# 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_shelx1
_database_code_depnum_ccdc_archive 'CCDC 1944088'
loop_
_audit_author_name
_audit_author_address
'Philip Lightfoot'
;University of St Andrews
United Kingdom
;
_audit_update_record             
;
2019-09-05 deposited with the CCDC.	2019-09-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C6 Co Cs Li3 O12'
_chemical_formula_weight         476.72

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c :H'
_space_group_name_Hall           '-R 3 2"c'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   11.5264(8)
_cell_length_b                   11.5264(8)
_cell_length_c                   15.2164(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1750.8(3)
_cell_formula_units_Z            6
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    907
_cell_measurement_theta_min      2.4
_cell_measurement_theta_max      27.5

_exptl_crystal_description       prism
_exptl_crystal_colour            pink
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.713
_exptl_crystal_F_000             1338
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_exptl_absorpt_coefficient_mu    4.611
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.791
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
'The program SADABS-2008/1 - G.M. Sheldrick was used to apply a multi-scan absorption correction.'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Sealed Tube'
_diffrn_measurement_device_type  'Rigaku Mercury2 (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 13.6612
_diffrn_reflns_number            5481
_diffrn_reflns_av_unetI/netI     0.0182
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.367
_diffrn_reflns_theta_max         27.512
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measured_fraction_theta_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_point_group_measured_fraction_full 0.980
_reflns_number_total             444
_reflns_number_gt                387
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Crystalmaker (Palmer, 2014)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         444
_refine_ls_number_parameters     37
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0228
_refine_ls_R_factor_gt           0.0202
_refine_ls_wR_factor_ref         0.0955
_refine_ls_wR_factor_gt          0.0920
_refine_ls_goodness_of_fit_ref   0.853
_refine_ls_restrained_S_all      0.853
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cs1 Cs 0.6667 0.3333 0.3333 0.0121(3) Uani 1 6 d S T P . .
Co1 Co 0.3333 0.6667 0.4167 0.0093(4) Uani 1 6 d S T P . .
O2 O 0.43451(19) 0.59156(19) 0.34257(16) 0.0150(5) Uani 1 1 d . . . . .
O1 O 0.61970(16) 0.57658(16) 0.34969(11) 0.0176(4) Uani 1 1 d . . . . .
C1 C 0.5465(2) 0.6192(2) 0.37627(13) 0.0133(5) Uani 1 1 d . . . . .
Li1 Li 0.7965(5) 0.6667 0.4167 0.0186(10) Uani 1 2 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cs1 O1 3.1199(15) 33_545 ?
Cs1 O1 3.1199(16) 32 ?
Cs1 O1 3.1199(15) 3_665 ?
Cs1 O1 3.1199(15) 2_655 ?
Cs1 O1 3.1199(15) . ?
Cs1 O1 3.1200(15) 31_655 ?
Cs1 O2 3.207(2) 35_545 ?
Cs1 O2 3.207(2) 36 ?
Cs1 O2 3.207(2) 6_655 ?
Cs1 O2 3.207(2) 5_665 ?
Cs1 O2 3.207(2) 34_655 ?
Cs1 O2 3.207(2) 4 ?
Co1 O2 2.095(2) 11_565 ?
Co1 O2 2.095(2) 3_565 ?
Co1 O2 2.095(2) 2_665 ?
Co1 O2 2.095(2) 12 ?
Co1 O2 2.095(2) . ?
Co1 O2 2.095(2) 10_455 ?
Co1 Cs1 3.8041(3) 4 ?
Co1 Cs1 3.8042(3) 7_455 ?
O2 C1 1.272(3) . ?
O2 Li1 2.185(3) 33_545 ?
O2 Cs1 3.207(2) 4 ?
O1 C1 1.238(3) . ?
O1 Li1 2.038(5) . ?
O1 Li1 2.215(5) 33_545 ?
C1 C1 1.552(4) 11_565 ?
C1 Li1 2.474(4) 33_545 ?
C1 Li1 2.722(6) . ?
Li1 O1 2.038(5) 11_565 ?
Li1 O2 2.185(3) 36 ?
Li1 O2 2.185(3) 32 ?
Li1 O1 2.215(5) 36 ?
Li1 O1 2.215(5) 32 ?
Li1 C1 2.474(4) 36 ?
Li1 C1 2.474(4) 32 ?
Li1 C1 2.722(6) 11_565 ?
Li1 Cs1 3.5860(8) 10 ?

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_3
_geom_angle_publ_flag
O1 Cs1 O1 119.371(8) 33_545 32 ?
O1 Cs1 O1 180.0 33_545 3_665 ?
O1 Cs1 O1 60.629(8) 32 3_665 ?
O1 Cs1 O1 60.629(8) 33_545 2_655 ?
O1 Cs1 O1 180.0 32 2_655 ?
O1 Cs1 O1 119.370(8) 3_665 2_655 ?
O1 Cs1 O1 60.631(8) 33_545 . ?
O1 Cs1 O1 60.630(8) 32 . ?
O1 Cs1 O1 119.370(8) 3_665 . ?
O1 Cs1 O1 119.370(8) 2_655 . ?
O1 Cs1 O1 119.370(8) 33_545 31_655 ?
O1 Cs1 O1 119.369(8) 32 31_655 ?
O1 Cs1 O1 60.630(8) 3_665 31_655 ?
O1 Cs1 O1 60.630(8) 2_655 31_655 ?
O1 Cs1 O1 180.0 . 31_655 ?
O1 Cs1 O2 62.62(5) 33_545 35_545 ?
O1 Cs1 O2 117.68(5) 32 35_545 ?
O1 Cs1 O2 117.38(5) 3_665 35_545 ?
O1 Cs1 O2 62.32(5) 2_655 35_545 ?
O1 Cs1 O2 78.74(4) . 35_545 ?
O1 Cs1 O2 101.26(4) 31_655 35_545 ?
O1 Cs1 O2 101.26(4) 33_545 36 ?
O1 Cs1 O2 62.62(5) 32 36 ?
O1 Cs1 O2 78.74(4) 3_665 36 ?
O1 Cs1 O2 117.38(5) 2_655 36 ?
O1 Cs1 O2 62.32(5) . 36 ?
O1 Cs1 O2 117.68(5) 31_655 36 ?
O2 Cs1 O2 56.97(7) 35_545 36 ?
O1 Cs1 O2 78.74(4) 33_545 6_655 ?
O1 Cs1 O2 117.38(5) 32 6_655 ?
O1 Cs1 O2 101.26(4) 3_665 6_655 ?
O1 Cs1 O2 62.62(5) 2_655 6_655 ?
O1 Cs1 O2 117.68(5) . 6_655 ?
O1 Cs1 O2 62.32(5) 31_655 6_655 ?
O2 Cs1 O2 123.03(7) 35_545 6_655 ?
O2 Cs1 O2 180.0 36 6_655 ?
O1 Cs1 O2 117.38(5) 33_545 5_665 ?
O1 Cs1 O2 62.32(5) 32 5_665 ?
O1 Cs1 O2 62.62(5) 3_665 5_665 ?
O1 Cs1 O2 117.68(5) 2_655 5_665 ?
O1 Cs1 O2 101.26(4) . 5_665 ?
O1 Cs1 O2 78.74(4) 31_655 5_665 ?
O2 Cs1 O2 180.0 35_545 5_665 ?
O2 Cs1 O2 123.03(7) 36 5_665 ?
O2 Cs1 O2 56.97(7) 6_655 5_665 ?
O1 Cs1 O2 117.68(5) 33_545 34_655 ?
O1 Cs1 O2 101.26(4) 32 34_655 ?
O1 Cs1 O2 62.32(5) 3_665 34_655 ?
O1 Cs1 O2 78.74(4) 2_655 34_655 ?
O1 Cs1 O2 117.38(5) . 34_655 ?
O1 Cs1 O2 62.62(5) 31_655 34_655 ?
O2 Cs1 O2 56.97(7) 35_545 34_655 ?
O2 Cs1 O2 56.97(7) 36 34_655 ?
O2 Cs1 O2 123.03(7) 6_655 34_655 ?
O2 Cs1 O2 123.03(7) 5_665 34_655 ?
O1 Cs1 O2 62.32(5) 33_545 4 ?
O1 Cs1 O2 78.74(4) 32 4 ?
O1 Cs1 O2 117.68(5) 3_665 4 ?
O1 Cs1 O2 101.26(4) 2_655 4 ?
O1 Cs1 O2 62.62(5) . 4 ?
O1 Cs1 O2 117.38(5) 31_655 4 ?
O2 Cs1 O2 123.03(7) 35_545 4 ?
O2 Cs1 O2 123.03(7) 36 4 ?
O2 Cs1 O2 56.97(7) 6_655 4 ?
O2 Cs1 O2 56.97(7) 5_665 4 ?
O2 Cs1 O2 180.0 34_655 4 ?
O2 Co1 O2 171.78(10) 11_565 3_565 ?
O2 Co1 O2 92.51(11) 11_565 2_665 ?
O2 Co1 O2 93.77(9) 3_565 2_665 ?
O2 Co1 O2 93.77(9) 11_565 12 ?
O2 Co1 O2 80.51(12) 3_565 12 ?
O2 Co1 O2 171.78(10) 2_665 12 ?
O2 Co1 O2 80.52(12) 11_565 . ?
O2 Co1 O2 93.77(9) 3_565 . ?
O2 Co1 O2 93.76(9) 2_665 . ?
O2 Co1 O2 92.51(11) 12 . ?
O2 Co1 O2 93.76(9) 11_565 10_455 ?
O2 Co1 O2 92.51(11) 3_565 10_455 ?
O2 Co1 O2 80.51(12) 2_665 10_455 ?
O2 Co1 O2 93.76(9) 12 10_455 ?
O2 Co1 O2 171.78(10) . 10_455 ?
O2 Co1 Cs1 122.55(7) 11_565 4 ?
O2 Co1 Cs1 57.45(7) 3_565 4 ?
O2 Co1 Cs1 57.45(7) 2_665 4 ?
O2 Co1 Cs1 122.55(7) 12 4 ?
O2 Co1 Cs1 57.44(7) . 4 ?
O2 Co1 Cs1 122.56(7) 10_455 4 ?
O2 Co1 Cs1 57.45(7) 11_565 7_455 ?
O2 Co1 Cs1 122.55(7) 3_565 7_455 ?
O2 Co1 Cs1 122.55(7) 2_665 7_455 ?
O2 Co1 Cs1 57.45(7) 12 7_455 ?
O2 Co1 Cs1 122.56(7) . 7_455 ?
O2 Co1 Cs1 57.44(7) 10_455 7_455 ?
Cs1 Co1 Cs1 180.0 4 7_455 ?
C1 O2 Co1 112.58(17) . . ?
C1 O2 Li1 87.21(19) . 33_545 ?
Co1 O2 Li1 158.57(17) . 33_545 ?
C1 O2 Cs1 136.81(16) . 4 ?
Co1 O2 Cs1 89.14(7) . 4 ?
Li1 O2 Cs1 80.98(7) 33_545 4 ?
C1 O1 Li1 109.95(18) . . ?
C1 O1 Li1 86.68(13) . 33_545 ?
Li1 O1 Li1 162.74(18) . 33_545 ?
C1 O1 Cs1 147.34(14) . . ?
Li1 O1 Cs1 85.36(11) . . ?
Li1 O1 Cs1 82.60(6) 33_545 . ?
O1 C1 O2 125.2(2) . . ?
O1 C1 C1 117.94(12) . 11_565 ?
O2 C1 C1 116.85(14) . 11_565 ?
O1 C1 Li1 63.35(13) . 33_545 ?
O2 C1 Li1 61.88(15) . 33_545 ?
C1 C1 Li1 178.01(19) 11_565 33_545 ?
O1 C1 Li1 44.74(11) . . ?
O2 C1 Li1 168.81(18) . . ?
C1 C1 Li1 73.43(6) 11_565 . ?
Li1 C1 Li1 107.96(13) 33_545 . ?
O1 Li1 O1 83.6(3) . 11_565 ?
O1 Li1 O2 101.64(12) . 36 ?
O1 Li1 O2 100.97(12) 11_565 36 ?
O1 Li1 O2 100.96(12) . 32 ?
O1 Li1 O2 101.64(12) 11_565 32 ?
O2 Li1 O2 149.5(3) 36 32 ?
O1 Li1 O1 162.08(8) . 36 ?
O1 Li1 O1 95.46(5) 11_565 36 ?
O2 Li1 O1 60.87(11) 36 36 ?
O2 Li1 O1 96.75(19) 32 36 ?
O1 Li1 O1 95.46(5) . 32 ?
O1 Li1 O1 162.08(8) 11_565 32 ?
O2 Li1 O1 96.75(19) 36 32 ?
O2 Li1 O1 60.87(11) 32 32 ?
O1 Li1 O1 90.8(2) 36 32 ?
O1 Li1 C1 132.39(9) . 36 ?
O1 Li1 C1 99.01(7) 11_565 36 ?
O2 Li1 C1 30.91(8) 36 36 ?
O2 Li1 C1 124.4(2) 32 36 ?
O1 Li1 C1 29.97(8) 36 36 ?
O1 Li1 C1 94.8(2) 32 36 ?
O1 Li1 C1 99.01(7) . 32 ?
O1 Li1 C1 132.39(9) 11_565 32 ?
O2 Li1 C1 124.4(2) 36 32 ?
O2 Li1 C1 30.90(8) 32 32 ?
O1 Li1 C1 94.8(2) 36 32 ?
O1 Li1 C1 29.97(8) 32 32 ?
C1 Li1 C1 112.2(3) 36 32 ?
O1 Li1 C1 25.31(10) . . ?
O1 Li1 C1 58.36(17) 11_565 . ?
O2 Li1 C1 105.83(16) 36 . ?
O2 Li1 C1 103.38(16) 32 . ?
O1 Li1 C1 149.50(16) 36 . ?
O1 Li1 C1 118.99(10) 32 . ?
C1 Li1 C1 131.19(15) 36 . ?
C1 Li1 C1 114.20(9) 32 . ?
O1 Li1 C1 58.36(17) . 11_565 ?
O1 Li1 C1 25.31(10) 11_565 11_565 ?
O2 Li1 C1 103.38(16) 36 11_565 ?
O2 Li1 C1 105.83(16) 32 11_565 ?
O1 Li1 C1 118.99(10) 36 11_565 ?
O1 Li1 C1 149.50(16) 32 11_565 ?
C1 Li1 C1 114.20(9) 36 11_565 ?
C1 Li1 C1 131.19(15) 32 11_565 ?
C1 Li1 C1 33.14(12) . 11_565 ?
O1 Li1 Cs1 132.40(19) . 10 ?
O1 Li1 Cs1 60.13(4) 11_565 10 ?
O2 Li1 Cs1 114.00(10) 36 10 ?
O2 Li1 Cs1 62.03(7) 32 10 ?
O1 Li1 Cs1 59.63(5) 36 10 ?
O1 Li1 Cs1 109.84(14) 32 10 ?
C1 Li1 Cs1 86.09(8) 36 10 ?
C1 Li1 Cs1 86.35(8) 32 10 ?
C1 Li1 Cs1 110.78(14) . 10 ?
C1 Li1 Cs1 82.65(8) 11_565 10 ?
O1 Li1 Cs1 60.13(4) . . ?
O1 Li1 Cs1 132.40(19) 11_565 . ?
O2 Li1 Cs1 62.03(7) 36 . ?
O2 Li1 Cs1 114.00(10) 32 . ?
O1 Li1 Cs1 109.84(14) 36 . ?
O1 Li1 Cs1 59.63(5) 32 . ?
C1 Li1 Cs1 86.35(8) 36 . ?
C1 Li1 Cs1 86.09(8) 32 . ?
C1 Li1 Cs1 82.65(8) . . ?
C1 Li1 Cs1 110.78(14) 11_565 . ?
Cs1 Li1 Cs1 166.4(2) 10 . ?

_refine_diff_density_max         0.587
_refine_diff_density_min         -1.314
_refine_diff_density_rms         0.112

####################################################################### 
# 
# 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_shelx5
_database_code_depnum_ccdc_archive 'CCDC 1944092'
loop_
_audit_author_name
_audit_author_address
'Philip Lightfoot'
;University of St Andrews
United Kingdom
;
_audit_update_record             
;
2019-09-05 deposited with the CCDC.	2019-09-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C6 Li3 Ni O12 Rb'
_chemical_formula_weight         429.06

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c :H'
_space_group_name_Hall           '-R 3 2"c'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   11.3796(7)
_cell_length_b                   11.3796(7)
_cell_length_c                   14.9962(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1681.8(2)
_cell_formula_units_Z            6
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    830
_cell_measurement_theta_min      2.5
_cell_measurement_theta_max      27.5

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.542
_exptl_crystal_F_000             1236
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    6.114
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.675
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
'The program SADABS-2008/1 - G.M. Sheldrick was used to apply a multi-scan absorption correction.'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Sealed Tube'
_diffrn_measurement_device_type  'Rigaku Mercury2 (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 13.6612
_diffrn_reflns_number            5226
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_av_R_equivalents  0.0747
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.414
_diffrn_reflns_theta_max         27.502
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             441
_reflns_number_gt                362
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Crystalmaker (Palmer, 2014)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         441
_refine_ls_number_parameters     37
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0328
_refine_ls_wR_factor_ref         0.1131
_refine_ls_wR_factor_gt          0.1025
_refine_ls_goodness_of_fit_ref   0.876
_refine_ls_restrained_S_all      0.876
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Rb1 Rb 0.6667 0.3333 0.3333 0.0167(3) Uani 1 6 d S T P . .
Ni1 Ni 0.3333 0.6667 0.4167 0.0116(4) Uani 1 6 d S T P . .
O2 O 0.40962(19) 0.56897(18) 0.34180(15) 0.0150(5) Uani 1 1 d . . . . .
O1 O 0.42726(18) 0.38291(18) 0.34995(13) 0.0168(5) Uani 1 1 d . . . . .
C1 C 0.3822(2) 0.4560(2) 0.37620(16) 0.0140(5) Uani 1 1 d . . . . .
Li1 Li 0.3333 0.2046(6) 0.4167 0.0205(13) Uani 1 2 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rb1 O1 3.0560(17) 32 ?
Rb1 O1 3.0560(17) . ?
Rb1 O1 3.0561(17) 33_545 ?
Rb1 O1 3.0561(17) 2_655 ?
Rb1 O1 3.0561(17) 3_665 ?
Rb1 O1 3.0561(17) 31_655 ?
Rb1 O2 3.139(2) 36 ?
Rb1 O2 3.139(2) 35_545 ?
Rb1 O2 3.139(2) 6_655 ?
Rb1 O2 3.139(2) 5_665 ?
Rb1 O2 3.139(2) 34_655 ?
Rb1 O2 3.139(2) 4 ?
Ni1 O2 2.053(2) 12 ?
Ni1 O2 2.053(2) 11_565 ?
Ni1 O2 2.053(2) . ?
Ni1 O2 2.053(2) 3_565 ?
Ni1 O2 2.053(2) 2_665 ?
Ni1 O2 2.053(2) 10_455 ?
Ni1 Rb1 3.7491(3) 4 ?
Ni1 Rb1 3.7491(2) 7_455 ?
O2 C1 1.271(3) . ?
O2 Li1 2.161(3) 32 ?
O2 Rb1 3.139(2) 4 ?
O1 C1 1.239(3) . ?
O1 Li1 2.022(6) . ?
O1 Li1 2.174(6) 32 ?
C1 C1 1.550(5) 12 ?
C1 Li1 2.437(5) 32 ?
C1 Li1 2.695(7) . ?
Li1 O1 2.023(6) 12 ?
Li1 O2 2.161(3) 33_545 ?
Li1 O2 2.161(3) 35_545 ?
Li1 O1 2.174(5) 35_545 ?
Li1 O1 2.174(5) 33_545 ?
Li1 C1 2.437(5) 35_545 ?
Li1 C1 2.437(5) 33_545 ?
Li1 C1 2.696(7) 12 ?
Li1 Rb1 3.5411(9) 10_445 ?

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_3
_geom_angle_publ_flag
O1 Rb1 O1 60.659(10) 32 . ?
O1 Rb1 O1 119.344(10) 32 33_545 ?
O1 Rb1 O1 60.658(10) . 33_545 ?
O1 Rb1 O1 180.0 32 2_655 ?
O1 Rb1 O1 119.342(10) . 2_655 ?
O1 Rb1 O1 60.657(10) 33_545 2_655 ?
O1 Rb1 O1 60.657(10) 32 3_665 ?
O1 Rb1 O1 119.343(10) . 3_665 ?
O1 Rb1 O1 180.0 33_545 3_665 ?
O1 Rb1 O1 119.342(10) 2_655 3_665 ?
O1 Rb1 O1 119.342(10) 32 31_655 ?
O1 Rb1 O1 180.0 . 31_655 ?
O1 Rb1 O1 119.341(10) 33_545 31_655 ?
O1 Rb1 O1 60.658(10) 2_655 31_655 ?
O1 Rb1 O1 60.658(10) 3_665 31_655 ?
O1 Rb1 O2 62.97(5) 32 36 ?
O1 Rb1 O2 78.83(5) . 36 ?
O1 Rb1 O2 117.74(5) 33_545 36 ?
O1 Rb1 O2 117.03(5) 2_655 36 ?
O1 Rb1 O2 62.26(5) 3_665 36 ?
O1 Rb1 O2 101.17(5) 31_655 36 ?
O1 Rb1 O2 101.17(5) 32 35_545 ?
O1 Rb1 O2 62.26(5) . 35_545 ?
O1 Rb1 O2 62.97(5) 33_545 35_545 ?
O1 Rb1 O2 78.83(5) 2_655 35_545 ?
O1 Rb1 O2 117.03(5) 3_665 35_545 ?
O1 Rb1 O2 117.74(5) 31_655 35_545 ?
O2 Rb1 O2 56.62(6) 36 35_545 ?
O1 Rb1 O2 117.03(5) 32 6_655 ?
O1 Rb1 O2 101.17(5) . 6_655 ?
O1 Rb1 O2 62.26(5) 33_545 6_655 ?
O1 Rb1 O2 62.97(5) 2_655 6_655 ?
O1 Rb1 O2 117.74(5) 3_665 6_655 ?
O1 Rb1 O2 78.83(5) 31_655 6_655 ?
O2 Rb1 O2 180.0 36 6_655 ?
O2 Rb1 O2 123.38(6) 35_545 6_655 ?
O1 Rb1 O2 78.83(5) 32 5_665 ?
O1 Rb1 O2 117.74(5) . 5_665 ?
O1 Rb1 O2 117.03(5) 33_545 5_665 ?
O1 Rb1 O2 101.17(5) 2_655 5_665 ?
O1 Rb1 O2 62.97(5) 3_665 5_665 ?
O1 Rb1 O2 62.26(5) 31_655 5_665 ?
O2 Rb1 O2 123.38(6) 36 5_665 ?
O2 Rb1 O2 180.0 35_545 5_665 ?
O2 Rb1 O2 56.62(6) 6_655 5_665 ?
O1 Rb1 O2 117.74(5) 32 34_655 ?
O1 Rb1 O2 117.04(5) . 34_655 ?
O1 Rb1 O2 101.17(5) 33_545 34_655 ?
O1 Rb1 O2 62.26(5) 2_655 34_655 ?
O1 Rb1 O2 78.83(5) 3_665 34_655 ?
O1 Rb1 O2 62.96(5) 31_655 34_655 ?
O2 Rb1 O2 56.62(6) 36 34_655 ?
O2 Rb1 O2 56.62(6) 35_545 34_655 ?
O2 Rb1 O2 123.38(6) 6_655 34_655 ?
O2 Rb1 O2 123.38(6) 5_665 34_655 ?
O1 Rb1 O2 62.26(5) 32 4 ?
O1 Rb1 O2 62.97(5) . 4 ?
O1 Rb1 O2 78.83(5) 33_545 4 ?
O1 Rb1 O2 117.74(5) 2_655 4 ?
O1 Rb1 O2 101.17(5) 3_665 4 ?
O1 Rb1 O2 117.03(5) 31_655 4 ?
O2 Rb1 O2 123.38(6) 36 4 ?
O2 Rb1 O2 123.38(6) 35_545 4 ?
O2 Rb1 O2 56.62(6) 6_655 4 ?
O2 Rb1 O2 56.62(6) 5_665 4 ?
O2 Rb1 O2 180.0 34_655 4 ?
O2 Ni1 O2 92.95(9) 12 11_565 ?
O2 Ni1 O2 82.31(11) 12 . ?
O2 Ni1 O2 92.17(11) 11_565 . ?
O2 Ni1 O2 92.17(11) 12 3_565 ?
O2 Ni1 O2 173.19(10) 11_565 3_565 ?
O2 Ni1 O2 92.95(9) . 3_565 ?
O2 Ni1 O2 173.20(10) 12 2_665 ?
O2 Ni1 O2 82.31(11) 11_565 2_665 ?
O2 Ni1 O2 92.95(9) . 2_665 ?
O2 Ni1 O2 92.95(9) 3_565 2_665 ?
O2 Ni1 O2 92.95(9) 12 10_455 ?
O2 Ni1 O2 92.95(9) 11_565 10_455 ?
O2 Ni1 O2 173.20(10) . 10_455 ?
O2 Ni1 O2 82.31(11) 3_565 10_455 ?
O2 Ni1 O2 92.17(11) 2_665 10_455 ?
O2 Ni1 Rb1 123.15(6) 12 4 ?
O2 Ni1 Rb1 123.15(6) 11_565 4 ?
O2 Ni1 Rb1 56.85(6) . 4 ?
O2 Ni1 Rb1 56.85(6) 3_565 4 ?
O2 Ni1 Rb1 56.85(6) 2_665 4 ?
O2 Ni1 Rb1 123.15(6) 10_455 4 ?
O2 Ni1 Rb1 56.85(6) 12 7_455 ?
O2 Ni1 Rb1 56.85(6) 11_565 7_455 ?
O2 Ni1 Rb1 123.15(6) . 7_455 ?
O2 Ni1 Rb1 123.15(6) 3_565 7_455 ?
O2 Ni1 Rb1 123.15(6) 2_665 7_455 ?
O2 Ni1 Rb1 56.85(6) 10_455 7_455 ?
Rb1 Ni1 Rb1 180.0 4 7_455 ?
C1 O2 Ni1 111.70(17) . . ?
C1 O2 Li1 86.4(2) . 32 ?
Ni1 O2 Li1 160.1(2) . 32 ?
C1 O2 Rb1 136.58(16) . 4 ?
Ni1 O2 Rb1 89.95(7) . 4 ?
Li1 O2 Rb1 81.60(7) 32 4 ?
C1 O1 Li1 109.1(2) . . ?
C1 O1 Li1 86.60(15) . 32 ?
Li1 O1 Li1 163.0(2) . 32 ?
C1 O1 Rb1 148.86(16) . . ?
Li1 O1 Rb1 85.87(13) . . ?
Li1 O1 Rb1 83.41(8) 32 . ?
O1 C1 O2 125.1(2) . . ?
O1 C1 C1 118.14(14) . 12 ?
O2 C1 C1 116.73(15) . 12 ?
O1 C1 Li1 62.91(15) . 32 ?
O2 C1 Li1 62.23(15) . 32 ?
C1 C1 Li1 178.74(17) 12 32 ?
O1 C1 Li1 45.15(12) . . ?
O2 C1 Li1 168.74(19) . . ?
C1 C1 Li1 73.30(7) 12 . ?
Li1 C1 Li1 107.81(15) 32 . ?
O1 Li1 O1 84.7(3) . 12 ?
O1 Li1 O2 101.94(13) . 33_545 ?
O1 Li1 O2 99.90(13) 12 33_545 ?
O1 Li1 O2 99.90(13) . 35_545 ?
O1 Li1 O2 101.94(13) 12 35_545 ?
O2 Li1 O2 150.3(4) 33_545 35_545 ?
O1 Li1 O1 161.29(10) . 35_545 ?
O1 Li1 O1 94.64(6) 12 35_545 ?
O2 Li1 O1 96.6(2) 33_545 35_545 ?
O2 Li1 O1 61.86(13) 35_545 35_545 ?
O1 Li1 O1 94.64(6) . 33_545 ?
O1 Li1 O1 161.29(10) 12 33_545 ?
O2 Li1 O1 61.86(13) 33_545 33_545 ?
O2 Li1 O1 96.6(2) 35_545 33_545 ?
O1 Li1 O1 91.8(3) 35_545 33_545 ?
O1 Li1 C1 131.13(10) . 35_545 ?
O1 Li1 C1 99.35(8) 12 35_545 ?
O2 Li1 C1 124.7(3) 33_545 35_545 ?
O2 Li1 C1 31.37(10) 35_545 35_545 ?
O1 Li1 C1 30.49(9) 35_545 35_545 ?
O1 Li1 C1 95.1(3) 33_545 35_545 ?
O1 Li1 C1 99.35(8) . 33_545 ?
O1 Li1 C1 131.13(10) 12 33_545 ?
O2 Li1 C1 31.37(10) 33_545 33_545 ?
O2 Li1 C1 124.7(3) 35_545 33_545 ?
O1 Li1 C1 95.1(3) 35_545 33_545 ?
O1 Li1 C1 30.49(9) 33_545 33_545 ?
C1 Li1 C1 112.6(3) 35_545 33_545 ?
O1 Li1 C1 25.74(12) . . ?
O1 Li1 C1 59.04(19) 12 . ?
O2 Li1 C1 103.41(18) 33_545 . ?
O2 Li1 C1 105.02(19) 35_545 . ?
O1 Li1 C1 149.04(19) 35_545 . ?
O1 Li1 C1 118.37(12) 33_545 . ?
C1 Li1 C1 130.79(18) 35_545 . ?
C1 Li1 C1 114.21(11) 33_545 . ?
O1 Li1 C1 59.04(19) . 12 ?
O1 Li1 C1 25.74(12) 12 12 ?
O2 Li1 C1 105.02(19) 33_545 12 ?
O2 Li1 C1 103.42(18) 35_545 12 ?
O1 Li1 C1 118.37(12) 35_545 12 ?
O1 Li1 C1 149.04(19) 33_545 12 ?
C1 Li1 C1 114.21(11) 35_545 12 ?
C1 Li1 C1 130.79(18) 33_545 12 ?
C1 Li1 C1 33.41(13) . 12 ?
O1 Li1 Rb1 133.6(2) . 10_445 ?
O1 Li1 Rb1 59.40(5) 12 10_445 ?
O2 Li1 Rb1 61.27(6) 33_545 10_445 ?
O2 Li1 Rb1 114.72(11) 35_545 10_445 ?
O1 Li1 Rb1 59.02(6) 35_545 10_445 ?
O1 Li1 Rb1 110.18(17) 33_545 10_445 ?
C1 Li1 Rb1 86.26(10) 35_545 10_445 ?
C1 Li1 Rb1 85.97(10) 33_545 10_445 ?
C1 Li1 Rb1 111.23(16) . 10_445 ?
C1 Li1 Rb1 82.62(9) 12 10_445 ?
O1 Li1 Rb1 59.40(5) . . ?
O1 Li1 Rb1 133.6(2) 12 . ?
O2 Li1 Rb1 114.71(11) 33_545 . ?
O2 Li1 Rb1 61.27(6) 35_545 . ?
O1 Li1 Rb1 110.18(17) 35_545 . ?
O1 Li1 Rb1 59.02(6) 33_545 . ?
C1 Li1 Rb1 85.97(10) 35_545 . ?
C1 Li1 Rb1 86.26(10) 33_545 . ?
C1 Li1 Rb1 82.63(9) . . ?
C1 Li1 Rb1 111.23(16) 12 . ?
Rb1 Li1 Rb1 166.0(2) 10_445 . ?

_refine_diff_density_max         0.706
_refine_diff_density_min         -0.840
_refine_diff_density_rms         0.123

####################################################################### 
# 
# 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_shelx8
_database_code_depnum_ccdc_archive 'CCDC 1944095'
loop_
_audit_author_name
_audit_author_address
'Philip Lightfoot'
;University of St Andrews
United Kingdom
;
_audit_update_record             
;
2019-09-05 deposited with the CCDC.	2019-09-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 Co O12, K, 3(Li)'
_chemical_formula_sum            'C6 Co K Li3 O12'
_chemical_formula_weight         382.91

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c :H'
_space_group_name_Hall           '-R 3 2"c'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   11.3215(9)
_cell_length_b                   11.3215(9)
_cell_length_c                   15.0942(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1675.5(3)
_cell_formula_units_Z            6
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    581
_cell_measurement_theta_min      2.5
_cell_measurement_theta_max      27.5

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.277
_exptl_crystal_F_000             1122
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_exptl_absorpt_coefficient_mu    1.979
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.511
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
'The program SADABS-2008/1 - G.M. Sheldrick was used to apply a multi-scan absorption correction.'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Sealed Tube'
_diffrn_measurement_device_type  'Rigaku Mercury2 (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 13.6612
_diffrn_reflns_number            5415
_diffrn_reflns_av_unetI/netI     0.0550
_diffrn_reflns_av_R_equivalents  0.1083
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.407
_diffrn_reflns_theta_max         27.501
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             436
_reflns_number_gt                284
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Crystalmaker (Palmer, 2014)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         436
_refine_ls_number_parameters     37
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0329
_refine_ls_wR_factor_ref         0.1000
_refine_ls_wR_factor_gt          0.0808
_refine_ls_goodness_of_fit_ref   0.631
_refine_ls_restrained_S_all      0.631
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.3333 0.6667 0.4167 0.0128(3) Uani 1 6 d S T P . .
K1 K 1.0000 1.0000 0.5000 0.0259(4) Uani 1 6 d S T P . .
O1 O 0.7158(2) 0.7606(2) 0.48333(15) 0.0177(5) Uani 1 1 d . . . . .
O2 O 0.5099(2) 0.7397(2) 0.49255(15) 0.0169(5) Uani 1 1 d . . . . .
C1 C 0.5969(3) 0.7144(3) 0.4573(2) 0.0155(6) Uani 1 1 d . . . . .
Li1 Li 0.8003(7) 0.6667 0.4167 0.0178(15) Uani 1 2 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O2 2.083(2) 11_565 ?
Co1 O2 2.083(2) 12 ?
Co1 O2 2.083(2) 10_455 ?
Co1 O2 2.083(2) . ?
Co1 O2 2.083(2) 2_665 ?
Co1 O2 2.083(2) 3_565 ?
Co1 K1 3.7735(3) 16_445 ?
Co1 K1 3.7736(3) 13_444 ?
K1 O1 3.007(2) . ?
K1 O1 3.007(2) 19_776 ?
K1 O1 3.007(2) 21_656 ?
K1 O1 3.007(2) 3_675 ?
K1 O1 3.007(2) 20_566 ?
K1 O1 3.007(2) 2_765 ?
K1 O2 3.152(2) 28_665 ?
K1 O2 3.152(2) 16 ?
K1 O2 3.152(2) 30_565 ?
K1 O2 3.152(2) 18_655 ?
K1 O2 3.152(2) 29 ?
K1 O2 3.152(2) 17_665 ?
O1 C1 1.240(4) . ?
O1 Li1 2.019(6) . ?
O1 Li1 2.165(6) 20_566 ?
O2 C1 1.271(4) . ?
O2 Li1 2.130(3) 20_566 ?
O2 K1 3.152(2) 16_445 ?
C1 C1 1.542(6) 11_565 ?
C1 Li1 2.418(5) 20_566 ?
C1 Li1 2.686(8) . ?
Li1 O1 2.019(6) 11_565 ?
Li1 O2 2.130(3) 21_656 ?
Li1 O2 2.130(3) 28_665 ?
Li1 O1 2.165(6) 28_665 ?
Li1 O1 2.165(6) 21_656 ?
Li1 C1 2.418(5) 28_665 ?
Li1 C1 2.418(5) 21_656 ?
Li1 C1 2.687(8) 11_565 ?
Li1 K1 3.5218(9) 10_445 ?

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_3
_geom_angle_publ_flag
O2 Co1 O2 92.68(8) 11_565 12 ?
O2 Co1 O2 92.68(8) 11_565 10_455 ?
O2 Co1 O2 92.67(8) 12 10_455 ?
O2 Co1 O2 80.82(12) 11_565 . ?
O2 Co1 O2 170.45(11) 12 . ?
O2 Co1 O2 94.59(12) 10_455 . ?
O2 Co1 O2 170.45(12) 11_565 2_665 ?
O2 Co1 O2 94.59(12) 12 2_665 ?
O2 Co1 O2 80.82(12) 10_455 2_665 ?
O2 Co1 O2 92.67(8) . 2_665 ?
O2 Co1 O2 94.59(12) 11_565 3_565 ?
O2 Co1 O2 80.82(12) 12 3_565 ?
O2 Co1 O2 170.45(11) 10_455 3_565 ?
O2 Co1 O2 92.67(8) . 3_565 ?
O2 Co1 O2 92.67(8) 2_665 3_565 ?
O2 Co1 K1 123.35(6) 11_565 16_445 ?
O2 Co1 K1 123.35(6) 12 16_445 ?
O2 Co1 K1 123.35(6) 10_455 16_445 ?
O2 Co1 K1 56.65(6) . 16_445 ?
O2 Co1 K1 56.65(6) 2_665 16_445 ?
O2 Co1 K1 56.65(6) 3_565 16_445 ?
O2 Co1 K1 56.65(6) 11_565 13_444 ?
O2 Co1 K1 56.65(6) 12 13_444 ?
O2 Co1 K1 56.65(6) 10_455 13_444 ?
O2 Co1 K1 123.35(6) . 13_444 ?
O2 Co1 K1 123.35(6) 2_665 13_444 ?
O2 Co1 K1 123.35(6) 3_565 13_444 ?
K1 Co1 K1 180.0 16_445 13_444 ?
O1 K1 O1 180.0 . 19_776 ?
O1 K1 O1 60.693(13) . 21_656 ?
O1 K1 O1 119.307(13) 19_776 21_656 ?
O1 K1 O1 119.307(13) . 3_675 ?
O1 K1 O1 60.693(13) 19_776 3_675 ?
O1 K1 O1 180.0 21_656 3_675 ?
O1 K1 O1 60.693(13) . 20_566 ?
O1 K1 O1 119.307(13) 19_776 20_566 ?
O1 K1 O1 119.307(13) 21_656 20_566 ?
O1 K1 O1 60.693(13) 3_675 20_566 ?
O1 K1 O1 119.307(13) . 2_765 ?
O1 K1 O1 60.693(13) 19_776 2_765 ?
O1 K1 O1 60.693(13) 21_656 2_765 ?
O1 K1 O1 119.307(14) 3_675 2_765 ?
O1 K1 O1 180.0 20_566 2_765 ?
O1 K1 O2 62.32(6) . 28_665 ?
O1 K1 O2 117.68(6) 19_776 28_665 ?
O1 K1 O2 62.65(6) 21_656 28_665 ?
O1 K1 O2 117.35(6) 3_675 28_665 ?
O1 K1 O2 101.78(6) 20_566 28_665 ?
O1 K1 O2 78.22(6) 2_765 28_665 ?
O1 K1 O2 117.68(6) . 16 ?
O1 K1 O2 62.32(6) 19_776 16 ?
O1 K1 O2 117.35(6) 21_656 16 ?
O1 K1 O2 62.65(6) 3_675 16 ?
O1 K1 O2 78.22(6) 20_566 16 ?
O1 K1 O2 101.78(6) 2_765 16 ?
O2 K1 O2 180.0 28_665 16 ?
O1 K1 O2 117.35(6) . 30_565 ?
O1 K1 O2 62.65(6) 19_776 30_565 ?
O1 K1 O2 101.79(6) 21_656 30_565 ?
O1 K1 O2 78.21(6) 3_675 30_565 ?
O1 K1 O2 117.68(6) 20_566 30_565 ?
O1 K1 O2 62.32(6) 2_765 30_565 ?
O2 K1 O2 57.13(6) 28_665 30_565 ?
O2 K1 O2 122.87(7) 16 30_565 ?
O1 K1 O2 62.65(6) . 18_655 ?
O1 K1 O2 117.35(6) 19_776 18_655 ?
O1 K1 O2 78.21(6) 21_656 18_655 ?
O1 K1 O2 101.79(6) 3_675 18_655 ?
O1 K1 O2 62.32(6) 20_566 18_655 ?
O1 K1 O2 117.68(6) 2_765 18_655 ?
O2 K1 O2 122.87(6) 28_665 18_655 ?
O2 K1 O2 57.13(6) 16 18_655 ?
O2 K1 O2 180.0 30_565 18_655 ?
O1 K1 O2 78.22(6) . 29 ?
O1 K1 O2 101.79(6) 19_776 29 ?
O1 K1 O2 117.68(6) 21_656 29 ?
O1 K1 O2 62.32(6) 3_675 29 ?
O1 K1 O2 62.65(6) 20_566 29 ?
O1 K1 O2 117.35(6) 2_765 29 ?
O2 K1 O2 57.13(6) 28_665 29 ?
O2 K1 O2 122.87(6) 16 29 ?
O2 K1 O2 57.13(6) 30_565 29 ?
O2 K1 O2 122.87(6) 18_655 29 ?
O1 K1 O2 101.78(6) . 17_665 ?
O1 K1 O2 78.21(6) 19_776 17_665 ?
O1 K1 O2 62.32(6) 21_656 17_665 ?
O1 K1 O2 117.68(6) 3_675 17_665 ?
O1 K1 O2 117.35(6) 20_566 17_665 ?
O1 K1 O2 62.65(6) 2_765 17_665 ?
O2 K1 O2 122.87(6) 28_665 17_665 ?
O2 K1 O2 57.13(6) 16 17_665 ?
O2 K1 O2 122.87(6) 30_565 17_665 ?
O2 K1 O2 57.13(6) 18_655 17_665 ?
O2 K1 O2 180.0 29 17_665 ?
C1 O1 Li1 108.7(2) . . ?
C1 O1 Li1 85.94(18) . 20_566 ?
Li1 O1 Li1 163.6(2) . 20_566 ?
C1 O1 K1 148.62(19) . . ?
Li1 O1 K1 86.63(14) . . ?
Li1 O1 K1 84.15(9) 20_566 . ?
C1 O2 Co1 112.21(19) . . ?
C1 O2 Li1 86.7(2) . 20_566 ?
Co1 O2 Li1 158.7(2) . 20_566 ?
C1 O2 K1 138.71(18) . 16_445 ?
Co1 O2 K1 89.84(7) . 16_445 ?
Li1 O2 K1 81.13(7) 20_566 16_445 ?
O1 C1 O2 124.9(3) . . ?
O1 C1 C1 118.28(17) . 11_565 ?
O2 C1 C1 116.82(17) . 11_565 ?
O1 C1 Li1 63.30(17) . 20_566 ?
O2 C1 Li1 61.61(17) . 20_566 ?
C1 C1 Li1 178.20(19) 11_565 20_566 ?
O1 C1 Li1 45.38(15) . . ?
O2 C1 Li1 168.3(2) . . ?
C1 C1 Li1 73.32(8) 11_565 . ?
Li1 C1 Li1 108.34(18) 20_566 . ?
O1 Li1 O1 85.0(3) . 11_565 ?
O1 Li1 O2 101.41(15) . 21_656 ?
O1 Li1 O2 100.43(15) 11_565 21_656 ?
O1 Li1 O2 100.43(15) . 28_665 ?
O1 Li1 O2 101.41(15) 11_565 28_665 ?
O2 Li1 O2 150.2(4) 21_656 28_665 ?
O1 Li1 O1 162.06(12) . 28_665 ?
O1 Li1 O1 93.07(8) 11_565 28_665 ?
O2 Li1 O1 96.5(2) 21_656 28_665 ?
O2 Li1 O1 62.41(14) 28_665 28_665 ?
O1 Li1 O1 93.07(8) . 21_656 ?
O1 Li1 O1 162.06(12) 11_565 21_656 ?
O2 Li1 O1 62.41(14) 21_656 21_656 ?
O2 Li1 O1 96.5(2) 28_665 21_656 ?
O1 Li1 O1 94.1(3) 28_665 21_656 ?
O1 Li1 C1 131.86(13) . 28_665 ?
O1 Li1 C1 98.11(10) 11_565 28_665 ?
O2 Li1 C1 124.7(3) 21_656 28_665 ?
O2 Li1 C1 31.65(11) 28_665 28_665 ?
O1 Li1 C1 30.76(12) 28_665 28_665 ?
O1 Li1 C1 96.4(3) 21_656 28_665 ?
O1 Li1 C1 98.11(10) . 21_656 ?
O1 Li1 C1 131.86(13) 11_565 21_656 ?
O2 Li1 C1 31.65(11) 21_656 21_656 ?
O2 Li1 C1 124.7(3) 28_665 21_656 ?
O1 Li1 C1 96.4(3) 28_665 21_656 ?
O1 Li1 C1 30.76(12) 21_656 21_656 ?
C1 Li1 C1 113.5(3) 28_665 21_656 ?
O1 Li1 C1 25.92(13) . . ?
O1 Li1 C1 59.1(2) 11_565 . ?
O2 Li1 C1 103.0(2) 21_656 . ?
O2 Li1 C1 105.5(2) 28_665 . ?
O1 Li1 C1 148.3(2) 28_665 . ?
O1 Li1 C1 117.07(14) 21_656 . ?
C1 Li1 C1 130.9(2) 28_665 . ?
C1 Li1 C1 113.26(13) 21_656 . ?
O1 Li1 C1 59.1(2) . 11_565 ?
O1 Li1 C1 25.92(13) 11_565 11_565 ?
O2 Li1 C1 105.5(2) 21_656 11_565 ?
O2 Li1 C1 103.0(2) 28_665 11_565 ?
O1 Li1 C1 117.07(14) 28_665 11_565 ?
O1 Li1 C1 148.3(2) 21_656 11_565 ?
C1 Li1 C1 113.26(13) 28_665 11_565 ?
C1 Li1 C1 130.9(2) 21_656 11_565 ?
C1 Li1 C1 33.36(16) . 11_565 ?
O1 Li1 K1 132.8(2) . 10_445 ?
O1 Li1 K1 58.47(6) 11_565 10_445 ?
O2 Li1 K1 62.17(6) 21_656 10_445 ?
O2 Li1 K1 114.35(11) 28_665 10_445 ?
O1 Li1 K1 58.14(6) 28_665 10_445 ?
O1 Li1 K1 112.52(19) 21_656 10_445 ?
C1 Li1 K1 85.61(11) 28_665 10_445 ?
C1 Li1 K1 87.72(11) 21_656 10_445 ?
C1 Li1 K1 110.18(17) . 10_445 ?
C1 Li1 K1 81.87(10) 11_565 10_445 ?
O1 Li1 K1 58.47(6) . . ?
O1 Li1 K1 132.8(2) 11_565 . ?
O2 Li1 K1 114.35(11) 21_656 . ?
O2 Li1 K1 62.17(6) 28_665 . ?
O1 Li1 K1 112.52(19) 28_665 . ?
O1 Li1 K1 58.14(6) 21_656 . ?
C1 Li1 K1 87.72(11) 28_665 . ?
C1 Li1 K1 85.61(11) 21_656 . ?
C1 Li1 K1 81.87(11) . . ?
C1 Li1 K1 110.17(17) 11_565 . ?
K1 Li1 K1 167.8(2) 10_445 . ?

_refine_diff_density_max         0.442
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.091

####################################################################### 
# 
# 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_shelx3
_database_code_depnum_ccdc_archive 'CCDC 1944090'
loop_
_audit_author_name
_audit_author_address
'Philip Lightfoot'
;University of St Andrews
United Kingdom
;
_audit_update_record             
;
2019-09-05 deposited with the CCDC.	2019-09-06 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT974_shelx3              
;
PROBLEM: Check Calcd Negative Resid. Density on       Fe1      -2.77 eA-3
RESPONSE: about 10% of atomic scattering, no detrimental effect to final model
;
# Added during the CSD deposition process: Thursday 05 September 2019 08:23 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C6 Cs Fe Li3 O12'
_chemical_formula_weight         473.64

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c :H'
_space_group_name_Hall           '-R 3 2"c'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   11.6046(8)
_cell_length_b                   11.6046(8)
_cell_length_c                   15.1779(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1770.1(3)
_cell_formula_units_Z            6
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    874
_cell_measurement_theta_min      2.4
_cell_measurement_theta_max      27.5

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.666
_exptl_crystal_F_000             1332
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_exptl_absorpt_coefficient_mu    4.385
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.480
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
'The program SADABS-2008/1 - G.M. Sheldrick was used to apply a multi-scan absorption correction.'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Sealed Tube'
_diffrn_measurement_device_type  'Rigaku Mercury2 (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 13.6612
_diffrn_reflns_number            5297
_diffrn_reflns_av_unetI/netI     0.0475
_diffrn_reflns_av_R_equivalents  0.0994
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.364
_diffrn_reflns_theta_max         27.551
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measured_fraction_theta_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_point_group_measured_fraction_full 0.969
_reflns_number_total             447
_reflns_number_gt                400
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Crystalmaker (Palmer, 2014)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         447
_refine_ls_number_parameters     37
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0346
_refine_ls_wR_factor_ref         0.1357
_refine_ls_wR_factor_gt          0.1153
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_restrained_S_all      1.145
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cs1 Cs 1.0000 1.0000 0.5000 0.0118(4) Uani 1 6 d S T P . .
Fe1 Fe 1.0000 1.0000 0.7500 0.0104(6) Uani 1 6 d S T P . .
O2 O 0.8203(3) 0.8943(3) 0.6763(2) 0.0148(7) Uani 1 1 d . . . . .
O1 O 0.62112(19) 0.7114(2) 0.68325(14) 0.0159(6) Uani 1 1 d . . . . .
C1 C 0.7365(3) 0.7839(2) 0.70967(18) 0.0120(6) Uani 1 1 d . . . . .
Li1 Li 0.5362(7) 0.5362(7) 0.7500 0.0184(14) Uani 1 2 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cs1 O1 3.1228(19) 28_665 ?
Cs1 O1 3.1228(19) 16 ?
Cs1 O1 3.123(2) 30_565 ?
Cs1 O1 3.123(2) 18_655 ?
Cs1 O1 3.1230(19) 29 ?
Cs1 O1 3.1230(19) 17_665 ?
Cs1 O2 3.234(4) . ?
Cs1 O2 3.234(4) 3_675 ?
Cs1 O2 3.234(4) 21_656 ?
Cs1 O2 3.234(4) 2_765 ?
Cs1 O2 3.234(4) 20_566 ?
Cs1 O2 3.234(4) 19_776 ?
Fe1 O2 2.132(3) . ?
Fe1 O2 2.132(3) 6_766 ?
Fe1 O2 2.132(3) 5_676 ?
Fe1 O2 2.132(3) 4_556 ?
Fe1 O2 2.132(3) 2_765 ?
Fe1 O2 2.132(3) 3_675 ?
Fe1 Cs1 3.7945(3) 4_556 ?
O2 C1 1.264(4) . ?
O2 Li1 2.177(4) 27_556 ?
O1 C1 1.239(3) . ?
O1 Li1 2.032(7) . ?
O1 Li1 2.230(7) 27_556 ?
O1 Cs1 3.1228(19) 16_445 ?
C1 C1 1.551(5) 4_556 ?
C1 Li1 2.475(5) 27_556 ?
C1 Li1 2.713(9) . ?
Li1 O1 2.032(7) 4_556 ?
Li1 O2 2.177(4) 26_456 ?
Li1 O2 2.177(4) 35_545 ?
Li1 O1 2.230(7) 26_456 ?
Li1 O1 2.230(7) 35_545 ?
Li1 C1 2.475(5) 26_456 ?
Li1 C1 2.475(5) 35_545 ?
Li1 C1 2.713(9) 4_556 ?
Li1 Cs1 3.6052(10) 16_445 ?
Li1 Cs1 3.6052(10) 7_445 ?

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_3
_geom_angle_publ_flag
O1 Cs1 O1 180.0 28_665 16 ?
O1 Cs1 O1 119.360(11) 28_665 30_565 ?
O1 Cs1 O1 60.640(11) 16 30_565 ?
O1 Cs1 O1 60.640(11) 28_665 18_655 ?
O1 Cs1 O1 119.360(11) 16 18_655 ?
O1 Cs1 O1 180.0 30_565 18_655 ?
O1 Cs1 O1 119.357(11) 28_665 29 ?
O1 Cs1 O1 60.643(11) 16 29 ?
O1 Cs1 O1 119.355(11) 30_565 29 ?
O1 Cs1 O1 60.645(11) 18_655 29 ?
O1 Cs1 O1 60.643(11) 28_665 17_665 ?
O1 Cs1 O1 119.357(11) 16 17_665 ?
O1 Cs1 O1 60.645(11) 30_565 17_665 ?
O1 Cs1 O1 119.355(11) 18_655 17_665 ?
O1 Cs1 O1 180.0 29 17_665 ?
O1 Cs1 O2 78.28(6) 28_665 . ?
O1 Cs1 O2 101.72(6) 16 . ?
O1 Cs1 O2 118.13(7) 30_565 . ?
O1 Cs1 O2 61.87(7) 18_655 . ?
O1 Cs1 O2 62.06(7) 29 . ?
O1 Cs1 O2 117.94(7) 17_665 . ?
O1 Cs1 O2 118.13(7) 28_665 3_675 ?
O1 Cs1 O2 61.87(7) 16 3_675 ?
O1 Cs1 O2 62.06(7) 30_565 3_675 ?
O1 Cs1 O2 117.94(7) 18_655 3_675 ?
O1 Cs1 O2 78.28(6) 29 3_675 ?
O1 Cs1 O2 101.72(6) 17_665 3_675 ?
O2 Cs1 O2 58.18(9) . 3_675 ?
O1 Cs1 O2 61.87(7) 28_665 21_656 ?
O1 Cs1 O2 118.13(7) 16 21_656 ?
O1 Cs1 O2 117.94(7) 30_565 21_656 ?
O1 Cs1 O2 62.06(7) 18_655 21_656 ?
O1 Cs1 O2 101.72(6) 29 21_656 ?
O1 Cs1 O2 78.28(6) 17_665 21_656 ?
O2 Cs1 O2 121.82(10) . 21_656 ?
O2 Cs1 O2 180.0 3_675 21_656 ?
O1 Cs1 O2 62.06(7) 28_665 2_765 ?
O1 Cs1 O2 117.94(7) 16 2_765 ?
O1 Cs1 O2 78.28(6) 30_565 2_765 ?
O1 Cs1 O2 101.72(6) 18_655 2_765 ?
O1 Cs1 O2 118.13(7) 29 2_765 ?
O1 Cs1 O2 61.87(7) 17_665 2_765 ?
O2 Cs1 O2 58.18(9) . 2_765 ?
O2 Cs1 O2 58.18(9) 3_675 2_765 ?
O2 Cs1 O2 121.82(9) 21_656 2_765 ?
O1 Cs1 O2 117.94(7) 28_665 20_566 ?
O1 Cs1 O2 62.06(7) 16 20_566 ?
O1 Cs1 O2 101.72(6) 30_565 20_566 ?
O1 Cs1 O2 78.28(6) 18_655 20_566 ?
O1 Cs1 O2 61.87(7) 29 20_566 ?
O1 Cs1 O2 118.13(7) 17_665 20_566 ?
O2 Cs1 O2 121.82(9) . 20_566 ?
O2 Cs1 O2 121.82(9) 3_675 20_566 ?
O2 Cs1 O2 58.18(9) 21_656 20_566 ?
O2 Cs1 O2 180.0 2_765 20_566 ?
O1 Cs1 O2 101.72(6) 28_665 19_776 ?
O1 Cs1 O2 78.28(6) 16 19_776 ?
O1 Cs1 O2 61.87(7) 30_565 19_776 ?
O1 Cs1 O2 118.13(7) 18_655 19_776 ?
O1 Cs1 O2 117.94(7) 29 19_776 ?
O1 Cs1 O2 62.06(7) 17_665 19_776 ?
O2 Cs1 O2 180.0 . 19_776 ?
O2 Cs1 O2 121.82(10) 3_675 19_776 ?
O2 Cs1 O2 58.18(9) 21_656 19_776 ?
O2 Cs1 O2 121.82(9) 2_765 19_776 ?
O2 Cs1 O2 58.18(9) 20_566 19_776 ?
O2 Fe1 O2 170.12(15) . 6_766 ?
O2 Fe1 O2 92.65(18) . 5_676 ?
O2 Fe1 O2 95.02(14) 6_766 5_676 ?
O2 Fe1 O2 78.08(18) . 4_556 ?
O2 Fe1 O2 95.02(14) 6_766 4_556 ?
O2 Fe1 O2 95.02(14) 5_676 4_556 ?
O2 Fe1 O2 95.02(14) . 2_765 ?
O2 Fe1 O2 78.08(18) 6_766 2_765 ?
O2 Fe1 O2 170.12(15) 5_676 2_765 ?
O2 Fe1 O2 92.65(18) 4_556 2_765 ?
O2 Fe1 O2 95.02(14) . 3_675 ?
O2 Fe1 O2 92.65(18) 6_766 3_675 ?
O2 Fe1 O2 78.08(18) 5_676 3_675 ?
O2 Fe1 O2 170.12(15) 4_556 3_675 ?
O2 Fe1 O2 95.02(14) 2_765 3_675 ?
O2 Fe1 Cs1 58.37(10) . . ?
O2 Fe1 Cs1 121.63(10) 6_766 . ?
O2 Fe1 Cs1 121.63(10) 5_676 . ?
O2 Fe1 Cs1 121.63(10) 4_556 . ?
O2 Fe1 Cs1 58.37(10) 2_765 . ?
O2 Fe1 Cs1 58.37(10) 3_675 . ?
O2 Fe1 Cs1 121.63(10) . 4_556 ?
O2 Fe1 Cs1 58.37(10) 6_766 4_556 ?
O2 Fe1 Cs1 58.37(10) 5_676 4_556 ?
O2 Fe1 Cs1 58.37(10) 4_556 4_556 ?
O2 Fe1 Cs1 121.63(10) 2_765 4_556 ?
O2 Fe1 Cs1 121.63(10) 3_675 4_556 ?
Cs1 Fe1 Cs1 180.0 . 4_556 ?
C1 O2 Fe1 114.1(2) . . ?
C1 O2 Li1 87.8(3) . 27_556 ?
Fe1 O2 Li1 156.5(2) . 27_556 ?
C1 O2 Cs1 137.7(2) . . ?
Fe1 O2 Cs1 87.47(11) . . ?
Li1 O2 Cs1 81.01(11) 27_556 . ?
C1 O1 Li1 109.7(2) . . ?
C1 O1 Li1 86.01(16) . 27_556 ?
Li1 O1 Li1 163.5(3) . 27_556 ?
C1 O1 Cs1 147.34(19) . 16_445 ?
Li1 O1 Cs1 86.01(16) . 16_445 ?
Li1 O1 Cs1 82.87(9) 27_556 16_445 ?
O1 C1 O2 125.5(3) . . ?
O1 C1 C1 117.98(16) . 4_556 ?
O2 C1 C1 116.51(19) . 4_556 ?
O1 C1 Li1 64.03(17) . 27_556 ?
O2 C1 Li1 61.5(2) . 27_556 ?
C1 C1 Li1 177.5(2) 4_556 27_556 ?
O1 C1 Li1 44.84(14) . . ?
O2 C1 Li1 169.1(2) . . ?
C1 C1 Li1 73.39(8) 4_556 . ?
Li1 C1 Li1 108.71(18) 27_556 . ?
O1 Li1 O1 84.0(3) 4_556 . ?
O1 Li1 O2 102.27(17) 4_556 26_456 ?
O1 Li1 O2 101.49(17) . 26_456 ?
O1 Li1 O2 101.49(17) 4_556 35_545 ?
O1 Li1 O2 102.27(17) . 35_545 ?
O2 Li1 O2 147.8(5) 26_456 35_545 ?
O1 Li1 O1 162.50(11) 4_556 26_456 ?
O1 Li1 O1 95.30(7) . 26_456 ?
O2 Li1 O1 60.63(17) 26_456 26_456 ?
O2 Li1 O1 95.8(3) 35_545 26_456 ?
O1 Li1 O1 95.31(7) 4_556 35_545 ?
O1 Li1 O1 162.50(11) . 35_545 ?
O2 Li1 O1 95.8(3) 26_456 35_545 ?
O2 Li1 O1 60.63(17) 35_545 35_545 ?
O1 Li1 O1 90.5(3) 26_456 35_545 ?
O1 Li1 C1 132.80(12) 4_556 26_456 ?
O1 Li1 C1 99.22(9) . 26_456 ?
O2 Li1 C1 30.68(12) 26_456 26_456 ?
O2 Li1 C1 123.2(3) 35_545 26_456 ?
O1 Li1 C1 29.96(10) 26_456 26_456 ?
O1 Li1 C1 94.1(3) 35_545 26_456 ?
O1 Li1 C1 99.22(9) 4_556 35_545 ?
O1 Li1 C1 132.80(12) . 35_545 ?
O2 Li1 C1 123.2(3) 26_456 35_545 ?
O2 Li1 C1 30.68(12) 35_545 35_545 ?
O1 Li1 C1 94.1(3) 26_456 35_545 ?
O1 Li1 C1 29.96(10) 35_545 35_545 ?
C1 Li1 C1 111.2(4) 26_456 35_545 ?
O1 Li1 C1 25.47(13) 4_556 4_556 ?
O1 Li1 C1 58.6(2) . 4_556 ?
O2 Li1 C1 106.7(2) 26_456 4_556 ?
O2 Li1 C1 104.1(2) 35_545 4_556 ?
O1 Li1 C1 149.8(2) 26_456 4_556 ?
O1 Li1 C1 119.03(13) 35_545 4_556 ?
C1 Li1 C1 131.8(2) 26_456 4_556 ?
C1 Li1 C1 114.61(13) 35_545 4_556 ?
O1 Li1 C1 58.6(2) 4_556 . ?
O1 Li1 C1 25.47(13) . . ?
O2 Li1 C1 104.1(2) 26_456 . ?
O2 Li1 C1 106.7(2) 35_545 . ?
O1 Li1 C1 119.03(13) 26_456 . ?
O1 Li1 C1 149.8(2) 35_545 . ?
C1 Li1 C1 114.61(13) 26_456 . ?
C1 Li1 C1 131.8(2) 35_545 . ?
C1 Li1 C1 33.21(16) 4_556 . ?
O1 Li1 Cs1 132.6(3) 4_556 16_445 ?
O1 Li1 Cs1 59.78(6) . 16_445 ?
O2 Li1 Cs1 113.52(15) 26_456 16_445 ?
O2 Li1 Cs1 62.38(10) 35_545 16_445 ?
O1 Li1 Cs1 59.26(6) 26_456 16_445 ?
O1 Li1 Cs1 110.3(2) 35_545 16_445 ?
C1 Li1 Cs1 85.76(11) 26_456 16_445 ?
C1 Li1 Cs1 86.70(11) 35_545 16_445 ?
C1 Li1 Cs1 110.71(19) 4_556 16_445 ?
C1 Li1 Cs1 82.49(10) . 16_445 ?
O1 Li1 Cs1 59.78(6) 4_556 7_445 ?
O1 Li1 Cs1 132.6(3) . 7_445 ?
O2 Li1 Cs1 62.38(10) 26_456 7_445 ?
O2 Li1 Cs1 113.52(15) 35_545 7_445 ?
O1 Li1 Cs1 110.3(2) 26_456 7_445 ?
O1 Li1 Cs1 59.26(7) 35_545 7_445 ?
C1 Li1 Cs1 86.70(11) 26_456 7_445 ?
C1 Li1 Cs1 85.76(11) 35_545 7_445 ?
C1 Li1 Cs1 82.49(10) 4_556 7_445 ?
C1 Li1 Cs1 110.71(19) . 7_445 ?
Cs1 Li1 Cs1 166.6(3) 16_445 7_445 ?

_refine_diff_density_max         1.878
_refine_diff_density_min         -2.836
_refine_diff_density_rms         0.522

####################################################################### 
# 
# 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_shelx4
_database_code_depnum_ccdc_archive 'CCDC 1944091'
loop_
_audit_author_name
_audit_author_address
'Philip Lightfoot'
;University of St Andrews
United Kingdom
;
_audit_update_record             
;
2019-09-05 deposited with the CCDC.	2019-09-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C6 Fe Li3 O12 Rb'
_chemical_formula_weight         426.20

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c :H'
_space_group_name_Hall           '-R 3 2"c'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   11.4780(8)
_cell_length_b                   11.4780(8)
_cell_length_c                   15.1001(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1722.8(3)
_cell_formula_units_Z            6
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    867
_cell_measurement_theta_min      2.5
_cell_measurement_theta_max      27.5

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.465
_exptl_crystal_F_000             1224
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_exptl_absorpt_coefficient_mu    5.592
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.818
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
'The program SADABS-2008/1 - G.M. Sheldrick was used to apply a multi-scan absorption correction.'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Rigaku Mercury2 (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 13.6612
_diffrn_reflns_number            5535
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.389
_diffrn_reflns_theta_max         27.493
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             446
_reflns_number_gt                334
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Crystalmaker (Palmer, 2014)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         446
_refine_ls_number_parameters     37
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0251
_refine_ls_wR_factor_ref         0.1084
_refine_ls_wR_factor_gt          0.0886
_refine_ls_goodness_of_fit_ref   0.815
_refine_ls_restrained_S_all      0.815
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Rb1 Rb 0.6667 0.3333 0.3333 0.0185(3) Uani 1 6 d S T P . .
Fe1 Fe 0.3333 0.6667 0.4167 0.0119(3) Uani 1 6 d S T P . .
O1 O 0.6233(2) 0.5744(2) 0.34997(14) 0.0194(5) Uani 1 1 d . . . . .
O2 O 0.4404(2) 0.5939(2) 0.34142(14) 0.0180(5) Uani 1 1 d . . . . .
C1 C 0.5519(3) 0.6194(3) 0.37615(19) 0.0165(6) Uani 1 1 d . . . . .
Li1 Li 0.7999(7) 0.6667 0.4167 0.0215(15) Uani 1 2 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rb1 O1 3.057(2) 33_545 ?
Rb1 O1 3.057(2) 3_665 ?
Rb1 O1 3.057(2) 32 ?
Rb1 O1 3.057(2) 2_655 ?
Rb1 O1 3.057(2) . ?
Rb1 O1 3.057(2) 31_655 ?
Rb1 O2 3.193(2) 35_545 ?
Rb1 O2 3.193(2) 36 ?
Rb1 O2 3.193(2) 5_665 ?
Rb1 O2 3.193(2) 6_655 ?
Rb1 O2 3.193(2) 34_655 ?
Rb1 O2 3.193(2) 4 ?
Fe1 O2 2.127(2) 11_565 ?
Fe1 O2 2.127(2) 2_665 ?
Fe1 O2 2.127(2) 3_565 ?
Fe1 O2 2.127(2) . ?
Fe1 O2 2.127(2) 12 ?
Fe1 O2 2.127(2) 10_455 ?
Fe1 Rb1 3.7751(3) 4 ?
Fe1 Rb1 3.7751(3) 7_455 ?
O1 C1 1.232(4) . ?
O1 Li1 2.024(6) . ?
O1 Li1 2.196(6) 33_545 ?
O2 C1 1.275(4) . ?
O2 Li1 2.138(3) 33_545 ?
O2 Rb1 3.193(2) 4 ?
C1 C1 1.543(6) 11_565 ?
C1 Li1 2.439(5) 33_545 ?
C1 Li1 2.688(8) . ?
Li1 O1 2.024(6) 11_565 ?
Li1 O2 2.138(3) 32 ?
Li1 O2 2.138(3) 36 ?
Li1 O1 2.196(6) 36 ?
Li1 O1 2.196(6) 32 ?
Li1 C1 2.439(5) 36 ?
Li1 C1 2.439(5) 32 ?
Li1 C1 2.688(8) 11_565 ?
Li1 Rb1 3.5651(8) 10 ?

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_3
_geom_angle_publ_flag
O1 Rb1 O1 180.0 33_545 3_665 ?
O1 Rb1 O1 119.334(12) 33_545 32 ?
O1 Rb1 O1 60.667(12) 3_665 32 ?
O1 Rb1 O1 60.667(12) 33_545 2_655 ?
O1 Rb1 O1 119.332(12) 3_665 2_655 ?
O1 Rb1 O1 180.0 32 2_655 ?
O1 Rb1 O1 60.668(12) 33_545 . ?
O1 Rb1 O1 119.332(12) 3_665 . ?
O1 Rb1 O1 60.669(12) 32 . ?
O1 Rb1 O1 119.332(12) 2_655 . ?
O1 Rb1 O1 119.332(12) 33_545 31_655 ?
O1 Rb1 O1 60.667(12) 3_665 31_655 ?
O1 Rb1 O1 119.331(12) 32 31_655 ?
O1 Rb1 O1 60.668(12) 2_655 31_655 ?
O1 Rb1 O1 180.0 . 31_655 ?
O1 Rb1 O2 61.80(5) 33_545 35_545 ?
O1 Rb1 O2 118.21(5) 3_665 35_545 ?
O1 Rb1 O2 117.95(6) 32 35_545 ?
O1 Rb1 O2 62.05(6) 2_655 35_545 ?
O1 Rb1 O2 78.02(6) . 35_545 ?
O1 Rb1 O2 101.98(6) 31_655 35_545 ?
O1 Rb1 O2 101.99(6) 33_545 36 ?
O1 Rb1 O2 78.01(6) 3_665 36 ?
O1 Rb1 O2 61.79(5) 32 36 ?
O1 Rb1 O2 118.21(5) 2_655 36 ?
O1 Rb1 O2 62.05(6) . 36 ?
O1 Rb1 O2 117.95(6) 31_655 36 ?
O2 Rb1 O2 58.37(6) 35_545 36 ?
O1 Rb1 O2 118.21(5) 33_545 5_665 ?
O1 Rb1 O2 61.79(5) 3_665 5_665 ?
O1 Rb1 O2 62.05(6) 32 5_665 ?
O1 Rb1 O2 117.95(6) 2_655 5_665 ?
O1 Rb1 O2 101.98(6) . 5_665 ?
O1 Rb1 O2 78.01(6) 31_655 5_665 ?
O2 Rb1 O2 180.0 35_545 5_665 ?
O2 Rb1 O2 121.63(6) 36 5_665 ?
O1 Rb1 O2 78.01(6) 33_545 6_655 ?
O1 Rb1 O2 101.99(6) 3_665 6_655 ?
O1 Rb1 O2 118.21(5) 32 6_655 ?
O1 Rb1 O2 61.79(5) 2_655 6_655 ?
O1 Rb1 O2 117.95(6) . 6_655 ?
O1 Rb1 O2 62.05(6) 31_655 6_655 ?
O2 Rb1 O2 121.63(6) 35_545 6_655 ?
O2 Rb1 O2 180.0 36 6_655 ?
O2 Rb1 O2 58.37(6) 5_665 6_655 ?
O1 Rb1 O2 117.95(6) 33_545 34_655 ?
O1 Rb1 O2 62.05(6) 3_665 34_655 ?
O1 Rb1 O2 101.99(6) 32 34_655 ?
O1 Rb1 O2 78.01(6) 2_655 34_655 ?
O1 Rb1 O2 118.21(5) . 34_655 ?
O1 Rb1 O2 61.79(5) 31_655 34_655 ?
O2 Rb1 O2 58.37(6) 35_545 34_655 ?
O2 Rb1 O2 58.37(6) 36 34_655 ?
O2 Rb1 O2 121.63(6) 5_665 34_655 ?
O2 Rb1 O2 121.63(6) 6_655 34_655 ?
O1 Rb1 O2 62.05(6) 33_545 4 ?
O1 Rb1 O2 117.95(6) 3_665 4 ?
O1 Rb1 O2 78.01(6) 32 4 ?
O1 Rb1 O2 101.99(6) 2_655 4 ?
O1 Rb1 O2 61.79(5) . 4 ?
O1 Rb1 O2 118.21(5) 31_655 4 ?
O2 Rb1 O2 121.63(6) 35_545 4 ?
O2 Rb1 O2 121.63(6) 36 4 ?
O2 Rb1 O2 58.37(6) 5_665 4 ?
O2 Rb1 O2 58.37(6) 6_655 4 ?
O2 Rb1 O2 180.0 34_655 4 ?
O2 Fe1 O2 94.10(11) 11_565 2_665 ?
O2 Fe1 O2 169.37(11) 11_565 3_565 ?
O2 Fe1 O2 94.12(8) 2_665 3_565 ?
O2 Fe1 O2 78.58(11) 11_565 . ?
O2 Fe1 O2 94.12(8) 2_665 . ?
O2 Fe1 O2 94.12(8) 3_565 . ?
O2 Fe1 O2 94.12(8) 11_565 12 ?
O2 Fe1 O2 169.37(11) 2_665 12 ?
O2 Fe1 O2 78.57(11) 3_565 12 ?
O2 Fe1 O2 94.11(11) . 12 ?
O2 Fe1 O2 94.12(8) 11_565 10_455 ?
O2 Fe1 O2 78.58(11) 2_665 10_455 ?
O2 Fe1 O2 94.10(11) 3_565 10_455 ?
O2 Fe1 O2 169.37(11) . 10_455 ?
O2 Fe1 O2 94.12(8) 12 10_455 ?
O2 Fe1 Rb1 122.30(6) 11_565 4 ?
O2 Fe1 Rb1 57.71(6) 2_665 4 ?
O2 Fe1 Rb1 57.71(6) 3_565 4 ?
O2 Fe1 Rb1 57.71(6) . 4 ?
O2 Fe1 Rb1 122.30(6) 12 4 ?
O2 Fe1 Rb1 122.29(6) 10_455 4 ?
O2 Fe1 Rb1 57.71(6) 11_565 7_455 ?
O2 Fe1 Rb1 122.29(6) 2_665 7_455 ?
O2 Fe1 Rb1 122.29(6) 3_565 7_455 ?
O2 Fe1 Rb1 122.29(6) . 7_455 ?
O2 Fe1 Rb1 57.71(6) 12 7_455 ?
O2 Fe1 Rb1 57.70(6) 10_455 7_455 ?
Rb1 Fe1 Rb1 180.0 4 7_455 ?
C1 O1 Li1 108.9(2) . . ?
C1 O1 Li1 85.84(17) . 33_545 ?
Li1 O1 Li1 163.9(2) . 33_545 ?
C1 O1 Rb1 148.10(18) . . ?
Li1 O1 Rb1 86.61(14) . . ?
Li1 O1 Rb1 83.77(9) 33_545 . ?
C1 O2 Fe1 113.67(19) . . ?
C1 O2 Li1 87.4(2) . 33_545 ?
Fe1 O2 Li1 156.8(2) . 33_545 ?
C1 O2 Rb1 138.92(17) . 4 ?
Fe1 O2 Rb1 88.03(7) . 4 ?
Li1 O2 Rb1 81.33(6) 33_545 4 ?
O1 C1 O2 125.1(3) . . ?
O1 C1 C1 118.39(16) . 11_565 ?
O2 C1 C1 116.55(17) . 11_565 ?
O1 C1 Li1 63.91(17) . 33_545 ?
O2 C1 Li1 61.16(17) . 33_545 ?
C1 C1 Li1 177.38(18) 11_565 33_545 ?
O1 C1 Li1 45.44(14) . . ?
O2 C1 Li1 168.7(2) . . ?
C1 C1 Li1 73.32(8) 11_565 . ?
Li1 C1 Li1 109.10(17) 33_545 . ?
O1 Li1 O1 84.6(3) . 11_565 ?
O1 Li1 O2 101.72(14) . 32 ?
O1 Li1 O2 101.47(14) 11_565 32 ?
O1 Li1 O2 101.47(14) . 36 ?
O1 Li1 O2 101.72(14) 11_565 36 ?
O2 Li1 O2 148.5(4) 32 36 ?
O1 Li1 O1 162.56(12) . 36 ?
O1 Li1 O1 93.98(7) 11_565 36 ?
O2 Li1 O1 95.6(2) 32 36 ?
O2 Li1 O1 61.72(14) 36 36 ?
O1 Li1 O1 93.98(7) . 32 ?
O1 Li1 O1 162.55(12) 11_565 32 ?
O2 Li1 O1 61.72(14) 32 32 ?
O2 Li1 O1 95.6(2) 36 32 ?
O1 Li1 O1 92.5(3) 36 32 ?
O1 Li1 C1 132.75(12) . 36 ?
O1 Li1 C1 98.65(9) 11_565 36 ?
O2 Li1 C1 123.2(3) 32 36 ?
O2 Li1 C1 31.48(11) 36 36 ?
O1 Li1 C1 30.25(11) 36 36 ?
O1 Li1 C1 95.1(3) 32 36 ?
O1 Li1 C1 98.65(9) . 32 ?
O1 Li1 C1 132.75(12) 11_565 32 ?
O2 Li1 C1 31.48(11) 32 32 ?
O2 Li1 C1 123.2(3) 36 32 ?
O1 Li1 C1 95.1(3) 36 32 ?
O1 Li1 C1 30.25(11) 32 32 ?
C1 Li1 C1 111.8(3) 36 32 ?
O1 Li1 C1 25.70(13) . . ?
O1 Li1 C1 58.9(2) 11_565 . ?
O2 Li1 C1 103.78(19) 32 . ?
O2 Li1 C1 106.4(2) 36 . ?
O1 Li1 C1 149.1(2) 36 . ?
O1 Li1 C1 117.87(12) 32 . ?
C1 Li1 C1 131.8(2) 36 . ?
C1 Li1 C1 114.03(12) 32 . ?
O1 Li1 C1 58.9(2) . 11_565 ?
O1 Li1 C1 25.70(13) 11_565 11_565 ?
O2 Li1 C1 106.4(2) 32 11_565 ?
O2 Li1 C1 103.79(19) 36 11_565 ?
O1 Li1 C1 117.87(12) 36 11_565 ?
O1 Li1 C1 149.1(2) 32 11_565 ?
C1 Li1 C1 114.03(12) 36 11_565 ?
C1 Li1 C1 131.8(2) 32 11_565 ?
C1 Li1 C1 33.37(16) . 11_565 ?
O1 Li1 Rb1 132.6(2) . 10 ?
O1 Li1 Rb1 58.87(6) 11_565 10 ?
O2 Li1 Rb1 62.30(6) 32 10 ?
O2 Li1 Rb1 113.97(11) 36 10 ?
O1 Li1 Rb1 58.48(6) 36 10 ?
O1 Li1 Rb1 111.95(18) 32 10 ?
C1 Li1 Rb1 85.38(11) 36 10 ?
C1 Li1 Rb1 87.69(11) 32 10 ?
C1 Li1 Rb1 110.25(17) . 10 ?
C1 Li1 Rb1 81.97(10) 11_565 10 ?
O1 Li1 Rb1 58.87(6) . . ?
O1 Li1 Rb1 132.6(2) 11_565 . ?
O2 Li1 Rb1 113.97(11) 32 . ?
O2 Li1 Rb1 62.30(6) 36 . ?
O1 Li1 Rb1 111.95(18) 36 . ?
O1 Li1 Rb1 58.48(6) 32 . ?
C1 Li1 Rb1 87.69(11) 36 . ?
C1 Li1 Rb1 85.38(11) 32 . ?
C1 Li1 Rb1 81.97(10) . . ?
C1 Li1 Rb1 110.25(17) 11_565 . ?
Rb1 Li1 Rb1 167.6(2) 10 . ?

_refine_diff_density_max         0.363
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.085

####################################################################### 
# 
# 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_shelx2
_database_code_depnum_ccdc_archive 'CCDC 1944089'
loop_
_audit_author_name
_audit_author_address
'Philip Lightfoot'
;University of St Andrews
United Kingdom
;
_audit_update_record             
;
2019-09-05 deposited with the CCDC.	2019-09-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 Co O12, Rb, 3(Li)'
_chemical_formula_sum            'C6 Co Li3 O12 Rb'
_chemical_formula_weight         429.28

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c :H'
_space_group_name_Hall           '-R 3 2"c'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   11.4019(8)
_cell_length_b                   11.4019(8)
_cell_length_c                   15.1029(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1700.4(3)
_cell_formula_units_Z            6
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    796
_cell_measurement_theta_min      2.5
_cell_measurement_theta_max      27.5

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.515
_exptl_crystal_F_000             1230
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.09
_exptl_absorpt_coefficient_mu    5.849
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.562
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
'The program SADABS-2008/1 - G.M. Sheldrick was used to apply a multi-scan absorption correction.'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Sealed Tube'
_diffrn_measurement_device_type  'Rigaku Mercury2 (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 13.6612
_diffrn_reflns_number            5449
_diffrn_reflns_av_unetI/netI     0.0397
_diffrn_reflns_av_R_equivalents  0.0803
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.396
_diffrn_reflns_theta_max         27.509
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             444
_reflns_number_gt                285
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Crystalmaker (Palmer, 2014)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         444
_refine_ls_number_parameters     37
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0274
_refine_ls_wR_factor_ref         0.0931
_refine_ls_wR_factor_gt          0.0736
_refine_ls_goodness_of_fit_ref   0.610
_refine_ls_restrained_S_all      0.610
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Rb1 Rb 0.6667 0.3333 0.3333 0.0167(3) Uani 1 6 d S T P . .
Co1 Co 1.0000 1.0000 0.2500 0.0105(3) Uani 1 6 d S T P . .
O1 O 0.7128(2) 0.6198(2) 0.31693(17) 0.0178(6) Uani 1 1 d . . . . .
O2 O 0.8972(2) 0.8235(2) 0.32551(16) 0.0155(5) Uani 1 1 d . . . . .
C1 C 0.7853(3) 0.7377(3) 0.2906(2) 0.0145(7) Uani 1 1 d . . . . .
Li1 Li 0.5347(8) 0.5347(8) 0.2500 0.0217(18) Uani 1 2 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rb1 O1 3.048(2) 33_545 ?
Rb1 O1 3.048(2) 3_665 ?
Rb1 O1 3.048(2) 2_655 ?
Rb1 O1 3.048(2) 32 ?
Rb1 O1 3.048(2) . ?
Rb1 O1 3.048(2) 31_655 ?
Rb1 O2 3.164(2) 29_545 ?
Rb1 O2 3.164(2) 28_665 ?
Rb1 O2 3.164(2) 30_455 ?
Rb1 O2 3.164(2) 12_655 ?
Rb1 O2 3.164(2) 10_445 ?
Rb1 O2 3.164(2) 11_565 ?
Co1 O2 2.089(2) 2_765 ?
Co1 O2 2.089(2) 5_675 ?
Co1 O2 2.089(2) 4 ?
Co1 O2 2.089(2) . ?
Co1 O2 2.089(2) 3_675 ?
Co1 O2 2.089(2) 6_765 ?
Co1 Rb1 3.7757(3) 10 ?
Co1 Rb1 3.7757(3) 13_554 ?
O1 C1 1.240(4) . ?
O1 Li1 2.029(7) . ?
O1 Li1 2.178(6) 32 ?
O2 C1 1.271(4) . ?
O2 Li1 2.147(3) 32 ?
O2 Rb1 3.164(2) 10 ?
C1 C1 1.545(6) 4 ?
C1 Li1 2.436(6) 32 ?
C1 Li1 2.699(9) . ?
Li1 O1 2.029(7) 4 ?
Li1 O2 2.147(3) 30_455 ?
Li1 O2 2.147(3) 33_545 ?
Li1 O1 2.178(6) 30_455 ?
Li1 O1 2.178(6) 33_545 ?
Li1 C1 2.436(6) 30_455 ?
Li1 C1 2.436(6) 33_545 ?
Li1 C1 2.699(9) 4 ?
Li1 Rb1 3.5460(10) 4 ?

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_3
_geom_angle_publ_flag
O1 Rb1 O1 180.00(8) 33_545 3_665 ?
O1 Rb1 O1 60.653(13) 33_545 2_655 ?
O1 Rb1 O1 119.347(13) 3_665 2_655 ?
O1 Rb1 O1 119.348(13) 33_545 32 ?
O1 Rb1 O1 60.652(13) 3_665 32 ?
O1 Rb1 O1 180.0 2_655 32 ?
O1 Rb1 O1 60.653(13) 33_545 . ?
O1 Rb1 O1 119.347(14) 3_665 . ?
O1 Rb1 O1 119.347(13) 2_655 . ?
O1 Rb1 O1 60.654(13) 32 . ?
O1 Rb1 O1 119.347(14) 33_545 31_655 ?
O1 Rb1 O1 60.653(13) 3_665 31_655 ?
O1 Rb1 O1 60.654(13) 2_655 31_655 ?
O1 Rb1 O1 119.345(13) 32 31_655 ?
O1 Rb1 O1 180.0 . 31_655 ?
O1 Rb1 O2 101.63(6) 33_545 29_545 ?
O1 Rb1 O2 78.37(6) 3_665 29_545 ?
O1 Rb1 O2 62.35(6) 2_655 29_545 ?
O1 Rb1 O2 117.65(6) 32 29_545 ?
O1 Rb1 O2 117.55(6) . 29_545 ?
O1 Rb1 O2 62.45(6) 31_655 29_545 ?
O1 Rb1 O2 117.65(6) 33_545 28_665 ?
O1 Rb1 O2 62.35(6) 3_665 28_665 ?
O1 Rb1 O2 117.55(6) 2_655 28_665 ?
O1 Rb1 O2 62.45(6) 32 28_665 ?
O1 Rb1 O2 78.37(6) . 28_665 ?
O1 Rb1 O2 101.63(6) 31_655 28_665 ?
O2 Rb1 O2 57.27(7) 29_545 28_665 ?
O1 Rb1 O2 62.45(6) 33_545 30_455 ?
O1 Rb1 O2 117.55(6) 3_665 30_455 ?
O1 Rb1 O2 78.37(6) 2_655 30_455 ?
O1 Rb1 O2 101.63(6) 32 30_455 ?
O1 Rb1 O2 62.35(6) . 30_455 ?
O1 Rb1 O2 117.65(6) 31_655 30_455 ?
O2 Rb1 O2 57.26(7) 29_545 30_455 ?
O2 Rb1 O2 57.26(7) 28_665 30_455 ?
O1 Rb1 O2 117.55(6) 33_545 12_655 ?
O1 Rb1 O2 62.45(6) 3_665 12_655 ?
O1 Rb1 O2 101.63(6) 2_655 12_655 ?
O1 Rb1 O2 78.37(6) 32 12_655 ?
O1 Rb1 O2 117.65(6) . 12_655 ?
O1 Rb1 O2 62.35(6) 31_655 12_655 ?
O2 Rb1 O2 122.74(7) 29_545 12_655 ?
O2 Rb1 O2 122.74(7) 28_665 12_655 ?
O2 Rb1 O2 180.0 30_455 12_655 ?
O1 Rb1 O2 62.35(6) 33_545 10_445 ?
O1 Rb1 O2 117.65(6) 3_665 10_445 ?
O1 Rb1 O2 62.45(6) 2_655 10_445 ?
O1 Rb1 O2 117.55(6) 32 10_445 ?
O1 Rb1 O2 101.63(6) . 10_445 ?
O1 Rb1 O2 78.37(6) 31_655 10_445 ?
O2 Rb1 O2 122.74(7) 29_545 10_445 ?
O2 Rb1 O2 180.0 28_665 10_445 ?
O2 Rb1 O2 122.73(7) 30_455 10_445 ?
O2 Rb1 O2 57.26(7) 12_655 10_445 ?
O1 Rb1 O2 78.37(6) 33_545 11_565 ?
O1 Rb1 O2 101.63(6) 3_665 11_565 ?
O1 Rb1 O2 117.65(6) 2_655 11_565 ?
O1 Rb1 O2 62.35(6) 32 11_565 ?
O1 Rb1 O2 62.45(6) . 11_565 ?
O1 Rb1 O2 117.55(6) 31_655 11_565 ?
O2 Rb1 O2 180.0 29_545 11_565 ?
O2 Rb1 O2 122.74(7) 28_665 11_565 ?
O2 Rb1 O2 122.73(7) 30_455 11_565 ?
O2 Rb1 O2 57.26(7) 12_655 11_565 ?
O2 Rb1 O2 57.26(7) 10_445 11_565 ?
O2 Co1 O2 93.88(12) 2_765 5_675 ?
O2 Co1 O2 170.91(11) 2_765 4 ?
O2 Co1 O2 93.05(9) 5_675 4 ?
O2 Co1 O2 93.04(9) 2_765 . ?
O2 Co1 O2 170.91(11) 5_675 . ?
O2 Co1 O2 80.72(12) 4 . ?
O2 Co1 O2 93.04(9) 2_765 3_675 ?
O2 Co1 O2 80.72(12) 5_675 3_675 ?
O2 Co1 O2 93.88(12) 4 3_675 ?
O2 Co1 O2 93.05(9) . 3_675 ?
O2 Co1 O2 80.72(12) 2_765 6_765 ?
O2 Co1 O2 93.04(9) 5_675 6_765 ?
O2 Co1 O2 93.04(9) 4 6_765 ?
O2 Co1 O2 93.88(12) . 6_765 ?
O2 Co1 O2 170.91(11) 3_675 6_765 ?
O2 Co1 Rb1 56.92(7) 2_765 10 ?
O2 Co1 Rb1 123.08(6) 5_675 10 ?
O2 Co1 Rb1 123.08(6) 4 10 ?
O2 Co1 Rb1 56.92(6) . 10 ?
O2 Co1 Rb1 56.92(6) 3_675 10 ?
O2 Co1 Rb1 123.08(6) 6_765 10 ?
O2 Co1 Rb1 123.08(7) 2_765 13_554 ?
O2 Co1 Rb1 56.92(6) 5_675 13_554 ?
O2 Co1 Rb1 56.92(6) 4 13_554 ?
O2 Co1 Rb1 123.08(7) . 13_554 ?
O2 Co1 Rb1 123.08(6) 3_675 13_554 ?
O2 Co1 Rb1 56.92(6) 6_765 13_554 ?
Rb1 Co1 Rb1 180.0 10 13_554 ?
C1 O1 Li1 108.9(3) . . ?
C1 O1 Li1 86.36(18) . 32 ?
Li1 O1 Li1 163.4(3) . 32 ?
C1 O1 Rb1 148.5(2) . . ?
Li1 O1 Rb1 86.14(16) . . ?
Li1 O1 Rb1 83.69(10) 32 . ?
C1 O2 Co1 112.3(2) . . ?
C1 O2 Li1 87.0(2) . 32 ?
Co1 O2 Li1 158.6(2) . 32 ?
C1 O2 Rb1 138.17(19) . 10 ?
Co1 O2 Rb1 89.49(8) . 10 ?
Li1 O2 Rb1 81.35(7) 32 10 ?
O1 C1 O2 124.7(3) . . ?
O1 C1 C1 118.33(18) . 4 ?
O2 C1 C1 116.92(19) . 4 ?
O1 C1 Li1 63.12(19) . 32 ?
O2 C1 Li1 61.64(18) . 32 ?
C1 C1 Li1 178.1(3) 4 32 ?
O1 C1 Li1 45.34(16) . . ?
O2 C1 Li1 168.4(3) . . ?
C1 C1 Li1 73.37(9) 4 . ?
Li1 C1 Li1 108.2(2) 32 . ?
O1 Li1 O1 84.6(4) 4 . ?
O1 Li1 O2 101.55(17) 4 30_455 ?
O1 Li1 O2 100.75(16) . 30_455 ?
O1 Li1 O2 100.75(16) 4 33_545 ?
O1 Li1 O2 101.55(17) . 33_545 ?
O2 Li1 O2 149.7(5) 30_455 33_545 ?
O1 Li1 O1 94.00(8) 4 30_455 ?
O1 Li1 O1 162.04(13) . 30_455 ?
O2 Li1 O1 61.91(17) 30_455 30_455 ?
O2 Li1 O1 96.3(3) 33_545 30_455 ?
O1 Li1 O1 162.04(13) 4 33_545 ?
O1 Li1 O1 94.00(8) . 33_545 ?
O2 Li1 O1 96.3(3) 30_455 33_545 ?
O2 Li1 O1 61.91(17) 33_545 33_545 ?
O1 Li1 O1 92.7(4) 30_455 33_545 ?
O1 Li1 C1 98.64(10) 4 30_455 ?
O1 Li1 C1 131.95(14) . 30_455 ?
O2 Li1 C1 31.40(12) 30_455 30_455 ?
O2 Li1 C1 124.3(4) 33_545 30_455 ?
O1 Li1 C1 30.52(13) 30_455 30_455 ?
O1 Li1 C1 95.6(3) 33_545 30_455 ?
O1 Li1 C1 131.95(14) 4 33_545 ?
O1 Li1 C1 98.64(10) . 33_545 ?
O2 Li1 C1 124.3(4) 30_455 33_545 ?
O2 Li1 C1 31.40(12) 33_545 33_545 ?
O1 Li1 C1 95.6(3) 30_455 33_545 ?
O1 Li1 C1 30.52(13) 33_545 33_545 ?
C1 Li1 C1 112.8(4) 30_455 33_545 ?
O1 Li1 C1 25.76(15) 4 4 ?
O1 Li1 C1 58.9(2) . 4 ?
O2 Li1 C1 103.3(2) 30_455 4 ?
O2 Li1 C1 105.7(2) 33_545 4 ?
O1 Li1 C1 117.85(14) 30_455 4 ?
O1 Li1 C1 148.8(2) 33_545 4 ?
C1 Li1 C1 113.76(14) 30_455 4 ?
C1 Li1 C1 131.1(2) 33_545 4 ?
O1 Li1 C1 58.9(2) 4 . ?
O1 Li1 C1 25.76(15) . . ?
O2 Li1 C1 105.7(2) 30_455 . ?
O2 Li1 C1 103.3(2) 33_545 . ?
O1 Li1 C1 148.8(2) 30_455 . ?
O1 Li1 C1 117.85(14) 33_545 . ?
C1 Li1 C1 131.1(2) 30_455 . ?
C1 Li1 C1 113.76(14) 33_545 . ?
C1 Li1 C1 33.27(18) 4 . ?
O1 Li1 Rb1 59.05(7) 4 4 ?
O1 Li1 Rb1 132.8(3) . 4 ?
O2 Li1 Rb1 114.38(13) 30_455 4 ?
O2 Li1 Rb1 61.89(7) 33_545 4 ?
O1 Li1 Rb1 58.68(7) 30_455 4 ?
O1 Li1 Rb1 111.4(2) 33_545 4 ?
C1 Li1 Rb1 85.87(12) 30_455 4 ?
C1 Li1 Rb1 87.04(13) 33_545 4 ?
C1 Li1 Rb1 82.22(11) 4 4 ?
C1 Li1 Rb1 110.4(2) . 4 ?
O1 Li1 Rb1 132.8(3) 4 . ?
O1 Li1 Rb1 59.05(7) . . ?
O2 Li1 Rb1 61.89(7) 30_455 . ?
O2 Li1 Rb1 114.38(13) 33_545 . ?
O1 Li1 Rb1 111.4(2) 30_455 . ?
O1 Li1 Rb1 58.68(7) 33_545 . ?
C1 Li1 Rb1 87.04(13) 30_455 . ?
C1 Li1 Rb1 85.87(12) 33_545 . ?
C1 Li1 Rb1 110.4(2) 4 . ?
C1 Li1 Rb1 82.22(11) . . ?
Rb1 Li1 Rb1 167.2(3) 4 . ?

_refine_diff_density_max         0.458
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.112

####################################################################### 
# 
# 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_shelx6
_database_code_depnum_ccdc_archive 'CCDC 1944093'
loop_
_audit_author_name
_audit_author_address
'Philip Lightfoot'
;University of St Andrews
United Kingdom
;
_audit_update_record             
;
2019-09-05 deposited with the CCDC.	2019-09-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 Ni O12, K, 3(Li)'
_chemical_formula_sum            'C6 K Li3 Ni O12'
_chemical_formula_weight         382.69

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c :H'
_space_group_name_Hall           '-R 3 2"c'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   11.3071(8)
_cell_length_b                   11.3071(8)
_cell_length_c                   14.9434(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1654.6(3)
_cell_formula_units_Z            6
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    927
_cell_measurement_theta_min      2.5
_cell_measurement_theta_max      27.5

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.304
_exptl_crystal_F_000             1128
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    2.207
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.769
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
'The program SADABS-2008/1 - G.M. Sheldrick was used to apply a multi-scan absorption correction.'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Sealed Tube'
_diffrn_measurement_device_type  'Rigaku Mercury2 (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 13.6612
_diffrn_reflns_number            5246
_diffrn_reflns_av_unetI/netI     0.0176
_diffrn_reflns_av_R_equivalents  0.0432
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.430
_diffrn_reflns_theta_max         27.504
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.985
_reflns_number_total             426
_reflns_number_gt                380
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Crystalmaker (Palmer, 2014)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         426
_refine_ls_number_parameters     37
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0246
_refine_ls_R_factor_gt           0.0216
_refine_ls_wR_factor_ref         0.0791
_refine_ls_wR_factor_gt          0.0748
_refine_ls_goodness_of_fit_ref   0.711
_refine_ls_restrained_S_all      0.711
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.3333 0.6667 0.4167 0.0106(2) Uani 1 6 d S T P . .
K1 K 1.0000 1.0000 0.5000 0.0237(3) Uani 1 6 d S T P . .
O2 O 0.50800(11) 0.74299(10) 0.49212(7) 0.0143(3) Uani 1 1 d . . . . .
O1 O 0.71298(9) 0.76186(10) 0.48313(6) 0.0159(3) Uani 1 1 d . . . . .
C1 C 0.59370(13) 0.71565(12) 0.45701(8) 0.0132(3) Uani 1 1 d . . . . .
Li1 Li 0.7973(3) 0.6667 0.4167 0.0162(6) Uani 1 2 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O2 2.0523(10) 12 ?
Ni1 O2 2.0523(10) . ?
Ni1 O2 2.0523(10) 10_455 ?
Ni1 O2 2.0523(10) 3_565 ?
Ni1 O2 2.0523(10) 11_565 ?
Ni1 O2 2.0524(10) 2_665 ?
Ni1 K1 3.7358(3) 16_445 ?
Ni1 K1 3.7359(3) 13_444 ?
K1 O1 3.0179(9) 20_566 ?
K1 O1 3.0179(9) 2_765 ?
K1 O1 3.0179(9) . ?
K1 O1 3.0179(9) 19_776 ?
K1 O1 3.0180(9) 21_656 ?
K1 O1 3.0180(9) 3_675 ?
K1 O2 3.1215(11) 16 ?
K1 O2 3.1215(11) 28_665 ?
K1 O2 3.1215(11) 30_565 ?
K1 O2 3.1215(11) 18_655 ?
K1 O2 3.1216(11) 17_665 ?
K1 O2 3.1216(11) 29 ?
O2 C1 1.2686(16) . ?
O2 Li1 2.1344(14) 20_566 ?
O2 K1 3.1216(11) 16_445 ?
O1 C1 1.2408(16) . ?
O1 Li1 2.020(3) . ?
O1 Li1 2.152(3) 20_566 ?
C1 C1 1.541(2) 11_565 ?
C1 Li1 2.415(2) 20_566 ?
C1 Li1 2.691(4) . ?
Li1 O1 2.020(3) 11_565 ?
Li1 O2 2.1343(14) 28_665 ?
Li1 O2 2.1344(14) 21_656 ?
Li1 O1 2.152(3) 28_665 ?
Li1 O1 2.152(3) 21_656 ?
Li1 C1 2.415(2) 28_665 ?
Li1 C1 2.415(2) 21_656 ?
Li1 C1 2.691(4) 11_565 ?
Li1 K1 3.5172(5) 10_445 ?

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_3
_geom_angle_publ_flag
O2 Ni1 O2 173.04(5) 12 . ?
O2 Ni1 O2 92.71(4) 12 10_455 ?
O2 Ni1 O2 92.52(6) . 10_455 ?
O2 Ni1 O2 82.46(5) 12 3_565 ?
O2 Ni1 O2 92.71(4) . 3_565 ?
O2 Ni1 O2 173.04(5) 10_455 3_565 ?
O2 Ni1 O2 92.71(4) 12 11_565 ?
O2 Ni1 O2 82.46(5) . 11_565 ?
O2 Ni1 O2 92.71(4) 10_455 11_565 ?
O2 Ni1 O2 92.52(6) 3_565 11_565 ?
O2 Ni1 O2 92.52(6) 12 2_665 ?
O2 Ni1 O2 92.71(4) . 2_665 ?
O2 Ni1 O2 82.46(5) 10_455 2_665 ?
O2 Ni1 O2 92.71(4) 3_565 2_665 ?
O2 Ni1 O2 173.04(5) 11_565 2_665 ?
O2 Ni1 K1 123.32(3) 12 16_445 ?
O2 Ni1 K1 56.68(3) . 16_445 ?
O2 Ni1 K1 123.32(3) 10_455 16_445 ?
O2 Ni1 K1 56.68(3) 3_565 16_445 ?
O2 Ni1 K1 123.32(3) 11_565 16_445 ?
O2 Ni1 K1 56.68(3) 2_665 16_445 ?
O2 Ni1 K1 56.68(3) 12 13_444 ?
O2 Ni1 K1 123.32(3) . 13_444 ?
O2 Ni1 K1 56.68(3) 10_455 13_444 ?
O2 Ni1 K1 123.32(3) 3_565 13_444 ?
O2 Ni1 K1 56.68(3) 11_565 13_444 ?
O2 Ni1 K1 123.32(3) 2_665 13_444 ?
K1 Ni1 K1 180.0 16_445 13_444 ?
O1 K1 O1 180.0 20_566 2_765 ?
O1 K1 O1 60.689(5) 20_566 . ?
O1 K1 O1 119.311(5) 2_765 . ?
O1 K1 O1 119.312(5) 20_566 19_776 ?
O1 K1 O1 60.688(5) 2_765 19_776 ?
O1 K1 O1 180.0 . 19_776 ?
O1 K1 O1 119.311(5) 20_566 21_656 ?
O1 K1 O1 60.689(5) 2_765 21_656 ?
O1 K1 O1 60.690(5) . 21_656 ?
O1 K1 O1 119.309(5) 19_776 21_656 ?
O1 K1 O1 60.689(5) 20_566 3_675 ?
O1 K1 O1 119.311(5) 2_765 3_675 ?
O1 K1 O1 119.310(5) . 3_675 ?
O1 K1 O1 60.691(5) 19_776 3_675 ?
O1 K1 O1 180.0 21_656 3_675 ?
O1 K1 O2 78.70(2) 20_566 16 ?
O1 K1 O2 101.30(2) 2_765 16 ?
O1 K1 O2 117.91(2) . 16 ?
O1 K1 O2 62.09(2) 19_776 16 ?
O1 K1 O2 117.04(3) 21_656 16 ?
O1 K1 O2 62.96(3) 3_675 16 ?
O1 K1 O2 101.30(2) 20_566 28_665 ?
O1 K1 O2 78.70(2) 2_765 28_665 ?
O1 K1 O2 62.09(2) . 28_665 ?
O1 K1 O2 117.91(2) 19_776 28_665 ?
O1 K1 O2 62.96(3) 21_656 28_665 ?
O1 K1 O2 117.04(3) 3_675 28_665 ?
O2 K1 O2 180.0 16 28_665 ?
O1 K1 O2 117.91(2) 20_566 30_565 ?
O1 K1 O2 62.09(2) 2_765 30_565 ?
O1 K1 O2 117.04(3) . 30_565 ?
O1 K1 O2 62.96(3) 19_776 30_565 ?
O1 K1 O2 101.30(2) 21_656 30_565 ?
O1 K1 O2 78.70(2) 3_675 30_565 ?
O2 K1 O2 123.18(3) 16 30_565 ?
O2 K1 O2 56.82(3) 28_665 30_565 ?
O1 K1 O2 62.09(2) 20_566 18_655 ?
O1 K1 O2 117.91(2) 2_765 18_655 ?
O1 K1 O2 62.96(3) . 18_655 ?
O1 K1 O2 117.04(3) 19_776 18_655 ?
O1 K1 O2 78.70(2) 21_656 18_655 ?
O1 K1 O2 101.30(2) 3_675 18_655 ?
O2 K1 O2 56.82(3) 16 18_655 ?
O2 K1 O2 123.18(3) 28_665 18_655 ?
O2 K1 O2 180.0 30_565 18_655 ?
O1 K1 O2 117.04(3) 20_566 17_665 ?
O1 K1 O2 62.96(3) 2_765 17_665 ?
O1 K1 O2 101.30(2) . 17_665 ?
O1 K1 O2 78.70(2) 19_776 17_665 ?
O1 K1 O2 62.09(2) 21_656 17_665 ?
O1 K1 O2 117.91(2) 3_675 17_665 ?
O2 K1 O2 56.82(3) 16 17_665 ?
O2 K1 O2 123.18(3) 28_665 17_665 ?
O2 K1 O2 123.18(3) 30_565 17_665 ?
O2 K1 O2 56.82(3) 18_655 17_665 ?
O1 K1 O2 62.96(3) 20_566 29 ?
O1 K1 O2 117.04(3) 2_765 29 ?
O1 K1 O2 78.70(2) . 29 ?
O1 K1 O2 101.30(2) 19_776 29 ?
O1 K1 O2 117.91(2) 21_656 29 ?
O1 K1 O2 62.09(2) 3_675 29 ?
O2 K1 O2 123.18(3) 16 29 ?
O2 K1 O2 56.82(3) 28_665 29 ?
O2 K1 O2 56.82(3) 30_565 29 ?
O2 K1 O2 123.18(3) 18_655 29 ?
O2 K1 O2 180.0 17_665 29 ?
C1 O2 Ni1 111.23(8) . . ?
C1 O2 Li1 86.48(10) . 20_566 ?
Ni1 O2 Li1 160.45(10) . 20_566 ?
C1 O2 K1 137.13(8) . 16_445 ?
Ni1 O2 K1 90.00(4) . 16_445 ?
Li1 O2 K1 81.68(3) 20_566 16_445 ?
C1 O1 Li1 108.90(11) . . ?
C1 O1 Li1 86.36(8) . 20_566 ?
Li1 O1 Li1 162.99(11) . 20_566 ?
C1 O1 K1 149.27(8) . . ?
Li1 O1 K1 86.16(6) . . ?
Li1 O1 K1 83.95(4) 20_566 . ?
O1 C1 O2 124.69(12) . . ?
O1 C1 C1 118.25(8) . 11_565 ?
O2 C1 C1 117.06(7) . 11_565 ?
O1 C1 Li1 62.79(8) . 20_566 ?
O2 C1 Li1 61.90(7) . 20_566 ?
C1 C1 Li1 178.94(5) 11_565 20_566 ?
O1 C1 Li1 45.23(7) . . ?
O2 C1 Li1 168.20(9) . . ?
C1 C1 Li1 73.37(3) 11_565 . ?
Li1 C1 Li1 107.68(8) 20_566 . ?
O1 Li1 O1 84.82(14) . 11_565 ?
O1 Li1 O2 99.33(7) . 28_665 ?
O1 Li1 O2 101.89(7) 11_565 28_665 ?
O1 Li1 O2 101.89(7) . 21_656 ?
O1 Li1 O2 99.34(7) 11_565 21_656 ?
O2 Li1 O2 151.1(2) 28_665 21_656 ?
O1 Li1 O1 161.16(5) . 28_665 ?
O1 Li1 O1 93.88(3) 11_565 28_665 ?
O2 Li1 O1 62.47(7) 28_665 28_665 ?
O2 Li1 O1 96.87(11) 21_656 28_665 ?
O1 Li1 O1 93.88(3) . 21_656 ?
O1 Li1 O1 161.16(5) 11_565 21_656 ?
O2 Li1 O1 96.87(11) 28_665 21_656 ?
O2 Li1 O1 62.47(7) 21_656 21_656 ?
O1 Li1 O1 93.26(15) 28_665 21_656 ?
O1 Li1 C1 130.79(5) . 28_665 ?
O1 Li1 C1 99.07(4) 11_565 28_665 ?
O2 Li1 C1 31.62(5) 28_665 28_665 ?
O2 Li1 C1 125.28(15) 21_656 28_665 ?
O1 Li1 C1 30.85(5) 28_665 28_665 ?
O1 Li1 C1 95.99(13) 21_656 28_665 ?
O1 Li1 C1 99.07(4) . 21_656 ?
O1 Li1 C1 130.79(5) 11_565 21_656 ?
O2 Li1 C1 125.28(15) 28_665 21_656 ?
O2 Li1 C1 31.62(5) 21_656 21_656 ?
O1 Li1 C1 95.99(13) 28_665 21_656 ?
O1 Li1 C1 30.85(5) 21_656 21_656 ?
C1 Li1 C1 113.39(15) 28_665 21_656 ?
O1 Li1 C1 25.86(6) . . ?
O1 Li1 C1 59.00(10) 11_565 . ?
O2 Li1 C1 104.61(10) 28_665 . ?
O2 Li1 C1 103.04(10) 21_656 . ?
O1 Li1 C1 148.36(9) 28_665 . ?
O1 Li1 C1 117.68(6) 21_656 . ?
C1 Li1 C1 130.43(9) 28_665 . ?
C1 Li1 C1 113.81(6) 21_656 . ?
O1 Li1 C1 59.00(10) . 11_565 ?
O1 Li1 C1 25.86(6) 11_565 11_565 ?
O2 Li1 C1 103.04(10) 28_665 11_565 ?
O2 Li1 C1 104.62(10) 21_656 11_565 ?
O1 Li1 C1 117.68(6) 28_665 11_565 ?
O1 Li1 C1 148.36(9) 21_656 11_565 ?
C1 Li1 C1 113.81(6) 28_665 11_565 ?
C1 Li1 C1 130.43(9) 21_656 11_565 ?
C1 Li1 C1 33.27(7) . 11_565 ?
O1 Li1 K1 133.47(11) . 10_445 ?
O1 Li1 K1 58.88(3) 11_565 10_445 ?
O2 Li1 K1 114.87(5) 28_665 10_445 ?
O2 Li1 K1 61.42(3) 21_656 10_445 ?
O1 Li1 K1 58.57(3) 28_665 10_445 ?
O1 Li1 K1 111.24(9) 21_656 10_445 ?
C1 Li1 K1 86.23(5) 28_665 10_445 ?
C1 Li1 K1 86.47(5) 21_656 10_445 ?
C1 Li1 K1 110.84(8) . 10_445 ?
C1 Li1 K1 82.32(5) 11_565 10_445 ?
O1 Li1 K1 58.88(3) . . ?
O1 Li1 K1 133.48(11) 11_565 . ?
O2 Li1 K1 61.42(3) 28_665 . ?
O2 Li1 K1 114.87(5) 21_656 . ?
O1 Li1 K1 111.24(9) 28_665 . ?
O1 Li1 K1 58.57(3) 21_656 . ?
C1 Li1 K1 86.47(5) 28_665 . ?
C1 Li1 K1 86.22(5) 21_656 . ?
C1 Li1 K1 82.32(5) . . ?
C1 Li1 K1 110.84(8) 11_565 . ?
K1 Li1 K1 166.68(12) 10_445 . ?

_refine_diff_density_max         0.500
_refine_diff_density_min         -0.643
_refine_diff_density_rms         0.084

####################################################################### 
# 
# 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_shelx7
_database_code_depnum_ccdc_archive 'CCDC 1944094'
loop_
_audit_author_name
_audit_author_address
'Philip Lightfoot'
;University of St Andrews
United Kingdom
;
_audit_update_record             
;
2019-09-05 deposited with the CCDC.	2019-09-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C6 Cs Li3 Ni O12'
_chemical_formula_weight         476.50

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c :H'
_space_group_name_Hall           '-R 3 2"c'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   11.4908(8)
_cell_length_b                   11.4908(8)
_cell_length_c                   15.1534(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1732.8(3)
_cell_formula_units_Z            6
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    820
_cell_measurement_theta_min      2.4
_cell_measurement_theta_max      27.5

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.740
_exptl_crystal_F_000             1344
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_exptl_absorpt_coefficient_mu    4.853
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.806
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
'The program SADABS-2008/1 - G.M. Sheldrick was used to apply a multi-scan absorption correction.'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Sealed Tube'
_diffrn_measurement_device_type  'Rigaku Mercury2 (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 13.6612
_diffrn_reflns_number            5412
_diffrn_reflns_av_unetI/netI     0.0141
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.380
_diffrn_reflns_theta_max         27.495
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 0.983
_reflns_number_total             442
_reflns_number_gt                391
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Crystalmaker (Palmer, 2014)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         442
_refine_ls_number_parameters     37
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0253
_refine_ls_R_factor_gt           0.0229
_refine_ls_wR_factor_ref         0.1043
_refine_ls_wR_factor_gt          0.1012
_refine_ls_goodness_of_fit_ref   0.935
_refine_ls_restrained_S_all      0.935
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cs1 Cs 0.6667 0.3333 0.3333 0.0142(3) Uani 1 6 d S T P . .
Ni1 Ni 1.0000 1.0000 0.2500 0.0100(4) Uani 1 6 d S T P . .
O2 O 0.90354(18) 0.8263(2) 0.32349(17) 0.0154(5) Uani 1 1 d . . . . .
O1 O 0.71709(16) 0.62600(16) 0.31685(11) 0.0192(5) Uani 1 1 d . . . . .
C1 C 0.7907(2) 0.7425(2) 0.29009(14) 0.0154(5) Uani 1 1 d . . . . .
Li1 Li 0.5389(5) 0.5389(5) 0.2500 0.0208(11) Uani 1 2 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cs1 O1 3.1240(17) 33_545 ?
Cs1 O1 3.1240(17) . ?
Cs1 O1 3.1241(17) 3_665 ?
Cs1 O1 3.1241(17) 2_655 ?
Cs1 O1 3.1241(17) 32 ?
Cs1 O1 3.1241(17) 31_655 ?
Cs1 O2 3.186(2) 29_545 ?
Cs1 O2 3.186(2) 28_665 ?
Cs1 O2 3.187(2) 30_455 ?
Cs1 O2 3.187(2) 12_655 ?
Cs1 O2 3.187(2) 10_445 ?
Cs1 O2 3.187(2) 11_565 ?
Ni1 O2 2.059(2) . ?
Ni1 O2 2.059(2) 4 ?
Ni1 O2 2.059(2) 2_765 ?
Ni1 O2 2.059(2) 3_675 ?
Ni1 O2 2.059(2) 6_765 ?
Ni1 O2 2.059(2) 5_675 ?
Ni1 Cs1 3.7883(3) 10 ?
Ni1 Cs1 3.7883(3) 13_554 ?
O2 C1 1.271(3) . ?
O2 Li1 2.197(3) 32 ?
O2 Cs1 3.187(2) 10 ?
O1 C1 1.241(3) . ?
O1 Li1 2.042(5) . ?
O1 Li1 2.203(5) 32 ?
C1 C1 1.547(4) 4 ?
C1 Li1 2.477(4) 32 ?
C1 Li1 2.728(6) . ?
Li1 O1 2.042(5) 4 ?
Li1 O2 2.197(3) 30_455 ?
Li1 O2 2.197(3) 33_545 ?
Li1 O1 2.203(5) 30_455 ?
Li1 O1 2.203(5) 33_545 ?
Li1 C1 2.477(4) 30_455 ?
Li1 C1 2.477(4) 33_545 ?
Li1 C1 2.728(6) 4 ?
Li1 Cs1 3.5774(8) 4 ?

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_3
_geom_angle_publ_flag
O1 Cs1 O1 60.633(9) 33_545 . ?
O1 Cs1 O1 180.00(5) 33_545 3_665 ?
O1 Cs1 O1 119.367(9) . 3_665 ?
O1 Cs1 O1 60.632(9) 33_545 2_655 ?
O1 Cs1 O1 119.368(9) . 2_655 ?
O1 Cs1 O1 119.368(9) 3_665 2_655 ?
O1 Cs1 O1 119.369(9) 33_545 32 ?
O1 Cs1 O1 60.633(9) . 32 ?
O1 Cs1 O1 60.631(9) 3_665 32 ?
O1 Cs1 O1 180.0 2_655 32 ?
O1 Cs1 O1 119.368(9) 33_545 31_655 ?
O1 Cs1 O1 180.0 . 31_655 ?
O1 Cs1 O1 60.632(9) 3_665 31_655 ?
O1 Cs1 O1 60.633(9) 2_655 31_655 ?
O1 Cs1 O1 119.366(9) 32 31_655 ?
O1 Cs1 O2 100.85(4) 33_545 29_545 ?
O1 Cs1 O2 116.80(5) . 29_545 ?
O1 Cs1 O2 79.15(4) 3_665 29_545 ?
O1 Cs1 O2 62.36(5) 2_655 29_545 ?
O1 Cs1 O2 117.63(5) 32 29_545 ?
O1 Cs1 O2 63.20(5) 31_655 29_545 ?
O1 Cs1 O2 117.63(5) 33_545 28_665 ?
O1 Cs1 O2 79.14(4) . 28_665 ?
O1 Cs1 O2 62.37(5) 3_665 28_665 ?
O1 Cs1 O2 116.80(5) 2_655 28_665 ?
O1 Cs1 O2 63.20(5) 32 28_665 ?
O1 Cs1 O2 100.85(4) 31_655 28_665 ?
O2 Cs1 O2 56.16(7) 29_545 28_665 ?
O1 Cs1 O2 63.20(5) 33_545 30_455 ?
O1 Cs1 O2 62.36(5) . 30_455 ?
O1 Cs1 O2 116.80(5) 3_665 30_455 ?
O1 Cs1 O2 79.14(4) 2_655 30_455 ?
O1 Cs1 O2 100.86(4) 32 30_455 ?
O1 Cs1 O2 117.64(5) 31_655 30_455 ?
O2 Cs1 O2 56.16(7) 29_545 30_455 ?
O2 Cs1 O2 56.16(7) 28_665 30_455 ?
O1 Cs1 O2 116.80(5) 33_545 12_655 ?
O1 Cs1 O2 117.63(5) . 12_655 ?
O1 Cs1 O2 63.20(5) 3_665 12_655 ?
O1 Cs1 O2 100.86(4) 2_655 12_655 ?
O1 Cs1 O2 79.15(4) 32 12_655 ?
O1 Cs1 O2 62.37(5) 31_655 12_655 ?
O2 Cs1 O2 123.84(7) 29_545 12_655 ?
O2 Cs1 O2 123.84(7) 28_665 12_655 ?
O2 Cs1 O2 180.0 30_455 12_655 ?
O1 Cs1 O2 62.36(5) 33_545 10_445 ?
O1 Cs1 O2 100.85(4) . 10_445 ?
O1 Cs1 O2 117.64(5) 3_665 10_445 ?
O1 Cs1 O2 63.20(5) 2_655 10_445 ?
O1 Cs1 O2 116.80(5) 32 10_445 ?
O1 Cs1 O2 79.15(4) 31_655 10_445 ?
O2 Cs1 O2 123.84(7) 29_545 10_445 ?
O2 Cs1 O2 180.0 28_665 10_445 ?
O2 Cs1 O2 123.83(7) 30_455 10_445 ?
O2 Cs1 O2 56.16(7) 12_655 10_445 ?
O1 Cs1 O2 79.14(4) 33_545 11_565 ?
O1 Cs1 O2 63.20(5) . 11_565 ?
O1 Cs1 O2 100.86(4) 3_665 11_565 ?
O1 Cs1 O2 117.63(5) 2_655 11_565 ?
O1 Cs1 O2 62.37(5) 32 11_565 ?
O1 Cs1 O2 116.80(5) 31_655 11_565 ?
O2 Cs1 O2 180.0 29_545 11_565 ?
O2 Cs1 O2 123.84(7) 28_665 11_565 ?
O2 Cs1 O2 123.83(7) 30_455 11_565 ?
O2 Cs1 O2 56.16(7) 12_655 11_565 ?
O2 Cs1 O2 56.16(7) 10_445 11_565 ?
O2 Ni1 O2 82.16(12) . 4 ?
O2 Ni1 O2 93.51(9) . 2_765 ?
O2 Ni1 O2 173.85(9) 4 2_765 ?
O2 Ni1 O2 93.51(9) . 3_675 ?
O2 Ni1 O2 91.12(11) 4 3_675 ?
O2 Ni1 O2 93.51(9) 2_765 3_675 ?
O2 Ni1 O2 91.12(11) . 6_765 ?
O2 Ni1 O2 93.51(9) 4 6_765 ?
O2 Ni1 O2 82.16(12) 2_765 6_765 ?
O2 Ni1 O2 173.85(9) 3_675 6_765 ?
O2 Ni1 O2 173.85(9) . 5_675 ?
O2 Ni1 O2 93.51(9) 4 5_675 ?
O2 Ni1 O2 91.12(11) 2_765 5_675 ?
O2 Ni1 O2 82.16(12) 3_675 5_675 ?
O2 Ni1 O2 93.51(9) 6_765 5_675 ?
O2 Ni1 Cs1 57.26(7) . 10 ?
O2 Ni1 Cs1 122.74(7) 4 10 ?
O2 Ni1 Cs1 57.26(7) 2_765 10 ?
O2 Ni1 Cs1 57.26(7) 3_675 10 ?
O2 Ni1 Cs1 122.74(7) 6_765 10 ?
O2 Ni1 Cs1 122.74(7) 5_675 10 ?
O2 Ni1 Cs1 122.74(7) . 13_554 ?
O2 Ni1 Cs1 57.26(7) 4 13_554 ?
O2 Ni1 Cs1 122.74(7) 2_765 13_554 ?
O2 Ni1 Cs1 122.74(7) 3_675 13_554 ?
O2 Ni1 Cs1 57.26(7) 6_765 13_554 ?
O2 Ni1 Cs1 57.26(7) 5_675 13_554 ?
Cs1 Ni1 Cs1 180.0 10 13_554 ?
C1 O2 Ni1 111.68(18) . . ?
C1 O2 Li1 86.8(2) . 32 ?
Ni1 O2 Li1 160.18(16) . 32 ?
C1 O2 Cs1 135.41(15) . 10 ?
Ni1 O2 Cs1 89.81(8) . 10 ?
Li1 O2 Cs1 81.03(7) 32 10 ?
C1 O1 Li1 110.00(18) . . ?
C1 O1 Li1 87.30(13) . 32 ?
Li1 O1 Li1 162.07(19) . 32 ?
C1 O1 Cs1 147.90(15) . . ?
Li1 O1 Cs1 84.91(11) . . ?
Li1 O1 Cs1 82.43(6) 32 . ?
O1 C1 O2 125.0(2) . . ?
O1 C1 C1 118.01(13) . 4 ?
O2 C1 C1 116.98(15) . 4 ?
O1 C1 Li1 62.67(13) . 32 ?
O2 C1 Li1 62.35(16) . 32 ?
C1 C1 Li1 178.8(2) 4 32 ?
O1 C1 Li1 44.69(11) . . ?
O2 C1 Li1 168.74(18) . . ?
C1 C1 Li1 73.53(6) 4 . ?
Li1 C1 Li1 107.23(13) 32 . ?
O1 Li1 O1 83.5(3) 4 . ?
O1 Li1 O2 101.04(12) 4 30_455 ?
O1 Li1 O2 100.79(12) . 30_455 ?
O1 Li1 O2 100.79(12) 4 33_545 ?
O1 Li1 O2 101.04(12) . 33_545 ?
O2 Li1 O2 150.6(3) 30_455 33_545 ?
O1 Li1 O1 95.90(6) 4 30_455 ?
O1 Li1 O1 161.28(8) . 30_455 ?
O2 Li1 O1 60.86(11) 30_455 30_455 ?
O2 Li1 O1 97.46(19) 33_545 30_455 ?
O1 Li1 O1 161.28(8) 4 33_545 ?
O1 Li1 O1 95.90(6) . 33_545 ?
O2 Li1 O1 97.46(19) 30_455 33_545 ?
O2 Li1 O1 60.86(11) 33_545 33_545 ?
O1 Li1 O1 90.6(2) 30_455 33_545 ?
O1 Li1 C1 99.49(7) 4 30_455 ?
O1 Li1 C1 131.50(9) . 30_455 ?
O2 Li1 C1 30.83(9) 30_455 30_455 ?
O2 Li1 C1 125.3(2) 33_545 30_455 ?
O1 Li1 C1 30.03(8) 30_455 30_455 ?
O1 Li1 C1 94.9(2) 33_545 30_455 ?
O1 Li1 C1 131.50(9) 4 33_545 ?
O1 Li1 C1 99.49(7) . 33_545 ?
O2 Li1 C1 125.3(2) 30_455 33_545 ?
O2 Li1 C1 30.83(9) 33_545 33_545 ?
O1 Li1 C1 94.9(2) 30_455 33_545 ?
O1 Li1 C1 30.03(8) 33_545 33_545 ?
C1 Li1 C1 112.7(3) 30_455 33_545 ?
O1 Li1 C1 58.18(17) 4 . ?
O1 Li1 C1 25.31(10) . . ?
O2 Li1 C1 105.04(16) 30_455 . ?
O2 Li1 C1 103.14(16) 33_545 . ?
O1 Li1 C1 149.28(16) 30_455 . ?
O1 Li1 C1 119.30(10) 33_545 . ?
C1 Li1 C1 130.58(15) 30_455 . ?
C1 Li1 C1 114.38(10) 33_545 . ?
O1 Li1 C1 25.31(10) 4 4 ?
O1 Li1 C1 58.18(17) . 4 ?
O2 Li1 C1 103.14(15) 30_455 4 ?
O2 Li1 C1 105.04(16) 33_545 4 ?
O1 Li1 C1 119.30(10) 30_455 4 ?
O1 Li1 C1 149.28(16) 33_545 4 ?
C1 Li1 C1 114.38(10) 30_455 4 ?
C1 Li1 C1 130.58(15) 33_545 4 ?
C1 Li1 C1 32.95(12) . 4 ?
O1 Li1 Cs1 60.44(5) 4 4 ?
O1 Li1 Cs1 132.84(19) . 4 ?
O2 Li1 Cs1 114.32(9) 30_455 4 ?
O2 Li1 Cs1 61.62(7) 33_545 4 ?
O1 Li1 Cs1 59.96(5) 30_455 4 ?
O1 Li1 Cs1 108.95(14) 33_545 4 ?
C1 Li1 Cs1 86.56(9) 30_455 4 ?
C1 Li1 Cs1 85.49(8) 33_545 4 ?
C1 Li1 Cs1 111.18(14) . 4 ?
C1 Li1 Cs1 83.02(8) 4 4 ?
O1 Li1 Cs1 132.84(19) 4 . ?
O1 Li1 Cs1 60.44(5) . . ?
O2 Li1 Cs1 61.62(7) 30_455 . ?
O2 Li1 Cs1 114.32(9) 33_545 . ?
O1 Li1 Cs1 108.95(14) 30_455 . ?
O1 Li1 Cs1 59.96(5) 33_545 . ?
C1 Li1 Cs1 85.49(8) 30_455 . ?
C1 Li1 Cs1 86.56(9) 33_545 . ?
C1 Li1 Cs1 83.02(8) . . ?
C1 Li1 Cs1 111.18(14) 4 . ?
Cs1 Li1 Cs1 165.6(2) 4 . ?

_refine_diff_density_max         0.700
_refine_diff_density_min         -0.982
_refine_diff_density_rms         0.111

