# Electronic Supplementary Material (ESI) for Chemical Science.
# 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_StepI_100
_database_code_depnum_ccdc_archive 'CCDC 1868681'
loop_
_audit_author_name
_audit_author_address
'Igor Huskic'
;McGill University
Canada
;
_audit_update_record             
;
2018-09-19 deposited with the CCDC.	2019-04-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        
'Sodium magnesium Iron(iii) oxalate nonahydrate'
_chemical_name_common            Stepanovite
_chemical_formula_moiety         'Na Fe C6 O12 2-, Mg O6 H12 2+, H6 O3'
_chemical_formula_sum            'C6 H18 Fe Mg Na O21'
_chemical_compound_source        synthetic
_chemical_properties_physical    
photo-sensitive,Heat-sensitive,Light-sensitive,Photo-sensitive
_exptl_crystal_recrystallization_method water
_chemical_melting_point          ?

_exptl_crystal_description       'rhombohedral block'
_exptl_crystal_colour            green
_diffrn_ambient_temperature      100(2)
_chemical_formula_weight         529.35

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'
H H 0.0000 0.0000 '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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mg Mg 0.0486 0.0363 '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'

_space_group_crystal_system      trigonal
_space_group_IT_number           161
_space_group_name_H-M_alt        'R 3 c'
_space_group_name_Hall           'R 3 -2"c'
_chemical_absolute_configuration .

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'

_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.
;

_cell_length_a                   9.8670(9)
_cell_length_b                   9.8670(9)
_cell_length_c                   36.735(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3097.2(6)
_cell_formula_units_Z            6
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    17286
_cell_measurement_theta_min      5.258
_cell_measurement_theta_max      56.578
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.703
_exptl_crystal_F_000             1626
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_absorpt_coefficient_mu    0.878
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6198
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   'SADABS-2012/1, G. Sheldrick'
_exptl_absorpt_special_details   ?
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'Bruker PHOTON 100 CMOS'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15115
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_theta_min         2.447
_diffrn_reflns_theta_max         28.276
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measured_fraction_theta_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_point_group_measured_fraction_full 0.960
_reflns_number_total             1657
_reflns_number_gt                1629
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.975
_reflns_Friedel_fraction_max     0.956
_reflns_Friedel_fraction_full    0.952

_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'APEX 2, Bruker-AXS'
_computing_cell_refinement       'SAINT V8.35A, Bruker-AXS'
_computing_data_reduction        'SAINT V8.35A, Bruker-AXS'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          'Refined as a 2-component twin.,Twin'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0384P)²+0.2611P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 794 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.006(6)
_refine_ls_number_reflns         1657
_refine_ls_number_parameters     100
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0229
_refine_ls_R_factor_gt           0.0225
_refine_ls_wR_factor_ref         0.0549
_refine_ls_wR_factor_gt          0.0547
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_restrained_S_all      1.106
_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 0.000000 0.000000 0.41809(2) 0.02307(13) Uani 1 3 d S T P . .
Mg1 Mg 0.333333 0.666667 0.41621(4) 0.0237(2) Uani 1 3 d S T P . .
Na1 Na 0.666667 0.333333 0.41486(7) 0.0341(4) Uani 1 3 d S T P . .
O1 O 0.17758(15) 0.15714(15) 0.38721(4) 0.0313(3) Uani 1 1 d . . . . .
C1 C 0.3147(2) 0.20549(19) 0.40002(5) 0.0251(3) Uani 1 1 d . . . . .
O2 O 0.18138(14) 0.01664(15) 0.44663(4) 0.0296(3) Uani 1 1 d . . . . .
C2 C 0.31690(19) 0.1199(2) 0.43526(5) 0.0251(3) Uani 1 1 d . . . . .
O3 O 0.44188(16) 0.15296(18) 0.44895(4) 0.0397(3) Uani 1 1 d . . . . .
O4 O 0.43722(15) 0.30863(17) 0.38724(4) 0.0365(3) Uani 1 1 d . . . . .
O5 O 0.52790(15) 0.80042(19) 0.44865(4) 0.0346(3) Uani 1 1 d D . . . .
H5B H 0.504057 0.840860 0.465077 0.052 Uiso 1 1 d R U . . .
H5A H 0.614728 0.809155 0.450398 0.052 Uiso 1 1 d DR U . . .
O6 O 0.4685(2) 0.60825(16) 0.38437(4) 0.0363(3) Uani 1 1 d . . . . .
H6B H 0.463559 0.528203 0.383304 0.054 Uiso 1 1 d DR U . . .
H6A H 0.485494 0.639937 0.362434 0.054 Uiso 1 1 d DR U . . .
O7 O 0.47700(16) 0.47824(15) 0.49930(4) 0.0305(3) Uani 1 1 d D . . . .
H7A H 0.543(2) 0.492(3) 0.4847(6) 0.042(8) Uiso 1 1 d D . . . .
H7B H 0.489(3) 0.545(2) 0.5135(6) 0.037(7) Uiso 1 1 d D . . . .


_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 2.0088(13) . ?
Fe1 O2 2.0089(13) 2 ?
Fe1 O2 2.0089(13) 3 ?
Fe1 O1 2.0109(13) 2 ?
Fe1 O1 2.0109(13) 3 ?
Fe1 O1 2.0110(14) . ?
Mg1 O6 2.0613(19) . ?
Mg1 O6 2.0613(19) 3_565 ?
Mg1 O6 2.0613(19) 2_665 ?
Mg1 O5 2.0770(17) 2_665 ?
Mg1 O5 2.0771(17) . ?
Mg1 O5 2.0771(17) 3_565 ?
Na1 O4 2.3796(19) 3_665 ?
Na1 O4 2.3796(19) . ?
Na1 O4 2.3796(19) 2_655 ?
Na1 O3 2.389(2) 3_665 ?
Na1 O3 2.389(2) 2_655 ?
Na1 O3 2.389(2) . ?
Na1 C1 3.0933(18) 2_655 ?
Na1 C1 3.0933(18) . ?
Na1 C1 3.0933(18) 3_665 ?
Na1 C2 3.1047(18) 2_655 ?
Na1 C2 3.1047(18) 3_665 ?
Na1 C2 3.1047(18) . ?
O1 C1 1.278(2) . ?
C1 O4 1.220(2) . ?
C1 C2 1.552(2) . ?
O2 C2 1.280(2) . ?
C2 O3 1.216(2) . ?
O5 H5B 0.8200 . ?
O5 H5A 0.8196 . ?
O6 H6B 0.7675 . ?
O6 H6A 0.8502 . ?
O7 H7A 0.801(3) . ?
O7 H7B 0.801(3) . ?

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 95.24(6) . 2 ?
O2 Fe1 O2 95.24(6) . 3 ?
O2 Fe1 O2 95.24(6) 2 3 ?
O2 Fe1 O1 170.50(6) . 2 ?
O2 Fe1 O1 80.45(5) 2 2 ?
O2 Fe1 O1 93.60(6) 3 2 ?
O2 Fe1 O1 93.59(6) . 3 ?
O2 Fe1 O1 170.50(6) 2 3 ?
O2 Fe1 O1 80.45(5) 3 3 ?
O1 Fe1 O1 91.31(6) 2 3 ?
O2 Fe1 O1 80.45(5) . . ?
O2 Fe1 O1 93.60(6) 2 . ?
O2 Fe1 O1 170.50(5) 3 . ?
O1 Fe1 O1 91.31(6) 2 . ?
O1 Fe1 O1 91.31(6) 3 . ?
O6 Mg1 O6 90.98(9) . 3_565 ?
O6 Mg1 O6 90.98(9) . 2_665 ?
O6 Mg1 O6 90.98(9) 3_565 2_665 ?
O6 Mg1 O5 179.28(10) . 2_665 ?
O6 Mg1 O5 89.74(6) 3_565 2_665 ?
O6 Mg1 O5 88.94(6) 2_665 2_665 ?
O6 Mg1 O5 88.94(6) . . ?
O6 Mg1 O5 179.28(10) 3_565 . ?
O6 Mg1 O5 89.74(6) 2_665 . ?
O5 Mg1 O5 90.35(9) 2_665 . ?
O6 Mg1 O5 89.73(6) . 3_565 ?
O6 Mg1 O5 88.94(6) 3_565 3_565 ?
O6 Mg1 O5 179.28(10) 2_665 3_565 ?
O5 Mg1 O5 90.35(9) 2_665 3_565 ?
O5 Mg1 O5 90.35(9) . 3_565 ?
O4 Na1 O4 103.14(9) 3_665 . ?
O4 Na1 O4 103.14(9) 3_665 2_655 ?
O4 Na1 O4 103.14(9) . 2_655 ?
O4 Na1 O3 70.48(5) 3_665 3_665 ?
O4 Na1 O3 92.41(6) . 3_665 ?
O4 Na1 O3 164.27(8) 2_655 3_665 ?
O4 Na1 O3 92.41(6) 3_665 2_655 ?
O4 Na1 O3 164.27(8) . 2_655 ?
O4 Na1 O3 70.48(4) 2_655 2_655 ?
O3 Na1 O3 95.04(10) 3_665 2_655 ?
O4 Na1 O3 164.27(8) 3_665 . ?
O4 Na1 O3 70.48(5) . . ?
O4 Na1 O3 92.41(6) 2_655 . ?
O3 Na1 O3 95.04(10) 3_665 . ?
O3 Na1 O3 95.04(10) 2_655 . ?
O4 Na1 C1 98.59(7) 3_665 2_655 ?
O4 Na1 C1 123.98(9) . 2_655 ?
O4 Na1 C1 21.00(4) 2_655 2_655 ?
O3 Na1 C1 143.61(9) 3_665 2_655 ?
O3 Na1 C1 49.73(4) 2_655 2_655 ?
O3 Na1 C1 96.79(6) . 2_655 ?
O4 Na1 C1 123.98(9) 3_665 . ?
O4 Na1 C1 21.00(4) . . ?
O4 Na1 C1 98.59(7) 2_655 . ?
O3 Na1 C1 96.80(6) 3_665 . ?
O3 Na1 C1 143.61(9) 2_655 . ?
O3 Na1 C1 49.74(4) . . ?
C1 Na1 C1 116.96(4) 2_655 . ?
O4 Na1 C1 21.01(4) 3_665 3_665 ?
O4 Na1 C1 98.59(7) . 3_665 ?
O4 Na1 C1 123.98(9) 2_655 3_665 ?
O3 Na1 C1 49.73(4) 3_665 3_665 ?
O3 Na1 C1 96.80(6) 2_655 3_665 ?
O3 Na1 C1 143.61(9) . 3_665 ?
C1 Na1 C1 116.97(4) 2_655 3_665 ?
C1 Na1 C1 116.96(4) . 3_665 ?
O4 Na1 C2 94.48(5) 3_665 2_655 ?
O4 Na1 C2 151.07(6) . 2_655 ?
O4 Na1 C2 49.87(4) 2_655 2_655 ?
O3 Na1 C2 115.24(9) 3_665 2_655 ?
O3 Na1 C2 20.78(4) 2_655 2_655 ?
O3 Na1 C2 97.40(8) . 2_655 ?
C1 Na1 C2 28.99(4) 2_655 2_655 ?
C1 Na1 C2 137.07(4) . 2_655 ?
C1 Na1 C2 105.67(4) 3_665 2_655 ?
O4 Na1 C2 49.87(4) 3_665 3_665 ?
O4 Na1 C2 94.48(5) . 3_665 ?
O4 Na1 C2 151.07(6) 2_655 3_665 ?
O3 Na1 C2 20.78(4) 3_665 3_665 ?
O3 Na1 C2 97.40(8) 2_655 3_665 ?
O3 Na1 C2 115.24(9) . 3_665 ?
C1 Na1 C2 137.07(4) 2_655 3_665 ?
C1 Na1 C2 105.67(4) . 3_665 ?
C1 Na1 C2 28.99(4) 3_665 3_665 ?
C2 Na1 C2 114.37(5) 2_655 3_665 ?
O4 Na1 C2 151.07(6) 3_665 . ?
O4 Na1 C2 49.87(4) . . ?
O4 Na1 C2 94.48(5) 2_655 . ?
O3 Na1 C2 97.40(8) 3_665 . ?
O3 Na1 C2 115.24(9) 2_655 . ?
O3 Na1 C2 20.79(4) . . ?
C1 Na1 C2 105.67(4) 2_655 . ?
C1 Na1 C2 28.99(4) . . ?
C1 Na1 C2 137.07(4) 3_665 . ?
C2 Na1 C2 114.37(5) 2_655 . ?
C2 Na1 C2 114.37(5) 3_665 . ?
C1 O1 Fe1 115.57(10) . . ?
O4 C1 O1 126.32(16) . . ?
O4 C1 C2 119.84(16) . . ?
O1 C1 C2 113.85(14) . . ?
O4 C1 Na1 44.37(10) . . ?
O1 C1 Na1 168.53(13) . . ?
C2 C1 Na1 75.91(10) . . ?
C2 O2 Fe1 115.35(11) . . ?
O3 C2 O2 126.48(16) . . ?
O3 C2 C1 119.17(16) . . ?
O2 C2 C1 114.34(14) . . ?
O3 C2 Na1 44.22(11) . . ?
O2 C2 Na1 169.50(12) . . ?
C1 C2 Na1 75.10(10) . . ?
C2 O3 Na1 114.99(13) . . ?
C1 O4 Na1 114.63(13) . . ?
Mg1 O5 H5B 109.4 . . ?
Mg1 O5 H5A 134.2 . . ?
H5B O5 H5A 115.5 . . ?
Mg1 O6 H6B 126.8 . . ?
Mg1 O6 H6A 118.1 . . ?
H6B O6 H6A 103.3 . . ?
H7A O7 H7B 121.7(7) . . ?

_refine_diff_density_max         0.256
_refine_diff_density_min         -0.586
_refine_diff_density_rms         0.058

####################################################################### 
# 
# 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_StepII_297K
_database_code_depnum_ccdc_archive 'CCDC 1868683'
loop_
_audit_author_name
_audit_author_address
'Igor Huskic'
;McGill University
Canada
;
_audit_update_record             
;
2018-09-19 deposited with the CCDC.	2019-04-01 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT111_StepII_297K         
;
PROBLEM: ADDSYM Detects New (Pseudo) Centre of Symmetry .        100 %Fit
RESPONSE: Refinement in the centrosymmetric P-3c resulted in a higher Rwp value than refinement in P3c. Pseudosymmetry is present because most of the structure conforms to the higher symmetry, however one of the Mg(H2O)6 cations does not. Structural analogues present in CSD have been solved in P3c using Cu radiation, but this was not applicable because of iron(iii) present in structure.
;
_vrf_PLAT113_StepII_297K         
;
PROBLEM: ADDSYM Suggests Possible Pseudo/New  Space Group      P-3c1 Check
RESPONSE: Refinement in the centrosymmetric P-3c resulted in a higher Rwp value than refinement in P3c. Pseudosymmetry is present because most of the structure conforms to the higher symmetry, however one of the Mg(H2O)6 cations does not. Structural analogues present in CSD have been solved in P3c using Cu radiation, but this was not applicable because of iron(iii) present in structure.
;
# Added during the CSD deposition process: Wednesday 19 September 2018 05:00 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        
'sodium magnesium iron(III) oxalate nonahydrate'
_chemical_name_common            'Stepanovite, hexagonal polzmorph'
_chemical_formula_moiety         'Na Fe C6 O12 2-,Mg H12 O6 2+, H6 O3'
_chemical_formula_sum            'C6 H18 Fe Mg Na O21'
_chemical_compound_source        synthetic
_chemical_properties_physical    
'photo-sensitive, moisture-sensitive,Heat-sensitive,Light-sensitive,Photo-sensitive'
_exptl_crystal_recrystallization_method Water
_chemical_melting_point          ?

_exptl_crystal_description       'hexagonal prism'
_exptl_crystal_colour            green
_diffrn_ambient_temperature      297
_diffrn_ambient_pressure         101325
_chemical_formula_weight         529.35

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'
H H 0.0000 0.0000 '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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mg Mg 0.0486 0.0363 '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'

_space_group_crystal_system      trigonal
_space_group_IT_number           158
_space_group_name_H-M_alt        'P 3 c 1'
_space_group_name_Hall           'P 3 -2"c'
_chemical_absolute_configuration .

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'

_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.
;

_cell_length_a                   16.9954(12)
_cell_length_b                   16.9954(12)
_cell_length_c                   12.3838(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3097.8(5)
_cell_formula_units_Z            6
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    82752
_cell_measurement_theta_min      4.788
_cell_measurement_theta_max      57.425
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.703
_exptl_crystal_F_000             1626
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_absorpt_coefficient_mu    0.878
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6882
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_process_details   'SADABS-2012/1, G. Sheldrick'
_exptl_absorpt_special_details   ?
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Bruker D8'
_diffrn_measurement_device_type  'Bruker PHOTON 100 CMOS'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            78149
_diffrn_reflns_av_unetI/netI     0.0225
_diffrn_reflns_av_R_equivalents  0.0569
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.397
_diffrn_reflns_theta_max         28.780
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5364
_reflns_number_gt                4591
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.994
_reflns_Friedel_fraction_max     0.995
_reflns_Friedel_fraction_full    0.998

_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'APEX 2, Bruker-AXS'
_computing_cell_refinement       'SAINT V8.35A, Bruker-AXS'
_computing_data_reduction        'SAINT V8.35A, Bruker-AXS'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          'Refined as a 2-component inversion twin.,Twin'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0378P)²+1.4381P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.41(2)
_refine_ls_number_reflns         5364
_refine_ls_number_parameters     339
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0295
_refine_ls_wR_factor_ref         0.0787
_refine_ls_wR_factor_gt          0.0744
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_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 0.67205(6) 0.67644(3) 0.49287(9) 0.00930(10) Uani 1 1 d . . . . .
Mg1 Mg 0.333333 0.666667 0.4897(3) 0.0106(6) Uani 1 3 d S T P . .
Na1 Na 0.34305(8) 0.3385(2) 0.4933(4) 0.0102(2) Uani 1 1 d . . . . .
O1 O 0.7366(2) 0.6296(2) 0.3997(3) 0.0128(7) Uani 1 1 d . . . . .
C1 C 0.8102(3) 0.6370(3) 0.4419(3) 0.0103(8) Uani 1 1 d . . . . .
Mg2 Mg 0.666667 0.333333 0.5042(2) 0.0093(5) Uani 1 3 d S T P . .
O2 O 0.7871(2) 0.7229(2) 0.5786(3) 0.0121(7) Uani 1 1 d . . . . .
C2 C 0.8403(3) 0.6936(3) 0.5476(3) 0.0105(8) Uani 1 1 d . . . . .
O3 O 0.8534(2) 0.6034(2) 0.4064(3) 0.0116(7) Uani 1 1 d . . . . .
Mg3 Mg 0.000000 0.000000 0.4957(3) 0.0089(3) Uani 1 3 d S T P . .
C3 C 0.5295(3) 0.5026(3) 0.5470(4) 0.0108(9) Uani 1 1 d . . . . .
O4 O 0.9103(2) 0.7072(2) 0.5912(3) 0.0160(7) Uani 1 1 d . . . . .
C4 C 0.4999(3) 0.5299(3) 0.4418(4) 0.0101(9) Uani 1 1 d . . . . .
O5 O 0.6098(2) 0.5606(2) 0.5797(3) 0.0134(8) Uani 1 1 d . . . . .
C5 C 0.6385(3) 0.8179(4) 0.5468(4) 0.0116(8) Uani 1 1 d . . . . .
O6 O 0.5555(3) 0.6102(2) 0.4082(3) 0.0128(8) Uani 1 1 d . . . . .
C6 C 0.6988(3) 0.8500(3) 0.4445(3) 0.0093(8) Uani 1 1 d . . . . .
O7 O 0.4774(2) 0.4295(2) 0.5896(3) 0.0155(7) Uani 1 1 d . . . . .
O8 O 0.4283(2) 0.4748(2) 0.3982(3) 0.0167(8) Uani 1 1 d . . . . .
O9 O 0.6266(2) 0.7429(2) 0.5849(3) 0.0124(7) Uani 1 1 d . . . . .
O10 O 0.7162(2) 0.7902(2) 0.4050(3) 0.0137(7) Uani 1 1 d . . . . .
O11 O 0.7257(2) 0.9260(2) 0.4077(3) 0.0141(7) Uani 1 1 d . . . . .
O12 O 0.6070(2) 0.8640(2) 0.5830(3) 0.0151(8) Uani 1 1 d . . . . .
O13 O 0.2529(2) 0.5554(2) 0.3928(3) 0.0139(7) Uani 1 1 d D . . . .
H13B H 0.268(3) 0.529(3) 0.344(3) 0.015 Uiso 1 1 d . U . . .
H13A H 0.2004(18) 0.539(3) 0.381(4) 0.015(12) Uiso 1 1 d D . . . .
O14 O 0.3635(2) 0.5847(2) 0.5831(3) 0.0140(7) Uani 1 1 d D . . . .
H14B H 0.382(4) 0.605(4) 0.642(3) 0.07(2) Uiso 1 1 d D . . . .
H14A H 0.336(3) 0.5286(17) 0.587(4) 0.013(12) Uiso 1 1 d D . . . .
O15 O 0.7778(2) 0.4129(2) 0.4086(2) 0.0155(6) Uani 1 1 d D . . . .
H15B H 0.794(3) 0.4656(19) 0.401(4) 0.024(14) Uiso 1 1 d D . . . .
H15A H 0.800(3) 0.397(3) 0.358(3) 0.015 Uiso 1 1 d . U . . .
O16 O 0.5552(2) 0.2503(2) 0.5994(2) 0.0154(6) Uani 1 1 d D . . . .
H16B H 0.518(2) 0.1938(18) 0.598(4) 0.019(12) Uiso 1 1 d D . . . .
H16A H 0.555(5) 0.277(4) 0.655(3) 0.07(2) Uiso 1 1 d D . . . .
O17 O 0.11135(19) 0.0811(2) 0.3998(2) 0.0148(5) Uani 1 1 d D . . . .
H17B H 0.134(3) 0.063(3) 0.350(3) 0.015 Uiso 1 1 d . U . . .
H17A H 0.126(3) 0.1330(18) 0.394(4) 0.021(12) Uiso 1 1 d D . . . .
O18 O -0.11146(19) -0.08199(19) 0.5896(2) 0.0138(5) Uani 1 1 d . . . . .
H18B H -0.108(4) -0.048(4) 0.644(5) 0.06(2) Uiso 1 1 d . . . . .
H18A H -0.145(3) -0.139(3) 0.593(3) 0.015(11) Uiso 1 1 d . . . . .
O19 O 0.16024(18) 0.15759(17) 0.7422(3) 0.0126(5) Uani 1 1 d D . . . .
H19B H 0.196(2) 0.172(3) 0.697(3) 0.015 Uiso 1 1 d . U . . .
H19A H 0.172(3) 0.200(3) 0.779(4) 0.035(14) Uiso 1 1 d D . . . .
O20 O 0.6615(2) 0.49076(19) 0.2484(3) 0.0134(6) Uani 1 1 d . . . . .
H20B H 0.690(4) 0.538(4) 0.279(5) 0.042(14) Uiso 1 1 d . . . . .
H20A H 0.638(3) 0.503(3) 0.198(4) 0.018(11) Uiso 1 1 d . . . . .
O21 O 0.3367(3) 0.5078(2) 0.2409(3) 0.0126(5) Uani 1 1 d D . . . .
H21B H 0.314(3) 0.468(3) 0.200(4) 0.015 Uiso 1 1 d . U . . .
H21A H 0.374(3) 0.499(3) 0.269(4) 0.025(13) Uiso 1 1 d D . . . .


_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 2.008(4) . ?
Fe1 O10 2.009(4) . ?
Fe1 O1 2.010(4) . ?
Fe1 O9 2.011(4) . ?
Fe1 O6 2.015(4) . ?
Fe1 O5 2.017(4) . ?
Mg1 O14 2.063(4) 3_565 ?
Mg1 O14 2.063(4) 2_665 ?
Mg1 O14 2.063(4) . ?
Mg1 O13 2.073(4) 3_565 ?
Mg1 O13 2.073(4) . ?
Mg1 O13 2.073(4) 2_665 ?
Na1 O8 2.345(5) . ?
Na1 O7 2.345(4) . ?
Na1 O4 2.350(5) 2_655 ?
Na1 O11 2.357(4) 3_565 ?
Na1 O12 2.363(5) 3_565 ?
Na1 O3 2.370(5) 2_655 ?
Na1 C6 3.054(5) 3_565 ?
Na1 C1 3.059(6) 2_655 ?
Na1 C5 3.070(6) 3_565 ?
Na1 C2 3.070(6) 2_655 ?
Na1 C4 3.070(5) . ?
Na1 C3 3.070(5) . ?
O1 C1 1.304(6) . ?
C1 O3 1.215(6) . ?
C1 C2 1.552(6) . ?
Mg2 O15 2.060(4) . ?
Mg2 O15 2.060(4) 3_665 ?
Mg2 O15 2.060(4) 2_655 ?
Mg2 O16 2.072(4) 3_665 ?
Mg2 O16 2.072(4) . ?
Mg2 O16 2.072(4) 2_655 ?
O2 C2 1.289(6) . ?
C2 O4 1.218(6) . ?
Mg3 O18 2.060(4) 3 ?
Mg3 O18 2.060(4) . ?
Mg3 O18 2.060(4) 2 ?
Mg3 O17 2.069(4) 3 ?
Mg3 O17 2.069(4) 2 ?
Mg3 O17 2.069(4) . ?
C3 O7 1.227(6) . ?
C3 O5 1.286(5) . ?
C3 C4 1.549(4) . ?
C4 O8 1.229(6) . ?
C4 O6 1.280(6) . ?
C5 O12 1.234(6) . ?
C5 O9 1.276(6) . ?
C5 C6 1.546(5) . ?
C6 O11 1.222(6) . ?
C6 O10 1.289(6) . ?
O13 H13B 0.86(4) . ?
O13 H13A 0.80(2) . ?
O14 H14B 0.80(3) . ?
O14 H14A 0.83(2) . ?
O15 H15B 0.80(3) . ?
O15 H15A 0.84(4) . ?
O16 H16B 0.85(3) . ?
O16 H16A 0.83(3) . ?
O17 H17B 0.87(4) . ?
O17 H17A 0.79(2) . ?
O18 H18B 0.87(5) . ?
O18 H18A 0.84(4) . ?
O19 H19B 0.77(4) . ?
O19 H19A 0.79(3) . ?
O20 H20B 0.80(6) . ?
O20 H20A 0.82(4) . ?
O21 H21B 0.78(5) . ?
O21 H21A 0.79(3) . ?

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 O10 94.95(11) . . ?
O2 Fe1 O1 80.92(15) . . ?
O10 Fe1 O1 93.15(14) . . ?
O2 Fe1 O9 92.98(14) . . ?
O10 Fe1 O9 80.21(10) . . ?
O1 Fe1 O9 170.62(10) . . ?
O2 Fe1 O6 170.72(10) . . ?
O10 Fe1 O6 92.63(14) . . ?
O1 Fe1 O6 93.35(15) . . ?
O9 Fe1 O6 93.57(16) . . ?
O2 Fe1 O5 91.94(14) . . ?
O10 Fe1 O5 171.72(15) . . ?
O1 Fe1 O5 92.46(12) . . ?
O9 Fe1 O5 94.87(15) . . ?
O6 Fe1 O5 80.96(9) . . ?
O14 Mg1 O14 91.59(19) 3_565 2_665 ?
O14 Mg1 O14 91.59(19) 3_565 . ?
O14 Mg1 O14 91.59(19) 2_665 . ?
O14 Mg1 O13 88.99(13) 3_565 3_565 ?
O14 Mg1 O13 89.54(14) 2_665 3_565 ?
O14 Mg1 O13 178.7(2) . 3_565 ?
O14 Mg1 O13 89.53(14) 3_565 . ?
O14 Mg1 O13 178.7(2) 2_665 . ?
O14 Mg1 O13 88.99(13) . . ?
O13 Mg1 O13 89.88(18) 3_565 . ?
O14 Mg1 O13 178.7(2) 3_565 2_665 ?
O14 Mg1 O13 88.99(13) 2_665 2_665 ?
O14 Mg1 O13 89.53(14) . 2_665 ?
O13 Mg1 O13 89.88(18) 3_565 2_665 ?
O13 Mg1 O13 89.88(18) . 2_665 ?
O8 Na1 O7 71.72(10) . . ?
O8 Na1 O4 165.64(13) . 2_655 ?
O7 Na1 O4 98.12(19) . 2_655 ?
O8 Na1 O11 102.45(19) . 3_565 ?
O7 Na1 O11 166.3(2) . 3_565 ?
O4 Na1 O11 89.60(12) 2_655 3_565 ?
O8 Na1 O12 92.64(19) . 3_565 ?
O7 Na1 O12 95.25(19) . 3_565 ?
O4 Na1 O12 98.51(18) 2_655 3_565 ?
O11 Na1 O12 72.37(10) 3_565 3_565 ?
O8 Na1 O3 98.97(18) . 2_655 ?
O7 Na1 O3 95.36(13) . 2_655 ?
O4 Na1 O3 71.34(16) 2_655 2_655 ?
O11 Na1 O3 97.78(17) 3_565 2_655 ?
O12 Na1 O3 166.25(12) 3_565 2_655 ?
O8 Na1 C6 99.99(17) . 3_565 ?
O7 Na1 C6 145.5(2) . 3_565 ?
O4 Na1 C6 94.08(13) 2_655 3_565 ?
O11 Na1 C6 21.56(12) 3_565 3_565 ?
O12 Na1 C6 50.85(13) 3_565 3_565 ?
O3 Na1 C6 119.18(16) 2_655 3_565 ?
O8 Na1 C1 120.37(18) . 2_655 ?
O7 Na1 C1 101.15(15) . 2_655 ?
O4 Na1 C1 50.34(14) 2_655 2_655 ?
O11 Na1 C1 92.45(16) 3_565 2_655 ?
O12 Na1 C1 146.30(16) 3_565 2_655 ?
O3 Na1 C1 21.41(12) 2_655 2_655 ?
C6 Na1 C1 111.42(13) 3_565 2_655 ?
O8 Na1 C5 97.70(17) . 3_565 ?
O7 Na1 C5 116.87(19) . 3_565 ?
O4 Na1 C5 95.98(15) 2_655 3_565 ?
O11 Na1 C5 50.72(12) 3_565 3_565 ?
O12 Na1 C5 21.66(12) 3_565 3_565 ?
O3 Na1 C5 147.03(15) 2_655 3_565 ?
C6 Na1 C5 29.25(9) 3_565 3_565 ?
C1 Na1 C5 133.26(10) 2_655 3_565 ?
O8 Na1 C2 148.88(18) . 2_655 ?
O7 Na1 C2 101.71(17) . 2_655 ?
O4 Na1 C2 21.08(12) 2_655 2_655 ?
O11 Na1 C2 89.55(13) 3_565 2_655 ?
O12 Na1 C2 118.44(17) 3_565 2_655 ?
O3 Na1 C2 50.54(14) 2_655 2_655 ?
C6 Na1 C2 101.20(9) 3_565 2_655 ?
C1 Na1 C2 29.33(11) 2_655 2_655 ?
C5 Na1 C2 111.84(12) 3_565 2_655 ?
O8 Na1 C4 21.29(12) . . ?
O7 Na1 C4 50.44(13) . . ?
O4 Na1 C4 147.39(17) 2_655 . ?
O11 Na1 C4 122.97(19) 3_565 . ?
O12 Na1 C4 93.52(16) 3_565 . ?
O3 Na1 C4 99.97(15) 2_655 . ?
C6 Na1 C4 116.72(16) 3_565 . ?
C1 Na1 C4 119.60(13) 2_655 . ?
C5 Na1 C4 105.77(15) 3_565 . ?
C2 Na1 C4 141.09(11) 2_655 . ?
O8 Na1 C3 50.49(13) . . ?
O7 Na1 C3 21.24(12) . . ?
O4 Na1 C3 118.85(18) 2_655 . ?
O11 Na1 C3 150.91(19) 3_565 . ?
O12 Na1 C3 95.84(17) 3_565 . ?
O3 Na1 C3 97.22(13) 2_655 . ?
C6 Na1 C3 137.80(16) 3_565 . ?
C1 Na1 C3 109.97(11) 2_655 . ?
C5 Na1 C3 115.28(16) 3_565 . ?
C2 Na1 C3 119.10(14) 2_655 . ?
C4 Na1 C3 29.22(7) . . ?
C1 O1 Fe1 114.8(3) . . ?
O3 C1 O1 125.9(4) . . ?
O3 C1 C2 120.4(4) . . ?
O1 C1 C2 113.7(3) . . ?
O3 C1 Na1 45.4(2) . 3_665 ?
O1 C1 Na1 168.3(3) . 3_665 ?
C2 C1 Na1 75.7(2) . 3_665 ?
O15 Mg2 O15 90.29(17) . 3_665 ?
O15 Mg2 O15 90.29(17) . 2_655 ?
O15 Mg2 O15 90.29(17) 3_665 2_655 ?
O15 Mg2 O16 90.47(13) . 3_665 ?
O15 Mg2 O16 178.50(14) 3_665 3_665 ?
O15 Mg2 O16 88.41(12) 2_655 3_665 ?
O15 Mg2 O16 178.50(14) . . ?
O15 Mg2 O16 88.41(12) 3_665 . ?
O15 Mg2 O16 90.47(13) 2_655 . ?
O16 Mg2 O16 90.85(17) 3_665 . ?
O15 Mg2 O16 88.41(12) . 2_655 ?
O15 Mg2 O16 90.47(13) 3_665 2_655 ?
O15 Mg2 O16 178.50(15) 2_655 2_655 ?
O16 Mg2 O16 90.85(17) 3_665 2_655 ?
O16 Mg2 O16 90.85(17) . 2_655 ?
C2 O2 Fe1 115.1(3) . . ?
O4 C2 O2 127.0(4) . . ?
O4 C2 C1 118.6(4) . . ?
O2 C2 C1 114.4(4) . . ?
O4 C2 Na1 43.9(2) . 3_665 ?
O2 C2 Na1 169.2(3) . 3_665 ?
C1 C2 Na1 74.9(2) . 3_665 ?
C1 O3 Na1 113.2(3) . 3_665 ?
O18 Mg3 O18 91.24(19) 3 . ?
O18 Mg3 O18 91.24(19) 3 2 ?
O18 Mg3 O18 91.24(19) . 2 ?
O18 Mg3 O17 179.3(2) 3 3 ?
O18 Mg3 O17 88.94(12) . 3 ?
O18 Mg3 O17 89.47(12) 2 3 ?
O18 Mg3 O17 88.94(11) 3 2 ?
O18 Mg3 O17 89.47(12) . 2 ?
O18 Mg3 O17 179.3(2) 2 2 ?
O17 Mg3 O17 90.35(19) 3 2 ?
O18 Mg3 O17 89.47(12) 3 . ?
O18 Mg3 O17 179.3(2) . . ?
O18 Mg3 O17 88.94(12) 2 . ?
O17 Mg3 O17 90.35(19) 3 . ?
O17 Mg3 O17 90.35(19) 2 . ?
O7 C3 O5 126.4(5) . . ?
O7 C3 C4 119.1(5) . . ?
O5 C3 C4 114.5(5) . . ?
O7 C3 Na1 43.8(2) . . ?
O5 C3 Na1 169.3(4) . . ?
C4 C3 Na1 75.4(3) . . ?
C2 O4 Na1 115.0(3) . 3_665 ?
O8 C4 O6 126.2(5) . . ?
O8 C4 C3 119.2(5) . . ?
O6 C4 C3 114.6(5) . . ?
O8 C4 Na1 43.9(2) . . ?
O6 C4 Na1 169.8(4) . . ?
C3 C4 Na1 75.4(3) . . ?
C3 O5 Fe1 114.7(3) . . ?
O12 C5 O9 126.7(4) . . ?
O12 C5 C6 119.6(5) . . ?
O9 C5 C6 113.8(5) . . ?
O12 C5 Na1 45.0(3) . 2_665 ?
O9 C5 Na1 170.5(3) . 2_665 ?
C6 C5 Na1 74.8(3) . 2_665 ?
C4 O6 Fe1 114.9(3) . . ?
O11 C6 O10 125.4(4) . . ?
O11 C6 C5 120.7(5) . . ?
O10 C6 C5 113.9(5) . . ?
O11 C6 Na1 45.1(2) . 2_665 ?
O10 C6 Na1 168.9(3) . 2_665 ?
C5 C6 Na1 75.9(3) . 2_665 ?
C3 O7 Na1 114.9(3) . . ?
C4 O8 Na1 114.8(3) . . ?
C5 O9 Fe1 115.9(3) . . ?
C6 O10 Fe1 115.5(3) . . ?
C6 O11 Na1 113.3(3) . 2_665 ?
C5 O12 Na1 113.4(3) . 2_665 ?
Mg1 O13 H13B 131(3) . . ?
Mg1 O13 H13A 122(3) . . ?
H13B O13 H13A 104(4) . . ?
Mg1 O14 H14B 113(5) . . ?
Mg1 O14 H14A 128(3) . . ?
H14B O14 H14A 108(5) . . ?
Mg2 O15 H15B 120(4) . . ?
Mg2 O15 H15A 128(3) . . ?
H15B O15 H15A 108(5) . . ?
Mg2 O16 H16B 132(3) . . ?
Mg2 O16 H16A 111(5) . . ?
H16B O16 H16A 116(6) . . ?
Mg3 O17 H17B 126(3) . . ?
Mg3 O17 H17A 118(3) . . ?
H17B O17 H17A 113(5) . . ?
Mg3 O18 H18B 105(4) . . ?
Mg3 O18 H18A 132(3) . . ?
H18B O18 H18A 121(5) . . ?
H19B O19 H19A 110(4) . . ?
H20B O20 H20A 104(5) . . ?
H21B O21 H21A 102(4) . . ?

_refine_diff_density_max         0.551
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.061

####################################################################### 
# 
# 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_StepII_100
_database_code_depnum_ccdc_archive 'CCDC 1868682'
loop_
_audit_author_name
_audit_author_address
'Igor Huskic'
;McGill University
Canada
;
_audit_update_record             
;
2018-09-19 deposited with the CCDC.	2019-04-01 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT113_StepII_100          
;
PROBLEM: ADDSYM Suggests Possible Pseudo/New  Space Group      P-3c1 Check
RESPONSE: Refinement in the centrosymmetric P-3c resulted in a higher Rwp value than refinement in P3c. Pseudosymmetry is present because most of the structure conforms to the higher symmetry, however one of the Mg(H2O)6 cations does not. Structural analogues present in CSD have been solved in P3c using Cu radiation, but this was not applicable because of iron(iii) present in structure.
;
_vrf_PLAT417_StepII_100          
;
PROBLEM: Short Inter D-H..H-D       H15A     ..H20A     .       2.05 Ang.
RESPONSE: H20A and H15A are engaged in hydrogen bonding with O15 as the acceptor/donor.
;
# Added during the CSD deposition process: Wednesday 19 September 2018 05:00 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        
'sodium magnesium iron(III) oxalate nonahydrate'
_chemical_name_common            'Stepanovite, hexagonal polymorph'
_chemical_formula_moiety         'Na Fe C6 O12 2-,Mg H12 O6 2+, H6 O3'
_chemical_formula_sum            'C6 H18 Fe Mg Na O21'
_chemical_compound_source        synthetic
_chemical_properties_physical    
'moisture-sensitive, photo-sensitive,Heat-sensitive,Light-sensitive,Photo-sensitive'
_exptl_crystal_recrystallization_method water
_chemical_melting_point          ?

_exptl_crystal_description       'hexagonal prism'
_exptl_crystal_colour            green
_diffrn_ambient_temperature      100
_diffrn_ambient_pressure         101325
_chemical_formula_weight         529.35

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'
H H 0.0000 0.0000 '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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mg Mg 0.0486 0.0363 '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'

_space_group_crystal_system      trigonal
_space_group_IT_number           158
_space_group_name_H-M_alt        'P 3 c 1'
_space_group_name_Hall           'P 3 -2"c'
_chemical_absolute_configuration .

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'

_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.
;

_cell_length_a                   17.0033(11)
_cell_length_b                   17.0033(11)
_cell_length_c                   12.4160(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3108.7(4)
_cell_formula_units_Z            6
_cell_measurement_temperature    100
_cell_measurement_reflns_used    174810
_cell_measurement_theta_min      4.789
_cell_measurement_theta_max      79.556
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.697
_exptl_crystal_F_000             1626
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_absorpt_coefficient_mu    0.875
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6717
_exptl_absorpt_correction_T_max  0.7478
_exptl_absorpt_process_details   'SADABS-2012/1, G. Sheldrick'
_exptl_absorpt_special_details   ?
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Bruker D8'
_diffrn_measurement_device_type  'Bruker PHOTON 100 CMOS'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            168331
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_av_R_equivalents  0.0547
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.767
_diffrn_reflns_theta_max         39.871
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             12725
_reflns_number_gt                11489
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.997
_reflns_Friedel_fraction_max     0.998
_reflns_Friedel_fraction_full    0.998

_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'APEX 2, Bruker-AXS'
_computing_cell_refinement       'SAINT V8.35A, Bruker-AXS'
_computing_data_reduction        'SAINT V8.35A, Bruker-AXS'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          'Refined as a 2-component inversion twin.,Twin'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0429P)²+0.7817P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.148(11)
_refine_ls_number_reflns         12725
_refine_ls_number_parameters     343
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0351
_refine_ls_wR_factor_ref         0.0879
_refine_ls_wR_factor_gt          0.0851
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_restrained_S_all      1.099
_refine_ls_shift/su_max          0.001
_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 0.33871(2) 0.32888(2) 0.50060(4) 0.00742(4) Uani 1 1 d . . . . .
Na1 Na 0.00970(4) 0.33807(9) 0.50093(17) 0.01034(9) Uani 1 1 d . . . . .
Mg1 Mg 0.333333 0.666667 0.48948(11) 0.0084(2) Uani 1 3 d S T P . .
O1 O 0.27689(9) 0.38268(9) 0.41410(13) 0.0112(2) Uani 1 1 d . . . . .
C1 C 0.19671(11) 0.36122(11) 0.44711(16) 0.0092(3) Uani 1 1 d . . . . .
Mg2 Mg 0.666667 0.333333 0.49811(15) 0.00833(12) Uani 1 3 d S T P . .
O2 O 0.22252(10) 0.27891(9) 0.58596(13) 0.0109(2) Uani 1 1 d . . . . .
C2 C 0.16725(11) 0.30439(12) 0.55232(15) 0.0089(3) Uani 1 1 d . . . . .
O3 O 0.09517(10) 0.28695(11) 0.59517(14) 0.0149(3) Uani 1 1 d . . . . .
C3 C 0.47612(11) 0.50566(12) 0.55221(15) 0.0089(3) Uani 1 1 d . . . . .
Mg3 Mg 0.000000 0.000000 0.50447(13) 0.00951(19) Uani 1 3 d S T P . .
O4 O 0.14466(9) 0.38193(10) 0.40416(13) 0.0137(2) Uani 1 1 d . . . . .
C4 C 0.50706(12) 0.47956(11) 0.44697(15) 0.0088(2) Uani 1 1 d . . . . .
O5 O 0.40303(9) 0.43982(9) 0.59373(12) 0.0107(2) Uani 1 1 d . . . . .
C5 C 0.30503(11) 0.15399(12) 0.44735(15) 0.0089(2) Uani 1 1 d . . . . .
O6 O 0.45425(10) 0.39741(9) 0.41552(13) 0.0107(2) Uani 1 1 d . . . . .
C6 C 0.36520(11) 0.18220(12) 0.55001(15) 0.0090(2) Uani 1 1 d . . . . .
O7 O 0.57692(10) 0.53601(9) 0.40228(13) 0.0142(2) Uani 1 1 d . . . . .
O8 O 0.52014(10) 0.58300(9) 0.58806(13) 0.0120(2) Uani 1 1 d . . . . .
O9 O 0.29302(10) 0.21685(10) 0.40828(13) 0.0113(2) Uani 1 1 d . . . . .
O10 O 0.38244(10) 0.25977(9) 0.58862(13) 0.0111(2) Uani 1 1 d . . . . .
O11 O 0.27309(10) 0.07639(9) 0.41161(14) 0.0128(2) Uani 1 1 d . . . . .
O12 O 0.39226(9) 0.13305(10) 0.58649(13) 0.0130(2) Uani 1 1 d . . . . .
O13 O 0.11133(11) 0.08119(10) 0.60121(13) 0.0137(2) Uani 1 1 d . . . . .
H13B H 0.1233(19) 0.123(2) 0.610(2) 0.021 Uiso 1 1 d . U . . .
H13A H 0.1472(19) 0.074(2) 0.648(2) 0.021 Uiso 1 1 d . U . . .
O14 O 0.03082(10) 0.11189(10) 0.41083(13) 0.0137(2) Uani 1 1 d . . . . .
H14B H -0.001(2) 0.1433(19) 0.405(3) 0.021 Uiso 1 1 d . U . . .
H14A H 0.056(2) 0.112(2) 0.356(2) 0.021 Uiso 1 1 d . U . . .
O15 O 0.41581(9) 0.77807(10) 0.39418(12) 0.0134(2) Uani 1 1 d . . . . .
H15B H 0.479(2) 0.8163(19) 0.393(2) 0.020 Uiso 1 1 d . U . . .
H15A H 0.387(2) 0.782(2) 0.339(2) 0.020 Uiso 1 1 d . U . . .
O16 O 0.25287(9) 0.55530(10) 0.58484(12) 0.0136(2) Uani 1 1 d . . . . .
H16B H 0.262(2) 0.520(2) 0.640(3) 0.020 Uiso 1 1 d . U . . .
H16A H 0.209(2) 0.5440(19) 0.591(3) 0.020 Uiso 1 1 d . U . . .
O17 O 0.63706(9) 0.41517(9) 0.59368(11) 0.0136(2) Uani 1 1 d . . . . .
H17B H 0.670(2) 0.461(2) 0.601(2) 0.020 Uiso 1 1 d . U . . .
H17A H 0.593(2) 0.404(2) 0.645(2) 0.020 Uiso 1 1 d . U . . .
O18 O 0.74815(8) 0.44468(9) 0.40369(11) 0.0127(2) Uani 1 1 d . . . . .
H18B H 0.718(2) 0.445(2) 0.348(2) 0.019 Uiso 1 1 d . U . . .
H18A H 0.8092(19) 0.4800(18) 0.400(2) 0.019 Uiso 1 1 d . U . . .
O19 O 0.66386(10) 0.49091(8) 0.25120(12) 0.01121(18) Uani 1 1 d . . . . .
H19B H 0.6425(19) 0.5025(19) 0.294(2) 0.017 Uiso 1 1 d . U . . .
H19A H 0.6938(19) 0.538(2) 0.213(2) 0.017 Uiso 1 1 d . U . . .
O20 O 0.49571(9) 0.67177(10) 0.24490(12) 0.0116(2) Uani 1 1 d D . . . .
H20B H 0.5162(19) 0.6427(18) 0.214(2) 0.017 Uiso 1 1 d D U . . .
H20A H 0.5276(19) 0.696(2) 0.293(3) 0.017 Uiso 1 1 d . U . . .
O21 O 0.15886(9) 0.16250(9) 0.25260(14) 0.0117(2) Uani 1 1 d . . . . .
H21B H 0.196(2) 0.179(2) 0.299(2) 0.018 Uiso 1 1 d . U . . .
H21A H 0.172(2) 0.2112(19) 0.218(3) 0.018 Uiso 1 1 d . U . . .


_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 O10 2.0003(15) . ?
Fe1 O5 2.0071(14) . ?
Fe1 O6 2.0110(16) . ?
Fe1 O1 2.0143(16) . ?
Fe1 O9 2.0164(15) . ?
Fe1 O2 2.0174(16) . ?
Na1 O3 2.345(2) . ?
Na1 O4 2.357(2) . ?
Na1 O12 2.3587(19) 2 ?
Na1 O7 2.361(2) 3_565 ?
Na1 O8 2.371(2) 3_565 ?
Na1 O11 2.373(2) 2 ?
Na1 C6 3.061(2) 2 ?
Na1 C3 3.072(2) 3_565 ?
Na1 C2 3.073(2) . ?
Na1 C4 3.074(2) 3_565 ?
Na1 C5 3.074(2) 2 ?
Na1 C1 3.0758(19) . ?
Mg1 O16 2.0661(17) . ?
Mg1 O16 2.0661(17) 3_565 ?
Mg1 O16 2.0661(17) 2_665 ?
Mg1 O15 2.0733(16) . ?
Mg1 O15 2.0733(16) 2_665 ?
Mg1 O15 2.0733(16) 3_565 ?
O1 C1 1.289(2) . ?
C1 O4 1.226(2) . ?
C1 C2 1.5515(16) . ?
Mg2 O18 2.0628(17) 3_665 ?
Mg2 O18 2.0628(17) 2_655 ?
Mg2 O18 2.0628(17) . ?
Mg2 O17 2.0732(18) 3_665 ?
Mg2 O17 2.0732(18) 2_655 ?
Mg2 O17 2.0732(18) . ?
O2 C2 1.285(2) . ?
C2 O3 1.229(2) . ?
C3 O8 1.226(2) . ?
C3 O5 1.293(2) . ?
C3 C4 1.554(2) . ?
Mg3 O14 2.0612(18) 3 ?
Mg3 O14 2.0612(18) . ?
Mg3 O14 2.0613(18) 2 ?
Mg3 O13 2.0781(18) 3 ?
Mg3 O13 2.0781(18) . ?
Mg3 O13 2.0782(18) 2 ?
C4 O7 1.225(2) . ?
C4 O6 1.287(2) . ?
C5 O11 1.231(2) . ?
C5 O9 1.280(2) . ?
C5 C6 1.5526(19) . ?
C6 O12 1.225(2) . ?
C6 O10 1.292(2) . ?
O13 H13B 0.65(3) . ?
O13 H13A 0.90(3) . ?
O14 H14B 0.94(3) . ?
O14 H14A 0.81(3) . ?
O15 H15B 0.94(3) . ?
O15 H15A 0.87(3) . ?
O16 H16B 0.98(3) . ?
O16 H16A 0.68(3) . ?
O17 H17B 0.70(3) . ?
O17 H17A 0.93(3) . ?
O18 H18B 0.86(3) . ?
O18 H18A 0.90(3) . ?
O19 H19B 0.73(3) . ?
O19 H19A 0.84(3) . ?
O20 H20B 0.83(2) . ?
O20 H20A 0.78(3) . ?
O21 H21B 0.79(3) . ?
O21 H21A 0.86(3) . ?

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
O10 Fe1 O5 92.84(6) . . ?
O10 Fe1 O6 94.88(5) . . ?
O5 Fe1 O6 80.95(6) . . ?
O10 Fe1 O1 171.79(6) . . ?
O5 Fe1 O1 92.47(5) . . ?
O6 Fe1 O1 92.13(6) . . ?
O10 Fe1 O9 80.59(4) . . ?
O5 Fe1 O9 170.70(4) . . ?
O6 Fe1 O9 92.99(6) . . ?
O1 Fe1 O9 94.81(6) . . ?
O10 Fe1 O2 92.24(6) . . ?
O5 Fe1 O2 92.97(6) . . ?
O6 Fe1 O2 170.85(4) . . ?
O1 Fe1 O2 81.24(4) . . ?
O9 Fe1 O2 93.85(6) . . ?
O3 Na1 O4 71.69(4) . . ?
O3 Na1 O12 102.53(9) . 2 ?
O4 Na1 O12 166.39(8) . 2 ?
O3 Na1 O7 165.67(6) . 3_565 ?
O4 Na1 O7 97.88(9) . 3_565 ?
O12 Na1 O7 89.72(6) 2 3_565 ?
O3 Na1 O8 99.06(8) . 3_565 ?
O4 Na1 O8 95.45(6) . 3_565 ?
O12 Na1 O8 97.66(8) 2 3_565 ?
O7 Na1 O8 71.61(7) 3_565 3_565 ?
O3 Na1 O11 92.32(8) . 2 ?
O4 Na1 O11 95.29(9) . 2 ?
O12 Na1 O11 72.32(4) 2 2 ?
O7 Na1 O11 98.55(8) 3_565 2 ?
O8 Na1 O11 166.34(5) 3_565 2 ?
O3 Na1 C6 99.94(7) . 2 ?
O4 Na1 C6 145.50(9) . 2 ?
O12 Na1 C6 21.53(5) 2 2 ?
O7 Na1 C6 94.17(5) 3_565 2 ?
O8 Na1 C6 119.04(8) 3_565 2 ?
O11 Na1 C6 50.83(5) 2 2 ?
O3 Na1 C3 120.53(8) . 3_565 ?
O4 Na1 C3 101.03(6) . 3_565 ?
O12 Na1 C3 92.52(7) 2 3_565 ?
O7 Na1 C3 50.51(6) 3_565 3_565 ?
O8 Na1 C3 21.49(5) 3_565 3_565 ?
O11 Na1 C3 146.47(7) 2 3_565 ?
C6 Na1 C3 111.49(6) 2 3_565 ?
O3 Na1 C2 21.24(5) . . ?
O4 Na1 C2 50.45(5) . . ?
O12 Na1 C2 123.07(8) 2 . ?
O7 Na1 C2 147.17(8) 3_565 . ?
O8 Na1 C2 99.79(6) 3_565 . ?
O11 Na1 C2 93.55(7) 2 . ?
C6 Na1 C2 116.83(6) 2 . ?
C3 Na1 C2 119.40(5) 3_565 . ?
O3 Na1 C4 149.02(8) . 3_565 ?
O4 Na1 C4 101.69(7) . 3_565 ?
O12 Na1 C4 89.49(5) 2 3_565 ?
O7 Na1 C4 21.30(5) 3_565 3_565 ?
O8 Na1 C4 50.61(6) 3_565 3_565 ?
O11 Na1 C4 118.62(8) 2 3_565 ?
C6 Na1 C4 101.19(4) 2 3_565 ?
C3 Na1 C4 29.29(5) 3_565 3_565 ?
C2 Na1 C4 140.97(5) . 3_565 ?
O3 Na1 C5 97.64(7) . 2 ?
O4 Na1 C5 116.85(9) . 2 ?
O12 Na1 C5 50.75(5) 2 2 ?
O7 Na1 C5 95.88(6) 3_565 2 ?
O8 Na1 C5 146.96(7) 3_565 2 ?
O11 Na1 C5 21.60(5) 2 2 ?
C6 Na1 C5 29.32(4) 2 2 ?
C3 Na1 C5 133.30(4) 3_565 2 ?
C2 Na1 C5 105.95(6) . 2 ?
C4 Na1 C5 111.80(5) 3_565 2 ?
O3 Na1 C1 50.45(5) . . ?
O4 Na1 C1 21.25(5) . . ?
O12 Na1 C1 151.02(8) 2 . ?
O7 Na1 C1 118.61(8) 3_565 . ?
O8 Na1 C1 97.17(5) 3_565 . ?
O11 Na1 C1 95.90(7) 2 . ?
C6 Na1 C1 137.92(6) 2 . ?
C3 Na1 C1 109.79(4) 3_565 . ?
C2 Na1 C1 29.23(3) . . ?
C4 Na1 C1 119.04(6) 3_565 . ?
C5 Na1 C1 115.39(6) 2 . ?
O16 Mg1 O16 90.42(8) . 3_565 ?
O16 Mg1 O16 90.42(8) . 2_665 ?
O16 Mg1 O16 90.42(8) 3_565 2_665 ?
O16 Mg1 O15 179.08(6) . . ?
O16 Mg1 O15 90.11(6) 3_565 . ?
O16 Mg1 O15 88.82(6) 2_665 . ?
O16 Mg1 O15 90.10(6) . 2_665 ?
O16 Mg1 O15 88.82(6) 3_565 2_665 ?
O16 Mg1 O15 179.08(6) 2_665 2_665 ?
O15 Mg1 O15 90.66(8) . 2_665 ?
O16 Mg1 O15 88.82(6) . 3_565 ?
O16 Mg1 O15 179.08(6) 3_565 3_565 ?
O16 Mg1 O15 90.10(6) 2_665 3_565 ?
O15 Mg1 O15 90.66(8) . 3_565 ?
O15 Mg1 O15 90.66(8) 2_665 3_565 ?
C1 O1 Fe1 114.84(12) . . ?
O4 C1 O1 126.40(18) . . ?
O4 C1 C2 119.37(17) . . ?
O1 C1 C2 114.22(17) . . ?
O4 C1 Na1 44.17(10) . . ?
O1 C1 Na1 169.89(13) . . ?
C2 C1 Na1 75.30(11) . . ?
O18 Mg2 O18 90.89(9) 3_665 2_655 ?
O18 Mg2 O18 90.89(9) 3_665 . ?
O18 Mg2 O18 90.89(9) 2_655 . ?
O18 Mg2 O17 89.22(5) 3_665 3_665 ?
O18 Mg2 O17 179.69(12) 2_655 3_665 ?
O18 Mg2 O17 89.40(5) . 3_665 ?
O18 Mg2 O17 89.40(5) 3_665 2_655 ?
O18 Mg2 O17 89.21(5) 2_655 2_655 ?
O18 Mg2 O17 179.69(11) . 2_655 ?
O17 Mg2 O17 90.50(9) 3_665 2_655 ?
O18 Mg2 O17 179.69(11) 3_665 . ?
O18 Mg2 O17 89.40(5) 2_655 . ?
O18 Mg2 O17 89.22(5) . . ?
O17 Mg2 O17 90.49(9) 3_665 . ?
O17 Mg2 O17 90.49(9) 2_655 . ?
C2 O2 Fe1 114.48(13) . . ?
O3 C2 O2 125.95(18) . . ?
O3 C2 C1 119.16(17) . . ?
O2 C2 C1 114.88(17) . . ?
O3 C2 Na1 43.75(10) . . ?
O2 C2 Na1 169.26(14) . . ?
C1 C2 Na1 75.47(11) . . ?
C2 O3 Na1 115.01(14) . . ?
O8 C3 O5 126.21(17) . . ?
O8 C3 C4 119.95(15) . . ?
O5 C3 C4 113.83(14) . . ?
O8 C3 Na1 45.09(10) . 2_665 ?
O5 C3 Na1 168.46(14) . 2_665 ?
C4 C3 Na1 75.43(9) . 2_665 ?
O14 Mg3 O14 91.30(9) 3 . ?
O14 Mg3 O14 91.31(9) 3 2 ?
O14 Mg3 O14 91.30(9) . 2 ?
O14 Mg3 O13 89.21(6) 3 3 ?
O14 Mg3 O13 179.00(11) . 3 ?
O14 Mg3 O13 89.55(6) 2 3 ?
O14 Mg3 O13 89.55(6) 3 . ?
O14 Mg3 O13 89.20(6) . . ?
O14 Mg3 O13 179.00(11) 2 . ?
O13 Mg3 O13 89.94(9) 3 . ?
O14 Mg3 O13 179.00(11) 3 2 ?
O14 Mg3 O13 89.55(6) . 2 ?
O14 Mg3 O13 89.20(6) 2 2 ?
O13 Mg3 O13 89.94(9) 3 2 ?
O13 Mg3 O13 89.94(9) . 2 ?
C1 O4 Na1 114.58(13) . . ?
O7 C4 O6 126.18(17) . . ?
O7 C4 C3 119.42(15) . . ?
O6 C4 C3 114.40(15) . . ?
O7 C4 Na1 44.45(10) . 2_665 ?
O6 C4 Na1 169.00(13) . 2_665 ?
C3 C4 Na1 75.27(9) . 2_665 ?
C3 O5 Fe1 114.84(12) . . ?
O11 C5 O9 126.11(18) . . ?
O11 C5 C6 119.75(18) . . ?
O9 C5 C6 114.13(17) . . ?
O11 C5 Na1 45.19(11) . 3 ?
O9 C5 Na1 170.04(14) . 3 ?
C6 C5 Na1 74.85(12) . 3 ?
C4 O6 Fe1 114.77(12) . . ?
O12 C6 O10 126.06(17) . . ?
O12 C6 C5 120.48(18) . . ?
O10 C6 C5 113.46(17) . . ?
O12 C6 Na1 44.97(10) . 3 ?
O10 C6 Na1 169.56(14) . 3 ?
C5 C6 Na1 75.83(12) . 3 ?
C4 O7 Na1 114.25(13) . 2_665 ?
C3 O8 Na1 113.42(13) . 2_665 ?
C5 O9 Fe1 115.25(12) . . ?
C6 O10 Fe1 115.84(12) . . ?
C5 O11 Na1 113.21(13) . 3 ?
C6 O12 Na1 113.50(13) . 3 ?
Mg3 O13 H13B 120(3) . . ?
Mg3 O13 H13A 138(2) . . ?
H13B O13 H13A 101(3) . . ?
Mg3 O14 H14B 128.0(19) . . ?
Mg3 O14 H14A 112(2) . . ?
H14B O14 H14A 113(3) . . ?
Mg1 O15 H15B 130.9(18) . . ?
Mg1 O15 H15A 112(2) . . ?
H15B O15 H15A 116(3) . . ?
Mg1 O16 H16B 137.5(18) . . ?
Mg1 O16 H16A 117(3) . . ?
H16B O16 H16A 103(3) . . ?
Mg2 O17 H17B 119(2) . . ?
Mg2 O17 H17A 135(2) . . ?
H17B O17 H17A 105(3) . . ?
Mg2 O18 H18B 109.2(19) . . ?
Mg2 O18 H18A 131.4(18) . . ?
H18B O18 H18A 117(3) . . ?
H19B O19 H19A 108(2) . . ?
H20B O20 H20A 106(3) . . ?
H21B O21 H21A 104(3) . . ?

_refine_diff_density_max         0.478
_refine_diff_density_min         -0.713
_refine_diff_density_rms         0.120

####################################################################### 
# 
# 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_StepI_dehydr
_database_code_depnum_ccdc_archive 'CCDC 1868684'
loop_
_audit_author_name
_audit_author_address
'Igor Huskic'
;McGill University
Canada
;
_audit_update_record             
;
2018-09-19 deposited with the CCDC.	2019-04-01 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT097_StepI_dehydr        
;
PROBLEM: Large Reported Max.  (Positive) Residual Density       3.62 eA-3
RESPONSE: Due to the stress damage upon heating and cooling of the crystal, the quality was of the crystal was somewhat poor. The structure was solved as as a twin with 4 components, however, some twinning belonging to smaller domains was unnacounted for.
;
_vrf_PLAT420_StepI_dehydr        
;
PROBLEM: D-H Without Acceptor       O11      --H11A     .     Please Check
RESPONSE: The hydrogens belonging to water molecules were located from the electron density map and their positions were allowed to refine with gentle restraints.
;
# Added during the CSD deposition process: Wednesday 19 September 2018 05:00 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        
'Sodium magnesium iron(III) oxalate hexahydrate'
_chemical_name_common            ?
_chemical_formula_moiety         'Na Fe C6 O12 2-, Mg (H2O)6 2+'
_chemical_formula_sum            'C6 H12 Fe Mg Na O18'
_chemical_compound_source        synthetic
_chemical_properties_physical    
'moisture-sensitive, photo-sensitive,Moisture-sensitive,Deliquescent,Light-sensitive'
_exptl_crystal_recrystallization_method 'dehydrated from nonahydrate'
_chemical_melting_point          ?

_exptl_crystal_description       rhombohedral
_exptl_crystal_colour            'dull green'
_diffrn_ambient_temperature      100(2)
_diffrn_ambient_pressure         101325
_chemical_formula_weight         475.31

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'
H H 0.0000 0.0000 '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'
Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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           146
_space_group_name_H-M_alt        'R 3'
_space_group_name_Hall           'R 3'
_chemical_absolute_configuration .

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'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'
'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'

_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.
;

_cell_length_a                   9.77454(19)
_cell_length_b                   9.77454(19)
_cell_length_c                   29.7940(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2465.20(13)
_cell_formula_units_Z            6
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    23935
_cell_measurement_theta_min      5.566
_cell_measurement_theta_max      74.781
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.921
_exptl_crystal_F_000             1446
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    1.079
_shelx_estimated_absorpt_T_min   0.813
_shelx_estimated_absorpt_T_max   0.813
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6468
_exptl_absorpt_correction_T_max  0.7474
_exptl_absorpt_process_details   'SADABS-2012/1, G. Sheldrick'
_exptl_absorpt_special_details   ?
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Bruker D8'
_diffrn_measurement_device_type  'Bruker PHOTON 100 CMOS'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            58144
_diffrn_reflns_av_unetI/netI     0.0548
_diffrn_reflns_av_R_equivalents  0.1089
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_theta_min         2.051
_diffrn_reflns_theta_max         39.297
_diffrn_reflns_theta_full        25.250
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6325
_reflns_number_gt                5643
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.981
_reflns_Friedel_fraction_max     0.959
_reflns_Friedel_fraction_full    0.999

_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'APEX 2, Bruker-AXS'
_computing_cell_refinement       'SAINT V8.35A, Bruker-AXS'
_computing_data_reduction        'SAINT V8.35A, Bruker-AXS'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          'Refined as a 2-component inversion twin.,Twin'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0830P)²+6.4457P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Twinning involves inversion, so Flack parameter cannot be determined
;
_refine_ls_abs_structure_Flack   ?
_refine_ls_number_reflns         6325
_refine_ls_number_parameters     168
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0607
_refine_ls_wR_factor_ref         0.1672
_refine_ls_wR_factor_gt          0.1522
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_restrained_S_all      1.086
_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 0.000000 0.000000 0.41242(3) 0.0140(3) Uani 1 3 d S T P . .
Mg1 Mg 0.666667 0.333333 0.42073(15) 0.0138(4) Uani 1 3 d S T P . .
Na1 Na 0.333333 0.666667 0.43316(14) 0.0174(6) Uani 1 3 d S T P . .
O1 O 0.3449(5) 0.4986(5) 0.55196(14) 0.0147(6) Uani 1 1 d . . . . .
C1 C 0.4517(5) 0.4678(5) 0.56489(16) 0.0127(7) Uani 1 1 d . . . . .
Na2 Na 0.666667 0.333333 0.58851(16) 0.0149(7) Uani 1 3 d S T P . .
Fe2 Fe 0.333333 0.666667 0.58757(3) 0.0130(2) Uani 1 3 d S T P . .
Mg2 Mg 1.000000 1.000000 0.58810(12) 0.0126(4) Uani 1 3 d S T P . .
O2 O 0.4916(5) 0.6439(5) 0.62564(14) 0.0168(7) Uani 1 1 d . . . . .
C2 C 0.5405(5) 0.5561(5) 0.60811(18) 0.0135(7) Uani 1 1 d . . . . .
O3 O 0.4876(5) 0.3772(5) 0.54645(15) 0.0190(7) Uani 1 1 d . . . . .
C3 C 0.2003(5) 0.3227(6) 0.39811(17) 0.0138(7) Uani 1 1 d . . . . .
O8 O 0.1587(5) 0.1899(5) 0.37898(13) 0.0162(6) Uani 1 1 d . . . . .
O9 O 0.9482(4) 0.8037(5) 0.62616(14) 0.0177(6) Uani 1 1 d . . . . .
H9A H 0.844884 0.735081 0.626863 0.027 Uiso 1 1 d R U . . .
H9B H 0.979742 0.829093 0.654479 0.027 Uiso 1 1 d R U . . .
O10 O 1.0566(5) 1.1947(5) 0.54724(14) 0.0175(6) Uani 1 1 d . . . . .
H10A H 1.049835 1.170124 0.518441 0.026 Uiso 1 1 d R U . . .
H10B H 1.154114 1.272240 0.552187 0.026 Uiso 1 1 d R U . . .
O11 O 0.4704(5) 0.2838(5) 0.45911(15) 0.0198(8) Uani 1 1 d . . . . .
H11A H 0.402409 0.308717 0.445402 0.030 Uiso 1 1 d R U . . .
H11B H 0.495883 0.336873 0.485646 0.030 Uiso 1 1 d R U . . .
O12 O 0.6125(5) 0.4752(5) 0.38232(14) 0.0187(7) Uani 1 1 d . . . . .
H12A H 0.690190 0.574416 0.382830 0.028 Uiso 1 1 d R U . . .
H12B H 0.526511 0.473865 0.392182 0.028 Uiso 1 1 d R U . . .
O7 O 0.0033(4) 0.1690(5) 0.45258(14) 0.0144(6) Uani 1 1 d . . . . .
O6 O 0.1309(5) 0.4317(5) 0.46126(15) 0.0198(7) Uani 1 1 d . . . . .
O5 O 0.3064(5) 0.4535(4) 0.38515(14) 0.0179(6) Uani 1 1 d . . . . .
C4 C 0.1072(5) 0.3143(6) 0.44125(17) 0.0141(7) Uani 1 1 d . . . . .
O4 O 0.6495(5) 0.5396(4) 0.62241(14) 0.0176(6) Uani 1 1 d . . . . .


_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 O8 1.991(4) . ?
Fe1 O8 1.992(4) 2 ?
Fe1 O8 1.992(4) 3 ?
Fe1 O7 2.027(4) 3 ?
Fe1 O7 2.027(4) 2 ?
Fe1 O7 2.027(4) . ?
Mg1 O12 2.061(5) 2_655 ?
Mg1 O12 2.061(5) 3_665 ?
Mg1 O12 2.061(5) . ?
Mg1 O11 2.072(5) . ?
Mg1 O11 2.072(5) 2_655 ?
Mg1 O11 2.072(5) 3_665 ?
Na1 O6 2.312(4) 3_565 ?
Na1 O6 2.312(4) 2_665 ?
Na1 O6 2.312(5) . ?
Na1 O5 2.431(5) 3_565 ?
Na1 O5 2.431(5) 2_665 ?
Na1 O5 2.431(5) . ?
Na1 C4 3.032(5) 3_565 ?
Na1 C4 3.032(5) . ?
Na1 C4 3.032(5) 2_665 ?
Na1 C3 3.117(5) . ?
Na1 C3 3.117(5) 3_565 ?
Na1 C3 3.117(5) 2_665 ?
O1 C1 1.282(6) . ?
O1 Fe2 2.006(4) . ?
C1 O3 1.232(6) . ?
C1 C2 1.552(6) . ?
C1 Na2 3.066(5) . ?
Na2 O4 2.335(4) 3_665 ?
Na2 O4 2.335(4) 2_655 ?
Na2 O4 2.335(4) . ?
Na2 O3 2.360(5) . ?
Na2 O3 2.360(5) 2_655 ?
Na2 O3 2.360(5) 3_665 ?
Na2 C2 3.048(5) 3_665 ?
Na2 C2 3.048(5) 2_655 ?
Na2 C2 3.048(4) . ?
Fe2 O2 2.018(4) 2_665 ?
Fe2 O2 2.018(4) 3_565 ?
Fe2 O2 2.018(4) . ?
Mg2 O9 2.062(4) . ?
Mg2 O9 2.062(4) 2_765 ?
Mg2 O9 2.062(4) 3_675 ?
Mg2 O10 2.087(5) 2_765 ?
Mg2 O10 2.087(4) 3_675 ?
Mg2 O10 2.088(4) . ?
O2 C2 1.284(6) . ?
C2 O4 1.231(6) . ?
C3 O5 1.239(6) . ?
C3 O8 1.283(6) . ?
C3 C4 1.553(6) . ?
O9 H9A 0.8907 . ?
O9 H9B 0.8900 . ?
O10 H10A 0.8846 . ?
O10 H10B 0.8841 . ?
O11 H11A 0.9106 . ?
O11 H11B 0.9092 . ?
O12 H12A 0.8835 . ?
O12 H12B 0.8838 . ?
O7 C4 1.312(6) . ?
O6 C4 1.208(6) . ?

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
O8 Fe1 O8 97.16(16) . 2 ?
O8 Fe1 O8 97.16(16) . 3 ?
O8 Fe1 O8 97.16(16) 2 3 ?
O8 Fe1 O7 93.08(16) . 3 ?
O8 Fe1 O7 169.75(17) 2 3 ?
O8 Fe1 O7 81.26(16) 3 3 ?
O8 Fe1 O7 169.75(16) . 2 ?
O8 Fe1 O7 81.26(16) 2 2 ?
O8 Fe1 O7 93.09(16) 3 2 ?
O7 Fe1 O7 88.70(17) 3 2 ?
O8 Fe1 O7 81.26(16) . . ?
O8 Fe1 O7 93.08(16) 2 . ?
O8 Fe1 O7 169.75(16) 3 . ?
O7 Fe1 O7 88.70(17) 3 . ?
O7 Fe1 O7 88.70(17) 2 . ?
O12 Mg1 O12 92.2(2) 2_655 3_665 ?
O12 Mg1 O12 92.2(2) 2_655 . ?
O12 Mg1 O12 92.2(2) 3_665 . ?
O12 Mg1 O11 88.58(16) 2_655 . ?
O12 Mg1 O11 178.7(2) 3_665 . ?
O12 Mg1 O11 86.79(17) . . ?
O12 Mg1 O11 86.79(17) 2_655 2_655 ?
O12 Mg1 O11 88.58(16) 3_665 2_655 ?
O12 Mg1 O11 178.7(2) . 2_655 ?
O11 Mg1 O11 92.5(2) . 2_655 ?
O12 Mg1 O11 178.7(2) 2_655 3_665 ?
O12 Mg1 O11 86.79(17) 3_665 3_665 ?
O12 Mg1 O11 88.59(16) . 3_665 ?
O11 Mg1 O11 92.5(2) . 3_665 ?
O11 Mg1 O11 92.5(2) 2_655 3_665 ?
O6 Na1 O6 107.66(15) 3_565 2_665 ?
O6 Na1 O6 107.66(15) 3_565 . ?
O6 Na1 O6 107.66(15) 2_665 . ?
O6 Na1 O5 71.92(14) 3_565 3_565 ?
O6 Na1 O5 160.8(2) 2_665 3_565 ?
O6 Na1 O5 90.29(15) . 3_565 ?
O6 Na1 O5 90.29(15) 3_565 2_665 ?
O6 Na1 O5 71.92(14) 2_665 2_665 ?
O6 Na1 O5 160.8(2) . 2_665 ?
O5 Na1 O5 88.89(18) 3_565 2_665 ?
O6 Na1 O5 160.8(2) 3_565 . ?
O6 Na1 O5 90.29(15) 2_665 . ?
O6 Na1 O5 71.92(14) . . ?
O5 Na1 O5 88.89(18) 3_565 . ?
O5 Na1 O5 88.89(18) 2_665 . ?
O6 Na1 C4 21.13(13) 3_565 3_565 ?
O6 Na1 C4 127.55(17) 2_665 3_565 ?
O6 Na1 C4 103.71(15) . 3_565 ?
O5 Na1 C4 50.81(13) 3_565 3_565 ?
O5 Na1 C4 90.55(14) 2_665 3_565 ?
O5 Na1 C4 139.69(19) . 3_565 ?
O6 Na1 C4 127.55(17) 3_565 . ?
O6 Na1 C4 103.71(15) 2_665 . ?
O6 Na1 C4 21.13(13) . . ?
O5 Na1 C4 90.55(14) 3_565 . ?
O5 Na1 C4 139.69(19) 2_665 . ?
O5 Na1 C4 50.81(13) . . ?
C4 Na1 C4 119.38(4) 3_565 . ?
O6 Na1 C4 103.72(15) 3_565 2_665 ?
O6 Na1 C4 21.13(13) 2_665 2_665 ?
O6 Na1 C4 127.55(16) . 2_665 ?
O5 Na1 C4 139.69(19) 3_565 2_665 ?
O5 Na1 C4 50.81(13) 2_665 2_665 ?
O5 Na1 C4 90.55(14) . 2_665 ?
C4 Na1 C4 119.38(4) 3_565 2_665 ?
C4 Na1 C4 119.38(4) . 2_665 ?
O6 Na1 C3 151.98(14) 3_565 . ?
O6 Na1 C3 96.87(14) 2_665 . ?
O6 Na1 C3 50.33(13) . . ?
O5 Na1 C3 89.33(16) 3_565 . ?
O5 Na1 C3 110.48(18) 2_665 . ?
O5 Na1 C3 21.59(13) . . ?
C4 Na1 C3 135.28(13) 3_565 . ?
C4 Na1 C3 29.22(11) . . ?
C4 Na1 C3 104.01(12) 2_665 . ?
O6 Na1 C3 50.33(13) 3_565 3_565 ?
O6 Na1 C3 151.98(14) 2_665 3_565 ?
O6 Na1 C3 96.87(14) . 3_565 ?
O5 Na1 C3 21.59(13) 3_565 3_565 ?
O5 Na1 C3 89.33(15) 2_665 3_565 ?
O5 Na1 C3 110.48(18) . 3_565 ?
C4 Na1 C3 29.22(11) 3_565 3_565 ?
C4 Na1 C3 104.01(12) . 3_565 ?
C4 Na1 C3 135.28(13) 2_665 3_565 ?
C3 Na1 C3 109.36(12) . 3_565 ?
O6 Na1 C3 96.87(14) 3_565 2_665 ?
O6 Na1 C3 50.33(13) 2_665 2_665 ?
O6 Na1 C3 151.98(13) . 2_665 ?
O5 Na1 C3 110.48(18) 3_565 2_665 ?
O5 Na1 C3 21.59(13) 2_665 2_665 ?
O5 Na1 C3 89.33(16) . 2_665 ?
C4 Na1 C3 104.01(12) 3_565 2_665 ?
C4 Na1 C3 135.28(13) . 2_665 ?
C4 Na1 C3 29.22(11) 2_665 2_665 ?
C3 Na1 C3 109.36(12) . 2_665 ?
C3 Na1 C3 109.36(12) 3_565 2_665 ?
C1 O1 Fe2 114.8(3) . . ?
O3 C1 O1 126.3(5) . . ?
O3 C1 C2 119.3(4) . . ?
O1 C1 C2 114.4(4) . . ?
O3 C1 Na2 44.9(3) . . ?
O1 C1 Na2 169.4(3) . . ?
C2 C1 Na2 74.7(2) . . ?
O4 Na2 O4 102.67(19) 3_665 2_655 ?
O4 Na2 O4 102.67(19) 3_665 . ?
O4 Na2 O4 102.67(19) 2_655 . ?
O4 Na2 O3 165.64(18) 3_665 . ?
O4 Na2 O3 91.59(15) 2_655 . ?
O4 Na2 O3 72.10(14) . . ?
O4 Na2 O3 91.59(15) 3_665 2_655 ?
O4 Na2 O3 72.10(14) 2_655 2_655 ?
O4 Na2 O3 165.64(18) . 2_655 ?
O3 Na2 O3 94.4(2) . 2_655 ?
O4 Na2 O3 72.10(14) 3_665 3_665 ?
O4 Na2 O3 165.64(17) 2_655 3_665 ?
O4 Na2 O3 91.59(15) . 3_665 ?
O3 Na2 O3 94.4(2) . 3_665 ?
O3 Na2 O3 94.4(2) 2_655 3_665 ?
O4 Na2 C2 21.67(13) 3_665 3_665 ?
O4 Na2 C2 124.3(2) 2_655 3_665 ?
O4 Na2 C2 96.71(15) . 3_665 ?
O3 Na2 C2 144.08(19) . 3_665 ?
O3 Na2 C2 97.20(15) 2_655 3_665 ?
O3 Na2 C2 50.95(14) 3_665 3_665 ?
O4 Na2 C2 96.71(15) 3_665 2_655 ?
O4 Na2 C2 21.67(13) 2_655 2_655 ?
O4 Na2 C2 124.3(2) . 2_655 ?
O3 Na2 C2 97.20(15) . 2_655 ?
O3 Na2 C2 50.95(14) 2_655 2_655 ?
O3 Na2 C2 144.08(19) 3_665 2_655 ?
C2 Na2 C2 116.42(9) 3_665 2_655 ?
O4 Na2 C2 124.3(2) 3_665 . ?
O4 Na2 C2 96.71(15) 2_655 . ?
O4 Na2 C2 21.68(13) . . ?
O3 Na2 C2 50.95(14) . . ?
O3 Na2 C2 144.08(19) 2_655 . ?
O3 Na2 C2 97.20(15) 3_665 . ?
C2 Na2 C2 116.42(9) 3_665 . ?
C2 Na2 C2 116.42(9) 2_655 . ?
O4 Na2 C1 152.30(16) 3_665 . ?
O4 Na2 C1 92.52(14) 2_655 . ?
O4 Na2 C1 50.84(13) . . ?
O3 Na2 C1 21.65(13) . . ?
O3 Na2 C1 115.27(19) 2_655 . ?
O3 Na2 C1 97.87(17) 3_665 . ?
C2 Na2 C1 137.62(12) 3_665 . ?
C2 Na2 C1 105.33(12) 2_655 . ?
C2 Na2 C1 29.40(11) . . ?
O4 Na2 C1 92.52(14) 3_665 2_655 ?
O4 Na2 C1 50.84(13) 2_655 2_655 ?
O4 Na2 C1 152.30(16) . 2_655 ?
O3 Na2 C1 97.87(17) . 2_655 ?
O3 Na2 C1 21.65(13) 2_655 2_655 ?
O3 Na2 C1 115.27(19) 3_665 2_655 ?
C2 Na2 C1 105.33(12) 3_665 2_655 ?
C2 Na2 C1 29.40(11) 2_655 2_655 ?
C2 Na2 C1 137.62(12) . 2_655 ?
C1 Na2 C1 114.89(10) . 2_655 ?
O4 Na2 C1 50.84(13) 3_665 3_665 ?
O4 Na2 C1 152.30(16) 2_655 3_665 ?
O4 Na2 C1 92.52(14) . 3_665 ?
O3 Na2 C1 115.27(19) . 3_665 ?
O3 Na2 C1 97.87(17) 2_655 3_665 ?
O3 Na2 C1 21.65(13) 3_665 3_665 ?
C2 Na2 C1 29.40(11) 3_665 3_665 ?
C2 Na2 C1 137.62(11) 2_655 3_665 ?
C2 Na2 C1 105.33(12) . 3_665 ?
C1 Na2 C1 114.89(10) . 3_665 ?
C1 Na2 C1 114.89(10) 2_655 3_665 ?
O1 Fe2 O1 94.61(17) . 2_665 ?
O1 Fe2 O1 94.61(17) . 3_565 ?
O1 Fe2 O1 94.60(17) 2_665 3_565 ?
O1 Fe2 O2 171.38(17) . 2_665 ?
O1 Fe2 O2 81.19(16) 2_665 2_665 ?
O1 Fe2 O2 93.23(16) 3_565 2_665 ?
O1 Fe2 O2 93.23(17) . 3_565 ?
O1 Fe2 O2 171.38(17) 2_665 3_565 ?
O1 Fe2 O2 81.19(16) 3_565 3_565 ?
O2 Fe2 O2 91.49(17) 2_665 3_565 ?
O1 Fe2 O2 81.19(15) . . ?
O1 Fe2 O2 93.23(17) 2_665 . ?
O1 Fe2 O2 171.38(17) 3_565 . ?
O2 Fe2 O2 91.49(17) 2_665 . ?
O2 Fe2 O2 91.49(17) 3_565 . ?
O9 Mg2 O9 92.7(2) . 2_765 ?
O9 Mg2 O9 92.7(2) . 3_675 ?
O9 Mg2 O9 92.7(2) 2_765 3_675 ?
O9 Mg2 O10 89.94(16) . 2_765 ?
O9 Mg2 O10 177.3(2) 2_765 2_765 ?
O9 Mg2 O10 87.95(16) 3_675 2_765 ?
O9 Mg2 O10 87.95(15) . 3_675 ?
O9 Mg2 O10 89.94(16) 2_765 3_675 ?
O9 Mg2 O10 177.3(2) 3_675 3_675 ?
O10 Mg2 O10 89.4(2) 2_765 3_675 ?
O9 Mg2 O10 177.3(2) . . ?
O9 Mg2 O10 87.95(15) 2_765 . ?
O9 Mg2 O10 89.94(16) 3_675 . ?
O10 Mg2 O10 89.4(2) 2_765 . ?
O10 Mg2 O10 89.4(2) 3_675 . ?
C2 O2 Fe2 114.0(3) . . ?
O4 C2 O2 125.6(5) . . ?
O4 C2 C1 119.6(4) . . ?
O2 C2 C1 114.7(4) . . ?
O4 C2 Na2 44.5(3) . . ?
O2 C2 Na2 167.0(4) . . ?
C1 C2 Na2 75.9(2) . . ?
C1 O3 Na2 113.4(3) . . ?
O5 C3 O8 125.7(5) . . ?
O5 C3 C4 118.6(4) . . ?
O8 C3 C4 115.7(4) . . ?
O5 C3 Na1 46.2(3) . . ?
O8 C3 Na1 171.9(4) . . ?
C4 C3 Na1 72.3(3) . . ?
C3 O8 Fe1 115.2(3) . . ?
Mg2 O9 H9A 111.8 . . ?
Mg2 O9 H9B 111.9 . . ?
H9A O9 H9B 107.0 . . ?
Mg2 O10 H10A 111.6 . . ?
Mg2 O10 H10B 111.4 . . ?
H10A O10 H10B 107.3 . . ?
Mg1 O11 H11A 113.8 . . ?
Mg1 O11 H11B 112.9 . . ?
H11A O11 H11B 105.4 . . ?
Mg1 O12 H12A 111.1 . . ?
Mg1 O12 H12B 111.6 . . ?
H12A O12 H12B 107.5 . . ?
C4 O7 Fe1 114.8(3) . . ?
C4 O6 Na1 115.3(3) . . ?
C3 O5 Na1 112.2(3) . . ?
O6 C4 O7 125.3(5) . . ?
O6 C4 C3 122.0(4) . . ?
O7 C4 C3 112.7(4) . . ?
O6 C4 Na1 43.6(3) . . ?
O7 C4 Na1 168.7(4) . . ?
C3 C4 Na1 78.4(3) . . ?
C2 O4 Na2 113.8(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe2 O1 C1 O3 -174.9(4) . . . . ?
Fe2 O1 C1 C2 5.2(5) . . . . ?
Fe2 O1 C1 Na2 152.9(18) . . . . ?
Fe2 O2 C2 O4 171.1(4) . . . . ?
Fe2 O2 C2 C1 -8.1(5) . . . . ?
Fe2 O2 C2 Na2 -151.8(13) . . . . ?
O3 C1 C2 O4 2.8(7) . . . . ?
O1 C1 C2 O4 -177.2(5) . . . . ?
Na2 C1 C2 O4 8.7(4) . . . . ?
O3 C1 C2 O2 -177.9(5) . . . . ?
O1 C1 C2 O2 2.0(6) . . . . ?
Na2 C1 C2 O2 -172.1(4) . . . . ?
O3 C1 C2 Na2 -5.8(4) . . . . ?
O1 C1 C2 Na2 174.1(4) . . . . ?
O1 C1 O3 Na2 -172.0(4) . . . . ?
C2 C1 O3 Na2 7.9(6) . . . . ?
O5 C3 O8 Fe1 173.5(4) . . . . ?
C4 C3 O8 Fe1 -6.4(5) . . . . ?
O8 C3 O5 Na1 179.1(4) . . . . ?
C4 C3 O5 Na1 -1.1(5) . . . . ?
Na1 O6 C4 O7 176.9(4) . . . . ?
Na1 O6 C4 C3 -3.4(6) . . . . ?
Fe1 O7 C4 O6 -178.2(4) . . . . ?
Fe1 O7 C4 C3 2.1(5) . . . . ?
Fe1 O7 C4 Na1 -167.1(15) . . . . ?
O5 C3 C4 O6 3.2(7) . . . . ?
O8 C3 C4 O6 -176.9(5) . . . . ?
Na1 C3 C4 O6 2.4(4) . . . . ?
O5 C3 C4 O7 -177.0(5) . . . . ?
O8 C3 C4 O7 2.8(6) . . . . ?
Na1 C3 C4 O7 -177.8(4) . . . . ?
O5 C3 C4 Na1 0.8(4) . . . . ?
O8 C3 C4 Na1 -179.3(4) . . . . ?
O2 C2 O4 Na2 168.9(4) . . . . ?
C1 C2 O4 Na2 -12.0(6) . . . . ?

_refine_diff_density_max         3.617
_refine_diff_density_min         -1.649
_refine_diff_density_rms         0.176

####################################################################### 
# 
# 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_StepII_dehydr
_database_code_depnum_ccdc_archive 'CCDC 1868685'
loop_
_audit_author_name
_audit_author_address
'Igor Huskic'
;McGill University
Canada
;
_audit_update_record             
;
2018-09-19 deposited with the CCDC.	2019-04-01 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT112_StepII_dehydr       
;
PROBLEM: ADDSYM Detects New (Pseudo) Symm. Elem         c        100 %Fit
RESPONSE: Refinement in the centrosymmetric P-3 resulted in a higher Rwp value than refinement in P3.
;
_vrf_PLAT112_StepII_dehydr_2     
;
PROBLEM: ADDSYM Detects New (Pseudo) Symm. Elem         c        100 %Fit
RESPONSE: Refinement in the centrosymmetric P-3 resulted in a higher Rwp value than refinement in P3.
;
_vrf_PLAT112_StepII_dehydr_3     
;
PROBLEM: ADDSYM Detects New (Pseudo) Symm. Elem         c        100 %Fit
RESPONSE: Refinement in the centrosymmetric P-3 resulted in a higher Rwp value than refinement in P3.
;
_vrf_PLAT341_StepII_dehydr       
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............       0.02 Ang.
RESPONSE: Result of low quality data due to thermal stress on the crystal upon dehydration
;
_vrf_PLAT420_StepII_dehydr       
;
PROBLEM: D-H Without Acceptor       O10      --H10B     .     Please Check
RESPONSE: The hydrogens belonging to water molecules were located from the electron density map and their positions were allowed to refine with gentle restraints.
;
_vrf_PLAT420_StepII_dehydr_2     
;
PROBLEM: D-H Without Acceptor       O11      --H11B     .     Please Check
RESPONSE: The hydrogens belonging to water molecules were located from the electron density map and their positions were allowed to refine with gentle restraints.
;
_vrf_PLAT420_StepII_dehydr_3     
;
PROBLEM: D-H Without Acceptor       O12      --H12B     .     Please Check
RESPONSE: The hydrogens belonging to water molecules were located from the electron density map and their positions were allowed to refine with gentle restraints.
;
# Added during the CSD deposition process: Wednesday 19 September 2018 05:00 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        
'Sodium magnesium iron(III) oxalate hexahydrate'
_chemical_name_common            ?
_chemical_formula_moiety         'Na Fe C6 O12 2-, Mg H12 O6 2+ '
_chemical_formula_sum            'C6 H12 Fe Mg Na O18'
_chemical_compound_source        synthetic
_chemical_properties_physical    
'hygroscopic, , photo-sensitive, moisture-sensitive,Moisture-sensitive,Hygroscopic,Light-sensitive'
_exptl_crystal_recrystallization_method dehydrated
_chemical_melting_point          ?

_exptl_crystal_description       'hexagonal prism'
_exptl_crystal_colour            green
_diffrn_ambient_temperature      293(2)
_diffrn_ambient_pressure         101325
_chemical_formula_weight         475.30

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'
Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           143
_space_group_name_H-M_alt        'P 3'
_space_group_name_Hall           'P 3'
_chemical_absolute_configuration .

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'

_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.
;

_cell_length_a                   9.7560(8)
_cell_length_b                   9.7560(8)
_cell_length_c                   10.117(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     833.9(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    18866
_cell_measurement_theta_min      4.980
_cell_measurement_theta_max      52.475
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.893
_exptl_crystal_F_000             482
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_absorpt_coefficient_mu    1.063
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5448
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'SADABS-2012/1, G. Sheldrick'
_exptl_absorpt_special_details   ?
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Bruker D8'
_diffrn_measurement_device_type  'Bruker PHOTON 100 CMOS'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9881
_diffrn_reflns_av_unetI/netI     0.0428
_diffrn_reflns_av_R_equivalents  0.0488
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.411
_diffrn_reflns_theta_max         27.455
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             2500
_reflns_number_gt                2289
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_max     0.991
_reflns_Friedel_fraction_full    0.989

_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'APEX 2, Bruker-AXS'
_computing_cell_refinement       'SAINT V8.35A, Bruker-AXS'
_computing_data_reduction        'SAINT V8.35A, Bruker-AXS'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          'Refined as a 4-component inversion twin.,Twin'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0570P)²+2.3795P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Twinning involves inversion, so Flack parameter cannot be determined
;
_refine_ls_abs_structure_Flack   ?
_refine_ls_number_reflns         2500
_refine_ls_number_parameters     170
_refine_ls_number_restraints     50
_refine_ls_R_factor_all          0.0669
_refine_ls_R_factor_gt           0.0576
_refine_ls_wR_factor_ref         0.1475
_refine_ls_wR_factor_gt          0.1382
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_restrained_S_all      1.143
_refine_ls_shift/su_max          0.001
_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 0.333333 0.666667 0.2550(5) 0.0211(6) Uani 1 3 d S T P . .
O1 O 0.1719(14) 0.1615(15) 0.8399(13) 0.050(3) Uani 1 1 d . . . . .
Mg1 Mg 0.666667 0.333333 0.2470(16) 0.0202(12) Uani 1 3 d S T P . .
Na1 Na 0.000000 0.000000 0.2191(7) 0.0123(14) Uani 1 3 d S TU P . .
C1 C 0.311(2) 0.1947(19) 0.8049(16) 0.036(4) Uani 1 1 d . . . . .
C2 C 0.323(2) 0.113(2) 0.6782(17) 0.038(4) Uani 1 1 d . U . . .
Fe2 Fe 0.000000 0.000000 0.7311(6) 0.0423(14) Uani 1 3 d S T P . .
Mg2 Mg 0.333333 0.666667 0.7427(14) 0.0361(16) Uani 1 3 d S TU P . .
Na2 Na 0.666667 0.333333 0.745(4) 0.061(4) Uani 1 3 d S T P . .
O2 O 0.1829(12) 0.0209(15) 0.6270(11) 0.042(3) Uani 1 1 d . . . . .
O3 O 0.4347(15) 0.2785(17) 0.8636(17) 0.052(4) Uani 1 1 d . . . . .
C3 C 0.2131(15) 0.3453(16) 0.3094(13) 0.019(2) Uani 1 1 d . U . . .
O4 O 0.4527(16) 0.1434(17) 0.6347(15) 0.041(3) Uani 1 1 d . . . . .
C4 C 0.1275(16) 0.3488(18) 0.1795(15) 0.023(3) Uani 1 1 d . . . . .
O6 O 0.0314(13) 0.2282(13) 0.1246(11) 0.036(2) Uani 1 1 d . U . . .
O5 O 0.1921(14) 0.2122(14) 0.3465(12) 0.038(3) Uani 1 1 d . U . . .
O12 O 0.4709(10) 0.1899(11) 0.3588(11) 0.032(2) Uani 1 1 d . . . . .
H12A H 0.487141 0.226011 0.451220 0.048 Uiso 1 1 d DR U . . .
H12B H 0.450809 0.080585 0.358784 0.048 Uiso 1 1 d DR U . . .
O11 O 0.5194(10) 0.3819(10) 0.1252(10) 0.030(2) Uani 1 1 d . . . . .
H11A H 0.527429 0.485435 0.148583 0.045 Uiso 1 1 d DR U . . .
H11B H 0.405532 0.299436 0.136063 0.045 Uiso 1 1 d DR U . . .
O10 O 0.5326(15) 0.7257(15) 0.8603(19) 0.063(4) Uani 1 1 d D . . . .
H10A H 0.633796 0.808189 0.818056 0.095 Uiso 1 1 d DR U . . .
H10B H 0.545878 0.631389 0.874803 0.095 Uiso 1 1 d DR U . . .
O9 O 0.3860(14) 0.5233(14) 0.6330(16) 0.054(3) Uani 1 1 d D . . . .
H9A H 0.300934 0.455085 0.558347 0.081 Uiso 1 1 d DR U . . .
H9B H 0.394925 0.433849 0.686961 0.081 Uiso 1 1 d DR U . . .
O8 O 0.3012(11) 0.4782(11) 0.3663(9) 0.020(2) Uani 1 1 d . U . . .
O7 O 0.1648(11) 0.4906(12) 0.1443(8) 0.024(2) Uani 1 1 d . . . . .


_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 O7 2.021(10) . ?
Fe1 O7 2.021(10) 3_565 ?
Fe1 O7 2.021(10) 2_665 ?
Fe1 O8 2.042(9) 3_565 ?
Fe1 O8 2.042(9) 2_665 ?
Fe1 O8 2.042(9) . ?
O1 C1 1.28(2) . ?
O1 Fe2 1.966(12) . ?
Mg1 O12 2.053(13) 2_655 ?
Mg1 O12 2.053(13) 3_665 ?
Mg1 O12 2.053(13) . ?
Mg1 O11 2.118(14) . ?
Mg1 O11 2.118(14) 2_655 ?
Mg1 O11 2.118(14) 3_665 ?
Na1 O6 2.298(11) 2 ?
Na1 O6 2.298(11) 3 ?
Na1 O6 2.298(11) . ?
Na1 O5 2.362(13) . ?
Na1 O5 2.362(13) 3 ?
Na1 O5 2.362(13) 2 ?
Na1 C4 3.009(15) 2 ?
Na1 C4 3.009(15) 3 ?
Na1 C4 3.009(15) . ?
Na1 C3 3.083(14) 2 ?
Na1 C3 3.083(14) . ?
Na1 C3 3.083(14) 3 ?
C1 O3 1.22(2) . ?
C1 C2 1.54(2) . ?
C1 Na2 3.088(18) . ?
C2 O4 1.23(2) . ?
C2 O2 1.31(2) . ?
C2 Na2 3.02(2) . ?
Fe2 O2 1.993(10) . ?
Fe2 O2 1.993(11) 3 ?
Fe2 O2 1.993(10) 2 ?
Mg2 O9 2.043(15) . ?
Mg2 O9 2.043(15) 3_565 ?
Mg2 O9 2.043(15) 2_665 ?
Mg2 O10 2.099(17) 2_665 ?
Mg2 O10 2.099(17) 3_565 ?
Mg2 O10 2.099(17) . ?
Na2 O4 2.27(2) 2_655 ?
Na2 O4 2.27(2) 3_665 ?
Na2 O4 2.27(2) . ?
Na2 O3 2.37(2) . ?
Na2 O3 2.37(2) 2_655 ?
Na2 O3 2.37(2) 3_665 ?
C3 O5 1.266(17) . ?
C3 O8 1.279(17) . ?
C3 C4 1.566(14) . ?
C4 O6 1.212(19) . ?
C4 O7 1.292(18) . ?
O12 H12A 0.9834 . ?
O12 H12B 0.9833 . ?
O11 H11A 1.0013 . ?
O11 H11B 1.0002 . ?
O10 H10A 1.0056 . ?
O10 H10B 1.0019 . ?
O9 H9A 1.0719 . ?
O9 H9B 1.0692 . ?

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
O7 Fe1 O7 92.2(4) . 3_565 ?
O7 Fe1 O7 92.2(4) . 2_665 ?
O7 Fe1 O7 92.2(4) 3_565 2_665 ?
O7 Fe1 O8 94.8(3) . 3_565 ?
O7 Fe1 O8 81.2(3) 3_565 3_565 ?
O7 Fe1 O8 170.6(3) 2_665 3_565 ?
O7 Fe1 O8 170.6(3) . 2_665 ?
O7 Fe1 O8 94.8(3) 3_565 2_665 ?
O7 Fe1 O8 81.2(3) 2_665 2_665 ?
O8 Fe1 O8 92.5(4) 3_565 2_665 ?
O7 Fe1 O8 81.2(3) . . ?
O7 Fe1 O8 170.6(3) 3_565 . ?
O7 Fe1 O8 94.8(3) 2_665 . ?
O8 Fe1 O8 92.5(4) 3_565 . ?
O8 Fe1 O8 92.5(4) 2_665 . ?
C1 O1 Fe2 114.9(10) . . ?
O12 Mg1 O12 92.5(7) 2_655 3_665 ?
O12 Mg1 O12 92.5(7) 2_655 . ?
O12 Mg1 O12 92.5(7) 3_665 . ?
O12 Mg1 O11 177.7(9) 2_655 . ?
O12 Mg1 O11 89.6(4) 3_665 . ?
O12 Mg1 O11 88.2(4) . . ?
O12 Mg1 O11 88.2(4) 2_655 2_655 ?
O12 Mg1 O11 177.7(9) 3_665 2_655 ?
O12 Mg1 O11 89.6(4) . 2_655 ?
O11 Mg1 O11 89.6(7) . 2_655 ?
O12 Mg1 O11 89.6(4) 2_655 3_665 ?
O12 Mg1 O11 88.2(4) 3_665 3_665 ?
O12 Mg1 O11 177.7(9) . 3_665 ?
O11 Mg1 O11 89.6(7) . 3_665 ?
O11 Mg1 O11 89.6(7) 2_655 3_665 ?
O6 Na1 O6 103.9(4) 2 3 ?
O6 Na1 O6 103.9(4) 2 . ?
O6 Na1 O6 103.9(4) 3 . ?
O6 Na1 O5 166.4(4) 2 . ?
O6 Na1 O5 89.7(3) 3 . ?
O6 Na1 O5 73.4(3) . . ?
O6 Na1 O5 89.7(3) 2 3 ?
O6 Na1 O5 73.4(3) 3 3 ?
O6 Na1 O5 166.4(4) . 3 ?
O5 Na1 O5 93.1(4) . 3 ?
O6 Na1 O5 73.4(3) 2 2 ?
O6 Na1 O5 166.4(4) 3 2 ?
O6 Na1 O5 89.7(3) . 2 ?
O5 Na1 O5 93.1(4) . 2 ?
O5 Na1 O5 93.1(4) 3 2 ?
O6 Na1 C4 21.5(4) 2 2 ?
O6 Na1 C4 124.7(4) 3 2 ?
O6 Na1 C4 101.2(4) . 2 ?
O5 Na1 C4 144.9(5) . 2 ?
O5 Na1 C4 90.9(4) 3 2 ?
O5 Na1 C4 51.9(4) 2 2 ?
O6 Na1 C4 101.2(4) 2 3 ?
O6 Na1 C4 21.5(4) 3 3 ?
O6 Na1 C4 124.7(4) . 3 ?
O5 Na1 C4 90.9(4) . 3 ?
O5 Na1 C4 51.9(4) 3 3 ?
O5 Na1 C4 144.9(5) 2 3 ?
C4 Na1 C4 118.26(14) 2 3 ?
O6 Na1 C4 124.7(4) 2 . ?
O6 Na1 C4 101.2(4) 3 . ?
O6 Na1 C4 21.5(4) . . ?
O5 Na1 C4 51.9(4) . . ?
O5 Na1 C4 144.9(5) 3 . ?
O5 Na1 C4 90.9(4) 2 . ?
C4 Na1 C4 118.26(14) 2 . ?
C4 Na1 C4 118.26(14) 3 . ?
O6 Na1 C3 51.3(4) 2 2 ?
O6 Na1 C3 151.5(4) 3 2 ?
O6 Na1 C3 96.7(4) . 2 ?
O5 Na1 C3 115.3(4) . 2 ?
O5 Na1 C3 90.8(4) 3 2 ?
O5 Na1 C3 22.2(4) 2 2 ?
C4 Na1 C3 29.8(3) 2 2 ?
C4 Na1 C3 136.6(2) 3 2 ?
C4 Na1 C3 105.1(2) . 2 ?
O6 Na1 C3 151.5(4) 2 . ?
O6 Na1 C3 96.7(4) 3 . ?
O6 Na1 C3 51.3(4) . . ?
O5 Na1 C3 22.2(4) . . ?
O5 Na1 C3 115.3(4) 3 . ?
O5 Na1 C3 90.8(4) 2 . ?
C4 Na1 C3 136.6(2) 2 . ?
C4 Na1 C3 105.1(2) 3 . ?
C4 Na1 C3 29.8(3) . . ?
C3 Na1 C3 111.6(3) 2 . ?
O6 Na1 C3 96.7(4) 2 3 ?
O6 Na1 C3 51.3(4) 3 3 ?
O6 Na1 C3 151.5(4) . 3 ?
O5 Na1 C3 90.8(4) . 3 ?
O5 Na1 C3 22.2(4) 3 3 ?
O5 Na1 C3 115.3(4) 2 3 ?
C4 Na1 C3 105.1(2) 2 3 ?
C4 Na1 C3 29.8(3) 3 3 ?
C4 Na1 C3 136.6(2) . 3 ?
C3 Na1 C3 111.6(3) 2 3 ?
C3 Na1 C3 111.6(3) . 3 ?
O3 C1 O1 127.1(16) . . ?
O3 C1 C2 116.6(18) . . ?
O1 C1 C2 116.2(16) . . ?
O3 C1 Na2 44.3(11) . . ?
O1 C1 Na2 169.6(11) . . ?
C2 C1 Na2 73.0(13) . . ?
O4 C2 O2 128.2(17) . . ?
O4 C2 C1 120.4(19) . . ?
O2 C2 C1 111.4(17) . . ?
O4 C2 Na2 42.6(11) . . ?
O2 C2 Na2 169.5(13) . . ?
C1 C2 Na2 77.8(12) . . ?
O1 Fe2 O1 91.7(6) . 2 ?
O1 Fe2 O1 91.7(6) . 3 ?
O1 Fe2 O1 91.7(6) 2 3 ?
O1 Fe2 O2 81.5(4) . . ?
O1 Fe2 O2 172.1(5) 2 . ?
O1 Fe2 O2 92.6(5) 3 . ?
O1 Fe2 O2 172.1(5) . 3 ?
O1 Fe2 O2 92.6(5) 2 3 ?
O1 Fe2 O2 81.5(4) 3 3 ?
O2 Fe2 O2 94.6(5) . 3 ?
O1 Fe2 O2 92.6(5) . 2 ?
O1 Fe2 O2 81.5(4) 2 2 ?
O1 Fe2 O2 172.1(5) 3 2 ?
O2 Fe2 O2 94.6(5) . 2 ?
O2 Fe2 O2 94.6(5) 3 2 ?
O9 Mg2 O9 93.3(8) . 3_565 ?
O9 Mg2 O9 93.3(8) . 2_665 ?
O9 Mg2 O9 93.3(8) 3_565 2_665 ?
O9 Mg2 O10 177.8(9) . 2_665 ?
O9 Mg2 O10 86.8(5) 3_565 2_665 ?
O9 Mg2 O10 88.9(5) 2_665 2_665 ?
O9 Mg2 O10 86.8(5) . 3_565 ?
O9 Mg2 O10 88.9(5) 3_565 3_565 ?
O9 Mg2 O10 177.8(9) 2_665 3_565 ?
O10 Mg2 O10 91.0(8) 2_665 3_565 ?
O9 Mg2 O10 88.9(5) . . ?
O9 Mg2 O10 177.8(9) 3_565 . ?
O9 Mg2 O10 86.8(5) 2_665 . ?
O10 Mg2 O10 91.0(8) 2_665 . ?
O10 Mg2 O10 91.0(8) 3_565 . ?
O4 Na2 O4 98.0(11) 2_655 3_665 ?
O4 Na2 O4 98.0(11) 2_655 . ?
O4 Na2 O4 98.0(11) 3_665 . ?
O4 Na2 O3 163.5(4) 2_655 . ?
O4 Na2 O3 96.0(4) 3_665 . ?
O4 Na2 O3 71.4(3) . . ?
O4 Na2 O3 71.4(3) 2_655 2_655 ?
O4 Na2 O3 163.5(4) 3_665 2_655 ?
O4 Na2 O3 96.0(4) . 2_655 ?
O3 Na2 O3 96.7(11) . 2_655 ?
O4 Na2 O3 96.0(4) 2_655 3_665 ?
O4 Na2 O3 71.4(3) 3_665 3_665 ?
O4 Na2 O3 163.5(4) . 3_665 ?
O3 Na2 O3 96.7(11) . 3_665 ?
O3 Na2 O3 96.7(11) 2_655 3_665 ?
O4 Na2 C2 119.3(10) 2_655 . ?
O4 Na2 C2 96.4(8) 3_665 . ?
O4 Na2 C2 21.5(4) . . ?
O3 Na2 C2 50.1(5) . . ?
O3 Na2 C2 99.8(5) 2_655 . ?
O3 Na2 C2 144.2(8) 3_665 . ?
O4 Na2 C2 21.5(4) 2_655 2_655 ?
O4 Na2 C2 119.3(10) 3_665 2_655 ?
O4 Na2 C2 96.4(8) . 2_655 ?
O3 Na2 C2 144.2(8) . 2_655 ?
O3 Na2 C2 50.1(5) 2_655 2_655 ?
O3 Na2 C2 99.8(5) 3_665 2_655 ?
C2 Na2 C2 115.1(5) . 2_655 ?
O4 Na2 C2 96.4(8) 2_655 3_665 ?
O4 Na2 C2 21.5(4) 3_665 3_665 ?
O4 Na2 C2 119.3(10) . 3_665 ?
O3 Na2 C2 99.8(5) . 3_665 ?
O3 Na2 C2 144.2(8) 2_655 3_665 ?
O3 Na2 C2 50.1(5) 3_665 3_665 ?
C2 Na2 C2 115.1(5) . 3_665 ?
C2 Na2 C2 115.1(5) 2_655 3_665 ?
O4 Na2 C1 147.8(9) 2_655 . ?
O4 Na2 C1 94.4(5) 3_665 . ?
O4 Na2 C1 50.7(4) . . ?
O3 Na2 C1 21.1(4) . . ?
O3 Na2 C1 101.2(8) 2_655 . ?
O3 Na2 C1 116.2(10) 3_665 . ?
C2 Na2 C1 29.2(4) . . ?
C2 Na2 C1 137.4(3) 2_655 . ?
C2 Na2 C1 105.5(3) 3_665 . ?
O4 Na2 C1 50.7(4) 2_655 2_655 ?
O4 Na2 C1 147.8(9) 3_665 2_655 ?
O4 Na2 C1 94.4(5) . 2_655 ?
O3 Na2 C1 116.2(10) . 2_655 ?
O3 Na2 C1 21.1(4) 2_655 2_655 ?
O3 Na2 C1 101.2(8) 3_665 2_655 ?
C2 Na2 C1 105.5(3) . 2_655 ?
C2 Na2 C1 29.2(4) 2_655 2_655 ?
C2 Na2 C1 137.4(3) 3_665 2_655 ?
C1 Na2 C1 116.3(5) . 2_655 ?
O4 Na2 C1 94.4(5) 2_655 3_665 ?
O4 Na2 C1 50.7(4) 3_665 3_665 ?
O4 Na2 C1 147.8(9) . 3_665 ?
O3 Na2 C1 101.2(8) . 3_665 ?
O3 Na2 C1 116.2(10) 2_655 3_665 ?
O3 Na2 C1 21.1(4) 3_665 3_665 ?
C2 Na2 C1 137.4(3) . 3_665 ?
C2 Na2 C1 105.5(3) 2_655 3_665 ?
C2 Na2 C1 29.2(4) 3_665 3_665 ?
C1 Na2 C1 116.2(5) . 3_665 ?
C1 Na2 C1 116.3(5) 2_655 3_665 ?
C2 O2 Fe2 115.7(11) . . ?
C1 O3 Na2 114.6(14) . . ?
O5 C3 O8 126.0(12) . . ?
O5 C3 C4 117.1(14) . . ?
O8 C3 C4 116.8(13) . . ?
O5 C3 Na1 44.9(7) . . ?
O8 C3 Na1 170.1(9) . . ?
C4 C3 Na1 72.5(9) . . ?
C2 O4 Na2 115.9(13) . . ?
O6 C4 O7 125.4(14) . . ?
O6 C4 C3 121.7(15) . . ?
O7 C4 C3 112.8(13) . . ?
O6 C4 Na1 44.0(8) . . ?
O7 C4 Na1 169.5(10) . . ?
C3 C4 Na1 77.7(9) . . ?
C4 O6 Na1 114.4(10) . . ?
C3 O5 Na1 112.8(9) . . ?
Mg1 O12 H12A 110.5 . . ?
Mg1 O12 H12B 110.6 . . ?
H12A O12 H12B 107.3 . . ?
Mg1 O11 H11A 111.6 . . ?
Mg1 O11 H11B 111.2 . . ?
H11A O11 H11B 106.3 . . ?
Mg2 O10 H10A 112.5 . . ?
Mg2 O10 H10B 111.0 . . ?
H10A O10 H10B 105.7 . . ?
Mg2 O9 H9A 115.2 . . ?
Mg2 O9 H9B 115.6 . . ?
H9A O9 H9B 102.0 . . ?
C3 O8 Fe1 112.8(8) . . ?
C4 O7 Fe1 115.5(9) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe2 O1 C1 O3 -172.3(16) . . . . ?
Fe2 O1 C1 C2 4.4(16) . . . . ?
Fe2 O1 C1 Na2 155(6) . . . . ?
O3 C1 C2 O4 -5.8(18) . . . . ?
O1 C1 C2 O4 177.1(16) . . . . ?
Na2 C1 C2 O4 2.4(12) . . . . ?
O3 C1 C2 O2 177.0(17) . . . . ?
O1 C1 C2 O2 0.0(16) . . . . ?
Na2 C1 C2 O2 -174.7(13) . . . . ?
O3 C1 C2 Na2 -8.3(13) . . . . ?
O1 C1 C2 Na2 174.7(13) . . . . ?
O4 C2 O2 Fe2 178.8(14) . . . . ?
C1 C2 O2 Fe2 -4.4(15) . . . . ?
Na2 C2 O2 Fe2 -155(5) . . . . ?
O1 C1 O3 Na2 -172.0(14) . . . . ?
C2 C1 O3 Na2 11.3(18) . . . . ?
O2 C2 O4 Na2 173.1(14) . . . . ?
C1 C2 O4 Na2 -3.5(18) . . . . ?
O5 C3 C4 O6 8.1(13) . . . . ?
O8 C3 C4 O6 -173.7(14) . . . . ?
Na1 C3 C4 O6 2.7(10) . . . . ?
O5 C3 C4 O7 -175.3(13) . . . . ?
O8 C3 C4 O7 2.9(11) . . . . ?
Na1 C3 C4 O7 179.3(10) . . . . ?
O5 C3 C4 Na1 5.4(9) . . . . ?
O8 C3 C4 Na1 -176.4(10) . . . . ?
O7 C4 O6 Na1 -180.0(10) . . . . ?
C3 C4 O6 Na1 -3.8(13) . . . . ?
O8 C3 O5 Na1 174.7(10) . . . . ?
C4 C3 O5 Na1 -7.2(12) . . . . ?
O5 C3 O8 Fe1 169.2(11) . . . . ?
C4 C3 O8 Fe1 -8.9(11) . . . . ?
O6 C4 O7 Fe1 -178.8(11) . . . . ?
C3 C4 O7 Fe1 4.8(11) . . . . ?
Na1 C4 O7 Fe1 -179(4) . . . . ?

_refine_diff_density_max         1.308
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.116

