# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 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_LI3CO2SBO6_ILS_VAR_8_publ
_database_code_depnum_ccdc_archive 'CCDC 1883837'
loop_
_audit_author_name
_audit_author_address
'Igor Shukaev'
;Southern Federal University, Rostov-on-Don
Russia
;
_audit_update_record             
;
2018-12-07 deposited with the CCDC.	2019-08-02 downloaded from the CCDC.
;
_publcif_datablock.id            {96dad6ff-9cd3-4f91-8717-be00ccc008e2}

# start Validation Reply Form
_vrf_PLAT701_I                   
;
PROBLEM: Bond    Calc   11.565(6), Rep    2.129(6), Dev..    1572.67 Sigma 
RESPONSE: It is an obvious error of PLATON software. All distances and angles
were verified first by the GSAS program, later using Diamond and Vesta programs.
;
_vrf_PLAT702_I                   
;
PROBLEM: Angle   Calc  117.02(10), Rep     94.2(2), Dev..     228.40 Sigma 
RESPONSE: It is an obvious error of PLATON software. All distances and angles
were verified first by the GSAS program, later using Diamond and Vesta programs.
;
_vrf_PLAT021_I                   
;
PROBLEM: Ratio Unique / Expected Reflections too High ...      2.000
RESPONSE: Reported reflections correspond both to alpha1 and alpha2 wavelengths.
;
# end Validation Reply Form

_pd_block_id                     
2016-01-10T22:06|LI3CO2SBO6_ILS_VAR_8|ils|rigaku

_audit_creation_method           'from EXP file using GSAS2CIF'
_audit_creation_date             2016-01-10T22:06

_refine_ls_number_constraints    ?

_pd_char_colour                  reddish-brown
_refine_ls_shift/su_max          0.07
_refine_ls_shift/su_mean         0.01
_computing_structure_refinement  GSAS
_refine_ls_number_parameters     56
_refine_ls_goodness_of_fit_all   2.25
_refine_ls_number_restraints     12
_refine_ls_matrix_type           full
_chemical_name_systematic        'lithium cobalt(+2) antimony oxide'

_chemical_name_common            'lithium cobalt antimonate'
_chemical_formula_moiety         'Co2 Li3 O6 Sb'
_symmetry_space_group_name_Hall  '-c 2y'

_exptl_crystal_density_diffrn    5.133
_cell_measurement_temperature    298

_pd_phase_name                   Li3Co2SbO6
_cell_length_a                   5.24111(16)
_cell_length_b                   9.03910(23)
_cell_length_c                   5.18179(12)
_cell_angle_alpha                90.0
_cell_angle_beta                 110.0493(22)
_cell_angle_gamma                90.0
_cell_volume                     230.610(11)
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/m 1'

loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +x,+y,+z
2 -x,+y,-z
-1 -x,-y,-z
-2 +x,-y,+z
101 +x+1/2,+y+1/2,+z
102 -x+1/2,+y+1/2,-z
-101 -x+1/2,-y+1/2,-z
-102 +x+1/2,-y+1/2,+z

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_thermal_displace_type
_atom_site_U_iso_or_equiv
_atom_site_symmetry_multiplicity
Sb M1_SB 0.0 0.0 0.0 1.0 Uiso 0.02190(22) 2
Co M2_CO 0.0 0.33459(31) 0.0 0.95 Uiso 0.0206(4) 4
Li Li1_Li 0.0 0.1653(20) 0.5 0.9576(19) Uiso 0.02 4
Li Li2_Li 0.0 0.5 0.5 0.985(4) Uiso 0.02 2
O O1 0.7643(15) 0.0 0.2336(12) 1.0 Uiso 0.02 4
O O2 0.2287(11) 0.1596(6) 0.2256(7) 1.0 Uiso 0.02 8
Li M2_Li 0.0 0.33459(31) 0.0 0.05 Uiso 0.0206(4) 4
Co Li1_Co 0.0 0.1653(20) 0.5 0.0424(19) Uiso 0.02 4
Co Li2_Co 0.0 0.5 0.5 0.015(4) Uiso 0.02 2

_chemical_formula_sum            'Co2 Li3 O6 Sb'
_chemical_formula_weight         356.43
_cell_formula_units_Z            2

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
_geom_bond_publ_flag
M1_SB O1 2.004(8) . 1_455 n
M1_SB O1 2.004(8) . 2_655 n
M1_SB O2 1.981(5) . 1_555 n
M1_SB O2 1.981(5) . 2_555 n
M1_SB O2 1.981(5) . -1_555 n
M1_SB O2 1.981(5) . -2_555 n
M2_CO O1 2.114(5) . 101_455 n
M2_CO O1 2.114(5) . 102_555 n
M2_CO O2 2.084(5) . 1_555 n
M2_CO O2 2.084(5) . 2_555 n
M2_CO O2 2.129(6) . -101_445 n
M2_CO O2 2.129(6) . -102_345 n
Li1_Li O1 2.120(14) . 1_455 n
Li1_Li O1 2.120(14) . 2_656 n
Li1_Li O2 2.152(5) . 1_555 n
Li1_Li O2 2.152(5) . 2_556 n
Li1_Li O2 2.272(14) . -101_446 n
Li1_Li O2 2.272(14) . -102_345 n
Li2_Li O1 2.266(8) . 101_455 n
Li2_Li O1 2.266(8) . 102_556 n
Li2_Li O2 2.177(4) . 101_455 n
Li2_Li O2 2.177(4) . 102_556 n
Li2_Li O2 2.177(4) . -101_446 n
Li2_Li O2 2.177(4) . -102_345 n


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
_geom_angle_publ_flag
O1 M1_SB O1 180.0 1_455 . 2_655 n
O1 M1_SB O2 90.98(19) 1_455 . 1_555 n
O1 M1_SB O2 89.02(19) 1_455 . 2_555 n
O1 M1_SB O2 89.02(19) 1_455 . -1_555 n
O1 M1_SB O2 90.98(19) 1_455 . -2_555 n
O1 M1_SB O2 89.02(19) 2_655 . 1_555 n
O1 M1_SB O2 90.98(19) 2_655 . 2_555 n
O1 M1_SB O2 90.98(19) 2_655 . -1_555 n
O1 M1_SB O2 89.02(19) 2_655 . -2_555 n
O2 M1_SB O2 86.51(26) 1_555 . 2_555 n
O2 M1_SB O2 180.0 1_555 . -1_555 n
O2 M1_SB O2 93.49(26) 1_555 . -2_555 n
O2 M1_SB O2 93.49(26) 2_555 . -1_555 n
O2 M1_SB O2 180.0 2_555 . -2_555 n
O1 M2_CO O1 89.98(25) 101_455 . 102_555 n
O1 M2_CO O2 94.46(17) 101_455 . 1_555 n
O1 M2_CO O2 174.68(24) 101_455 . 2_555 n
O1 M2_CO O2 82.35(25) 101_455 . -101_555 n
O1 M2_CO O2 95.63(26) 101_455 . -102_455 n
O1 M2_CO O2 174.68(24) 102_555 . 1_555 n
O1 M2_CO O2 94.46(17) 102_555 . 2_555 n
O1 M2_CO O2 95.63(26) 102_555 . -101_555 n
O1 M2_CO O2 82.35(25) 102_555 . -102_455 n
O2 M2_CO O2 81.26(27) 1_555 . 2_555 n
O2 M2_CO O2 87.87(18) 1_555 . -101_555 n
O2 M2_CO O2 94.28(18) 1_555 . -102_455 n
O2 M2_CO O2 94.28(18) 2_555 . -101_555 n
O2 M2_CO O2 87.87(18) 2_555 . -102_455 n
O2 M2_CO O2 177.17(32) -101_555 . -102_455 n
M1_SB O1 M2_CO 94.18(23) 1_655 . 101_545 n
M1_SB O1 M2_CO 94.18(23) 1_655 . -101_445 n
M2_CO O1 M2_CO 90.02(25) 101_545 . -101_445 n
M1_SB O2 M2_CO 96.11(17) 1_555 . 1_555 n
M1_SB O2 M2_CO 94.41(19) 1_555 . -101_445 n
M2_CO O2 M2_CO 92.13(18) 1_555 . -101_445 n

_diffrn_ambient_temperature      298
_diffrn_measurement_device_type  Rigaku
_pd_meas_scan_method             cont
_pd_spec_mount_mode              reflection
_pd_spec_shape                   flat_sheet

loop_
_atom_type_symbol
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
Sb 2.0 0.000 0.000 19.6418 5.30340 19.0455 0.46070 5.03710 27.9074 2.68270
75.2825 4.59090 International_Tables_Vol_C
Co 4.0 0.000 0.000 12.2841 4.27910 7.34090 0.27840 4.00340 13.5359 2.34880
71.1692 1.01180 International_Tables_Vol_C
Li 6.0 0.000 0.000 1.12820 3.95460 0.75080 1.05240 0.61750 85.3905 0.46530
168.261 0.03770 International_Tables_Vol_C
O 12.0 0.000 0.000 3.04850 13.2771 2.28680 5.70110 1.54630 0.32390 0.86700
32.9089 0.25080 International_Tables_Vol_C
_diffrn_radiation_probe          x-ray
_diffrn_radiation_polarisn_ratio 0.707

loop_
_diffrn_radiation_wavelength
_diffrn_radiation_wavelength_wt
_diffrn_radiation_type
_diffrn_radiation_wavelength_id
1.540600 1.000 'Cu K\a1' 1
1.544400 0.500 'Cu K\a2' 2
_pd_proc_ls_prof_R_factor        0.0558
_pd_proc_ls_prof_wR_factor       0.0753
_pd_proc_ls_prof_wR_expected     0.0337
_refine_ls_R_Fsqd_factor         0.03259

_pd_proc_ls_background_function  
;   GSAS Background function number 1 with 18 terms.
 Shifted Chebyshev function of 1st kind
      1:    512.353     2:   -359.393     3:    148.202     4:   -51.3893    
      5:    44.0575     6:   -60.6529     7:    57.4487     8:   -34.6864    
      9:    11.6516    10:   -3.68274    11:  -0.319548    12:    3.20568    
     13:   -2.47042    14:  -0.793810    15:    10.0951    16:   -10.7257    
     17:   -1.46775    18:    4.70860    
;

_exptl_absorpt_process_details   
;   GSAS Absorption/surface roughness correction: function number 2
 Surface roughness abs. correction (Pitschke, et al.)
Terms =     0.89940E-01    0.70358E-01
Correction is refined.
;
_exptl_absorpt_correction_T_min  0.75730
_exptl_absorpt_correction_T_max  1.00126

_gsas_exptl_extinct_corr_T_min   1.00000
_gsas_exptl_extinct_corr_T_max   1.00000
_pd_proc_ls_pref_orient_corr     
;   March-Dollase
 AXIS  1 Ratio=     0.993 Frac     1.000  h= 0.000  k= 0.000  l= 1.000
 AXIS  2 Ratio=     1.000 Frac     0.000  h= 0.000  k= 1.000  l= 0.000
 Prefered orientation correction range: Min=   0.99008, Max=   1.02014
;

_pd_proc_ls_profile_function     
;
 CW Profile function number 3 with  19 terms
 Pseudovoigt profile coefficients as parameterized in
 P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83.
 Asymmetry correction of L.W. Finger, D.E. Cox & A. P. Jephcoat (1994).
 J. Appl. Cryst.,27,892-900.
 #1(GU)   =  665.942 #2(GV)   = -185.705 #3(GW)   =   17.836
 #4(GP)   =   21.129 #5(LX)   =    8.300 #6(LY)   =   10.762
 #7(S/L)  =   0.0068 #8(H/L)  =   0.0068
 #9(trns) =    -5.05 #10(shft)=   3.4998
 #11(stec)=    36.97 #12(ptec)=    -1.38 #13(sfec)=    80.17
 #14(L11) =   -0.682 #15(L22) =    0.015 #16(L33) =   -1.801
 #17(L12) =   -0.055 #18(L13) =   -0.895 #19(L23) =    0.299
 Peak tails are ignored  where the intensity is below 0.0004 times the peak
   Stacking fault sublattice vectors:
             0.0   0.0   1.0;   2.0   1.0   0.0;   0.0   3.0   0.0
;
_pd_proc_ls_peak_cutoff          0.00040
_pd_proc_info_datetime           2016-01-10T22:06:21
_pd_calc_method                  'Rietveld Refinement'

_pd_meas_2theta_range_min        6.02
_pd_meas_2theta_range_max        99.98
_pd_meas_2theta_range_inc        0.02
_pd_proc_2theta_range_min        6.02
_pd_proc_2theta_range_max        99.98
_pd_proc_2theta_range_inc        0.02
_pd_meas_number_of_points        4699
_pd_proc_number_of_points        4699

_reflns_number_total             256
_reflns_limit_h_min              0
_reflns_limit_h_max              5
_reflns_limit_k_min              0
_reflns_limit_k_max              10
_reflns_limit_l_min              -5
_reflns_limit_l_max              5
_reflns_d_resolution_high        1.009
_reflns_d_resolution_low         4.868

loop_
_publcif_info_exptl_table_extra_item
?

loop_
_publcif_info_exptl_table_header_item
?

_exptl_crystal_preparation       'Magnetic properties'
