# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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. 
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#######################################################################

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1503284'
_audit_update_record             
;
2016-09-13 deposited with the CCDC.
2017-09-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        'trilithium potassium iron(II) trioxalate'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 Fe O12, K, 3(Li)'
_chemical_formula_sum            'C6 Fe K Li3 O12'
_chemical_formula_weight         379.83

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
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'
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                   11.3897(8)
_cell_length_b                   11.3897(8)
_cell_length_c                   15.1197(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1698.6(3)
_cell_formula_units_Z            6
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    1004
_cell_measurement_theta_min      2.5
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.228
_exptl_crystal_F_000             1116
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    1.768
_shelx_estimated_absorpt_T_min   0.843
_shelx_estimated_absorpt_T_max   0.949
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.899
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_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            5486
_diffrn_reflns_av_unetI/netI     0.0224
_diffrn_reflns_av_R_equivalents  0.0635
_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         3.395
_diffrn_reflns_theta_max         27.459
_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             444
_reflns_number_gt                336
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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          0.0449
_refine_ls_R_factor_gt           0.0269
_refine_ls_wR_factor_ref         0.1052
_refine_ls_wR_factor_gt          0.0797
_refine_ls_goodness_of_fit_ref   0.807
_refine_ls_restrained_S_all      0.807
_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
Fe1 Fe 0.0000 0.0000 0.2500 0.0124(3) Uani 1 6 d S T P . .
K2 K 0.6667 0.3333 0.3333 0.0272(4) Uani 1 6 d S T P . .
O1 O 0.38490(18) 0.29134(18) 0.31640(12) 0.0174(5) Uani 1 1 d . . . . .
O2 O 0.17997(18) 0.10804(17) 0.32579(12) 0.0166(5) Uani 1 1 d . . . . .
C1 C 0.2669(2) 0.2193(3) 0.29054(16) 0.0134(5) Uani 1 1 d . . . . .
Li1 Li 0.4691(5) 0.4691(5) 0.2500 0.0180(12) 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
Fe1 O2 2.1229(17) 6 ?
Fe1 O2 2.1229(17) 3 ?
Fe1 O2 2.1229(17) 4 ?
Fe1 O2 2.1229(17) . ?
Fe1 O2 2.1230(17) 5 ?
Fe1 O2 2.1230(17) 2 ?
Fe1 K2 3.7799(3) 10_445 ?
Fe1 K2 3.7799(3) 13_444 ?
K2 O1 3.0097(19) 2_655 ?
K2 O1 3.0097(19) 3_665 ?
K2 O1 3.0097(19) 31_655 ?
K2 O1 3.0097(19) 33_545 ?
K2 O1 3.0097(19) . ?
K2 O1 3.0097(19) 32 ?
K2 O2 3.1829(18) 30 ?
K2 O2 3.1830(18) 28 ?
K2 O2 3.1830(18) 29 ?
K2 O2 3.1830(18) 11 ?
K2 O2 3.1830(18) 10 ?
K2 O2 3.1830(18) 12 ?
O1 C1 1.236(3) . ?
O1 Li1 2.021(5) . ?
O1 Li1 2.178(4) 33_545 ?
O2 C1 1.271(3) . ?
O2 Li1 2.118(3) 33_545 ?
O2 K2 3.1830(18) 10_445 ?
C1 C1 1.545(5) 4 ?
C1 Li1 2.416(4) 33_545 ?
C1 Li1 2.687(6) . ?
Li1 O1 2.021(5) 4 ?
Li1 O2 2.118(3) 32 ?
Li1 O2 2.118(3) 29 ?
Li1 O1 2.178(4) 32 ?
Li1 O1 2.178(4) 29 ?
Li1 C1 2.416(4) 32 ?
Li1 C1 2.416(4) 29 ?
Li1 C1 2.687(6) 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
O2 Fe1 O2 94.97(10) 6 3 ?
O2 Fe1 O2 93.61(7) 6 4 ?
O2 Fe1 O2 168.88(10) 3 4 ?
O2 Fe1 O2 168.89(10) 6 . ?
O2 Fe1 O2 93.61(7) 3 . ?
O2 Fe1 O2 78.82(10) 4 . ?
O2 Fe1 O2 93.61(7) 6 5 ?
O2 Fe1 O2 78.82(10) 3 5 ?
O2 Fe1 O2 93.61(7) 4 5 ?
O2 Fe1 O2 94.97(10) . 5 ?
O2 Fe1 O2 78.82(10) 6 2 ?
O2 Fe1 O2 93.61(7) 3 2 ?
O2 Fe1 O2 94.98(10) 4 2 ?
O2 Fe1 O2 93.61(7) . 2 ?
O2 Fe1 O2 168.88(10) 5 2 ?
O2 Fe1 K2 122.67(5) 6 10_445 ?
O2 Fe1 K2 57.33(5) 3 10_445 ?
O2 Fe1 K2 122.67(5) 4 10_445 ?
O2 Fe1 K2 57.33(5) . 10_445 ?
O2 Fe1 K2 122.67(5) 5 10_445 ?
O2 Fe1 K2 57.33(5) 2 10_445 ?
O2 Fe1 K2 57.33(5) 6 13_444 ?
O2 Fe1 K2 122.67(5) 3 13_444 ?
O2 Fe1 K2 57.33(5) 4 13_444 ?
O2 Fe1 K2 122.67(5) . 13_444 ?
O2 Fe1 K2 57.33(5) 5 13_444 ?
O2 Fe1 K2 122.67(5) 2 13_444 ?
K2 Fe1 K2 180.0 10_445 13_444 ?
O1 K2 O1 119.284(10) 2_655 3_665 ?
O1 K2 O1 60.715(10) 2_655 31_655 ?
O1 K2 O1 60.716(10) 3_665 31_655 ?
O1 K2 O1 60.716(10) 2_655 33_545 ?
O1 K2 O1 180.0 3_665 33_545 ?
O1 K2 O1 119.285(10) 31_655 33_545 ?
O1 K2 O1 119.285(10) 2_655 . ?
O1 K2 O1 119.284(10) 3_665 . ?
O1 K2 O1 180.0 31_655 . ?
O1 K2 O1 60.715(10) 33_545 . ?
O1 K2 O1 180.0 2_655 32 ?
O1 K2 O1 60.715(10) 3_665 32 ?
O1 K2 O1 119.284(10) 31_655 32 ?
O1 K2 O1 119.285(10) 33_545 32 ?
O1 K2 O1 60.716(10) . 32 ?
O1 K2 O2 77.83(5) 2_655 30 ?
O1 K2 O2 62.02(5) 3_665 30 ?
O1 K2 O2 62.05(5) 31_655 30 ?
O1 K2 O2 117.97(5) 33_545 30 ?
O1 K2 O2 117.95(5) . 30 ?
O1 K2 O2 102.17(5) 32 30 ?
O1 K2 O2 62.03(5) 2_655 28 ?
O1 K2 O2 117.96(5) 3_665 28 ?
O1 K2 O2 102.18(5) 31_655 28 ?
O1 K2 O2 62.04(5) 33_545 28 ?
O1 K2 O2 77.82(5) . 28 ?
O1 K2 O2 117.97(5) 32 28 ?
O2 K2 O2 58.19(5) 30 28 ?
O1 K2 O2 117.96(5) 2_655 29 ?
O1 K2 O2 77.82(5) 3_665 29 ?
O1 K2 O2 117.98(5) 31_655 29 ?
O1 K2 O2 102.17(5) 33_545 29 ?
O1 K2 O2 62.02(5) . 29 ?
O1 K2 O2 62.04(5) 32 29 ?
O2 K2 O2 58.19(5) 30 29 ?
O2 K2 O2 58.19(5) 28 29 ?
O1 K2 O2 62.05(5) 2_655 11 ?
O1 K2 O2 102.18(5) 3_665 11 ?
O1 K2 O2 62.03(5) 31_655 11 ?
O1 K2 O2 77.83(5) 33_545 11 ?
O1 K2 O2 117.97(5) . 11 ?
O1 K2 O2 117.96(5) 32 11 ?
O2 K2 O2 121.82(5) 30 11 ?
O2 K2 O2 121.82(5) 28 11 ?
O2 K2 O2 180.0 29 11 ?
O1 K2 O2 117.97(5) 2_655 10 ?
O1 K2 O2 62.05(5) 3_665 10 ?
O1 K2 O2 77.83(5) 31_655 10 ?
O1 K2 O2 117.96(5) 33_545 10 ?
O1 K2 O2 102.18(5) . 10 ?
O1 K2 O2 62.03(5) 32 10 ?
O2 K2 O2 121.81(5) 30 10 ?
O2 K2 O2 180.00(3) 28 10 ?
O2 K2 O2 121.81(5) 29 10 ?
O2 K2 O2 58.18(5) 11 10 ?
O1 K2 O2 102.18(5) 2_655 12 ?
O1 K2 O2 117.97(5) 3_665 12 ?
O1 K2 O2 117.96(5) 31_655 12 ?
O1 K2 O2 62.03(5) 33_545 12 ?
O1 K2 O2 62.05(5) . 12 ?
O1 K2 O2 77.83(5) 32 12 ?
O2 K2 O2 180.0 30 12 ?
O2 K2 O2 121.81(5) 28 12 ?
O2 K2 O2 121.81(5) 29 12 ?
O2 K2 O2 58.18(5) 11 12 ?
O2 K2 O2 58.18(5) 10 12 ?
C1 O1 Li1 108.74(19) . . ?
C1 O1 Li1 85.34(14) . 33_545 ?
Li1 O1 Li1 163.90(19) . 33_545 ?
C1 O1 K2 148.32(15) . . ?
Li1 O1 K2 87.08(11) . . ?
Li1 O1 K2 84.40(8) 33_545 . ?
C1 O2 Li1 87.14(17) . 33_545 ?
C1 O2 Fe1 113.38(15) . . ?
Li1 O2 Fe1 157.18(18) 33_545 . ?
C1 O2 K2 139.68(15) . 10_445 ?
Li1 O2 K2 81.06(5) 33_545 10_445 ?
Fe1 O2 K2 88.51(6) . 10_445 ?
O1 C1 O2 125.1(2) . . ?
O1 C1 C1 118.29(14) . 4 ?
O2 C1 C1 116.58(13) . 4 ?
O1 C1 Li1 63.99(13) . 33_545 ?
O2 C1 Li1 61.15(13) . 33_545 ?
C1 C1 Li1 177.65(11) 4 33_545 ?
O1 C1 Li1 45.42(12) . . ?
O2 C1 Li1 168.30(18) . . ?
C1 C1 Li1 73.29(6) 4 . ?
Li1 C1 Li1 109.03(14) 33_545 . ?
O1 Li1 O1 84.9(2) . 4 ?
O1 Li1 O2 101.44(12) . 32 ?
O1 Li1 O2 100.98(12) 4 32 ?
O1 Li1 O2 100.98(12) . 29 ?
O1 Li1 O2 101.44(12) 4 29 ?
O2 Li1 O2 149.5(3) 32 29 ?
O1 Li1 O1 92.79(7) . 32 ?
O1 Li1 O1 162.46(10) 4 32 ?
O2 Li1 O1 62.38(12) 32 32 ?
O2 Li1 O1 96.08(18) 29 32 ?
O1 Li1 O1 162.46(10) . 29 ?
O1 Li1 O1 92.79(7) 4 29 ?
O2 Li1 O1 96.08(18) 32 29 ?
O2 Li1 O1 62.38(12) 29 29 ?
O1 Li1 O1 94.5(3) 32 29 ?
O1 Li1 C1 97.93(8) . 32 ?
O1 Li1 C1 132.44(10) 4 32 ?
O2 Li1 C1 31.71(9) 32 32 ?
O2 Li1 C1 124.1(3) 29 32 ?
O1 Li1 C1 30.67(10) 32 32 ?
O1 Li1 C1 96.4(2) 29 32 ?
O1 Li1 C1 132.44(10) . 29 ?
O1 Li1 C1 97.94(8) 4 29 ?
O2 Li1 C1 124.1(3) 32 29 ?
O2 Li1 C1 31.71(9) 29 29 ?
O1 Li1 C1 96.4(2) 32 29 ?
O1 Li1 C1 30.67(10) 29 29 ?
C1 Li1 C1 113.2(3) 32 29 ?
O1 Li1 C1 25.84(11) . . ?
O1 Li1 C1 59.09(16) 4 . ?
O2 Li1 C1 103.25(16) 32 . ?
O2 Li1 C1 105.99(17) 29 . ?
O1 Li1 C1 116.78(11) 32 . ?
O1 Li1 C1 148.21(16) 29 . ?
C1 Li1 C1 113.25(10) 32 . ?
C1 Li1 C1 131.32(16) 29 . ?
O1 Li1 C1 59.09(16) . 4 ?
O1 Li1 C1 25.84(11) 4 4 ?
O2 Li1 C1 105.99(17) 32 4 ?
O2 Li1 C1 103.25(16) 29 4 ?
O1 Li1 C1 148.21(17) 32 4 ?
O1 Li1 C1 116.79(11) 29 4 ?
C1 Li1 C1 131.32(16) 32 4 ?
C1 Li1 C1 113.25(10) 29 4 ?
C1 Li1 C1 33.41(12) . 4 ?
O1 Li1 K2 132.43(19) . 4 ?
O1 Li1 K2 58.15(15) 4 4 ?
O2 Li1 K2 62.69(5) 32 4 ?
O2 Li1 K2 113.97(9) 29 4 ?
O1 Li1 K2 113.40(16) 32 4 ?
O1 Li1 K2 57.83(5) 29 4 ?
C1 Li1 K2 88.53(9) 32 4 ?
C1 Li1 K2 85.18(8) 29 4 ?
C1 Li1 K2 109.82(13) . 4 ?
C1 Li1 K2 81.47(8) 4 4 ?
O1 Li1 K2 58.15(15) . . ?
O1 Li1 K2 132.43(19) 4 . ?
O2 Li1 K2 113.97(9) 32 . ?
O2 Li1 K2 62.69(5) 29 . ?
O1 Li1 K2 57.83(5) 32 . ?
O1 Li1 K2 113.40(16) 29 . ?
C1 Li1 K2 85.18(8) 32 . ?
C1 Li1 K2 88.53(9) 29 . ?
C1 Li1 K2 81.47(8) . . ?
C1 Li1 K2 109.82(13) 4 . ?
K2 Li1 K2 168.6(2) 4 . ?

_refine_diff_density_max         0.262
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.079


_exptl_crystal_recrystallization_method 'hydrothermal method'
