Reply Form


_audit_creation_method           TOPAS

_chemical_name_common            Ag3LiIr2O6
_chemical_formula_sum            'Ag3 Ir2 Li O6'
_chemical_formula_weight         810.973

_cell_length_a                   5.2867(8)
_cell_length_b                   9.1501(12)
_cell_length_c                   6.5030(8)
_cell_angle_alpha                90
_cell_angle_beta                 106.065(10)
_cell_angle_gamma                90
_cell_volume                     302.30(7)
_symmetry_space_group_name_H-M   C2/m
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      12

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z '
'-x, y, -z '
'x, -y, z '
'-x, -y, -z '
'x+1/2, y+1/2, z '
'-x+1/2, y+1/2, -z '
'x+1/2, -y+1/2, z '
'-x+1/2, -y+1/2, -z '

_cell_formula_units_Z            2
_cell_measurement_temperature    298

_exptl_crystal_description       'microcrystalline powder'
_exptl_crystal_colour            black

_exptl_crystal_density_diffrn    8.91

loop_
_atom_type_symbol
_atom_type_oxidation_number
Ir 4
Li 1
Ag 1
O -2

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
Ir1 Ir 4 g 0 0.3339(7) 0 1 0.10(6)
Li2 Li 2 a 0 0 0 1 0.10(6)
O1 O 4 i 0.405(16) 0 0.190(8) 1 1.9(3)
O2 O 8 j 0.395(11) 0.3320(10) 0.166(4) 1 1.9(3)
Ag1 Ag 4 h 0.5 0.3320(10) 0.5 1 0.10(6)
Ag2 Ag 2 d 0.5 0 0.5 1 0.10(6)

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_multiplicity

Ir1 Li1 3.049(3) 2

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
Ir1 O1 Li1 91.377(6) 1_555 1_555 1_555

# Powder diffraction data for histogram  1
#==============================================================================
# 4. INSTRUMENT CHARACTERIZATION

_exptl_special_details           
; ?
;

# if regions of the data are excluded, the reason(s) are supplied here:
_pd_proc_info_excluded_regions   
;
 ?
;

# The following item is used to identify the equipment used to record
# the powder pattern when the diffractogram was measured at a laboratory
# other than the authors' home institution, e.g. when neutron or synchrotron
# radiation is used.

_pd_instr_location               
; 
'SLS (Swiss Light Source)'
;
_pd_calibration_special_details  
# description of the method used
# to calibrate the instrument
; 
'Standard Reference Materials NIST SRM640c (Silicon powder)'
;

_diffrn_ambient_temperature      298
_diffrn_source                   ?
_diffrn_source_target            ?
_diffrn_source_type              Ag-tube
_diffrn_measurement_device_type  Stoe-Stadi-P
_diffrn_detector                 
; 
 multi MYTHEN II (Dectris)   
;
_diffrn_detector_type            ? # make or model of detector

_pd_meas_scan_method             step
_pd_meas_special_details         
;  ?
;

# The following two items identify the program(s) used (if appropriate).
_computing_data_collection       ?
_computing_data_reduction        ?

# Describe any processing performed on the data, prior to refinement.
# For example: a manual Lp correction or a precomputed absorption correction
_pd_proc_info_data_reduction     binning

# The following items are used to define the size of the instrument.
# Not all distances are appropriate for all instrument types.

_pd_instr_dist_src/mono          ?
_pd_instr_dist_mono/spec         ?
_pd_instr_dist_src/spec          ?
_pd_instr_dist_spec/anal         ?
_pd_instr_dist_anal/detc         ?
_pd_instr_dist_spec/detc         ?

# 5. Specimen size and mounting information

# The next three fields give the specimen dimensions in mm.  The equatorial
# plane contains the incident and diffracted beam.

_pd_spec_size_axial              ? # perpendicular to
# equatorial plane

_pd_spec_size_equat              ? # parallel to
# scattering vector
# in transmission

_pd_spec_size_thick              ? # parallel to
# scattering vector
# in reflection

_pd_spec_mounting                
# This field should be
# used to give details of the
# container.
; 
'0.5 mm glass capillary'
;

_pd_spec_mount_mode              transmission

_pd_spec_shape                   cylinder

_diffrn_radiation_probe          X-ray
_diffrn_radiation_wavelength     0.5594
_diffrn_radiation_type           'Ag K\a'
_refine_ls_number_parameters     39
_pd_proc_ls_prof_R_factor        0.0383
_pd_proc_ls_prof_wR_factor       0.0684
_pd_proc_ls_prof_wR_expected     0.0020
_refine_ls_R_Fsqd_factor         0.0233
_pd_proc_ls_background_function  
;   
'Chebyshev polynomial'
;

_exptl_absorpt_process_details   
;   
 ?
;
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?

_pd_proc_ls_profile_function     
;
 Fundamental parameters
;
_pd_proc_ls_peak_cutoff          0.00100
_pd_proc_info_datetime           ?
_pd_calc_method                  'Rietveld Refinement'

#---- raw/calc data loop -----
_pd_meas_2theta_range_min        2.0
_pd_meas_2theta_range_max        100.0
_pd_meas_2theta_range_inc        0.001
_pd_proc_2theta_range_min        4.0
_pd_proc_2theta_range_max        60.0
_pd_proc_2theta_range_inc        0.001
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Ag3LiRu2O6
_database_code_depnum_ccdc_archive 'CCDC 1912804'
loop_
_audit_author_name
_audit_author_address
'Sebastian Bette'
;Max Planck Institute for Solid State Research
Germany
;
_audit_update_record             
;
2019-04-29 deposited with the CCDC.	2019-05-27 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_POWD002_Ag3LiRu2O6          
;
PROBLEM: _refine_ls_goodness_of_fit_all is missing (this is chi, i.e.
RESPONSE: We did not report any GOF, as its definition is not suitable for up-to-date detectors. Modern point sensitive Mythen detectors (the devices we used) provide large global and local count rates, smooth intensity distribution with little statistical fluctuations and a high dynamic range; therefor weak reflections can be accurately measure in proximity of strong peaks. In addition these devices are almost noise free. Accordingly the powder pattern is treated by the software like if the scan time was far too long, although the applied scan time was moderate (see Table S1 in the supporting information). This leads to an artificial high GOF value, even for good fits. Hence we reported Rwp-, are R-F^2^- and R-p-values as well as a figure (Table S1) showing the fit of the whole powder pattern as the quality of the refinement might be better judged be these criteria. This problem is well known to powder diffractionists using a synchrotron beam line source and a 2D image plate detector or an array of Mythen detectors. 
;
# Added during the CSD deposition process: Monday 29 April 2019 10:27 AM
# end Validation Reply Form


_audit_creation_method           TOPAS

_chemical_name_common            Ag3LiRu2O6
_chemical_formula_sum            'Ag3 Li O6 Ru2'
_chemical_formula_weight         628.679

_cell_length_a                   5.2259(6)
_cell_length_b                   9.0356(10)
_cell_length_c                   6.5267(6)
_cell_angle_alpha                90
_cell_angle_beta                 105.716(10)
_cell_angle_gamma                90
_cell_volume                     296.66(6)
_symmetry_space_group_name_H-M   C2/m
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      12

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z '
'-x, y, -z '
'x, -y, z '
'-x, -y, -z '
'x+1/2, y+1/2, z '
'-x+1/2, y+1/2, -z '
'x+1/2, -y+1/2, z '
'-x+1/2, -y+1/2, -z '

_cell_formula_units_Z            2
_cell_measurement_temperature    298

_exptl_crystal_description       'microcrystalline powder'
_exptl_crystal_colour            black

_exptl_crystal_density_diffrn    7.04

loop_
_atom_type_symbol
_atom_type_oxidation_number
Ru 4
Li 1
Ag 1
O -2

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
Ru1 Ru 4 g 0 0.3337(11) 0 1 0.10(6)
Li2 Li 2 a 0 0 0 1 0.10(6)
O1 O 4 i 0.390(14) 0 0.152(8) 1 1.9(3)
O2 O 8 j 0.398(9) 0.3234(6) 0.164(4) 1 1.9(3)
Ag1 Ag 4 h 0.5 0.3234(6) 0.5 1 0.10(6)
Ag2 Ag 2 d 0.5 0 0.5 1 0.10(6)

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_multiplicity

Ru1 Li1 3.014(5) 2

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
Ru1 O1 Li1 98.429(4) 1_555 1_555 1_555

# Powder diffraction data for histogram  1
#==============================================================================
# 4. INSTRUMENT CHARACTERIZATION

_exptl_special_details           
; ?
;

# if regions of the data are excluded, the reason(s) are supplied here:
_pd_proc_info_excluded_regions   
;
 ?
;

# The following item is used to identify the equipment used to record
# the powder pattern when the diffractogram was measured at a laboratory
# other than the authors' home institution, e.g. when neutron or synchrotron
# radiation is used.

_pd_instr_location               
; 
'SLS (Swiss Light Source)'
;
_pd_calibration_special_details  
# description of the method used
# to calibrate the instrument
; 
'Standard Reference Materials NIST SRM640c (Silicon powder)'
;

_diffrn_ambient_temperature      298
_diffrn_source                   ?
_diffrn_source_target            ?
_diffrn_source_type              Mo-tube
_diffrn_measurement_device_type  Stoe-Stadi-P
_diffrn_detector                 
; 
 multi MYTHEN II (Dectris)   
;
_diffrn_detector_type            ? # make or model of detector

_pd_meas_scan_method             step
_pd_meas_special_details         
;  ?
;

# The following two items identify the program(s) used (if appropriate).
_computing_data_collection       ?
_computing_data_reduction        ?

# Describe any processing performed on the data, prior to refinement.
# For example: a manual Lp correction or a precomputed absorption correction
_pd_proc_info_data_reduction     binning

# The following items are used to define the size of the instrument.
# Not all distances are appropriate for all instrument types.

_pd_instr_dist_src/mono          ?
_pd_instr_dist_mono/spec         ?
_pd_instr_dist_src/spec          ?
_pd_instr_dist_spec/anal         ?
_pd_instr_dist_anal/detc         ?
_pd_instr_dist_spec/detc         ?

# 5. Specimen size and mounting information

# The next three fields give the specimen dimensions in mm.  The equatorial
# plane contains the incident and diffracted beam.

_pd_spec_size_axial              ? # perpendicular to
# equatorial plane

_pd_spec_size_equat              ? # parallel to
# scattering vector
# in transmission

_pd_spec_size_thick              ? # parallel to
# scattering vector
# in reflection

_pd_spec_mounting                
# This field should be
# used to give details of the
# container.
; 
'0.5 mm glass capillary'
;

_pd_spec_mount_mode              transmission

_pd_spec_shape                   cylinder

_diffrn_radiation_probe          X-ray
_diffrn_radiation_wavelength     0.7093
_diffrn_radiation_type           'Mo K\a'
_refine_ls_number_parameters     39
_pd_proc_ls_prof_R_factor        0.0479
_pd_proc_ls_prof_wR_factor       0.0679
_pd_proc_ls_prof_wR_expected     0.0020
_refine_ls_R_Fsqd_factor         0.0247
_pd_proc_ls_background_function  
;   
'Chebyshev polynomial'
;

_exptl_absorpt_process_details   
;   
 ?
;
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?

_pd_proc_ls_profile_function     
;
 Fundamental parameters
;
_pd_proc_ls_peak_cutoff          0.00100
_pd_proc_info_datetime           ?
_pd_calc_method                  'Rietveld Refinement'

#---- raw/calc data loop -----
_pd_meas_2theta_range_min        2.0
_pd_meas_2theta_range_max        100.0
_pd_meas_2theta_range_inc        0.001
_pd_proc_2theta_range_min        4.0
_pd_proc_2theta_range_max        85.0
_pd_proc_2theta_range_inc        0.001
